# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Feng Luo' _publ_contact_author_email ecitluofeng@163.com _publ_author_name 'Feng Luo' data_1 _database_code_depnum_ccdc_archive 'CCDC 877925' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H44 N8 O16 Zn2' _chemical_formula_weight 1311.81 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 15.8517(5) _cell_length_b 11.2658(4) _cell_length_c 34.8339(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6220.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4467 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 24.15 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 0.846 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8490 _exptl_absorpt_correction_T_max 0.8836 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25243 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10753 _reflns_number_gt 7743 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The carbonyl oxygen atoms O13,14,15,16 have large enlongated thermal ellipsoids, indicative of disorder. However, we can not find suitable Q peak to give the disorder mode. Moreover, although no major peaks of electron density remain in the refinement, it is possible diffuse density corresponding to additional disordered solvent remains. And this is treated by Platon Squeeze program, which is attached at the end of this file. ; _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^)+(0.0968P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.199(18) _refine_ls_number_reflns 10753 _refine_ls_number_parameters 812 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1824 _refine_ls_wR_factor_gt 0.1621 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8183(6) 0.5456(11) 0.7452(3) 0.077(3) Uani 1 1 d . . . H1 H 0.8442 0.5548 0.7215 0.092 Uiso 1 1 calc R . . C2 C 0.8256(5) 0.5032(6) 0.8110(3) 0.044(2) Uani 1 1 d . . . H2 H 0.8577 0.4812 0.8321 0.053 Uiso 1 1 calc R . . C3 C 0.2558(5) 1.1406(6) 0.8356(2) 0.0398(17) Uani 1 1 d . . . H3 H 0.2758 1.1598 0.8599 0.048 Uiso 1 1 calc R . . C4 C 0.2115(5) 0.8338(6) 0.5785(2) 0.0405(18) Uani 1 1 d . . . H4 H 0.2426 0.8999 0.5861 0.049 Uiso 1 1 calc R . . C5 C 0.8271(4) 0.5648(6) 0.9080(2) 0.0335(16) Uani 1 1 d . . . C6 C 0.2011(4) 0.8750(6) 0.98996(19) 0.0364(16) Uani 1 1 d . . . H6 H 0.1930 0.8007 1.0010 0.044 Uiso 1 1 calc R . . C7 C 1.2855(5) 0.1647(6) 1.0635(3) 0.0416(17) Uani 1 1 d . . . C8 C 0.6944(5) 0.5500(7) 0.7848(2) 0.046(2) Uani 1 1 d . . . H8 H 0.6366 0.5622 0.7870 0.055 Uiso 1 1 calc R . . C9 C 0.2007(5) 0.6276(7) 0.5717(3) 0.055(2) Uani 1 1 d . . . H9 H 0.2229 0.5516 0.5746 0.066 Uiso 1 1 calc R . . C10 C 0.5477(5) 0.6585(6) 0.8644(2) 0.0420(18) Uani 1 1 d . . . C11 C 0.1457(5) 0.9663(6) 0.99839(19) 0.0353(16) Uani 1 1 d . . . C12 C 0.9305(5) 0.4551(6) 0.9490(2) 0.0389(18) Uani 1 1 d . . . H12 H 0.9035 0.3848 0.9423 0.047 Uiso 1 1 calc R . . C13 C 0.0892(5) 0.7563(6) 0.5534(3) 0.054(2) Uani 1 1 d . . . H13 H 0.0355 0.7665 0.5431 0.065 Uiso 1 1 calc R . . C14 C 1.1638(5) 0.3049(6) 1.0654(2) 0.0466(18) Uani 1 1 d . . . H14 H 1.1448 0.2649 1.0871 0.056 Uiso 1 1 calc R . . C15 C 0.9012(5) 0.5609(6) 0.9349(2) 0.0348(16) Uani 1 1 d . . . C16 C 0.3105(5) 1.1316(7) 0.8043(2) 0.0465(19) Uani 1 1 d . . . C17 C 0.2467(5) 0.7261(6) 0.5823(2) 0.0419(17) Uani 1 1 d . . . C18 C -0.0605(6) 1.0038(7) 0.6220(3) 0.061(3) Uani 1 1 d . . . H18 H -0.0914 0.9782 0.6008 0.074 Uiso 1 1 calc R . . C19 C 0.2279(5) 1.0948(6) 0.95691(18) 0.0349(16) Uani 1 1 d . . . H19 H 0.2371 1.1687 0.9458 0.042 Uiso 1 1 calc R . . C20 C 0.8652(5) 0.5160(8) 0.7766(3) 0.059(2) Uani 1 1 d . . . H20 H 0.9231 0.5046 0.7745 0.071 Uiso 1 1 calc R . . C21 C 0.4935(4) 0.7568(6) 0.8808(2) 0.0350(16) Uani 1 1 d . . . C22 C 0.4212(5) 0.7935(6) 0.8620(2) 0.0459(19) Uani 1 1 d . . . H22 H 0.4061 0.7575 0.8390 0.055 Uiso 1 1 calc R . . C23 C 0.5541(6) 1.1278(7) 0.8669(3) 0.058(2) Uani 1 1 d . . . H23 H 0.5301 1.0525 0.8658 0.070 Uiso 1 1 calc R . . C24 C 0.5118(5) 1.2248(6) 0.8527(2) 0.0413(17) Uani 1 1 d . . . C25 C 0.5041(5) 0.6483(6) 0.5985(2) 0.0445(18) Uani 1 1 d . . . H25 H 0.4825 0.6726 0.5749 0.053 Uiso 1 1 calc R . . C26 C 1.2362(4) 0.2678(6) 1.04807(19) 0.0376(16) Uani 1 1 d . . . C27 C -0.1020(7) 1.0161(9) 0.6561(3) 0.074(3) Uani 1 1 d . . . H27 H -0.1599 1.0042 0.6580 0.089 Uiso 1 1 calc R . . C28 C 0.5904(5) 0.6282(6) 0.6027(2) 0.048(2) Uani 1 1 d . . . H28 H 0.6264 0.6333 0.5817 0.057 Uiso 1 1 calc R . . C29 C 1.1464(5) 0.4604(7) 1.0205(2) 0.0448(19) Uani 1 1 d . . . C30 C 0.9400(5) 0.6666(7) 0.9454(2) 0.0445(18) Uani 1 1 d . . . H30 H 0.9202 0.7384 0.9358 0.053 Uiso 1 1 calc R . . C31 C 0.5714(5) 0.5964(10) 0.6705(2) 0.060(3) Uani 1 1 d . . . C32 C -0.0548(6) 1.0467(10) 0.6872(3) 0.063(2) Uani 1 1 d . . . H32 H -0.0801 1.0558 0.7111 0.076 Uiso 1 1 calc R . . C33 C 0.1926(5) 1.0999(8) 0.7627(3) 0.054(2) Uani 1 1 d . . . C34 C 0.0683(5) 1.0575(8) 0.6473(2) 0.051(2) Uani 1 1 d . . . H34 H 0.1253 1.0746 0.6442 0.061 Uiso 1 1 calc R . . C35 C 0.1601(5) 1.0777(6) 0.9822(2) 0.0372(17) Uani 1 1 d . . . H35 H 0.1246 1.1408 0.9881 0.045 Uiso 1 1 calc R . . C36 C 0.3714(5) 0.8820(6) 0.8767(2) 0.0471(19) Uani 1 1 d . . . H36 H 0.3221 0.9048 0.8642 0.056 Uiso 1 1 calc R . . C37 C 0.7335(6) 0.5619(9) 0.7487(2) 0.065(3) Uani 1 1 d . . . C38 C 0.4508(5) 0.6321(6) 0.6294(2) 0.0436(18) Uani 1 1 d . . . C39 C 0.4837(5) 0.6111(8) 0.6650(2) 0.060(2) Uani 1 1 d . . . H39 H 0.4478 0.6064 0.6861 0.072 Uiso 1 1 calc R . . C40 C 0.1705(5) 1.1198(7) 0.8291(2) 0.0465(19) Uani 1 1 d . . . H40 H 0.1336 1.1215 0.8499 0.056 Uiso 1 1 calc R . . C41 C 0.6667(5) 1.2555(7) 0.8835(2) 0.055(2) Uani 1 1 d . . . H41 H 0.7202 1.2644 0.8941 0.066 Uiso 1 1 calc R . . C42 C 1.0013(5) 0.4516(6) 0.9736(2) 0.050(2) Uani 1 1 d . . . H42 H 1.0223 0.3796 0.9826 0.060 Uiso 1 1 calc R . . C43 C 1.0379(4) 0.5551(6) 0.9839(2) 0.0355(16) Uani 1 1 d . . . C44 C 0.1207(5) 0.6444(6) 0.5567(3) 0.061(2) Uani 1 1 d . . . H44 H 0.0886 0.5795 0.5490 0.074 Uiso 1 1 calc R . . C45 C 0.2784(5) 1.1142(8) 0.7679(3) 0.060(2) Uani 1 1 d . . . H45 H 0.3145 1.1121 0.7469 0.072 Uiso 1 1 calc R . . C46 C 1.0081(5) 0.6645(6) 0.9701(2) 0.055(2) Uani 1 1 d . . . H46 H 1.0339 0.7349 0.9776 0.066 Uiso 1 1 calc R . . C47 C 0.3561(5) 0.6442(8) 0.6241(2) 0.053(2) Uani 1 1 d . . . C48 C 0.5501(5) 1.3367(7) 0.8546(2) 0.0436(19) Uani 1 1 d . . . H48 H 0.5214 1.4023 0.8451 0.052 Uiso 1 1 calc R . . C49 C 0.3955(5) 0.9364(6) 0.9103(2) 0.0439(18) Uani 1 1 d . . . C50 C 0.4666(5) 0.9008(7) 0.9288(2) 0.050(2) Uani 1 1 d . . . H50 H 0.4816 0.9367 0.9519 0.060 Uiso 1 1 calc R . . C51 C 1.2627(5) 0.3305(6) 1.0154(2) 0.0440(18) Uani 1 1 d . . . H51 H 1.3117 0.3075 1.0027 0.053 Uiso 1 1 calc R . . C52 C 0.2686(5) 0.8928(6) 0.96533(19) 0.0399(17) Uani 1 1 d . . . H52 H 0.3057 0.8310 0.9600 0.048 Uiso 1 1 calc R . . C53 C 0.4020(5) 1.1472(8) 0.8096(2) 0.060(2) Uani 1 1 d . . . C54 C 0.1386(5) 1.0969(8) 0.7932(2) 0.054(2) Uani 1 1 d . . . H54 H 0.0817 1.0798 0.7897 0.065 Uiso 1 1 calc R . . C55 C 1.1177(5) 0.4008(6) 1.0516(2) 0.0460(19) Uani 1 1 d . . . H55 H 1.0677 0.4235 1.0635 0.055 Uiso 1 1 calc R . . C56 C 0.5158(5) 0.8137(6) 0.9142(2) 0.0430(18) Uani 1 1 d . . . H56 H 0.5651 0.7922 0.9268 0.052 Uiso 1 1 calc R . . C57 C 0.0324(6) 1.0645(8) 0.6829(2) 0.055(2) Uani 1 1 d . . . C58 C 0.6307(6) 1.1441(7) 0.8823(3) 0.070(3) Uani 1 1 d . . . H58 H 0.6600 1.0795 0.8923 0.084 Uiso 1 1 calc R . . C59 C 0.6215(5) 0.6006(8) 0.6388(2) 0.055(2) Uani 1 1 d . . . H59 H 0.6788 0.5844 0.6414 0.066 Uiso 1 1 calc R . . C60 C 1.2164(6) 0.4264(7) 1.0017(2) 0.052(2) Uani 1 1 d . . . H60 H 1.2336 0.4666 0.9797 0.062 Uiso 1 1 calc R . . C61 C 0.2802(5) 1.0026(5) 0.9489(2) 0.0354(16) Uani 1 1 d . . . C62 C 0.6010(7) 0.5709(10) 0.7096(3) 0.075(3) Uani 1 1 d . . . C63 C 0.1605(6) 1.0744(10) 0.7232(3) 0.072(3) Uani 1 1 d . . . C64 C 0.0727(5) 0.9479(6) 1.0249(2) 0.0324(17) Uani 1 1 d . . . N1 N 0.1324(3) 0.8513(5) 0.5642(2) 0.0406(14) Uani 1 1 d . . . N2 N 0.3304(4) 0.7153(5) 0.5953(2) 0.0481(17) Uani 1 1 d . . . H2A H 0.3681 0.7575 0.5840 0.058 Uiso 1 1 calc R . . N3 N 0.6854(5) 0.5917(8) 0.7160(2) 0.070(2) Uani 1 1 d . . . H3A H 0.7121 0.6273 0.6978 0.084 Uiso 1 1 calc R . . N4 N 0.7398(5) 0.5214(5) 0.81617(17) 0.0391(15) Uani 1 1 d . . . N5 N 0.4267(4) 1.2147(5) 0.84008(19) 0.0446(16) Uani 1 1 d . . . H5 H 0.3886 1.2534 0.8524 0.054 Uiso 1 1 calc R . . N6 N 0.0783(5) 1.0988(8) 0.7165(2) 0.070(2) Uani 1 1 d . . . H6A H 0.0515 1.1379 0.7338 0.084 Uiso 1 1 calc R . . N7 N 0.0217(4) 1.0261(5) 0.61695(18) 0.0438(16) Uani 1 1 d . . . N8 N 0.6268(4) 1.3515(5) 0.86969(17) 0.0419(14) Uani 1 1 d . . . O1 O 0.9655(6) 0.2348(8) 0.7639(2) 0.125(3) Uani 1 1 d . . . O2 O 0.7977(6) 0.7337(9) 0.6663(2) 0.127(3) Uani 1 1 d . . . O3 O 0.7812(3) 0.4717(4) 0.90512(16) 0.0415(13) Uani 1 1 d . . . O4 O 0.8127(4) 0.6565(5) 0.88985(15) 0.0550(14) Uani 1 1 d . . . O5 O 1.2620(4) 0.1133(5) 1.09276(19) 0.0666(17) Uani 1 1 d . . . O6 O 1.3524(3) 0.1385(4) 1.04497(16) 0.0511(14) Uani 1 1 d . . . O7 O 1.1081(4) 0.5637(4) 1.00820(17) 0.0577(16) Uani 1 1 d . . . O8 O 0.6119(3) 0.6300(5) 0.88439(17) 0.0524(14) Uani 1 1 d . . . O9 O 0.5270(4) 0.6104(4) 0.83394(17) 0.0590(15) Uani 1 1 d . . . O10 O 0.3471(4) 1.0305(4) 0.92373(16) 0.0507(14) Uani 1 1 d . . . O11 O 0.0679(3) 0.8536(5) 1.04364(15) 0.0532(14) Uani 1 1 d . . . O12 O 0.0173(3) 1.0284(4) 1.02642(14) 0.0411(12) Uani 1 1 d . . . O13 O 0.4558(4) 1.0948(9) 0.7894(2) 0.119(4) Uani 1 1 d . . . O14 O 0.2071(5) 1.0330(11) 0.6968(2) 0.133(4) Uani 1 1 d . . . O15 O 0.3072(4) 0.5928(8) 0.6453(2) 0.105(3) Uani 1 1 d . . . O16 O 0.5563(5) 0.5290(12) 0.7344(3) 0.155(5) Uani 1 1 d . . . Zn1 Zn 0.07286(5) 1.01470(7) 0.56262(2) 0.0372(2) Uani 1 1 d . . . Zn2 Zn 0.68917(6) 0.51091(7) 0.86834(2) 0.0364(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 C1 0.037(6) 0.113(8) 0.080(7) 0.014(7) 0.006(5) 0.017(6) C2 0.030(5) 0.054(5) 0.048(6) -0.002(3) -0.011(4) 0.020(4) C3 0.034(4) 0.042(3) 0.043(4) -0.006(3) -0.004(4) -0.006(4) C4 0.029(4) 0.043(4) 0.050(4) 0.012(3) -0.015(4) -0.009(4) C5 0.025(4) 0.042(4) 0.033(4) 0.004(3) -0.002(3) 0.000(3) C6 0.028(4) 0.036(3) 0.045(4) 0.003(3) 0.010(3) 0.008(3) C7 0.027(4) 0.042(4) 0.056(5) 0.001(4) -0.006(4) 0.004(3) C8 0.036(5) 0.071(5) 0.032(4) -0.004(4) -0.002(3) 0.005(4) C9 0.035(5) 0.041(4) 0.088(6) 0.005(4) -0.016(5) 0.000(4) C10 0.030(4) 0.046(4) 0.050(5) -0.002(4) 0.007(4) 0.000(4) C11 0.025(4) 0.045(4) 0.036(4) -0.001(3) 0.001(3) 0.006(3) C12 0.037(5) 0.029(3) 0.051(4) -0.004(3) -0.013(4) 0.011(3) C13 0.030(4) 0.047(4) 0.085(6) 0.007(4) -0.020(4) 0.001(4) C14 0.036(4) 0.040(3) 0.064(5) -0.001(4) 0.006(4) 0.000(4) C15 0.020(4) 0.039(4) 0.045(4) -0.001(3) -0.010(3) 0.000(3) C16 0.025(4) 0.068(5) 0.047(4) -0.019(4) -0.009(4) -0.001(4) C17 0.018(4) 0.049(4) 0.059(4) 0.012(3) -0.006(4) 0.007(4) C18 0.056(7) 0.079(7) 0.049(7) 0.000(4) -0.006(5) -0.024(5) C19 0.030(4) 0.042(3) 0.033(3) -0.001(3) 0.008(3) 0.002(3) C20 0.025(4) 0.102(7) 0.051(5) 0.000(4) -0.009(4) 0.021(5) C21 0.018(4) 0.045(4) 0.042(4) 0.003(3) 0.006(3) 0.001(3) C22 0.040(5) 0.047(4) 0.051(4) -0.007(4) 0.000(4) 0.000(4) C23 0.043(5) 0.045(4) 0.086(6) 0.009(5) -0.007(5) -0.010(4) C24 0.023(4) 0.052(4) 0.049(4) 0.003(3) -0.010(4) -0.001(4) C25 0.035(4) 0.040(4) 0.059(5) 0.006(3) -0.012(4) 0.004(4) C26 0.026(4) 0.045(4) 0.041(4) -0.005(3) 0.001(3) 0.010(3) C27 0.053(6) 0.124(9) 0.046(6) 0.008(5) -0.004(5) 0.005(6) C28 0.047(5) 0.050(4) 0.046(4) 0.011(4) 0.004(4) 0.009(4) C29 0.033(4) 0.055(4) 0.046(4) -0.006(4) -0.018(4) 0.020(4) C30 0.031(4) 0.049(4) 0.054(4) 0.006(3) -0.012(4) 0.000(4) C31 0.027(4) 0.118(8) 0.037(4) 0.022(5) -0.005(4) -0.008(5) C32 0.033(5) 0.107(7) 0.049(5) -0.008(5) -0.002(4) -0.001(5) C33 0.037(5) 0.063(5) 0.063(5) -0.011(4) -0.018(4) -0.007(4) C34 0.032(5) 0.067(5) 0.053(5) -0.003(4) -0.008(4) -0.006(4) C35 0.028(4) 0.036(3) 0.048(4) -0.008(3) 0.004(4) 0.008(3) C36 0.029(4) 0.053(4) 0.059(5) -0.001(4) 0.003(4) 0.000(4) C37 0.049(6) 0.112(7) 0.035(4) 0.010(5) -0.008(4) 0.019(6) C38 0.038(5) 0.053(4) 0.040(4) 0.009(3) -0.003(4) 0.001(4) C39 0.032(5) 0.101(7) 0.048(5) 0.016(4) -0.004(4) -0.010(5) C40 0.023(4) 0.056(5) 0.061(5) -0.011(4) -0.006(4) 0.003(4) C41 0.036(5) 0.053(5) 0.076(6) 0.004(4) -0.019(4) 0.000(4) C42 0.046(5) 0.046(4) 0.057(5) -0.001(4) -0.017(4) 0.021(4) C43 0.019(4) 0.036(4) 0.052(4) -0.004(3) -0.003(3) 0.005(3) C44 0.045(5) 0.038(4) 0.101(7) -0.004(4) -0.032(5) -0.009(4) C45 0.037(5) 0.084(6) 0.061(5) -0.016(4) 0.007(4) -0.015(5) C46 0.045(5) 0.045(4) 0.074(5) 0.002(4) -0.014(5) -0.007(4) C47 0.023(4) 0.073(5) 0.062(5) 0.016(4) -0.010(4) -0.006(4) C48 0.028(4) 0.051(4) 0.052(5) 0.004(3) -0.007(4) -0.002(4) C49 0.032(4) 0.049(4) 0.050(4) 0.003(3) 0.015(4) 0.002(4) C50 0.053(5) 0.059(4) 0.039(4) -0.009(3) 0.011(4) 0.007(4) C51 0.041(5) 0.054(4) 0.037(4) -0.004(3) 0.003(4) 0.015(4) C52 0.027(4) 0.045(4) 0.048(4) -0.002(3) 0.006(4) 0.008(4) C53 0.023(4) 0.088(6) 0.070(6) -0.031(5) -0.008(4) 0.004(5) C54 0.021(4) 0.093(6) 0.048(5) -0.004(4) -0.006(4) -0.015(5) C55 0.023(4) 0.053(4) 0.062(5) -0.002(4) 0.005(4) 0.014(4) C56 0.035(4) 0.048(4) 0.046(4) -0.007(3) -0.001(4) 0.010(4) C57 0.044(5) 0.076(6) 0.046(5) -0.012(4) -0.001(4) 0.002(5) C58 0.048(6) 0.041(4) 0.120(8) 0.010(4) -0.042(6) -0.004(4) C59 0.035(5) 0.089(6) 0.041(4) 0.000(4) 0.001(4) 0.012(5) C60 0.058(6) 0.058(5) 0.040(4) 0.007(3) 0.002(4) 0.004(4) C61 0.027(4) 0.044(4) 0.035(4) 0.000(3) 0.006(3) 0.003(3) C62 0.048(6) 0.114(8) 0.063(6) 0.018(6) -0.021(5) -0.020(6) C63 0.020(5) 0.127(9) 0.070(6) -0.011(6) -0.004(5) -0.001(6) C64 0.025(4) 0.042(4) 0.031(4) -0.002(3) 0.003(3) -0.009(3) N1 0.019(3) 0.038(3) 0.064(4) 0.002(3) -0.005(3) 0.001(3) N2 0.021(3) 0.047(3) 0.076(5) 0.013(3) -0.001(3) 0.001(3) N3 0.044(5) 0.122(7) 0.045(4) 0.030(4) 0.009(4) -0.010(5) N4 0.042(4) 0.046(3) 0.030(3) -0.006(3) -0.001(3) 0.012(3) N5 0.023(3) 0.051(3) 0.060(4) -0.017(3) -0.005(3) -0.003(3) N6 0.046(5) 0.102(6) 0.063(5) -0.003(4) -0.012(4) -0.002(4) N7 0.033(4) 0.051(3) 0.047(4) -0.003(3) -0.015(4) -0.005(3) N8 0.039(4) 0.041(3) 0.046(3) 0.004(3) -0.013(3) 0.004(3) O1 0.121(7) 0.160(8) 0.095(6) 0.002(5) 0.019(6) 0.046(7) O2 0.103(7) 0.176(9) 0.101(6) 0.027(6) -0.002(5) -0.043(6) O3 0.025(3) 0.048(3) 0.052(3) 0.000(2) -0.014(3) -0.010(2) O4 0.054(4) 0.058(3) 0.054(3) 0.013(3) -0.023(3) -0.008(3) O5 0.059(4) 0.066(3) 0.074(4) 0.022(3) 0.000(3) 0.013(3) O6 0.043(3) 0.044(3) 0.067(4) 0.004(2) 0.007(3) 0.013(3) O7 0.046(4) 0.041(3) 0.086(4) -0.004(3) -0.029(3) 0.009(3) O8 0.029(3) 0.050(3) 0.078(4) -0.005(3) -0.001(3) 0.012(3) O9 0.056(4) 0.056(3) 0.066(4) -0.014(3) 0.003(3) 0.007(3) O10 0.048(3) 0.041(3) 0.064(3) 0.006(2) 0.031(3) 0.014(3) O11 0.049(4) 0.055(3) 0.055(3) 0.009(2) 0.005(3) -0.004(3) O12 0.030(3) 0.052(3) 0.042(3) 0.008(2) 0.012(2) 0.005(3) O13 0.043(4) 0.221(10) 0.092(5) -0.093(6) -0.011(4) 0.021(6) O14 0.057(5) 0.280(12) 0.062(5) -0.041(6) 0.000(4) 0.039(7) O15 0.033(4) 0.181(8) 0.101(5) 0.070(6) 0.005(4) -0.009(5) O16 0.044(5) 0.342(15) 0.080(7) 0.098(8) -0.001(4) -0.018(7) Zn1 0.0310(5) 0.0418(4) 0.0387(5) 0.0018(5) -0.0066(4) -0.0013(4) Zn2 0.0285(4) 0.0434(5) 0.0373(5) -0.0002(4) -0.0062(4) 0.0074(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C37 1.362(12) . ? C1 C20 1.361(13) . ? C1 H1 0.9300 . ? C2 C20 1.361(14) . ? C2 N4 1.387(10) . ? C2 H2 0.9300 . ? C3 C40 1.392(10) . ? C3 C16 1.397(10) . ? C3 H3 0.9300 . ? C4 C17 1.343(9) . ? C4 N1 1.364(9) . ? C4 H4 0.9300 . ? C5 O4 1.232(8) . ? C5 O3 1.281(8) . ? C5 C15 1.505(9) . ? C6 C11 1.385(9) . ? C6 C52 1.385(9) . ? C6 H6 0.9300 . ? C7 O5 1.229(9) . ? C7 O6 1.277(9) . ? C7 C26 1.500(9) . ? C8 N4 1.347(10) . ? C8 C37 1.409(11) . ? C8 H8 0.9300 . ? C9 C44 1.385(11) . ? C9 C17 1.378(10) . ? C9 H9 0.9300 . ? C10 O9 1.237(9) . ? C10 O8 1.274(10) . ? C10 C21 1.513(10) . ? C11 C35 1.395(10) . ? C11 C64 1.494(10) . ? C12 C15 1.370(9) . ? C12 C42 1.414(10) . ? C12 H12 0.9300 . ? C13 N1 1.325(9) . ? C13 C44 1.361(10) . ? C13 H13 0.9300 . ? C14 C26 1.363(10) . ? C14 C55 1.391(10) . ? C14 H14 0.9300 . ? C15 C30 1.388(10) . ? C16 C45 1.379(11) . ? C16 C53 1.472(10) . ? C17 N2 1.406(9) . ? C18 N7 1.338(11) . ? C18 C27 1.366(15) . ? C18 H18 0.9300 . ? C19 C61 1.357(9) . ? C19 C35 1.403(10) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C56 1.372(9) . ? C21 C22 1.383(10) . ? C22 C36 1.371(10) . ? C22 H22 0.9300 . ? C23 C58 1.341(12) . ? C23 C24 1.373(10) . ? C23 H23 0.9300 . ? C24 C48 1.401(10) . ? C24 N5 1.424(9) . ? C25 C38 1.380(10) . ? C25 C28 1.395(10) . ? C25 H25 0.9300 . ? C26 C51 1.405(10) . ? C27 C32 1.362(13) . ? C27 H27 0.9300 . ? C28 C59 1.384(10) . ? C28 H28 0.9300 . ? C29 C55 1.354(10) . ? C29 C60 1.344(11) . ? C29 O7 1.381(9) . ? C30 C46 1.381(10) . ? C30 H30 0.9300 . ? C31 C59 1.361(11) . ? C31 C39 1.412(11) . ? C31 C62 1.469(12) . ? C32 C57 1.406(12) . ? C32 H32 0.9300 . ? C33 C45 1.382(11) . ? C33 C54 1.364(11) . ? C33 C63 1.496(12) . ? C34 N7 1.337(10) . ? C34 C57 1.366(11) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C49 1.373(11) . ? C36 H36 0.9300 . ? C37 N3 1.412(10) . ? C38 C39 1.369(10) . ? C38 C47 1.518(10) . ? C39 H39 0.9300 . ? C40 C54 1.374(10) . ? C40 H40 0.9300 . ? C41 N8 1.342(9) . ? C41 C58 1.379(11) . ? C41 H41 0.9300 . ? C42 C43 1.350(10) . ? C42 H42 0.9300 . ? C43 C46 1.404(10) . ? C43 O7 1.403(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 O15 1.217(9) . ? C47 N2 1.345(10) . ? C48 N8 1.334(10) . ? C48 H48 0.9300 . ? C49 C50 1.359(11) . ? C49 O10 1.390(9) . ? C50 C56 1.353(10) . ? C50 H50 0.9300 . ? C51 C60 1.390(10) . ? C51 H51 0.9300 . ? C52 C61 1.376(9) . ? C52 H52 0.9300 . ? C53 O13 1.253(10) . ? C53 N5 1.364(10) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 N6 1.431(11) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 O10 1.411(9) . ? C62 O16 1.214(12) . ? C62 N3 1.377(11) . ? C63 O14 1.266(12) . ? C63 N6 1.352(11) . ? C64 O11 1.249(9) . ? C64 O12 1.264(9) . ? N1 Zn1 2.070(5) . ? N2 H2A 0.8600 . ? N3 H3A 0.8600 . ? N4 Zn2 1.990(6) . ? N5 H5 0.8600 . ? N6 H6A 0.8600 . ? N7 Zn1 2.063(7) . ? N8 Zn2 2.051(6) 1_565 ? O3 Zn2 1.991(5) . ? O6 Zn1 1.931(5) 3_645 ? O8 Zn2 1.900(5) . ? O12 Zn1 1.967(5) 2_575 ? Zn1 O6 1.931(5) 3_664 ? Zn1 O12 1.967(5) 2_574 ? Zn2 N8 2.051(6) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 C1 C20 120.0(10) . . ? C37 C1 H1 120.0 . . ? C20 C1 H1 120.0 . . ? C20 C2 N4 123.5(8) . . ? C20 C2 H2 118.3 . . ? N4 C2 H2 118.3 . . ? C40 C3 C16 117.7(7) . . ? C40 C3 H3 121.2 . . ? C16 C3 H3 121.2 . . ? C17 C4 N1 123.3(7) . . ? C17 C4 H4 118.4 . . ? N1 C4 H4 118.4 . . ? O4 C5 O3 122.8(7) . . ? O4 C5 C15 119.2(6) . . ? O3 C5 C15 118.0(6) . . ? C11 C6 C52 120.9(6) . . ? C11 C6 H6 119.5 . . ? C52 C6 H6 119.5 . . ? O5 C7 O6 124.2(7) . . ? O5 C7 C26 120.4(7) . . ? O6 C7 C26 115.4(7) . . ? N4 C8 C37 120.8(7) . . ? N4 C8 H8 119.6 . . ? C37 C8 H8 119.6 . . ? C44 C9 C17 118.4(7) . . ? C44 C9 H9 120.8 . . ? C17 C9 H9 120.8 . . ? O9 C10 O8 124.7(7) . . ? O9 C10 C21 119.6(7) . . ? O8 C10 C21 115.6(7) . . ? C6 C11 C35 118.6(6) . . ? C6 C11 C64 121.3(6) . . ? C35 C11 C64 120.1(6) . . ? C15 C12 C42 120.7(7) . . ? C15 C12 H12 119.7 . . ? C42 C12 H12 119.7 . . ? N1 C13 C44 122.2(7) . . ? N1 C13 H13 118.9 . . ? C44 C13 H13 118.9 . . ? C26 C14 C55 121.8(8) . . ? C26 C14 H14 119.1 . . ? C55 C14 H14 119.1 . . ? C12 C15 C30 120.2(6) . . ? C12 C15 C5 120.8(6) . . ? C30 C15 C5 119.0(6) . . ? C45 C16 C3 119.9(7) . . ? C45 C16 C53 119.7(7) . . ? C3 C16 C53 120.3(7) . . ? C4 C17 C9 118.8(7) . . ? C4 C17 N2 120.1(7) . . ? C9 C17 N2 121.0(6) . . ? N7 C18 C27 124.3(10) . . ? N7 C18 H18 117.9 . . ? C27 C18 H18 117.9 . . ? C61 C19 C35 119.5(6) . . ? C61 C19 H19 120.2 . . ? C35 C19 H19 120.2 . . ? C2 C20 C1 118.7(8) . . ? C2 C20 H20 120.6 . . ? C1 C20 H20 120.6 . . ? C56 C21 C22 118.3(7) . . ? C56 C21 C10 121.0(7) . . ? C22 C21 C10 120.7(7) . . ? C36 C22 C21 121.2(7) . . ? C36 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C58 C23 C24 118.5(7) . . ? C58 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C23 C24 C48 119.2(7) . . ? C23 C24 N5 120.7(7) . . ? C48 C24 N5 119.8(7) . . ? C38 C25 C28 119.8(7) . . ? C38 C25 H25 120.1 . . ? C28 C25 H25 120.1 . . ? C14 C26 C51 117.2(7) . . ? C14 C26 C7 121.1(7) . . ? C51 C26 C7 121.7(7) . . ? C32 C27 C18 117.0(10) . . ? C32 C27 H27 121.5 . . ? C18 C27 H27 121.5 . . ? C59 C28 C25 118.9(8) . . ? C59 C28 H28 120.6 . . ? C25 C28 H28 120.6 . . ? C55 C29 C60 121.8(7) . . ? C55 C29 O7 121.3(7) . . ? C60 C29 O7 116.8(7) . . ? C46 C30 C15 119.7(7) . . ? C46 C30 H30 120.2 . . ? C15 C30 H30 120.2 . . ? C59 C31 C39 117.5(7) . . ? C59 C31 C62 124.9(8) . . ? C39 C31 C62 117.5(8) . . ? C27 C32 C57 119.4(9) . . ? C27 C32 H32 120.3 . . ? C57 C32 H32 120.3 . . ? C45 C33 C54 121.2(8) . . ? C45 C33 C63 118.6(8) . . ? C54 C33 C63 120.0(7) . . ? N7 C34 C57 120.2(8) . . ? N7 C34 H34 119.9 . . ? C57 C34 H34 119.9 . . ? C11 C35 C19 120.2(6) . . ? C11 C35 H35 119.9 . . ? C19 C35 H35 119.9 . . ? C22 C36 C49 118.8(8) . . ? C22 C36 H36 120.6 . . ? C49 C36 H36 120.6 . . ? C1 C37 N3 119.6(9) . . ? C1 C37 C8 120.1(8) . . ? N3 C37 C8 120.4(8) . . ? C39 C38 C25 119.8(7) . . ? C39 C38 C47 120.2(7) . . ? C25 C38 C47 119.9(7) . . ? C38 C39 C31 121.2(8) . . ? C38 C39 H39 119.4 . . ? C31 C39 H39 119.4 . . ? C54 C40 C3 122.5(7) . . ? C54 C40 H40 118.8 . . ? C3 C40 H40 118.8 . . ? N8 C41 C58 121.9(7) . . ? N8 C41 H41 119.1 . . ? C58 C41 H41 119.1 . . ? C43 C42 C12 118.5(7) . . ? C43 C42 H42 120.8 . . ? C12 C42 H42 120.8 . . ? C42 C43 C46 121.6(7) . . ? C42 C43 O7 124.1(6) . . ? C46 C43 O7 114.3(6) . . ? C13 C44 C9 119.7(7) . . ? C13 C44 H44 120.1 . . ? C9 C44 H44 120.1 . . ? C33 C45 C16 120.1(8) . . ? C33 C45 H45 119.9 . . ? C16 C45 H45 119.9 . . ? C30 C46 C43 119.4(7) . . ? C30 C46 H46 120.3 . . ? C43 C46 H46 120.3 . . ? O15 C47 N2 122.8(7) . . ? O15 C47 C38 120.8(7) . . ? N2 C47 C38 116.4(7) . . ? N8 C48 C24 121.7(7) . . ? N8 C48 H48 119.1 . . ? C24 C48 H48 119.1 . . ? C50 C49 C36 120.2(7) . . ? C50 C49 O10 121.5(7) . . ? C36 C49 O10 118.2(7) . . ? C49 C50 C56 120.8(7) . . ? C49 C50 H50 119.6 . . ? C56 C50 H50 119.6 . . ? C60 C51 C26 120.7(7) . . ? C60 C51 H51 119.6 . . ? C26 C51 H51 119.6 . . ? C61 C52 C6 119.4(6) . . ? C61 C52 H52 120.3 . . ? C6 C52 H52 120.3 . . ? O13 C53 N5 120.2(7) . . ? O13 C53 C16 123.0(7) . . ? N5 C53 C16 116.6(7) . . ? C40 C54 C33 118.3(7) . . ? C40 C54 H54 120.8 . . ? C33 C54 H54 120.8 . . ? C29 C55 C14 119.0(7) . . ? C29 C55 H55 120.5 . . ? C14 C55 H55 120.5 . . ? C50 C56 C21 120.6(7) . . ? C50 C56 H56 119.7 . . ? C21 C56 H56 119.7 . . ? C34 C57 C32 119.9(8) . . ? C34 C57 N6 123.1(8) . . ? C32 C57 N6 116.8(8) . . ? C23 C58 C41 120.7(8) . . ? C23 C58 H58 119.6 . . ? C41 C58 H58 119.6 . . ? C31 C59 C28 122.4(8) . . ? C31 C59 H59 118.8 . . ? C28 C59 H59 118.8 . . ? C29 C60 C51 119.4(7) . . ? C29 C60 H60 120.3 . . ? C51 C60 H60 120.3 . . ? C19 C61 C52 121.3(7) . . ? C19 C61 O10 114.6(6) . . ? C52 C61 O10 124.0(6) . . ? O16 C62 N3 121.3(9) . . ? O16 C62 C31 123.3(9) . . ? N3 C62 C31 115.4(9) . . ? O14 C63 N6 120.8(9) . . ? O14 C63 C33 122.7(8) . . ? N6 C63 C33 116.5(9) . . ? O11 C64 O12 123.1(7) . . ? O11 C64 C11 119.3(7) . . ? O12 C64 C11 117.6(6) . . ? C13 N1 C4 117.6(6) . . ? C13 N1 Zn1 118.4(5) . . ? C4 N1 Zn1 123.9(5) . . ? C47 N2 C17 125.3(7) . . ? C47 N2 H2A 117.4 . . ? C17 N2 H2A 117.4 . . ? C62 N3 C37 128.0(8) . . ? C62 N3 H3A 116.0 . . ? C37 N3 H3A 116.0 . . ? C8 N4 C2 116.9(7) . . ? C8 N4 Zn2 122.7(5) . . ? C2 N4 Zn2 120.3(6) . . ? C53 N5 C24 123.9(7) . . ? C53 N5 H5 118.0 . . ? C24 N5 H5 118.0 . . ? C63 N6 C57 125.1(9) . . ? C63 N6 H6A 117.4 . . ? C57 N6 H6A 117.4 . . ? C34 N7 C18 119.0(8) . . ? C34 N7 Zn1 121.6(5) . . ? C18 N7 Zn1 119.4(6) . . ? C41 N8 C48 118.0(7) . . ? C41 N8 Zn2 119.1(5) . 1_565 ? C48 N8 Zn2 122.7(5) . 1_565 ? C5 O3 Zn2 106.6(4) . . ? C7 O6 Zn1 121.0(5) . 3_645 ? C29 O7 C43 118.6(6) . . ? C10 O8 Zn2 122.2(5) . . ? C49 O10 C61 117.1(5) . . ? C64 O12 Zn1 110.8(4) . 2_575 ? O6 Zn1 O12 114.9(2) 3_664 2_574 ? O6 Zn1 N7 119.2(2) 3_664 . ? O12 Zn1 N7 108.5(2) 2_574 . ? O6 Zn1 N1 111.8(2) 3_664 . ? O12 Zn1 N1 97.4(2) 2_574 . ? N7 Zn1 N1 102.1(3) . . ? O8 Zn2 N4 119.1(2) . . ? O8 Zn2 O3 116.1(2) . . ? N4 Zn2 O3 107.8(3) . . ? O8 Zn2 N8 107.5(3) . 1_545 ? N4 Zn2 N8 105.5(2) . 1_545 ? O3 Zn2 N8 98.3(2) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C52 C6 C11 C35 -1.3(11) . . . . ? C52 C6 C11 C64 179.9(6) . . . . ? C42 C12 C15 C30 -1.3(11) . . . . ? C42 C12 C15 C5 178.6(7) . . . . ? O4 C5 C15 C12 -165.4(7) . . . . ? O3 C5 C15 C12 14.8(10) . . . . ? O4 C5 C15 C30 14.5(11) . . . . ? O3 C5 C15 C30 -165.3(7) . . . . ? C40 C3 C16 C45 6.2(11) . . . . ? C40 C3 C16 C53 -177.2(8) . . . . ? N1 C4 C17 C9 -0.9(12) . . . . ? N1 C4 C17 N2 176.5(7) . . . . ? C44 C9 C17 C4 1.6(13) . . . . ? C44 C9 C17 N2 -175.8(8) . . . . ? N4 C2 C20 C1 -1.4(14) . . . . ? C37 C1 C20 C2 -0.1(17) . . . . ? O9 C10 C21 C56 -178.5(7) . . . . ? O8 C10 C21 C56 3.0(10) . . . . ? O9 C10 C21 C22 -0.2(11) . . . . ? O8 C10 C21 C22 -178.7(7) . . . . ? C56 C21 C22 C36 -1.9(11) . . . . ? C10 C21 C22 C36 179.7(7) . . . . ? C58 C23 C24 C48 0.4(13) . . . . ? C58 C23 C24 N5 -172.9(8) . . . . ? C55 C14 C26 C51 -0.1(11) . . . . ? C55 C14 C26 C7 179.6(7) . . . . ? O5 C7 C26 C14 -1.5(11) . . . . ? O6 C7 C26 C14 -179.7(7) . . . . ? O5 C7 C26 C51 178.2(7) . . . . ? O6 C7 C26 C51 0.0(10) . . . . ? N7 C18 C27 C32 -3.9(15) . . . . ? C38 C25 C28 C59 -4.7(11) . . . . ? C12 C15 C30 C46 -0.2(11) . . . . ? C5 C15 C30 C46 180.0(7) . . . . ? C18 C27 C32 C57 0.4(15) . . . . ? C6 C11 C35 C19 2.0(11) . . . . ? C64 C11 C35 C19 -179.2(6) . . . . ? C61 C19 C35 C11 -1.0(11) . . . . ? C21 C22 C36 C49 1.6(11) . . . . ? C20 C1 C37 N3 -179.5(10) . . . . ? C20 C1 C37 C8 1.1(17) . . . . ? N4 C8 C37 C1 -0.8(15) . . . . ? N4 C8 C37 N3 179.9(8) . . . . ? C28 C25 C38 C39 8.2(11) . . . . ? C28 C25 C38 C47 -175.1(7) . . . . ? C25 C38 C39 C31 -5.0(14) . . . . ? C47 C38 C39 C31 178.3(9) . . . . ? C59 C31 C39 C38 -1.8(15) . . . . ? C62 C31 C39 C38 -178.4(9) . . . . ? C16 C3 C40 C54 -3.2(11) . . . . ? C15 C12 C42 C43 2.0(12) . . . . ? C12 C42 C43 C46 -1.2(12) . . . . ? C12 C42 C43 O7 179.8(7) . . . . ? N1 C13 C44 C9 -0.4(15) . . . . ? C17 C9 C44 C13 -1.0(14) . . . . ? C54 C33 C45 C16 -3.2(15) . . . . ? C63 C33 C45 C16 -176.6(8) . . . . ? C3 C16 C45 C33 -3.2(13) . . . . ? C53 C16 C45 C33 -179.8(8) . . . . ? C15 C30 C46 C43 0.9(12) . . . . ? C42 C43 C46 C30 -0.2(12) . . . . ? O7 C43 C46 C30 178.9(7) . . . . ? C39 C38 C47 O15 -29.1(14) . . . . ? C25 C38 C47 O15 154.2(9) . . . . ? C39 C38 C47 N2 150.1(8) . . . . ? C25 C38 C47 N2 -26.6(11) . . . . ? C23 C24 C48 N8 0.2(12) . . . . ? N5 C24 C48 N8 173.5(7) . . . . ? C22 C36 C49 C50 -1.5(11) . . . . ? C22 C36 C49 O10 176.4(7) . . . . ? C36 C49 C50 C56 1.7(12) . . . . ? O10 C49 C50 C56 -176.1(7) . . . . ? C14 C26 C51 C60 0.2(11) . . . . ? C7 C26 C51 C60 -179.5(7) . . . . ? C11 C6 C52 C61 -0.4(11) . . . . ? C45 C16 C53 O13 -34.5(14) . . . . ? C3 C16 C53 O13 148.9(10) . . . . ? C45 C16 C53 N5 151.0(8) . . . . ? C3 C16 C53 N5 -25.6(12) . . . . ? C3 C40 C54 C33 -2.9(13) . . . . ? C45 C33 C54 C40 6.1(14) . . . . ? C63 C33 C54 C40 179.5(8) . . . . ? C60 C29 C55 C14 2.9(12) . . . . ? O7 C29 C55 C14 -172.8(7) . . . . ? C26 C14 C55 C29 -1.4(12) . . . . ? C49 C50 C56 C21 -2.1(12) . . . . ? C22 C21 C56 C50 2.1(11) . . . . ? C10 C21 C56 C50 -179.5(7) . . . . ? N7 C34 C57 C32 -4.4(14) . . . . ? N7 C34 C57 N6 -179.3(8) . . . . ? C27 C32 C57 C34 3.6(15) . . . . ? C27 C32 C57 N6 178.8(9) . . . . ? C24 C23 C58 C41 -0.7(16) . . . . ? N8 C41 C58 C23 0.5(15) . . . . ? C39 C31 C59 C28 5.4(15) . . . . ? C62 C31 C59 C28 -178.2(10) . . . . ? C25 C28 C59 C31 -2.3(13) . . . . ? C55 C29 C60 C51 -2.8(12) . . . . ? O7 C29 C60 C51 173.1(7) . . . . ? C26 C51 C60 C29 1.2(12) . . . . ? C35 C19 C61 C52 -0.8(11) . . . . ? C35 C19 C61 O10 -178.8(6) . . . . ? C6 C52 C61 C19 1.5(11) . . . . ? C6 C52 C61 O10 179.4(7) . . . . ? C59 C31 C62 O16 -154.4(13) . . . . ? C39 C31 C62 O16 21.9(19) . . . . ? C59 C31 C62 N3 22.1(17) . . . . ? C39 C31 C62 N3 -161.6(10) . . . . ? C45 C33 C63 O14 20.4(17) . . . . ? C54 C33 C63 O14 -153.2(12) . . . . ? C45 C33 C63 N6 -159.2(10) . . . . ? C54 C33 C63 N6 27.3(14) . . . . ? C6 C11 C64 O11 9.5(11) . . . . ? C35 C11 C64 O11 -169.3(7) . . . . ? C6 C11 C64 O12 -168.7(6) . . . . ? C35 C11 C64 O12 12.5(10) . . . . ? C44 C13 N1 C4 1.1(13) . . . . ? C44 C13 N1 Zn1 -174.0(7) . . . . ? C17 C4 N1 C13 -0.5(12) . . . . ? C17 C4 N1 Zn1 174.4(6) . . . . ? O15 C47 N2 C17 -9.9(14) . . . . ? C38 C47 N2 C17 170.9(7) . . . . ? C4 C17 N2 C47 129.3(9) . . . . ? C9 C17 N2 C47 -53.4(12) . . . . ? O16 C62 N3 C37 5(2) . . . . ? C31 C62 N3 C37 -171.3(10) . . . . ? C1 C37 N3 C62 154.4(12) . . . . ? C8 C37 N3 C62 -26.3(16) . . . . ? C37 C8 N4 C2 -0.6(11) . . . . ? C37 C8 N4 Zn2 177.0(7) . . . . ? C20 C2 N4 C8 1.7(11) . . . . ? C20 C2 N4 Zn2 -176.0(6) . . . . ? O13 C53 N5 C24 -4.2(14) . . . . ? C16 C53 N5 C24 170.5(7) . . . . ? C23 C24 N5 C53 -64.5(11) . . . . ? C48 C24 N5 C53 122.3(9) . . . . ? O14 C63 N6 C57 10.5(18) . . . . ? C33 C63 N6 C57 -169.9(8) . . . . ? C34 C57 N6 C63 -33.4(15) . . . . ? C32 C57 N6 C63 151.6(10) . . . . ? C57 C34 N7 C18 1.1(12) . . . . ? C57 C34 N7 Zn1 179.8(6) . . . . ? C27 C18 N7 C34 3.2(14) . . . . ? C27 C18 N7 Zn1 -175.6(7) . . . . ? C58 C41 N8 C48 0.0(12) . . . . ? C58 C41 N8 Zn2 -174.7(7) . . . 1_565 ? C24 C48 N8 C41 -0.4(12) . . . . ? C24 C48 N8 Zn2 174.1(6) . . . 1_565 ? O4 C5 O3 Zn2 -1.0(8) . . . . ? C15 C5 O3 Zn2 178.7(5) . . . . ? O5 C7 O6 Zn1 -2.0(11) . . . 3_645 ? C26 C7 O6 Zn1 176.1(4) . . . 3_645 ? C55 C29 O7 C43 -84.8(9) . . . . ? C60 C29 O7 C43 99.2(9) . . . . ? C42 C43 O7 C29 4.6(11) . . . . ? C46 C43 O7 C29 -174.5(7) . . . . ? O9 C10 O8 Zn2 2.8(11) . . . . ? C21 C10 O8 Zn2 -178.8(4) . . . . ? C50 C49 O10 C61 -91.9(9) . . . . ? C36 C49 O10 C61 90.2(9) . . . . ? C19 C61 O10 C49 -171.3(6) . . . . ? C52 C61 O10 C49 10.7(11) . . . . ? O11 C64 O12 Zn1 1.4(9) . . . 2_575 ? C11 C64 O12 Zn1 179.5(5) . . . 2_575 ? C34 N7 Zn1 O6 -44.0(7) . . . 3_664 ? C18 N7 Zn1 O6 134.7(6) . . . 3_664 ? C34 N7 Zn1 O12 -178.1(6) . . . 2_574 ? C18 N7 Zn1 O12 0.6(7) . . . 2_574 ? C34 N7 Zn1 N1 79.8(6) . . . . ? C18 N7 Zn1 N1 -101.5(6) . . . . ? C13 N1 Zn1 O6 -140.8(6) . . . 3_664 ? C4 N1 Zn1 O6 44.4(7) . . . 3_664 ? C13 N1 Zn1 O12 -20.2(7) . . . 2_574 ? C4 N1 Zn1 O12 164.9(6) . . . 2_574 ? C13 N1 Zn1 N7 90.6(7) . . . . ? C4 N1 Zn1 N7 -84.3(6) . . . . ? C10 O8 Zn2 N4 52.5(7) . . . . ? C10 O8 Zn2 O3 -176.1(6) . . . . ? C10 O8 Zn2 N8 -67.3(6) . . . 1_545 ? C8 N4 Zn2 O8 -43.1(7) . . . . ? C2 N4 Zn2 O8 134.5(5) . . . . ? C8 N4 Zn2 O3 -178.1(6) . . . . ? C2 N4 Zn2 O3 -0.5(6) . . . . ? C8 N4 Zn2 N8 77.7(6) . . . 1_545 ? C2 N4 Zn2 N8 -104.8(5) . . . 1_545 ? C5 O3 Zn2 O8 -65.3(5) . . . . ? C5 O3 Zn2 N4 71.3(5) . . . . ? C5 O3 Zn2 N8 -179.4(4) . . . 1_545 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.870 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.079 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.872 0.248 0.283 196 63 ' ' 2 0.628 0.248 0.783 196 63 ' ' 3 0.372 0.751 0.283 196 63 ' ' 4 0.128 0.751 0.783 196 63 ' ' _platon_squeeze_details ; ; # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 877926' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49.50 H40.50 N6.50 O12.50 Zn2' _chemical_formula_weight 1057.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9501(4) _cell_length_b 20.6804(9) _cell_length_c 21.8474(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.217(2) _cell_angle_gamma 90.00 _cell_volume 4934.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.65 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2172 _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7452 _exptl_absorpt_correction_T_max 0.8032 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34960 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8636 _reflns_number_gt 6837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some DMF molecules are disordered and show two kinds of mode. One is structure-disordered on two methyl sites and the other one is site-disordered with the site-occupation of 0.5. ; _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^)+(0.0370P)^2^+12.7799P] 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 8636 _refine_ls_number_parameters 665 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0775 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.129 _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 C1 C 1.4371(4) 0.2547(2) 0.23283(19) 0.0294(9) Uani 1 1 d . . . C2 C 0.6861(4) 0.2525(2) -0.1479(2) 0.0320(10) Uani 1 1 d . . . C3 C 0.6668(5) 0.5555(2) 0.2362(2) 0.0438(12) Uani 1 1 d . . . H3 H 0.6616 0.6004 0.2352 0.053 Uiso 1 1 calc R . . C4 C 0.6690(5) 0.4556(2) 0.2907(2) 0.0427(12) Uani 1 1 d . . . H4 H 0.6657 0.4339 0.3278 0.051 Uiso 1 1 calc R . . C5 C 0.6804(4) 0.2560(2) 0.1168(2) 0.0338(10) Uani 1 1 d . . . C6 C 1.3013(4) 0.2515(2) 0.2370(2) 0.0310(10) Uani 1 1 d . . . C7 C 0.6829(4) 0.4534(2) 0.1864(2) 0.0321(10) Uani 1 1 d . . . H7 H 0.6897 0.4299 0.1505 0.038 Uiso 1 1 calc R . . C8 C 1.0462(4) 0.2486(2) 0.2416(2) 0.0334(10) Uani 1 1 d . . . C9 C 0.9086(4) 0.2488(2) 0.2398(2) 0.0358(11) Uani 1 1 d . . . C10 C 1.2293(4) 0.2230(2) 0.1909(2) 0.0372(11) Uani 1 1 d . . . H10 H 1.2649 0.2045 0.1577 0.045 Uiso 1 1 calc R . . C11 C 0.6779(4) 0.5199(2) 0.1825(2) 0.0349(10) Uani 1 1 d . . . C12 C 0.7582(4) 0.2039(2) 0.0214(2) 0.0345(10) Uani 1 1 d . . . C13 C 0.6398(5) 0.5755(2) -0.0067(2) 0.0431(12) Uani 1 1 d . . . H13 H 0.6322 0.5320 0.0031 0.052 Uiso 1 1 calc R . . C14 C 0.6638(5) 0.5220(2) 0.2904(2) 0.0495(14) Uani 1 1 d . . . H14 H 0.6583 0.5444 0.3271 0.059 Uiso 1 1 calc R . . C15 C 0.6478(5) 0.6211(2) 0.0399(2) 0.0397(11) Uani 1 1 d . . . C16 C 0.7557(4) 0.2015(2) -0.0442(2) 0.0332(10) Uani 1 1 d . . . C17 C 0.6527(5) 0.3066(2) 0.0147(2) 0.0418(12) Uani 1 1 d . . . H17 H 0.6206 0.3423 0.0338 0.050 Uiso 1 1 calc R . . C18 C 0.6536(5) 0.3054(2) -0.0501(2) 0.0416(12) Uani 1 1 d . . . H18 H 0.6229 0.3404 -0.0731 0.050 Uiso 1 1 calc R . . C19 C 0.6679(6) 0.4465(3) -0.3269(2) 0.0520(14) Uani 1 1 d . . . H19 H 0.6780 0.4218 -0.3617 0.062 Uiso 1 1 calc R . . C20 C 0.6985(4) 0.2558(2) 0.04964(19) 0.0323(10) Uani 1 1 d . . . C21 C 1.1191(4) 0.2753(2) 0.2922(2) 0.0352(11) Uani 1 1 d . . . C22 C 1.2491(4) 0.2772(2) 0.2895(2) 0.0309(10) Uani 1 1 d . . . C23 C 0.8151(5) 0.1489(2) -0.0713(2) 0.0437(12) Uani 1 1 d . . . H23 H 0.8131 0.1461 -0.1139 0.052 Uiso 1 1 calc R . . C24 C 0.6428(5) 0.5934(2) -0.0677(2) 0.0396(11) Uani 1 1 d . . . C25 C 1.2713(5) 0.3249(3) 0.3918(2) 0.0494(13) Uani 1 1 d . . . H25 H 1.3205 0.3416 0.4246 0.059 Uiso 1 1 calc R . . C26 C 0.6606(7) 0.5125(3) -0.3323(3) 0.0667(19) Uani 1 1 d . . . H26 H 0.6659 0.5322 -0.3703 0.080 Uiso 1 1 calc R . . C27 C 1.0688(5) 0.2984(3) 0.3467(2) 0.0517(14) Uani 1 1 d . . . H27 H 0.9847 0.2968 0.3499 0.062 Uiso 1 1 calc R . . C28 C 1.3231(4) 0.3019(2) 0.3408(2) 0.0414(12) Uani 1 1 d . . . H28 H 1.4078 0.3024 0.3396 0.050 Uiso 1 1 calc R . . C29 C 1.1014(4) 0.2217(2) 0.1935(2) 0.0400(11) Uani 1 1 d . . . H29 H 1.0533 0.2021 0.1619 0.048 Uiso 1 1 calc R . . C30 C 0.6992(4) 0.2533(2) -0.07906(19) 0.0318(10) Uani 1 1 d . . . C31 C 0.6384(4) 0.5189(2) -0.2255(2) 0.0348(10) Uani 1 1 d . . . C32 C 1.1440(5) 0.3230(3) 0.3943(3) 0.0572(15) Uani 1 1 d . . . H32 H 1.1094 0.3387 0.4290 0.069 Uiso 1 1 calc R . . C33 C 0.6451(4) 0.4521(2) -0.2224(2) 0.0315(10) Uani 1 1 d . . . H33 H 0.6387 0.4313 -0.1850 0.038 Uiso 1 1 calc R . . C34 C 0.8243(5) 0.1553(3) 0.0558(2) 0.0480(13) Uani 1 1 d . . . H34 H 0.8286 0.1570 0.0984 0.058 Uiso 1 1 calc R . . C35 C 0.6594(6) 0.6858(3) 0.0244(2) 0.0558(15) Uani 1 1 d . . . H35 H 0.6631 0.7171 0.0550 0.067 Uiso 1 1 calc R . . C36 C 0.6411(5) 0.6059(2) 0.1062(2) 0.0456(13) Uani 1 1 d . . . C37 C 0.6568(5) 0.6581(2) -0.0821(2) 0.0512(14) Uani 1 1 d . . . H37 H 0.6602 0.6705 -0.1229 0.061 Uiso 1 1 calc R . . C38 C 0.6657(7) 0.7042(3) -0.0365(3) 0.0631(18) Uani 1 1 d . . . H38 H 0.6758 0.7475 -0.0463 0.076 Uiso 1 1 calc R . . C39 C 0.8750(6) 0.1022(3) -0.0365(3) 0.0591(16) Uani 1 1 d . . . H39 H 0.9116 0.0677 -0.0554 0.071 Uiso 1 1 calc R . . C40 C 0.6453(6) 0.5492(2) -0.2810(2) 0.0535(15) Uani 1 1 d . . . H40 H 0.6397 0.5940 -0.2838 0.064 Uiso 1 1 calc R . . C41 C 0.6396(5) 0.5404(2) -0.1139(2) 0.0470(13) Uani 1 1 d . . . C42 C 0.8812(6) 0.1065(3) 0.0279(3) 0.0632(17) Uani 1 1 d . . . H42 H 0.9247 0.0756 0.0515 0.076 Uiso 1 1 calc R . . C43 C 0.8626(8) 0.4368(4) 0.0157(4) 0.096(3) Uani 1 1 d . . . H43 H 0.8323 0.4557 -0.0210 0.116 Uiso 1 1 calc R . . C44 C 0.9886(10) 0.3563(6) 0.0653(6) 0.153(4) Uani 1 1 d U . . H44A H 1.0570 0.3804 0.0833 0.230 Uiso 1 1 calc R . . H44B H 1.0153 0.3138 0.0546 0.230 Uiso 1 1 calc R . . H44C H 0.9270 0.3528 0.0942 0.230 Uiso 1 1 calc R . . C45 C 0.9733(10) 0.3638(6) -0.0467(5) 0.159(5) Uani 1 1 d U . . H45A H 0.9312 0.3874 -0.0797 0.238 Uiso 1 1 calc R . . H45B H 0.9517 0.3189 -0.0500 0.238 Uiso 1 1 calc R . . H45C H 1.0601 0.3685 -0.0489 0.238 Uiso 1 1 calc R . . C46A C -0.0060(15) 0.5429(9) 0.3059(10) 0.117(3) Uani 0.595(9) 1 d P A 1 H46A H -0.0061 0.5878 0.3039 0.140 Uiso 0.595(9) 1 calc PR A 1 C47A C 0.0192(17) 0.5433(9) 0.1958(9) 0.117(3) Uani 0.595(9) 1 d P A 1 H47A H -0.0429 0.5296 0.1652 0.175 Uiso 0.595(9) 1 d PR A 1 H47B H 0.0985 0.5354 0.1813 0.175 Uiso 0.595(9) 1 d PR A 1 H47C H 0.0100 0.5886 0.2035 0.175 Uiso 0.595(9) 1 d PR A 1 C48A C 0.0206(13) 0.4398(7) 0.2491(7) 0.117(3) Uani 0.595(9) 1 d P A 1 H48A H -0.0470 0.4226 0.2238 0.175 Uiso 0.595(9) 1 d PR A 1 H48B H 0.0234 0.4199 0.2888 0.175 Uiso 0.595(9) 1 d PR A 1 H48C H 0.0956 0.4312 0.2304 0.175 Uiso 0.595(9) 1 d PR A 1 C49 C 0.5549(13) 0.0414(7) -0.0151(7) 0.145(8) Uani 0.50 1 d PRU . . C50 C 0.3694(15) 0.0120(8) 0.0231(8) 0.166(10) Uani 0.50 1 d PU . . C51 C 0.4424(15) 0.1198(8) 0.0542(8) 0.128(8) Uani 0.50 1 d PRD . . H51 H 0.5042 0.1500 0.0629 0.153 Uiso 0.50 1 calc PR B 1 C46B C -0.012(2) 0.4707(14) 0.3106(14) 0.117(3) Uani 0.405(9) 1 d P A 2 H46B H -0.0200 0.4261 0.3146 0.140 Uiso 0.405(9) 1 calc PR A 2 C47B C 0.009(2) 0.4513(13) 0.2061(12) 0.117(3) Uani 0.405(9) 1 d P A 2 H47D H -0.0400 0.4643 0.1699 0.175 Uiso 0.405(9) 1 calc PR A 2 H47E H -0.0241 0.4121 0.2219 0.175 Uiso 0.405(9) 1 calc PR A 2 H47F H 0.0915 0.4440 0.1962 0.175 Uiso 0.405(9) 1 calc PR A 2 C48B C 0.003(2) 0.5632(13) 0.2344(14) 0.117(3) Uani 0.405(9) 1 d P A 2 H48D H -0.0093 0.5928 0.2672 0.175 Uiso 0.405(9) 1 calc PR A 2 H48E H -0.0630 0.5673 0.2033 0.175 Uiso 0.405(9) 1 calc PR A 2 H48F H 0.0791 0.5730 0.2171 0.175 Uiso 0.405(9) 1 calc PR A 2 N1 N 0.6786(3) 0.42081(18) 0.23963(17) 0.0323(8) Uani 1 1 d . . . N2 N 0.6834(4) 0.54702(19) 0.12439(18) 0.0414(10) Uani 1 1 d D . . N3 N 0.6247(4) 0.55864(19) -0.17399(18) 0.0396(10) Uani 1 1 d D . . N4 N 0.6609(3) 0.41701(17) -0.27313(16) 0.0301(8) Uani 1 1 d . . . N5 N 0.9386(4) 0.3888(2) 0.0112(2) 0.0877(19) Uani 1 1 d . . . N6 N 0.0064(4) 0.5052(2) 0.2553(2) 0.094(2) Uani 1 1 d R . . N7 N 0.4532(4) 0.0558(2) 0.0168(2) 0.143(6) Uani 0.50 1 d PRU A . O1 O 0.6532(3) 0.20336(16) 0.14104(14) 0.0397(8) Uani 1 1 d . . . O2 O 0.6899(3) 0.30957(16) 0.14522(14) 0.0407(8) Uani 1 1 d . . . O3 O 0.7039(3) 0.30509(16) -0.17507(14) 0.0395(8) Uani 1 1 d . . . O4 O 0.6569(3) 0.19980(16) -0.17419(14) 0.0391(8) Uani 1 1 d . . . O5 O 0.8562(3) 0.19663(17) 0.22479(16) 0.0440(8) Uani 1 1 d . . . O6 O 0.8568(3) 0.30053(17) 0.25177(17) 0.0452(9) Uani 1 1 d . . . O7 O 1.4942(3) 0.20233(15) 0.23657(15) 0.0367(7) Uani 1 1 d . . . O8 O 1.4838(3) 0.31001(15) 0.22469(14) 0.0341(7) Uani 1 1 d . . . O9 O 0.5984(5) 0.6443(2) 0.14104(18) 0.0776(15) Uani 1 1 d . . . O10 O 0.6504(6) 0.48419(19) -0.09846(17) 0.0886(18) Uani 1 1 d . . . O11 O 0.8275(5) 0.4594(3) 0.0618(2) 0.0959(18) Uani 1 1 d . . . O12 O -0.0171(10) 0.5136(6) 0.3546(4) 0.214(5) Uani 1 1 d . . . O13 O 0.340(2) 0.1227(17) 0.0695(16) 0.160(13) Uani 0.25 1 d PDU C 1 O14 O 0.198(2) 0.1132(14) 0.0688(12) 0.125(8) Uani 0.25 1 d PU D 2 Zn1 Zn 0.67359(4) 0.32287(2) 0.23641(2) 0.02634(14) Uani 1 1 d . . . Zn2 Zn 0.67409(4) 0.18051(2) 0.23291(2) 0.02527(14) Uani 1 1 d . . . H1M H 0.723(3) 0.5220(17) 0.0989(15) 0.022(11) Uiso 1 1 d D . . H2M H 0.607(5) 0.5994(11) -0.186(2) 0.062(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(2) 0.039(3) 0.021(2) 0.0000(18) 0.0042(17) -0.0026(19) C2 0.029(2) 0.045(3) 0.023(2) 0.000(2) 0.0037(18) 0.002(2) C3 0.064(3) 0.031(3) 0.036(3) -0.005(2) 0.005(2) 0.001(2) C4 0.060(3) 0.040(3) 0.028(3) 0.002(2) 0.000(2) 0.003(2) C5 0.033(2) 0.047(3) 0.021(2) 0.001(2) 0.0036(18) 0.001(2) C6 0.026(2) 0.031(2) 0.037(3) 0.0029(19) 0.0075(19) -0.0024(18) C7 0.040(2) 0.034(2) 0.023(2) -0.0020(18) 0.0027(19) 0.0001(19) C8 0.026(2) 0.036(3) 0.039(3) 0.002(2) 0.0045(19) 0.0020(19) C9 0.029(2) 0.047(3) 0.031(3) 0.009(2) -0.0001(19) -0.003(2) C10 0.033(2) 0.044(3) 0.036(3) -0.001(2) 0.007(2) -0.003(2) C11 0.045(3) 0.031(2) 0.029(2) 0.0014(19) 0.003(2) 0.001(2) C12 0.035(2) 0.042(3) 0.026(2) 0.005(2) 0.0044(19) -0.001(2) C13 0.063(3) 0.030(3) 0.036(3) 0.002(2) 0.001(2) 0.004(2) C14 0.080(4) 0.037(3) 0.031(3) -0.006(2) 0.003(3) 0.002(3) C15 0.061(3) 0.029(2) 0.029(3) -0.0004(19) 0.002(2) 0.002(2) C16 0.035(2) 0.042(3) 0.023(2) 0.0019(19) 0.0057(19) 0.001(2) C17 0.058(3) 0.044(3) 0.025(2) -0.003(2) 0.008(2) 0.008(2) C18 0.058(3) 0.046(3) 0.021(2) 0.003(2) 0.003(2) 0.011(2) C19 0.084(4) 0.039(3) 0.035(3) 0.001(2) 0.017(3) -0.003(3) C20 0.040(2) 0.038(3) 0.019(2) 0.0018(18) 0.0032(18) -0.004(2) C21 0.029(2) 0.034(2) 0.044(3) 0.002(2) 0.007(2) 0.0014(19) C22 0.027(2) 0.030(2) 0.037(3) 0.0086(19) 0.0070(19) 0.0018(18) C23 0.051(3) 0.050(3) 0.033(3) -0.002(2) 0.016(2) 0.004(2) C24 0.057(3) 0.033(3) 0.029(3) -0.002(2) 0.003(2) 0.001(2) C25 0.055(3) 0.056(3) 0.036(3) -0.002(2) -0.003(3) 0.001(3) C26 0.131(6) 0.035(3) 0.036(3) 0.010(2) 0.021(3) -0.006(3) C27 0.042(3) 0.068(4) 0.047(3) -0.003(3) 0.010(2) 0.005(3) C28 0.037(3) 0.044(3) 0.043(3) 0.006(2) -0.004(2) 0.000(2) C29 0.030(2) 0.048(3) 0.041(3) -0.004(2) -0.002(2) -0.007(2) C30 0.038(2) 0.040(3) 0.018(2) -0.0023(19) 0.0042(18) 0.001(2) C31 0.042(3) 0.034(3) 0.028(2) 0.0005(19) 0.003(2) -0.001(2) C32 0.057(3) 0.072(4) 0.043(3) -0.008(3) 0.011(3) 0.010(3) C33 0.039(2) 0.036(2) 0.020(2) 0.0038(18) 0.0047(19) 0.0012(19) C34 0.057(3) 0.053(3) 0.034(3) 0.008(2) 0.007(2) 0.015(3) C35 0.096(5) 0.035(3) 0.036(3) -0.004(2) -0.004(3) 0.001(3) C36 0.068(4) 0.036(3) 0.033(3) -0.002(2) 0.005(3) 0.009(2) C37 0.083(4) 0.034(3) 0.036(3) 0.001(2) 0.001(3) -0.001(3) C38 0.120(6) 0.029(3) 0.040(3) 0.001(2) 0.009(3) -0.011(3) C39 0.073(4) 0.055(4) 0.050(4) 0.001(3) 0.018(3) 0.023(3) C40 0.100(5) 0.024(3) 0.037(3) 0.003(2) 0.012(3) -0.001(3) C41 0.073(4) 0.036(3) 0.031(3) -0.001(2) 0.000(3) 0.008(2) C42 0.073(4) 0.071(4) 0.046(3) 0.017(3) 0.011(3) 0.036(3) C43 0.096(6) 0.099(6) 0.095(7) 0.005(5) 0.016(5) 0.027(5) C44 0.125(7) 0.155(8) 0.176(8) 0.006(7) -0.010(7) 0.029(6) C45 0.145(7) 0.180(8) 0.157(8) -0.058(7) 0.050(7) 0.009(7) C46A 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) C47A 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) C48A 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) C49 0.137(11) 0.156(12) 0.143(11) 0.002(9) 0.004(9) -0.003(9) C50 0.169(12) 0.171(13) 0.158(13) 0.003(9) 0.024(9) -0.024(9) C51 0.115(15) 0.088(13) 0.17(2) 0.046(13) -0.053(15) -0.023(12) C46B 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) C47B 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) C48B 0.107(5) 0.115(6) 0.125(8) 0.003(6) -0.010(7) -0.027(5) N1 0.035(2) 0.032(2) 0.030(2) 0.0011(16) 0.0056(17) 0.0004(16) N2 0.065(3) 0.032(2) 0.029(2) 0.0011(17) 0.013(2) 0.0063(19) N3 0.058(3) 0.029(2) 0.031(2) -0.0033(17) 0.0003(19) 0.0064(19) N4 0.034(2) 0.029(2) 0.027(2) 0.0007(15) 0.0056(16) -0.0002(15) N5 0.067(4) 0.094(5) 0.104(5) -0.030(4) 0.027(4) 0.009(3) N6 0.090(5) 0.087(5) 0.102(5) 0.002(4) -0.010(4) -0.008(4) N7 0.152(10) 0.153(10) 0.121(9) 0.014(8) -0.016(8) -0.017(8) O1 0.055(2) 0.044(2) 0.0210(16) 0.0028(14) 0.0081(15) -0.0059(16) O2 0.053(2) 0.044(2) 0.0259(17) -0.0019(15) 0.0103(15) -0.0032(16) O3 0.0474(19) 0.048(2) 0.0228(17) 0.0007(15) 0.0013(14) 0.0011(16) O4 0.0459(19) 0.047(2) 0.0242(17) -0.0035(14) 0.0017(14) -0.0073(15) O5 0.0277(16) 0.052(2) 0.052(2) -0.0045(17) 0.0063(15) -0.0051(15) O6 0.0278(16) 0.047(2) 0.061(2) 0.0032(17) 0.0033(16) 0.0062(15) O7 0.0291(15) 0.0355(18) 0.047(2) 0.0053(15) 0.0104(14) 0.0041(14) O8 0.0278(15) 0.0376(18) 0.0371(18) 0.0063(14) 0.0041(13) -0.0043(13) O9 0.144(4) 0.054(3) 0.035(2) 0.0024(19) 0.012(3) 0.040(3) O10 0.199(6) 0.034(2) 0.031(2) -0.0021(17) -0.003(3) 0.016(3) O11 0.124(5) 0.095(4) 0.073(4) -0.001(3) 0.033(3) 0.047(3) O12 0.266(12) 0.272(12) 0.102(6) -0.016(8) -0.003(7) -0.121(10) O13 0.170(15) 0.153(15) 0.157(15) 0.018(9) 0.019(10) 0.006(10) O14 0.127(11) 0.134(12) 0.111(11) 0.009(9) -0.011(9) -0.010(9) Zn1 0.0293(3) 0.0288(3) 0.0212(3) 0.00109(19) 0.0037(2) 0.0001(2) Zn2 0.0284(3) 0.0274(3) 0.0204(3) 0.00012(19) 0.00402(19) -0.00071(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O7 1.250(5) . ? C1 O8 1.270(5) . ? C1 C6 1.499(6) . ? C2 O3 1.261(5) . ? C2 O4 1.262(5) . ? C2 C30 1.501(6) . ? C3 C14 1.376(7) . ? C3 C11 1.398(6) . ? C3 H3 0.9300 . ? C4 N1 1.337(6) . ? C4 C14 1.375(7) . ? C4 H4 0.9300 . ? C5 O1 1.256(5) . ? C5 O2 1.271(6) . ? C5 C20 1.494(6) . ? C6 C10 1.366(6) . ? C6 C22 1.422(6) . ? C7 N1 1.349(6) . ? C7 C11 1.378(6) . ? C7 H7 0.9300 . ? C8 C29 1.369(7) . ? C8 C21 1.426(6) . ? C8 C9 1.505(6) . ? C9 O6 1.248(6) . ? C9 O5 1.254(6) . ? C10 C29 1.406(6) . ? C10 H10 0.9300 . ? C11 N2 1.394(6) . ? C12 C34 1.421(6) . ? C12 C20 1.421(6) . ? C12 C16 1.432(6) . ? C13 C24 1.385(7) . ? C13 C15 1.387(6) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C35 1.388(7) . ? C15 C36 1.490(7) . ? C16 C23 1.420(7) . ? C16 C30 1.428(6) . ? C17 C20 1.372(6) . ? C17 C18 1.416(6) . ? C17 H17 0.9300 . ? C18 C30 1.362(6) . ? C18 H18 0.9300 . ? C19 N4 1.331(6) . ? C19 C26 1.371(7) . ? C19 H19 0.9300 . ? C21 C22 1.429(6) . ? C21 C27 1.430(7) . ? C22 C28 1.428(6) . ? C23 C39 1.366(7) . ? C23 H23 0.9300 . ? C24 C37 1.387(7) . ? C24 C41 1.489(7) . ? C25 C28 1.372(7) . ? C25 C32 1.400(8) . ? C25 H25 0.9300 . ? C26 C40 1.375(7) . ? C26 H26 0.9300 . ? C27 C32 1.376(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C31 C40 1.372(7) . ? C31 C33 1.384(6) . ? C31 N3 1.410(6) . ? C32 H32 0.9300 . ? C33 N4 1.347(5) . ? C33 H33 0.9300 . ? C34 C42 1.353(8) . ? C34 H34 0.9300 . ? C35 C38 1.389(7) . ? C35 H35 0.9300 . ? C36 O9 1.217(6) . ? C36 N2 1.352(6) . ? C37 C38 1.377(7) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C42 1.408(8) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 O10 1.214(6) . ? C41 N3 1.363(6) . ? C42 H42 0.9300 . ? C43 O11 1.199(9) . ? C43 N5 1.304(9) . ? C43 H43 0.9300 . ? C44 N5 1.433(11) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 N5 1.443(11) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46A O12 1.238(19) . ? C46A N6 1.37(2) . ? C46A H46A 0.9300 . ? C47A N6 1.535(18) . ? C47A H47A 0.9600 . ? C47A H47B 0.9600 . ? C47A H47C 0.9600 . ? C48A N6 1.369(15) . ? C48A H48A 0.9600 . ? C48A H48B 0.9600 . ? C48A H48C 0.9600 . ? C49 N7 1.389(16) . ? C49 C50 1.40(2) 3_655 ? C50 N7 1.304(16) . ? C50 C49 1.40(2) 3_655 ? C51 O13 1.198(10) . ? C51 N7 1.564(18) . ? C51 H51 0.9300 . ? C46B O12 1.31(3) . ? C46B N6 1.43(3) . ? C46B H48B 1.2292 . ? C46B H46B 0.9300 . ? C47B N6 1.55(3) . ? C47B H48A 0.9523 . ? C47B H48C 1.1339 . ? C47B H47D 0.9600 . ? C47B H47E 0.9600 . ? C47B H47F 0.9600 . ? C48B N6 1.28(3) . ? C48B H47C 0.8634 . ? C48B H48D 0.9600 . ? C48B H48E 0.9600 . ? C48B H48F 0.9600 . ? N1 Zn1 2.027(4) . ? N2 H1M 0.895(10) . ? N3 H2M 0.898(10) . ? N4 Zn2 2.025(4) 4_565 ? O1 Zn2 2.058(3) . ? O2 Zn1 2.032(3) . ? O3 Zn2 2.035(3) 4_565 ? O4 Zn1 2.030(3) 4_565 ? O5 Zn2 2.042(3) . ? O6 Zn1 2.062(3) . ? O7 Zn2 2.028(3) 1_655 ? O8 Zn1 2.092(3) 1_655 ? Zn1 O4 2.030(3) 4_566 ? Zn1 O8 2.092(3) 1_455 ? Zn1 Zn2 2.9451(7) . ? Zn2 N4 2.025(4) 4_566 ? Zn2 O7 2.028(3) 1_455 ? Zn2 O3 2.035(3) 4_566 ? 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 O7 C1 O8 125.8(4) . . ? O7 C1 C6 116.8(4) . . ? O8 C1 C6 117.4(4) . . ? O3 C2 O4 125.0(4) . . ? O3 C2 C30 117.1(4) . . ? O4 C2 C30 117.9(4) . . ? C14 C3 C11 117.7(5) . . ? C14 C3 H3 121.1 . . ? C11 C3 H3 121.1 . . ? N1 C4 C14 122.6(5) . . ? N1 C4 H4 118.7 . . ? C14 C4 H4 118.7 . . ? O1 C5 O2 124.2(4) . . ? O1 C5 C20 117.7(4) . . ? O2 C5 C20 118.0(4) . . ? C10 C6 C22 120.8(4) . . ? C10 C6 C1 119.7(4) . . ? C22 C6 C1 119.4(4) . . ? N1 C7 C11 123.2(4) . . ? N1 C7 H7 118.4 . . ? C11 C7 H7 118.4 . . ? C29 C8 C21 119.9(4) . . ? C29 C8 C9 118.6(4) . . ? C21 C8 C9 121.5(4) . . ? O6 C9 O5 125.9(4) . . ? O6 C9 C8 117.9(4) . . ? O5 C9 C8 116.3(4) . . ? C6 C10 C29 120.0(5) . . ? C6 C10 H10 120.0 . . ? C29 C10 H10 120.0 . . ? C7 C11 N2 116.9(4) . . ? C7 C11 C3 118.8(4) . . ? N2 C11 C3 124.3(4) . . ? C34 C12 C20 122.5(4) . . ? C34 C12 C16 118.5(4) . . ? C20 C12 C16 119.0(4) . . ? C24 C13 C15 121.3(5) . . ? C24 C13 H13 119.3 . . ? C15 C13 H13 119.3 . . ? C4 C14 C3 120.2(5) . . ? C4 C14 H14 119.9 . . ? C3 C14 H14 119.9 . . ? C13 C15 C35 118.6(5) . . ? C13 C15 C36 124.5(4) . . ? C35 C15 C36 116.9(4) . . ? C23 C16 C30 123.1(4) . . ? C23 C16 C12 117.9(4) . . ? C30 C16 C12 119.0(4) . . ? C20 C17 C18 120.9(4) . . ? C20 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C30 C18 C17 120.5(4) . . ? C30 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? N4 C19 C26 121.7(5) . . ? N4 C19 H19 119.1 . . ? C26 C19 H19 119.1 . . ? C17 C20 C12 119.8(4) . . ? C17 C20 C5 118.4(4) . . ? C12 C20 C5 121.8(4) . . ? C8 C21 C22 118.8(4) . . ? C8 C21 C27 123.1(4) . . ? C22 C21 C27 118.1(4) . . ? C6 C22 C28 121.9(4) . . ? C6 C22 C21 118.9(4) . . ? C28 C22 C21 119.1(4) . . ? C39 C23 C16 121.7(5) . . ? C39 C23 H23 119.1 . . ? C16 C23 H23 119.1 . . ? C13 C24 C37 119.2(4) . . ? C13 C24 C41 117.1(4) . . ? C37 C24 C41 123.6(5) . . ? C28 C25 C32 119.6(5) . . ? C28 C25 H25 120.2 . . ? C32 C25 H25 120.2 . . ? C19 C26 C40 119.3(5) . . ? C19 C26 H26 120.4 . . ? C40 C26 H26 120.4 . . ? C32 C27 C21 120.5(5) . . ? C32 C27 H27 119.7 . . ? C21 C27 H27 119.7 . . ? C25 C28 C22 121.1(5) . . ? C25 C28 H28 119.4 . . ? C22 C28 H28 119.4 . . ? C8 C29 C10 121.4(4) . . ? C8 C29 H29 119.3 . . ? C10 C29 H29 119.3 . . ? C18 C30 C16 120.3(4) . . ? C18 C30 C2 117.5(4) . . ? C16 C30 C2 122.2(4) . . ? C40 C31 C33 119.6(4) . . ? C40 C31 N3 117.0(4) . . ? C33 C31 N3 123.4(4) . . ? C27 C32 C25 121.5(5) . . ? C27 C32 H32 119.3 . . ? C25 C32 H32 119.3 . . ? N4 C33 C31 120.5(4) . . ? N4 C33 H33 119.8 . . ? C31 C33 H33 119.8 . . ? C42 C34 C12 121.6(5) . . ? C42 C34 H34 119.2 . . ? C12 C34 H34 119.2 . . ? C15 C35 C38 120.6(5) . . ? C15 C35 H35 119.7 . . ? C38 C35 H35 119.7 . . ? O9 C36 N2 123.0(5) . . ? O9 C36 C15 121.3(5) . . ? N2 C36 C15 115.8(4) . . ? C38 C37 C24 120.4(5) . . ? C38 C37 H37 119.8 . . ? C24 C37 H37 119.8 . . ? C37 C38 C35 119.9(5) . . ? C37 C38 H38 120.1 . . ? C35 C38 H38 120.1 . . ? C23 C39 C42 119.9(5) . . ? C23 C39 H39 120.1 . . ? C42 C39 H39 120.1 . . ? C31 C40 C26 119.1(5) . . ? C31 C40 H40 120.5 . . ? C26 C40 H40 120.5 . . ? O10 C41 N3 122.4(5) . . ? O10 C41 C24 121.2(5) . . ? N3 C41 C24 116.4(4) . . ? C34 C42 C39 120.4(5) . . ? C34 C42 H42 119.8 . . ? C39 C42 H42 119.8 . . ? O11 C43 N5 127.2(8) . . ? O11 C43 H43 116.4 . . ? N5 C43 H43 116.4 . . ? N5 C44 H44A 109.5 . . ? N5 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N5 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 H45A 109.5 . . ? N5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O12 C46A N6 116.0(16) . . ? O12 C46A H46A 122.0 . . ? N6 C46A H46A 122.0 . . ? N6 C47A H47A 109.5 . . ? N6 C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? N6 C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? N6 C48A H48A 109.6 . . ? N6 C48A H48B 109.4 . . ? H48A C48A H48B 109.5 . . ? N6 C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? N7 C49 C50 137.4(14) . 3_655 ? N7 C50 C49 96.2(13) . 3_655 ? O13 C51 N7 107(2) . . ? O13 C51 H51 126.4 . . ? N7 C51 H51 126.4 . . ? O12 C46B N6 107(2) . . ? O12 C46B H48B 153.1 . . ? N6 C46B H48B 91.7 . . ? O12 C46B H46B 126.4 . . ? N6 C46B H46B 126.4 . . ? H48B C46B H46B 39.0 . . ? N6 C47B H48A 97.1 . . ? N6 C47B H48C 89.7 . . ? H48A C47B H48C 97.1 . . ? N6 C47B H47D 109.5 . . ? N6 C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? N6 C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? N6 C48B H47C 147.7 . . ? N6 C48B H48D 109.5 . . ? N6 C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? N6 C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C4 N1 C7 117.4(4) . . ? C4 N1 Zn1 124.2(3) . . ? C7 N1 Zn1 118.2(3) . . ? C36 N2 C11 126.4(4) . . ? C36 N2 H1M 121(3) . . ? C11 N2 H1M 113(3) . . ? C41 N3 C31 126.4(4) . . ? C41 N3 H2M 123(4) . . ? C31 N3 H2M 111(4) . . ? C19 N4 C33 119.9(4) . . ? C19 N4 Zn2 120.4(3) . 4_565 ? C33 N4 Zn2 119.7(3) . 4_565 ? C43 N5 C44 120.2(7) . . ? C43 N5 C45 123.3(8) . . ? C44 N5 C45 116.4(8) . . ? C48B N6 C46A 75.7(14) . . ? C48B N6 C48A 152.8(15) . . ? C46A N6 C48A 131.4(11) . . ? C48B N6 C46B 139.9(18) . . ? C46A N6 C46B 64.7(14) . . ? C48A N6 C46B 67.4(13) . . ? C48B N6 C47A 38.9(13) . . ? C46A N6 C47A 114.4(11) . . ? C48A N6 C47A 113.9(10) . . ? C46B N6 C47A 176.9(13) . . ? C48B N6 C47B 115.4(16) . . ? C46A N6 C47B 167.9(13) . . ? C48A N6 C47B 38.1(10) . . ? C46B N6 C47B 103.7(15) . . ? C47A N6 C47B 77.0(12) . . ? C50 N7 C49 120.0(10) . . ? C50 N7 C51 116.9(13) . . ? C49 N7 C51 122.5(9) . . ? C5 O1 Zn2 126.7(3) . . ? C5 O2 Zn1 126.0(3) . . ? C2 O3 Zn2 124.9(3) . 4_565 ? C2 O4 Zn1 126.8(3) . 4_565 ? C9 O5 Zn2 123.3(3) . . ? C9 O6 Zn1 127.6(3) . . ? C1 O7 Zn2 132.3(3) . 1_655 ? C1 O8 Zn1 120.2(3) . 1_655 ? C46A O12 C46B 71.9(15) . . ? N1 Zn1 O4 101.63(14) . 4_566 ? N1 Zn1 O2 99.51(14) . . ? O4 Zn1 O2 158.86(14) 4_566 . ? N1 Zn1 O6 101.24(14) . . ? O4 Zn1 O6 86.98(14) 4_566 . ? O2 Zn1 O6 88.54(14) . . ? N1 Zn1 O8 98.92(13) . 1_455 ? O4 Zn1 O8 85.95(13) 4_566 1_455 ? O2 Zn1 O8 91.20(13) . 1_455 ? O6 Zn1 O8 159.60(13) . 1_455 ? N1 Zn1 Zn2 178.32(10) . . ? O4 Zn1 Zn2 78.14(10) 4_566 . ? O2 Zn1 Zn2 80.72(9) . . ? O6 Zn1 Zn2 77.09(10) . . ? O8 Zn1 Zn2 82.73(9) 1_455 . ? N4 Zn2 O7 99.17(14) 4_566 1_455 ? N4 Zn2 O3 102.44(14) 4_566 4_566 ? O7 Zn2 O3 90.79(13) 1_455 4_566 ? N4 Zn2 O5 102.84(14) 4_566 . ? O7 Zn2 O5 157.58(14) 1_455 . ? O3 Zn2 O5 88.60(14) 4_566 . ? N4 Zn2 O1 99.37(14) 4_566 . ? O7 Zn2 O1 87.07(13) 1_455 . ? O3 Zn2 O1 158.14(14) 4_566 . ? O5 Zn2 O1 85.23(14) . . ? N4 Zn2 Zn1 175.39(10) 4_566 . ? O7 Zn2 Zn1 76.87(9) 1_455 . ? O3 Zn2 Zn1 80.13(10) 4_566 . ? O5 Zn2 Zn1 80.95(10) . . ? O1 Zn2 Zn1 78.20(9) . . ? 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 O7 C1 C6 C10 -68.0(6) . . . . ? O8 C1 C6 C10 110.7(5) . . . . ? O7 C1 C6 C22 111.0(5) . . . . ? O8 C1 C6 C22 -70.3(5) . . . . ? C29 C8 C9 O6 -132.0(5) . . . . ? C21 C8 C9 O6 48.2(6) . . . . ? C29 C8 C9 O5 46.5(6) . . . . ? C21 C8 C9 O5 -133.3(5) . . . . ? C22 C6 C10 C29 3.1(7) . . . . ? C1 C6 C10 C29 -177.9(4) . . . . ? N1 C7 C11 N2 -180.0(4) . . . . ? N1 C7 C11 C3 -0.5(7) . . . . ? C14 C3 C11 C7 1.2(7) . . . . ? C14 C3 C11 N2 -179.3(5) . . . . ? N1 C4 C14 C3 0.9(9) . . . . ? C11 C3 C14 C4 -1.4(8) . . . . ? C24 C13 C15 C35 -0.2(8) . . . . ? C24 C13 C15 C36 177.9(5) . . . . ? C34 C12 C16 C23 2.8(7) . . . . ? C20 C12 C16 C23 -179.5(4) . . . . ? C34 C12 C16 C30 -174.3(4) . . . . ? C20 C12 C16 C30 3.4(6) . . . . ? C20 C17 C18 C30 0.6(8) . . . . ? C18 C17 C20 C12 6.0(7) . . . . ? C18 C17 C20 C5 -172.2(4) . . . . ? C34 C12 C20 C17 169.8(5) . . . . ? C16 C12 C20 C17 -7.9(7) . . . . ? C34 C12 C20 C5 -12.1(7) . . . . ? C16 C12 C20 C5 170.2(4) . . . . ? O1 C5 C20 C17 139.2(5) . . . . ? O2 C5 C20 C17 -38.8(6) . . . . ? O1 C5 C20 C12 -38.9(6) . . . . ? O2 C5 C20 C12 143.0(4) . . . . ? C29 C8 C21 C22 4.0(7) . . . . ? C9 C8 C21 C22 -176.2(4) . . . . ? C29 C8 C21 C27 -173.6(5) . . . . ? C9 C8 C21 C27 6.2(7) . . . . ? C10 C6 C22 C28 174.2(4) . . . . ? C1 C6 C22 C28 -4.8(6) . . . . ? C10 C6 C22 C21 -2.6(7) . . . . ? C1 C6 C22 C21 178.4(4) . . . . ? C8 C21 C22 C6 -1.0(6) . . . . ? C27 C21 C22 C6 176.8(4) . . . . ? C8 C21 C22 C28 -177.8(4) . . . . ? C27 C21 C22 C28 -0.1(7) . . . . ? C30 C16 C23 C39 175.8(5) . . . . ? C12 C16 C23 C39 -1.2(8) . . . . ? C15 C13 C24 C37 1.4(8) . . . . ? C15 C13 C24 C41 177.1(5) . . . . ? N4 C19 C26 C40 -0.2(10) . . . . ? C8 C21 C27 C32 179.1(5) . . . . ? C22 C21 C27 C32 1.5(8) . . . . ? C32 C25 C28 C22 1.3(8) . . . . ? C6 C22 C28 C25 -178.1(5) . . . . ? C21 C22 C28 C25 -1.3(7) . . . . ? C21 C8 C29 C10 -3.7(7) . . . . ? C9 C8 C29 C10 176.5(4) . . . . ? C6 C10 C29 C8 0.1(7) . . . . ? C17 C18 C30 C16 -5.1(7) . . . . ? C17 C18 C30 C2 174.1(4) . . . . ? C23 C16 C30 C18 -173.9(5) . . . . ? C12 C16 C30 C18 3.0(7) . . . . ? C23 C16 C30 C2 6.9(7) . . . . ? C12 C16 C30 C2 -176.2(4) . . . . ? O3 C2 C30 C18 40.5(6) . . . . ? O4 C2 C30 C18 -138.7(5) . . . . ? O3 C2 C30 C16 -140.2(4) . . . . ? O4 C2 C30 C16 40.6(6) . . . . ? C21 C27 C32 C25 -1.6(9) . . . . ? C28 C25 C32 C27 0.2(9) . . . . ? C40 C31 C33 N4 1.4(7) . . . . ? N3 C31 C33 N4 -178.5(4) . . . . ? C20 C12 C34 C42 -179.5(5) . . . . ? C16 C12 C34 C42 -1.9(8) . . . . ? C13 C15 C35 C38 -1.4(9) . . . . ? C36 C15 C35 C38 -179.6(6) . . . . ? C13 C15 C36 O9 -148.9(6) . . . . ? C35 C15 C36 O9 29.2(8) . . . . ? C13 C15 C36 N2 30.2(8) . . . . ? C35 C15 C36 N2 -151.7(5) . . . . ? C13 C24 C37 C38 -1.0(9) . . . . ? C41 C24 C37 C38 -176.4(6) . . . . ? C24 C37 C38 C35 -0.6(10) . . . . ? C15 C35 C38 C37 1.8(10) . . . . ? C16 C23 C39 C42 -1.5(9) . . . . ? C33 C31 C40 C26 -0.9(9) . . . . ? N3 C31 C40 C26 179.0(6) . . . . ? C19 C26 C40 C31 0.3(10) . . . . ? C13 C24 C41 O10 -9.6(9) . . . . ? C37 C24 C41 O10 165.9(6) . . . . ? C13 C24 C41 N3 170.8(5) . . . . ? C37 C24 C41 N3 -13.7(8) . . . . ? C12 C34 C42 C39 -0.8(10) . . . . ? C23 C39 C42 C34 2.5(10) . . . . ? C14 C4 N1 C7 -0.1(7) . . . . ? C14 C4 N1 Zn1 -175.2(4) . . . . ? C11 C7 N1 C4 -0.1(7) . . . . ? C11 C7 N1 Zn1 175.3(4) . . . . ? O9 C36 N2 C11 4.5(9) . . . . ? C15 C36 N2 C11 -174.6(5) . . . . ? C7 C11 N2 C36 156.6(5) . . . . ? C3 C11 N2 C36 -22.8(8) . . . . ? O10 C41 N3 C31 -10.5(10) . . . . ? C24 C41 N3 C31 169.1(5) . . . . ? C40 C31 N3 C41 -166.4(5) . . . . ? C33 C31 N3 C41 13.6(8) . . . . ? C26 C19 N4 C33 0.6(8) . . . . ? C26 C19 N4 Zn2 -179.3(5) . . . 4_565 ? C31 C33 N4 C19 -1.3(7) . . . . ? C31 C33 N4 Zn2 178.7(3) . . . 4_565 ? O11 C43 N5 C44 0.8(14) . . . . ? O11 C43 N5 C45 178.3(10) . . . . ? O12 C46A N6 C48B 176(2) . . . . ? O12 C46A N6 C48A -7(2) . . . . ? O12 C46A N6 C46B 3.0(16) . . . . ? O12 C46A N6 C47A 179.7(13) . . . . ? O12 C46A N6 C47B 19(7) . . . . ? O12 C46B N6 C48B -13(3) . . . . ? O12 C46B N6 C46A -2.6(14) . . . . ? O12 C46B N6 C48A 169(2) . . . . ? O12 C46B N6 C47A -77(25) . . . . ? O12 C46B N6 C47B -179.2(16) . . . . ? C49 C50 N7 C49 23.4(18) 3_655 . . . ? C49 C50 N7 C51 -148.0(9) 3_655 . . . ? C50 C49 N7 C50 -36(3) 3_655 . . . ? C50 C49 N7 C51 135.2(14) 3_655 . . . ? O13 C51 N7 C50 -18(3) . . . . ? O13 C51 N7 C49 171(2) . . . . ? O2 C5 O1 Zn2 -22.5(7) . . . . ? C20 C5 O1 Zn2 159.6(3) . . . . ? O1 C5 O2 Zn1 3.6(7) . . . . ? C20 C5 O2 Zn1 -178.5(3) . . . . ? O4 C2 O3 Zn2 6.1(6) . . . 4_565 ? C30 C2 O3 Zn2 -173.1(3) . . . 4_565 ? O3 C2 O4 Zn1 17.5(6) . . . 4_565 ? C30 C2 O4 Zn1 -163.4(3) . . . 4_565 ? O6 C9 O5 Zn2 -12.3(7) . . . . ? C8 C9 O5 Zn2 169.3(3) . . . . ? O5 C9 O6 Zn1 -12.0(7) . . . . ? C8 C9 O6 Zn1 166.3(3) . . . . ? O8 C1 O7 Zn2 0.7(7) . . . 1_655 ? C6 C1 O7 Zn2 179.3(3) . . . 1_655 ? O7 C1 O8 Zn1 -14.2(6) . . . 1_655 ? C6 C1 O8 Zn1 167.2(3) . . . 1_655 ? N6 C46A O12 C46B -3.1(16) . . . . ? N6 C46B O12 C46A 2.8(15) . . . . ? C4 N1 Zn1 O4 -1.5(4) . . . 4_566 ? C7 N1 Zn1 O4 -176.5(3) . . . 4_566 ? C4 N1 Zn1 O2 178.9(4) . . . . ? C7 N1 Zn1 O2 3.9(3) . . . . ? C4 N1 Zn1 O6 -90.7(4) . . . . ? C7 N1 Zn1 O6 94.3(3) . . . . ? C4 N1 Zn1 O8 86.2(4) . . . 1_455 ? C7 N1 Zn1 O8 -88.9(3) . . . 1_455 ? C4 N1 Zn1 Zn2 -84(4) . . . . ? C7 N1 Zn1 Zn2 101(4) . . . . ? C5 O2 Zn1 N1 -172.9(4) . . . . ? C5 O2 Zn1 O4 8.2(6) . . . 4_566 ? C5 O2 Zn1 O6 86.0(4) . . . . ? C5 O2 Zn1 O8 -73.6(4) . . . 1_455 ? C5 O2 Zn1 Zn2 8.8(3) . . . . ? C9 O6 Zn1 N1 -160.7(4) . . . . ? C9 O6 Zn1 O4 98.1(4) . . . 4_566 ? C9 O6 Zn1 O2 -61.3(4) . . . . ? C9 O6 Zn1 O8 28.3(7) . . . 1_455 ? C9 O6 Zn1 Zn2 19.6(4) . . . . ? C9 O5 Zn2 N4 -163.3(4) . . . 4_566 ? C9 O5 Zn2 O7 27.8(6) . . . 1_455 ? C9 O5 Zn2 O3 -60.9(4) . . . 4_566 ? C9 O5 Zn2 O1 98.1(4) . . . . ? C9 O5 Zn2 Zn1 19.4(3) . . . . ? C5 O1 Zn2 N4 -162.9(4) . . . 4_566 ? C5 O1 Zn2 O7 98.3(4) . . . 1_455 ? C5 O1 Zn2 O3 13.5(6) . . . 4_566 ? C5 O1 Zn2 O5 -60.7(4) . . . . ? C5 O1 Zn2 Zn1 21.1(4) . . . . ? N1 Zn1 Zn2 N4 -168(4) . . . 4_566 ? O4 Zn1 Zn2 N4 109.6(13) 4_566 . . 4_566 ? O2 Zn1 Zn2 N4 -70.2(13) . . . 4_566 ? O6 Zn1 Zn2 N4 -160.8(13) . . . 4_566 ? O8 Zn1 Zn2 N4 22.2(13) 1_455 . . 4_566 ? N1 Zn1 Zn2 O7 161(4) . . . 1_455 ? O4 Zn1 Zn2 O7 78.51(13) 4_566 . . 1_455 ? O2 Zn1 Zn2 O7 -101.28(14) . . . 1_455 ? O6 Zn1 Zn2 O7 168.10(14) . . . 1_455 ? O8 Zn1 Zn2 O7 -8.85(13) 1_455 . . 1_455 ? N1 Zn1 Zn2 O3 68(4) . . . 4_566 ? O4 Zn1 Zn2 O3 -14.65(13) 4_566 . . 4_566 ? O2 Zn1 Zn2 O3 165.57(14) . . . 4_566 ? O6 Zn1 Zn2 O3 74.94(14) . . . 4_566 ? O8 Zn1 Zn2 O3 -102.01(13) 1_455 . . 4_566 ? N1 Zn1 Zn2 O5 -22(4) . . . . ? O4 Zn1 Zn2 O5 -104.79(14) 4_566 . . . ? O2 Zn1 Zn2 O5 75.42(14) . . . . ? O6 Zn1 Zn2 O5 -15.20(14) . . . . ? O8 Zn1 Zn2 O5 167.85(13) 1_455 . . . ? N1 Zn1 Zn2 O1 -109(4) . . . . ? O4 Zn1 Zn2 O1 168.23(13) 4_566 . . . ? O2 Zn1 Zn2 O1 -11.56(14) . . . . ? O6 Zn1 Zn2 O1 -102.18(14) . . . . ? O8 Zn1 Zn2 O1 80.87(13) 1_455 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.543 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.079 # Attachment '- 3.cif' data_l2011052649_0m _database_code_depnum_ccdc_archive 'CCDC 877927' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Cd N4 O11' _chemical_formula_weight 676.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1561(6) _cell_length_b 10.2773(6) _cell_length_c 14.4890(9) _cell_angle_alpha 85.432(4) _cell_angle_beta 72.012(3) _cell_angle_gamma 83.560(3) _cell_volume 1427.70(15) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 7261 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 24.53 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8515 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20618 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5011 _reflns_number_gt 4404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.7227P] 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 5011 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.4896(3) -0.6288(3) 0.6209(2) 0.0329(6) Uani 1 1 d . . . C2 C 1.4186(3) -0.2603(3) 0.6415(2) 0.0385(7) Uani 1 1 d . . . C3 C 0.6642(3) 0.3092(3) 0.8238(2) 0.0369(7) Uani 1 1 d . . . C4 C 0.6326(3) 0.6641(3) 0.8920(2) 0.0388(7) Uani 1 1 d . . . C5 C 0.6836(3) 0.9290(3) 1.1269(2) 0.0382(7) Uani 1 1 d . . . H5 H 0.6233 0.8715 1.1665 0.046 Uiso 1 1 calc R . . C6 C 0.6929(3) 0.5396(3) 0.8622(2) 0.0397(7) Uani 1 1 d . . . H6 H 0.7877 0.5184 0.8513 0.048 Uiso 1 1 calc R . . C7 C 0.4695(3) 0.4819(3) 0.8631(2) 0.0426(8) Uani 1 1 d . . . H7 H 0.4139 0.4203 0.8554 0.051 Uiso 1 1 calc R . . C8 C 1.4191(3) -0.5046(3) 0.6381(2) 0.0332(6) Uani 1 1 d . . . H8 H 1.3224 -0.4949 0.6590 0.040 Uiso 1 1 calc R . . C9 C 0.8601(3) 0.1639(3) 0.7317(2) 0.0363(7) Uani 1 1 d . . . C10 C 0.4927(3) 0.6969(3) 0.9035(2) 0.0457(8) Uani 1 1 d . . . H10 H 0.4529 0.7807 0.9213 0.055 Uiso 1 1 calc R . . C11 C 1.6331(3) -0.6415(3) 0.5882(2) 0.0398(7) Uani 1 1 d . . . H11 H 1.6804 -0.7242 0.5754 0.048 Uiso 1 1 calc R . . C12 C 0.8017(3) 1.0113(3) 0.9687(2) 0.0446(8) Uani 1 1 d . . . H12 H 0.8239 1.0115 0.9014 0.054 Uiso 1 1 calc R . . C13 C 0.8218(3) 1.0956(3) 1.1109(3) 0.0430(8) Uani 1 1 d . . . H13 H 0.8595 1.1540 1.1392 0.052 Uiso 1 1 calc R . . C14 C 1.6376(3) -0.4104(3) 0.5927(2) 0.0428(8) Uani 1 1 d . . . H14 H 1.6875 -0.3376 0.5841 0.051 Uiso 1 1 calc R . . C15 C 0.9986(3) 0.1340(3) 0.7244(2) 0.0380(7) Uani 1 1 d . . . H15 H 1.0427 0.1921 0.7483 0.046 Uiso 1 1 calc R . . C16 C 0.7194(3) 0.7574(3) 0.9139(2) 0.0424(8) Uani 1 1 d . . . C17 C 0.6111(3) 0.4475(3) 0.8487(2) 0.0371(7) Uani 1 1 d . . . C18 C 1.7074(3) -0.5332(3) 0.5741(3) 0.0468(8) Uani 1 1 d . . . H18 H 1.8040 -0.5430 0.5522 0.056 Uiso 1 1 calc R . . C19 C 0.4120(3) 0.6063(4) 0.8885(3) 0.0496(9) Uani 1 1 d . . . H19 H 0.3183 0.6294 0.8957 0.059 Uiso 1 1 calc R . . C20 C 1.0068(3) -0.0579(4) 0.6534(3) 0.0536(9) Uani 1 1 d . . . H20 H 1.0571 -0.1335 0.6251 0.064 Uiso 1 1 calc R . . C21 C 0.7923(3) 0.0751(3) 0.7004(3) 0.0454(8) Uani 1 1 d . . . H21 H 0.6984 0.0911 0.7057 0.054 Uiso 1 1 calc R . . C22 C 1.4932(3) -0.3949(3) 0.6241(2) 0.0335(6) Uani 1 1 d . . . C23 C 1.4089(3) -0.7475(3) 0.6400(2) 0.0388(7) Uani 1 1 d . . . C24 C 0.7142(3) 0.9241(3) 1.0273(2) 0.0369(7) Uani 1 1 d . . . C25 C 0.8682(4) -0.0376(4) 0.6610(3) 0.0563(10) Uani 1 1 d . . . H25 H 0.8257 -0.0996 0.6397 0.068 Uiso 1 1 calc R . . C26 C 0.8555(3) 1.0982(3) 1.0120(3) 0.0465(8) Uani 1 1 d . . . H26 H 0.9144 1.1582 0.9741 0.056 Uiso 1 1 calc R . . Cd1 Cd 1.30811(2) -0.00064(2) 0.663095(16) 0.03443(9) Uani 1 1 d . . . H1W H 1.3757 -0.0469 0.4682 0.041 Uiso 1 1 d R . . H2W H 1.3659 0.0757 0.4670 0.041 Uiso 1 1 d R . . N1 N 1.0723(2) 0.0256(3) 0.68478(19) 0.0410(6) Uani 1 1 d . . . N2 N 0.7963(2) 0.2872(3) 0.76804(19) 0.0408(6) Uani 1 1 d . . . H2 H 0.8461 0.3526 0.7532 0.049 Uiso 1 1 calc R . . N3 N 0.6525(3) 0.8323(3) 0.99074(19) 0.0405(6) Uani 1 1 d . . . H3 H 0.5660 0.8230 1.0191 0.049 Uiso 1 1 calc R . . N4 N 0.7364(2) 1.0121(2) 1.16859(19) 0.0379(6) Uani 1 1 d . . . O1 O 1.3210(2) 0.0139(2) 0.49882(16) 0.0466(5) Uani 1 1 d . . . O2 O 1.4905(2) -0.1643(2) 0.62674(18) 0.0507(6) Uani 1 1 d . . . O3 O 1.2893(2) -0.2445(2) 0.67023(19) 0.0528(6) Uani 1 1 d . . . O4 O 1.4772(2) -0.8590(2) 0.62989(17) 0.0465(6) Uani 1 1 d . . . O5 O 1.2794(2) -0.7353(2) 0.6667(2) 0.0653(8) Uani 1 1 d . . . O6 O 0.5886(2) 0.2196(2) 0.85328(17) 0.0495(6) Uani 1 1 d . . . O7 O 0.8415(2) 0.7662(3) 0.8678(2) 0.0660(8) Uani 1 1 d . . . O8 O 0.0237(4) 0.4369(4) 0.6558(3) 0.1086(12) Uani 1 1 d . . . O9 O 0.0741(4) 0.6191(4) 0.7692(4) 0.153(2) Uani 1 1 d . . . O10 O 0.1178(9) 0.3663(8) 0.8723(6) 0.228(3) Uani 1 1 d . . . O11 O 0.0441(14) 0.2936(17) 0.4840(12) 0.235(7) Uani 0.50 1 d P . . O12 O 0.9652(16) 0.4112(16) 0.0277(15) 0.259(8) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0402(16) 0.0267(15) 0.0328(17) -0.0021(13) -0.0123(13) -0.0034(12) C2 0.0483(19) 0.0261(16) 0.0371(18) -0.0016(13) -0.0082(14) 0.0006(13) C3 0.0326(15) 0.0442(18) 0.0326(17) -0.0050(14) -0.0078(13) -0.0023(13) C4 0.0400(17) 0.0444(18) 0.0288(16) -0.0066(14) -0.0049(13) -0.0026(14) C5 0.0352(15) 0.0383(17) 0.0373(18) -0.0021(14) -0.0039(13) -0.0073(13) C6 0.0316(15) 0.0476(19) 0.0350(17) -0.0066(15) -0.0027(12) -0.0015(13) C7 0.0356(16) 0.052(2) 0.0414(19) -0.0097(16) -0.0136(14) 0.0000(14) C8 0.0334(15) 0.0286(15) 0.0353(17) -0.0013(13) -0.0075(12) -0.0015(12) C9 0.0318(15) 0.0395(17) 0.0336(17) -0.0031(14) -0.0046(12) -0.0008(12) C10 0.0477(19) 0.045(2) 0.043(2) -0.0105(16) -0.0152(15) 0.0095(15) C11 0.0397(17) 0.0282(16) 0.048(2) -0.0044(14) -0.0101(14) 0.0040(12) C12 0.0480(19) 0.046(2) 0.0345(18) -0.0001(15) -0.0051(14) -0.0056(15) C13 0.0415(17) 0.0350(17) 0.054(2) -0.0056(16) -0.0138(15) -0.0065(13) C14 0.0417(17) 0.0305(17) 0.055(2) 0.0042(15) -0.0128(15) -0.0094(13) C15 0.0316(15) 0.0432(18) 0.0374(18) -0.0065(15) -0.0066(13) -0.0041(13) C16 0.0388(17) 0.0445(19) 0.0374(18) -0.0046(15) -0.0018(14) -0.0023(14) C17 0.0342(15) 0.0455(19) 0.0293(16) -0.0046(14) -0.0064(12) -0.0008(13) C18 0.0333(16) 0.0402(19) 0.063(2) 0.0000(17) -0.0105(15) -0.0013(13) C19 0.0367(17) 0.058(2) 0.057(2) -0.0145(18) -0.0198(16) 0.0105(15) C20 0.0450(19) 0.053(2) 0.067(2) -0.0264(19) -0.0212(17) 0.0087(16) C21 0.0350(16) 0.051(2) 0.053(2) -0.0096(17) -0.0182(15) 0.0006(14) C22 0.0406(16) 0.0266(15) 0.0317(16) 0.0004(13) -0.0095(13) -0.0019(12) C23 0.0468(19) 0.0298(17) 0.0399(18) -0.0010(14) -0.0114(14) -0.0099(13) C24 0.0300(15) 0.0378(17) 0.0389(18) -0.0046(14) -0.0058(13) 0.0020(12) C25 0.050(2) 0.053(2) 0.076(3) -0.023(2) -0.0310(19) -0.0013(16) C26 0.0460(18) 0.0394(19) 0.047(2) 0.0052(16) -0.0024(15) -0.0127(14) Cd1 0.03072(12) 0.03070(13) 0.03977(15) -0.00658(9) -0.00705(9) -0.00099(8) N1 0.0313(13) 0.0455(16) 0.0441(16) -0.0092(13) -0.0083(11) 0.0007(11) N2 0.0285(13) 0.0388(15) 0.0499(16) -0.0090(13) -0.0028(11) -0.0029(10) N3 0.0337(13) 0.0460(16) 0.0388(15) -0.0110(13) -0.0029(11) -0.0077(11) N4 0.0361(13) 0.0363(14) 0.0409(15) -0.0068(12) -0.0096(11) -0.0039(11) O1 0.0429(12) 0.0527(14) 0.0409(13) -0.0036(11) -0.0064(10) -0.0081(10) O2 0.0549(14) 0.0231(11) 0.0631(16) 0.0018(11) -0.0020(11) -0.0063(10) O3 0.0443(13) 0.0328(13) 0.0751(17) -0.0107(12) -0.0095(12) 0.0031(10) O4 0.0559(14) 0.0231(11) 0.0582(15) -0.0086(10) -0.0117(11) -0.0047(10) O5 0.0420(14) 0.0405(14) 0.108(2) 0.0024(14) -0.0142(14) -0.0111(11) O6 0.0374(12) 0.0453(14) 0.0560(15) -0.0092(12) 0.0036(10) -0.0086(10) O7 0.0436(14) 0.0652(17) 0.0747(18) -0.0282(15) 0.0116(12) -0.0115(12) O8 0.082(2) 0.115(3) 0.121(3) 0.020(2) -0.014(2) -0.044(2) O9 0.073(2) 0.082(3) 0.245(6) -0.055(3) 0.052(3) -0.0199(19) O10 0.292(9) 0.204(7) 0.212(7) -0.044(6) -0.121(7) 0.027(6) O11 0.154(11) 0.252(17) 0.258(17) -0.049(13) 0.011(10) -0.029(11) O12 0.194(14) 0.206(15) 0.40(3) -0.008(16) -0.104(15) -0.057(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C11 1.381(4) . ? C1 C8 1.392(4) . ? C1 C23 1.506(4) . ? C2 O3 1.244(4) . ? C2 O2 1.259(4) . ? C2 C22 1.502(4) . ? C3 O6 1.230(4) . ? C3 N2 1.340(4) . ? C3 C17 1.494(4) . ? C4 C10 1.385(4) . ? C4 C6 1.395(4) . ? C4 C16 1.485(4) . ? C5 N4 1.329(4) . ? C5 C24 1.382(4) . ? C5 H5 0.9300 . ? C6 C17 1.389(4) . ? C6 H6 0.9300 . ? C7 C19 1.373(5) . ? C7 C17 1.396(4) . ? C7 H7 0.9300 . ? C8 C22 1.392(4) . ? C8 H8 0.9300 . ? C9 C15 1.379(4) . ? C9 C21 1.383(4) . ? C9 N2 1.419(4) . ? C10 C19 1.378(5) . ? C10 H10 0.9300 . ? C11 C18 1.381(4) . ? C11 H11 0.9300 . ? C12 C26 1.378(5) . ? C12 C24 1.381(4) . ? C12 H12 0.9300 . ? C13 N4 1.339(4) . ? C13 C26 1.365(5) . ? C13 H13 0.9300 . ? C14 C18 1.379(4) . ? C14 C22 1.389(4) . ? C14 H14 0.9300 . ? C15 N1 1.335(4) . ? C15 H15 0.9300 . ? C16 O7 1.224(4) . ? C16 N3 1.359(4) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 N1 1.327(4) . ? C20 C25 1.371(5) . ? C20 H20 0.9300 . ? C21 C25 1.376(5) . ? C21 H21 0.9300 . ? C23 O5 1.245(4) . ? C23 O4 1.265(4) . ? C24 N3 1.408(4) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? Cd1 O4 2.289(2) 1_565 ? Cd1 N1 2.304(2) . ? Cd1 O2 2.319(2) . ? Cd1 N4 2.335(3) 2_767 ? Cd1 O1 2.337(2) . ? Cd1 O3 2.526(2) . ? N2 H2 0.8600 . ? N3 H3 0.8600 . ? N4 Cd1 2.335(3) 2_767 ? O1 H1W 0.8429 . ? O1 H2W 0.8435 . ? O4 Cd1 2.289(2) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 C1 C8 119.4(3) . . ? C11 C1 C23 120.8(3) . . ? C8 C1 C23 119.8(3) . . ? O3 C2 O2 121.1(3) . . ? O3 C2 C22 120.8(3) . . ? O2 C2 C22 118.1(3) . . ? O6 C3 N2 121.7(3) . . ? O6 C3 C17 120.8(3) . . ? N2 C3 C17 117.4(3) . . ? C10 C4 C6 119.6(3) . . ? C10 C4 C16 121.3(3) . . ? C6 C4 C16 119.1(3) . . ? N4 C5 C24 123.1(3) . . ? N4 C5 H5 118.5 . . ? C24 C5 H5 118.5 . . ? C17 C6 C4 119.9(3) . . ? C17 C6 H6 120.0 . . ? C4 C6 H6 120.0 . . ? C19 C7 C17 120.4(3) . . ? C19 C7 H7 119.8 . . ? C17 C7 H7 119.8 . . ? C22 C8 C1 120.1(3) . . ? C22 C8 H8 120.0 . . ? C1 C8 H8 120.0 . . ? C15 C9 C21 118.7(3) . . ? C15 C9 N2 117.6(3) . . ? C21 C9 N2 123.6(3) . . ? C19 C10 C4 120.4(3) . . ? C19 C10 H10 119.8 . . ? C4 C10 H10 119.8 . . ? C1 C11 C18 120.9(3) . . ? C1 C11 H11 119.6 . . ? C18 C11 H11 119.6 . . ? C26 C12 C24 118.6(3) . . ? C26 C12 H12 120.7 . . ? C24 C12 H12 120.7 . . ? N4 C13 C26 122.5(3) . . ? N4 C13 H13 118.7 . . ? C26 C13 H13 118.7 . . ? C18 C14 C22 120.4(3) . . ? C18 C14 H14 119.8 . . ? C22 C14 H14 119.8 . . ? N1 C15 C9 123.1(3) . . ? N1 C15 H15 118.5 . . ? C9 C15 H15 118.5 . . ? O7 C16 N3 122.1(3) . . ? O7 C16 C4 123.4(3) . . ? N3 C16 C4 114.5(3) . . ? C6 C17 C7 119.4(3) . . ? C6 C17 C3 123.7(3) . . ? C7 C17 C3 116.8(3) . . ? C14 C18 C11 119.7(3) . . ? C14 C18 H18 120.1 . . ? C11 C18 H18 120.1 . . ? C7 C19 C10 120.2(3) . . ? C7 C19 H19 119.9 . . ? C10 C19 H19 119.9 . . ? N1 C20 C25 122.8(3) . . ? N1 C20 H20 118.6 . . ? C25 C20 H20 118.6 . . ? C25 C21 C9 118.0(3) . . ? C25 C21 H21 121.0 . . ? C9 C21 H21 121.0 . . ? C14 C22 C8 119.5(3) . . ? C14 C22 C2 119.8(3) . . ? C8 C22 C2 120.6(3) . . ? O5 C23 O4 121.7(3) . . ? O5 C23 C1 120.6(3) . . ? O4 C23 C1 117.7(3) . . ? C12 C24 C5 118.3(3) . . ? C12 C24 N3 123.2(3) . . ? C5 C24 N3 118.5(3) . . ? C20 C25 C21 119.7(3) . . ? C20 C25 H25 120.2 . . ? C21 C25 H25 120.2 . . ? C13 C26 C12 119.5(3) . . ? C13 C26 H26 120.2 . . ? C12 C26 H26 120.2 . . ? O4 Cd1 N1 133.95(9) 1_565 . ? O4 Cd1 O2 85.54(8) 1_565 . ? N1 Cd1 O2 138.98(9) . . ? O4 Cd1 N4 96.12(8) 1_565 2_767 ? N1 Cd1 N4 89.62(9) . 2_767 ? O2 Cd1 N4 97.59(9) . 2_767 ? O4 Cd1 O1 89.19(8) 1_565 . ? N1 Cd1 O1 82.87(8) . . ? O2 Cd1 O1 88.09(9) . . ? N4 Cd1 O1 172.49(8) 2_767 . ? O4 Cd1 O3 138.78(8) 1_565 . ? N1 Cd1 O3 86.80(9) . . ? O2 Cd1 O3 53.26(7) . . ? N4 Cd1 O3 88.85(9) 2_767 . ? O1 Cd1 O3 90.64(8) . . ? C20 N1 C15 117.7(3) . . ? C20 N1 Cd1 123.1(2) . . ? C15 N1 Cd1 119.1(2) . . ? C3 N2 C9 124.8(3) . . ? C3 N2 H2 117.6 . . ? C9 N2 H2 117.6 . . ? C16 N3 C24 124.9(3) . . ? C16 N3 H3 117.6 . . ? C24 N3 H3 117.6 . . ? C5 N4 C13 118.0(3) . . ? C5 N4 Cd1 120.2(2) . 2_767 ? C13 N4 Cd1 121.7(2) . 2_767 ? Cd1 O1 H1W 111.5 . . ? Cd1 O1 H2W 113.6 . . ? H1W O1 H2W 95.8 . . ? C2 O2 Cd1 97.49(19) . . ? C2 O3 Cd1 88.10(18) . . ? C23 O4 Cd1 103.35(18) . 1_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 C4 C6 C17 -3.2(5) . . . . ? C16 C4 C6 C17 175.0(3) . . . . ? C11 C1 C8 C22 -1.2(5) . . . . ? C23 C1 C8 C22 177.6(3) . . . . ? C6 C4 C10 C19 2.1(5) . . . . ? C16 C4 C10 C19 -176.0(3) . . . . ? C8 C1 C11 C18 1.2(5) . . . . ? C23 C1 C11 C18 -177.5(3) . . . . ? C21 C9 C15 N1 2.8(5) . . . . ? N2 C9 C15 N1 -174.9(3) . . . . ? C10 C4 C16 O7 -144.7(4) . . . . ? C6 C4 C16 O7 37.2(5) . . . . ? C10 C4 C16 N3 36.0(5) . . . . ? C6 C4 C16 N3 -142.1(3) . . . . ? C4 C6 C17 C7 1.5(5) . . . . ? C4 C6 C17 C3 -175.4(3) . . . . ? C19 C7 C17 C6 1.2(5) . . . . ? C19 C7 C17 C3 178.4(3) . . . . ? O6 C3 C17 C6 147.2(3) . . . . ? N2 C3 C17 C6 -33.2(5) . . . . ? O6 C3 C17 C7 -29.8(5) . . . . ? N2 C3 C17 C7 149.8(3) . . . . ? C22 C14 C18 C11 -0.9(5) . . . . ? C1 C11 C18 C14 -0.2(5) . . . . ? C17 C7 C19 C10 -2.3(5) . . . . ? C4 C10 C19 C7 0.6(5) . . . . ? C15 C9 C21 C25 -1.6(5) . . . . ? N2 C9 C21 C25 176.0(3) . . . . ? C18 C14 C22 C8 0.9(5) . . . . ? C18 C14 C22 C2 -178.3(3) . . . . ? C1 C8 C22 C14 0.2(5) . . . . ? C1 C8 C22 C2 179.4(3) . . . . ? O3 C2 C22 C14 -179.5(3) . . . . ? O2 C2 C22 C14 0.0(5) . . . . ? O3 C2 C22 C8 1.2(5) . . . . ? O2 C2 C22 C8 -179.2(3) . . . . ? C11 C1 C23 O5 -177.8(3) . . . . ? C8 C1 C23 O5 3.4(5) . . . . ? C11 C1 C23 O4 3.6(5) . . . . ? C8 C1 C23 O4 -175.2(3) . . . . ? C26 C12 C24 C5 0.6(5) . . . . ? C26 C12 C24 N3 179.3(3) . . . . ? N4 C5 C24 C12 -1.2(5) . . . . ? N4 C5 C24 N3 -179.9(3) . . . . ? N1 C20 C25 C21 1.7(6) . . . . ? C9 C21 C25 C20 -0.5(6) . . . . ? N4 C13 C26 C12 -0.7(5) . . . . ? C24 C12 C26 C13 0.3(5) . . . . ? C25 C20 N1 C15 -0.5(6) . . . . ? C25 C20 N1 Cd1 -175.7(3) . . . . ? C9 C15 N1 C20 -1.7(5) . . . . ? C9 C15 N1 Cd1 173.6(2) . . . . ? O4 Cd1 N1 C20 142.7(3) 1_565 . . . ? O2 Cd1 N1 C20 -18.0(4) . . . . ? N4 Cd1 N1 C20 -119.1(3) 2_767 . . . ? O1 Cd1 N1 C20 60.8(3) . . . . ? O3 Cd1 N1 C20 -30.3(3) . . . . ? O4 Cd1 N1 C15 -32.4(3) 1_565 . . . ? O2 Cd1 N1 C15 166.9(2) . . . . ? N4 Cd1 N1 C15 65.7(2) 2_767 . . . ? O1 Cd1 N1 C15 -114.3(2) . . . . ? O3 Cd1 N1 C15 154.6(2) . . . . ? O6 C3 N2 C9 4.5(5) . . . . ? C17 C3 N2 C9 -175.1(3) . . . . ? C15 C9 N2 C3 -144.8(3) . . . . ? C21 C9 N2 C3 37.6(5) . . . . ? O7 C16 N3 C24 -1.7(5) . . . . ? C4 C16 N3 C24 177.6(3) . . . . ? C12 C24 N3 C16 44.0(5) . . . . ? C5 C24 N3 C16 -137.4(3) . . . . ? C24 C5 N4 C13 0.8(5) . . . . ? C24 C5 N4 Cd1 -175.1(2) . . . 2_767 ? C26 C13 N4 C5 0.2(5) . . . . ? C26 C13 N4 Cd1 176.0(2) . . . 2_767 ? O3 C2 O2 Cd1 -2.1(3) . . . . ? C22 C2 O2 Cd1 178.3(2) . . . . ? O4 Cd1 O2 C2 179.5(2) 1_565 . . . ? N1 Cd1 O2 C2 -14.3(3) . . . . ? N4 Cd1 O2 C2 84.0(2) 2_767 . . . ? O1 Cd1 O2 C2 -91.1(2) . . . . ? O3 Cd1 O2 C2 1.12(18) . . . . ? O2 C2 O3 Cd1 1.9(3) . . . . ? C22 C2 O3 Cd1 -178.5(3) . . . . ? O4 Cd1 O3 C2 -3.5(3) 1_565 . . . ? N1 Cd1 O3 C2 168.8(2) . . . . ? O2 Cd1 O3 C2 -1.12(18) . . . . ? N4 Cd1 O3 C2 -101.5(2) 2_767 . . . ? O1 Cd1 O3 C2 86.0(2) . . . . ? O5 C23 O4 Cd1 2.8(4) . . . 1_545 ? C1 C23 O4 Cd1 -178.6(2) . . . 1_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.863 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.067 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 877928' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 Cd N4 O8' _chemical_formula_weight 628.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 8.2505(9) _cell_length_b 30.086(3) _cell_length_c 10.3031(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.9130(10) _cell_angle_gamma 90.00 _cell_volume 2519.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9950 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7816 _exptl_absorpt_correction_T_max 0.8223 _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19129 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4433 _reflns_number_gt 4270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+5.7419P] 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 4433 _refine_ls_number_parameters 364 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.247 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2779(4) 0.46711(12) 0.1610(3) 0.0256(8) Uani 1 1 d . . . C2 C 0.2606(4) 0.46815(12) -0.0861(3) 0.0261(8) Uani 1 1 d . . . H2 H 0.1565 0.4808 -0.0946 0.031 Uiso 1 1 calc R . . C3 C 0.3492(4) 0.45824(12) 0.0387(3) 0.0246(7) Uani 1 1 d . . . C4 C 0.5063(5) 0.44056(13) 0.0506(3) 0.0303(8) Uani 1 1 d . . . H4 H 0.5665 0.4348 0.1338 0.036 Uiso 1 1 calc R . . C5 C 0.2405(4) 0.47021(12) 0.6658(3) 0.0272(8) Uani 1 1 d . . . C6 C 0.5744(5) 0.43142(14) -0.0606(4) 0.0354(9) Uani 1 1 d . . . H6 H 0.6797 0.4195 -0.0520 0.042 Uiso 1 1 calc R . . C7 C 0.4852(5) 0.44011(14) 0.8157(4) 0.0328(9) Uani 1 1 d . . . H7 H 0.5298 0.4334 0.7411 0.039 Uiso 1 1 calc R . . C8 C 0.3288(4) 0.45891(12) 0.8022(3) 0.0259(8) Uani 1 1 d . . . C9 C 0.1395(5) 0.58164(14) 0.3066(4) 0.0352(9) Uani 1 1 d . . . H9 H 0.0593 0.5698 0.2413 0.042 Uiso 1 1 calc R . . C10 C 0.1741(6) 0.62603(15) 0.3044(4) 0.0481(12) Uani 1 1 d . . . H10 H 0.1165 0.6440 0.2386 0.058 Uiso 1 1 calc R . . C11 C 0.2936(6) 0.64434(15) 0.3989(4) 0.0468(11) Uani 1 1 d . . . H11 H 0.3196 0.6744 0.3963 0.056 Uiso 1 1 calc R . . C12 C 0.3750(5) 0.61712(13) 0.4983(4) 0.0341(9) Uani 1 1 d . . . C13 C 0.3319(5) 0.57224(13) 0.4950(4) 0.0309(8) Uani 1 1 d . . . H13 H 0.3846 0.5537 0.5613 0.037 Uiso 1 1 calc R . . C14 C 0.5310(6) 0.67431(14) 0.6389(5) 0.0444(11) Uani 1 1 d . . . C15 C 0.6513(5) 0.68225(14) 0.7630(4) 0.0383(10) Uani 1 1 d . . . C16 C 0.7120(7) 0.64867(16) 0.8494(5) 0.0536(13) Uani 1 1 d . . . H16 H 0.6845 0.6193 0.8283 0.064 Uiso 1 1 calc R . . C17 C 0.8133(8) 0.65862(17) 0.9669(5) 0.0714(18) Uani 1 1 d . . . H17 H 0.8531 0.6359 1.0249 0.086 Uiso 1 1 calc R . . C18 C 0.8560(7) 0.70215(16) 0.9990(5) 0.0614(15) Uani 1 1 d . . . H18 H 0.9225 0.7087 1.0791 0.074 Uiso 1 1 calc R . . C19 C 0.7998(6) 0.73617(14) 0.9119(5) 0.0437(11) Uani 1 1 d . . . C20 C 0.6961(6) 0.72614(14) 0.7955(4) 0.0438(11) Uani 1 1 d . . . H20 H 0.6555 0.7489 0.7380 0.053 Uiso 1 1 calc R . . C21 C 0.1634(6) 0.28428(15) 0.5555(5) 0.0477(11) Uani 1 1 d . . . C22 C -0.0080(5) 0.33120(14) 0.3855(4) 0.0394(10) Uani 1 1 d . . . C23 C -0.1237(6) 0.32809(15) 0.2716(5) 0.0503(12) Uani 1 1 d . . . H23 H -0.1713 0.3008 0.2456 0.060 Uiso 1 1 calc R . . C24 C -0.1679(6) 0.36519(16) 0.1975(5) 0.0532(13) Uani 1 1 d . . . H24 H -0.2468 0.3635 0.1215 0.064 Uiso 1 1 calc R . . C25 C -0.0941(5) 0.40511(15) 0.2370(4) 0.0435(11) Uani 1 1 d . . . H25 H -0.1235 0.4303 0.1859 0.052 Uiso 1 1 calc R . . C26 C 0.0611(5) 0.37271(13) 0.4205(4) 0.0357(9) Uani 1 1 d . . . H26 H 0.1386 0.3754 0.4971 0.043 Uiso 1 1 calc R . . Cd1 Cd 0.14747(3) 0.479301(9) 0.38506(2) 0.02580(10) Uani 1 1 d . . . N1 N 0.2187(4) 0.55470(10) 0.4010(3) 0.0297(7) Uani 1 1 d . . . N2 N 0.4966(4) 0.63126(11) 0.6030(3) 0.0378(8) Uani 1 1 d D . . N3 N 0.0347(5) 0.29142(12) 0.4560(4) 0.0488(10) Uani 1 1 d D . . N4 N 0.0187(4) 0.40888(11) 0.3466(3) 0.0326(7) Uani 1 1 d . . . O1 O 0.1190(3) 0.49536(10) 0.6520(3) 0.0397(7) Uani 1 1 d . . . O2 O 0.2983(4) 0.45423(11) 0.5706(3) 0.0445(8) Uani 1 1 d . . . O3 O 0.1430(3) 0.48688(9) 0.1525(2) 0.0346(6) Uani 1 1 d . . . O4 O 0.3569(3) 0.45307(9) 0.2704(2) 0.0322(6) Uani 1 1 d . . . O5 O 0.4637(5) 0.70557(11) 0.5757(4) 0.0768(13) Uani 1 1 d . . . O6 O 0.2445(5) 0.31444(12) 0.6134(4) 0.0834(15) Uani 1 1 d . . . O8 O 0.4928(7) 0.32912(19) 0.8339(7) 0.126(2) Uani 1 1 d . . . O7 O 0.2440(7) 0.77204(19) 0.6116(11) 0.166(4) Uani 1 1 d D . . H3M H -0.031(10) 0.270(2) 0.424(10) 0.199 Uiso 1 1 d D . . H2M H 0.554(11) 0.610(2) 0.644(9) 0.199 Uiso 1 1 d D . . H2W H 0.306(11) 0.795(2) 0.609(11) 0.199 Uiso 1 1 d D . . H1W H 0.313(11) 0.755(3) 0.585(12) 0.199 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0322(19) 0.0233(19) 0.0214(17) -0.0009(15) 0.0052(15) -0.0035(15) C2 0.0297(19) 0.0239(19) 0.0243(18) 0.0005(15) 0.0037(15) 0.0021(14) C3 0.0292(18) 0.0239(19) 0.0206(17) 0.0002(14) 0.0044(14) -0.0001(14) C4 0.035(2) 0.036(2) 0.0186(17) 0.0026(15) 0.0022(15) 0.0035(17) C5 0.031(2) 0.028(2) 0.0217(18) 0.0019(15) 0.0028(15) -0.0026(16) C6 0.029(2) 0.049(3) 0.028(2) 0.0038(18) 0.0051(16) 0.0151(18) C7 0.038(2) 0.040(2) 0.0220(18) 0.0002(16) 0.0101(16) 0.0077(18) C8 0.0307(19) 0.027(2) 0.0198(17) 0.0012(15) 0.0040(14) 0.0024(15) C9 0.041(2) 0.037(2) 0.0256(19) 0.0012(17) 0.0012(17) -0.0014(18) C10 0.062(3) 0.035(3) 0.040(2) 0.008(2) -0.009(2) 0.001(2) C11 0.068(3) 0.027(2) 0.042(2) 0.0031(19) 0.000(2) -0.005(2) C12 0.038(2) 0.031(2) 0.032(2) -0.0019(17) 0.0032(17) -0.0010(17) C13 0.036(2) 0.028(2) 0.0273(19) 0.0010(16) 0.0027(16) 0.0009(16) C14 0.052(3) 0.030(2) 0.047(3) -0.005(2) -0.003(2) -0.004(2) C15 0.043(2) 0.029(2) 0.041(2) -0.0095(18) 0.0052(19) -0.0052(18) C16 0.074(3) 0.031(2) 0.050(3) -0.006(2) -0.006(2) -0.011(2) C17 0.108(5) 0.037(3) 0.056(3) 0.005(2) -0.025(3) -0.013(3) C18 0.087(4) 0.039(3) 0.049(3) -0.006(2) -0.017(3) -0.014(3) C19 0.049(3) 0.031(2) 0.048(3) -0.008(2) 0.000(2) -0.0052(19) C20 0.051(3) 0.031(2) 0.047(3) -0.005(2) 0.000(2) -0.0019(19) C21 0.056(3) 0.029(2) 0.053(3) 0.008(2) -0.005(2) 0.003(2) C22 0.042(2) 0.030(2) 0.044(2) 0.0086(19) 0.0011(19) 0.0038(18) C23 0.050(3) 0.030(2) 0.064(3) 0.003(2) -0.009(2) -0.001(2) C24 0.058(3) 0.040(3) 0.052(3) 0.006(2) -0.018(2) -0.001(2) C25 0.044(2) 0.037(2) 0.045(2) 0.010(2) -0.006(2) 0.0003(19) C26 0.038(2) 0.032(2) 0.035(2) 0.0048(18) 0.0002(17) 0.0041(17) Cd1 0.03145(16) 0.02699(17) 0.01849(14) 0.00070(11) 0.00304(10) 0.00390(11) N1 0.0322(16) 0.0299(18) 0.0267(16) -0.0047(14) 0.0042(13) -0.0040(14) N2 0.044(2) 0.0288(19) 0.0377(19) -0.0057(15) -0.0016(15) -0.0049(15) N3 0.051(2) 0.031(2) 0.058(2) 0.0117(18) -0.0073(19) 0.0015(17) N4 0.0352(18) 0.0281(18) 0.0333(17) 0.0057(14) 0.0029(14) 0.0031(14) O1 0.0335(15) 0.0508(18) 0.0339(15) 0.0125(13) 0.0031(12) 0.0122(13) O2 0.0558(18) 0.059(2) 0.0183(13) 0.0001(13) 0.0044(12) 0.0219(15) O3 0.0375(15) 0.0444(17) 0.0234(13) 0.0029(12) 0.0096(11) 0.0089(13) O4 0.0398(15) 0.0379(16) 0.0184(12) 0.0024(11) 0.0036(11) 0.0045(12) O5 0.103(3) 0.0324(19) 0.077(3) -0.0050(18) -0.036(2) 0.0005(19) O6 0.102(3) 0.033(2) 0.093(3) 0.013(2) -0.046(3) -0.001(2) O8 0.118(5) 0.091(4) 0.163(6) -0.004(4) 0.009(4) 0.003(3) O7 0.073(4) 0.064(3) 0.348(11) -0.003(5) 0.003(5) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O3 1.252(4) . ? C1 O4 1.272(4) . ? C1 C3 1.503(5) . ? C2 C8 1.393(5) 1_554 ? C2 C3 1.398(5) . ? C2 H2 0.9300 . ? C3 C4 1.386(5) . ? C4 C6 1.388(5) . ? C4 H4 0.9300 . ? C5 O1 1.244(5) . ? C5 O2 1.258(4) . ? C5 C8 1.507(5) . ? C6 C7 1.382(5) 1_554 ? C6 H6 0.9300 . ? C7 C6 1.382(5) 1_556 ? C7 C8 1.394(5) . ? C7 H7 0.9300 . ? C8 C2 1.393(5) 1_556 ? C9 N1 1.346(5) . ? C9 C10 1.366(6) . ? C9 H9 0.9300 . ? C10 C11 1.376(6) . ? C10 H10 0.9300 . ? C11 C12 1.391(6) . ? C11 H11 0.9300 . ? C12 C13 1.395(5) . ? C12 N2 1.407(5) . ? C13 N1 1.333(5) . ? C13 H13 0.9300 . ? C14 O5 1.222(5) . ? C14 N2 1.363(5) . ? C14 C15 1.497(6) . ? C15 C16 1.382(6) . ? C15 C20 1.396(6) . ? C16 C17 1.381(7) . ? C16 H16 0.9300 . ? C17 C18 1.381(7) . ? C17 H17 0.9300 . ? C18 C19 1.387(7) . ? C18 H18 0.9300 . ? C19 C20 1.381(6) . ? C19 C21 1.505(6) 2_656 ? C20 H20 0.9300 . ? C21 O6 1.221(6) . ? C21 N3 1.360(6) . ? C21 C19 1.505(6) 2_646 ? C22 C23 1.382(6) . ? C22 C26 1.394(6) . ? C22 N3 1.413(5) . ? C23 C24 1.366(6) . ? C23 H23 0.9300 . ? C24 C25 1.376(6) . ? C24 H24 0.9300 . ? C25 N4 1.339(5) . ? C25 H25 0.9300 . ? C26 N4 1.339(5) . ? C26 H26 0.9300 . ? Cd1 O2 2.226(3) . ? Cd1 O1 2.296(3) 3_566 ? Cd1 N1 2.342(3) . ? Cd1 N4 2.373(3) . ? Cd1 O4 2.389(3) . ? Cd1 O3 2.401(3) . ? N2 H2M 0.86(2) . ? N3 H3M 0.86(2) . ? O1 Cd1 2.296(3) 3_566 ? O7 H2W 0.86(2) . ? O7 H1W 0.85(2) . ? 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 C1 O4 122.2(3) . . ? O3 C1 C3 119.8(3) . . ? O4 C1 C3 117.9(3) . . ? C8 C2 C3 119.7(3) 1_554 . ? C8 C2 H2 120.1 1_554 . ? C3 C2 H2 120.1 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 C1 119.3(3) . . ? C2 C3 C1 121.0(3) . . ? C3 C4 C6 120.6(3) . . ? C3 C4 H4 119.7 . . ? C6 C4 H4 119.7 . . ? O1 C5 O2 123.4(3) . . ? O1 C5 C8 119.6(3) . . ? O2 C5 C8 117.0(3) . . ? C7 C6 C4 119.8(3) 1_554 . ? C7 C6 H6 120.1 1_554 . ? C4 C6 H6 120.1 . . ? C6 C7 C8 120.4(3) 1_556 . ? C6 C7 H7 119.8 1_556 . ? C8 C7 H7 119.8 . . ? C2 C8 C7 119.8(3) 1_556 . ? C2 C8 C5 121.7(3) 1_556 . ? C7 C8 C5 118.4(3) . . ? N1 C9 C10 121.6(4) . . ? N1 C9 H9 119.2 . . ? C10 C9 H9 119.2 . . ? C9 C10 C11 120.4(4) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C12 118.8(4) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C11 C12 C13 117.6(4) . . ? C11 C12 N2 125.2(4) . . ? C13 C12 N2 117.2(3) . . ? N1 C13 C12 123.0(4) . . ? N1 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? O5 C14 N2 122.2(4) . . ? O5 C14 C15 120.4(4) . . ? N2 C14 C15 117.4(4) . . ? C16 C15 C20 119.0(4) . . ? C16 C15 C14 123.2(4) . . ? C20 C15 C14 117.7(4) . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.4(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 119.2(4) . . ? C20 C19 C21 118.4(4) . 2_656 ? C18 C19 C21 122.2(4) . 2_656 ? C19 C20 C15 120.9(4) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? O6 C21 N3 122.8(4) . . ? O6 C21 C19 122.2(4) . 2_646 ? N3 C21 C19 114.9(4) . 2_646 ? C23 C22 C26 118.2(4) . . ? C23 C22 N3 117.0(4) . . ? C26 C22 N3 124.8(4) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 119.1(4) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N4 C25 C24 122.1(4) . . ? N4 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? N4 C26 C22 121.7(4) . . ? N4 C26 H26 119.1 . . ? C22 C26 H26 119.1 . . ? O2 Cd1 O1 129.29(10) . 3_566 ? O2 Cd1 N1 99.87(11) . . ? O1 Cd1 N1 84.93(11) 3_566 . ? O2 Cd1 N4 90.51(12) . . ? O1 Cd1 N4 83.13(11) 3_566 . ? N1 Cd1 N4 167.52(11) . . ? O2 Cd1 O4 88.16(9) . . ? O1 Cd1 O4 141.33(9) 3_566 . ? N1 Cd1 O4 99.23(10) . . ? N4 Cd1 O4 87.92(10) . . ? O2 Cd1 O3 143.10(10) . . ? O1 Cd1 O3 87.29(9) 3_566 . ? N1 Cd1 O3 86.48(10) . . ? N4 Cd1 O3 89.35(10) . . ? O4 Cd1 O3 54.96(9) . . ? C13 N1 C9 118.6(3) . . ? C13 N1 Cd1 124.8(3) . . ? C9 N1 Cd1 116.6(2) . . ? C14 N2 C12 125.7(4) . . ? C14 N2 H2M 120(7) . . ? C12 N2 H2M 114(7) . . ? C21 N3 C22 127.9(4) . . ? C21 N3 H3M 122(7) . . ? C22 N3 H3M 110(7) . . ? C25 N4 C26 119.1(4) . . ? C25 N4 Cd1 116.3(3) . . ? C26 N4 Cd1 124.4(3) . . ? C5 O1 Cd1 161.9(3) . 3_566 ? C5 O2 Cd1 108.0(2) . . ? C1 O3 Cd1 91.4(2) . . ? C1 O4 Cd1 91.4(2) . . ? H2W O7 H1W 93(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 C8 C2 C3 C4 2.0(6) 1_554 . . . ? C8 C2 C3 C1 -179.0(3) 1_554 . . . ? O3 C1 C3 C4 173.3(4) . . . . ? O4 C1 C3 C4 -8.3(5) . . . . ? O3 C1 C3 C2 -5.8(5) . . . . ? O4 C1 C3 C2 172.7(3) . . . . ? C2 C3 C4 C6 -1.9(6) . . . . ? C1 C3 C4 C6 179.1(4) . . . . ? C3 C4 C6 C7 0.2(6) . . . 1_554 ? C6 C7 C8 C2 -1.3(6) 1_556 . . 1_556 ? C6 C7 C8 C5 176.5(4) 1_556 . . . ? O1 C5 C8 C2 13.3(6) . . . 1_556 ? O2 C5 C8 C2 -168.7(4) . . . 1_556 ? O1 C5 C8 C7 -164.5(4) . . . . ? O2 C5 C8 C7 13.6(5) . . . . ? N1 C9 C10 C11 0.8(7) . . . . ? C9 C10 C11 C12 -1.8(8) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C10 C11 C12 N2 -178.4(4) . . . . ? C11 C12 C13 N1 0.6(6) . . . . ? N2 C12 C13 N1 -179.9(4) . . . . ? O5 C14 C15 C16 169.6(5) . . . . ? N2 C14 C15 C16 -8.2(7) . . . . ? O5 C14 C15 C20 -6.6(7) . . . . ? N2 C14 C15 C20 175.5(4) . . . . ? C20 C15 C16 C17 1.0(8) . . . . ? C14 C15 C16 C17 -175.2(5) . . . . ? C15 C16 C17 C18 -0.5(10) . . . . ? C16 C17 C18 C19 -1.3(10) . . . . ? C17 C18 C19 C20 2.4(9) . . . . ? C17 C18 C19 C21 177.3(6) . . . 2_656 ? C18 C19 C20 C15 -1.9(8) . . . . ? C21 C19 C20 C15 -176.9(4) 2_656 . . . ? C16 C15 C20 C19 0.1(7) . . . . ? C14 C15 C20 C19 176.6(4) . . . . ? C26 C22 C23 C24 -0.4(8) . . . . ? N3 C22 C23 C24 -178.7(5) . . . . ? C22 C23 C24 C25 0.9(8) . . . . ? C23 C24 C25 N4 -0.7(8) . . . . ? C23 C22 C26 N4 -0.4(7) . . . . ? N3 C22 C26 N4 177.8(4) . . . . ? C12 C13 N1 C9 -1.6(6) . . . . ? C12 C13 N1 Cd1 177.6(3) . . . . ? C10 C9 N1 C13 0.9(6) . . . . ? C10 C9 N1 Cd1 -178.4(4) . . . . ? O2 Cd1 N1 C13 5.2(3) . . . . ? O1 Cd1 N1 C13 134.2(3) 3_566 . . . ? N4 Cd1 N1 C13 151.1(5) . . . . ? O4 Cd1 N1 C13 -84.5(3) . . . . ? O3 Cd1 N1 C13 -138.2(3) . . . . ? O2 Cd1 N1 C9 -175.6(3) . . . . ? O1 Cd1 N1 C9 -46.5(3) 3_566 . . . ? N4 Cd1 N1 C9 -29.6(7) . . . . ? O4 Cd1 N1 C9 94.7(3) . . . . ? O3 Cd1 N1 C9 41.1(3) . . . . ? O5 C14 N2 C12 -5.0(8) . . . . ? C15 C14 N2 C12 172.9(4) . . . . ? C11 C12 N2 C14 13.9(7) . . . . ? C13 C12 N2 C14 -165.6(4) . . . . ? O6 C21 N3 C22 13.5(9) . . . . ? C19 C21 N3 C22 -165.7(5) 2_646 . . . ? C23 C22 N3 C21 167.3(5) . . . . ? C26 C22 N3 C21 -10.9(8) . . . . ? C24 C25 N4 C26 -0.1(7) . . . . ? C24 C25 N4 Cd1 174.5(4) . . . . ? C22 C26 N4 C25 0.6(6) . . . . ? C22 C26 N4 Cd1 -173.5(3) . . . . ? O2 Cd1 N4 C25 -179.9(3) . . . . ? O1 Cd1 N4 C25 50.6(3) 3_566 . . . ? N1 Cd1 N4 C25 33.6(7) . . . . ? O4 Cd1 N4 C25 -91.8(3) . . . . ? O3 Cd1 N4 C25 -36.8(3) . . . . ? O2 Cd1 N4 C26 -5.6(3) . . . . ? O1 Cd1 N4 C26 -135.2(3) 3_566 . . . ? N1 Cd1 N4 C26 -152.1(4) . . . . ? O4 Cd1 N4 C26 82.5(3) . . . . ? O3 Cd1 N4 C26 137.5(3) . . . . ? O2 C5 O1 Cd1 80.2(9) . . . 3_566 ? C8 C5 O1 Cd1 -101.9(8) . . . 3_566 ? O1 C5 O2 Cd1 0.3(5) . . . . ? C8 C5 O2 Cd1 -177.7(3) . . . . ? O1 Cd1 O2 C5 -23.7(3) 3_566 . . . ? N1 Cd1 O2 C5 67.8(3) . . . . ? N4 Cd1 O2 C5 -105.2(3) . . . . ? O4 Cd1 O2 C5 166.9(3) . . . . ? O3 Cd1 O2 C5 165.2(2) . . . . ? O4 C1 O3 Cd1 -0.9(4) . . . . ? C3 C1 O3 Cd1 177.5(3) . . . . ? O2 Cd1 O3 C1 2.6(3) . . . . ? O1 Cd1 O3 C1 -170.6(2) 3_566 . . . ? N1 Cd1 O3 C1 104.3(2) . . . . ? N4 Cd1 O3 C1 -87.4(2) . . . . ? O4 Cd1 O3 C1 0.5(2) . . . . ? O3 C1 O4 Cd1 0.9(4) . . . . ? C3 C1 O4 Cd1 -177.5(3) . . . . ? O2 Cd1 O4 C1 -179.2(2) . . . . ? O1 Cd1 O4 C1 13.9(3) 3_566 . . . ? N1 Cd1 O4 C1 -79.5(2) . . . . ? N4 Cd1 O4 C1 90.2(2) . . . . ? O3 Cd1 O4 C1 -0.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.670 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.075