# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_mo-da541pnna-04 _database_code_depnum_ccdc_archive 'CCDC 910862' #TrackingRef 'Mo-DA541Pnna-04X.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90.50 H104 N6 O10.50 Zn3' _chemical_formula_weight 1639.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 27.692(7) _cell_length_b 23.442(6) _cell_length_c 14.633(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9499(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4713 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 20.56 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.147 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3452 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8554 _exptl_absorpt_correction_T_max 0.9237 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 7792 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2635 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 25.44 _reflns_number_total 7792 _reflns_number_gt 2941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.1719P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7792 _refine_ls_number_parameters 773 _refine_ls_number_restraints 741 _refine_ls_R_factor_all 0.1864 _refine_ls_R_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.3151 _refine_ls_wR_factor_gt 0.2954 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 1.059 _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 1.0833(3) -0.0009(4) -0.0226(6) 0.062(2) Uani 1 1 d D . . C2 C 1.1063(3) -0.0351(3) -0.0940(6) 0.068(3) Uani 1 1 d D . . C3 C 1.0897(4) -0.0243(4) -0.1836(6) 0.078(3) Uani 1 1 d D . . H3 H 1.1041 -0.0456 -0.2317 0.094 Uiso 1 1 calc R . . C4 C 1.0551(4) 0.0137(4) -0.2064(6) 0.077(3) Uani 1 1 d D . . H4 H 1.0455 0.0182 -0.2683 0.092 Uiso 1 1 calc R . . C5 C 1.0338(3) 0.0460(3) -0.1385(6) 0.070(3) Uani 1 1 d D . . H5 H 1.0091 0.0724 -0.1543 0.084 Uiso 1 1 calc R . . C6 C 1.0481(3) 0.0407(4) -0.0453(6) 0.064(2) Uani 1 1 d D . . C7 C 1.0251(3) 0.0764(3) 0.0164(6) 0.058(2) Uani 1 1 d D . . H7 H 0.9999 0.0997 -0.0071 0.070 Uiso 1 1 calc R . . C8 C 1.1459(3) -0.0760(4) -0.0715(5) 0.077(3) Uani 1 1 d D . . C9 C 1.1276(3) -0.1252(3) -0.0073(6) 0.081(3) Uani 1 1 d D . . H9A H 1.1180 -0.1091 0.0519 0.122 Uiso 1 1 calc R . . H9B H 1.1535 -0.1530 0.0019 0.122 Uiso 1 1 calc R . . H9C H 1.0998 -0.1441 -0.0355 0.122 Uiso 1 1 calc R . . C10 C 1.1885(3) -0.0462(5) -0.0250(8) 0.111(4) Uani 1 1 d D . . H10A H 1.2011 -0.0162 -0.0652 0.167 Uiso 1 1 calc R . . H10B H 1.2140 -0.0741 -0.0126 0.167 Uiso 1 1 calc R . . H10C H 1.1777 -0.0291 0.0327 0.167 Uiso 1 1 calc R . . C11 C 1.1650(4) -0.1058(4) -0.1608(6) 0.101(3) Uani 1 1 d D . . H11A H 1.1390 -0.1285 -0.1881 0.151 Uiso 1 1 calc R . . H11B H 1.1922 -0.1307 -0.1455 0.151 Uiso 1 1 calc R . . H11C H 1.1756 -0.0767 -0.2045 0.151 Uiso 1 1 calc R . . C17 C 1.0401(3) 0.0448(3) 0.3640(6) 0.070(3) Uani 1 1 d D . . H17 H 1.0226 0.0669 0.4073 0.083 Uiso 1 1 calc R . . C18 C 1.0658(3) -0.0052(4) 0.3981(6) 0.062(2) Uani 1 1 d D . . C19 C 1.0656(4) -0.0126(4) 0.4928(6) 0.086(3) Uani 1 1 d D . . H19 H 1.0510 0.0157 0.5302 0.103 Uiso 1 1 calc R . . C20 C 1.0858(4) -0.0598(4) 0.5334(7) 0.084(3) Uani 1 1 d D . . H20 H 1.0867 -0.0635 0.5981 0.100 Uiso 1 1 calc R . . C21 C 1.1046(3) -0.1015(4) 0.4776(7) 0.076(3) Uani 1 1 d D . . H21 H 1.1167 -0.1352 0.5055 0.092 Uiso 1 1 calc R . . C22 C 1.1069(3) -0.0974(3) 0.3833(6) 0.066(2) Uani 1 1 d D . . C23 C 1.0864(3) -0.0461(4) 0.3418(6) 0.065(3) Uani 1 1 d D . . C24 C 1.1258(4) -0.1446(3) 0.3230(6) 0.081(3) Uani 1 1 d D . . C25 C 1.1692(4) -0.1244(4) 0.2683(7) 0.092(3) Uani 1 1 d D . . H25A H 1.1607 -0.0896 0.2349 0.138 Uiso 1 1 calc R . . H25B H 1.1787 -0.1541 0.2248 0.138 Uiso 1 1 calc R . . H25C H 1.1961 -0.1165 0.3099 0.138 Uiso 1 1 calc R . . C26 C 1.1439(4) -0.1965(4) 0.3810(7) 0.101(4) Uani 1 1 d D . . H26A H 1.1687 -0.1837 0.4240 0.151 Uiso 1 1 calc R . . H26B H 1.1576 -0.2255 0.3403 0.151 Uiso 1 1 calc R . . H26C H 1.1167 -0.2129 0.4150 0.151 Uiso 1 1 calc R . . C27 C 1.0858(4) -0.1663(4) 0.2574(7) 0.097(4) Uani 1 1 d D . . H27A H 1.0587 -0.1813 0.2932 0.146 Uiso 1 1 calc R . . H27B H 1.0989 -0.1966 0.2185 0.146 Uiso 1 1 calc R . . H27C H 1.0746 -0.1347 0.2191 0.146 Uiso 1 1 calc R . . N1 N 1.0344(2) 0.0813(3) 0.1036(5) 0.0619(19) Uani 1 1 d D . . N2 N 1.0391(2) 0.0616(3) 0.2797(5) 0.0599(19) Uani 1 1 d D . . O1 O 1.0965(2) -0.0109(2) 0.0620(4) 0.0822(19) Uani 1 1 d D . . O2 O 1.0896(2) -0.0411(2) 0.2529(4) 0.0778(19) Uani 1 1 d D . . Zn1 Zn 1.07861(4) 0.02553(4) 0.17502(7) 0.0699(5) Uani 1 1 d D B . C12 C 1.0101(3) 0.1204(4) 0.1582(6) 0.056(2) Uani 1 1 d . . . C13 C 0.9868(3) 0.1699(3) 0.1240(5) 0.058(2) Uani 1 1 d . . . H13 H 0.9869 0.1781 0.0604 0.069 Uiso 1 1 calc R . . C14 C 0.9630(3) 0.1928(3) 0.2807(6) 0.057(2) Uani 1 1 d . . . C15 C 0.9868(3) 0.1440(4) 0.3105(6) 0.066(3) Uani 1 1 d . . . H15 H 0.9857 0.1347 0.3736 0.079 Uiso 1 1 calc R . . C16 C 1.0116(3) 0.1091(3) 0.2527(6) 0.056(2) Uani 1 1 d . . . C28 C 0.9381(3) 0.2381(3) 0.3371(5) 0.055(2) Uani 1 1 d . . . H28 H 0.9379 0.2292 0.4040 0.066 Uiso 1 1 calc R . . C29 C 0.9639(3) 0.2943(3) 0.3150(5) 0.053(2) Uani 1 1 d . . . C30 C 0.8881(3) 0.2428(3) 0.2972(5) 0.052(2) Uani 1 1 d . . . C31 C 0.8442(4) 0.2353(3) 0.3409(6) 0.062(2) Uani 1 1 d . . . H31 H 0.8438 0.2251 0.4037 0.074 Uiso 1 1 calc R . . C32 C 0.8017(3) 0.2421(3) 0.2960(6) 0.056(2) Uani 1 1 d . . . O1M O 1.1411(3) 0.0734(3) 0.1981(4) 0.099(2) Uani 1 1 d DU . . H1OM H 1.1342 0.1078 0.1844 0.148 Uiso 0.75 1 d PR A 1 H1O H 1.1662 0.0558 0.1994 0.148 Uiso 0.25 1 d PR A 2 C1M C 1.1871(5) 0.0452(10) 0.2084(18) 0.222(11) Uani 0.75 1 d PDU B 1 H1M1 H 1.2090 0.0638 0.1651 0.334 Uiso 0.75 1 d PR B 1 H1M2 H 1.1849 0.0045 0.1941 0.334 Uiso 0.75 1 d PR B 1 H1M3 H 1.1995 0.0501 0.2707 0.334 Uiso 0.75 1 d PR B 1 C1M' C 1.1503(11) 0.1153(10) 0.1289(15) 0.053(8) Uani 0.25 1 d PDU B 2 H1M4 H 1.1838 0.1098 0.1092 0.079 Uiso 0.25 1 d PR B 2 H1M5 H 1.1473 0.1520 0.1605 0.079 Uiso 0.25 1 d PR B 2 H1M6 H 1.1290 0.1149 0.0754 0.079 Uiso 0.25 1 d PR B 2 C33 C 0.6573(4) 0.2041(7) 0.4087(10) 0.071(2) Uani 0.50 1 d PDU . -1 C34 C 0.6117(4) 0.1915(7) 0.4551(9) 0.076(2) Uani 0.50 1 d PDU . -1 C35 C 0.6165(5) 0.1558(7) 0.5323(10) 0.075(3) Uani 0.50 1 d PDU . -1 H35A H 0.5878 0.1427 0.5611 0.091 Uiso 0.50 1 calc PR . -1 C36 C 0.6594(5) 0.1391(7) 0.5680(9) 0.074(3) Uani 0.50 1 d PDU . -1 H36A H 0.6602 0.1184 0.6237 0.089 Uiso 0.50 1 calc PR . -1 C37 C 0.7022(4) 0.1521(7) 0.5236(9) 0.070(3) Uani 0.50 1 d PDU . -1 H37A H 0.7317 0.1374 0.5468 0.084 Uiso 0.50 1 calc PR . -1 C38 C 0.7028(4) 0.1870(7) 0.4438(9) 0.067(2) Uani 0.50 1 d PDU . -1 C39 C 0.7472(4) 0.1964(6) 0.4024(9) 0.061(3) Uani 0.50 1 d PDU . -1 H39A H 0.7745 0.1779 0.4284 0.074 Uiso 0.50 1 calc PR . -1 C40 C 0.5654(4) 0.2136(6) 0.4166(8) 0.079(3) Uani 0.50 1 d PDU . -1 C41 C 0.5200(5) 0.1935(7) 0.4725(12) 0.084(4) Uani 0.50 1 d PDU . -1 H41A H 0.5191 0.1517 0.4742 0.126 Uiso 0.50 1 calc PR . -1 H41B H 0.4906 0.2078 0.4430 0.126 Uiso 0.50 1 calc PR . -1 H41C H 0.5220 0.2084 0.5349 0.126 Uiso 0.50 1 calc PR . -1 C42 C 0.5639(7) 0.2789(5) 0.4130(14) 0.082(4) Uani 0.50 1 d PDU . -1 H42A H 0.5916 0.2930 0.3780 0.123 Uiso 0.50 1 calc PR . -1 H42B H 0.5651 0.2942 0.4752 0.123 Uiso 0.50 1 calc PR . -1 H42C H 0.5339 0.2912 0.3834 0.123 Uiso 0.50 1 calc PR . -1 C43 C 0.5577(6) 0.1897(8) 0.3170(10) 0.084(4) Uani 0.50 1 d PDU . -1 H43A H 0.5843 0.2025 0.2777 0.125 Uiso 0.50 1 calc PR . -1 H43B H 0.5270 0.2038 0.2927 0.125 Uiso 0.50 1 calc PR . -1 H43C H 0.5572 0.1479 0.3188 0.125 Uiso 0.50 1 calc PR . -1 C44 C 0.7487(6) 0.2763(8) 0.0761(9) 0.119(7) Uani 0.25 1 d PDU . -1 H44A H 0.7758 0.2701 0.0375 0.143 Uiso 0.25 1 calc PR . -1 C45 C 0.7035(6) 0.2927(7) 0.0324(9) 0.119(6) Uani 0.25 1 d PDU . -1 C46 C 0.7060(8) 0.3090(9) -0.0594(10) 0.119(6) Uani 0.25 1 d PDU . -1 H46A H 0.7364 0.3088 -0.0893 0.143 Uiso 0.25 1 calc PR . -1 C47 C 0.6656(9) 0.3253(10) -0.1074(11) 0.120(6) Uani 0.25 1 d PDU . -1 H47A H 0.6679 0.3363 -0.1698 0.143 Uiso 0.25 1 calc PR . -1 C48 C 0.6217(8) 0.3253(10) -0.0631(12) 0.120(6) Uani 0.25 1 d PDU . -1 H48A H 0.5939 0.3366 -0.0966 0.144 Uiso 0.25 1 calc PR . -1 C49 C 0.6159(6) 0.3098(9) 0.0278(13) 0.120(6) Uani 0.25 1 d PDU . -1 C50 C 0.6587(6) 0.2869(16) 0.0740(10) 0.119(6) Uani 0.25 1 d PDU . -1 C51 C 0.5674(6) 0.3075(10) 0.0746(15) 0.121(6) Uani 0.25 1 d PDU . -1 C52 C 0.5287(8) 0.3350(17) 0.015(2) 0.123(7) Uani 0.25 1 d PDU . -1 H52A H 0.5385 0.3739 -0.0004 0.185 Uiso 0.25 1 calc PR . -1 H52B H 0.4981 0.3361 0.0492 0.185 Uiso 0.25 1 calc PR . -1 H52C H 0.5245 0.3126 -0.0406 0.185 Uiso 0.25 1 calc PR . -1 C53 C 0.5505(12) 0.2445(12) 0.090(3) 0.121(7) Uani 0.25 1 d PDU . -1 H53A H 0.5542 0.2230 0.0329 0.182 Uiso 0.25 1 calc PR . -1 H53B H 0.5165 0.2442 0.1086 0.182 Uiso 0.25 1 calc PR . -1 H53C H 0.5703 0.2268 0.1378 0.182 Uiso 0.25 1 calc PR . -1 C54 C 0.5691(12) 0.3379(18) 0.1687(19) 0.120(7) Uani 0.25 1 d PDU . -1 H54A H 0.5725 0.3791 0.1594 0.180 Uiso 0.25 1 calc PR . -1 H54B H 0.5966 0.3237 0.2040 0.180 Uiso 0.25 1 calc PR . -1 H54C H 0.5391 0.3302 0.2021 0.180 Uiso 0.25 1 calc PR . -1 N3 N 0.7549(3) 0.2286(7) 0.3306(8) 0.061(3) Uani 0.50 1 d PDU . -1 N4 N 0.7551(5) 0.2694(18) 0.1632(10) 0.119(7) Uani 0.25 1 d PDU . -1 O3 O 0.6540(3) 0.2444(6) 0.3469(8) 0.070(3) Uani 0.50 1 d PDU . -1 O4 O 0.6536(4) 0.2739(16) 0.1602(8) 0.119(7) Uani 0.25 1 d PDU . -1 Zn2 Zn 0.70067(8) 0.27055(8) 0.2599(2) 0.0858(9) Uani 0.50 1 d PD . -1 C44' C 0.7592(8) 0.269(2) 0.0741(19) 0.150(7) Uani 0.25 1 d PDU . -2 H44' H 0.7869 0.2586 0.0395 0.180 Uiso 0.25 1 d PR . -2 C45' C 0.7152(8) 0.270(2) 0.0194(16) 0.150(7) Uani 0.25 1 d PDU . -2 C46' C 0.7211(10) 0.264(2) -0.0752(17) 0.151(7) Uani 0.25 1 d PDU . -2 H46' H 0.7516 0.2527 -0.0991 0.181 Uiso 0.25 1 calc PR . -2 C47' C 0.6832(11) 0.274(2) -0.1341(15) 0.151(7) Uani 0.25 1 d PDU . -2 H47' H 0.6879 0.2740 -0.1984 0.181 Uiso 0.25 1 calc PR . -2 C48' C 0.6384(10) 0.284(2) -0.0965(18) 0.151(7) Uani 0.25 1 d PDU . -2 H48' H 0.6132 0.2960 -0.1357 0.181 Uiso 0.25 1 calc PR . -2 C49' C 0.6279(7) 0.2763(18) -0.0043(17) 0.151(7) Uani 0.25 1 d PDU . -2 C50' C 0.6691(8) 0.267(2) 0.0565(16) 0.150(7) Uani 0.25 1 d PDU . -2 C51' C 0.5769(7) 0.2714(13) 0.0309(19) 0.151(7) Uani 0.25 1 d PDU . -2 C52' C 0.5411(9) 0.280(2) -0.047(2) 0.153(8) Uani 0.25 1 d PDU . -2 H52D H 0.5444 0.3191 -0.0707 0.230 Uiso 0.25 1 calc PR . -2 H52E H 0.5082 0.2747 -0.0238 0.230 Uiso 0.25 1 calc PR . -2 H52F H 0.5476 0.2527 -0.0955 0.230 Uiso 0.25 1 calc PR . -2 C53' C 0.5662(16) 0.2103(15) 0.069(3) 0.152(8) Uani 0.25 1 d PDU . -2 H53D H 0.5699 0.1822 0.0200 0.228 Uiso 0.25 1 calc PR . -2 H53E H 0.5331 0.2089 0.0926 0.228 Uiso 0.25 1 calc PR . -2 H53F H 0.5889 0.2015 0.1186 0.228 Uiso 0.25 1 calc PR . -2 C54' C 0.5672(13) 0.3155(19) 0.108(3) 0.152(8) Uani 0.25 1 d PDU . -2 H54D H 0.5730 0.3540 0.0843 0.228 Uiso 0.25 1 calc PR . -2 H54E H 0.5888 0.3080 0.1593 0.228 Uiso 0.25 1 calc PR . -2 H54F H 0.5336 0.3122 0.1280 0.228 Uiso 0.25 1 calc PR . -2 N4' N 0.7618(9) 0.2546(12) 0.1595(17) 0.048(10) Uani 0.25 1 d PDU . -2 O4' O 0.6608(9) 0.263(2) 0.1442(16) 0.128(17) Uani 0.25 1 d PDU . -2 O2M O 0.6961(6) 0.3623(7) 0.2880(11) 0.134(6) Uani 0.50 1 d PDU . -1 H2OM H 0.6873 0.3897 0.2325 0.201 Uiso 0.50 1 d PRD . -1 C2M C 0.6700(8) 0.3796(10) 0.3677(13) 0.126(8) Uani 0.50 1 d PDU . -1 H2M1 H 0.6378 0.3945 0.3539 0.188 Uiso 0.50 1 d PR . -1 H2M2 H 0.6886 0.4087 0.4006 0.188 Uiso 0.50 1 d PR . -1 H2M3 H 0.6671 0.3454 0.4058 0.188 Uiso 0.50 1 d PR . -1 O1S O 0.7179(7) 0.0613(9) 0.3055(13) 0.168(9) Uani 0.50 1 d PD . . H1S H 0.7440 0.0548 0.3329 0.253 Uiso 0.50 1 d PR . . C1S C 0.6768(9) 0.0422(14) 0.3560(18) 0.192(15) Uani 0.50 1 d PD . . H1S1 H 0.6705 0.0017 0.3440 0.288 Uiso 0.50 1 d PR . . H1S2 H 0.6480 0.0645 0.3412 0.288 Uiso 0.50 1 d PR . . H1S3 H 0.6849 0.0473 0.4207 0.288 Uiso 0.50 1 d PR . . O2S O 0.5931(10) 0.2500 0.7500 0.241(19) Uani 0.25 1 d PD C 2 H2S H 0.5830 0.2676 0.7962 0.362 Uiso 0.25 1 d PR C 2 C2S C 0.6446(10) 0.2500 0.7500 0.158(19) Uani 0.25 1 d PD C 2 H2S1 H 0.6564 0.2108 0.7565 0.236 Uiso 0.25 1 d PR C 2 H2S2 H 0.6564 0.2731 0.8012 0.236 Uiso 0.25 1 d PR C 2 H2S3 H 0.6564 0.2661 0.6924 0.236 Uiso 0.25 1 d PR C 2 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 0.090(7) 0.050(5) 0.046(6) 0.006(5) 0.007(6) -0.004(5) C2 0.093(7) 0.050(6) 0.060(7) -0.007(5) 0.000(6) -0.011(5) C3 0.124(9) 0.055(6) 0.056(7) -0.022(5) 0.020(6) -0.022(6) C4 0.130(9) 0.051(6) 0.049(6) 0.004(5) -0.002(6) 0.000(6) C5 0.115(8) 0.041(5) 0.054(6) 0.011(5) 0.002(6) -0.005(5) C6 0.085(7) 0.054(6) 0.054(6) 0.017(5) 0.001(6) -0.002(5) C7 0.087(7) 0.039(5) 0.049(6) 0.004(5) 0.009(5) -0.003(4) C8 0.092(8) 0.069(7) 0.070(7) -0.017(6) -0.001(6) 0.003(6) C9 0.111(8) 0.064(6) 0.069(7) 0.008(5) -0.001(6) 0.015(6) C10 0.096(8) 0.100(8) 0.138(10) -0.038(8) 0.004(8) -0.015(7) C11 0.135(10) 0.074(7) 0.094(8) -0.002(6) 0.018(7) 0.010(7) C17 0.124(8) 0.042(5) 0.042(6) 0.005(5) 0.000(6) 0.008(5) C18 0.103(7) 0.047(5) 0.037(5) 0.011(5) 0.001(5) 0.007(5) C19 0.139(9) 0.059(7) 0.060(7) 0.009(5) -0.004(6) 0.005(6) C20 0.128(9) 0.072(7) 0.050(6) 0.030(6) -0.002(6) 0.021(6) C21 0.101(8) 0.074(7) 0.053(7) 0.032(6) -0.011(6) -0.018(6) C22 0.082(7) 0.047(6) 0.068(7) 0.010(5) -0.012(6) -0.014(5) C23 0.087(7) 0.056(6) 0.052(7) 0.017(5) -0.012(5) -0.012(5) C24 0.104(8) 0.063(7) 0.077(7) 0.014(6) -0.004(7) -0.001(6) C25 0.110(8) 0.066(7) 0.100(8) 0.001(6) -0.009(7) 0.004(6) C26 0.146(10) 0.072(7) 0.084(8) 0.034(6) -0.027(7) 0.023(7) C27 0.137(9) 0.072(7) 0.082(8) 0.000(6) -0.044(7) 0.008(6) N1 0.094(6) 0.047(4) 0.045(5) 0.003(4) 0.004(4) 0.002(4) N2 0.089(5) 0.040(4) 0.050(5) 0.014(4) -0.007(4) 0.008(4) O1 0.119(5) 0.072(4) 0.055(4) 0.000(3) -0.005(4) 0.015(4) O2 0.127(6) 0.051(4) 0.055(4) 0.009(3) -0.003(4) 0.014(3) Zn1 0.1085(10) 0.0535(7) 0.0476(8) 0.0070(5) -0.0058(6) 0.0074(6) C12 0.077(6) 0.044(5) 0.047(6) 0.002(5) 0.003(5) -0.007(5) C13 0.096(7) 0.045(5) 0.033(5) 0.010(4) 0.003(5) 0.008(5) C14 0.081(6) 0.047(5) 0.044(5) 0.006(5) -0.003(5) 0.000(5) C15 0.102(7) 0.049(6) 0.046(6) 0.026(5) -0.002(5) -0.002(5) C16 0.089(7) 0.035(5) 0.046(6) 0.004(5) 0.004(5) 0.001(5) C28 0.083(7) 0.050(5) 0.032(5) 0.012(4) 0.004(5) -0.002(5) C29 0.077(6) 0.042(5) 0.042(5) 0.024(4) 0.003(5) -0.002(4) C30 0.065(6) 0.045(5) 0.047(5) 0.019(4) -0.003(5) -0.001(4) C31 0.092(8) 0.049(5) 0.044(5) 0.017(4) 0.010(6) 0.004(5) C32 0.050(6) 0.061(6) 0.058(6) 0.022(5) 0.005(5) 0.009(4) O1M 0.106(4) 0.092(4) 0.099(4) -0.007(3) -0.008(3) -0.004(3) C1M 0.222(12) 0.221(12) 0.224(12) -0.004(4) 0.000(4) -0.001(4) C1M' 0.053(10) 0.055(10) 0.051(10) 0.004(5) 0.002(5) -0.009(5) C33 0.072(3) 0.073(4) 0.068(4) 0.005(3) 0.004(3) 0.000(3) C34 0.074(3) 0.079(4) 0.074(3) 0.004(3) 0.004(3) -0.001(3) C35 0.074(4) 0.079(4) 0.073(4) 0.005(3) 0.005(3) -0.005(3) C36 0.074(4) 0.077(4) 0.070(4) 0.006(3) 0.005(3) -0.005(3) C37 0.072(4) 0.073(4) 0.066(4) 0.006(3) 0.003(3) -0.003(3) C38 0.069(3) 0.069(4) 0.064(3) 0.004(3) 0.004(3) -0.003(3) C39 0.067(4) 0.060(4) 0.058(4) 0.004(3) 0.000(3) -0.003(3) C40 0.076(3) 0.082(4) 0.079(4) 0.002(3) 0.003(3) 0.001(3) C41 0.078(4) 0.086(6) 0.087(5) 0.001(5) 0.006(4) 0.002(4) C42 0.081(6) 0.082(4) 0.083(6) 0.001(4) 0.000(5) 0.001(4) C43 0.080(6) 0.088(6) 0.083(4) -0.003(4) -0.001(4) -0.002(5) C44 0.119(7) 0.120(8) 0.118(7) 0.002(4) -0.001(3) 0.000(4) C45 0.119(7) 0.120(7) 0.119(7) 0.002(3) -0.001(3) 0.001(3) C46 0.119(7) 0.120(7) 0.119(7) 0.002(4) -0.001(3) 0.001(4) C47 0.120(7) 0.120(7) 0.119(7) 0.001(4) -0.002(3) 0.000(4) C48 0.120(7) 0.120(7) 0.120(7) 0.000(4) -0.002(3) 0.001(4) C49 0.120(7) 0.121(7) 0.120(7) 0.001(3) -0.001(3) 0.000(3) C50 0.120(7) 0.120(7) 0.119(7) 0.001(3) -0.001(3) -0.001(3) C51 0.120(7) 0.122(7) 0.121(7) 0.001(3) -0.001(3) 0.000(3) C52 0.122(8) 0.124(8) 0.124(8) 0.003(5) -0.002(5) 0.000(5) C53 0.120(8) 0.121(7) 0.122(9) 0.000(4) 0.000(5) 0.000(4) C54 0.119(8) 0.119(8) 0.121(8) 0.001(5) 0.001(4) 0.001(5) N3 0.068(5) 0.059(5) 0.057(5) 0.005(4) 0.000(4) -0.003(4) N4 0.120(8) 0.119(8) 0.118(8) 0.002(4) -0.001(4) 0.000(4) O3 0.069(4) 0.070(5) 0.072(4) 0.003(3) 0.005(3) 0.002(3) O4 0.118(8) 0.119(8) 0.119(7) -0.001(4) -0.001(4) -0.001(4) Zn2 0.0947(17) 0.0631(19) 0.100(2) 0.006(2) -0.0159(16) -0.0048(11) C44' 0.150(8) 0.151(8) 0.150(8) 0.001(4) -0.001(4) -0.001(4) C45' 0.150(7) 0.149(8) 0.150(8) 0.001(3) -0.001(3) 0.000(3) C46' 0.151(8) 0.151(8) 0.150(8) 0.001(4) -0.001(3) 0.000(4) C47' 0.151(8) 0.151(8) 0.150(8) 0.001(4) -0.001(3) 0.000(4) C48' 0.151(8) 0.151(8) 0.151(8) 0.001(4) -0.001(3) 0.000(4) C49' 0.151(7) 0.150(8) 0.151(7) 0.001(3) -0.001(3) 0.000(3) C50' 0.150(7) 0.149(8) 0.150(8) 0.001(4) -0.001(3) 0.000(4) C51' 0.151(7) 0.151(8) 0.152(8) 0.000(3) -0.001(3) 0.001(4) C52' 0.153(8) 0.153(9) 0.153(8) 0.000(4) -0.003(5) 0.000(5) C53' 0.152(9) 0.152(8) 0.152(9) 0.000(4) -0.001(5) -0.001(5) C54' 0.152(9) 0.153(9) 0.152(8) -0.001(5) -0.002(4) 0.000(5) N4' 0.052(11) 0.047(11) 0.045(10) 0.008(5) 0.000(5) 0.000(5) O4' 0.125(17) 0.127(17) 0.133(17) -0.001(6) -0.005(6) -0.001(6) O2M 0.132(7) 0.138(7) 0.133(7) -0.007(5) -0.012(5) -0.013(5) C2M 0.124(9) 0.127(9) 0.126(9) -0.011(5) 0.001(5) -0.005(5) O1S 0.111(14) 0.21(2) 0.183(18) -0.048(15) 0.083(14) -0.047(14) C1S 0.17(3) 0.18(3) 0.23(4) -0.06(3) -0.07(3) -0.06(3) O2S 0.14(3) 0.25(4) 0.33(5) -0.09(4) 0.000 0.000 C2S 0.04(2) 0.13(3) 0.30(6) -0.05(3) 0.000 0.000 _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 O1 1.312(9) . ? C1 C6 1.419(11) . ? C1 C2 1.461(10) . ? C2 C3 1.411(11) . ? C2 C8 1.495(11) . ? C3 C4 1.352(11) . ? C4 C5 1.381(11) . ? C5 C6 1.426(10) . ? C6 C7 1.387(10) . ? C7 N1 1.306(9) . ? C8 C10 1.530(11) . ? C8 C9 1.573(10) . ? C8 C11 1.573(10) . ? C17 N2 1.296(9) . ? C17 C18 1.458(11) . ? C18 C23 1.388(12) . ? C18 C19 1.397(11) . ? C19 C20 1.375(11) . ? C20 C21 1.376(12) . ? C21 C22 1.386(11) . ? C22 C23 1.462(11) . ? C22 C24 1.508(6) . ? C23 O2 1.310(9) . ? C24 C25 1.520(10) . ? C24 C27 1.550(11) . ? C24 C26 1.566(10) . ? N1 C12 1.389(10) . ? N1 Zn1 2.074(6) . ? N2 C16 1.404(10) . ? N2 Zn1 2.064(7) . ? O1 Zn1 1.926(6) . ? O2 Zn1 1.956(6) . ? Zn1 O1M 2.089(7) . ? C12 C16 1.408(11) . ? C12 C13 1.419(11) . ? C13 C29 1.381(10) 4 ? C14 C15 1.391(11) . ? C14 C29 1.432(10) 4 ? C14 C28 1.512(11) . ? C15 C16 1.362(11) . ? C28 C30 1.508(11) . ? C28 C29 1.532(11) . ? C29 C13 1.382(10) 4 ? C29 C14 1.432(10) 4 ? C30 C31 1.384(11) . ? C30 C30 1.421(15) 4 ? C31 C32 1.358(11) . ? C32 N4' 1.28(2) 4 ? C32 C32 1.397(16) 4 ? C32 N3 1.426(13) . ? C32 N4 1.447(15) 4 ? O1M C1M' 1.433(6) . ? O1M C1M 1.444(6) . ? C33 O3 1.310(10) . ? C33 C38 1.418(11) . ? C33 C34 1.465(11) . ? C34 C35 1.411(11) . ? C34 C40 1.493(12) . ? C35 C36 1.357(12) . ? C36 C37 1.383(11) . ? C37 C38 1.427(11) . ? C38 C39 1.390(11) . ? C39 N3 1.310(10) . ? C40 C42 1.532(12) . ? C40 C41 1.572(11) . ? C40 C43 1.576(11) . ? C44 N4 1.298(10) . ? C44 C45 1.459(12) . ? C45 C50 1.388(12) . ? C45 C46 1.398(12) . ? C46 C47 1.375(12) . ? C47 C48 1.377(13) . ? C48 C49 1.388(12) . ? C49 C50 1.466(12) . ? C49 C51 1.508(5) . ? C50 O4 1.305(11) . ? C51 C52 1.522(11) . ? C51 C54 1.550(11) . ? C51 C53 1.566(10) . ? N3 Zn2 2.073(8) . ? N4 C32 1.447(15) 4 ? N4 Zn2 2.067(8) . ? O3 Zn2 1.915(7) . ? O4 Zn2 1.958(8) . ? Zn2 O2M 2.193(17) . ? C44' N4' 1.297(11) . ? C44' C45' 1.458(12) . ? C45' C50' 1.389(12) . ? C45' C46' 1.400(12) . ? C46' C47' 1.377(13) . ? C47' C48' 1.377(13) . ? C48' C49' 1.390(12) . ? C49' C50' 1.464(12) . ? C49' C51' 1.508(7) . ? C50' O4' 1.307(11) . ? C51' C52' 1.523(11) . ? C51' C54' 1.550(12) . ? C51' C53' 1.566(11) . ? N4' C32 1.28(2) 4 ? O2M C2M 1.431(5) . ? O1S C1S 1.430(6) . ? O2S C2S 1.425(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 122.3(7) . . ? O1 C1 C2 117.2(8) . . ? C6 C1 C2 120.5(8) . . ? C3 C2 C1 115.2(8) . . ? C3 C2 C8 123.9(7) . . ? C1 C2 C8 120.9(7) . . ? C4 C3 C2 125.3(8) . . ? C3 C4 C5 119.1(8) . . ? C4 C5 C6 121.5(8) . . ? C7 C6 C1 125.4(8) . . ? C7 C6 C5 116.3(8) . . ? C1 C6 C5 118.3(8) . . ? N1 C7 C6 126.8(8) . . ? C2 C8 C10 111.8(7) . . ? C2 C8 C9 111.4(7) . . ? C10 C8 C9 108.5(7) . . ? C2 C8 C11 110.4(7) . . ? C10 C8 C11 108.3(7) . . ? C9 C8 C11 106.2(7) . . ? N2 C17 C18 125.5(8) . . ? C23 C18 C19 120.2(8) . . ? C23 C18 C17 123.7(8) . . ? C19 C18 C17 115.9(8) . . ? C20 C19 C18 121.9(9) . . ? C19 C20 C21 118.0(9) . . ? C20 C21 C22 124.0(9) . . ? C21 C22 C23 116.9(8) . . ? C21 C22 C24 123.3(8) . . ? C23 C22 C24 119.7(7) . . ? O2 C23 C18 123.6(8) . . ? O2 C23 C22 117.5(8) . . ? C18 C23 C22 118.9(8) . . ? C22 C24 C25 110.7(7) . . ? C22 C24 C27 110.8(8) . . ? C25 C24 C27 110.0(8) . . ? C22 C24 C26 111.3(7) . . ? C25 C24 C26 105.9(8) . . ? C27 C24 C26 108.0(7) . . ? C7 N1 C12 121.6(7) . . ? C7 N1 Zn1 123.6(6) . . ? C12 N1 Zn1 114.3(5) . . ? C17 N2 C16 121.3(7) . . ? C17 N2 Zn1 124.8(6) . . ? C16 N2 Zn1 113.8(5) . . ? C1 O1 Zn1 131.3(6) . . ? C23 O2 Zn1 129.9(5) . . ? O1 Zn1 O2 96.1(2) . . ? O1 Zn1 N2 162.8(3) . . ? O2 Zn1 N2 88.7(2) . . ? O1 Zn1 N1 89.9(3) . . ? O2 Zn1 N1 152.7(3) . . ? N2 Zn1 N1 78.6(3) . . ? O1 Zn1 O1M 99.4(3) . . ? O2 Zn1 O1M 101.9(3) . . ? N2 Zn1 O1M 95.7(3) . . ? N1 Zn1 O1M 103.4(3) . . ? N1 C12 C16 115.3(7) . . ? N1 C12 C13 123.7(7) . . ? C16 C12 C13 120.9(8) . . ? C29 C13 C12 118.5(7) 4 . ? C15 C14 C29 118.2(8) . 4 ? C15 C14 C28 128.5(8) . . ? C29 C14 C28 113.2(7) 4 . ? C16 C15 C14 122.6(8) . . ? C15 C16 N2 125.1(8) . . ? C15 C16 C12 118.8(8) . . ? N2 C16 C12 116.1(8) . . ? C30 C28 C14 104.9(7) . . ? C30 C28 C29 106.5(6) . . ? C14 C28 C29 106.0(6) . . ? C13 C29 C14 120.8(7) 4 4 ? C13 C29 C28 126.9(7) 4 . ? C14 C29 C28 112.4(7) 4 . ? C31 C30 C30 118.6(5) . 4 ? C31 C30 C28 128.2(7) . . ? C30 C30 C28 113.2(4) 4 . ? C32 C31 C30 121.5(8) . . ? N4' C32 C31 120.6(14) 4 . ? N4' C32 C32 118.2(12) 4 4 ? C31 C32 C32 119.8(5) . 4 ? N4' C32 N3 18.6(16) 4 . ? C31 C32 N3 126.1(8) . . ? C32 C32 N3 113.7(6) 4 . ? N4' C32 N4 15(2) 4 4 ? C31 C32 N4 123.5(8) . 4 ? C32 C32 N4 116.5(5) 4 4 ? N3 C32 N4 4.0(16) . 4 ? C1M' O1M C1M 103.3(17) . . ? C1M' O1M Zn1 113.6(13) . . ? C1M O1M Zn1 120.2(12) . . ? O3 C33 C38 121.1(9) . . ? O3 C33 C34 113.9(9) . . ? C38 C33 C34 122.7(9) . . ? C35 C34 C33 114.2(9) . . ? C35 C34 C40 126.0(8) . . ? C33 C34 C40 119.7(8) . . ? C36 C35 C34 124.1(9) . . ? C35 C36 C37 120.4(10) . . ? C36 C37 C38 121.3(9) . . ? C39 C38 C33 125.7(9) . . ? C39 C38 C37 117.3(9) . . ? C33 C38 C37 116.7(9) . . ? N3 C39 C38 125.7(9) . . ? C34 C40 C42 112.7(9) . . ? C34 C40 C41 112.7(8) . . ? C42 C40 C41 107.1(9) . . ? C34 C40 C43 109.9(8) . . ? C42 C40 C43 108.6(9) . . ? C41 C40 C43 105.4(8) . . ? N4 C44 C45 125.4(10) . . ? C50 C45 C46 119.5(10) . . ? C50 C45 C44 123.4(9) . . ? C46 C45 C44 116.7(10) . . ? C47 C46 C45 121.8(11) . . ? C46 C47 C48 118.5(11) . . ? C47 C48 C49 123.6(11) . . ? C48 C49 C50 116.4(9) . . ? C48 C49 C51 123.3(10) . . ? C50 C49 C51 119.7(9) . . ? O4 C50 C45 122.8(10) . . ? O4 C50 C49 116.4(11) . . ? C45 C50 C49 118.9(10) . . ? C49 C51 C52 110.7(9) . . ? C49 C51 C54 111.2(10) . . ? C52 C51 C54 109.3(10) . . ? C49 C51 C53 111.4(9) . . ? C52 C51 C53 105.6(10) . . ? C54 C51 C53 108.4(10) . . ? C39 N3 C32 124.1(8) . . ? C39 N3 Zn2 123.8(7) . . ? C32 N3 Zn2 112.0(6) . . ? C44 N4 C32 123.3(10) . 4 ? C44 N4 Zn2 124.9(8) . . ? C32 N4 Zn2 111.8(8) 4 . ? C33 O3 Zn2 129.9(7) . . ? C50 O4 Zn2 131.2(9) . . ? O3 Zn2 O4 93.4(4) . . ? O3 Zn2 N4 160.5(12) . . ? O4 Zn2 N4 88.6(5) . . ? O3 Zn2 N3 90.3(4) . . ? O4 Zn2 N3 150.9(11) . . ? N4 Zn2 N3 78.9(5) . . ? O3 Zn2 O2M 98.7(7) . . ? O4 Zn2 O2M 93.5(12) . . ? N4 Zn2 O2M 100.5(13) . . ? N3 Zn2 O2M 114.4(6) . . ? N4' C44' C45' 125.2(12) . . ? C50' C45' C46' 119.2(11) . . ? C50' C45' C44' 123.6(10) . . ? C46' C45' C44' 116.4(11) . . ? C47' C46' C45' 120.9(12) . . ? C46' C47' C48' 117.7(11) . . ? C47' C48' C49' 123.7(12) . . ? C48' C49' C50' 116.5(10) . . ? C48' C49' C51' 122.5(10) . . ? C50' C49' C51' 120.6(10) . . ? O4' C50' C45' 123.3(11) . . ? O4' C50' C49' 118.0(12) . . ? C45' C50' C49' 118.0(10) . . ? C49' C51' C52' 110.2(9) . . ? C49' C51' C54' 111.1(10) . . ? C52' C51' C54' 109.6(10) . . ? C49' C51' C53' 111.7(10) . . ? C52' C51' C53' 105.5(10) . . ? C54' C51' C53' 108.6(10) . . ? C32 N4' C44' 121.3(19) 4 . ? C2M O2M Zn2 117.4(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 177.7(8) . . . . ? C6 C1 C2 C3 -1.7(12) . . . . ? O1 C1 C2 C8 -5.0(12) . . . . ? C6 C1 C2 C8 175.5(8) . . . . ? C1 C2 C3 C4 -0.6(13) . . . . ? C8 C2 C3 C4 -177.7(9) . . . . ? C2 C3 C4 C5 1.0(15) . . . . ? C3 C4 C5 C6 1.0(14) . . . . ? O1 C1 C6 C7 2.4(14) . . . . ? C2 C1 C6 C7 -178.2(8) . . . . ? O1 C1 C6 C5 -175.9(8) . . . . ? C2 C1 C6 C5 3.5(12) . . . . ? C4 C5 C6 C7 178.4(8) . . . . ? C4 C5 C6 C1 -3.1(13) . . . . ? C1 C6 C7 N1 6.1(14) . . . . ? C5 C6 C7 N1 -175.6(8) . . . . ? C3 C2 C8 C10 119.1(9) . . . . ? C1 C2 C8 C10 -57.8(10) . . . . ? C3 C2 C8 C9 -119.3(9) . . . . ? C1 C2 C8 C9 63.8(10) . . . . ? C3 C2 C8 C11 -1.5(11) . . . . ? C1 C2 C8 C11 -178.5(7) . . . . ? N2 C17 C18 C23 -10.3(15) . . . . ? N2 C17 C18 C19 174.5(9) . . . . ? C23 C18 C19 C20 0.5(15) . . . . ? C17 C18 C19 C20 175.8(9) . . . . ? C18 C19 C20 C21 -3.0(16) . . . . ? C19 C20 C21 C22 3.9(15) . . . . ? C20 C21 C22 C23 -2.3(14) . . . . ? C20 C21 C22 C24 -177.4(9) . . . . ? C19 C18 C23 O2 -177.3(9) . . . . ? C17 C18 C23 O2 7.8(14) . . . . ? C19 C18 C23 C22 1.2(13) . . . . ? C17 C18 C23 C22 -173.8(8) . . . . ? C21 C22 C23 O2 178.2(8) . . . . ? C24 C22 C23 O2 -6.4(12) . . . . ? C21 C22 C23 C18 -0.4(12) . . . . ? C24 C22 C23 C18 175.0(8) . . . . ? C21 C22 C24 C25 -119.9(9) . . . . ? C23 C22 C24 C25 65.1(10) . . . . ? C21 C22 C24 C27 117.9(9) . . . . ? C23 C22 C24 C27 -57.2(10) . . . . ? C21 C22 C24 C26 -2.3(12) . . . . ? C23 C22 C24 C26 -177.4(8) . . . . ? C6 C7 N1 C12 177.4(8) . . . . ? C6 C7 N1 Zn1 -11.3(12) . . . . ? C18 C17 N2 C16 177.3(8) . . . . ? C18 C17 N2 Zn1 -5.7(12) . . . . ? C6 C1 O1 Zn1 -4.0(13) . . . . ? C2 C1 O1 Zn1 176.5(6) . . . . ? C18 C23 O2 Zn1 11.8(13) . . . . ? C22 C23 O2 Zn1 -166.7(6) . . . . ? C1 O1 Zn1 O2 152.9(8) . . . . ? C1 O1 Zn1 N2 47.4(13) . . . . ? C1 O1 Zn1 N1 -0.4(8) . . . . ? C1 O1 Zn1 O1M -103.9(8) . . . . ? C23 O2 Zn1 O1 176.5(7) . . . . ? C23 O2 Zn1 N2 -20.1(8) . . . . ? C23 O2 Zn1 N1 -81.7(9) . . . . ? C23 O2 Zn1 O1M 75.5(8) . . . . ? C17 N2 Zn1 O1 123.0(9) . . . . ? C16 N2 Zn1 O1 -59.7(11) . . . . ? C17 N2 Zn1 O2 16.4(7) . . . . ? C16 N2 Zn1 O2 -166.4(6) . . . . ? C17 N2 Zn1 N1 172.0(7) . . . . ? C16 N2 Zn1 N1 -10.7(5) . . . . ? C17 N2 Zn1 O1M -85.4(7) . . . . ? C16 N2 Zn1 O1M 91.8(6) . . . . ? C7 N1 Zn1 O1 7.6(7) . . . . ? C12 N1 Zn1 O1 179.4(6) . . . . ? C7 N1 Zn1 O2 -95.6(8) . . . . ? C12 N1 Zn1 O2 76.2(8) . . . . ? C7 N1 Zn1 N2 -159.5(7) . . . . ? C12 N1 Zn1 N2 12.3(5) . . . . ? C7 N1 Zn1 O1M 107.3(7) . . . . ? C12 N1 Zn1 O1M -80.9(6) . . . . ? C7 N1 C12 C16 160.0(7) . . . . ? Zn1 N1 C12 C16 -12.0(9) . . . . ? C7 N1 C12 C13 -22.5(12) . . . . ? Zn1 N1 C12 C13 165.5(6) . . . . ? N1 C12 C13 C29 -179.7(7) . . . 4 ? C16 C12 C13 C29 -2.4(12) . . . 4 ? C29 C14 C15 C16 1.4(13) 4 . . . ? C28 C14 C15 C16 -173.9(8) . . . . ? C14 C15 C16 N2 175.3(8) . . . . ? C14 C15 C16 C12 -4.8(13) . . . . ? C17 N2 C16 C15 5.0(13) . . . . ? Zn1 N2 C16 C15 -172.3(7) . . . . ? C17 N2 C16 C12 -174.9(8) . . . . ? Zn1 N2 C16 C12 7.8(9) . . . . ? N1 C12 C16 C15 -177.1(8) . . . . ? C13 C12 C16 C15 5.3(12) . . . . ? N1 C12 C16 N2 2.8(11) . . . . ? C13 C12 C16 N2 -174.8(7) . . . . ? C15 C14 C28 C30 -127.2(9) . . . . ? C29 C14 C28 C30 57.4(8) 4 . . . ? C15 C14 C28 C29 120.4(9) . . . . ? C29 C14 C28 C29 -55.1(8) 4 . . . ? C30 C28 C29 C13 126.6(9) . . . 4 ? C14 C28 C29 C13 -122.0(9) . . . 4 ? C30 C28 C29 C14 -54.2(9) . . . 4 ? C14 C28 C29 C14 57.2(8) . . . 4 ? C14 C28 C30 C31 122.1(9) . . . . ? C29 C28 C30 C31 -125.8(8) . . . . ? C14 C28 C30 C30 -58.3(10) . . . 4 ? C29 C28 C30 C30 53.8(10) . . . 4 ? C30 C30 C31 C32 -0.9(14) 4 . . . ? C28 C30 C31 C32 178.6(8) . . . . ? C30 C31 C32 N4' -167.1(17) . . . 4 ? C30 C31 C32 C32 -1.0(15) . . . 4 ? C30 C31 C32 N3 171.6(11) . . . . ? C30 C31 C32 N4 175(2) . . . 4 ? O1 Zn1 O1M C1M' 62.7(14) . . . . ? O2 Zn1 O1M C1M' 161.1(14) . . . . ? N2 Zn1 O1M C1M' -109.1(14) . . . . ? N1 Zn1 O1M C1M' -29.5(14) . . . . ? O1 Zn1 O1M C1M -60.3(13) . . . . ? O2 Zn1 O1M C1M 38.0(13) . . . . ? N2 Zn1 O1M C1M 127.9(13) . . . . ? N1 Zn1 O1M C1M -152.5(13) . . . . ? O3 C33 C34 C35 -169.2(16) . . . . ? C38 C33 C34 C35 -6(3) . . . . ? O3 C33 C34 C40 14(2) . . . . ? C38 C33 C34 C40 176.7(15) . . . . ? C33 C34 C35 C36 7(3) . . . . ? C40 C34 C35 C36 -176.3(16) . . . . ? C34 C35 C36 C37 -7(3) . . . . ? C35 C36 C37 C38 5(3) . . . . ? O3 C33 C38 C39 -20(3) . . . . ? C34 C33 C38 C39 178.4(17) . . . . ? O3 C33 C38 C37 167.0(17) . . . . ? C34 C33 C38 C37 5(3) . . . . ? C36 C37 C38 C39 -178.2(16) . . . . ? C36 C37 C38 C33 -4(3) . . . . ? C33 C38 C39 N3 9(3) . . . . ? C37 C38 C39 N3 -177.8(17) . . . . ? C35 C34 C40 C42 122.0(18) . . . . ? C33 C34 C40 C42 -61.4(16) . . . . ? C35 C34 C40 C41 1(2) . . . . ? C33 C34 C40 C41 177.2(14) . . . . ? C35 C34 C40 C43 -116.7(17) . . . . ? C33 C34 C40 C43 60.0(17) . . . . ? N4 C44 C45 C50 -20(3) . . . . ? N4 C44 C45 C46 168(2) . . . . ? C50 C45 C46 C47 6.9(18) . . . . ? C44 C45 C46 C47 180.00(15) . . . . ? C45 C46 C47 C48 0.0(3) . . . . ? C46 C47 C48 C49 0.0(5) . . . . ? C47 C48 C49 C50 -6.4(17) . . . . ? C47 C48 C49 C51 -177.2(15) . . . . ? C46 C45 C50 O4 -177(2) . . . . ? C44 C45 C50 O4 10(4) . . . . ? C46 C45 C50 C49 -13(3) . . . . ? C44 C45 C50 C49 174.1(15) . . . . ? C48 C49 C50 O4 178(2) . . . . ? C51 C49 C50 O4 -11(4) . . . . ? C48 C49 C50 C45 13(3) . . . . ? C51 C49 C50 C45 -176(2) . . . . ? C48 C49 C51 C52 -10.9(18) . . . . ? C50 C49 C51 C52 179(2) . . . . ? C48 C49 C51 C54 -132.6(16) . . . . ? C50 C49 C51 C54 57(3) . . . . ? C48 C49 C51 C53 106.3(16) . . . . ? C50 C49 C51 C53 -64(3) . . . . ? C38 C39 N3 C32 173.0(15) . . . . ? C38 C39 N3 Zn2 -2(3) . . . . ? N4' C32 N3 C39 -94(4) 4 . . . ? C31 C32 N3 C39 -16(2) . . . . ? C32 C32 N3 C39 157.4(16) 4 . . . ? N4 C32 N3 C39 -66(22) 4 . . . ? N4' C32 N3 Zn2 82(4) 4 . . . ? C31 C32 N3 Zn2 160.3(8) . . . . ? C32 C32 N3 Zn2 -26.8(16) 4 . . . ? N4 C32 N3 Zn2 110(23) 4 . . . ? C45 C44 N4 C32 -174(2) . . . 4 ? C45 C44 N4 Zn2 8(4) . . . . ? C38 C33 O3 Zn2 24(3) . . . . ? C34 C33 O3 Zn2 -172.6(12) . . . . ? C45 C50 O4 Zn2 11(5) . . . . ? C49 C50 O4 Zn2 -154(3) . . . . ? C33 O3 Zn2 O4 136(2) . . . . ? C33 O3 Zn2 N4 41(3) . . . . ? C33 O3 Zn2 N3 -15.0(18) . . . . ? C33 O3 Zn2 O2M -129.8(17) . . . . ? C50 O4 Zn2 O3 -177(3) . . . . ? C50 O4 Zn2 N4 -17(3) . . . . ? C50 O4 Zn2 N3 -81(4) . . . . ? C50 O4 Zn2 O2M 84(3) . . . . ? C44 N4 Zn2 O3 103(2) . . . . ? C32 N4 Zn2 O3 -75(4) 4 . . . ? C44 N4 Zn2 O4 7(3) . . . . ? C32 N4 Zn2 O4 -171(3) 4 . . . ? C44 N4 Zn2 N3 160(3) . . . . ? C32 N4 Zn2 N3 -18(2) 4 . . . ? C44 N4 Zn2 O2M -86(3) . . . . ? C32 N4 Zn2 O2M 96(2) 4 . . . ? C39 N3 Zn2 O3 3.7(17) . . . . ? C32 N3 Zn2 O3 -172.1(11) . . . . ? C39 N3 Zn2 O4 -93.8(19) . . . . ? C32 N3 Zn2 O4 90.4(16) . . . . ? C39 N3 Zn2 N4 -160.0(17) . . . . ? C32 N3 Zn2 N4 24.2(18) . . . . ? C39 N3 Zn2 O2M 103.4(16) . . . . ? C32 N3 Zn2 O2M -72.4(12) . . . . ? N4' C44' C45' C50' 14(7) . . . . ? N4' C44' C45' C46' -155(5) . . . . ? C50' C45' C46' C47' 22(6) . . . . ? C44' C45' C46' C47' -168(4) . . . . ? C45' C46' C47' C48' -7(7) . . . . ? C46' C47' C48' C49' -9(7) . . . . ? C47' C48' C49' C50' 10(6) . . . . ? C47' C48' C49' C51' -163(4) . . . . ? C46' C45' C50' O4' 170(5) . . . . ? C44' C45' C50' O4' 0(7) . . . . ? C46' C45' C50' C49' -20(5) . . . . ? C44' C45' C50' C49' 171(4) . . . . ? C48' C49' C50' O4' 175(5) . . . . ? C51' C49' C50' O4' -12(6) . . . . ? C48' C49' C50' C45' 5(6) . . . . ? C51' C49' C50' C45' 178(3) . . . . ? C48' C49' C51' C52' -4(4) . . . . ? C50' C49' C51' C52' -177(4) . . . . ? C48' C49' C51' C54' -126(4) . . . . ? C50' C49' C51' C54' 61(4) . . . . ? C48' C49' C51' C53' 113(4) . . . . ? C50' C49' C51' C53' -60(4) . . . . ? C45' C44' N4' C32 -177(3) . . . 4 ? O3 Zn2 O2M C2M 11.2(14) . . . . ? O4 Zn2 O2M C2M 105.2(14) . . . . ? N4 Zn2 O2M C2M -165.6(14) . . . . ? N3 Zn2 O2M C2M -83.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.088 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.115 data_mo_da811_c2c _database_code_depnum_ccdc_archive 'CCDC 910863' #TrackingRef 'mo_DA811_C2cX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.80 H49.60 Cl0.60 N5.80 O4 Zn2' _chemical_formula_weight 1161.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.9324(18) _cell_length_b 11.9002(9) _cell_length_c 21.784(2) _cell_angle_alpha 90.00 _cell_angle_beta 124.409(2) _cell_angle_gamma 90.00 _cell_volume 5332.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9655 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 29.33 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396.8 _exptl_absorpt_coefficient_mu 0.989 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9076 _exptl_absorpt_correction_T_max 0.9615 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 52545 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 29.40 _reflns_number_total 7323 _reflns_number_gt 6309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0477P)^2^+8.5242P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7323 _refine_ls_number_parameters 398 _refine_ls_number_restraints 327 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.070789(8) 0.283067(15) 0.318102(10) 0.01484(6) Uani 1 1 d . . . N1 N 0.06585(6) 0.45273(12) 0.33903(8) 0.0169(3) Uani 1 1 d U . . N2 N 0.16372(7) 0.34114(12) 0.35714(8) 0.0168(3) Uani 1 1 d U . . O1 O -0.02364(5) 0.27495(9) 0.29392(6) 0.0158(2) Uani 1 1 d U . . O2 O 0.10673(6) 0.14773(10) 0.37572(7) 0.0191(2) Uani 1 1 d U . . C1 C -0.04630(7) 0.33353(14) 0.32707(9) 0.0155(3) Uani 1 1 d U . . C2 C -0.10044(8) 0.29376(14) 0.32626(9) 0.0167(3) Uani 1 1 d U . . C3 C -0.12227(8) 0.35625(15) 0.36231(9) 0.0184(3) Uani 1 1 d U . . H3 H -0.1584 0.3290 0.3617 0.022 Uiso 1 1 calc R . . C4 C -0.09347(8) 0.45661(15) 0.39912(10) 0.0210(3) Uani 1 1 d U . . H4 H -0.1090 0.4964 0.4240 0.025 Uiso 1 1 calc R . . C5 C -0.04201(8) 0.49678(14) 0.39866(9) 0.0199(3) Uani 1 1 d U . . H5 H -0.0222 0.5658 0.4230 0.024 Uiso 1 1 calc R . . C6 C -0.01817(8) 0.43787(14) 0.36296(9) 0.0175(3) Uani 1 1 d U . . C7 C 0.03355(8) 0.49409(14) 0.36323(9) 0.0184(3) Uani 1 1 d U . . H7 H 0.0445 0.5680 0.3831 0.022 Uiso 1 1 calc R . . C8 C 0.11326(8) 0.51834(14) 0.33855(9) 0.0173(3) Uani 1 1 d U . . C9 C 0.10985(9) 0.63444(15) 0.32943(10) 0.0216(3) Uani 1 1 d U . . H9 H 0.0747 0.6754 0.3241 0.026 Uiso 1 1 calc R . . C10 C 0.15820(9) 0.68996(16) 0.32820(11) 0.0247(4) Uani 1 1 d U . . H10 H 0.1569 0.7695 0.3236 0.030 Uiso 1 1 calc R . . C11 C 0.20835(9) 0.62968(16) 0.33373(10) 0.0244(4) Uani 1 1 d U . . H11 H 0.2407 0.6683 0.3317 0.029 Uiso 1 1 calc R . . C12 C 0.21201(8) 0.51353(15) 0.34217(10) 0.0214(3) Uani 1 1 d U . . H12 H 0.2462 0.4728 0.3452 0.026 Uiso 1 1 calc R . . C13 C 0.16511(8) 0.45754(14) 0.34615(9) 0.0177(3) Uani 1 1 d U . . C14 C 0.21652(8) 0.28415(14) 0.39879(9) 0.0180(3) Uani 1 1 d U . . H14 H 0.2566 0.3221 0.4183 0.022 Uiso 1 1 calc R . . C15 C 0.21928(8) 0.16741(15) 0.41789(9) 0.0181(3) Uani 1 1 d U . . C16 C 0.28099(8) 0.11574(16) 0.45398(9) 0.0217(3) Uani 1 1 d U . . H16 H 0.3171 0.1585 0.4633 0.026 Uiso 1 1 calc R . . C17 C 0.29008(8) 0.00519(16) 0.47591(10) 0.0235(3) Uani 1 1 d U . . H17 H 0.3316 -0.0291 0.4985 0.028 Uiso 1 1 calc R . . C18 C 0.23737(9) -0.05597(16) 0.46450(10) 0.0233(3) Uani 1 1 d U . . H18 H 0.2437 -0.1320 0.4804 0.028 Uiso 1 1 calc R . . C19 C 0.17605(8) -0.00870(14) 0.43055(9) 0.0191(3) Uani 1 1 d U . . C20 C 0.16490(8) 0.10545(14) 0.40549(9) 0.0172(3) Uani 1 1 d U . . C21 C -0.13635(8) 0.18873(15) 0.28846(9) 0.0183(3) Uani 1 1 d U . . C22 C -0.20449(8) 0.18951(16) 0.24834(9) 0.0212(3) Uani 1 1 d U . . H22 H -0.2265 0.2583 0.2418 0.025 Uiso 1 1 calc R . . C23 C -0.24033(9) 0.09146(17) 0.21812(10) 0.0259(4) Uani 1 1 d U . . H23 H -0.2864 0.0935 0.1912 0.031 Uiso 1 1 calc R . . C24 C -0.20895(10) -0.00863(18) 0.22728(12) 0.0310(4) Uani 1 1 d U . . H24 H -0.2332 -0.0761 0.2073 0.037 Uiso 1 1 calc R . . C25 C -0.14162(10) -0.01065(17) 0.26579(13) 0.0331(4) Uani 1 1 d U . . H25 H -0.1201 -0.0799 0.2721 0.040 Uiso 1 1 calc R . . C26 C -0.10542(9) 0.08731(16) 0.29516(11) 0.0261(4) Uani 1 1 d U . . H26 H -0.0596 0.0852 0.3198 0.031 Uiso 1 1 calc R . . C27 C 0.12153(8) -0.07670(14) 0.41979(10) 0.0206(3) Uani 1 1 d U . . C28 C 0.06125(9) -0.07834(15) 0.35113(10) 0.0216(3) Uani 1 1 d U . . H28 H 0.0550 -0.0347 0.3110 0.026 Uiso 1 1 calc R . . C29 C 0.01069(9) -0.14296(15) 0.34100(11) 0.0259(4) Uani 1 1 d U . . H29 H -0.0294 -0.1453 0.2935 0.031 Uiso 1 1 calc R . . C30 C 0.01784(10) -0.20415(16) 0.39910(13) 0.0299(4) Uani 1 1 d U . . H30 H -0.0177 -0.2456 0.3924 0.036 Uiso 1 1 calc R . . C31 C 0.07701(11) -0.20434(18) 0.46681(13) 0.0335(4) Uani 1 1 d U . . H31 H 0.0826 -0.2474 0.5068 0.040 Uiso 1 1 calc R . . C32 C 0.12882(10) -0.14195(17) 0.47723(11) 0.0291(4) Uani 1 1 d U . . H32 H 0.1696 -0.1439 0.5240 0.035 Uiso 1 1 calc R . . N1S N 0.13810(15) 0.7939(3) 0.10533(17) 0.0740(10) Uani 0.90 1 d PU A 1 C1S C 0.09810(13) 0.8319(2) 0.04969(15) 0.0394(5) Uani 0.90 1 d PU A 1 C2S C 0.04769(12) 0.8798(2) -0.02120(15) 0.0368(5) Uani 0.90 1 d PU A 1 H2S1 H 0.0583 0.8671 -0.0576 0.055 Uiso 0.90 1 calc PR A 1 H2S2 H 0.0446 0.9607 -0.0154 0.055 Uiso 0.90 1 calc PR A 1 H2S3 H 0.0060 0.8441 -0.0386 0.055 Uiso 0.90 1 calc PR A 1 C1T C 0.0738(7) 0.8587(10) 0.0023(8) 0.105(5) Uani 0.10 1 d PDU B 2 H1T H 0.0943 0.8710 -0.0254 0.126 Uiso 0.10 1 calc PR B 2 Cl1T Cl -0.0004(7) 0.9305(12) -0.0447(8) 0.113(3) Uani 0.10 1 d PDU B 2 Cl2T Cl 0.1275(7) 0.9078(13) 0.0932(7) 0.118(3) Uani 0.10 1 d PDU B 2 Cl3T Cl 0.0609(6) 0.7143(9) 0.0030(7) 0.101(3) Uani 0.10 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01301(9) 0.01206(10) 0.01938(10) 0.00018(7) 0.00910(7) -0.00016(6) N1 0.0155(6) 0.0136(6) 0.0214(6) -0.0001(5) 0.0102(5) -0.0020(5) N2 0.0162(6) 0.0147(7) 0.0205(6) -0.0014(5) 0.0110(5) -0.0013(5) O1 0.0142(5) 0.0149(6) 0.0192(5) -0.0013(4) 0.0100(4) -0.0006(4) O2 0.0155(5) 0.0155(6) 0.0271(6) 0.0039(5) 0.0125(5) 0.0024(4) C1 0.0139(6) 0.0139(7) 0.0182(7) 0.0022(6) 0.0088(6) 0.0024(5) C2 0.0143(7) 0.0164(8) 0.0182(7) 0.0017(6) 0.0085(6) 0.0010(6) C3 0.0156(7) 0.0207(8) 0.0208(7) 0.0030(6) 0.0115(6) 0.0018(6) C4 0.0215(8) 0.0205(8) 0.0249(8) 0.0002(7) 0.0155(7) 0.0030(6) C5 0.0219(8) 0.0150(8) 0.0245(8) -0.0021(6) 0.0142(7) -0.0007(6) C6 0.0168(7) 0.0150(8) 0.0216(7) 0.0002(6) 0.0113(6) 0.0002(6) C7 0.0181(7) 0.0136(7) 0.0225(7) -0.0005(6) 0.0108(6) -0.0017(6) C8 0.0172(7) 0.0148(7) 0.0211(7) -0.0014(6) 0.0115(6) -0.0036(6) C9 0.0231(8) 0.0160(8) 0.0282(8) 0.0017(7) 0.0160(7) -0.0004(6) C10 0.0300(9) 0.0171(8) 0.0314(9) 0.0007(7) 0.0200(8) -0.0044(7) C11 0.0260(8) 0.0222(9) 0.0300(9) -0.0019(7) 0.0188(7) -0.0082(7) C12 0.0199(7) 0.0217(8) 0.0258(8) -0.0020(7) 0.0149(7) -0.0034(6) C13 0.0173(7) 0.0162(8) 0.0191(7) -0.0015(6) 0.0100(6) -0.0029(6) C14 0.0149(7) 0.0196(8) 0.0203(7) -0.0027(6) 0.0105(6) -0.0023(6) C15 0.0169(7) 0.0192(8) 0.0178(7) 0.0000(6) 0.0096(6) 0.0021(6) C16 0.0160(7) 0.0261(9) 0.0218(8) 0.0014(7) 0.0099(6) 0.0022(6) C17 0.0188(8) 0.0270(9) 0.0224(8) 0.0037(7) 0.0101(6) 0.0072(7) C18 0.0238(8) 0.0215(9) 0.0223(8) 0.0048(7) 0.0116(7) 0.0062(7) C19 0.0201(7) 0.0176(8) 0.0191(7) 0.0014(6) 0.0108(6) 0.0016(6) C20 0.0177(7) 0.0169(8) 0.0172(7) 0.0004(6) 0.0101(6) 0.0022(6) C21 0.0179(7) 0.0195(8) 0.0206(7) -0.0013(6) 0.0127(6) -0.0032(6) C22 0.0182(7) 0.0256(9) 0.0218(8) -0.0001(7) 0.0125(6) -0.0026(6) C23 0.0202(8) 0.0353(10) 0.0237(8) -0.0045(7) 0.0133(7) -0.0095(7) C24 0.0309(10) 0.0286(10) 0.0381(10) -0.0111(8) 0.0223(9) -0.0154(8) C25 0.0317(10) 0.0207(9) 0.0513(12) -0.0076(9) 0.0260(10) -0.0060(8) C26 0.0211(8) 0.0200(9) 0.0385(10) -0.0044(7) 0.0176(8) -0.0040(7) C27 0.0230(8) 0.0141(8) 0.0258(8) 0.0030(6) 0.0145(7) 0.0027(6) C28 0.0240(8) 0.0142(8) 0.0270(8) 0.0029(6) 0.0146(7) 0.0024(6) C29 0.0239(8) 0.0157(8) 0.0362(10) 0.0015(7) 0.0159(8) 0.0017(7) C30 0.0324(10) 0.0179(9) 0.0477(12) 0.0037(8) 0.0277(9) 0.0013(7) C31 0.0423(11) 0.0256(10) 0.0396(11) 0.0117(8) 0.0274(10) 0.0023(8) C32 0.0312(9) 0.0254(10) 0.0280(9) 0.0091(8) 0.0150(8) 0.0037(8) N1S 0.0585(17) 0.109(3) 0.0565(16) 0.0118(16) 0.0334(14) 0.0458(17) C1S 0.0359(12) 0.0477(15) 0.0446(13) -0.0055(11) 0.0288(11) 0.0077(11) C2S 0.0365(12) 0.0406(14) 0.0436(12) 0.0024(11) 0.0288(11) 0.0019(10) C1T 0.105(6) 0.105(5) 0.106(6) 0.000(5) 0.060(4) -0.002(4) Cl1T 0.115(5) 0.106(5) 0.114(5) 0.000(4) 0.062(3) 0.002(4) Cl2T 0.115(5) 0.124(5) 0.111(5) -0.006(4) 0.062(3) -0.010(4) Cl3T 0.098(5) 0.106(4) 0.107(5) 0.002(3) 0.062(4) 0.000(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 Zn1 O2 1.9237(12) . ? Zn1 O1 2.0259(12) 2 ? Zn1 N2 2.0838(14) . ? Zn1 N1 2.0887(14) . ? Zn1 O1 2.1044(11) . ? Zn1 Zn1 3.0702(4) 2 ? N1 C7 1.284(2) . ? N1 C8 1.422(2) . ? N2 C14 1.291(2) . ? N2 C13 1.409(2) . ? O1 C1 1.3370(18) . ? O1 Zn1 2.0258(12) 2 ? O2 C20 1.3094(19) . ? C1 C2 1.421(2) . ? C1 C6 1.423(2) . ? C2 C3 1.396(2) . ? C2 C21 1.486(2) . ? C3 C4 1.391(2) . ? C4 C5 1.375(2) . ? C5 C6 1.404(2) . ? C6 C7 1.450(2) . ? C8 C9 1.392(2) . ? C8 C13 1.407(2) . ? C9 C10 1.388(2) . ? C10 C11 1.387(3) . ? C11 C12 1.391(3) . ? C12 C13 1.390(2) . ? C14 C15 1.441(2) . ? C15 C16 1.413(2) . ? C15 C20 1.429(2) . ? C16 C17 1.374(3) . ? C17 C18 1.396(3) . ? C18 C19 1.387(2) . ? C19 C20 1.432(2) . ? C19 C27 1.482(2) . ? C21 C26 1.395(2) . ? C21 C22 1.404(2) . ? C22 C23 1.389(3) . ? C23 C24 1.376(3) . ? C24 C25 1.389(3) . ? C25 C26 1.389(3) . ? C27 C32 1.394(2) . ? C27 C28 1.398(2) . ? C28 C29 1.384(2) . ? C29 C30 1.382(3) . ? C30 C31 1.376(3) . ? C31 C32 1.393(3) . ? N1S C1S 1.141(4) . ? C1S C2S 1.448(4) . ? C1T Cl2T 1.749(5) . ? C1T Cl1T 1.749(5) . ? C1T Cl3T 1.749(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 119.03(5) . 2 ? O2 Zn1 N2 90.62(5) . . ? O1 Zn1 N2 105.18(5) 2 . ? O2 Zn1 N1 136.88(5) . . ? O1 Zn1 N1 104.08(5) 2 . ? N2 Zn1 N1 77.26(5) . . ? O2 Zn1 O1 99.65(5) . . ? O1 Zn1 O1 83.73(5) 2 . ? N2 Zn1 O1 161.10(5) . . ? N1 Zn1 O1 84.46(5) . . ? O2 Zn1 Zn1 119.19(4) . 2 ? O1 Zn1 Zn1 42.97(3) 2 2 ? N2 Zn1 Zn1 143.16(4) . 2 ? N1 Zn1 Zn1 91.92(4) . 2 ? O1 Zn1 Zn1 41.01(3) . 2 ? C7 N1 C8 120.63(14) . . ? C7 N1 Zn1 126.02(12) . . ? C8 N1 Zn1 112.18(10) . . ? C14 N2 C13 121.50(14) . . ? C14 N2 Zn1 124.73(12) . . ? C13 N2 Zn1 112.65(10) . . ? C1 O1 Zn1 119.41(10) . 2 ? C1 O1 Zn1 126.54(10) . . ? Zn1 O1 Zn1 96.02(5) 2 . ? C20 O2 Zn1 128.46(11) . . ? O1 C1 C2 120.53(14) . . ? O1 C1 C6 121.61(14) . . ? C2 C1 C6 117.85(14) . . ? C3 C2 C1 119.02(15) . . ? C3 C2 C21 117.10(14) . . ? C1 C2 C21 123.88(14) . . ? C4 C3 C2 122.92(15) . . ? C5 C4 C3 118.31(15) . . ? C4 C5 C6 121.29(16) . . ? C5 C6 C1 120.56(15) . . ? C5 C6 C7 114.90(15) . . ? C1 C6 C7 124.48(15) . . ? N1 C7 C6 125.75(16) . . ? C9 C8 C13 120.34(15) . . ? C9 C8 N1 124.22(15) . . ? C13 C8 N1 115.41(14) . . ? C10 C9 C8 119.45(16) . . ? C11 C10 C9 120.16(17) . . ? C10 C11 C12 120.96(16) . . ? C13 C12 C11 119.33(16) . . ? C12 C13 C8 119.70(16) . . ? C12 C13 N2 125.71(15) . . ? C8 C13 N2 114.59(14) . . ? N2 C14 C15 124.96(15) . . ? C16 C15 C20 119.95(16) . . ? C16 C15 C14 116.09(15) . . ? C20 C15 C14 123.90(15) . . ? C17 C16 C15 121.61(16) . . ? C16 C17 C18 118.90(16) . . ? C19 C18 C17 121.79(17) . . ? C18 C19 C20 120.42(16) . . ? C18 C19 C27 119.94(16) . . ? C20 C19 C27 119.64(15) . . ? O2 C20 C15 124.23(15) . . ? O2 C20 C19 118.40(15) . . ? C15 C20 C19 117.30(14) . . ? C26 C21 C22 118.27(16) . . ? C26 C21 C2 123.06(15) . . ? C22 C21 C2 118.52(15) . . ? C23 C22 C21 121.17(17) . . ? C24 C23 C22 119.84(17) . . ? C23 C24 C25 119.76(18) . . ? C26 C25 C24 120.81(19) . . ? C25 C26 C21 120.08(17) . . ? C32 C27 C28 117.93(17) . . ? C32 C27 C19 121.27(16) . . ? C28 C27 C19 120.80(15) . . ? C29 C28 C27 120.65(17) . . ? C30 C29 C28 120.83(18) . . ? C31 C30 C29 119.21(18) . . ? C30 C31 C32 120.51(18) . . ? C31 C32 C27 120.80(19) . . ? N1S C1S C2S 179.5(3) . . ? Cl2T C1T Cl1T 112.4(9) . . ? Cl2T C1T Cl3T 110.2(9) . . ? Cl1T C1T Cl3T 110.3(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 O2 Zn1 N1 C7 -67.97(16) . . . . ? O1 Zn1 N1 C7 112.34(14) 2 . . . ? N2 Zn1 N1 C7 -144.95(15) . . . . ? O1 Zn1 N1 C7 30.24(14) . . . . ? Zn1 Zn1 N1 C7 70.61(14) 2 . . . ? O2 Zn1 N1 C8 99.68(12) . . . . ? O1 Zn1 N1 C8 -80.02(11) 2 . . . ? N2 Zn1 N1 C8 22.69(11) . . . . ? O1 Zn1 N1 C8 -162.11(11) . . . . ? Zn1 Zn1 N1 C8 -121.74(10) 2 . . . ? O2 Zn1 N2 C14 5.04(14) . . . . ? O1 Zn1 N2 C14 -115.35(13) 2 . . . ? N1 Zn1 N2 C14 143.28(14) . . . . ? O1 Zn1 N2 C14 128.36(16) . . . . ? Zn1 Zn1 N2 C14 -140.87(11) 2 . . . ? O2 Zn1 N2 C13 -162.94(11) . . . . ? O1 Zn1 N2 C13 76.67(11) 2 . . . ? N1 Zn1 N2 C13 -24.70(11) . . . . ? O1 Zn1 N2 C13 -39.6(2) . . . . ? Zn1 Zn1 N2 C13 51.15(14) 2 . . . ? O2 Zn1 O1 C1 102.21(12) . . . . ? O1 Zn1 O1 C1 -139.33(11) 2 . . . ? N2 Zn1 O1 C1 -19.8(2) . . . . ? N1 Zn1 O1 C1 -34.46(12) . . . . ? Zn1 Zn1 O1 C1 -133.84(14) 2 . . . ? O2 Zn1 O1 Zn1 -123.95(5) . . . 2 ? O1 Zn1 O1 Zn1 -5.49(6) 2 . . 2 ? N2 Zn1 O1 Zn1 114.00(15) . . . 2 ? N1 Zn1 O1 Zn1 99.38(5) . . . 2 ? O1 Zn1 O2 C20 90.23(14) 2 . . . ? N2 Zn1 O2 C20 -17.56(14) . . . . ? N1 Zn1 O2 C20 -89.44(15) . . . . ? O1 Zn1 O2 C20 178.37(13) . . . . ? Zn1 Zn1 O2 C20 139.80(12) 2 . . . ? Zn1 O1 C1 C2 78.55(16) 2 . . . ? Zn1 O1 C1 C2 -156.87(11) . . . . ? Zn1 O1 C1 C6 -100.34(15) 2 . . . ? Zn1 O1 C1 C6 24.2(2) . . . . ? O1 C1 C2 C3 179.12(14) . . . . ? C6 C1 C2 C3 -1.9(2) . . . . ? O1 C1 C2 C21 -1.4(2) . . . . ? C6 C1 C2 C21 177.54(15) . . . . ? C1 C2 C3 C4 0.2(2) . . . . ? C21 C2 C3 C4 -179.33(15) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? C3 C4 C5 C6 -0.9(3) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C4 C5 C6 C7 176.34(16) . . . . ? O1 C1 C6 C5 -178.74(15) . . . . ? C2 C1 C6 C5 2.3(2) . . . . ? O1 C1 C6 C7 4.3(2) . . . . ? C2 C1 C6 C7 -174.67(15) . . . . ? C8 N1 C7 C6 176.58(15) . . . . ? Zn1 N1 C7 C6 -16.7(2) . . . . ? C5 C6 C7 N1 174.47(16) . . . . ? C1 C6 C7 N1 -8.4(3) . . . . ? C7 N1 C8 C9 -30.9(2) . . . . ? Zn1 N1 C8 C9 160.69(14) . . . . ? C7 N1 C8 C13 150.71(16) . . . . ? Zn1 N1 C8 C13 -17.69(17) . . . . ? C13 C8 C9 C10 -0.3(3) . . . . ? N1 C8 C9 C10 -178.59(16) . . . . ? C8 C9 C10 C11 2.0(3) . . . . ? C9 C10 C11 C12 -1.4(3) . . . . ? C10 C11 C12 C13 -0.9(3) . . . . ? C11 C12 C13 C8 2.6(3) . . . . ? C11 C12 C13 N2 -177.72(16) . . . . ? C9 C8 C13 C12 -2.0(2) . . . . ? N1 C8 C13 C12 176.43(15) . . . . ? C9 C8 C13 N2 178.26(15) . . . . ? N1 C8 C13 N2 -3.3(2) . . . . ? C14 N2 C13 C12 34.7(3) . . . . ? Zn1 N2 C13 C12 -156.86(14) . . . . ? C14 N2 C13 C8 -145.58(16) . . . . ? Zn1 N2 C13 C8 22.84(17) . . . . ? C13 N2 C14 C15 174.53(15) . . . . ? Zn1 N2 C14 C15 7.6(2) . . . . ? N2 C14 C15 C16 170.11(16) . . . . ? N2 C14 C15 C20 -12.9(3) . . . . ? C20 C15 C16 C17 2.0(3) . . . . ? C14 C15 C16 C17 179.11(16) . . . . ? C15 C16 C17 C18 -2.3(3) . . . . ? C16 C17 C18 C19 1.1(3) . . . . ? C17 C18 C19 C20 0.4(3) . . . . ? C17 C18 C19 C27 -179.80(16) . . . . ? Zn1 O2 C20 C15 17.8(2) . . . . ? Zn1 O2 C20 C19 -165.19(11) . . . . ? C16 C15 C20 O2 176.69(15) . . . . ? C14 C15 C20 O2 -0.2(3) . . . . ? C16 C15 C20 C19 -0.3(2) . . . . ? C14 C15 C20 C19 -177.27(15) . . . . ? C18 C19 C20 O2 -178.01(15) . . . . ? C27 C19 C20 O2 2.2(2) . . . . ? C18 C19 C20 C15 -0.8(2) . . . . ? C27 C19 C20 C15 179.43(15) . . . . ? C3 C2 C21 C26 -134.38(18) . . . . ? C1 C2 C21 C26 46.1(2) . . . . ? C3 C2 C21 C22 41.0(2) . . . . ? C1 C2 C21 C22 -138.45(17) . . . . ? C26 C21 C22 C23 2.2(3) . . . . ? C2 C21 C22 C23 -173.49(15) . . . . ? C21 C22 C23 C24 -0.1(3) . . . . ? C22 C23 C24 C25 -0.9(3) . . . . ? C23 C24 C25 C26 -0.1(3) . . . . ? C24 C25 C26 C21 2.2(3) . . . . ? C22 C21 C26 C25 -3.2(3) . . . . ? C2 C21 C26 C25 172.24(18) . . . . ? C18 C19 C27 C32 46.6(2) . . . . ? C20 C19 C27 C32 -133.64(18) . . . . ? C18 C19 C27 C28 -132.59(18) . . . . ? C20 C19 C27 C28 47.2(2) . . . . ? C32 C27 C28 C29 0.0(3) . . . . ? C19 C27 C28 C29 179.21(16) . . . . ? C27 C28 C29 C30 2.3(3) . . . . ? C28 C29 C30 C31 -2.9(3) . . . . ? C29 C30 C31 C32 1.2(3) . . . . ? C30 C31 C32 C27 1.1(3) . . . . ? C28 C27 C32 C31 -1.7(3) . . . . ? C19 C27 C32 C31 179.13(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.742 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.072 data_mo_awk811-05 _database_code_depnum_ccdc_archive 'CCDC 910864' #TrackingRef 'mo_awk811-05X.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H27 N3 O2 Zn' _chemical_formula_weight 610.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.0990(9) _cell_length_b 14.7495(9) _cell_length_c 14.5848(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.860(2) _cell_angle_gamma 90.00 _cell_volume 2794.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2289 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.60 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9136 _exptl_absorpt_correction_T_max 0.9729 _exptl_absorpt_process_details ; TWINABS Version 2008/0 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Micorfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14488 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.02 _reflns_number_total 14657 _reflns_number_gt 10562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0806P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14657 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1269 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.910498(18) 0.772757(15) 0.465990(17) 0.01306(8) Uani 1 1 d . . . N1 N 0.98456(14) 0.70516(11) 0.38736(13) 0.0153(4) Uani 1 1 d . . . N2 N 0.90884(13) 0.87020(11) 0.35996(12) 0.0150(4) Uani 1 1 d . . . N3 N 0.75520(13) 0.73439(11) 0.41041(13) 0.0134(3) Uani 1 1 d . . . O1 O 0.96976(11) 0.68283(9) 0.57473(10) 0.0158(3) Uani 1 1 d . . . O2 O 0.90157(11) 0.87080(9) 0.55449(10) 0.0150(3) Uani 1 1 d . . . C1 C 0.92818(16) 0.83281(14) 0.27955(15) 0.0164(4) Uani 1 1 d . . . C2 C 0.90767(17) 0.87632(16) 0.18878(16) 0.0216(5) Uani 1 1 d . . . H2 H 0.8803 0.9360 0.1783 0.026 Uiso 1 1 calc R . . C3 C 0.92735(19) 0.83220(17) 0.11398(16) 0.0259(5) Uani 1 1 d . . . H3 H 0.9151 0.8625 0.0529 0.031 Uiso 1 1 calc R . . C4 C 0.9646(2) 0.74472(17) 0.12778(17) 0.0249(5) Uani 1 1 d . . . H4 H 0.9777 0.7151 0.0760 0.030 Uiso 1 1 calc R . . C5 C 0.98329(18) 0.69941(16) 0.21666(17) 0.0218(5) Uani 1 1 d . . . H5 H 1.0071 0.6385 0.2249 0.026 Uiso 1 1 calc R . . C6 C 0.96688(17) 0.74392(14) 0.29375(16) 0.0166(4) Uani 1 1 d . . . C7 C 1.05210(16) 0.64137(14) 0.42263(15) 0.0161(4) Uani 1 1 d . . . H7 H 1.0865 0.6219 0.3816 0.019 Uiso 1 1 calc R . . C8 C 1.08034(16) 0.59721(13) 0.51668(15) 0.0160(4) Uani 1 1 d . . . C9 C 1.03645(16) 0.61823(13) 0.58765(15) 0.0147(4) Uani 1 1 d . . . C10 C 1.06971(16) 0.56463(13) 0.67746(15) 0.0158(4) Uani 1 1 d . . . C11 C 1.14500(17) 0.49942(14) 0.69323(16) 0.0199(5) Uani 1 1 d . . . H11 H 1.1667 0.4649 0.7529 0.024 Uiso 1 1 calc R . . C12 C 1.19042(17) 0.48206(14) 0.62532(17) 0.0207(5) Uani 1 1 d . . . H12 H 1.2433 0.4379 0.6393 0.025 Uiso 1 1 calc R . . C13 C 1.15714(17) 0.52997(14) 0.53812(17) 0.0201(5) Uani 1 1 d . . . H13 H 1.1865 0.5176 0.4908 0.024 Uiso 1 1 calc R . . C14 C 1.02467(16) 0.57661(13) 0.75310(15) 0.0162(4) Uani 1 1 d . . . C15 C 0.91997(17) 0.59410(14) 0.72574(16) 0.0190(4) Uani 1 1 d . . . H15 H 0.8768 0.5998 0.6573 0.023 Uiso 1 1 calc R . . C16 C 0.87774(19) 0.60329(15) 0.79679(16) 0.0220(5) Uani 1 1 d . . . H16 H 0.8063 0.6155 0.7768 0.026 Uiso 1 1 calc R . . C17 C 0.93986(19) 0.59469(15) 0.89715(17) 0.0248(5) Uani 1 1 d . . . H17 H 0.9113 0.6013 0.9460 0.030 Uiso 1 1 calc R . . C18 C 1.04309(19) 0.57656(15) 0.92542(16) 0.0238(5) Uani 1 1 d . . . H18 H 1.0854 0.5698 0.9940 0.029 Uiso 1 1 calc R . . C19 C 1.08606(18) 0.56807(14) 0.85458(16) 0.0207(5) Uani 1 1 d . . . H19 H 1.1576 0.5564 0.8752 0.025 Uiso 1 1 calc R . . C20 C 0.87398(16) 0.99967(14) 0.44558(15) 0.0146(4) Uani 1 1 d . . . C21 C 0.85041(16) 1.09301(14) 0.43121(16) 0.0167(4) Uani 1 1 d . . . H21 H 0.8543 1.1226 0.3749 0.020 Uiso 1 1 calc R . . C22 C 0.82206(17) 1.14210(14) 0.49612(16) 0.0192(4) Uani 1 1 d . . . H22 H 0.8060 1.2048 0.4851 0.023 Uiso 1 1 calc R . . C23 C 0.81722(16) 1.09786(14) 0.57908(16) 0.0181(4) Uani 1 1 d . . . H23 H 0.7972 1.1315 0.6242 0.022 Uiso 1 1 calc R . . C24 C 0.84058(16) 1.00646(14) 0.59787(15) 0.0155(4) Uani 1 1 d . . . C25 C 0.87294(15) 0.95442(13) 0.53165(15) 0.0140(4) Uani 1 1 d . . . C26 C 0.82728(16) 0.96215(14) 0.68343(15) 0.0155(4) Uani 1 1 d . . . C27 C 0.86144(17) 1.00316(15) 0.77742(16) 0.0202(5) Uani 1 1 d . . . H27 H 0.8983 1.0587 0.7882 0.024 Uiso 1 1 calc R . . C28 C 0.84231(19) 0.96389(16) 0.85521(16) 0.0241(5) Uani 1 1 d . . . H28 H 0.8664 0.9925 0.9185 0.029 Uiso 1 1 calc R . . C29 C 0.78824(18) 0.88312(16) 0.84075(17) 0.0244(5) Uani 1 1 d . . . H29 H 0.7745 0.8566 0.8937 0.029 Uiso 1 1 calc R . . C30 C 0.75429(18) 0.84117(15) 0.74836(16) 0.0220(5) Uani 1 1 d . . . H30 H 0.7173 0.7857 0.7380 0.026 Uiso 1 1 calc R . . C31 C 0.77432(17) 0.88025(14) 0.67104(16) 0.0187(4) Uani 1 1 d . . . H31 H 0.7514 0.8505 0.6084 0.022 Uiso 1 1 calc R . . C32 C 0.89961(15) 0.95625(14) 0.36952(15) 0.0155(4) Uani 1 1 d . . . H32 H 0.9107 0.9945 0.3222 0.019 Uiso 1 1 calc R . . C33 C 0.69142(17) 0.73774(13) 0.31483(16) 0.0166(4) Uani 1 1 d . . . H33 H 0.7172 0.7600 0.2679 0.020 Uiso 1 1 calc R . . C34 C 0.58971(18) 0.71044(13) 0.28051(17) 0.0200(5) Uani 1 1 d . . . H34 H 0.5471 0.7127 0.2116 0.024 Uiso 1 1 calc R . . C35 C 0.55168(18) 0.67981(15) 0.34895(17) 0.0228(5) Uani 1 1 d . . . H35 H 0.4819 0.6613 0.3281 0.027 Uiso 1 1 calc R . . C36 C 0.61690(18) 0.67647(15) 0.44885(17) 0.0217(5) Uani 1 1 d . . . H36 H 0.5925 0.6557 0.4974 0.026 Uiso 1 1 calc R . . C37 C 0.71742(17) 0.70379(14) 0.47616(16) 0.0170(4) Uani 1 1 d . . . H37 H 0.7620 0.7009 0.5444 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01197(13) 0.01565(13) 0.01190(13) 0.00009(9) 0.00502(9) 0.00086(9) N1 0.0148(9) 0.0165(8) 0.0161(9) -0.0024(7) 0.0077(8) -0.0023(7) N2 0.0122(9) 0.0211(9) 0.0122(9) 0.0008(7) 0.0053(7) 0.0004(7) N3 0.0133(9) 0.0139(8) 0.0143(9) -0.0008(7) 0.0068(7) 0.0010(7) O1 0.0148(8) 0.0166(7) 0.0152(7) 0.0016(6) 0.0048(6) 0.0044(6) O2 0.0169(8) 0.0143(7) 0.0143(7) 0.0003(6) 0.0066(6) 0.0022(6) C1 0.0123(10) 0.0245(11) 0.0130(10) -0.0024(8) 0.0056(8) -0.0027(8) C2 0.0181(12) 0.0293(12) 0.0163(11) 0.0026(9) 0.0056(9) 0.0030(9) C3 0.0254(13) 0.0418(14) 0.0117(11) 0.0007(10) 0.0086(10) -0.0006(11) C4 0.0270(13) 0.0361(13) 0.0149(11) -0.0073(9) 0.0116(10) -0.0050(10) C5 0.0223(12) 0.0246(11) 0.0197(11) -0.0059(9) 0.0093(10) -0.0019(9) C6 0.0125(10) 0.0236(11) 0.0135(10) -0.0023(8) 0.0050(9) -0.0031(8) C7 0.0128(11) 0.0162(10) 0.0201(11) -0.0062(8) 0.0071(9) -0.0045(8) C8 0.0132(11) 0.0140(9) 0.0196(11) -0.0037(8) 0.0050(9) -0.0018(8) C9 0.0105(10) 0.0136(9) 0.0175(10) -0.0029(8) 0.0027(8) -0.0019(8) C10 0.0116(10) 0.0144(10) 0.0174(10) -0.0029(8) 0.0010(9) -0.0029(8) C11 0.0170(11) 0.0144(10) 0.0215(11) 0.0008(8) 0.0001(9) -0.0021(8) C12 0.0136(11) 0.0140(10) 0.0305(12) -0.0032(9) 0.0043(10) 0.0023(8) C13 0.0177(11) 0.0179(10) 0.0258(12) -0.0067(9) 0.0096(10) -0.0014(9) C14 0.0165(11) 0.0123(9) 0.0175(11) 0.0024(8) 0.0041(9) -0.0030(8) C15 0.0177(11) 0.0178(10) 0.0180(11) 0.0020(8) 0.0031(9) -0.0032(8) C16 0.0211(12) 0.0237(11) 0.0215(12) 0.0015(9) 0.0086(10) -0.0034(9) C17 0.0293(14) 0.0257(12) 0.0209(12) 0.0000(9) 0.0111(11) -0.0084(10) C18 0.0282(14) 0.0256(12) 0.0140(11) 0.0043(9) 0.0044(10) -0.0074(10) C19 0.0167(12) 0.0183(10) 0.0211(11) 0.0044(9) 0.0008(9) -0.0031(8) C20 0.0113(10) 0.0160(10) 0.0153(10) -0.0014(8) 0.0039(8) -0.0029(8) C21 0.0113(10) 0.0190(10) 0.0176(11) 0.0037(8) 0.0031(9) -0.0016(8) C22 0.0150(11) 0.0147(10) 0.0259(12) 0.0000(9) 0.0060(9) 0.0003(8) C23 0.0140(11) 0.0190(10) 0.0215(11) -0.0035(8) 0.0071(9) 0.0007(8) C24 0.0103(10) 0.0188(10) 0.0159(10) -0.0007(8) 0.0036(9) -0.0014(8) C25 0.0080(10) 0.0170(10) 0.0143(10) -0.0006(8) 0.0014(8) -0.0010(8) C26 0.0110(10) 0.0200(10) 0.0156(10) 0.0006(8) 0.0054(9) 0.0043(8) C27 0.0190(12) 0.0211(11) 0.0216(11) -0.0032(9) 0.0089(10) 0.0031(9) C28 0.0247(12) 0.0340(13) 0.0139(11) -0.0007(9) 0.0077(10) 0.0079(10) C29 0.0212(13) 0.0353(13) 0.0193(11) 0.0068(10) 0.0108(10) 0.0070(10) C30 0.0181(12) 0.0254(12) 0.0238(12) 0.0052(9) 0.0097(10) 0.0007(9) C31 0.0161(11) 0.0233(11) 0.0173(11) 0.0000(9) 0.0071(9) 0.0010(9) C32 0.0104(10) 0.0222(10) 0.0129(10) 0.0042(8) 0.0033(8) 0.0000(8) C33 0.0193(11) 0.0141(10) 0.0162(10) 0.0001(8) 0.0067(9) 0.0021(8) C34 0.0210(12) 0.0151(10) 0.0184(11) -0.0024(8) 0.0015(9) 0.0014(8) C35 0.0147(11) 0.0212(11) 0.0317(13) -0.0030(10) 0.0082(10) -0.0022(9) C36 0.0200(12) 0.0237(11) 0.0245(12) 0.0013(9) 0.0120(10) -0.0020(9) C37 0.0197(11) 0.0172(10) 0.0152(10) 0.0011(8) 0.0078(9) 0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O2 1.9747(14) . ? Zn1 O1 1.9857(14) . ? Zn1 N1 2.0808(17) . ? Zn1 N3 2.0959(18) . ? Zn1 N2 2.1046(17) . ? N1 C7 1.295(3) . ? N1 C6 1.410(3) . ? N2 C32 1.289(3) . ? N2 C1 1.415(3) . ? N3 C33 1.334(3) . ? N3 C37 1.343(3) . ? O1 C9 1.300(2) . ? O2 C25 1.300(2) . ? C1 C2 1.397(3) . ? C1 C6 1.404(3) . ? C2 C3 1.388(3) . ? C3 C4 1.378(3) . ? C4 C5 1.390(3) . ? C5 C6 1.397(3) . ? C7 C8 1.428(3) . ? C8 C13 1.411(3) . ? C8 C9 1.431(3) . ? C9 C10 1.443(3) . ? C10 C11 1.384(3) . ? C10 C14 1.482(3) . ? C11 C12 1.396(3) . ? C12 C13 1.369(3) . ? C14 C15 1.395(3) . ? C14 C19 1.400(3) . ? C15 C16 1.388(3) . ? C16 C17 1.389(3) . ? C17 C18 1.376(3) . ? C18 C19 1.392(3) . ? C20 C21 1.413(3) . ? C20 C25 1.427(3) . ? C20 C32 1.443(3) . ? C21 C22 1.369(3) . ? C22 C23 1.400(3) . ? C23 C24 1.390(3) . ? C24 C25 1.440(3) . ? C24 C26 1.484(3) . ? C26 C31 1.395(3) . ? C26 C27 1.401(3) . ? C27 C28 1.390(3) . ? C28 C29 1.386(3) . ? C29 C30 1.388(3) . ? C30 C31 1.390(3) . ? C33 C34 1.383(3) . ? C34 C35 1.380(3) . ? C35 C36 1.389(3) . ? C36 C37 1.375(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Zn1 O1 94.65(6) . . ? O2 Zn1 N1 152.15(7) . . ? O1 Zn1 N1 88.54(6) . . ? O2 Zn1 N3 97.37(6) . . ? O1 Zn1 N3 100.41(6) . . ? N1 Zn1 N3 109.27(7) . . ? O2 Zn1 N2 89.71(6) . . ? O1 Zn1 N2 157.53(6) . . ? N1 Zn1 N2 77.70(7) . . ? N3 Zn1 N2 100.86(7) . . ? C7 N1 C6 120.36(18) . . ? C7 N1 Zn1 125.34(15) . . ? C6 N1 Zn1 113.67(13) . . ? C32 N2 C1 122.24(17) . . ? C32 N2 Zn1 124.46(14) . . ? C1 N2 Zn1 113.08(13) . . ? C33 N3 C37 117.72(18) . . ? C33 N3 Zn1 124.95(14) . . ? C37 N3 Zn1 117.33(14) . . ? C9 O1 Zn1 131.43(13) . . ? C25 O2 Zn1 128.27(13) . . ? C2 C1 C6 119.62(19) . . ? C2 C1 N2 124.8(2) . . ? C6 C1 N2 115.51(18) . . ? C3 C2 C1 119.9(2) . . ? C4 C3 C2 120.4(2) . . ? C3 C4 C5 120.6(2) . . ? C4 C5 C6 119.6(2) . . ? C5 C6 C1 119.8(2) . . ? C5 C6 N1 124.5(2) . . ? C1 C6 N1 115.70(18) . . ? N1 C7 C8 126.91(19) . . ? C13 C8 C7 115.91(19) . . ? C13 C8 C9 120.15(19) . . ? C7 C8 C9 123.94(19) . . ? O1 C9 C8 123.06(18) . . ? O1 C9 C10 119.65(18) . . ? C8 C9 C10 117.29(18) . . ? C11 C10 C9 119.29(19) . . ? C11 C10 C14 118.82(19) . . ? C9 C10 C14 121.89(18) . . ? C10 C11 C12 122.9(2) . . ? C13 C12 C11 118.6(2) . . ? C12 C13 C8 121.7(2) . . ? C15 C14 C19 118.0(2) . . ? C15 C14 C10 121.38(19) . . ? C19 C14 C10 120.56(19) . . ? C16 C15 C14 121.2(2) . . ? C15 C16 C17 120.0(2) . . ? C18 C17 C16 119.6(2) . . ? C17 C18 C19 120.7(2) . . ? C18 C19 C14 120.5(2) . . ? C21 C20 C25 120.27(18) . . ? C21 C20 C32 115.67(18) . . ? C25 C20 C32 124.05(19) . . ? C22 C21 C20 121.87(19) . . ? C21 C22 C23 118.46(19) . . ? C24 C23 C22 122.38(19) . . ? C23 C24 C25 119.84(18) . . ? C23 C24 C26 119.70(18) . . ? C25 C24 C26 120.40(18) . . ? O2 C25 C20 124.12(18) . . ? O2 C25 C24 118.79(17) . . ? C20 C25 C24 117.07(18) . . ? C31 C26 C27 117.63(19) . . ? C31 C26 C24 120.59(18) . . ? C27 C26 C24 121.66(19) . . ? C28 C27 C26 121.1(2) . . ? C29 C28 C27 120.2(2) . . ? C28 C29 C30 119.5(2) . . ? C29 C30 C31 120.1(2) . . ? C30 C31 C26 121.4(2) . . ? N2 C32 C20 125.88(18) . . ? N3 C33 C34 123.4(2) . . ? C35 C34 C33 118.3(2) . . ? C34 C35 C36 119.0(2) . . ? C37 C36 C35 118.8(2) . . ? N3 C37 C36 122.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Zn1 N1 C7 87.7(2) . . . . ? O1 Zn1 N1 C7 -9.47(17) . . . . ? N3 Zn1 N1 C7 -109.99(17) . . . . ? N2 Zn1 N1 C7 152.65(18) . . . . ? O2 Zn1 N1 C6 -83.12(19) . . . . ? O1 Zn1 N1 C6 179.68(14) . . . . ? N3 Zn1 N1 C6 79.16(15) . . . . ? N2 Zn1 N1 C6 -18.20(14) . . . . ? O2 Zn1 N2 C32 -2.71(17) . . . . ? O1 Zn1 N2 C32 -104.2(2) . . . . ? N1 Zn1 N2 C32 -157.68(18) . . . . ? N3 Zn1 N2 C32 94.74(17) . . . . ? O2 Zn1 N2 C1 171.98(14) . . . . ? O1 Zn1 N2 C1 70.5(2) . . . . ? N1 Zn1 N2 C1 17.01(14) . . . . ? N3 Zn1 N2 C1 -90.57(14) . . . . ? O2 Zn1 N3 C33 119.00(15) . . . . ? O1 Zn1 N3 C33 -144.87(15) . . . . ? N1 Zn1 N3 C33 -52.76(16) . . . . ? N2 Zn1 N3 C33 27.88(16) . . . . ? O2 Zn1 N3 C37 -61.29(15) . . . . ? O1 Zn1 N3 C37 34.84(15) . . . . ? N1 Zn1 N3 C37 126.95(14) . . . . ? N2 Zn1 N3 C37 -152.41(14) . . . . ? O2 Zn1 O1 C9 -145.32(18) . . . . ? N1 Zn1 O1 C9 6.97(18) . . . . ? N3 Zn1 O1 C9 116.30(18) . . . . ? N2 Zn1 O1 C9 -44.8(3) . . . . ? O1 Zn1 O2 C25 175.94(16) . . . . ? N1 Zn1 O2 C25 80.3(2) . . . . ? N3 Zn1 O2 C25 -82.91(17) . . . . ? N2 Zn1 O2 C25 18.01(17) . . . . ? C32 N2 C1 C2 -21.3(3) . . . . ? Zn1 N2 C1 C2 163.86(18) . . . . ? C32 N2 C1 C6 161.4(2) . . . . ? Zn1 N2 C1 C6 -13.4(2) . . . . ? C6 C1 C2 C3 -1.2(3) . . . . ? N2 C1 C2 C3 -178.3(2) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 -1.8(4) . . . . ? C4 C5 C6 C1 2.3(3) . . . . ? C4 C5 C6 N1 -179.1(2) . . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? N2 C1 C6 C5 176.63(19) . . . . ? C2 C1 C6 N1 -179.54(19) . . . . ? N2 C1 C6 N1 -2.1(3) . . . . ? C7 N1 C6 C5 26.8(3) . . . . ? Zn1 N1 C6 C5 -161.80(18) . . . . ? C7 N1 C6 C1 -154.48(19) . . . . ? Zn1 N1 C6 C1 16.9(2) . . . . ? C6 N1 C7 C8 178.35(19) . . . . ? Zn1 N1 C7 C8 8.1(3) . . . . ? N1 C7 C8 C13 -179.5(2) . . . . ? N1 C7 C8 C9 -0.1(3) . . . . ? Zn1 O1 C9 C8 -2.3(3) . . . . ? Zn1 O1 C9 C10 177.22(13) . . . . ? C13 C8 C9 O1 176.01(19) . . . . ? C7 C8 C9 O1 -3.3(3) . . . . ? C13 C8 C9 C10 -3.5(3) . . . . ? C7 C8 C9 C10 177.21(18) . . . . ? O1 C9 C10 C11 -176.37(19) . . . . ? C8 C9 C10 C11 3.2(3) . . . . ? O1 C9 C10 C14 4.3(3) . . . . ? C8 C9 C10 C14 -176.12(18) . . . . ? C9 C10 C11 C12 -0.6(3) . . . . ? C14 C10 C11 C12 178.72(19) . . . . ? C10 C11 C12 C13 -1.8(3) . . . . ? C11 C12 C13 C8 1.4(3) . . . . ? C7 C8 C13 C12 -179.40(19) . . . . ? C9 C8 C13 C12 1.3(3) . . . . ? C11 C10 C14 C15 -141.2(2) . . . . ? C9 C10 C14 C15 38.1(3) . . . . ? C11 C10 C14 C19 37.0(3) . . . . ? C9 C10 C14 C19 -143.7(2) . . . . ? C19 C14 C15 C16 0.3(3) . . . . ? C10 C14 C15 C16 178.57(19) . . . . ? C14 C15 C16 C17 -0.3(3) . . . . ? C15 C16 C17 C18 -0.4(3) . . . . ? C16 C17 C18 C19 0.9(3) . . . . ? C17 C18 C19 C14 -0.9(3) . . . . ? C15 C14 C19 C18 0.2(3) . . . . ? C10 C14 C19 C18 -178.01(19) . . . . ? C25 C20 C21 C22 -2.6(3) . . . . ? C32 C20 C21 C22 178.2(2) . . . . ? C20 C21 C22 C23 0.4(3) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C22 C23 C24 C25 1.2(3) . . . . ? C22 C23 C24 C26 -176.0(2) . . . . ? Zn1 O2 C25 C20 -21.4(3) . . . . ? Zn1 O2 C25 C24 160.36(14) . . . . ? C21 C20 C25 O2 -174.26(19) . . . . ? C32 C20 C25 O2 4.8(3) . . . . ? C21 C20 C25 C24 4.0(3) . . . . ? C32 C20 C25 C24 -176.93(19) . . . . ? C23 C24 C25 O2 175.07(19) . . . . ? C26 C24 C25 O2 -7.8(3) . . . . ? C23 C24 C25 C20 -3.3(3) . . . . ? C26 C24 C25 C20 173.84(18) . . . . ? C23 C24 C26 C31 130.8(2) . . . . ? C25 C24 C26 C31 -46.3(3) . . . . ? C23 C24 C26 C27 -45.2(3) . . . . ? C25 C24 C26 C27 137.7(2) . . . . ? C31 C26 C27 C28 -0.6(3) . . . . ? C24 C26 C27 C28 175.6(2) . . . . ? C26 C27 C28 C29 -0.3(3) . . . . ? C27 C28 C29 C30 0.7(3) . . . . ? C28 C29 C30 C31 -0.2(3) . . . . ? C29 C30 C31 C26 -0.8(3) . . . . ? C27 C26 C31 C30 1.1(3) . . . . ? C24 C26 C31 C30 -175.1(2) . . . . ? C1 N2 C32 C20 176.1(2) . . . . ? Zn1 N2 C32 C20 -9.7(3) . . . . ? C21 C20 C32 N2 -169.3(2) . . . . ? C25 C20 C32 N2 11.6(3) . . . . ? C37 N3 C33 C34 -0.8(3) . . . . ? Zn1 N3 C33 C34 178.89(15) . . . . ? N3 C33 C34 C35 1.3(3) . . . . ? C33 C34 C35 C36 -0.8(3) . . . . ? C34 C35 C36 C37 -0.1(3) . . . . ? C33 N3 C37 C36 -0.2(3) . . . . ? Zn1 N3 C37 C36 -179.89(16) . . . . ? C35 C36 C37 N3 0.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.488 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.102 data_mo_da542_2_0m-sr _database_code_depnum_ccdc_archive 'CCDC 910865' #TrackingRef 'mo_da542_2_0m-srX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92.50 H105.50 N6 Ni3 O9.25 S3.25' _chemical_formula_weight 1729.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 13.2122(4) _cell_length_b 22.0668(7) _cell_length_c 22.7321(8) _cell_angle_alpha 100.0770(10) _cell_angle_beta 96.7840(10) _cell_angle_gamma 105.8970(10) _cell_volume 6178.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9001 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.57 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.930 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1825 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8748 _exptl_absorpt_correction_T_max 0.9730 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 72358 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 25.86 _reflns_number_total 23579 _reflns_number_gt 17204 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.1212P)^2^+0.6585P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23579 _refine_ls_number_parameters 1336 _refine_ls_number_restraints 560 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1846 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.051 0.500 1.160 2044 703 ' ' _platon_squeeze_details ; ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.74478(3) 0.81092(2) 0.612427(18) 0.02609(12) Uani 1 1 d . . . Ni2 Ni 0.41597(3) 0.427477(19) 0.82696(2) 0.03114(13) Uani 1 1 d . . . Ni3 Ni 0.92863(3) 0.903700(18) 1.129232(17) 0.02169(11) Uani 1 1 d . . . N1 N 0.6484(2) 0.80552(12) 0.66556(11) 0.0249(6) Uani 1 1 d . . . N2 N 0.8190(2) 0.77561(13) 0.66442(12) 0.0260(6) Uani 1 1 d . . . N5 N 0.79829(19) 0.88475(12) 1.07811(11) 0.0222(5) Uani 1 1 d . . . N6 N 0.96577(19) 0.85343(12) 1.06638(11) 0.0228(5) Uani 1 1 d . A . O1 O 0.67367(19) 0.84865(12) 0.56218(10) 0.0330(5) Uani 1 1 d . . . O2 O 0.83863(18) 0.81393(11) 0.55812(10) 0.0309(5) Uani 1 1 d . . . O5 O 0.88986(17) 0.95072(10) 1.19345(9) 0.0253(5) Uani 1 1 d . . . O6 O 1.06189(16) 0.92659(10) 1.17817(9) 0.0251(5) Uani 1 1 d . A . C1 C 0.5795(3) 0.85754(16) 0.56252(15) 0.0304(7) Uani 1 1 d . . . C2 C 0.5378(3) 0.88576(17) 0.51716(15) 0.0339(8) Uani 1 1 d . . . C3 C 0.4364(3) 0.89244(19) 0.51809(17) 0.0407(9) Uani 1 1 d . . . H3 H 0.4074 0.9101 0.4873 0.049 Uiso 1 1 calc R . . C4 C 0.3740(3) 0.8745(2) 0.56222(17) 0.0443(9) Uani 1 1 d . . . H4 H 0.3046 0.8794 0.5607 0.053 Uiso 1 1 calc R . . C5 C 0.4155(3) 0.85008(19) 0.60679(16) 0.0372(8) Uani 1 1 d . . . H5 H 0.3755 0.8389 0.6375 0.045 Uiso 1 1 calc R . . C6 C 0.5183(3) 0.84108(17) 0.60808(15) 0.0319(8) Uani 1 1 d . . . C7 C 0.5561(3) 0.81768(16) 0.65751(15) 0.0297(7) Uani 1 1 d . . . H7 H 0.5117 0.8101 0.6871 0.036 Uiso 1 1 calc R . . C8 C 0.6805(2) 0.78428(15) 0.71819(14) 0.0246(7) Uani 1 1 d . . . C9 C 0.6269(3) 0.78041(15) 0.76780(14) 0.0246(7) Uani 1 1 d . . . H9 H 0.5651 0.7943 0.7695 0.029 Uiso 1 1 calc R . . C10 C 0.6669(2) 0.75564(14) 0.81407(13) 0.0221(6) Uani 1 1 d . A . C11 C 0.7579(2) 0.73480(14) 0.81120(14) 0.0239(7) Uani 1 1 d . . . C12 C 0.8117(2) 0.74029(15) 0.76324(14) 0.0250(7) Uani 1 1 d . . . H12 H 0.8742 0.7270 0.7619 0.030 Uiso 1 1 calc R . . C13 C 0.7726(2) 0.76594(15) 0.71627(14) 0.0250(7) Uani 1 1 d . . . C14 C 0.9047(3) 0.75991(17) 0.65625(16) 0.0329(8) Uani 1 1 d . . . H14 H 0.9317 0.7394 0.6853 0.039 Uiso 1 1 calc R . . C15 C 0.9619(3) 0.77027(18) 0.60840(17) 0.0365(8) Uani 1 1 d . . . C16 C 1.0567(3) 0.7513(2) 0.60910(18) 0.0452(10) Uani 1 1 d . . . H16 H 1.0778 0.7315 0.6404 0.054 Uiso 1 1 calc R . . C17 C 1.1170(3) 0.7613(2) 0.56560(19) 0.0506(11) Uani 1 1 d . . . H17 H 1.1810 0.7495 0.5664 0.061 Uiso 1 1 calc R . . C18 C 1.0829(3) 0.7894(2) 0.51912(17) 0.0435(9) Uani 1 1 d . . . H18 H 1.1256 0.7959 0.4886 0.052 Uiso 1 1 calc R . . C19 C 0.9923(3) 0.80816(18) 0.51480(15) 0.0334(8) Uani 1 1 d . . . C20 C 0.9277(3) 0.79798(17) 0.56062(15) 0.0310(7) Uani 1 1 d . . . C21 C 0.6037(3) 0.91003(19) 0.47042(16) 0.0390(9) Uani 1 1 d . . . C22 C 0.5415(3) 0.9363(2) 0.42490(17) 0.0485(10) Uani 1 1 d . . . H22A H 0.5860 0.9504 0.3953 0.073 Uiso 1 1 calc R . . H22B H 0.5228 0.9730 0.4465 0.073 Uiso 1 1 calc R . . H22C H 0.4762 0.9023 0.4038 0.073 Uiso 1 1 calc R . . C23 C 0.6369(4) 0.8557(2) 0.43448(17) 0.0490(10) Uani 1 1 d . . . H23A H 0.6784 0.8720 0.4045 0.073 Uiso 1 1 calc R . . H23B H 0.5729 0.8205 0.4136 0.073 Uiso 1 1 calc R . . H23C H 0.6806 0.8397 0.4622 0.073 Uiso 1 1 calc R . . C24 C 0.7041(3) 0.9652(2) 0.50389(18) 0.0456(10) Uani 1 1 d . . . H24A H 0.7463 0.9492 0.5325 0.068 Uiso 1 1 calc R . . H24B H 0.6826 1.0005 0.5262 0.068 Uiso 1 1 calc R . . H24C H 0.7472 0.9810 0.4744 0.068 Uiso 1 1 calc R . . C25 C 0.9591(3) 0.8378(2) 0.46237(15) 0.0420(9) Uani 1 1 d . . . C26 C 0.9439(3) 0.9035(2) 0.48596(17) 0.0447(10) Uani 1 1 d . . . H26A H 0.8916 0.8988 0.5133 0.067 Uiso 1 1 calc R . . H26B H 0.9180 0.9200 0.4517 0.067 Uiso 1 1 calc R . . H26C H 1.0123 0.9339 0.5080 0.067 Uiso 1 1 calc R . . C27 C 0.8551(3) 0.7896(2) 0.42318(17) 0.0525(11) Uani 1 1 d . . . H27A H 0.8014 0.7786 0.4490 0.079 Uiso 1 1 calc R . . H27B H 0.8700 0.7503 0.4040 0.079 Uiso 1 1 calc R . . H27C H 0.8282 0.8093 0.3917 0.079 Uiso 1 1 calc R . . C28 C 1.0442(3) 0.8487(2) 0.42124(18) 0.0532(11) Uani 1 1 d . . . H28A H 1.0189 0.8659 0.3873 0.080 Uiso 1 1 calc R . . H28B H 1.0568 0.8077 0.4055 0.080 Uiso 1 1 calc R . . H28C H 1.1110 0.8796 0.4448 0.080 Uiso 1 1 calc R . . N4 N 0.3920(2) 0.50732(13) 0.83992(13) 0.0311(6) Uani 1 1 d U A . O3 O 0.43956(18) 0.34794(11) 0.81205(11) 0.0344(5) Uani 1 1 d U A . N3 N 0.5598(4) 0.4736(3) 0.8421(3) 0.0282(12) Uani 0.70 1 d PDU A 1 O4 O 0.2752(4) 0.3810(4) 0.81734(18) 0.0392(16) Uani 0.70 1 d PDU A 1 C29 C 0.5301(4) 0.3349(2) 0.8189(2) 0.0309(10) Uani 0.70 1 d PDU A 1 C30 C 0.5302(4) 0.2691(2) 0.8019(3) 0.0363(11) Uani 0.70 1 d PDU A 1 C31 C 0.6240(4) 0.2555(2) 0.8137(3) 0.0414(11) Uani 0.70 1 d PDU A 1 H31 H 0.6237 0.2119 0.8024 0.050 Uiso 0.70 1 calc PR A 1 C32 C 0.7228(4) 0.3030(2) 0.8423(3) 0.0486(12) Uani 0.70 1 d PDU A 1 H32 H 0.7851 0.2910 0.8529 0.058 Uiso 0.70 1 calc PR A 1 C33 C 0.7253(4) 0.3662(2) 0.8538(3) 0.0435(11) Uani 0.70 1 d PDU A 1 H33 H 0.7911 0.3990 0.8700 0.052 Uiso 0.70 1 calc PR A 1 C34 C 0.6300(4) 0.3832(2) 0.8418(2) 0.0324(9) Uani 0.70 1 d PDU A 1 C35 C 0.6393(4) 0.4494(2) 0.8515(2) 0.0301(9) Uani 0.70 1 d PDU A 1 H35 H 0.7088 0.4791 0.8661 0.036 Uiso 0.70 1 calc PR A 1 C42 C 0.2982(5) 0.5168(4) 0.8360(3) 0.0377(15) Uani 0.70 1 d PDU A 1 H42 H 0.2968 0.5602 0.8407 0.045 Uiso 0.70 1 calc PR A 1 C43 C 0.1984(5) 0.4681(3) 0.8254(3) 0.0451(15) Uani 0.70 1 d PDU A 1 C44 C 0.1059(5) 0.4888(3) 0.8250(4) 0.0563(16) Uani 0.70 1 d PDU A 1 H44 H 0.1126 0.5335 0.8311 0.068 Uiso 0.70 1 calc PR A 1 C45 C 0.0069(5) 0.4443(3) 0.8157(4) 0.0619(16) Uani 0.70 1 d PDU A 1 H45 H -0.0558 0.4576 0.8148 0.074 Uiso 0.70 1 calc PR A 1 C46 C -0.0001(5) 0.3788(3) 0.8075(4) 0.0573(16) Uani 0.70 1 d PDU A 1 H46 H -0.0691 0.3486 0.8020 0.069 Uiso 0.70 1 calc PR A 1 C47 C 0.0860(5) 0.3551(3) 0.8069(4) 0.0485(15) Uani 0.70 1 d PDU A 1 C48 C 0.1911(5) 0.4014(3) 0.8181(8) 0.0435(16) Uani 0.70 1 d PDU A 1 C49 C 0.4258(5) 0.2151(4) 0.7709(3) 0.0367(12) Uani 0.70 1 d PDU A 1 C50 C 0.3756(6) 0.2336(3) 0.7157(3) 0.0514(15) Uani 0.70 1 d PDU A 1 H50A H 0.3150 0.1971 0.6929 0.077 Uiso 0.70 1 calc PR A 1 H50B H 0.4289 0.2447 0.6896 0.077 Uiso 0.70 1 calc PR A 1 H50C H 0.3507 0.2709 0.7289 0.077 Uiso 0.70 1 calc PR A 1 C51 C 0.3489(4) 0.2069(3) 0.8172(3) 0.0403(13) Uani 0.70 1 d PDU A 1 H51A H 0.3388 0.2486 0.8333 0.060 Uiso 0.70 1 calc PR A 1 H51B H 0.3795 0.1910 0.8506 0.060 Uiso 0.70 1 calc PR A 1 H51C H 0.2798 0.1759 0.7972 0.060 Uiso 0.70 1 calc PR A 1 C52 C 0.4468(11) 0.1504(5) 0.7495(4) 0.049(3) Uani 0.70 1 d PDU A 1 H52A H 0.3802 0.1183 0.7273 0.073 Uiso 0.70 1 calc PR A 1 H52B H 0.4736 0.1357 0.7847 0.073 Uiso 0.70 1 calc PR A 1 H52C H 0.5001 0.1560 0.7227 0.073 Uiso 0.70 1 calc PR A 1 C53 C 0.0700(7) 0.2827(4) 0.7954(4) 0.0488(17) Uani 0.70 1 d PDU A 1 C54 C -0.0479(7) 0.2425(6) 0.7891(5) 0.068(3) Uani 0.70 1 d PDU A 1 H54A H -0.0906 0.2505 0.7546 0.103 Uiso 0.70 1 calc PR A 1 H54B H -0.0746 0.2550 0.8263 0.103 Uiso 0.70 1 calc PR A 1 H54C H -0.0533 0.1966 0.7822 0.103 Uiso 0.70 1 calc PR A 1 C55 C 0.1088(10) 0.2647(7) 0.7366(4) 0.066(3) Uani 0.70 1 d PDU A 1 H55A H 0.0637 0.2726 0.7031 0.100 Uiso 0.70 1 calc PR A 1 H55B H 0.1046 0.2189 0.7289 0.100 Uiso 0.70 1 calc PR A 1 H55C H 0.1830 0.2910 0.7396 0.100 Uiso 0.70 1 calc PR A 1 C56 C 0.1330(8) 0.2661(5) 0.8484(4) 0.059(2) Uani 0.70 1 d PDU A 1 H56A H 0.1272 0.2201 0.8388 0.088 Uiso 0.70 1 calc PR A 1 H56B H 0.1036 0.2758 0.8853 0.088 Uiso 0.70 1 calc PR A 1 H56C H 0.2083 0.2918 0.8549 0.088 Uiso 0.70 1 calc PR A 1 N3' N 0.5558(11) 0.4717(6) 0.8263(10) 0.053(3) Uani 0.30 1 d PDU A 2 O4' O 0.2732(9) 0.3819(8) 0.8161 0.037(3) Uani 0.30 1 d PDU A 2 C29' C 0.5231(8) 0.3321(4) 0.7954(8) 0.0480(18) Uani 0.30 1 d PDU A 2 C30' C 0.5194(8) 0.2656(4) 0.7778(8) 0.053(2) Uani 0.30 1 d PDU A 2 C31' C 0.6071(9) 0.2519(4) 0.7602(9) 0.064(2) Uani 0.30 1 d PDU A 2 H31' H 0.6038 0.2079 0.7484 0.076 Uiso 0.30 1 calc PR A 2 C32' C 0.7037(9) 0.2999(5) 0.7585(9) 0.071(2) Uani 0.30 1 d PDU A 2 H32' H 0.7626 0.2881 0.7453 0.085 Uiso 0.30 1 calc PR A 2 C33' C 0.7090(8) 0.3632(4) 0.7766(8) 0.068(2) Uani 0.30 1 d PDU A 2 H33' H 0.7727 0.3961 0.7765 0.081 Uiso 0.30 1 calc PR A 2 C34' C 0.6199(8) 0.3802(4) 0.7954(8) 0.0574(19) Uani 0.30 1 d PDU A 2 C35' C 0.6318(9) 0.4466(4) 0.8130(9) 0.056(2) Uani 0.30 1 d PDU A 2 H35' H 0.7008 0.4757 0.8154 0.067 Uiso 0.30 1 calc PR A 2 C42' C 0.3038(10) 0.5183(8) 0.8513(9) 0.036(2) Uani 0.30 1 d PDU A 2 H42' H 0.3065 0.5620 0.8655 0.043 Uiso 0.30 1 calc PR A 2 C43' C 0.2040(9) 0.4705(6) 0.8442(8) 0.037(2) Uani 0.30 1 d PDU A 2 C44' C 0.1149(9) 0.4923(5) 0.8546(7) 0.038(2) Uani 0.30 1 d PDU A 2 H44' H 0.1232 0.5372 0.8643 0.045 Uiso 0.30 1 calc PR A 2 C45' C 0.0168(9) 0.4485(5) 0.8505(7) 0.042(2) Uani 0.30 1 d PDU A 2 H45' H -0.0438 0.4625 0.8567 0.050 Uiso 0.30 1 calc PR A 2 C46' C 0.0077(9) 0.3826(5) 0.8372(7) 0.042(2) Uani 0.30 1 d PDU A 2 H46' H -0.0596 0.3529 0.8374 0.051 Uiso 0.30 1 calc PR A 2 C47' C 0.0892(10) 0.3579(5) 0.8238(9) 0.041(2) Uani 0.30 1 d PDU A 2 C48' C 0.1921(10) 0.4034(6) 0.8250(18) 0.039(2) Uani 0.30 1 d PDU A 2 C49' C 0.4153(11) 0.2116(9) 0.7753(7) 0.051(3) Uani 0.30 1 d PDU A 2 C50' C 0.3233(12) 0.2185(7) 0.7326(7) 0.052(3) Uani 0.30 1 d PDU A 2 H50D H 0.2585 0.1832 0.7312 0.078 Uiso 0.30 1 calc PR A 2 H50E H 0.3411 0.2167 0.6918 0.078 Uiso 0.30 1 calc PR A 2 H50F H 0.3110 0.2599 0.7473 0.078 Uiso 0.30 1 calc PR A 2 C51' C 0.3901(15) 0.2153(9) 0.8404(7) 0.060(3) Uani 0.30 1 d PDU A 2 H51D H 0.4500 0.2105 0.8671 0.091 Uiso 0.30 1 calc PR A 2 H51E H 0.3250 0.1806 0.8399 0.091 Uiso 0.30 1 calc PR A 2 H51F H 0.3794 0.2571 0.8553 0.091 Uiso 0.30 1 calc PR A 2 C52' C 0.429(3) 0.1452(14) 0.7520(11) 0.049(4) Uani 0.30 1 d PDU A 2 H52D H 0.3609 0.1116 0.7480 0.074 Uiso 0.30 1 calc PR A 2 H52E H 0.4834 0.1379 0.7809 0.074 Uiso 0.30 1 calc PR A 2 H52F H 0.4517 0.1438 0.7124 0.074 Uiso 0.30 1 calc PR A 2 C53' C 0.0819(15) 0.2842(9) 0.8125(8) 0.043(3) Uani 0.30 1 d PDU A 2 C54' C -0.0351(14) 0.2462(13) 0.8124(10) 0.047(4) Uani 0.30 1 d PDU A 2 H54D H -0.0827 0.2573 0.7824 0.071 Uiso 0.30 1 calc PR A 2 H54E H -0.0527 0.2573 0.8527 0.071 Uiso 0.30 1 calc PR A 2 H54F H -0.0441 0.1998 0.8018 0.071 Uiso 0.30 1 calc PR A 2 C55' C 0.1155(18) 0.2585(13) 0.7541(8) 0.047(4) Uani 0.30 1 d PDU A 2 H55D H 0.1898 0.2827 0.7543 0.070 Uiso 0.30 1 calc PR A 2 H55E H 0.0691 0.2634 0.7195 0.070 Uiso 0.30 1 calc PR A 2 H55F H 0.1095 0.2127 0.7509 0.070 Uiso 0.30 1 calc PR A 2 C56' C 0.1494(17) 0.2745(12) 0.8680(9) 0.047(4) Uani 0.30 1 d PDU A 2 H56D H 0.1516 0.2298 0.8627 0.070 Uiso 0.30 1 d PR A 2 H56E H 0.1187 0.2852 0.9042 0.070 Uiso 0.30 1 d PR A 2 H56F H 0.2221 0.3037 0.8730 0.070 Uiso 0.30 1 d PR A 2 C36 C 0.5783(3) 0.54089(16) 0.84823(15) 0.0310(7) Uani 1 1 d . . . C37 C 0.6785(3) 0.58564(15) 0.85352(14) 0.0274(7) Uani 1 1 d . A . H37 H 0.7409 0.5722 0.8523 0.033 Uiso 1 1 calc R . . C38 C 0.6843(2) 0.64956(15) 0.86047(13) 0.0239(7) Uani 1 1 d . . . C39 C 0.5924(2) 0.66966(14) 0.86304(13) 0.0228(6) Uani 1 1 d . A . C40 C 0.4941(3) 0.62532(15) 0.85751(14) 0.0253(7) Uani 1 1 d . . . H40 H 0.4319 0.6388 0.8596 0.030 Uiso 1 1 calc R A . C41 C 0.4872(3) 0.56016(15) 0.84879(15) 0.0276(7) Uani 1 1 d . A . C57 C 0.6160(2) 0.74250(14) 0.86926(13) 0.0222(6) Uani 1 1 d . . . H57 H 0.5510 0.7572 0.8715 0.027 Uiso 1 1 calc R A . C59 C 0.7878(3) 1.00402(16) 1.25093(14) 0.0267(7) Uani 1 1 d . . . C60 C 0.6984(3) 1.02508(17) 1.24990(15) 0.0329(8) Uani 1 1 d . . . H60 H 0.6892 1.0498 1.2864 0.040 Uiso 1 1 calc R . . C61 C 0.6208(3) 1.01211(18) 1.19807(15) 0.0344(8) Uani 1 1 d . . . H61 H 0.5618 1.0288 1.1993 0.041 Uiso 1 1 calc R . . C62 C 0.6313(3) 0.97495(17) 1.14555(15) 0.0317(8) Uani 1 1 d . . . H62 H 0.5779 0.9645 1.1104 0.038 Uiso 1 1 calc R . . C63 C 0.7215(2) 0.95196(15) 1.14336(14) 0.0255(7) Uani 1 1 d . . . C64 C 0.8029(3) 0.96809(15) 1.19544(14) 0.0253(7) Uani 1 1 d . . . C65 C 0.7228(2) 0.91040(15) 1.08883(14) 0.0246(7) Uani 1 1 d . . . H65 H 0.6632 0.9003 1.0571 0.029 Uiso 1 1 calc R . . C66 C 0.7886(2) 0.84110(14) 1.02237(13) 0.0216(6) Uani 1 1 d . A . C67 C 0.6991(2) 0.81699(14) 0.97514(13) 0.0224(6) Uani 1 1 d . . . H67 H 0.6370 0.8303 0.9782 0.027 Uiso 1 1 calc R A . C68 C 0.7034(2) 0.77403(14) 0.92467(13) 0.0219(6) Uani 1 1 d . A . C69 C 0.7958(2) 0.75422(14) 0.92071(13) 0.0227(6) Uani 1 1 d . . . C70 C 0.8835(2) 0.77796(14) 0.96596(13) 0.0233(6) Uani 1 1 d . A . H70 H 0.9450 0.7641 0.9628 0.028 Uiso 1 1 calc R . . C71 C 0.8811(2) 0.82257(14) 1.01643(13) 0.0221(6) Uani 1 1 d . . . C72 C 1.0590(3) 0.84641(15) 1.06362(15) 0.0281(7) Uani 1 1 d . . . H72 H 1.0670 0.8209 1.0272 0.034 Uiso 1 1 calc R A . C73 C 1.1506(3) 0.87334(16) 1.11002(15) 0.0299(7) Uani 1 1 d . A . C74 C 1.2459(3) 0.85974(18) 1.09795(17) 0.0364(8) Uani 1 1 d . . . H74 H 1.2460 0.8336 1.0600 0.044 Uiso 1 1 calc R A . C75 C 1.3374(3) 0.88370(19) 1.14015(17) 0.0393(9) Uani 1 1 d . A . H75 H 1.4022 0.8763 1.1315 0.047 Uiso 1 1 calc R . . C76 C 1.3332(3) 0.91994(17) 1.19725(16) 0.0360(8) Uani 1 1 d . . . H76 H 1.3963 0.9351 1.2271 0.043 Uiso 1 1 calc R A . C77 C 1.2435(3) 0.93460(16) 1.21208(15) 0.0296(7) Uani 1 1 d . A . C78 C 1.1475(3) 0.91163(15) 1.16670(14) 0.0263(7) Uani 1 1 d . . . C79 C 0.8671(3) 1.01734(17) 1.31024(14) 0.0327(8) Uani 1 1 d . . . C80 C 0.8320(3) 1.0538(2) 1.36403(16) 0.0455(10) Uani 1 1 d . . . H80A H 0.8234 1.0942 1.3550 0.068 Uiso 1 1 calc R . . H80B H 0.8864 1.0636 1.4005 0.068 Uiso 1 1 calc R . . H80C H 0.7638 1.0270 1.3710 0.068 Uiso 1 1 calc R . . C81 C 0.9779(3) 1.0594(2) 1.30408(17) 0.0424(9) Uani 1 1 d . . . H81A H 0.9724 1.1003 1.2952 0.064 Uiso 1 1 calc R . . H81B H 1.0040 1.0366 1.2710 0.064 Uiso 1 1 calc R . . H81C H 1.0279 1.0679 1.3421 0.064 Uiso 1 1 calc R . . C82 C 0.8747(3) 0.9538(2) 1.32472(16) 0.0422(9) Uani 1 1 d . . . H82A H 0.9286 0.9625 1.3612 0.063 Uiso 1 1 calc R . . H82B H 0.8952 0.9290 1.2905 0.063 Uiso 1 1 calc R . . H82C H 0.8052 0.9289 1.3318 0.063 Uiso 1 1 calc R . . C83 C 1.2459(3) 0.97513(17) 1.27346(15) 0.0330(8) Uani 1 1 d . . . C84 C 1.1596(3) 0.9397(2) 1.30597(16) 0.0406(9) Uani 1 1 d . A . H84A H 1.0888 0.9315 1.2819 0.061 Uiso 1 1 calc R . . H84B H 1.1643 0.9664 1.3460 0.061 Uiso 1 1 calc R . . H84C H 1.1708 0.8985 1.3107 0.061 Uiso 1 1 calc R . . C85 C 1.2287(3) 1.03939(17) 1.26521(16) 0.0367(8) Uani 1 1 d . A . H85A H 1.2878 1.0636 1.2482 0.055 Uiso 1 1 calc R . . H85B H 1.2260 1.0648 1.3046 0.055 Uiso 1 1 calc R . . H85C H 1.1611 1.0308 1.2376 0.055 Uiso 1 1 calc R . . C86 C 1.3537(3) 0.9907(2) 1.31577(17) 0.0484(10) Uani 1 1 d . A . H86A H 1.3657 0.9504 1.3229 0.073 Uiso 1 1 calc R . . H86B H 1.3528 1.0180 1.3545 0.073 Uiso 1 1 calc R . . H86C H 1.4113 1.0135 1.2969 0.073 Uiso 1 1 calc R . . C87 C 0.7850(2) 0.70430(14) 0.86334(13) 0.0228(6) Uani 1 1 d . A . H87 H 0.8499 0.6896 0.8610 0.027 Uiso 1 1 calc R . . S1S S 1.03765(8) 0.95083(5) 0.90895(4) 0.0417(2) Uani 1 1 d D . . O1S O 1.0717(2) 0.92012(17) 0.95798(14) 0.0665(9) Uani 1 1 d D . . C1S C 1.0057(5) 0.8919(3) 0.8411(2) 0.0776(16) Uani 1 1 d D . . H1S1 H 1.0700 0.8806 0.8325 0.116 Uiso 1 1 calc R . . H1S2 H 0.9778 0.9088 0.8077 0.116 Uiso 1 1 calc R . . H1S3 H 0.9513 0.8533 0.8454 0.116 Uiso 1 1 calc R . . C2S C 0.9047(3) 0.9515(3) 0.9140(2) 0.0604(12) Uani 1 1 d D . . H2S1 H 0.8653 0.9114 0.9245 0.091 Uiso 1 1 calc R . . H2S2 H 0.8693 0.9550 0.8749 0.091 Uiso 1 1 calc R . . H2S3 H 0.9063 0.9885 0.9455 0.091 Uiso 1 1 calc R . . S1T S 0.56065(9) 0.96150(6) 0.94413(5) 0.0470(3) Uani 1 1 d U . . O1T O 0.5319(2) 0.90702(15) 0.97599(12) 0.0504(7) Uani 1 1 d U . . C1T C 0.6084(4) 0.9319(2) 0.87823(18) 0.0542(11) Uani 1 1 d U . . H1T1 H 0.6596 0.9092 0.8893 0.081 Uiso 1 1 calc R . . H1T2 H 0.6437 0.9682 0.8610 0.081 Uiso 1 1 calc R . . H1T3 H 0.5482 0.9021 0.8482 0.081 Uiso 1 1 calc R . . C2T C 0.6818(4) 1.0142(2) 0.9869(2) 0.0612(12) Uani 1 1 d U . . H2T1 H 0.6714 1.0298 1.0281 0.092 Uiso 1 1 calc R . . H2T2 H 0.7060 1.0510 0.9678 0.092 Uiso 1 1 calc R . . H2T3 H 0.7357 0.9914 0.9885 0.092 Uiso 1 1 calc R . . S1U S 0.30064(13) 0.78227(10) 0.74742(8) 0.0570(5) Uani 0.65 1 d PU B 1 O1U O 0.4106(4) 0.8304(3) 0.7652(3) 0.0524(13) Uani 0.65 1 d PU B 1 C1U C 0.2130(7) 0.8146(7) 0.7861(5) 0.083(3) Uani 0.65 1 d PU B 1 H1U1 H 0.2497 0.8378 0.8272 0.124 Uiso 0.65 1 calc PR B 1 H1U2 H 0.1503 0.7795 0.7884 0.124 Uiso 0.65 1 calc PR B 1 H1U3 H 0.1901 0.8444 0.7642 0.124 Uiso 0.65 1 calc PR B 1 C2U C 0.3028(10) 0.7199(6) 0.7811(6) 0.107(3) Uani 0.65 1 d PU B 1 H2U1 H 0.3463 0.6956 0.7617 0.160 Uiso 0.65 1 calc PR B 1 H2U2 H 0.2297 0.6915 0.7769 0.160 Uiso 0.65 1 calc PR B 1 H2U3 H 0.3335 0.7366 0.8243 0.160 Uiso 0.65 1 calc PR B 1 S1U' S 0.3283(5) 0.8153(4) 0.8074(3) 0.135(2) Uani 0.35 1 d PDU C 2 O1U' O 0.4149 0.8219(10) 0.7705(6) 0.133(5) Uani 0.35 1 d PDU C 2 C1U' C 0.2090(8) 0.8003(11) 0.7564(8) 0.112(10) Uani 0.35 1 d PDU C 2 H1U4 H 0.2032 0.7648 0.7223 0.168 Uiso 0.35 1 calc PR C 2 H1U5 H 0.2092 0.8392 0.7411 0.168 Uiso 0.35 1 calc PR C 2 H1U6 H 0.1480 0.7886 0.7773 0.168 Uiso 0.35 1 calc PR C 2 C2U' C 0.2991(15) 0.7376(7) 0.8243(10) 0.145(10) Uani 0.35 1 d PDU C 2 H2U4 H 0.2993 0.7415 0.8679 0.218 Uiso 0.35 1 calc PR C 2 H2U5 H 0.3533 0.7174 0.8125 0.218 Uiso 0.35 1 calc PR C 2 H2U6 H 0.2285 0.7109 0.8017 0.218 Uiso 0.35 1 calc PR C 2 S1Y S 0.4461(4) 0.6859(2) 1.02622(17) 0.0540(11) Uani 0.25 1 d PDU D 1 O1Y O 0.4285(7) 0.7153(4) 0.9729(3) 0.0388(19) Uani 0.25 1 d PDU D 1 C1Y C 0.3734(13) 0.6036(4) 0.9974(8) 0.108(9) Uani 0.25 1 d PDU D 1 H1Y1 H 0.3908 0.5867 0.9583 0.161 Uiso 0.25 1 d PR D 1 H1Y2 H 0.2960 0.5962 0.9932 0.161 Uiso 0.25 1 d PR D 1 H1Y3 H 0.3962 0.5814 1.0279 0.161 Uiso 0.25 1 d PR D 1 C2Y C 0.5738(8) 0.6732(8) 1.0289(6) 0.057(4) Uani 0.25 1 d PDU D 1 H2Y1 H 0.5663 0.6278 1.0288 0.085 Uiso 0.25 1 calc PR D 1 H2Y2 H 0.6217 0.7005 1.0659 0.085 Uiso 0.25 1 calc PR D 1 H2Y3 H 0.6037 0.6843 0.9933 0.085 Uiso 0.25 1 calc PR D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0254(2) 0.0293(2) 0.0262(2) 0.01024(17) 0.00641(17) 0.00907(18) Ni2 0.0244(2) 0.0182(2) 0.0490(3) 0.00799(19) 0.00543(19) 0.00337(17) Ni3 0.0193(2) 0.0215(2) 0.0225(2) 0.00481(16) -0.00037(15) 0.00493(16) N1 0.0259(14) 0.0227(14) 0.0270(13) 0.0082(11) 0.0049(11) 0.0068(11) N2 0.0240(14) 0.0277(14) 0.0280(13) 0.0093(11) 0.0062(11) 0.0075(12) N5 0.0192(13) 0.0227(13) 0.0236(13) 0.0076(10) 0.0001(10) 0.0043(11) N6 0.0174(13) 0.0221(13) 0.0272(13) 0.0071(11) -0.0015(10) 0.0043(11) O1 0.0345(14) 0.0409(14) 0.0313(12) 0.0165(11) 0.0097(10) 0.0169(11) O2 0.0280(12) 0.0373(13) 0.0288(12) 0.0094(10) 0.0080(10) 0.0095(10) O5 0.0242(12) 0.0276(12) 0.0239(11) 0.0051(9) 0.0007(9) 0.0090(10) O6 0.0185(11) 0.0269(12) 0.0270(11) 0.0031(9) -0.0018(9) 0.0063(9) C1 0.0317(19) 0.0303(18) 0.0299(17) 0.0060(14) 0.0039(14) 0.0114(15) C2 0.040(2) 0.036(2) 0.0291(17) 0.0077(15) 0.0052(15) 0.0170(16) C3 0.046(2) 0.048(2) 0.0373(19) 0.0154(17) 0.0078(17) 0.0254(19) C4 0.042(2) 0.059(3) 0.043(2) 0.0177(19) 0.0062(17) 0.027(2) C5 0.0319(19) 0.051(2) 0.0373(19) 0.0175(17) 0.0108(15) 0.0191(17) C6 0.0330(19) 0.0334(19) 0.0332(17) 0.0121(15) 0.0064(15) 0.0128(15) C7 0.0298(18) 0.0273(18) 0.0329(17) 0.0089(14) 0.0070(14) 0.0081(14) C8 0.0224(16) 0.0215(16) 0.0280(16) 0.0064(13) 0.0011(13) 0.0044(13) C9 0.0228(16) 0.0199(16) 0.0291(16) 0.0040(13) 0.0042(13) 0.0042(13) C10 0.0233(16) 0.0140(14) 0.0238(15) 0.0012(12) 0.0013(12) 0.0001(12) C11 0.0248(16) 0.0166(15) 0.0263(15) 0.0041(12) 0.0011(13) 0.0017(13) C12 0.0218(16) 0.0231(16) 0.0289(16) 0.0060(13) 0.0027(13) 0.0053(13) C13 0.0243(16) 0.0198(16) 0.0281(16) 0.0047(13) 0.0044(13) 0.0024(13) C14 0.0339(19) 0.0352(19) 0.0365(18) 0.0153(15) 0.0092(15) 0.0156(16) C15 0.034(2) 0.039(2) 0.042(2) 0.0144(16) 0.0123(16) 0.0142(17) C16 0.041(2) 0.065(3) 0.048(2) 0.028(2) 0.0172(18) 0.029(2) C17 0.040(2) 0.075(3) 0.054(2) 0.030(2) 0.0222(19) 0.030(2) C18 0.036(2) 0.060(3) 0.037(2) 0.0126(18) 0.0156(16) 0.0133(19) C19 0.0259(18) 0.042(2) 0.0303(17) 0.0085(15) 0.0076(14) 0.0061(15) C20 0.0281(18) 0.0324(19) 0.0312(17) 0.0059(14) 0.0033(14) 0.0083(15) C21 0.051(2) 0.047(2) 0.0302(18) 0.0170(16) 0.0100(16) 0.0263(19) C22 0.058(3) 0.060(3) 0.034(2) 0.0200(19) 0.0076(18) 0.023(2) C23 0.061(3) 0.064(3) 0.0308(19) 0.0158(19) 0.0132(18) 0.028(2) C24 0.046(2) 0.055(3) 0.043(2) 0.0257(19) 0.0094(18) 0.015(2) C25 0.031(2) 0.071(3) 0.0233(17) 0.0153(17) 0.0068(14) 0.0101(19) C26 0.042(2) 0.059(3) 0.040(2) 0.0272(19) 0.0078(17) 0.015(2) C27 0.034(2) 0.089(3) 0.0311(19) 0.007(2) 0.0048(16) 0.017(2) C28 0.042(2) 0.086(3) 0.038(2) 0.027(2) 0.0100(18) 0.021(2) N4 0.0242(13) 0.0193(13) 0.0468(16) 0.0105(12) 0.0032(12) 0.0010(11) O3 0.0307(12) 0.0206(11) 0.0515(14) 0.0092(10) 0.0058(11) 0.0069(9) N3 0.024(2) 0.019(2) 0.042(3) 0.0086(18) 0.0057(19) 0.0043(18) O4 0.026(2) 0.026(3) 0.065(3) 0.010(3) 0.012(3) 0.004(2) C29 0.0309(18) 0.0212(17) 0.044(2) 0.0105(17) 0.0091(18) 0.0096(15) C30 0.0329(19) 0.0237(18) 0.052(2) 0.0081(18) 0.0097(18) 0.0071(16) C31 0.033(2) 0.023(2) 0.071(3) 0.008(2) 0.015(2) 0.0110(17) C32 0.030(2) 0.030(2) 0.088(3) 0.013(2) 0.011(2) 0.0124(18) C33 0.027(2) 0.028(2) 0.074(3) 0.009(2) 0.009(2) 0.0077(17) C34 0.0276(18) 0.0235(17) 0.048(2) 0.0130(18) 0.0097(18) 0.0068(15) C35 0.026(2) 0.0239(19) 0.040(2) 0.0087(18) 0.0061(19) 0.0054(16) C42 0.027(2) 0.025(2) 0.057(3) 0.007(2) 0.003(2) 0.0050(18) C43 0.0288(19) 0.028(2) 0.074(3) 0.009(2) 0.006(2) 0.0044(18) C44 0.031(2) 0.034(2) 0.098(4) 0.005(3) 0.002(3) 0.0097(19) C45 0.031(2) 0.040(3) 0.106(4) 0.006(3) 0.003(3) 0.007(2) C46 0.029(2) 0.037(2) 0.098(4) 0.008(3) 0.003(3) 0.002(2) C47 0.029(2) 0.030(2) 0.081(4) 0.010(2) 0.011(2) -0.0002(18) C48 0.030(2) 0.028(2) 0.070(4) 0.011(2) 0.010(2) 0.0035(19) C49 0.037(2) 0.023(2) 0.047(2) 0.002(2) 0.003(2) 0.009(2) C50 0.060(4) 0.037(3) 0.048(3) -0.003(3) -0.007(3) 0.015(3) C51 0.027(3) 0.026(3) 0.064(3) 0.007(3) 0.004(2) 0.003(2) C52 0.046(6) 0.028(3) 0.062(4) -0.005(3) -0.002(4) 0.010(4) C53 0.035(3) 0.029(2) 0.077(4) 0.008(3) 0.013(3) 0.000(2) C54 0.044(4) 0.036(4) 0.109(7) 0.006(5) 0.013(4) -0.008(3) C55 0.073(5) 0.039(5) 0.066(5) -0.002(4) 0.017(4) -0.010(4) C56 0.058(5) 0.034(4) 0.075(5) 0.017(4) 0.010(4) -0.004(4) N3' 0.032(5) 0.019(5) 0.103(8) 0.012(5) 0.007(6) 0.006(4) O4' 0.025(5) 0.020(5) 0.063(7) 0.011(6) 0.004(6) 0.002(4) C29' 0.033(3) 0.022(3) 0.085(4) 0.005(3) 0.006(3) 0.008(2) C30' 0.036(3) 0.024(3) 0.096(5) 0.004(4) 0.002(3) 0.011(3) C31' 0.039(4) 0.030(4) 0.115(5) -0.002(4) 0.004(4) 0.014(3) C32' 0.040(4) 0.037(4) 0.125(6) -0.005(4) 0.009(4) 0.011(3) C33' 0.037(4) 0.034(4) 0.122(6) -0.001(4) 0.011(4) 0.007(3) C34' 0.033(3) 0.026(3) 0.106(5) 0.004(4) 0.008(4) 0.006(3) C35' 0.033(4) 0.024(3) 0.106(6) 0.010(5) 0.007(5) 0.005(3) C42' 0.026(3) 0.021(3) 0.055(4) 0.008(4) 0.004(3) 0.001(3) C43' 0.026(3) 0.021(3) 0.061(5) 0.009(4) 0.007(4) 0.001(3) C44' 0.026(3) 0.022(4) 0.061(5) 0.007(4) 0.006(4) 0.002(3) C45' 0.027(4) 0.026(4) 0.064(5) 0.005(4) 0.008(4) -0.001(3) C46' 0.027(4) 0.026(4) 0.067(5) 0.011(4) 0.005(4) -0.002(3) C47' 0.026(4) 0.022(3) 0.070(5) 0.014(4) 0.001(4) -0.001(3) C48' 0.026(4) 0.021(3) 0.066(5) 0.012(4) 0.004(4) 0.002(3) C49' 0.039(4) 0.022(4) 0.088(5) 0.008(4) 0.000(4) 0.009(3) C50' 0.034(5) 0.029(6) 0.087(7) 0.002(6) 0.001(6) 0.011(5) C51' 0.056(8) 0.031(7) 0.087(7) 0.006(6) 0.004(6) 0.010(6) C52' 0.038(8) 0.023(5) 0.087(9) 0.015(6) 0.009(7) 0.010(5) C53' 0.027(4) 0.022(4) 0.073(6) 0.015(5) -0.003(5) -0.001(3) C54' 0.028(5) 0.020(6) 0.084(9) 0.016(8) -0.006(6) -0.003(5) C55' 0.037(7) 0.025(6) 0.074(8) 0.015(6) -0.003(6) 0.002(5) C56' 0.032(6) 0.023(7) 0.074(8) 0.008(7) -0.011(7) 0.001(6) C36 0.0293(18) 0.0212(17) 0.0391(19) 0.0064(14) 0.0038(14) 0.0030(14) C37 0.0241(17) 0.0232(17) 0.0343(17) 0.0059(14) 0.0033(13) 0.0072(13) C38 0.0240(16) 0.0222(16) 0.0218(15) 0.0038(12) -0.0006(12) 0.0035(13) C39 0.0254(16) 0.0193(15) 0.0215(14) 0.0016(12) 0.0013(12) 0.0063(13) C40 0.0231(16) 0.0257(17) 0.0273(16) 0.0097(13) 0.0030(13) 0.0061(13) C41 0.0239(17) 0.0226(16) 0.0334(17) 0.0067(13) 0.0032(13) 0.0025(13) C57 0.0198(15) 0.0198(15) 0.0260(15) 0.0058(12) 0.0033(12) 0.0039(12) C59 0.0251(17) 0.0288(17) 0.0247(16) 0.0064(13) 0.0034(13) 0.0057(14) C60 0.0345(19) 0.039(2) 0.0256(16) 0.0046(14) 0.0076(14) 0.0115(16) C61 0.0327(19) 0.041(2) 0.0329(18) 0.0070(15) 0.0067(15) 0.0165(16) C62 0.0262(18) 0.040(2) 0.0283(17) 0.0081(15) 0.0004(14) 0.0104(15) C63 0.0238(16) 0.0283(17) 0.0256(16) 0.0098(13) 0.0034(13) 0.0078(14) C64 0.0253(17) 0.0225(16) 0.0264(16) 0.0093(13) 0.0033(13) 0.0025(13) C65 0.0215(16) 0.0274(17) 0.0256(15) 0.0099(13) 0.0028(12) 0.0065(13) C66 0.0225(16) 0.0172(15) 0.0235(15) 0.0066(12) 0.0026(12) 0.0026(12) C67 0.0193(15) 0.0206(15) 0.0268(15) 0.0083(12) 0.0026(12) 0.0037(12) C68 0.0217(16) 0.0186(15) 0.0243(15) 0.0090(12) 0.0030(12) 0.0018(12) C69 0.0208(16) 0.0205(15) 0.0274(15) 0.0100(12) 0.0059(12) 0.0036(12) C70 0.0190(15) 0.0216(16) 0.0286(16) 0.0061(13) 0.0042(12) 0.0048(12) C71 0.0191(15) 0.0182(15) 0.0258(15) 0.0051(12) -0.0004(12) 0.0022(12) C72 0.0283(18) 0.0245(17) 0.0302(17) 0.0031(13) 0.0018(14) 0.0088(14) C73 0.0224(17) 0.0272(18) 0.0387(18) 0.0064(14) -0.0014(14) 0.0085(14) C74 0.0288(19) 0.037(2) 0.041(2) 0.0019(16) 0.0010(15) 0.0135(16) C75 0.0270(19) 0.047(2) 0.045(2) 0.0056(17) -0.0011(16) 0.0183(17) C76 0.0275(19) 0.036(2) 0.0401(19) 0.0044(16) -0.0070(15) 0.0105(16) C77 0.0285(18) 0.0258(17) 0.0313(17) 0.0090(14) -0.0025(14) 0.0045(14) C78 0.0248(17) 0.0236(17) 0.0298(16) 0.0088(13) -0.0002(13) 0.0061(13) C79 0.0280(18) 0.042(2) 0.0245(16) 0.0009(15) 0.0030(14) 0.0089(16) C80 0.037(2) 0.068(3) 0.0277(18) 0.0017(18) 0.0060(16) 0.015(2) C81 0.033(2) 0.051(2) 0.0338(19) -0.0053(17) 0.0028(16) 0.0070(18) C82 0.044(2) 0.059(3) 0.0262(17) 0.0158(17) 0.0029(16) 0.018(2) C83 0.0251(18) 0.039(2) 0.0288(17) 0.0054(15) -0.0042(14) 0.0042(15) C84 0.035(2) 0.052(2) 0.0293(18) 0.0120(17) -0.0002(15) 0.0059(18) C85 0.034(2) 0.0308(19) 0.0382(19) 0.0002(15) 0.0057(16) 0.0031(16) C86 0.033(2) 0.062(3) 0.039(2) -0.0016(19) -0.0079(17) 0.0078(19) C87 0.0187(15) 0.0223(16) 0.0264(15) 0.0055(13) 0.0031(12) 0.0049(13) S1S 0.0352(5) 0.0371(5) 0.0475(5) 0.0129(4) 0.0062(4) 0.0006(4) O1S 0.0542(19) 0.091(3) 0.0571(19) 0.0342(18) 0.0005(15) 0.0185(18) C1S 0.108(5) 0.074(4) 0.052(3) 0.003(3) 0.001(3) 0.041(3) C2S 0.045(3) 0.091(4) 0.055(3) 0.029(3) 0.010(2) 0.027(3) S1T 0.0470(6) 0.0627(7) 0.0417(5) 0.0126(5) 0.0024(4) 0.0346(5) O1T 0.0364(15) 0.0725(19) 0.0476(15) 0.0209(14) 0.0054(12) 0.0210(14) C1T 0.062(3) 0.072(3) 0.044(2) 0.0203(19) 0.0140(19) 0.039(2) C2T 0.059(3) 0.069(3) 0.050(2) 0.022(2) 0.001(2) 0.009(2) S1U 0.0332(8) 0.0903(14) 0.0475(9) 0.0033(9) 0.0057(7) 0.0267(9) O1U 0.036(2) 0.071(3) 0.057(3) 0.010(2) 0.016(2) 0.028(2) C1U 0.062(5) 0.096(8) 0.103(8) 0.023(7) 0.059(5) 0.027(5) C2U 0.075(6) 0.103(5) 0.150(7) 0.048(5) 0.018(6) 0.027(4) S1U' 0.115(5) 0.202(7) 0.115(5) 0.066(5) 0.017(3) 0.072(5) O1U' 0.108(8) 0.186(11) 0.138(10) 0.059(8) 0.022(6) 0.082(8) C1U' 0.099(9) 0.095(18) 0.16(3) 0.071(18) 0.003(11) 0.032(13) C2U' 0.16(2) 0.245(18) 0.133(19) 0.12(2) 0.075(18) 0.160(19) S1Y 0.073(3) 0.052(2) 0.0324(19) 0.0048(17) 0.0176(19) 0.010(2) O1Y 0.051(5) 0.037(5) 0.035(4) 0.001(3) 0.033(4) 0.017(4) C1Y 0.123(14) 0.058(7) 0.109(18) 0.030(8) 0.048(14) -0.045(12) C2Y 0.080(8) 0.071(12) 0.021(7) 0.032(7) 0.007(7) 0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.841(2) . ? Ni1 O2 1.847(2) . ? Ni1 N1 1.851(3) . ? Ni1 N2 1.853(3) . ? Ni2 O4 1.828(6) . ? Ni2 N3' 1.841(15) . ? Ni2 O4' 1.842(14) . ? Ni2 O3 1.846(2) . ? Ni2 N3 1.852(6) . ? Ni2 N4 1.854(3) . ? Ni3 O5 1.846(2) . ? Ni3 N6 1.850(3) . ? Ni3 O6 1.856(2) . ? Ni3 N5 1.858(2) . ? N1 C7 1.318(4) . ? N1 C8 1.420(4) . ? N2 C14 1.296(4) . ? N2 C13 1.414(4) . ? N5 C65 1.302(4) . ? N5 C66 1.420(4) . ? N6 C72 1.290(4) . ? N6 C71 1.420(4) . ? O1 C1 1.312(4) . ? O2 C20 1.315(4) . ? O5 C64 1.310(4) . ? O6 C78 1.304(4) . ? C1 C6 1.423(5) . ? C1 C2 1.426(5) . ? C2 C3 1.389(5) . ? C2 C21 1.529(5) . ? C3 C4 1.414(5) . ? C4 C5 1.356(5) . ? C5 C6 1.424(5) . ? C6 C7 1.411(5) . ? C8 C13 1.387(4) . ? C8 C9 1.404(4) . ? C9 C10 1.383(4) . ? C10 C11 1.404(4) . ? C10 C57 1.527(4) . ? C11 C12 1.375(4) . ? C11 C87 1.515(4) . ? C12 C13 1.403(4) . ? C14 C15 1.412(5) . ? C15 C20 1.423(5) . ? C15 C16 1.425(5) . ? C16 C17 1.351(5) . ? C17 C18 1.406(5) . ? C18 C19 1.368(5) . ? C19 C20 1.432(5) . ? C19 C25 1.532(5) . ? C21 C23 1.525(5) . ? C21 C22 1.534(5) . ? C21 C24 1.540(6) . ? C25 C26 1.530(6) . ? C25 C28 1.541(5) . ? C25 C27 1.547(5) . ? N4 C42' 1.299(17) . ? N4 C42 1.308(8) . ? N4 C41 1.427(4) . ? O3 C29 1.303(5) . ? O3 C29' 1.322(9) . ? N3 C35 1.315(6) . ? N3 C36 1.416(6) . ? O4 C48 1.308(5) . ? C29 C34 1.421(6) . ? C29 C30 1.436(6) . ? C30 C31 1.362(7) . ? C30 C49 1.548(8) . ? C31 C32 1.427(7) . ? C32 C33 1.364(7) . ? C33 C34 1.419(7) . ? C34 C35 1.408(6) . ? C42 C43 1.417(5) . ? C43 C44 1.416(6) . ? C43 C48 1.427(6) . ? C44 C45 1.371(7) . ? C45 C46 1.401(7) . ? C46 C47 1.376(7) . ? C47 C48 1.445(6) . ? C47 C53 1.522(10) . ? C49 C50 1.521(6) . ? C49 C52 1.535(5) . ? C49 C51 1.547(7) . ? C53 C55 1.515(8) . ? C53 C56 1.537(8) . ? C53 C54 1.543(6) . ? N3' C35' 1.314(7) . ? N3' C36 1.455(13) . ? O4' C48' 1.309(6) . ? C29' C34' 1.421(7) . ? C29' C30' 1.437(7) . ? C30' C31' 1.361(7) . ? C30' C49' 1.540(19) . ? C31' C32' 1.426(8) . ? C32' C33' 1.366(8) . ? C33' C34' 1.419(8) . ? C34' C35' 1.409(7) . ? C42' C43' 1.417(6) . ? C43' C44' 1.417(7) . ? C43' C48' 1.428(7) . ? C44' C45' 1.371(7) . ? C45' C46' 1.400(8) . ? C46' C47' 1.376(7) . ? C47' C48' 1.445(7) . ? C47' C53' 1.58(2) . ? C49' C50' 1.520(8) . ? C49' C52' 1.535(7) . ? C49' C51' 1.548(8) . ? C53' C55' 1.515(8) . ? C53' C56' 1.539(9) . ? C53' C54' 1.542(7) . ? C36 C41 1.383(5) . ? C36 C37 1.396(5) . ? C37 C38 1.372(4) . ? C38 C39 1.406(4) . ? C38 C87 1.518(4) . ? C39 C40 1.372(4) . ? C39 C57 1.529(4) . ? C40 C41 1.393(5) . ? C57 C68 1.522(4) . ? C59 C60 1.382(5) . ? C59 C64 1.434(4) . ? C59 C79 1.536(4) . ? C60 C61 1.399(5) . ? C61 C62 1.370(5) . ? C62 C63 1.420(5) . ? C63 C65 1.412(4) . ? C63 C64 1.424(4) . ? C66 C71 1.405(4) . ? C66 C67 1.411(4) . ? C67 C68 1.372(4) . ? C68 C69 1.412(4) . ? C69 C70 1.368(4) . ? C69 C87 1.517(4) . ? C70 C71 1.384(4) . ? C72 C73 1.420(4) . ? C73 C74 1.417(5) . ? C73 C78 1.424(5) . ? C74 C75 1.364(5) . ? C75 C76 1.416(5) . ? C76 C77 1.375(5) . ? C77 C78 1.444(4) . ? C77 C83 1.512(5) . ? C79 C82 1.522(5) . ? C79 C80 1.534(5) . ? C79 C81 1.541(5) . ? C83 C85 1.536(5) . ? C83 C86 1.538(5) . ? C83 C84 1.540(5) . ? S1S O1S 1.489(3) . ? S1S C1S 1.758(5) . ? S1S C2S 1.778(4) . ? S1T O1T 1.495(3) . ? S1T C2T 1.754(5) . ? S1T C1T 1.782(4) . ? S1U O1U 1.505(5) . ? S1U C2U 1.693(11) . ? S1U C1U 1.759(10) . ? S1U' O1U' 1.486(6) . ? S1U' C1U' 1.756(7) . ? S1U' C2U' 1.772(6) . ? S1Y O1Y 1.495(5) . ? S1Y C1Y 1.770(7) . ? S1Y C2Y 1.780(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O2 85.64(10) . . ? O1 Ni1 N1 94.37(11) . . ? O2 Ni1 N1 178.33(11) . . ? O1 Ni1 N2 178.12(12) . . ? O2 Ni1 N2 94.35(11) . . ? N1 Ni1 N2 85.69(11) . . ? O4 Ni2 N3' 172.9(7) . . ? O4 Ni2 O4' 1.4(6) . . ? N3' Ni2 O4' 172.0(7) . . ? O4 Ni2 O3 85.0(2) . . ? N3' Ni2 O3 93.4(3) . . ? O4' Ni2 O3 86.0(5) . . ? O4 Ni2 N3 176.0(3) . . ? N3' Ni2 N3 10.9(8) . . ? O4' Ni2 N3 177.1(2) . . ? O3 Ni2 N3 94.26(17) . . ? O4 Ni2 N4 95.0(2) . . ? N3' Ni2 N4 86.4(3) . . ? O4' Ni2 N4 94.0(5) . . ? O3 Ni2 N4 178.60(12) . . ? N3 Ni2 N4 85.80(17) . . ? O5 Ni3 N6 177.47(10) . . ? O5 Ni3 O6 85.82(9) . . ? N6 Ni3 O6 94.07(10) . . ? O5 Ni3 N5 94.57(10) . . ? N6 Ni3 N5 85.68(11) . . ? O6 Ni3 N5 176.67(10) . . ? C7 N1 C8 120.1(3) . . ? C7 N1 Ni1 126.2(2) . . ? C8 N1 Ni1 113.6(2) . . ? C14 N2 C13 120.8(3) . . ? C14 N2 Ni1 125.9(2) . . ? C13 N2 Ni1 113.3(2) . . ? C65 N5 C66 120.9(3) . . ? C65 N5 Ni3 125.3(2) . . ? C66 N5 Ni3 113.75(19) . . ? C72 N6 C71 119.4(3) . . ? C72 N6 Ni3 126.6(2) . . ? C71 N6 Ni3 114.0(2) . . ? C1 O1 Ni1 129.3(2) . . ? C20 O2 Ni1 129.7(2) . . ? C64 O5 Ni3 129.16(19) . . ? C78 O6 Ni3 129.20(19) . . ? O1 C1 C6 121.7(3) . . ? O1 C1 C2 119.6(3) . . ? C6 C1 C2 118.7(3) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C21 121.0(3) . . ? C1 C2 C21 121.2(3) . . ? C2 C3 C4 123.8(3) . . ? C5 C4 C3 118.5(4) . . ? C4 C5 C6 120.7(3) . . ? C7 C6 C1 123.0(3) . . ? C7 C6 C5 116.4(3) . . ? C1 C6 C5 120.6(3) . . ? N1 C7 C6 124.7(3) . . ? C13 C8 C9 121.4(3) . . ? C13 C8 N1 113.0(3) . . ? C9 C8 N1 125.7(3) . . ? C10 C9 C8 117.8(3) . . ? C9 C10 C11 120.9(3) . . ? C9 C10 C57 126.0(3) . . ? C11 C10 C57 112.9(3) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 C87 125.4(3) . . ? C10 C11 C87 113.6(3) . . ? C11 C12 C13 118.7(3) . . ? C8 C13 C12 120.2(3) . . ? C8 C13 N2 114.1(3) . . ? C12 C13 N2 125.8(3) . . ? N2 C14 C15 126.3(3) . . ? C14 C15 C20 122.5(3) . . ? C14 C15 C16 117.2(3) . . ? C20 C15 C16 120.2(3) . . ? C17 C16 C15 120.5(4) . . ? C16 C17 C18 118.6(4) . . ? C19 C18 C17 124.5(3) . . ? C18 C19 C20 117.6(3) . . ? C18 C19 C25 121.7(3) . . ? C20 C19 C25 120.7(3) . . ? O2 C20 C15 121.2(3) . . ? O2 C20 C19 120.2(3) . . ? C15 C20 C19 118.6(3) . . ? C23 C21 C2 110.6(3) . . ? C23 C21 C22 107.6(3) . . ? C2 C21 C22 112.2(3) . . ? C23 C21 C24 109.6(3) . . ? C2 C21 C24 108.7(3) . . ? C22 C21 C24 108.0(3) . . ? C26 C25 C19 111.2(3) . . ? C26 C25 C28 107.0(3) . . ? C19 C25 C28 111.8(3) . . ? C26 C25 C27 111.4(3) . . ? C19 C25 C27 107.8(3) . . ? C28 C25 C27 107.6(3) . . ? C42' N4 C42 15.0(11) . . ? C42' N4 C41 119.5(7) . . ? C42 N4 C41 120.8(4) . . ? C42' N4 Ni2 126.0(7) . . ? C42 N4 Ni2 125.5(4) . . ? C41 N4 Ni2 113.4(2) . . ? C29 O3 C29' 22.9(8) . . ? C29 O3 Ni2 128.5(3) . . ? C29' O3 Ni2 130.0(4) . . ? C35 N3 C36 121.2(5) . . ? C35 N3 Ni2 125.6(4) . . ? C36 N3 Ni2 113.0(3) . . ? C48 O4 Ni2 129.2(4) . . ? O3 C29 C34 123.0(4) . . ? O3 C29 C30 119.0(4) . . ? C34 C29 C30 118.0(4) . . ? C31 C30 C29 118.4(4) . . ? C31 C30 C49 120.9(5) . . ? C29 C30 C49 120.6(4) . . ? C30 C31 C32 123.7(5) . . ? C33 C32 C31 118.2(5) . . ? C32 C33 C34 120.3(5) . . ? C35 C34 C33 117.2(4) . . ? C35 C34 C29 121.8(4) . . ? C33 C34 C29 120.9(4) . . ? N3 C35 C34 125.3(4) . . ? N4 C42 C43 125.8(5) . . ? C44 C43 C42 116.9(4) . . ? C44 C43 C48 121.2(4) . . ? C42 C43 C48 121.8(4) . . ? C45 C44 C43 120.0(5) . . ? C44 C45 C46 118.6(5) . . ? C47 C46 C45 124.7(5) . . ? C46 C47 C48 117.4(4) . . ? C46 C47 C53 120.8(5) . . ? C48 C47 C53 121.7(5) . . ? O4 C48 C43 122.3(4) . . ? O4 C48 C47 119.5(4) . . ? C43 C48 C47 118.0(5) . . ? C50 C49 C52 108.0(4) . . ? C50 C49 C51 110.5(5) . . ? C52 C49 C51 108.8(5) . . ? C50 C49 C30 109.3(6) . . ? C52 C49 C30 111.7(6) . . ? C51 C49 C30 108.5(5) . . ? C55 C53 C47 106.8(7) . . ? C55 C53 C56 111.2(5) . . ? C47 C53 C56 110.4(6) . . ? C55 C53 C54 108.8(5) . . ? C47 C53 C54 113.0(7) . . ? C56 C53 C54 106.8(5) . . ? C35' N3' C36 121.4(10) . . ? C35' N3' Ni2 126.7(9) . . ? C36 N3' Ni2 111.7(6) . . ? C48' O4' Ni2 128.9(9) . . ? O3 C29' C34' 121.1(7) . . ? O3 C29' C30' 121.0(7) . . ? C34' C29' C30' 117.9(6) . . ? C31' C30' C29' 118.6(6) . . ? C31' C30' C49' 121.4(9) . . ? C29' C30' C49' 119.9(9) . . ? C30' C31' C32' 123.9(7) . . ? C33' C32' C31' 118.0(7) . . ? C32' C33' C34' 120.5(7) . . ? C35' C34' C33' 116.9(6) . . ? C35' C34' C29' 122.0(6) . . ? C33' C34' C29' 121.1(6) . . ? N3' C35' C34' 125.8(8) . . ? N4 C42' C43' 125.3(11) . . ? C42' C43' C44' 117.0(6) . . ? C42' C43' C48' 121.8(6) . . ? C44' C43' C48' 121.1(5) . . ? C45' C44' C43' 120.0(6) . . ? C44' C45' C46' 118.6(6) . . ? C47' C46' C45' 124.6(6) . . ? C46' C47' C48' 117.5(6) . . ? C46' C47' C53' 125.0(10) . . ? C48' C47' C53' 117.3(10) . . ? O4' C48' C43' 122.3(6) . . ? O4' C48' C47' 119.2(6) . . ? C43' C48' C47' 117.8(6) . . ? C50' C49' C52' 107.8(7) . . ? C50' C49' C30' 111.1(13) . . ? C52' C49' C30' 110.3(16) . . ? C50' C49' C51' 110.6(8) . . ? C52' C49' C51' 108.7(7) . . ? C30' C49' C51' 108.2(13) . . ? C55' C53' C56' 111.2(7) . . ? C55' C53' C54' 109.6(7) . . ? C56' C53' C54' 106.5(7) . . ? C55' C53' C47' 114.7(14) . . ? C56' C53' C47' 107.3(13) . . ? C54' C53' C47' 107.2(14) . . ? C41 C36 C37 121.1(3) . . ? C41 C36 N3 114.3(3) . . ? C37 C36 N3 124.6(4) . . ? C41 C36 N3' 113.3(6) . . ? C37 C36 N3' 123.7(6) . . ? N3 C36 N3' 13.9(11) . . ? C38 C37 C36 117.9(3) . . ? C37 C38 C39 121.2(3) . . ? C37 C38 C87 125.2(3) . . ? C39 C38 C87 113.6(3) . . ? C40 C39 C38 120.5(3) . . ? C40 C39 C57 126.7(3) . . ? C38 C39 C57 112.7(3) . . ? C39 C40 C41 118.7(3) . . ? C36 C41 C40 120.5(3) . . ? C36 C41 N4 112.9(3) . . ? C40 C41 N4 126.6(3) . . ? C68 C57 C10 106.5(2) . . ? C68 C57 C39 106.3(2) . . ? C10 C57 C39 103.8(2) . . ? C60 C59 C64 118.1(3) . . ? C60 C59 C79 120.8(3) . . ? C64 C59 C79 121.1(3) . . ? C59 C60 C61 123.7(3) . . ? C62 C61 C60 118.9(3) . . ? C61 C62 C63 120.4(3) . . ? C65 C63 C62 116.9(3) . . ? C65 C63 C64 122.6(3) . . ? C62 C63 C64 120.4(3) . . ? O5 C64 C63 121.5(3) . . ? O5 C64 C59 120.1(3) . . ? C63 C64 C59 118.4(3) . . ? N5 C65 C63 125.9(3) . . ? C71 C66 C67 120.0(3) . . ? C71 C66 N5 113.2(3) . . ? C67 C66 N5 126.8(3) . . ? C68 C67 C66 118.8(3) . . ? C67 C68 C69 120.2(3) . . ? C67 C68 C57 126.9(3) . . ? C69 C68 C57 112.9(3) . . ? C70 C69 C68 121.4(3) . . ? C70 C69 C87 125.4(3) . . ? C68 C69 C87 113.2(3) . . ? C69 C70 C71 119.0(3) . . ? C70 C71 C66 120.6(3) . . ? C70 C71 N6 126.3(3) . . ? C66 C71 N6 113.1(3) . . ? N6 C72 C73 125.9(3) . . ? C74 C73 C72 117.1(3) . . ? C74 C73 C78 121.0(3) . . ? C72 C73 C78 121.9(3) . . ? C75 C74 C73 120.8(3) . . ? C74 C75 C76 118.1(3) . . ? C77 C76 C75 124.0(3) . . ? C76 C77 C78 118.1(3) . . ? C76 C77 C83 121.1(3) . . ? C78 C77 C83 120.8(3) . . ? O6 C78 C73 122.2(3) . . ? O6 C78 C77 120.0(3) . . ? C73 C78 C77 117.9(3) . . ? C82 C79 C80 107.9(3) . . ? C82 C79 C59 109.7(3) . . ? C80 C79 C59 111.8(3) . . ? C82 C79 C81 110.0(3) . . ? C80 C79 C81 107.4(3) . . ? C59 C79 C81 109.9(3) . . ? C77 C83 C85 109.2(3) . . ? C77 C83 C86 112.0(3) . . ? C85 C83 C86 107.8(3) . . ? C77 C83 C84 111.2(3) . . ? C85 C83 C84 110.0(3) . . ? C86 C83 C84 106.6(3) . . ? C11 C87 C69 105.8(2) . . ? C11 C87 C38 104.2(2) . . ? C69 C87 C38 106.7(2) . . ? O1S S1S C1S 106.3(2) . . ? O1S S1S C2S 106.7(2) . . ? C1S S1S C2S 96.7(3) . . ? O1T S1T C2T 105.31(19) . . ? O1T S1T C1T 106.45(19) . . ? C2T S1T C1T 99.1(2) . . ? O1U S1U C2U 107.1(5) . . ? O1U S1U C1U 108.2(5) . . ? C2U S1U C1U 100.9(6) . . ? O1U' S1U' C1U' 106.3(6) . . ? O1U' S1U' C2U' 108.0(6) . . ? C1U' S1U' C2U' 96.5(6) . . ? O1Y S1Y C1Y 102.5(5) . . ? O1Y S1Y C2Y 107.2(5) . . ? C1Y S1Y C2Y 94.8(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 N1 C7 8.6(3) . . . . ? O2 Ni1 N1 C7 -82(4) . . . . ? N2 Ni1 N1 C7 -173.3(3) . . . . ? O1 Ni1 N1 C8 -173.2(2) . . . . ? O2 Ni1 N1 C8 96(4) . . . . ? N2 Ni1 N1 C8 4.9(2) . . . . ? O1 Ni1 N2 C14 -92(3) . . . . ? O2 Ni1 N2 C14 -1.8(3) . . . . ? N1 Ni1 N2 C14 176.5(3) . . . . ? O1 Ni1 N2 C13 89(3) . . . . ? O2 Ni1 N2 C13 178.8(2) . . . . ? N1 Ni1 N2 C13 -2.9(2) . . . . ? O5 Ni3 N5 C65 10.0(3) . . . . ? N6 Ni3 N5 C65 -172.5(3) . . . . ? O6 Ni3 N5 C65 -86.7(18) . . . . ? O5 Ni3 N5 C66 -173.6(2) . . . . ? N6 Ni3 N5 C66 3.9(2) . . . . ? O6 Ni3 N5 C66 89.7(18) . . . . ? O5 Ni3 N6 C72 -92(2) . . . . ? O6 Ni3 N6 C72 -4.4(3) . . . . ? N5 Ni3 N6 C72 172.2(3) . . . . ? O5 Ni3 N6 C71 91(2) . . . . ? O6 Ni3 N6 C71 178.1(2) . . . . ? N5 Ni3 N6 C71 -5.2(2) . . . . ? O2 Ni1 O1 C1 169.5(3) . . . . ? N1 Ni1 O1 C1 -8.8(3) . . . . ? N2 Ni1 O1 C1 -101(3) . . . . ? O1 Ni1 O2 C20 175.7(3) . . . . ? N1 Ni1 O2 C20 -94(4) . . . . ? N2 Ni1 O2 C20 -2.4(3) . . . . ? N6 Ni3 O5 C64 -102(2) . . . . ? O6 Ni3 O5 C64 170.2(3) . . . . ? N5 Ni3 O5 C64 -6.4(3) . . . . ? O5 Ni3 O6 C78 179.7(3) . . . . ? N6 Ni3 O6 C78 2.2(3) . . . . ? N5 Ni3 O6 C78 -83.4(18) . . . . ? Ni1 O1 C1 C6 4.2(5) . . . . ? Ni1 O1 C1 C2 -177.3(2) . . . . ? O1 C1 C2 C3 178.0(3) . . . . ? C6 C1 C2 C3 -3.4(5) . . . . ? O1 C1 C2 C21 -4.1(5) . . . . ? C6 C1 C2 C21 174.5(3) . . . . ? C1 C2 C3 C4 1.8(6) . . . . ? C21 C2 C3 C4 -176.2(4) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 -1.7(6) . . . . ? O1 C1 C6 C7 3.6(5) . . . . ? C2 C1 C6 C7 -174.9(3) . . . . ? O1 C1 C6 C5 -178.8(3) . . . . ? C2 C1 C6 C5 2.7(5) . . . . ? C4 C5 C6 C7 177.7(4) . . . . ? C4 C5 C6 C1 0.0(6) . . . . ? C8 N1 C7 C6 177.7(3) . . . . ? Ni1 N1 C7 C6 -4.3(5) . . . . ? C1 C6 C7 N1 -3.5(6) . . . . ? C5 C6 C7 N1 178.8(3) . . . . ? C7 N1 C8 C13 172.4(3) . . . . ? Ni1 N1 C8 C13 -5.9(3) . . . . ? C7 N1 C8 C9 -6.7(5) . . . . ? Ni1 N1 C8 C9 175.0(2) . . . . ? C13 C8 C9 C10 -2.1(4) . . . . ? N1 C8 C9 C10 177.0(3) . . . . ? C8 C9 C10 C11 -0.3(4) . . . . ? C8 C9 C10 C57 -174.9(3) . . . . ? C9 C10 C11 C12 2.1(4) . . . . ? C57 C10 C11 C12 177.3(3) . . . . ? C9 C10 C11 C87 -175.4(3) . . . . ? C57 C10 C11 C87 -0.2(4) . . . . ? C10 C11 C12 C13 -1.4(4) . . . . ? C87 C11 C12 C13 175.8(3) . . . . ? C9 C8 C13 C12 2.8(5) . . . . ? N1 C8 C13 C12 -176.4(3) . . . . ? C9 C8 C13 N2 -177.3(3) . . . . ? N1 C8 C13 N2 3.5(4) . . . . ? C11 C12 C13 C8 -1.0(5) . . . . ? C11 C12 C13 N2 179.1(3) . . . . ? C14 N2 C13 C8 -179.2(3) . . . . ? Ni1 N2 C13 C8 0.3(3) . . . . ? C14 N2 C13 C12 0.8(5) . . . . ? Ni1 N2 C13 C12 -179.7(2) . . . . ? C13 N2 C14 C15 -176.3(3) . . . . ? Ni1 N2 C14 C15 4.3(5) . . . . ? N2 C14 C15 C20 -2.7(6) . . . . ? N2 C14 C15 C16 177.8(4) . . . . ? C14 C15 C16 C17 -178.3(4) . . . . ? C20 C15 C16 C17 2.1(6) . . . . ? C15 C16 C17 C18 -1.3(7) . . . . ? C16 C17 C18 C19 0.5(7) . . . . ? C17 C18 C19 C20 -0.4(6) . . . . ? C17 C18 C19 C25 -179.2(4) . . . . ? Ni1 O2 C20 C15 4.2(5) . . . . ? Ni1 O2 C20 C19 -176.0(2) . . . . ? C14 C15 C20 O2 -1.7(6) . . . . ? C16 C15 C20 O2 177.8(3) . . . . ? C14 C15 C20 C19 178.5(3) . . . . ? C16 C15 C20 C19 -2.0(5) . . . . ? C18 C19 C20 O2 -178.7(3) . . . . ? C25 C19 C20 O2 0.2(5) . . . . ? C18 C19 C20 C15 1.1(5) . . . . ? C25 C19 C20 C15 -180.0(3) . . . . ? C3 C2 C21 C23 -124.3(4) . . . . ? C1 C2 C21 C23 57.9(5) . . . . ? C3 C2 C21 C22 -4.1(5) . . . . ? C1 C2 C21 C22 178.1(3) . . . . ? C3 C2 C21 C24 115.2(4) . . . . ? C1 C2 C21 C24 -62.6(4) . . . . ? C18 C19 C25 C26 -124.8(4) . . . . ? C20 C19 C25 C26 56.4(4) . . . . ? C18 C19 C25 C28 -5.3(5) . . . . ? C20 C19 C25 C28 175.9(3) . . . . ? C18 C19 C25 C27 112.8(4) . . . . ? C20 C19 C25 C27 -66.1(4) . . . . ? O4 Ni2 N4 C42' 13.4(11) . . . . ? N3' Ni2 N4 C42' -173.6(13) . . . . ? O4' Ni2 N4 C42' 14.3(11) . . . . ? O3 Ni2 N4 C42' 105(5) . . . . ? N3 Ni2 N4 C42' -162.8(11) . . . . ? O4 Ni2 N4 C42 -5.2(5) . . . . ? N3' Ni2 N4 C42 167.9(9) . . . . ? O4' Ni2 N4 C42 -4.2(5) . . . . ? O3 Ni2 N4 C42 86(5) . . . . ? N3 Ni2 N4 C42 178.7(5) . . . . ? O4 Ni2 N4 C41 -178.8(3) . . . . ? N3' Ni2 N4 C41 -5.8(7) . . . . ? O4' Ni2 N4 C41 -177.8(2) . . . . ? O3 Ni2 N4 C41 -87(5) . . . . ? N3 Ni2 N4 C41 5.1(3) . . . . ? O4 Ni2 O3 C29 -168.7(4) . . . . ? N3' Ni2 O3 C29 18.2(8) . . . . ? O4' Ni2 O3 C29 -169.7(4) . . . . ? N3 Ni2 O3 C29 7.4(4) . . . . ? N4 Ni2 O3 C29 100(5) . . . . ? O4 Ni2 O3 C29' 161.6(11) . . . . ? N3' Ni2 O3 C29' -11.4(13) . . . . ? O4' Ni2 O3 C29' 160.6(11) . . . . ? N3 Ni2 O3 C29' -22.3(11) . . . . ? N4 Ni2 O3 C29' 70(5) . . . . ? O4 Ni2 N3 C35 65(4) . . . . ? N3' Ni2 N3 C35 -99(2) . . . . ? O4' Ni2 N3 C35 81(10) . . . . ? O3 Ni2 N3 C35 -13.5(6) . . . . ? N4 Ni2 N3 C35 167.9(6) . . . . ? O4 Ni2 N3 C36 -109(4) . . . . ? N3' Ni2 N3 C36 86(2) . . . . ? O4' Ni2 N3 C36 -93(10) . . . . ? O3 Ni2 N3 C36 171.9(4) . . . . ? N4 Ni2 N3 C36 -6.7(4) . . . . ? N3' Ni2 O4 C48 -100(3) . . . . ? O4' Ni2 O4 C48 -42(18) . . . . ? O3 Ni2 O4 C48 -176.7(11) . . . . ? N3 Ni2 O4 C48 104(4) . . . . ? N4 Ni2 O4 C48 1.9(11) . . . . ? C29' O3 C29 C34 104.9(13) . . . . ? Ni2 O3 C29 C34 1.7(7) . . . . ? C29' O3 C29 C30 -74.1(12) . . . . ? Ni2 O3 C29 C30 -177.3(3) . . . . ? O3 C29 C30 C31 -174.9(5) . . . . ? C34 C29 C30 C31 6.1(8) . . . . ? O3 C29 C30 C49 5.0(8) . . . . ? C34 C29 C30 C49 -174.0(5) . . . . ? C29 C30 C31 C32 0.0(9) . . . . ? C49 C30 C31 C32 -179.9(6) . . . . ? C30 C31 C32 C33 -5.5(10) . . . . ? C31 C32 C33 C34 4.6(9) . . . . ? C32 C33 C34 C35 -176.4(6) . . . . ? C32 C33 C34 C29 1.5(9) . . . . ? O3 C29 C34 C35 -8.1(8) . . . . ? C30 C29 C34 C35 170.8(5) . . . . ? O3 C29 C34 C33 174.1(5) . . . . ? C30 C29 C34 C33 -7.0(8) . . . . ? C36 N3 C35 C34 -174.5(5) . . . . ? Ni2 N3 C35 C34 11.3(9) . . . . ? C33 C34 C35 N3 179.2(6) . . . . ? C29 C34 C35 N3 1.3(9) . . . . ? C42' N4 C42 C43 -93(4) . . . . ? C41 N4 C42 C43 177.9(5) . . . . ? Ni2 N4 C42 C43 4.7(9) . . . . ? N4 C42 C43 C44 177.8(7) . . . . ? N4 C42 C43 C48 0.5(13) . . . . ? C42 C43 C44 C45 -179.2(7) . . . . ? C48 C43 C44 C45 -1.9(13) . . . . ? C43 C44 C45 C46 0.8(12) . . . . ? C44 C45 C46 C47 -1.3(13) . . . . ? C45 C46 C47 C48 2.7(14) . . . . ? C45 C46 C47 C53 -177.7(8) . . . . ? Ni2 O4 C48 C43 2(2) . . . . ? Ni2 O4 C48 C47 177.5(7) . . . . ? C44 C43 C48 O4 178.9(11) . . . . ? C42 C43 C48 O4 -4.0(19) . . . . ? C44 C43 C48 C47 3.3(17) . . . . ? C42 C43 C48 C47 -179.5(9) . . . . ? C46 C47 C48 O4 -179.3(11) . . . . ? C53 C47 C48 O4 1.2(18) . . . . ? C46 C47 C48 C43 -3.6(16) . . . . ? C53 C47 C48 C43 176.8(9) . . . . ? C31 C30 C49 C50 -126.8(6) . . . . ? C29 C30 C49 C50 53.3(7) . . . . ? C31 C30 C49 C52 -7.4(8) . . . . ? C29 C30 C49 C52 172.8(6) . . . . ? C31 C30 C49 C51 112.6(6) . . . . ? C29 C30 C49 C51 -67.2(7) . . . . ? C46 C47 C53 C55 116.0(8) . . . . ? C48 C47 C53 C55 -64.5(11) . . . . ? C46 C47 C53 C56 -123.0(8) . . . . ? C48 C47 C53 C56 56.5(11) . . . . ? C46 C47 C53 C54 -3.6(10) . . . . ? C48 C47 C53 C54 176.0(10) . . . . ? O4 Ni2 N3' C35' -71(5) . . . . ? O4' Ni2 N3' C35' -79(5) . . . . ? O3 Ni2 N3' C35' 6(2) . . . . ? N3 Ni2 N3' C35' 101(4) . . . . ? N4 Ni2 N3' C35' -173(2) . . . . ? O4 Ni2 N3' C36 114(3) . . . . ? O4' Ni2 N3' C36 106(4) . . . . ? O3 Ni2 N3' C36 -169.2(12) . . . . ? N3 Ni2 N3' C36 -74(2) . . . . ? N4 Ni2 N3' C36 12.2(12) . . . . ? O4 Ni2 O4' C48' 127(18) . . . . ? N3' Ni2 O4' C48' -102(5) . . . . ? O3 Ni2 O4' C48' 172(2) . . . . ? N3 Ni2 O4' C48' 78(10) . . . . ? N4 Ni2 O4' C48' -9(2) . . . . ? C29 O3 C29' C34' -85.7(19) . . . . ? Ni2 O3 C29' C34' 10(2) . . . . ? C29 O3 C29' C30' 93(2) . . . . ? Ni2 O3 C29' C30' -171.1(11) . . . . ? O3 C29' C30' C31' 179.1(16) . . . . ? C34' C29' C30' C31' -2(3) . . . . ? O3 C29' C30' C49' 3(3) . . . . ? C34' C29' C30' C49' -178.2(16) . . . . ? C29' C30' C31' C32' 0(3) . . . . ? C49' C30' C31' C32' 176.5(17) . . . . ? C30' C31' C32' C33' 1(3) . . . . ? C31' C32' C33' C34' -1(3) . . . . ? C32' C33' C34' C35' -179.6(18) . . . . ? C32' C33' C34' C29' -1(3) . . . . ? O3 C29' C34' C35' 0(3) . . . . ? C30' C29' C34' C35' -178.9(17) . . . . ? O3 C29' C34' C33' -178.9(16) . . . . ? C30' C29' C34' C33' 2(3) . . . . ? C36 N3' C35' C34' 175.5(17) . . . . ? Ni2 N3' C35' C34' 1(3) . . . . ? C33' C34' C35' N3' 173(2) . . . . ? C29' C34' C35' N3' -6(3) . . . . ? C42 N4 C42' C43' 80(4) . . . . ? C41 N4 C42' C43' 179.7(13) . . . . ? Ni2 N4 C42' C43' -13(2) . . . . ? N4 C42' C43' C44' -175.4(17) . . . . ? N4 C42' C43' C48' 2(3) . . . . ? C42' C43' C44' C45' -177.7(15) . . . . ? C48' C43' C44' C45' 5(3) . . . . ? C43' C44' C45' C46' 1(2) . . . . ? C44' C45' C46' C47' -4(2) . . . . ? C45' C46' C47' C48' 2(3) . . . . ? C45' C46' C47' C53' 176.1(15) . . . . ? Ni2 O4' C48' C43' 2(4) . . . . ? Ni2 O4' C48' C47' -169.2(15) . . . . ? C42' C43' C48' O4' 4(4) . . . . ? C44' C43' C48' O4' -179(2) . . . . ? C42' C43' C48' C47' 175(2) . . . . ? C44' C43' C48' C47' -8(4) . . . . ? C46' C47' C48' O4' 176(3) . . . . ? C53' C47' C48' O4' 1(4) . . . . ? C46' C47' C48' C43' 4(4) . . . . ? C53' C47' C48' C43' -171(2) . . . . ? C31' C30' C49' C50' -118.7(18) . . . . ? C29' C30' C49' C50' 57(2) . . . . ? C31' C30' C49' C52' 1(2) . . . . ? C29' C30' C49' C52' 176.9(15) . . . . ? C31' C30' C49' C51' 119.7(18) . . . . ? C29' C30' C49' C51' -64.3(19) . . . . ? C46' C47' C53' C55' 128.1(17) . . . . ? C48' C47' C53' C55' -57(2) . . . . ? C46' C47' C53' C56' -107.9(18) . . . . ? C48' C47' C53' C56' 67(2) . . . . ? C46' C47' C53' C54' 6(2) . . . . ? C48' C47' C53' C54' -179(2) . . . . ? C35 N3 C36 C41 -167.8(5) . . . . ? Ni2 N3 C36 C41 7.0(5) . . . . ? C35 N3 C36 C37 12.1(8) . . . . ? Ni2 N3 C36 C37 -173.1(3) . . . . ? C35 N3 C36 N3' 103(3) . . . . ? Ni2 N3 C36 N3' -82(3) . . . . ? C35' N3' C36 C41 168.2(17) . . . . ? Ni2 N3' C36 C41 -16.7(16) . . . . ? C35' N3' C36 C37 4(3) . . . . ? Ni2 N3' C36 C37 178.8(6) . . . . ? C35' N3' C36 N3 -95(3) . . . . ? Ni2 N3' C36 N3 80(3) . . . . ? C41 C36 C37 C38 1.2(5) . . . . ? N3 C36 C37 C38 -178.6(4) . . . . ? N3' C36 C37 C38 164.6(11) . . . . ? C36 C37 C38 C39 0.8(5) . . . . ? C36 C37 C38 C87 -176.4(3) . . . . ? C37 C38 C39 C40 -1.2(5) . . . . ? C87 C38 C39 C40 176.3(3) . . . . ? C37 C38 C39 C57 -178.5(3) . . . . ? C87 C38 C39 C57 -1.0(4) . . . . ? C38 C39 C40 C41 -0.6(4) . . . . ? C57 C39 C40 C41 176.4(3) . . . . ? C37 C36 C41 C40 -3.0(5) . . . . ? N3 C36 C41 C40 176.9(4) . . . . ? N3' C36 C41 C40 -168.0(10) . . . . ? C37 C36 C41 N4 177.1(3) . . . . ? N3 C36 C41 N4 -3.0(5) . . . . ? N3' C36 C41 N4 12.2(11) . . . . ? C39 C40 C41 C36 2.6(5) . . . . ? C39 C40 C41 N4 -177.5(3) . . . . ? C42' N4 C41 C36 166.3(11) . . . . ? C42 N4 C41 C36 -176.4(5) . . . . ? Ni2 N4 C41 C36 -2.4(4) . . . . ? C42' N4 C41 C40 -13.5(11) . . . . ? C42 N4 C41 C40 3.8(6) . . . . ? Ni2 N4 C41 C40 177.8(3) . . . . ? C9 C10 C57 C68 -129.9(3) . . . . ? C11 C10 C57 C68 55.1(3) . . . . ? C9 C10 C57 C39 118.2(3) . . . . ? C11 C10 C57 C39 -56.8(3) . . . . ? C40 C39 C57 C68 128.1(3) . . . . ? C38 C39 C57 C68 -54.7(3) . . . . ? C40 C39 C57 C10 -119.7(3) . . . . ? C38 C39 C57 C10 57.4(3) . . . . ? C64 C59 C60 C61 1.4(5) . . . . ? C79 C59 C60 C61 -177.1(3) . . . . ? C59 C60 C61 C62 2.0(6) . . . . ? C60 C61 C62 C63 -2.2(5) . . . . ? C61 C62 C63 C65 175.8(3) . . . . ? C61 C62 C63 C64 -1.0(5) . . . . ? Ni3 O5 C64 C63 -0.9(4) . . . . ? Ni3 O5 C64 C59 178.9(2) . . . . ? C65 C63 C64 O5 7.5(5) . . . . ? C62 C63 C64 O5 -175.8(3) . . . . ? C65 C63 C64 C59 -172.3(3) . . . . ? C62 C63 C64 C59 4.3(5) . . . . ? C60 C59 C64 O5 175.7(3) . . . . ? C79 C59 C64 O5 -5.8(5) . . . . ? C60 C59 C64 C63 -4.5(5) . . . . ? C79 C59 C64 C63 174.0(3) . . . . ? C66 N5 C65 C63 177.0(3) . . . . ? Ni3 N5 C65 C63 -6.8(5) . . . . ? C62 C63 C65 N5 179.7(3) . . . . ? C64 C63 C65 N5 -3.6(5) . . . . ? C65 N5 C66 C71 174.8(3) . . . . ? Ni3 N5 C66 C71 -1.8(3) . . . . ? C65 N5 C66 C67 -4.5(5) . . . . ? Ni3 N5 C66 C67 178.9(2) . . . . ? C71 C66 C67 C68 1.9(4) . . . . ? N5 C66 C67 C68 -178.9(3) . . . . ? C66 C67 C68 C69 0.5(4) . . . . ? C66 C67 C68 C57 179.8(3) . . . . ? C10 C57 C68 C67 126.9(3) . . . . ? C39 C57 C68 C67 -122.8(3) . . . . ? C10 C57 C68 C69 -53.7(3) . . . . ? C39 C57 C68 C69 56.6(3) . . . . ? C67 C68 C69 C70 -1.3(4) . . . . ? C57 C68 C69 C70 179.3(3) . . . . ? C67 C68 C69 C87 177.3(3) . . . . ? C57 C68 C69 C87 -2.2(3) . . . . ? C68 C69 C70 C71 -0.3(4) . . . . ? C87 C69 C70 C71 -178.7(3) . . . . ? C69 C70 C71 C66 2.7(4) . . . . ? C69 C70 C71 N6 -177.9(3) . . . . ? C67 C66 C71 C70 -3.6(4) . . . . ? N5 C66 C71 C70 177.1(3) . . . . ? C67 C66 C71 N6 177.0(3) . . . . ? N5 C66 C71 N6 -2.3(4) . . . . ? C72 N6 C71 C70 8.4(5) . . . . ? Ni3 N6 C71 C70 -173.9(2) . . . . ? C72 N6 C71 C66 -172.2(3) . . . . ? Ni3 N6 C71 C66 5.5(3) . . . . ? C71 N6 C72 C73 -179.0(3) . . . . ? Ni3 N6 C72 C73 3.6(5) . . . . ? N6 C72 C73 C74 180.0(3) . . . . ? N6 C72 C73 C78 0.9(5) . . . . ? C72 C73 C74 C75 -179.9(3) . . . . ? C78 C73 C74 C75 -0.8(5) . . . . ? C73 C74 C75 C76 2.9(6) . . . . ? C74 C75 C76 C77 -2.6(6) . . . . ? C75 C76 C77 C78 0.0(5) . . . . ? C75 C76 C77 C83 -178.3(3) . . . . ? Ni3 O6 C78 C73 1.0(4) . . . . ? Ni3 O6 C78 C77 -179.6(2) . . . . ? C74 C73 C78 O6 177.7(3) . . . . ? C72 C73 C78 O6 -3.2(5) . . . . ? C74 C73 C78 C77 -1.7(5) . . . . ? C72 C73 C78 C77 177.3(3) . . . . ? C76 C77 C78 O6 -177.4(3) . . . . ? C83 C77 C78 O6 1.0(5) . . . . ? C76 C77 C78 C73 2.1(5) . . . . ? C83 C77 C78 C73 -179.6(3) . . . . ? C60 C59 C79 C82 120.7(4) . . . . ? C64 C59 C79 C82 -57.7(4) . . . . ? C60 C59 C79 C80 1.1(5) . . . . ? C64 C59 C79 C80 -177.4(3) . . . . ? C60 C59 C79 C81 -118.1(4) . . . . ? C64 C59 C79 C81 63.4(4) . . . . ? C76 C77 C83 C85 114.1(4) . . . . ? C78 C77 C83 C85 -64.2(4) . . . . ? C76 C77 C83 C86 -5.2(5) . . . . ? C78 C77 C83 C86 176.5(3) . . . . ? C76 C77 C83 C84 -124.3(4) . . . . ? C78 C77 C83 C84 57.4(4) . . . . ? C12 C11 C87 C69 127.1(3) . . . . ? C10 C11 C87 C69 -55.6(3) . . . . ? C12 C11 C87 C38 -120.6(3) . . . . ? C10 C11 C87 C38 56.7(3) . . . . ? C70 C69 C87 C11 -124.6(3) . . . . ? C68 C69 C87 C11 56.9(3) . . . . ? C70 C69 C87 C38 124.9(3) . . . . ? C68 C69 C87 C38 -53.7(3) . . . . ? C37 C38 C87 C11 121.3(3) . . . . ? C39 C38 C87 C11 -56.1(3) . . . . ? C37 C38 C87 C69 -127.0(3) . . . . ? C39 C38 C87 C69 55.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.252 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.092 data_mo_awk1005_05m _database_code_depnum_ccdc_archive 'CCDC 913293' #TrackingRef 'mo_awk1005_05mX.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H62 N4 O8 S4 Zn2' _chemical_formula_weight 1298.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1484(7) _cell_length_b 10.4688(8) _cell_length_c 17.6146(12) _cell_angle_alpha 98.405(3) _cell_angle_beta 97.457(4) _cell_angle_gamma 114.971(3) _cell_volume 1477.98(19) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 847 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.15 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 674 _exptl_absorpt_coefficient_mu 1.014 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9054 _exptl_absorpt_correction_T_max 0.9899 _exptl_absorpt_process_details ; TWINABS Version 2008/0 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Micorfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7022 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.1092 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 28.21 _reflns_number_total 7022 _reflns_number_gt 4662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution Sir2011 _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0671P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7022 _refine_ls_number_parameters 404 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.69999(6) 0.84737(5) 0.65908(3) 0.01270(14) Uani 1 1 d . . . S1 S 0.44991(14) 0.51349(11) 0.64892(7) 0.0223(3) Uani 1 1 d . . . N1 N 0.7169(4) 0.8869(3) 0.54671(18) 0.0127(7) Uani 1 1 d . . . N2 N 0.6126(4) 1.0032(3) 0.65553(18) 0.0144(7) Uani 1 1 d . . . O1 O 0.8780(3) 0.7883(3) 0.65937(15) 0.0155(6) Uani 1 1 d . . . O2 O 0.7251(4) 0.8936(3) 0.77423(15) 0.0189(7) Uani 1 1 d . . . O3 O 0.4890(4) 0.6570(3) 0.62524(17) 0.0209(7) Uani 1 1 d . . . C1 C 0.9467(5) 0.7646(4) 0.6015(2) 0.0148(8) Uani 1 1 d . . . C2 C 1.0622(5) 0.7079(4) 0.6146(2) 0.0160(9) Uani 1 1 d . . . C3 C 1.1398(5) 0.6827(4) 0.5554(2) 0.0181(9) Uani 1 1 d . . . H3 H 1.2170 0.6455 0.5655 0.022 Uiso 1 1 calc R . . C4 C 1.1076(5) 0.7105(4) 0.4814(2) 0.0183(9) Uani 1 1 d . . . H4 H 1.1607 0.6912 0.4414 0.022 Uiso 1 1 calc R . . C5 C 0.9980(5) 0.7661(4) 0.4677(2) 0.0163(9) Uani 1 1 d . . . H5 H 0.9762 0.7862 0.4177 0.020 Uiso 1 1 calc R . . C6 C 0.9162(5) 0.7943(4) 0.5262(2) 0.0134(8) Uani 1 1 d . . . C7 C 0.8079(5) 0.8570(4) 0.5036(2) 0.0140(8) Uani 1 1 d . . . H7 H 0.8032 0.8781 0.4530 0.017 Uiso 1 1 calc R . . C8 C 0.6114(5) 0.9436(4) 0.5194(2) 0.0134(8) Uani 1 1 d . . . C9 C 0.5576(5) 0.9409(4) 0.4417(2) 0.0133(8) Uani 1 1 d . . . H9 H 0.5971 0.9013 0.4018 0.016 Uiso 1 1 calc R . . C10 C 0.5534(5) 1.0048(4) 0.5789(2) 0.0127(8) Uani 1 1 d . . . C11 C 0.6276(5) 1.1009(4) 0.7146(2) 0.0147(8) Uani 1 1 d . . . H11 H 0.6047 1.1774 0.7032 0.018 Uiso 1 1 calc R . . C12 C 0.6760(5) 1.1030(4) 0.7961(2) 0.0144(8) Uani 1 1 d . . . C13 C 0.6782(5) 1.2162(4) 0.8521(2) 0.0171(9) Uani 1 1 d . . . H13 H 0.6575 1.2899 0.8347 0.021 Uiso 1 1 calc R . . C14 C 0.7094(6) 1.2208(5) 0.9305(2) 0.0213(10) Uani 1 1 d . . . H14 H 0.7139 1.2989 0.9674 0.026 Uiso 1 1 calc R . . C15 C 0.7347(5) 1.1107(4) 0.9563(2) 0.0195(9) Uani 1 1 d . . . H15 H 0.7523 1.1130 1.0109 0.023 Uiso 1 1 calc R . . C16 C 0.7349(5) 0.9983(4) 0.9044(2) 0.0153(9) Uani 1 1 d . . . C17 C 0.7144(5) 0.9954(4) 0.8212(2) 0.0138(8) Uani 1 1 d . . . C18 C 1.1048(5) 0.6754(4) 0.6922(2) 0.0145(8) Uani 1 1 d . . . C19 C 0.9869(6) 0.5730(5) 0.7222(3) 0.0223(10) Uani 1 1 d . . . H19 H 0.8759 0.5234 0.6933 0.027 Uiso 1 1 calc R . . C20 C 1.0273(6) 0.5417(5) 0.7931(3) 0.0267(11) Uani 1 1 d . . . H20 H 0.9445 0.4715 0.8125 0.032 Uiso 1 1 calc R . . C21 C 1.1874(6) 0.6123(5) 0.8355(3) 0.0254(10) Uani 1 1 d . . . H21 H 1.2154 0.5913 0.8844 0.030 Uiso 1 1 calc R . . C22 C 1.3068(6) 0.7132(5) 0.8069(3) 0.0275(11) Uani 1 1 d . . . H22 H 1.4177 0.7616 0.8359 0.033 Uiso 1 1 calc R . . C23 C 1.2650(6) 0.7447(5) 0.7349(2) 0.0213(9) Uani 1 1 d . . . H23 H 1.3480 0.8145 0.7153 0.026 Uiso 1 1 calc R . . C24 C 0.7491(5) 0.8761(4) 0.9341(2) 0.0158(9) Uani 1 1 d . . . C25 C 0.6481(6) 0.8130(5) 0.9842(2) 0.0237(10) Uani 1 1 d . . . H25 H 0.5760 0.8506 0.9999 0.028 Uiso 1 1 calc R . . C26 C 0.6508(6) 0.6967(5) 1.0113(3) 0.0292(11) Uani 1 1 d . . . H26 H 0.5790 0.6529 1.0443 0.035 Uiso 1 1 calc R . . C27 C 0.7596(7) 0.6442(5) 0.9901(3) 0.0320(12) Uani 1 1 d . . . H27 H 0.7650 0.5665 1.0101 0.038 Uiso 1 1 calc R . . C28 C 0.8591(6) 0.7045(5) 0.9402(3) 0.0269(11) Uani 1 1 d . . . H28 H 0.9315 0.6670 0.9248 0.032 Uiso 1 1 calc R . . C29 C 0.8541(6) 0.8200(5) 0.9123(3) 0.0219(10) Uani 1 1 d . . . H29 H 0.9235 0.8612 0.8778 0.026 Uiso 1 1 calc R . . C30 C 0.5810(6) 0.5554(5) 0.7428(3) 0.0241(10) Uani 1 1 d . . . H30A H 0.6949 0.6195 0.7411 0.036 Uiso 1 1 calc R . . H30B H 0.5755 0.4659 0.7560 0.036 Uiso 1 1 calc R . . H30C H 0.5445 0.6036 0.7827 0.036 Uiso 1 1 calc R . . C31 C 0.5511(6) 0.4347(5) 0.5917(3) 0.0264(11) Uani 1 1 d . . . H31A H 0.4903 0.3997 0.5369 0.040 Uiso 1 1 calc R . . H31B H 0.5543 0.3536 0.6122 0.040 Uiso 1 1 calc R . . H31C H 0.6639 0.5076 0.5946 0.040 Uiso 1 1 calc R . . S1S S 0.72511(16) 0.77930(13) 0.22396(7) 0.0196(3) Uani 0.85 1 d PDU A 1 O1S O 0.6756(6) 0.7923(9) 0.3022(4) 0.0244(11) Uani 0.85 1 d PDU A 1 C1S C 0.9245(8) 0.7866(6) 0.2428(5) 0.0348(16) Uani 0.85 1 d PDU A 1 H1S1 H 1.0003 0.8754 0.2817 0.052 Uiso 0.85 1 calc PR A 1 H1S2 H 0.9650 0.7858 0.1940 0.052 Uiso 0.85 1 calc PR A 1 H1S3 H 0.9181 0.7025 0.2632 0.052 Uiso 0.85 1 calc PR A 1 C2S C 0.7861(7) 0.9511(8) 0.1995(4) 0.0271(15) Uani 0.85 1 d PDU A 1 H2S1 H 0.6893 0.9688 0.1883 0.041 Uiso 0.85 1 calc PR A 1 H2S2 H 0.8347 0.9523 0.1530 0.041 Uiso 0.85 1 calc PR A 1 H2S3 H 0.8677 1.0267 0.2437 0.041 Uiso 0.85 1 calc PR A 1 S1S' S 0.8329(11) 0.8679(8) 0.2864(5) 0.0301(16) Uani 0.15 1 d PDU B 2 O1S' O 0.654(3) 0.788(5) 0.292(3) 0.0244(11) Uani 0.15 1 d PDU B 2 C1S' C 0.836(5) 0.960(5) 0.209(2) 0.0271(15) Uani 0.15 1 d PDU B 2 H1S4 H 0.7398 0.8997 0.1664 0.041 Uiso 0.15 1 calc PR B 2 H1S5 H 0.9372 0.9808 0.1895 0.041 Uiso 0.15 1 calc PR B 2 H1S6 H 0.8327 1.0513 0.2289 0.041 Uiso 0.15 1 calc PR B 2 C2S' C 0.883(6) 0.735(3) 0.237(3) 0.0348(16) Uani 0.15 1 d PDU B 2 H2S4 H 0.7841 0.6583 0.2010 0.052 Uiso 0.15 1 calc PR B 2 H2S5 H 0.9263 0.6946 0.2757 0.052 Uiso 0.15 1 calc PR B 2 H2S6 H 0.9673 0.7808 0.2072 0.052 Uiso 0.15 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0148(3) 0.0143(2) 0.0119(2) 0.00447(18) 0.00203(19) 0.0090(2) S1 0.0169(6) 0.0168(5) 0.0296(6) 0.0099(5) -0.0006(5) 0.0044(5) N1 0.0123(18) 0.0148(16) 0.0123(16) 0.0057(13) 0.0029(14) 0.0062(14) N2 0.0145(19) 0.0172(17) 0.0135(17) 0.0062(13) 0.0036(14) 0.0079(15) O1 0.0157(15) 0.0232(15) 0.0130(14) 0.0050(11) 0.0038(12) 0.0132(13) O2 0.0299(18) 0.0238(16) 0.0092(14) 0.0041(12) 0.0031(13) 0.0179(15) O3 0.0180(17) 0.0167(14) 0.0266(16) 0.0073(13) -0.0024(13) 0.0077(13) C1 0.012(2) 0.0136(19) 0.016(2) -0.0019(16) 0.0015(17) 0.0047(17) C2 0.015(2) 0.0134(19) 0.020(2) 0.0052(16) 0.0001(17) 0.0073(18) C3 0.013(2) 0.022(2) 0.025(2) 0.0077(18) 0.0056(18) 0.0114(19) C4 0.020(2) 0.024(2) 0.018(2) 0.0056(17) 0.0084(18) 0.015(2) C5 0.019(2) 0.021(2) 0.010(2) 0.0034(16) 0.0034(17) 0.0104(19) C6 0.013(2) 0.0121(18) 0.016(2) 0.0034(15) 0.0035(16) 0.0055(17) C7 0.013(2) 0.0128(18) 0.0120(19) 0.0018(15) -0.0030(16) 0.0041(17) C8 0.013(2) 0.0108(18) 0.015(2) 0.0035(15) 0.0009(16) 0.0041(16) C9 0.018(2) 0.0140(19) 0.0107(19) 0.0044(15) 0.0045(16) 0.0086(17) C10 0.015(2) 0.0111(18) 0.0119(19) 0.0061(15) 0.0031(16) 0.0042(17) C11 0.014(2) 0.0148(19) 0.017(2) 0.0043(16) 0.0058(17) 0.0064(18) C12 0.014(2) 0.015(2) 0.012(2) 0.0034(16) 0.0043(17) 0.0048(18) C13 0.014(2) 0.014(2) 0.021(2) 0.0021(17) 0.0024(18) 0.0049(18) C14 0.028(3) 0.022(2) 0.016(2) 0.0037(17) 0.0050(19) 0.013(2) C15 0.022(3) 0.023(2) 0.011(2) 0.0033(17) 0.0020(18) 0.009(2) C16 0.011(2) 0.019(2) 0.016(2) 0.0062(17) 0.0031(17) 0.0073(18) C17 0.012(2) 0.017(2) 0.014(2) 0.0046(16) 0.0038(16) 0.0063(18) C18 0.014(2) 0.017(2) 0.019(2) 0.0075(16) 0.0036(17) 0.0107(18) C19 0.015(2) 0.025(2) 0.027(2) 0.0086(19) 0.0021(19) 0.009(2) C20 0.026(3) 0.031(3) 0.031(3) 0.018(2) 0.011(2) 0.015(2) C21 0.030(3) 0.038(3) 0.017(2) 0.012(2) 0.005(2) 0.021(2) C22 0.025(3) 0.034(3) 0.024(2) 0.007(2) 0.001(2) 0.014(2) C23 0.016(2) 0.025(2) 0.022(2) 0.0084(18) 0.0055(19) 0.007(2) C24 0.018(2) 0.020(2) 0.0083(19) 0.0022(16) -0.0020(17) 0.0088(19) C25 0.024(3) 0.026(2) 0.014(2) 0.0012(18) -0.0018(19) 0.007(2) C26 0.038(3) 0.023(2) 0.020(2) 0.0078(19) 0.007(2) 0.007(2) C27 0.045(3) 0.022(2) 0.028(3) 0.007(2) 0.001(2) 0.016(2) C28 0.026(3) 0.027(2) 0.030(3) 0.010(2) 0.000(2) 0.015(2) C29 0.016(2) 0.027(2) 0.022(2) 0.0083(19) 0.0010(19) 0.009(2) C30 0.025(3) 0.023(2) 0.024(2) 0.0116(19) 0.002(2) 0.009(2) C31 0.028(3) 0.018(2) 0.031(3) 0.0041(19) -0.003(2) 0.011(2) S1S 0.0185(7) 0.0198(6) 0.0173(6) 0.0028(5) 0.0064(5) 0.0054(6) O1S 0.027(2) 0.0298(17) 0.022(3) 0.0077(17) 0.012(2) 0.0155(18) C1S 0.025(4) 0.032(4) 0.056(4) 0.018(4) 0.022(3) 0.014(4) C2S 0.024(4) 0.029(3) 0.025(3) 0.009(2) 0.003(3) 0.009(3) S1S' 0.037(4) 0.026(4) 0.030(4) 0.015(3) 0.014(3) 0.011(3) O1S' 0.027(2) 0.0298(17) 0.022(3) 0.0077(17) 0.012(2) 0.0155(18) C1S' 0.024(4) 0.029(3) 0.025(3) 0.009(2) 0.003(3) 0.009(3) C2S' 0.025(4) 0.032(4) 0.056(4) 0.018(4) 0.022(3) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.971(3) . ? Zn1 O2 1.975(3) . ? Zn1 O3 2.040(3) . ? Zn1 N1 2.092(3) . ? Zn1 N2 2.103(3) . ? S1 O3 1.525(3) . ? S1 C30 1.787(4) . ? S1 C31 1.788(5) . ? N1 C7 1.297(5) . ? N1 C8 1.401(5) . ? N2 C11 1.297(5) . ? N2 C10 1.393(5) . ? O1 C1 1.310(4) . ? O2 C17 1.296(4) . ? C1 C2 1.424(5) . ? C1 C6 1.426(6) . ? C2 C3 1.390(5) . ? C2 C18 1.498(5) . ? C3 C4 1.398(6) . ? C4 C5 1.369(5) . ? C5 C6 1.417(5) . ? C6 C7 1.447(5) . ? C8 C9 1.385(5) . ? C8 C10 1.423(5) . ? C9 C10 1.392(5) 2_676 ? C10 C9 1.392(5) 2_676 ? C11 C12 1.440(5) . ? C12 C13 1.418(5) . ? C12 C17 1.424(5) . ? C13 C14 1.362(6) . ? C14 C15 1.393(6) . ? C15 C16 1.381(5) . ? C16 C17 1.447(5) . ? C16 C24 1.499(5) . ? C18 C23 1.377(6) . ? C18 C19 1.390(6) . ? C19 C20 1.380(6) . ? C20 C21 1.376(6) . ? C21 C22 1.373(7) . ? C22 C23 1.403(6) . ? C24 C29 1.386(6) . ? C24 C25 1.391(6) . ? C25 C26 1.381(6) . ? C26 C27 1.389(7) . ? C27 C28 1.372(7) . ? C28 C29 1.386(6) . ? S1S O1S 1.510(6) . ? S1S C1S 1.778(7) . ? S1S C2S 1.782(6) . ? S1S' O1S' 1.512(9) . ? S1S' C1S' 1.779(9) . ? S1S' C2S' 1.784(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O2 96.39(11) . . ? O1 Zn1 O3 104.02(11) . . ? O2 Zn1 O3 102.48(12) . . ? O1 Zn1 N1 90.26(12) . . ? O2 Zn1 N1 157.44(12) . . ? O3 Zn1 N1 96.73(12) . . ? O1 Zn1 N2 151.27(13) . . ? O2 Zn1 N2 87.01(11) . . ? O3 Zn1 N2 103.04(12) . . ? N1 Zn1 N2 77.14(12) . . ? O3 S1 C30 106.56(18) . . ? O3 S1 C31 104.5(2) . . ? C30 S1 C31 98.1(2) . . ? C7 N1 C8 121.9(3) . . ? C7 N1 Zn1 125.1(3) . . ? C8 N1 Zn1 112.9(2) . . ? C11 N2 C10 121.1(3) . . ? C11 N2 Zn1 126.3(3) . . ? C10 N2 Zn1 112.1(2) . . ? C1 O1 Zn1 129.1(3) . . ? C17 O2 Zn1 132.0(3) . . ? S1 O3 Zn1 129.49(17) . . ? O1 C1 C2 118.3(4) . . ? O1 C1 C6 124.5(4) . . ? C2 C1 C6 117.2(4) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 C18 118.2(3) . . ? C1 C2 C18 121.3(4) . . ? C2 C3 C4 121.9(4) . . ? C5 C4 C3 118.6(4) . . ? C4 C5 C6 121.6(4) . . ? C5 C6 C1 120.2(4) . . ? C5 C6 C7 115.0(3) . . ? C1 C6 C7 124.8(4) . . ? N1 C7 C6 125.5(4) . . ? C9 C8 N1 126.1(3) . . ? C9 C8 C10 119.2(4) . . ? N1 C8 C10 114.7(3) . . ? C8 C9 C10 121.0(3) . 2_676 ? C9 C10 N2 124.4(3) 2_676 . ? C9 C10 C8 119.8(4) 2_676 . ? N2 C10 C8 115.8(3) . . ? N2 C11 C12 125.4(4) . . ? C13 C12 C17 120.3(4) . . ? C13 C12 C11 116.7(4) . . ? C17 C12 C11 123.0(3) . . ? C14 C13 C12 121.0(4) . . ? C13 C14 C15 119.8(4) . . ? C16 C15 C14 121.6(4) . . ? C15 C16 C17 120.2(4) . . ? C15 C16 C24 119.7(4) . . ? C17 C16 C24 120.1(3) . . ? O2 C17 C12 124.3(4) . . ? O2 C17 C16 119.0(3) . . ? C12 C17 C16 116.7(3) . . ? C23 C18 C19 118.1(4) . . ? C23 C18 C2 120.2(4) . . ? C19 C18 C2 121.7(4) . . ? C20 C19 C18 121.5(4) . . ? C21 C20 C19 119.9(5) . . ? C22 C21 C20 119.8(4) . . ? C21 C22 C23 120.0(4) . . ? C18 C23 C22 120.7(4) . . ? C29 C24 C25 118.4(4) . . ? C29 C24 C16 123.3(4) . . ? C25 C24 C16 118.3(4) . . ? C26 C25 C24 121.2(4) . . ? C25 C26 C27 119.4(5) . . ? C28 C27 C26 120.1(4) . . ? C27 C28 C29 120.1(4) . . ? C28 C29 C24 120.7(4) . . ? O1S S1S C1S 106.8(3) . . ? O1S S1S C2S 106.6(4) . . ? C1S S1S C2S 97.2(3) . . ? O1S' S1S' C1S' 106.5(8) . . ? O1S' S1S' C2S' 106.2(8) . . ? C1S' S1S' C2S' 97.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Zn1 N1 C7 6.6(3) . . . . ? O2 Zn1 N1 C7 114.1(4) . . . . ? O3 Zn1 N1 C7 -97.5(3) . . . . ? N2 Zn1 N1 C7 160.6(3) . . . . ? O1 Zn1 N1 C8 -176.5(3) . . . . ? O2 Zn1 N1 C8 -69.0(4) . . . . ? O3 Zn1 N1 C8 79.3(3) . . . . ? N2 Zn1 N1 C8 -22.6(3) . . . . ? O1 Zn1 N2 C11 -82.5(4) . . . . ? O2 Zn1 N2 C11 15.4(3) . . . . ? O3 Zn1 N2 C11 117.5(3) . . . . ? N1 Zn1 N2 C11 -148.5(4) . . . . ? O1 Zn1 N2 C10 89.2(3) . . . . ? O2 Zn1 N2 C10 -173.0(3) . . . . ? O3 Zn1 N2 C10 -70.8(3) . . . . ? N1 Zn1 N2 C10 23.2(3) . . . . ? O2 Zn1 O1 C1 -168.2(3) . . . . ? O3 Zn1 O1 C1 87.2(3) . . . . ? N1 Zn1 O1 C1 -9.8(3) . . . . ? N2 Zn1 O1 C1 -72.8(4) . . . . ? O1 Zn1 O2 C17 141.8(4) . . . . ? O3 Zn1 O2 C17 -112.2(4) . . . . ? N1 Zn1 O2 C17 35.5(6) . . . . ? N2 Zn1 O2 C17 -9.5(4) . . . . ? C30 S1 O3 Zn1 25.1(3) . . . . ? C31 S1 O3 Zn1 -78.1(3) . . . . ? O1 Zn1 O3 S1 40.9(3) . . . . ? O2 Zn1 O3 S1 -59.0(2) . . . . ? N1 Zn1 O3 S1 132.9(2) . . . . ? N2 Zn1 O3 S1 -148.8(2) . . . . ? Zn1 O1 C1 C2 -173.5(3) . . . . ? Zn1 O1 C1 C6 7.7(6) . . . . ? O1 C1 C2 C3 -179.2(4) . . . . ? C6 C1 C2 C3 -0.3(6) . . . . ? O1 C1 C2 C18 0.2(6) . . . . ? C6 C1 C2 C18 179.0(4) . . . . ? C1 C2 C3 C4 -0.5(6) . . . . ? C18 C2 C3 C4 -179.8(4) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C4 C5 C6 C1 -0.1(6) . . . . ? C4 C5 C6 C7 178.2(4) . . . . ? O1 C1 C6 C5 179.4(4) . . . . ? C2 C1 C6 C5 0.6(6) . . . . ? O1 C1 C6 C7 1.2(7) . . . . ? C2 C1 C6 C7 -177.6(4) . . . . ? C8 N1 C7 C6 -178.0(4) . . . . ? Zn1 N1 C7 C6 -1.4(6) . . . . ? C5 C6 C7 N1 177.5(4) . . . . ? C1 C6 C7 N1 -4.3(6) . . . . ? C7 N1 C8 C9 17.5(6) . . . . ? Zn1 N1 C8 C9 -159.5(3) . . . . ? C7 N1 C8 C10 -164.5(4) . . . . ? Zn1 N1 C8 C10 18.6(4) . . . . ? N1 C8 C9 C10 177.1(4) . . . 2_676 ? C10 C8 C9 C10 -0.9(7) . . . 2_676 ? C11 N2 C10 C9 -29.7(6) . . . 2_676 ? Zn1 N2 C10 C9 158.1(3) . . . 2_676 ? C11 N2 C10 C8 151.4(4) . . . . ? Zn1 N2 C10 C8 -20.8(4) . . . . ? C9 C8 C10 C9 0.9(6) . . . 2_676 ? N1 C8 C10 C9 -177.3(3) . . . 2_676 ? C9 C8 C10 N2 179.8(4) . . . . ? N1 C8 C10 N2 1.6(5) . . . . ? C10 N2 C11 C12 175.3(4) . . . . ? Zn1 N2 C11 C12 -13.7(6) . . . . ? N2 C11 C12 C13 -177.3(4) . . . . ? N2 C11 C12 C17 0.3(7) . . . . ? C17 C12 C13 C14 -3.0(7) . . . . ? C11 C12 C13 C14 174.7(4) . . . . ? C12 C13 C14 C15 -2.0(7) . . . . ? C13 C14 C15 C16 2.3(7) . . . . ? C14 C15 C16 C17 2.3(7) . . . . ? C14 C15 C16 C24 -175.1(4) . . . . ? Zn1 O2 C17 C12 1.1(6) . . . . ? Zn1 O2 C17 C16 178.2(3) . . . . ? C13 C12 C17 O2 -175.6(4) . . . . ? C11 C12 C17 O2 6.9(7) . . . . ? C13 C12 C17 C16 7.2(6) . . . . ? C11 C12 C17 C16 -170.3(4) . . . . ? C15 C16 C17 O2 175.8(4) . . . . ? C24 C16 C17 O2 -6.8(6) . . . . ? C15 C16 C17 C12 -6.9(6) . . . . ? C24 C16 C17 C12 170.5(4) . . . . ? C3 C2 C18 C23 59.7(5) . . . . ? C1 C2 C18 C23 -119.6(4) . . . . ? C3 C2 C18 C19 -118.5(5) . . . . ? C1 C2 C18 C19 62.1(5) . . . . ? C23 C18 C19 C20 0.7(6) . . . . ? C2 C18 C19 C20 178.9(4) . . . . ? C18 C19 C20 C21 -0.2(7) . . . . ? C19 C20 C21 C22 -0.3(7) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C19 C18 C23 C22 -0.6(6) . . . . ? C2 C18 C23 C22 -178.9(4) . . . . ? C21 C22 C23 C18 0.0(7) . . . . ? C15 C16 C24 C29 -134.2(4) . . . . ? C17 C16 C24 C29 48.4(6) . . . . ? C15 C16 C24 C25 47.8(6) . . . . ? C17 C16 C24 C25 -129.6(4) . . . . ? C29 C24 C25 C26 -0.4(6) . . . . ? C16 C24 C25 C26 177.6(4) . . . . ? C24 C25 C26 C27 1.8(7) . . . . ? C25 C26 C27 C28 -2.3(7) . . . . ? C26 C27 C28 C29 1.4(7) . . . . ? C27 C28 C29 C24 0.0(7) . . . . ? C25 C24 C29 C28 -0.5(6) . . . . ? C16 C24 C29 C28 -178.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.687 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.171