# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Craig Rice' _publ_contact_author_address ; Department of Chemical and Biological Sciences University of Huddersfield Queensgate Huddersfield West Yorkshire HD1 3DH UNITED KINGDOM ; _publ_contact_author_email C.R.RICE@HUD.AC.UK _publ_section_title ; Electrostatic Control of the Formation of Heteroleptic Transition Metal Helicates ; loop_ _publ_author_name 'Craig Rice' 'Christian J. Baylies' 'Lindsay P. Harding' 'J. Jeffery' 'Ryan Moon' ; T.Riis-Johannessen ; data_craigpm _database_code_depnum_ccdc_archive 'CCDC 637341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H78 Cl4 N15 O28.50 S4 Zn2' _chemical_formula_weight 2082.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.641(3) _cell_length_b 17.738(4) _cell_length_c 18.898(4) _cell_angle_alpha 75.86(3) _cell_angle_beta 82.89(3) _cell_angle_gamma 84.78(3) _cell_volume 4391.0(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6293 _cell_measurement_theta_min 4.420 _cell_measurement_theta_max 50.879 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2142 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724453 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'frames each covering 0.3\% in\w' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49434 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 20080 _reflns_number_gt 12221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0805P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20080 _refine_ls_number_parameters 1190 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1612 _refine_ls_wR_factor_gt 0.1368 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.042 _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 0.68315(3) 0.13589(3) 0.80643(2) 0.02370(12) Uani 1 1 d . . . Zn2 Zn 0.85624(3) 0.36294(3) 0.67948(2) 0.02114(12) Uani 1 1 d . . . N11 N 0.5875(3) 0.1136(2) 0.91532(17) 0.0266(8) Uani 1 1 d . . . C12 C 0.4889(3) 0.1176(3) 0.9281(2) 0.0315(10) Uani 1 1 d . . . H1 H 0.4522 0.1310 0.8880 0.038 Uiso 1 1 calc R . . C13 C 0.4386(4) 0.1028(3) 0.9977(2) 0.0361(11) Uani 1 1 d . . . H2 H 0.3697 0.1065 1.0043 0.043 Uiso 1 1 calc R . . C14 C 0.4929(4) 0.0824(3) 1.0572(2) 0.0377(11) Uani 1 1 d . . . H3 H 0.4611 0.0719 1.1047 0.045 Uiso 1 1 calc R . . C15 C 0.5957(3) 0.0777(3) 1.0454(2) 0.0329(11) Uani 1 1 d . . . H4 H 0.6337 0.0643 1.0848 0.039 Uiso 1 1 calc R . . C16 C 0.6403(3) 0.0935(2) 0.9741(2) 0.0265(9) Uani 1 1 d . . . N21 N 0.7785(2) 0.10454(19) 0.88224(16) 0.0227(7) Uani 1 1 d . . . C22 C 0.8743(3) 0.0964(2) 0.8676(2) 0.0254(9) Uani 1 1 d . . . S23 S 0.93433(8) 0.06861(7) 0.94518(6) 0.0305(3) Uani 1 1 d . . . C24 C 0.8237(3) 0.0667(3) 0.9986(2) 0.0314(10) Uani 1 1 d . . . H5 H 0.8161 0.0536 1.0496 0.038 Uiso 1 1 calc R . . C25 C 0.7477(3) 0.0872(2) 0.9553(2) 0.0262(9) Uani 1 1 d . . . N31 N 0.8485(2) 0.14591(18) 0.74394(16) 0.0186(7) Uani 1 1 d . . . C32 C 0.9163(3) 0.1133(2) 0.7913(2) 0.0224(9) Uani 1 1 d . . . C33 C 1.0147(3) 0.0983(2) 0.7677(2) 0.0251(9) Uani 1 1 d . . . H6 H 1.0593 0.0761 0.8016 0.030 Uiso 1 1 calc R . . C34 C 1.0463(3) 0.1164(2) 0.6937(2) 0.0243(9) Uani 1 1 d . . . H7 H 1.1122 0.1068 0.6769 0.029 Uiso 1 1 calc R . . C35 C 0.9771(3) 0.1494(2) 0.6445(2) 0.0216(8) Uani 1 1 d . . . C36 C 0.8795(3) 0.1643(2) 0.6724(2) 0.0184(8) Uani 1 1 d . . . N41 N 0.7739(2) 0.27750(18) 0.63094(16) 0.0180(7) Uani 1 1 d . . . C42 C 0.7014(3) 0.3170(2) 0.59087(19) 0.0206(8) Uani 1 1 d . . . C43 C 0.6584(3) 0.2849(2) 0.5431(2) 0.0240(9) Uani 1 1 d . . . H8 H 0.6087 0.3131 0.5164 0.029 Uiso 1 1 calc R . . C44 C 0.6898(3) 0.2110(2) 0.5356(2) 0.0227(9) Uani 1 1 d . . . H9 H 0.6617 0.1889 0.5037 0.027 Uiso 1 1 calc R . . C45 C 0.7642(3) 0.1699(2) 0.57616(19) 0.0204(8) Uani 1 1 d . . . C46 C 0.8032(3) 0.2056(2) 0.62365(19) 0.0182(8) Uani 1 1 d . . . N51 N 0.7300(2) 0.41870(19) 0.64629(16) 0.0201(7) Uani 1 1 d . . . C52 C 0.6757(3) 0.3946(2) 0.60489(19) 0.0199(8) Uani 1 1 d . . . S53 S 0.58341(8) 0.46206(7) 0.57389(6) 0.0308(3) Uani 1 1 d . . . C54 C 0.6226(3) 0.5247(3) 0.6191(2) 0.0313(10) Uani 1 1 d . . . H10 H 0.5938 0.5743 0.6188 0.038 Uiso 1 1 calc R . . C55 C 0.7016(3) 0.4917(2) 0.65542(19) 0.0222(9) Uani 1 1 d . . . N61 N 0.8471(3) 0.4753(2) 0.71502(18) 0.0274(8) Uani 1 1 d . . . C62 C 0.7642(3) 0.5207(2) 0.7002(2) 0.0242(9) Uani 1 1 d . . . C63 C 0.7405(3) 0.5885(3) 0.7242(2) 0.0314(10) Uani 1 1 d . . . H11 H 0.6817 0.6179 0.7142 0.038 Uiso 1 1 calc R . . C64 C 0.8067(4) 0.6114(3) 0.7637(2) 0.0372(11) Uani 1 1 d . . . H12 H 0.7935 0.6570 0.7801 0.045 Uiso 1 1 calc R . . C65 C 0.8926(4) 0.5656(3) 0.7784(2) 0.0391(12) Uani 1 1 d . . . H13 H 0.9381 0.5799 0.8047 0.047 Uiso 1 1 calc R . . C66 C 0.9101(4) 0.4984(3) 0.7535(2) 0.0353(11) Uani 1 1 d . . . H14 H 0.9680 0.4677 0.7637 0.042 Uiso 1 1 calc R . . N71 N 0.6682(2) 0.0336(2) 0.76531(16) 0.0227(7) Uani 1 1 d . . . C72 C 0.7159(3) -0.0377(2) 0.7854(2) 0.0265(9) Uani 1 1 d . . . H15 H 0.7586 -0.0461 0.8217 0.032 Uiso 1 1 calc R . . C73 C 0.7037(3) -0.0977(3) 0.7544(2) 0.0296(10) Uani 1 1 d . . . H16 H 0.7362 -0.1462 0.7703 0.036 Uiso 1 1 calc R . . C74 C 0.6422(3) -0.0855(3) 0.6987(2) 0.0291(10) Uani 1 1 d . . . H17 H 0.6346 -0.1251 0.6758 0.035 Uiso 1 1 calc R . . C75 C 0.5925(3) -0.0137(3) 0.6779(2) 0.0289(10) Uani 1 1 d . . . H18 H 0.5505 -0.0042 0.6411 0.035 Uiso 1 1 calc R . . C76 C 0.6062(3) 0.0442(2) 0.7128(2) 0.0215(9) Uani 1 1 d . . . N81 N 0.5811(2) 0.17119(19) 0.73583(16) 0.0217(7) Uani 1 1 d . . . C82 C 0.5304(3) 0.2387(2) 0.7248(2) 0.0244(9) Uani 1 1 d . . . S83 S 0.44665(7) 0.24707(6) 0.66226(5) 0.0272(2) Uani 1 1 d . . . C84 C 0.4825(3) 0.1545(2) 0.6531(2) 0.0251(9) Uani 1 1 d . . . H19 H 0.4562 0.1295 0.6224 0.030 Uiso 1 1 calc R . . C85 C 0.5551(3) 0.1224(2) 0.6972(2) 0.0244(9) Uani 1 1 d . . . N91 N 0.6407(2) 0.2762(2) 0.79465(16) 0.0213(7) Uani 1 1 d . . . C92 C 0.5539(3) 0.2959(2) 0.76317(19) 0.0227(9) Uani 1 1 d . . . C93 C 0.4949(3) 0.3616(3) 0.7708(2) 0.0290(10) Uani 1 1 d . . . H20 H 0.4362 0.3736 0.7489 0.035 Uiso 1 1 calc R . . C94 C 0.5240(3) 0.4094(3) 0.8112(2) 0.0300(10) Uani 1 1 d . . . H21 H 0.4840 0.4530 0.8180 0.036 Uiso 1 1 calc R . . C95 C 0.6130(3) 0.3919(2) 0.8416(2) 0.0250(9) Uani 1 1 d . . . C96 C 0.6696(3) 0.3240(2) 0.83096(19) 0.0214(9) Uani 1 1 d . . . N101 N 0.8459(2) 0.30611(19) 0.80793(16) 0.0199(7) Uani 1 1 d . . . C102 C 0.9371(3) 0.2862(2) 0.8311(2) 0.0211(8) Uani 1 1 d . . . C103 C 0.9512(3) 0.2639(2) 0.9046(2) 0.0243(9) Uani 1 1 d . . . H22 H 1.0148 0.2511 0.9186 0.029 Uiso 1 1 calc R . . C104 C 0.8712(3) 0.2608(2) 0.9572(2) 0.0266(9) Uani 1 1 d . . . H23 H 0.8797 0.2463 1.0068 0.032 Uiso 1 1 calc R . . C105 C 0.7779(3) 0.2798(3) 0.9341(2) 0.0268(9) Uani 1 1 d . . . C106 C 0.7686(3) 0.3034(2) 0.8583(2) 0.0224(9) Uani 1 1 d . . . N111 N 0.9915(2) 0.31880(19) 0.70357(16) 0.0205(7) Uani 1 1 d . . . C112 C 1.0160(3) 0.2912(2) 0.7708(2) 0.0229(9) Uani 1 1 d . . . S113 S 1.13979(8) 0.26610(7) 0.77248(6) 0.0317(3) Uani 1 1 d . . . C114 C 1.1570(3) 0.2945(2) 0.6787(2) 0.0273(9) Uani 1 1 d . . . H24 H 1.2177 0.2917 0.6506 0.033 Uiso 1 1 calc R . . C115 C 1.0703(3) 0.3218(2) 0.6510(2) 0.0216(8) Uani 1 1 d . . . N121 N 0.9505(2) 0.38457(18) 0.57138(16) 0.0205(7) Uani 1 1 d . . . C122 C 1.0460(3) 0.3554(2) 0.5756(2) 0.0220(9) Uani 1 1 d . . . C123 C 1.1118(3) 0.3547(2) 0.5144(2) 0.0259(9) Uani 1 1 d . . . H25 H 1.1764 0.3340 0.5189 0.031 Uiso 1 1 calc R . . C124 C 1.0797(3) 0.3857(2) 0.4459(2) 0.0285(10) Uani 1 1 d . . . H26 H 1.1221 0.3850 0.4035 0.034 Uiso 1 1 calc R . . C125 C 0.9836(3) 0.4176(2) 0.4415(2) 0.0286(10) Uani 1 1 d . . . H27 H 0.9612 0.4399 0.3960 0.034 Uiso 1 1 calc R . . C126 C 0.9221(3) 0.4161(2) 0.5045(2) 0.0252(9) Uani 1 1 d . . . H28 H 0.8577 0.4378 0.5009 0.030 Uiso 1 1 calc R . . O200 O 0.6520(2) 0.43412(18) 0.87962(15) 0.0306(7) Uani 1 1 d . . . C201 C 0.5887(3) 0.4969(3) 0.9008(2) 0.0312(10) Uani 1 1 d . . . H29A H 0.5292 0.4765 0.9301 0.037 Uiso 1 1 calc R . . H30B H 0.5695 0.5347 0.8575 0.037 Uiso 1 1 calc R . . C202 C 0.6451(4) 0.5346(3) 0.9442(2) 0.0375(11) Uani 1 1 d . . . H31C H 0.7090 0.5480 0.9175 0.045 Uiso 1 1 calc R . . H32D H 0.6090 0.5821 0.9519 0.045 Uiso 1 1 calc R . . O203 O 0.6586(2) 0.48218(19) 1.01322(15) 0.0363(8) Uani 1 1 d . . . C204 C 0.7135(4) 0.5187(4) 1.0547(3) 0.0570(16) Uani 1 1 d . . . H33E H 0.6755 0.5643 1.0653 0.068 Uiso 1 1 calc R . . H34F H 0.7752 0.5353 1.0262 0.068 Uiso 1 1 calc R . . C205 C 0.7347(4) 0.4618(4) 1.1252(3) 0.0498(14) Uani 1 1 d . . . H35G H 0.7602 0.4121 1.1155 0.060 Uiso 1 1 calc R . . H36H H 0.7839 0.4812 1.1480 0.060 Uiso 1 1 calc R . . O206 O 0.6461(2) 0.45265(18) 1.17211(15) 0.0342(7) Uani 1 1 d . . . C207 C 0.6650(4) 0.3983(4) 1.2396(2) 0.0517(15) Uani 1 1 d . . . H37I H 0.7169 0.4162 1.2610 0.062 Uiso 1 1 calc R . . H38J H 0.6873 0.3479 1.2300 0.062 Uiso 1 1 calc R . . C208 C 0.5766(4) 0.3908(4) 1.2902(3) 0.0540(15) Uani 1 1 d . . . H39K H 0.5914 0.3542 1.3354 0.065 Uiso 1 1 calc R . . H40L H 0.5575 0.4409 1.3017 0.065 Uiso 1 1 calc R . . O209 O 0.4938(2) 0.36510(19) 1.26394(16) 0.0360(8) Uani 1 1 d . . . C210 C 0.4901(4) 0.2852(3) 1.2697(2) 0.0461(14) Uani 1 1 d . . . H41A H 0.4311 0.2667 1.3009 0.055 Uiso 1 1 calc R . . H42B H 0.5471 0.2577 1.2925 0.055 Uiso 1 1 calc R . . C211 C 0.4891(4) 0.2675(3) 1.1961(3) 0.0432(12) Uani 1 1 d . . . H43C H 0.4650 0.2162 1.2023 0.052 Uiso 1 1 calc R . . H44D H 0.4453 0.3055 1.1669 0.052 Uiso 1 1 calc R . . O212 O 0.5866(2) 0.2699(2) 1.16020(15) 0.0402(8) Uani 1 1 d . . . C213 C 0.5882(3) 0.2785(3) 1.0843(2) 0.0355(11) Uani 1 1 d . . . H45E H 0.5623 0.3302 1.0614 0.043 Uiso 1 1 calc R . . H46F H 0.5481 0.2406 1.0743 0.043 Uiso 1 1 calc R . . C214 C 0.6940(3) 0.2657(3) 1.0549(2) 0.0326(11) Uani 1 1 d . . . H47G H 0.7347 0.3031 1.0650 0.039 Uiso 1 1 calc R . . H48H H 0.7199 0.2135 1.0765 0.039 Uiso 1 1 calc R . . O215 O 0.6917(2) 0.27652(18) 0.97704(14) 0.0321(7) Uani 1 1 d . . . O300 O 0.99597(19) 0.17070(16) 0.57073(14) 0.0237(6) Uani 1 1 d . . . C301 C 1.0946(3) 0.1509(3) 0.5404(2) 0.0266(9) Uani 1 1 d . . . H49A H 1.1121 0.0960 0.5591 0.032 Uiso 1 1 calc R . . H50B H 1.1421 0.1809 0.5540 0.032 Uiso 1 1 calc R . . C302 C 1.0958(3) 0.1691(3) 0.4580(2) 0.0288(10) Uani 1 1 d . . . H51C H 1.0641 0.2205 0.4407 0.035 Uiso 1 1 calc R . . H52D H 1.1636 0.1690 0.4353 0.035 Uiso 1 1 calc R . . O303 O 1.0450(2) 0.11270(17) 0.43873(14) 0.0281(7) Uani 1 1 d . . . C304 C 1.0572(3) 0.1180(3) 0.3620(2) 0.0304(10) Uani 1 1 d . . . H53E H 1.1269 0.1194 0.3441 0.037 Uiso 1 1 calc R . . H54F H 1.0235 0.1658 0.3368 0.037 Uiso 1 1 calc R . . C305 C 1.0154(3) 0.0494(3) 0.3459(2) 0.0319(10) Uani 1 1 d . . . H55G H 1.0389 0.0468 0.2959 0.038 Uiso 1 1 calc R . . H56H H 1.0406 0.0023 0.3782 0.038 Uiso 1 1 calc R . . O306 O 0.9102(2) 0.05139(18) 0.35445(14) 0.0305(7) Uani 1 1 d . . . C307 C 0.8671(3) 0.0960(3) 0.2896(2) 0.0349(11) Uani 1 1 d . . . H57I H 0.8936 0.0756 0.2474 0.042 Uiso 1 1 calc R . . H58J H 0.8828 0.1500 0.2798 0.042 Uiso 1 1 calc R . . C308 C 0.7583(3) 0.0899(3) 0.3027(2) 0.0351(11) Uani 1 1 d . . . H59K H 0.7291 0.1104 0.2570 0.042 Uiso 1 1 calc R . . H60L H 0.7434 0.0357 0.3206 0.042 Uiso 1 1 calc R . . O309 O 0.7174(2) 0.13277(17) 0.35510(14) 0.0286(7) Uani 1 1 d . . . C310 C 0.6159(3) 0.1207(3) 0.3787(2) 0.0279(10) Uani 1 1 d . . . H61A H 0.5826 0.1189 0.3367 0.034 Uiso 1 1 calc R . . H62B H 0.5862 0.1648 0.3972 0.034 Uiso 1 1 calc R . . C311 C 0.5982(3) 0.0474(2) 0.4371(2) 0.0266(9) Uani 1 1 d . . . H63C H 0.5274 0.0417 0.4478 0.032 Uiso 1 1 calc R . . H64D H 0.6274 0.0031 0.4187 0.032 Uiso 1 1 calc R . . O312 O 0.6385(2) 0.04695(16) 0.50343(14) 0.0254(6) Uani 1 1 d . . . C313 C 0.7381(3) 0.0132(2) 0.5077(2) 0.0246(9) Uani 1 1 d . . . H65E H 0.7575 -0.0098 0.4661 0.030 Uiso 1 1 calc R . . H66F H 0.7400 -0.0281 0.5519 0.030 Uiso 1 1 calc R . . C314 C 0.8105(3) 0.0712(2) 0.5082(2) 0.0243(9) Uani 1 1 d . . . H67G H 0.8772 0.0484 0.5004 0.029 Uiso 1 1 calc R . . H68H H 0.8016 0.1163 0.4679 0.029 Uiso 1 1 calc R . . O315 O 0.7991(2) 0.09599(15) 0.57676(14) 0.0228(6) Uani 1 1 d . . . Cl1 Cl 0.37018(7) 0.23633(6) 0.46994(5) 0.0239(2) Uani 1 1 d . . . O1A O 0.4634(2) 0.2708(2) 0.46058(17) 0.0403(8) Uani 1 1 d . . . O1B O 0.3241(2) 0.2304(2) 0.54367(15) 0.0366(8) Uani 1 1 d . . . O1C O 0.3061(2) 0.28444(19) 0.41975(15) 0.0368(8) Uani 1 1 d . . . O1D O 0.3845(3) 0.1609(2) 0.4547(2) 0.0514(10) Uani 1 1 d . . . Cl2 Cl 0.06883(8) 0.13529(7) 0.09759(6) 0.0357(3) Uani 1 1 d . . . O2A O -0.0184(3) 0.0929(2) 0.1039(2) 0.0539(10) Uani 1 1 d . . . O2B O 0.1537(2) 0.09230(19) 0.06964(16) 0.0385(8) Uani 1 1 d . . . O2C O 0.0843(3) 0.1466(2) 0.16758(17) 0.0460(9) Uani 1 1 d . . . O2D O 0.0555(3) 0.2098(2) 0.04759(18) 0.0551(10) Uani 1 1 d . . . Cl3 Cl 0.72420(9) 0.51808(7) 0.37935(6) 0.0348(3) Uani 1 1 d . . . O3A O 0.8134(3) 0.5033(3) 0.3358(2) 0.0748(13) Uani 1 1 d . . . O3B O 0.7485(3) 0.5496(2) 0.4381(2) 0.0550(10) Uani 1 1 d . . . O3C O 0.6776(4) 0.4475(2) 0.4096(2) 0.0796(16) Uani 1 1 d . . . O3D O 0.6616(3) 0.5718(3) 0.3363(2) 0.0783(14) Uani 1 1 d . . . Cl4 Cl 0.30236(8) 0.06702(8) 0.78860(6) 0.0480(4) Uani 1 1 d . . . O4A O 0.3900(2) 0.0160(2) 0.7864(2) 0.0637(12) Uani 1 1 d . . . O4B O 0.2743(2) 0.0987(2) 0.71605(17) 0.0455(9) Uani 1 1 d . . . O4C O 0.2235(2) 0.0228(3) 0.8317(2) 0.0727(15) Uani 1 1 d . . . O4D O 0.3213(3) 0.1294(3) 0.8189(2) 0.0805(14) Uani 1 1 d . . . N40A N -0.0242(9) 0.5939(7) 1.0206(6) 0.074(3) Uiso 0.50 1 d PD A 1 C40B C -0.0183(11) 0.6133(8) 0.9514(7) 0.078(4) Uiso 0.50 1 d PD A 1 C40C C 0.0128(8) 0.6463(6) 0.9048(5) 0.041(2) Uiso 0.50 1 d PD A 1 H69A H -0.0345 0.6867 0.8843 0.062 Uiso 0.50 1 calc PR A 1 H70B H 0.0339 0.6146 0.8705 0.062 Uiso 0.50 1 calc PR A 1 H71C H 0.0690 0.6693 0.9148 0.062 Uiso 0.50 1 calc PR A 1 C40D C 0.0844(9) 0.5371(8) 1.0480(7) 0.071(4) Uiso 0.50 1 d PD B 2 H72A H 0.0996 0.5637 0.9976 0.107 Uiso 0.50 1 calc PR B 2 H73B H 0.0841 0.4822 1.0516 0.107 Uiso 0.50 1 calc PR B 2 H74C H 0.1335 0.5464 1.0766 0.107 Uiso 0.50 1 calc PR B 2 C40E C -0.0147(6) 0.5665(5) 1.0761(4) 0.0232(17) Uiso 0.50 1 d PD B 2 N40F N -0.0701(8) 0.5830(6) 1.0998(5) 0.058(3) Uiso 0.50 1 d PD B 2 C403 C 0.1679(4) 0.7119(3) 0.6240(3) 0.0489(14) Uani 1 1 d . . . H75D H 0.1215 0.7315 0.5886 0.073 Uiso 1 1 calc R . . H76E H 0.2042 0.6663 0.6134 0.073 Uiso 1 1 calc R . . H77F H 0.2131 0.7511 0.6219 0.073 Uiso 1 1 calc R . . C404 C 0.1154(4) 0.6921(3) 0.6964(4) 0.0558(15) Uani 1 1 d . . . N405 N 0.0747(4) 0.6778(3) 0.7537(3) 0.0774(17) Uani 1 1 d . . . C406 C 0.2597(5) 0.2675(4) 0.9499(4) 0.081(2) Uani 1 1 d . . . H78G H 0.2179 0.3125 0.9305 0.121 Uiso 1 1 calc R . . H79H H 0.2274 0.2211 0.9516 0.121 Uiso 1 1 calc R . . H80I H 0.3211 0.2681 0.9189 0.121 Uiso 1 1 calc R . . C407 C 0.2793(5) 0.2688(4) 1.0241(5) 0.075(2) Uani 1 1 d . . . N408 N 0.2948(5) 0.2711(4) 1.0817(4) 0.098(2) Uani 1 1 d . . . O400 O 0.1447(9) 0.1357(7) 0.9164(6) 0.116(4) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0185(2) 0.0302(3) 0.0200(2) 0.00013(18) -0.01140(18) 0.0073(2) Zn2 0.0145(2) 0.0270(3) 0.0200(2) -0.00226(18) -0.00771(17) 0.00828(19) N11 0.0260(19) 0.029(2) 0.0225(17) -0.0011(14) -0.0097(14) 0.0029(16) C12 0.022(2) 0.032(3) 0.038(2) -0.0054(19) -0.0054(18) 0.0034(19) C13 0.029(3) 0.033(3) 0.042(3) -0.003(2) 0.001(2) 0.000(2) C14 0.040(3) 0.036(3) 0.030(2) -0.0017(19) 0.008(2) -0.001(2) C15 0.039(3) 0.030(3) 0.024(2) 0.0042(17) -0.0090(19) 0.004(2) C16 0.029(2) 0.026(2) 0.021(2) 0.0026(16) -0.0119(17) 0.0014(19) N21 0.0221(18) 0.0233(18) 0.0195(16) 0.0027(13) -0.0110(13) 0.0062(15) C22 0.023(2) 0.024(2) 0.026(2) 0.0016(16) -0.0110(17) 0.0050(18) S23 0.0274(6) 0.0343(6) 0.0264(5) 0.0036(4) -0.0188(4) 0.0076(5) C24 0.034(3) 0.034(3) 0.022(2) 0.0042(17) -0.0142(18) 0.005(2) C25 0.029(2) 0.024(2) 0.022(2) 0.0043(16) -0.0099(17) 0.0046(18) N31 0.0137(16) 0.0209(17) 0.0192(16) 0.0005(13) -0.0102(12) 0.0067(13) C32 0.018(2) 0.021(2) 0.025(2) 0.0031(16) -0.0119(16) 0.0025(17) C33 0.017(2) 0.026(2) 0.031(2) -0.0025(17) -0.0132(17) 0.0095(17) C34 0.0108(19) 0.032(2) 0.031(2) -0.0088(18) -0.0073(16) 0.0080(17) C35 0.018(2) 0.023(2) 0.0227(19) -0.0028(16) -0.0063(15) 0.0036(17) C36 0.0121(18) 0.018(2) 0.0244(19) -0.0029(15) -0.0098(15) 0.0056(15) N41 0.0117(15) 0.0231(18) 0.0163(15) 0.0003(12) -0.0045(12) 0.0047(13) C42 0.0136(19) 0.029(2) 0.0155(17) 0.0018(15) -0.0043(14) 0.0036(17) C43 0.017(2) 0.030(2) 0.0224(19) 0.0008(16) -0.0100(16) 0.0043(18) C44 0.020(2) 0.026(2) 0.0205(19) -0.0021(16) -0.0099(16) 0.0044(17) C45 0.017(2) 0.023(2) 0.0167(18) 0.0023(15) -0.0043(15) 0.0036(17) C46 0.0108(18) 0.025(2) 0.0155(17) 0.0007(15) -0.0015(14) 0.0009(16) N51 0.0177(17) 0.0249(18) 0.0144(15) 0.0000(13) -0.0037(12) 0.0061(14) C52 0.0156(19) 0.023(2) 0.0163(18) 0.0030(15) -0.0024(14) 0.0073(16) S53 0.0278(6) 0.0362(6) 0.0273(5) -0.0061(4) -0.0170(4) 0.0195(5) C54 0.033(3) 0.030(2) 0.028(2) -0.0052(18) -0.0093(18) 0.018(2) C55 0.021(2) 0.026(2) 0.0148(17) 0.0005(15) -0.0013(15) 0.0087(17) N61 0.0246(19) 0.030(2) 0.0246(18) -0.0015(14) -0.0065(14) 0.0060(16) C62 0.025(2) 0.026(2) 0.0160(18) 0.0041(15) -0.0002(15) 0.0039(18) C63 0.037(3) 0.030(2) 0.022(2) -0.0025(17) -0.0024(18) 0.011(2) C64 0.053(3) 0.032(3) 0.026(2) -0.0056(19) -0.004(2) 0.000(2) C65 0.044(3) 0.042(3) 0.033(2) -0.007(2) -0.014(2) -0.002(2) C66 0.037(3) 0.038(3) 0.031(2) -0.004(2) -0.016(2) 0.002(2) N71 0.0151(17) 0.032(2) 0.0184(16) 0.0009(13) -0.0074(13) 0.0034(15) C72 0.020(2) 0.031(2) 0.024(2) 0.0014(17) -0.0069(16) 0.0037(18) C73 0.024(2) 0.032(3) 0.029(2) 0.0005(18) -0.0037(17) 0.0038(19) C74 0.026(2) 0.032(3) 0.030(2) -0.0084(18) -0.0006(17) -0.0028(19) C75 0.020(2) 0.037(3) 0.027(2) 0.0018(18) -0.0090(17) -0.0060(19) C76 0.0140(19) 0.030(2) 0.0179(18) 0.0014(16) -0.0038(15) -0.0025(17) N81 0.0158(17) 0.0249(19) 0.0197(16) 0.0052(13) -0.0072(13) 0.0025(14) C82 0.0149(19) 0.032(2) 0.0195(19) 0.0062(16) -0.0038(15) 0.0044(17) S83 0.0169(5) 0.0349(6) 0.0254(5) 0.0037(4) -0.0121(4) 0.0050(4) C84 0.019(2) 0.033(2) 0.0205(19) 0.0016(17) -0.0078(16) -0.0038(18) C85 0.015(2) 0.034(2) 0.0208(19) 0.0024(17) -0.0051(15) -0.0028(18) N91 0.0117(16) 0.031(2) 0.0157(15) 0.0028(13) -0.0044(12) 0.0064(14) C92 0.0136(19) 0.033(2) 0.0170(18) 0.0038(16) -0.0078(15) 0.0051(17) C93 0.021(2) 0.034(3) 0.026(2) 0.0034(18) -0.0100(17) 0.0108(19) C94 0.023(2) 0.033(3) 0.029(2) 0.0001(18) -0.0086(17) 0.0107(19) C95 0.023(2) 0.031(2) 0.0178(19) -0.0017(16) -0.0014(16) 0.0055(18) C96 0.017(2) 0.026(2) 0.0168(18) 0.0023(15) -0.0051(15) 0.0066(17) N101 0.0167(17) 0.0239(18) 0.0176(15) -0.0001(13) -0.0085(13) 0.0034(14) C102 0.019(2) 0.021(2) 0.0208(19) 0.0005(15) -0.0100(15) 0.0051(16) C103 0.021(2) 0.030(2) 0.022(2) -0.0045(16) -0.0124(16) 0.0059(18) C104 0.028(2) 0.032(2) 0.0178(19) -0.0002(16) -0.0109(16) 0.0068(19) C105 0.024(2) 0.033(2) 0.020(2) -0.0007(17) -0.0083(16) 0.0066(19) C106 0.020(2) 0.025(2) 0.0194(19) -0.0007(15) -0.0083(15) 0.0071(17) N111 0.0150(16) 0.0241(18) 0.0212(16) -0.0025(13) -0.0061(13) 0.0038(14) C112 0.016(2) 0.025(2) 0.026(2) 0.0001(16) -0.0111(16) 0.0054(17) S113 0.0158(5) 0.0439(7) 0.0301(5) 0.0029(5) -0.0114(4) 0.0073(5) C114 0.015(2) 0.031(2) 0.030(2) 0.0016(18) -0.0010(16) 0.0034(18) C115 0.017(2) 0.020(2) 0.026(2) -0.0032(16) -0.0060(16) 0.0041(16) N121 0.0171(17) 0.0187(17) 0.0226(16) 0.0004(13) -0.0055(13) 0.0058(14) C122 0.022(2) 0.017(2) 0.024(2) 0.0011(15) -0.0047(16) 0.0019(17) C123 0.019(2) 0.026(2) 0.030(2) -0.0014(17) -0.0031(17) 0.0030(18) C124 0.030(2) 0.029(2) 0.024(2) -0.0040(17) 0.0039(17) -0.0009(19) C125 0.034(3) 0.029(2) 0.019(2) 0.0009(16) -0.0045(17) 0.000(2) C126 0.020(2) 0.030(2) 0.023(2) -0.0007(17) -0.0093(16) 0.0028(18) O200 0.0247(16) 0.0379(19) 0.0287(15) -0.0076(13) -0.0100(12) 0.0090(14) C201 0.032(2) 0.032(3) 0.026(2) -0.0021(18) -0.0076(18) 0.012(2) C202 0.042(3) 0.041(3) 0.025(2) 0.0016(19) -0.009(2) 0.005(2) O203 0.0383(19) 0.046(2) 0.0217(15) -0.0039(13) -0.0108(13) 0.0087(16) C204 0.055(4) 0.085(5) 0.030(3) 0.001(3) -0.015(2) -0.024(3) C205 0.036(3) 0.078(4) 0.033(3) -0.008(3) -0.012(2) 0.007(3) O206 0.0331(18) 0.0408(19) 0.0242(15) 0.0003(13) -0.0076(13) 0.0054(15) C207 0.047(3) 0.077(4) 0.026(2) 0.004(2) -0.013(2) -0.005(3) C208 0.045(3) 0.075(4) 0.038(3) 0.000(3) -0.016(2) -0.003(3) O209 0.0357(19) 0.0385(19) 0.0311(16) -0.0011(13) -0.0108(14) 0.0021(15) C210 0.066(4) 0.034(3) 0.027(2) 0.0002(19) 0.013(2) 0.010(3) C211 0.043(3) 0.036(3) 0.044(3) -0.003(2) 0.009(2) -0.002(2) O212 0.0397(19) 0.055(2) 0.0185(15) -0.0028(14) 0.0026(13) 0.0138(17) C213 0.031(3) 0.042(3) 0.024(2) 0.0025(19) -0.0020(18) 0.011(2) C214 0.033(3) 0.045(3) 0.0144(19) -0.0002(17) -0.0047(17) 0.008(2) O215 0.0244(16) 0.051(2) 0.0141(13) 0.0023(12) -0.0040(11) 0.0103(14) O300 0.0144(14) 0.0301(16) 0.0243(14) -0.0045(11) -0.0030(11) 0.0070(12) C301 0.014(2) 0.032(2) 0.033(2) -0.0085(18) -0.0019(16) 0.0059(18) C302 0.020(2) 0.033(3) 0.033(2) -0.0090(18) -0.0001(17) 0.0019(19) O303 0.0260(16) 0.0341(18) 0.0250(15) -0.0080(12) -0.0034(12) -0.0014(13) C304 0.021(2) 0.044(3) 0.026(2) -0.0099(19) -0.0009(17) 0.005(2) C305 0.026(2) 0.040(3) 0.029(2) -0.0094(19) -0.0046(18) 0.007(2) O306 0.0232(16) 0.0425(19) 0.0237(14) -0.0039(13) -0.0066(12) 0.0036(14) C307 0.031(3) 0.051(3) 0.020(2) -0.0011(19) -0.0087(18) 0.005(2) C308 0.037(3) 0.043(3) 0.024(2) -0.0051(19) -0.0111(19) 0.005(2) O309 0.0275(16) 0.0319(17) 0.0255(15) -0.0031(12) -0.0082(12) -0.0001(13) C310 0.022(2) 0.033(3) 0.028(2) -0.0054(18) -0.0108(17) 0.0054(19) C311 0.019(2) 0.032(2) 0.030(2) -0.0061(18) -0.0130(17) 0.0027(18) O312 0.0196(15) 0.0291(16) 0.0279(15) -0.0054(12) -0.0112(12) 0.0054(12) C313 0.019(2) 0.027(2) 0.028(2) -0.0058(17) -0.0116(16) 0.0072(18) C314 0.020(2) 0.026(2) 0.025(2) -0.0026(16) -0.0084(16) 0.0053(18) O315 0.0239(15) 0.0205(15) 0.0242(14) -0.0048(11) -0.0098(11) 0.0056(12) Cl1 0.0174(5) 0.0287(5) 0.0239(5) -0.0028(4) -0.0081(4) 0.0065(4) O1A 0.0226(17) 0.057(2) 0.0437(19) -0.0147(16) -0.0055(14) -0.0057(16) O1B 0.0237(16) 0.059(2) 0.0208(15) 0.0019(14) -0.0074(12) 0.0070(15) O1C 0.0282(17) 0.054(2) 0.0212(15) 0.0023(13) -0.0097(12) 0.0151(15) O1D 0.045(2) 0.029(2) 0.081(3) -0.0224(18) 0.0004(19) 0.0054(17) Cl2 0.0324(6) 0.0422(7) 0.0315(6) -0.0047(5) -0.0166(5) 0.0099(5) O2A 0.0286(19) 0.077(3) 0.065(2) -0.032(2) -0.0060(17) -0.0064(19) O2B 0.0334(18) 0.043(2) 0.0374(18) -0.0077(14) -0.0097(14) 0.0109(16) O2C 0.040(2) 0.067(3) 0.0359(18) -0.0176(16) -0.0176(15) 0.0075(18) O2D 0.063(3) 0.052(2) 0.045(2) 0.0037(17) -0.0328(18) 0.018(2) Cl3 0.0382(6) 0.0313(6) 0.0345(6) -0.0028(4) -0.0175(5) 0.0055(5) O3A 0.047(3) 0.093(4) 0.087(3) -0.033(3) -0.010(2) 0.022(2) O3B 0.069(3) 0.048(2) 0.055(2) -0.0154(17) -0.031(2) 0.003(2) O3C 0.157(5) 0.052(3) 0.037(2) -0.0160(18) 0.005(2) -0.049(3) O3D 0.064(3) 0.088(3) 0.078(3) -0.001(2) -0.049(2) 0.034(3) Cl4 0.0209(6) 0.0704(9) 0.0381(6) 0.0220(6) -0.0163(5) -0.0040(6) O4A 0.0252(19) 0.075(3) 0.063(2) 0.037(2) -0.0100(17) 0.0067(19) O4B 0.0300(18) 0.060(2) 0.0358(18) 0.0178(15) -0.0201(14) -0.0065(17) O4C 0.0218(19) 0.113(4) 0.052(2) 0.043(2) -0.0090(16) -0.004(2) O4D 0.059(3) 0.120(4) 0.076(3) -0.034(3) -0.046(2) 0.007(3) C403 0.043(3) 0.042(3) 0.057(3) 0.001(2) -0.013(3) 0.001(3) C404 0.039(3) 0.040(3) 0.083(5) -0.004(3) -0.010(3) 0.002(3) N405 0.063(4) 0.069(4) 0.088(4) -0.004(3) 0.010(3) -0.004(3) C406 0.064(5) 0.092(6) 0.081(5) -0.009(4) -0.026(4) 0.011(4) C407 0.070(5) 0.046(4) 0.115(6) -0.014(4) -0.040(5) -0.004(3) N408 0.118(6) 0.070(4) 0.116(6) -0.007(4) -0.062(5) -0.026(4) O400 0.108(9) 0.131(10) 0.091(8) -0.012(7) -0.019(7) 0.057(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 N21 1.999(3) . ? Zn1 N81 2.001(3) . ? Zn1 N71 2.176(4) . ? Zn1 N11 2.264(3) . ? Zn1 N31 2.413(3) . ? Zn1 N91 2.465(3) . ? Zn2 N51 1.997(3) . ? Zn2 N111 1.999(3) . ? Zn2 N121 2.243(3) . ? Zn2 N61 2.243(4) . ? Zn2 N41 2.376(3) . ? Zn2 N101 2.382(3) . ? N11 C12 1.335(5) . ? N11 C16 1.355(5) . ? C12 C13 1.383(6) . ? C13 C14 1.379(6) . ? C14 C15 1.390(7) . ? C15 C16 1.382(6) . ? C16 C25 1.464(6) . ? N21 C22 1.304(5) . ? N21 C25 1.361(5) . ? C22 C32 1.453(6) . ? C22 S23 1.712(4) . ? S23 C24 1.707(5) . ? C24 C25 1.368(5) . ? N31 C36 1.335(5) . ? N31 C32 1.359(4) . ? C32 C33 1.384(5) . ? C33 C34 1.379(6) . ? C34 C35 1.396(5) . ? C35 O300 1.350(4) . ? C35 C36 1.397(5) . ? C36 C46 1.495(5) . ? N41 C46 1.337(5) . ? N41 C42 1.356(4) . ? C42 C43 1.387(5) . ? C42 C52 1.469(6) . ? C43 C44 1.377(6) . ? C44 C45 1.392(5) . ? C45 O315 1.351(5) . ? C45 C46 1.395(5) . ? N51 C52 1.307(5) . ? N51 C55 1.363(5) . ? C52 S53 1.710(4) . ? S53 C54 1.712(5) . ? C54 C55 1.360(5) . ? C55 C62 1.477(6) . ? N61 C66 1.340(5) . ? N61 C62 1.344(5) . ? C62 C63 1.385(6) . ? C63 C64 1.385(6) . ? C64 C65 1.381(7) . ? C65 C66 1.376(7) . ? N71 C76 1.350(4) . ? N71 C72 1.358(5) . ? C72 C73 1.365(6) . ? C73 C74 1.391(6) . ? C74 C75 1.378(6) . ? C75 C76 1.386(6) . ? C76 C85 1.474(6) . ? N81 C82 1.311(5) . ? N81 C85 1.354(5) . ? C82 C92 1.460(6) . ? C82 S83 1.715(4) . ? S83 C84 1.715(4) . ? C84 C85 1.368(5) . ? N91 C96 1.326(5) . ? N91 C92 1.369(4) . ? C92 C93 1.383(6) . ? C93 C94 1.383(6) . ? C94 C95 1.384(5) . ? C95 O200 1.338(5) . ? C95 C96 1.414(6) . ? C96 C106 1.487(5) . ? N101 C106 1.326(5) . ? N101 C102 1.357(5) . ? C102 C103 1.381(5) . ? C102 C112 1.460(6) . ? C103 C104 1.377(6) . ? C104 C105 1.381(5) . ? C105 O215 1.340(5) . ? C105 C106 1.410(5) . ? N111 C112 1.318(5) . ? N111 C115 1.366(5) . ? C112 S113 1.709(4) . ? S113 C114 1.712(4) . ? C114 C115 1.354(5) . ? C115 C122 1.469(5) . ? N121 C126 1.340(5) . ? N121 C122 1.361(5) . ? C122 C123 1.376(6) . ? C123 C124 1.385(5) . ? C124 C125 1.383(6) . ? C125 C126 1.366(6) . ? O200 C201 1.450(5) . ? C201 C202 1.493(6) . ? C202 O203 1.427(5) . ? O203 C204 1.441(6) . ? C204 C205 1.504(7) . ? C205 O206 1.405(6) . ? O206 C207 1.434(5) . ? C207 C208 1.438(7) . ? C208 O209 1.441(6) . ? O209 C210 1.399(6) . ? C210 C211 1.500(7) . ? C211 O212 1.416(6) . ? O212 C213 1.403(5) . ? C213 C214 1.498(6) . ? C214 O215 1.440(4) . ? O300 C301 1.443(5) . ? C301 C302 1.509(5) . ? C302 O303 1.408(5) . ? O303 C304 1.420(5) . ? C304 C305 1.499(6) . ? C305 O306 1.422(5) . ? O306 C307 1.447(5) . ? C307 C308 1.483(6) . ? C308 O309 1.423(5) . ? O309 C310 1.421(5) . ? C310 C311 1.502(6) . ? C311 O312 1.428(4) . ? O312 C313 1.437(4) . ? C313 C314 1.492(6) . ? C314 O315 1.454(5) . ? Cl1 O1D 1.429(3) . ? Cl1 O1A 1.433(3) . ? Cl1 O1C 1.438(3) . ? Cl1 O1B 1.439(3) . ? Cl2 O2C 1.428(3) . ? Cl2 O2D 1.435(3) . ? Cl2 O2A 1.442(4) . ? Cl2 O2B 1.444(3) . ? Cl3 O3D 1.395(4) . ? Cl3 O3C 1.416(4) . ? Cl3 O3A 1.423(4) . ? Cl3 O3B 1.443(4) . ? Cl4 O4D 1.420(5) . ? Cl4 O4B 1.434(3) . ? Cl4 O4A 1.434(4) . ? Cl4 O4C 1.435(4) . ? N40A C40B 1.262(13) . ? C40B C40C 1.000(12) . ? C40D C40E 1.487(12) . ? C40E N40F 0.893(10) . ? C403 C404 1.441(8) . ? C404 N405 1.134(8) . ? C406 C407 1.465(10) . ? C407 N408 1.146(9) . ? 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 N21 Zn1 N81 175.66(14) . . ? N21 Zn1 N71 106.91(13) . . ? N81 Zn1 N71 76.14(13) . . ? N21 Zn1 N11 74.99(13) . . ? N81 Zn1 N11 101.42(13) . . ? N71 Zn1 N11 103.57(13) . . ? N21 Zn1 N31 72.10(12) . . ? N81 Zn1 N31 111.30(11) . . ? N71 Zn1 N31 89.31(12) . . ? N11 Zn1 N31 146.90(11) . . ? N21 Zn1 N91 106.14(12) . . ? N81 Zn1 N91 71.04(12) . . ? N71 Zn1 N91 146.80(11) . . ? N11 Zn1 N91 87.96(12) . . ? N31 Zn1 N91 97.78(11) . . ? N51 Zn2 N111 172.44(13) . . ? N51 Zn2 N121 99.17(12) . . ? N111 Zn2 N121 75.08(12) . . ? N51 Zn2 N61 74.94(13) . . ? N111 Zn2 N61 101.60(13) . . ? N121 Zn2 N61 105.35(13) . . ? N51 Zn2 N41 72.33(12) . . ? N111 Zn2 N41 111.55(12) . . ? N121 Zn2 N41 85.26(11) . . ? N61 Zn2 N41 146.82(11) . . ? N51 Zn2 N101 113.51(12) . . ? N111 Zn2 N101 72.33(12) . . ? N121 Zn2 N101 147.32(11) . . ? N61 Zn2 N101 83.64(12) . . ? N41 Zn2 N101 104.46(11) . . ? C12 N11 C16 117.8(4) . . ? C12 N11 Zn1 128.8(3) . . ? C16 N11 Zn1 113.4(3) . . ? N11 C12 C13 123.5(4) . . ? C14 C13 C12 118.4(4) . . ? C13 C14 C15 119.3(4) . . ? C16 C15 C14 118.7(4) . . ? N11 C16 C15 122.3(4) . . ? N11 C16 C25 114.3(3) . . ? C15 C16 C25 123.3(4) . . ? C22 N21 C25 113.5(3) . . ? C22 N21 Zn1 124.5(3) . . ? C25 N21 Zn1 122.0(3) . . ? N21 C22 C32 118.7(3) . . ? N21 C22 S23 112.6(3) . . ? C32 C22 S23 128.7(3) . . ? C24 S23 C22 90.4(2) . . ? C25 C24 S23 110.0(3) . . ? N21 C25 C24 113.5(4) . . ? N21 C25 C16 115.2(3) . . ? C24 C25 C16 131.3(4) . . ? C36 N31 C32 117.9(3) . . ? C36 N31 Zn1 130.4(2) . . ? C32 N31 Zn1 110.4(2) . . ? N31 C32 C33 122.3(4) . . ? N31 C32 C22 113.0(3) . . ? C33 C32 C22 124.7(3) . . ? C34 C33 C32 119.8(3) . . ? C33 C34 C35 118.5(4) . . ? O300 C35 C34 125.8(4) . . ? O300 C35 C36 115.5(3) . . ? C34 C35 C36 118.6(3) . . ? N31 C36 C35 122.9(3) . . ? N31 C36 C46 115.3(3) . . ? C35 C36 C46 121.7(3) . . ? C46 N41 C42 118.0(3) . . ? C46 N41 Zn2 129.0(2) . . ? C42 N41 Zn2 110.9(3) . . ? N41 C42 C43 121.9(4) . . ? N41 C42 C52 112.3(3) . . ? C43 C42 C52 125.8(3) . . ? C44 C43 C42 119.5(3) . . ? C43 C44 C45 119.2(4) . . ? O315 C45 C44 125.6(4) . . ? O315 C45 C46 116.3(3) . . ? C44 C45 C46 118.0(4) . . ? N41 C46 C45 123.3(3) . . ? N41 C46 C36 114.9(3) . . ? C45 C46 C36 121.8(3) . . ? C52 N51 C55 113.7(3) . . ? C52 N51 Zn2 123.6(3) . . ? C55 N51 Zn2 121.9(3) . . ? N51 C52 C42 117.8(3) . . ? N51 C52 S53 112.6(3) . . ? C42 C52 S53 129.6(3) . . ? C52 S53 C54 90.1(2) . . ? C55 C54 S53 110.5(3) . . ? C54 C55 N51 113.1(4) . . ? C54 C55 C62 132.5(4) . . ? N51 C55 C62 114.3(3) . . ? C66 N61 C62 117.9(4) . . ? C66 N61 Zn2 127.5(3) . . ? C62 N61 Zn2 114.4(3) . . ? N61 C62 C63 123.0(4) . . ? N61 C62 C55 113.7(4) . . ? C63 C62 C55 123.4(4) . . ? C64 C63 C62 118.2(4) . . ? C65 C64 C63 119.0(4) . . ? C66 C65 C64 119.2(4) . . ? N61 C66 C65 122.7(4) . . ? C76 N71 C72 117.7(4) . . ? C76 N71 Zn1 115.2(3) . . ? C72 N71 Zn1 127.2(3) . . ? N71 C72 C73 122.6(4) . . ? C72 C73 C74 119.3(4) . . ? C75 C74 C73 119.0(4) . . ? C74 C75 C76 118.9(4) . . ? N71 C76 C75 122.5(4) . . ? N71 C76 C85 113.4(4) . . ? C75 C76 C85 124.0(3) . . ? C82 N81 C85 113.9(3) . . ? C82 N81 Zn1 125.6(3) . . ? C85 N81 Zn1 120.4(3) . . ? N81 C82 C92 118.1(3) . . ? N81 C82 S83 112.4(3) . . ? C92 C82 S83 129.4(3) . . ? C84 S83 C82 90.0(2) . . ? C85 C84 S83 110.4(3) . . ? N81 C85 C84 113.2(4) . . ? N81 C85 C76 114.8(3) . . ? C84 C85 C76 132.0(4) . . ? C96 N91 C92 118.1(3) . . ? C96 N91 Zn1 129.6(2) . . ? C92 N91 Zn1 108.9(3) . . ? N91 C92 C93 122.0(4) . . ? N91 C92 C82 112.7(3) . . ? C93 C92 C82 125.3(3) . . ? C94 C93 C92 119.4(4) . . ? C93 C94 C95 119.5(4) . . ? O200 C95 C94 126.0(4) . . ? O200 C95 C96 116.1(3) . . ? C94 C95 C96 117.8(4) . . ? N91 C96 C95 123.1(3) . . ? N91 C96 C106 115.7(3) . . ? C95 C96 C106 121.1(4) . . ? C106 N101 C102 118.1(3) . . ? C106 N101 Zn2 129.4(2) . . ? C102 N101 Zn2 111.5(2) . . ? N101 C102 C103 122.2(4) . . ? N101 C102 C112 113.0(3) . . ? C103 C102 C112 124.8(3) . . ? C104 C103 C102 119.9(4) . . ? C103 C104 C105 118.3(3) . . ? O215 C105 C104 126.5(3) . . ? O215 C105 C106 114.4(3) . . ? C104 C105 C106 119.0(4) . . ? N101 C106 C105 122.4(4) . . ? N101 C106 C96 116.7(3) . . ? C105 C106 C96 120.9(4) . . ? C112 N111 C115 113.3(3) . . ? C112 N111 Zn2 124.3(3) . . ? C115 N111 Zn2 122.1(2) . . ? N111 C112 C102 117.6(3) . . ? N111 C112 S113 112.4(3) . . ? C102 C112 S113 130.0(3) . . ? C112 S113 C114 90.21(19) . . ? C115 C114 S113 110.7(3) . . ? C114 C115 N111 113.3(3) . . ? C114 C115 C122 132.1(4) . . ? N111 C115 C122 114.6(3) . . ? C126 N121 C122 117.7(3) . . ? C126 N121 Zn2 128.0(3) . . ? C122 N121 Zn2 114.1(2) . . ? N121 C122 C123 122.5(3) . . ? N121 C122 C115 113.9(3) . . ? C123 C122 C115 123.6(4) . . ? C122 C123 C124 118.6(4) . . ? C125 C124 C123 119.0(4) . . ? C126 C125 C124 119.3(4) . . ? N121 C126 C125 122.8(4) . . ? C95 O200 C201 116.8(3) . . ? O200 C201 C202 108.1(4) . . ? O203 C202 C201 109.4(4) . . ? C202 O203 C204 109.1(4) . . ? O203 C204 C205 109.5(5) . . ? O206 C205 C204 108.3(4) . . ? C205 O206 C207 109.0(4) . . ? O206 C207 C208 110.2(4) . . ? O209 C208 C207 114.5(4) . . ? C210 O209 C208 118.0(4) . . ? O209 C210 C211 111.8(4) . . ? O212 C211 C210 108.7(4) . . ? C213 O212 C211 112.2(4) . . ? O212 C213 C214 107.1(3) . . ? O215 C214 C213 104.8(3) . . ? C105 O215 C214 118.4(3) . . ? C35 O300 C301 116.4(3) . . ? O300 C301 C302 107.8(3) . . ? O303 C302 C301 109.1(3) . . ? C302 O303 C304 112.4(3) . . ? O303 C304 C305 110.0(4) . . ? O306 C305 C304 114.2(4) . . ? C305 O306 C307 112.7(3) . . ? O306 C307 C308 108.2(3) . . ? O309 C308 C307 109.8(4) . . ? C310 O309 C308 113.2(3) . . ? O309 C310 C311 114.1(3) . . ? O312 C311 C310 112.9(3) . . ? C311 O312 C313 114.6(3) . . ? O312 C313 C314 112.8(3) . . ? O315 C314 C313 112.2(3) . . ? C45 O315 C314 118.5(3) . . ? O1D Cl1 O1A 109.9(2) . . ? O1D Cl1 O1C 108.7(2) . . ? O1A Cl1 O1C 109.3(2) . . ? O1D Cl1 O1B 110.0(2) . . ? O1A Cl1 O1B 110.14(19) . . ? O1C Cl1 O1B 108.73(17) . . ? O2C Cl2 O2D 109.2(2) . . ? O2C Cl2 O2A 110.1(2) . . ? O2D Cl2 O2A 108.9(2) . . ? O2C Cl2 O2B 109.75(19) . . ? O2D Cl2 O2B 109.3(2) . . ? O2A Cl2 O2B 109.5(2) . . ? O3D Cl3 O3C 110.4(3) . . ? O3D Cl3 O3A 109.7(3) . . ? O3C Cl3 O3A 109.5(3) . . ? O3D Cl3 O3B 109.5(3) . . ? O3C Cl3 O3B 109.2(2) . . ? O3A Cl3 O3B 108.5(3) . . ? O4D Cl4 O4B 108.6(3) . . ? O4D Cl4 O4A 109.2(3) . . ? O4B Cl4 O4A 110.5(2) . . ? O4D Cl4 O4C 111.5(3) . . ? O4B Cl4 O4C 108.6(2) . . ? O4A Cl4 O4C 108.4(2) . . ? C40C C40B N40A 147.6(18) . . ? N40F C40E C40D 170.9(12) . . ? N405 C404 C403 178.7(7) . . ? N408 C407 C406 178.8(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.329 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.098 # Attachment '637342.cif' data_craig28m _database_code_depnum_ccdc_archive 'CCDC 637342' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H80.50 Ba2 Cl8 N15.50 O45 S4 Zn2' _chemical_formula_weight 2784.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -1.0456 8.4617 '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 16.9511(3) _cell_length_b 18.4571(3) _cell_length_c 20.1644(4) _cell_angle_alpha 108.4580(10) _cell_angle_beta 103.3020(10) _cell_angle_gamma 110.4970(10) _cell_volume 5176.26(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5770 _cell_measurement_theta_min 5.679 _cell_measurement_theta_max 140.014 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2790 _exptl_absorpt_coefficient_mu 9.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.241044 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source '4.8 kW rotating anode' _diffrn_radiation_monochromator 'Osmic ConFocal MaxFlux mirror optics' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Frames, each covering 0.3 \% in \w' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker-AXS SMART 6000' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'three-circle diffractometer' _diffrn_specimen_support 'glass fibre' _diffrn_radiation_collimation 'Osmic CMF12-38Cu6 (blue) mirror optics' _diffrn_radiation_probe X-ray _diffrn_source rotating-anode _diffrn_source_current 120 _diffrn_source_power 4.8 _diffrn_source_size '3 x 0.3mm' _diffrn_source_target Cu _diffrn_source_type 'MAC Science M18XCE' _diffrn_source_voltage 40 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41199 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0845 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 70.12 _reflns_number_total 17747 _reflns_number_gt 13016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _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^)+(0.0763P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17747 _refine_ls_number_parameters 1388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.096 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.44980(5) 0.66819(5) 0.23250(4) 0.01845(18) Uani 1 1 d . . . Zn2 Zn 0.18298(5) 0.46909(5) 0.27181(4) 0.01731(18) Uani 1 1 d . . . Ba1 Ba 0.16130(3) 0.85872(2) 0.32626(2) 0.02243(11) Uani 1 1 d . . . Ba2 Ba 0.44872(2) 0.24035(2) 0.196909(19) 0.01590(10) Uani 1 1 d . . . O1 O 0.0712(4) 0.8298(4) 0.1853(3) 0.0544(16) Uani 1 1 d . . . N11 N 0.5624(3) 0.6460(3) 0.1992(3) 0.0194(11) Uani 1 1 d . . . C12 C 0.6350(4) 0.6682(4) 0.2592(4) 0.0211(14) Uani 1 1 d . . . C13 C 0.7115(4) 0.6600(4) 0.2517(4) 0.0263(15) Uani 1 1 d . . . H1 H 0.7616 0.6759 0.2938 0.032 Uiso 1 1 calc R . . C14 C 0.7104(5) 0.6271(5) 0.1787(4) 0.0312(17) Uani 1 1 d . . . H2 H 0.7601 0.6202 0.1716 0.037 Uiso 1 1 calc R . . C15 C 0.6364(5) 0.6050(4) 0.1179(4) 0.0288(16) Uani 1 1 d . . . H3 H 0.6349 0.5836 0.0690 0.035 Uiso 1 1 calc R . . C16 C 0.5646(5) 0.6153(4) 0.1308(4) 0.0247(15) Uani 1 1 d . . . H4 H 0.5140 0.5998 0.0892 0.030 Uiso 1 1 calc R . . N21 N 0.5459(3) 0.7002(3) 0.3293(3) 0.0149(10) Uani 1 1 d . . . C22 C 0.5413(4) 0.7325(3) 0.3951(3) 0.0142(12) Uani 1 1 d . . . S23 S 0.64055(10) 0.76720(10) 0.46863(8) 0.0212(3) Uani 1 1 d . . . C24 C 0.6879(4) 0.7362(4) 0.4050(4) 0.0232(14) Uani 1 1 d . . . H5 H 0.7468 0.7418 0.4183 0.028 Uiso 1 1 calc R . . C25 C 0.6280(4) 0.7025(4) 0.3330(3) 0.0167(13) Uani 1 1 d . . . N31 N 0.3916(3) 0.7027(3) 0.3283(2) 0.0116(10) Uani 1 1 d . . . C32 C 0.3111(4) 0.7022(3) 0.3233(3) 0.0114(12) Uani 1 1 d . . . C33 C 0.2926(4) 0.7350(3) 0.3880(3) 0.0140(12) Uani 1 1 d . . . C34 C 0.3603(4) 0.7684(4) 0.4592(3) 0.0175(13) Uani 1 1 d . . . H6 H 0.3503 0.7905 0.5030 0.021 Uiso 1 1 calc R . . C35 C 0.4424(4) 0.7679(4) 0.4632(3) 0.0154(12) Uani 1 1 d . . . H7 H 0.4885 0.7894 0.5099 0.018 Uiso 1 1 calc R . . C36 C 0.4556(4) 0.7352(3) 0.3971(3) 0.0102(11) Uani 1 1 d . . . N41 N 0.1986(3) 0.5729(3) 0.2130(2) 0.0100(10) Uani 1 1 d . . . C42 C 0.2411(4) 0.6590(3) 0.2444(3) 0.0119(12) Uani 1 1 d . . . C43 C 0.2281(4) 0.7050(4) 0.2033(3) 0.0135(12) Uani 1 1 d . . . C44 C 0.1767(4) 0.6615(4) 0.1264(3) 0.0151(12) Uani 1 1 d . . . H8 H 0.1700 0.6909 0.0974 0.018 Uiso 1 1 calc R . . C45 C 0.1352(4) 0.5718(4) 0.0939(3) 0.0168(13) Uani 1 1 d . . . H9 H 0.1014 0.5403 0.0421 0.020 Uiso 1 1 calc R . . C46 C 0.1447(4) 0.5304(4) 0.1388(3) 0.0123(12) Uani 1 1 d . . . N51 N 0.1122(3) 0.4050(3) 0.1603(3) 0.0127(10) Uani 1 1 d . . . C52 C 0.1001(4) 0.4370(4) 0.1120(3) 0.0133(12) Uani 1 1 d . . . S53 S 0.02786(10) 0.35911(9) 0.02202(8) 0.0184(3) Uani 1 1 d . . . C54 C 0.0149(4) 0.2815(4) 0.0532(3) 0.0189(13) Uani 1 1 d . . . H10 H -0.0207 0.2229 0.0226 0.023 Uiso 1 1 calc R . . C55 C 0.0636(4) 0.3169(4) 0.1290(3) 0.0158(12) Uani 1 1 d . . . N61 N 0.1295(3) 0.3360(3) 0.2544(3) 0.0172(11) Uani 1 1 d . . . C62 C 0.0722(4) 0.2787(4) 0.1833(3) 0.0150(12) Uani 1 1 d . . . C63 C 0.0243(4) 0.1923(4) 0.1641(4) 0.0197(13) Uani 1 1 d . . . H11 H -0.0154 0.1537 0.1145 0.024 Uiso 1 1 calc R . . C64 C 0.0362(4) 0.1642(4) 0.2195(4) 0.0240(15) Uani 1 1 d . . . H12 H 0.0051 0.1063 0.2078 0.029 Uiso 1 1 calc R . . C65 C 0.0946(5) 0.2230(4) 0.2924(4) 0.0270(15) Uani 1 1 d . . . H13 H 0.1025 0.2056 0.3310 0.032 Uiso 1 1 calc R . . C66 C 0.1415(4) 0.3083(4) 0.3078(3) 0.0223(14) Uani 1 1 d . . . H14 H 0.1828 0.3476 0.3568 0.027 Uiso 1 1 calc R . . N71 N 0.4844(3) 0.7928(3) 0.2286(3) 0.0192(11) Uani 1 1 d . . . C72 C 0.4512(4) 0.7867(4) 0.1582(3) 0.0193(13) Uani 1 1 d . . . C73 C 0.4738(4) 0.8557(4) 0.1422(4) 0.0209(14) Uani 1 1 d . . . H15 H 0.4511 0.8483 0.0927 0.025 Uiso 1 1 calc R . . C74 C 0.5315(5) 0.9378(4) 0.2010(4) 0.0294(16) Uani 1 1 d . . . H16 H 0.5482 0.9861 0.1916 0.035 Uiso 1 1 calc R . . C75 C 0.5627(5) 0.9449(4) 0.2727(4) 0.0322(17) Uani 1 1 d . . . H17 H 0.5995 0.9988 0.3134 0.039 Uiso 1 1 calc R . . C76 C 0.5396(5) 0.8719(4) 0.2850(4) 0.0338(17) Uani 1 1 d . . . H18 H 0.5631 0.8778 0.3339 0.041 Uiso 1 1 calc R . . N81 N 0.3746(3) 0.6360(3) 0.1265(3) 0.0128(10) Uani 1 1 d . . . C82 C 0.3204(4) 0.5576(4) 0.0724(3) 0.0158(13) Uani 1 1 d . . . S83 S 0.27762(11) 0.55637(10) -0.01375(8) 0.0212(3) Uani 1 1 d . . . C84 C 0.3382(4) 0.6661(4) 0.0255(3) 0.0202(14) Uani 1 1 d . . . H19 H 0.3384 0.6993 -0.0008 0.024 Uiso 1 1 calc R . . C85 C 0.3857(4) 0.6971(4) 0.1004(3) 0.0163(13) Uani 1 1 d . . . N91 N 0.3496(3) 0.5060(3) 0.1643(3) 0.0121(10) Uani 1 1 d . . . C92 C 0.3397(4) 0.4429(4) 0.1857(3) 0.0150(13) Uani 1 1 d . . . C93 C 0.2880(4) 0.3548(4) 0.1325(3) 0.0150(12) Uani 1 1 d . . . C94 C 0.2448(4) 0.3352(4) 0.0582(3) 0.0194(14) Uani 1 1 d . . . H20 H 0.2100 0.2781 0.0226 0.023 Uiso 1 1 calc R . . C95 C 0.2530(4) 0.4006(4) 0.0362(3) 0.0170(13) Uani 1 1 d . . . H21 H 0.2232 0.3882 -0.0138 0.020 Uiso 1 1 calc R . . C96 C 0.3065(4) 0.4846(4) 0.0906(3) 0.0127(12) Uani 1 1 d . . . N101 N 0.3370(3) 0.4949(3) 0.3097(3) 0.0118(10) Uani 1 1 d . . . C102 C 0.3838(4) 0.4733(3) 0.2692(3) 0.0118(12) Uani 1 1 d . . . C103 C 0.4731(4) 0.4855(3) 0.3035(3) 0.0148(12) Uani 1 1 d . . . C104 C 0.5149(4) 0.5272(3) 0.3814(3) 0.0141(12) Uani 1 1 d . . . H22 H 0.5751 0.5397 0.4054 0.017 Uiso 1 1 calc R . . C105 C 0.4665(4) 0.5500(4) 0.4232(3) 0.0153(12) Uani 1 1 d . . . H23 H 0.4935 0.5774 0.4758 0.018 Uiso 1 1 calc R . . C106 C 0.3777(4) 0.5319(3) 0.3865(3) 0.0137(12) Uani 1 1 d . . . N111 N 0.2351(3) 0.5279(3) 0.3841(3) 0.0156(11) Uani 1 1 d . . . C112 C 0.3193(4) 0.5502(3) 0.4255(3) 0.0144(12) Uani 1 1 d . . . S113 S 0.34338(10) 0.59522(10) 0.52046(8) 0.0192(3) Uani 1 1 d . . . C114 C 0.2336(4) 0.5810(4) 0.5022(3) 0.0200(14) Uani 1 1 d . . . H24 H 0.2105 0.5964 0.5390 0.024 Uiso 1 1 calc R . . C115 C 0.1850(4) 0.5439(4) 0.4259(3) 0.0166(13) Uani 1 1 d . . . N121 N 0.0690(3) 0.4877(3) 0.3057(3) 0.0207(12) Uani 1 1 d . . . C122 C 0.0898(4) 0.5184(4) 0.3813(3) 0.0188(13) Uani 1 1 d . . . C123 C 0.0281(4) 0.5253(4) 0.4142(4) 0.0238(14) Uani 1 1 d . . . H25 H 0.0447 0.5458 0.4663 0.029 Uiso 1 1 calc R . . C124 C -0.0603(5) 0.5003(4) 0.3662(4) 0.0343(18) Uani 1 1 d . . . H26 H -0.1041 0.5038 0.3859 0.041 Uiso 1 1 calc R . . C125 C -0.0816(5) 0.4703(5) 0.2888(4) 0.0349(18) Uani 1 1 d . . . H27 H -0.1398 0.4539 0.2561 0.042 Uiso 1 1 calc R . . C126 C -0.0152(4) 0.4649(4) 0.2604(4) 0.0282(16) Uani 1 1 d . . . H28 H -0.0300 0.4448 0.2085 0.034 Uiso 1 1 calc R . . O200 O 0.2087(3) 0.7322(2) 0.3762(2) 0.0145(9) Uani 1 1 d . . . C201 C 0.1802(4) 0.7384(4) 0.4401(3) 0.0175(13) Uani 1 1 d . . . H29E H 0.2160 0.7961 0.4808 0.021 Uiso 1 1 calc R . . H30F H 0.1892 0.6986 0.4591 0.021 Uiso 1 1 calc R . . C202 C 0.0809(4) 0.7169(4) 0.4127(4) 0.0209(14) Uani 1 1 d . . . H31C H 0.0476 0.6667 0.3641 0.025 Uiso 1 1 calc R . . H32D H 0.0553 0.7043 0.4484 0.025 Uiso 1 1 calc R . . O203 O 0.0733(3) 0.7887(3) 0.4055(3) 0.0255(10) Uani 1 1 d . . . C204 C -0.0170(5) 0.7820(5) 0.3895(5) 0.042(2) Uani 1 1 d . . . H33G H -0.0467 0.7543 0.4168 0.050 Uiso 1 1 calc R . . H34H H -0.0537 0.7484 0.3358 0.050 Uiso 1 1 calc R . . C205 C -0.0058(6) 0.8718(6) 0.4148(6) 0.054(3) Uani 1 1 d . . . H35K H -0.0649 0.8708 0.4065 0.064 Uiso 1 1 calc R . . H36L H 0.0316 0.9051 0.4685 0.064 Uiso 1 1 calc R . . O206 O 0.0365(3) 0.9104(3) 0.3730(3) 0.0395(13) Uani 1 1 d . . . C207 C 0.0645(6) 1.0020(5) 0.4057(5) 0.046(2) Uani 1 1 d . . . H37I H 0.1100 1.0298 0.4568 0.055 Uiso 1 1 calc R . . H38J H 0.0125 1.0121 0.4081 0.055 Uiso 1 1 calc R . . C208 C 0.1036(5) 1.0381(5) 0.3565(5) 0.0354(18) Uani 1 1 d . . . H39A H 0.0581 1.0100 0.3054 0.043 Uiso 1 1 calc R . . H40B H 0.1216 1.0992 0.3764 0.043 Uiso 1 1 calc R . . O209 O 0.1802(3) 1.0238(3) 0.3561(3) 0.0271(10) Uani 1 1 d . . . C210 C 0.2334(4) 1.0727(4) 0.3252(4) 0.0218(14) Uani 1 1 d . . . H41E H 0.2556 1.1336 0.3552 0.026 Uiso 1 1 calc R . . H42F H 0.1964 1.0573 0.2737 0.026 Uiso 1 1 calc R . . C211 C 0.3119(5) 1.0529(4) 0.3264(4) 0.0244(15) Uani 1 1 d . . . H43C H 0.3499 1.0852 0.3062 0.029 Uiso 1 1 calc R . . H44D H 0.3489 1.0682 0.3778 0.029 Uiso 1 1 calc R . . O212 O 0.2748(3) 0.9623(2) 0.2805(2) 0.0198(9) Uani 1 1 d . . . C213 C 0.3392(4) 0.9376(4) 0.2585(4) 0.0239(15) Uani 1 1 d . . . H45G H 0.3858 0.9454 0.3022 0.029 Uiso 1 1 calc R . . H46H H 0.3685 0.9722 0.2355 0.029 Uiso 1 1 calc R . . C214 C 0.2867(4) 0.8438(4) 0.2021(3) 0.0197(13) Uani 1 1 d . . . H47A H 0.2302 0.8333 0.1663 0.024 Uiso 1 1 calc R . . H48B H 0.3225 0.8284 0.1743 0.024 Uiso 1 1 calc R . . O215 O 0.2675(3) 0.7924(2) 0.2441(2) 0.0178(9) Uani 1 1 d . . . O300 O 0.2823(3) 0.2939(2) 0.1585(2) 0.0163(9) Uani 1 1 d . . . C301 C 0.2092(4) 0.2081(3) 0.1042(3) 0.0164(13) Uani 1 1 d . . . H49C H 0.2229 0.1880 0.0597 0.020 Uiso 1 1 calc R . . H50D H 0.1523 0.2109 0.0884 0.020 Uiso 1 1 calc R . . C302 C 0.1992(4) 0.1469(4) 0.1382(4) 0.0235(14) Uani 1 1 d . . . H51E H 0.2058 0.1751 0.1901 0.028 Uiso 1 1 calc R . . H52F H 0.1385 0.0988 0.1105 0.028 Uiso 1 1 calc R . . O303 O 0.2657(3) 0.1155(3) 0.1370(2) 0.0227(10) Uani 1 1 d . . . C304 C 0.2322(5) 0.0387(4) 0.0697(4) 0.0320(17) Uani 1 1 d . . . H53A H 0.2151 0.0488 0.0254 0.038 Uiso 1 1 calc R . . H54B H 0.1788 -0.0064 0.0674 0.038 Uiso 1 1 calc R . . C305 C 0.3050(5) 0.0126(4) 0.0713(4) 0.0352(18) Uani 1 1 d . . . H55K H 0.3206 0.0010 0.1149 0.042 Uiso 1 1 calc R . . H56L H 0.2839 -0.0396 0.0261 0.042 Uiso 1 1 calc R . . O306 O 0.3833(3) 0.0793(3) 0.0753(3) 0.0302(11) Uani 1 1 d . . . C307 C 0.4502(5) 0.0530(5) 0.0637(5) 0.049(2) Uani 1 1 d . . . H57G H 0.4252 0.0062 0.0136 0.059 Uiso 1 1 calc R . . H58H H 0.4684 0.0328 0.1007 0.059 Uiso 1 1 calc R . . C308 C 0.5303(5) 0.1269(5) 0.0716(4) 0.042(2) Uani 1 1 d . . . H59I H 0.5753 0.1091 0.0608 0.050 Uiso 1 1 calc R . . H60J H 0.5120 0.1490 0.0363 0.050 Uiso 1 1 calc R . . O309 O 0.5676(3) 0.1911(3) 0.1472(3) 0.0321(12) Uani 1 1 d . . . C310 C 0.6581(4) 0.2555(4) 0.1708(4) 0.0343(18) Uani 1 1 d . . . H61C H 0.6888 0.2328 0.1413 0.041 Uiso 1 1 calc R . . H62D H 0.6918 0.2730 0.2237 0.041 Uiso 1 1 calc R . . C311 C 0.6556(5) 0.3313(5) 0.1603(4) 0.0355(18) Uani 1 1 d . . . H63A H 0.7167 0.3740 0.1727 0.043 Uiso 1 1 calc R . . H64B H 0.6187 0.3139 0.1082 0.043 Uiso 1 1 calc R . . O312 O 0.6164(3) 0.3655(3) 0.2106(2) 0.0264(11) Uani 1 1 d . . . C313 C 0.6386(4) 0.4530(4) 0.2278(4) 0.0266(15) Uani 1 1 d . . . H65E H 0.6078 0.4575 0.1835 0.032 Uiso 1 1 calc R . . H66F H 0.7039 0.4868 0.2438 0.032 Uiso 1 1 calc R . . C314 C 0.6081(4) 0.4853(4) 0.2906(3) 0.0204(14) Uani 1 1 d . . . H67G H 0.6204 0.4627 0.3270 0.024 Uiso 1 1 calc R . . H68H H 0.6401 0.5476 0.3167 0.024 Uiso 1 1 calc R . . O315 O 0.5109(3) 0.4559(3) 0.2558(2) 0.0175(9) Uani 1 1 d . . . N400 N 0.1427(5) 0.6869(5) 0.5949(5) 0.068(3) Uani 1 1 d . . . C401 C 0.1301(6) 0.7112(5) 0.6486(6) 0.053(2) Uani 1 1 d . . . C402 C 0.1138(11) 0.7453(8) 0.7161(7) 0.108(5) Uani 1 1 d . . . H69A H 0.1394 0.8067 0.7355 0.163 Uiso 1 1 calc R . . H70B H 0.1419 0.7308 0.7536 0.163 Uiso 1 1 calc R . . H71C H 0.0494 0.7212 0.7043 0.163 Uiso 1 1 calc R . . N403 N 0.6825(11) 1.0559(11) 0.1359(9) 0.067(5) Uiso 0.50 1 d P . . C404 C 0.7070(9) 1.0090(8) 0.1297(7) 0.023(3) Uiso 0.50 1 d P . . C405 C 0.7302(12) 0.9487(11) 0.1243(10) 0.049(4) Uiso 0.50 1 d P . . H40A H 0.7640 0.9578 0.1739 0.073 Uiso 0.50 1 calc PR . . H40C H 0.7674 0.9491 0.0948 0.073 Uiso 0.50 1 calc PR . . H40D H 0.6764 0.8942 0.0999 0.073 Uiso 0.50 1 calc PR . . N406 N 0.9197(6) 0.0697(6) 0.3080(6) 0.073(3) Uani 1 1 d . . . C407 C 0.8713(9) 0.0807(8) 0.3383(9) 0.089(4) Uani 1 1 d . . . C408 C 0.8134(9) 0.0883(9) 0.3782(7) 0.099(4) Uani 1 1 d . . . H72D H 0.7891 0.0381 0.3866 0.149 Uiso 1 1 calc R . . H73E H 0.7642 0.0937 0.3490 0.149 Uiso 1 1 calc R . . H74F H 0.8477 0.1383 0.4260 0.149 Uiso 1 1 calc R . . N409 N 0.7828(9) 0.8768(8) 0.3183(7) 0.122(4) Uiso 1 1 d . . . C410 C 0.8056(9) 0.8615(8) 0.2639(8) 0.090(4) Uiso 1 1 d . . . C411 C 0.8438(7) 0.8446(6) 0.2076(5) 0.063(3) Uiso 1 1 d . . . H75A H 0.8874 0.8980 0.2125 0.095 Uiso 1 1 calc R . . H76B H 0.7960 0.8143 0.1582 0.095 Uiso 1 1 calc R . . H77C H 0.8735 0.8103 0.2146 0.095 Uiso 1 1 calc R . . Cl1 Cl -0.05036(10) 0.62246(10) 0.17197(9) 0.0265(4) Uani 1 1 d . . . O1A O 0.0389(3) 0.6824(3) 0.2296(3) 0.0337(12) Uani 1 1 d . . . O1B O -0.0867(3) 0.6673(3) 0.1369(3) 0.0357(12) Uani 1 1 d . . . O1C O -0.1097(3) 0.5850(3) 0.2050(3) 0.0380(12) Uani 1 1 d . . . O1D O -0.0435(3) 0.5572(4) 0.1165(3) 0.0532(17) Uani 1 1 d . . . Cl2 Cl 0.34479(13) 0.98132(10) 0.49698(9) 0.0345(4) Uani 1 1 d . . . O2A O 0.3431(3) 0.9312(3) 0.4240(3) 0.0339(12) Uani 1 1 d . . . O2B O 0.2518(4) 0.9685(4) 0.4853(3) 0.0532(16) Uani 1 1 d . . . O2C O 0.4044(4) 1.0698(3) 0.5223(3) 0.0450(14) Uani 1 1 d . . . O2D O 0.3731(5) 0.9502(3) 0.5506(3) 0.0610(19) Uani 1 1 d . . . Cl3 Cl 0.42398(11) 0.29421(12) 0.01530(9) 0.0352(4) Uani 1 1 d . . . O3A O 0.4093(3) 0.2733(3) 0.0759(3) 0.0372(12) Uani 1 1 d . . . O3B O 0.4705(5) 0.3838(4) 0.0430(4) 0.085(3) Uani 1 1 d . . . O3C O 0.3370(3) 0.2623(4) -0.0427(3) 0.0447(14) Uani 1 1 d . . . O3D O 0.4734(4) 0.2534(6) -0.0153(4) 0.084(3) Uani 1 1 d . . . Cl4 Cl 0.56744(13) 0.17016(11) 0.30575(9) 0.0339(4) Uani 1 1 d . . . O4A O 0.4784(3) 0.1192(3) 0.2441(3) 0.0296(11) Uani 1 1 d . . . O4B O 0.5966(4) 0.2590(3) 0.3174(3) 0.0405(13) Uani 1 1 d . . . O4C O 0.6310(3) 0.1424(3) 0.2855(3) 0.0463(15) Uani 1 1 d . . . O4D O 0.5598(5) 0.1617(4) 0.3719(3) 0.066(2) Uani 1 1 d . . . Cl5 Cl 0.40500(9) 0.29907(9) 0.36027(7) 0.0175(3) Uani 1 1 d . . . O5A O 0.4787(3) 0.3510(3) 0.3447(2) 0.0204(9) Uani 1 1 d . . . O5B O 0.3467(3) 0.2215(3) 0.2914(2) 0.0239(10) Uani 1 1 d . . . O5C O 0.3578(3) 0.3457(3) 0.3840(3) 0.0392(13) Uani 1 1 d . . . O5D O 0.4424(3) 0.2778(3) 0.4179(2) 0.0264(10) Uani 1 1 d . . . Cl6 Cl 0.97450(11) 0.92036(10) 0.08326(9) 0.0282(4) Uani 1 1 d . . . O6A O 0.9193(4) 0.9644(4) 0.0864(3) 0.0534(16) Uani 1 1 d . . . O6B O 0.9226(4) 0.8347(3) 0.0757(3) 0.0433(14) Uani 1 1 d . . . O6C O 1.0544(4) 0.9670(3) 0.1521(3) 0.0444(14) Uani 1 1 d . . . O6D O 1.0003(4) 0.9146(3) 0.0193(3) 0.0419(13) Uani 1 1 d . . . Cl7 Cl 0.79402(10) 0.23175(10) 0.03760(9) 0.0244(3) Uani 1 1 d . . . O7A O 0.6954(3) 0.1895(3) 0.0141(3) 0.0351(12) Uani 1 1 d . . . O7B O 0.8273(4) 0.3220(3) 0.0785(4) 0.0633(19) Uani 1 1 d . . . O7C O 0.8143(3) 0.2140(4) -0.0284(3) 0.0445(15) Uani 1 1 d . . . O7D O 0.8342(3) 0.1999(4) 0.0841(3) 0.0418(13) Uani 1 1 d . . . Cl8 Cl 0.83334(11) 0.64703(11) 0.48066(9) 0.0281(4) Uani 1 1 d . . . O8A O 0.7499(3) 0.6087(3) 0.4909(3) 0.0411(13) Uani 1 1 d . . . O8B O 0.8687(4) 0.7390(3) 0.5139(3) 0.0464(14) Uani 1 1 d . . . O8C O 0.8982(4) 0.6250(4) 0.5152(3) 0.0491(15) Uani 1 1 d . . . O8D O 0.8148(3) 0.6170(3) 0.4006(3) 0.0386(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0191(4) 0.0213(4) 0.0153(4) 0.0088(3) 0.0034(3) 0.0110(4) Zn2 0.0193(4) 0.0149(4) 0.0114(4) 0.0024(3) 0.0011(3) 0.0073(3) Ba1 0.0286(2) 0.01993(19) 0.0261(2) 0.01322(16) 0.01588(18) 0.01258(17) Ba2 0.01635(18) 0.01550(17) 0.01500(17) 0.00523(14) 0.00550(15) 0.00798(15) O1 0.037(3) 0.064(4) 0.057(4) 0.046(3) 0.002(3) 0.011(3) N11 0.016(3) 0.022(3) 0.024(3) 0.012(2) 0.008(2) 0.010(2) C12 0.020(3) 0.020(3) 0.029(4) 0.014(3) 0.010(3) 0.012(3) C13 0.014(3) 0.033(4) 0.034(4) 0.014(3) 0.010(3) 0.013(3) C14 0.030(4) 0.042(4) 0.045(4) 0.027(4) 0.028(4) 0.025(3) C15 0.037(4) 0.036(4) 0.030(4) 0.020(3) 0.023(3) 0.024(3) C16 0.033(4) 0.030(4) 0.019(3) 0.015(3) 0.010(3) 0.020(3) N21 0.013(2) 0.016(2) 0.021(3) 0.013(2) 0.004(2) 0.008(2) C22 0.016(3) 0.006(3) 0.017(3) 0.006(2) 0.003(3) 0.003(2) S23 0.0158(7) 0.0233(8) 0.0167(7) 0.0056(6) -0.0001(6) 0.0078(6) C24 0.019(3) 0.023(3) 0.031(4) 0.015(3) 0.010(3) 0.011(3) C25 0.011(3) 0.015(3) 0.020(3) 0.008(3) -0.001(3) 0.005(2) N31 0.016(3) 0.009(2) 0.013(2) 0.0081(19) 0.007(2) 0.005(2) C32 0.016(3) 0.007(2) 0.014(3) 0.007(2) 0.006(2) 0.006(2) C33 0.017(3) 0.009(3) 0.015(3) 0.005(2) 0.004(3) 0.008(2) C34 0.024(3) 0.012(3) 0.018(3) 0.006(2) 0.008(3) 0.010(3) C35 0.016(3) 0.015(3) 0.013(3) 0.005(2) 0.003(3) 0.008(2) C36 0.011(3) 0.007(2) 0.011(3) 0.005(2) 0.001(2) 0.002(2) N41 0.010(2) 0.011(2) 0.009(2) 0.0028(19) 0.0012(19) 0.0078(19) C42 0.011(3) 0.012(3) 0.012(3) 0.002(2) 0.005(2) 0.007(2) C43 0.013(3) 0.014(3) 0.017(3) 0.008(2) 0.005(2) 0.009(2) C44 0.016(3) 0.021(3) 0.016(3) 0.012(3) 0.007(3) 0.013(3) C45 0.014(3) 0.023(3) 0.013(3) 0.006(3) 0.005(2) 0.010(3) C46 0.011(3) 0.017(3) 0.011(3) 0.006(2) 0.004(2) 0.010(2) N51 0.012(2) 0.011(2) 0.013(2) 0.005(2) 0.002(2) 0.005(2) C52 0.012(3) 0.015(3) 0.014(3) 0.007(2) 0.006(2) 0.007(2) S53 0.0180(7) 0.0181(7) 0.0130(7) 0.0048(6) 0.0007(6) 0.0070(6) C54 0.017(3) 0.014(3) 0.021(3) 0.007(3) 0.003(3) 0.005(3) C55 0.013(3) 0.014(3) 0.019(3) 0.007(2) 0.006(3) 0.006(2) N61 0.020(3) 0.015(2) 0.019(3) 0.009(2) 0.005(2) 0.010(2) C62 0.010(3) 0.014(3) 0.017(3) 0.004(2) 0.004(2) 0.004(2) C63 0.022(3) 0.013(3) 0.021(3) 0.005(3) 0.006(3) 0.009(3) C64 0.028(4) 0.014(3) 0.036(4) 0.013(3) 0.018(3) 0.012(3) C65 0.034(4) 0.024(3) 0.029(4) 0.015(3) 0.012(3) 0.017(3) C66 0.028(4) 0.021(3) 0.017(3) 0.008(3) 0.004(3) 0.012(3) N71 0.022(3) 0.017(3) 0.021(3) 0.010(2) 0.007(2) 0.009(2) C72 0.021(3) 0.019(3) 0.026(3) 0.013(3) 0.014(3) 0.011(3) C73 0.025(3) 0.020(3) 0.021(3) 0.009(3) 0.013(3) 0.012(3) C74 0.042(4) 0.022(3) 0.037(4) 0.019(3) 0.025(4) 0.018(3) C75 0.038(4) 0.017(3) 0.034(4) 0.008(3) 0.011(3) 0.009(3) C76 0.036(4) 0.023(3) 0.025(4) 0.006(3) 0.003(3) 0.006(3) N81 0.014(2) 0.014(2) 0.015(2) 0.008(2) 0.006(2) 0.009(2) C82 0.012(3) 0.019(3) 0.017(3) 0.006(3) 0.007(3) 0.009(2) S83 0.0270(8) 0.0258(8) 0.0132(7) 0.0097(6) 0.0063(6) 0.0145(7) C84 0.030(4) 0.024(3) 0.020(3) 0.016(3) 0.014(3) 0.017(3) C85 0.019(3) 0.018(3) 0.021(3) 0.011(3) 0.012(3) 0.013(3) N91 0.013(2) 0.012(2) 0.015(2) 0.008(2) 0.006(2) 0.008(2) C92 0.011(3) 0.014(3) 0.016(3) 0.001(2) 0.005(2) 0.006(2) C93 0.009(3) 0.015(3) 0.017(3) 0.007(2) 0.004(2) 0.002(2) C94 0.014(3) 0.013(3) 0.018(3) -0.001(2) 0.004(3) 0.001(2) C95 0.016(3) 0.021(3) 0.013(3) 0.008(3) 0.003(3) 0.009(3) C96 0.015(3) 0.015(3) 0.012(3) 0.006(2) 0.006(2) 0.010(2) N101 0.014(2) 0.008(2) 0.014(2) 0.0046(19) 0.003(2) 0.007(2) C102 0.009(3) 0.004(2) 0.016(3) 0.003(2) 0.002(2) 0.001(2) C103 0.014(3) 0.010(3) 0.021(3) 0.008(2) 0.008(3) 0.005(2) C104 0.006(3) 0.010(3) 0.015(3) 0.002(2) -0.005(2) 0.001(2) C105 0.015(3) 0.015(3) 0.010(3) 0.004(2) -0.002(2) 0.007(2) C106 0.016(3) 0.005(2) 0.016(3) 0.002(2) 0.002(3) 0.005(2) N111 0.015(3) 0.012(2) 0.016(2) 0.003(2) 0.005(2) 0.005(2) C112 0.021(3) 0.006(2) 0.017(3) 0.005(2) 0.008(3) 0.007(2) S113 0.0214(8) 0.0226(7) 0.0126(7) 0.0056(6) 0.0051(6) 0.0119(6) C114 0.024(3) 0.022(3) 0.016(3) 0.007(3) 0.010(3) 0.012(3) C115 0.018(3) 0.016(3) 0.017(3) 0.009(2) 0.007(3) 0.008(3) N121 0.021(3) 0.023(3) 0.019(3) 0.007(2) 0.004(2) 0.015(2) C122 0.016(3) 0.013(3) 0.022(3) 0.006(3) 0.003(3) 0.006(3) C123 0.023(3) 0.023(3) 0.027(3) 0.012(3) 0.011(3) 0.011(3) C124 0.024(4) 0.026(4) 0.057(5) 0.017(4) 0.019(4) 0.014(3) C125 0.018(4) 0.033(4) 0.041(4) 0.008(4) 0.001(3) 0.012(3) C126 0.023(4) 0.031(4) 0.027(4) 0.011(3) 0.003(3) 0.016(3) O200 0.014(2) 0.021(2) 0.0113(19) 0.0065(17) 0.0046(17) 0.0112(18) C201 0.026(3) 0.017(3) 0.020(3) 0.013(3) 0.014(3) 0.013(3) C202 0.025(3) 0.020(3) 0.028(3) 0.017(3) 0.018(3) 0.010(3) O203 0.021(2) 0.031(2) 0.044(3) 0.026(2) 0.021(2) 0.018(2) C204 0.024(4) 0.062(5) 0.071(6) 0.045(5) 0.031(4) 0.029(4) C205 0.065(6) 0.069(6) 0.106(8) 0.074(6) 0.071(6) 0.057(5) O206 0.044(3) 0.043(3) 0.072(4) 0.044(3) 0.041(3) 0.033(3) C207 0.062(5) 0.040(4) 0.080(6) 0.045(5) 0.055(5) 0.035(4) C208 0.040(4) 0.035(4) 0.064(5) 0.036(4) 0.033(4) 0.029(4) O209 0.034(3) 0.026(2) 0.036(3) 0.020(2) 0.017(2) 0.020(2) C210 0.028(4) 0.018(3) 0.023(3) 0.009(3) 0.012(3) 0.013(3) C211 0.033(4) 0.016(3) 0.028(3) 0.010(3) 0.013(3) 0.013(3) O212 0.022(2) 0.0124(19) 0.029(2) 0.0100(18) 0.012(2) 0.0096(18) C213 0.028(4) 0.017(3) 0.041(4) 0.019(3) 0.021(3) 0.014(3) C214 0.031(4) 0.020(3) 0.023(3) 0.014(3) 0.016(3) 0.019(3) O215 0.022(2) 0.0116(19) 0.020(2) 0.0082(17) 0.0057(18) 0.0077(18) O300 0.018(2) 0.0097(19) 0.017(2) 0.0047(16) 0.0061(18) 0.0029(17) C301 0.013(3) 0.010(3) 0.022(3) 0.007(2) 0.004(3) 0.004(2) C302 0.017(3) 0.021(3) 0.029(3) 0.007(3) 0.008(3) 0.009(3) O303 0.018(2) 0.015(2) 0.028(2) 0.0049(19) 0.0018(19) 0.0077(18) C304 0.027(4) 0.020(3) 0.031(4) -0.001(3) 0.005(3) 0.006(3) C305 0.032(4) 0.018(3) 0.040(4) 0.004(3) 0.009(4) 0.006(3) O306 0.033(3) 0.022(2) 0.035(3) 0.006(2) 0.015(2) 0.016(2) C307 0.040(5) 0.026(4) 0.059(5) -0.008(4) 0.022(4) 0.014(4) C308 0.042(4) 0.034(4) 0.037(4) -0.002(3) 0.027(4) 0.012(4) O309 0.023(2) 0.025(2) 0.039(3) 0.000(2) 0.013(2) 0.013(2) C310 0.022(4) 0.032(4) 0.041(4) 0.002(3) 0.014(3) 0.015(3) C311 0.026(4) 0.035(4) 0.036(4) 0.002(3) 0.019(3) 0.012(3) O312 0.022(2) 0.023(2) 0.032(2) 0.005(2) 0.016(2) 0.010(2) C313 0.014(3) 0.025(3) 0.037(4) 0.011(3) 0.012(3) 0.006(3) C314 0.010(3) 0.021(3) 0.023(3) 0.007(3) 0.005(3) 0.003(3) O315 0.013(2) 0.021(2) 0.019(2) 0.0075(18) 0.0073(18) 0.0103(18) N400 0.040(4) 0.067(5) 0.063(5) -0.006(4) 0.020(4) 0.020(4) C401 0.042(5) 0.042(5) 0.072(6) 0.013(5) 0.028(5) 0.023(4) C402 0.220(16) 0.125(11) 0.112(10) 0.085(9) 0.130(11) 0.145(12) N406 0.059(5) 0.088(7) 0.116(8) 0.071(6) 0.055(6) 0.042(5) C407 0.087(9) 0.078(8) 0.161(13) 0.087(9) 0.073(9) 0.054(7) C408 0.111(10) 0.107(10) 0.097(10) 0.035(8) 0.058(8) 0.066(9) Cl1 0.0173(7) 0.0344(8) 0.0257(8) 0.0116(7) 0.0064(7) 0.0124(7) O1A 0.026(3) 0.035(3) 0.029(3) 0.012(2) -0.002(2) 0.012(2) O1B 0.026(3) 0.049(3) 0.037(3) 0.031(3) 0.004(2) 0.016(2) O1C 0.033(3) 0.055(3) 0.046(3) 0.039(3) 0.020(2) 0.024(3) O1D 0.026(3) 0.049(3) 0.056(4) -0.005(3) 0.013(3) 0.014(3) Cl2 0.0477(11) 0.0195(7) 0.0279(8) 0.0109(7) 0.0072(8) 0.0108(8) O2A 0.043(3) 0.028(3) 0.024(2) 0.007(2) 0.003(2) 0.019(2) O2B 0.043(3) 0.062(4) 0.036(3) 0.015(3) 0.015(3) 0.011(3) O2C 0.049(3) 0.019(2) 0.046(3) 0.015(2) 0.010(3) 0.000(2) O2D 0.103(5) 0.031(3) 0.030(3) 0.014(2) -0.001(3) 0.027(3) Cl3 0.0293(9) 0.0530(11) 0.0265(8) 0.0209(8) 0.0148(8) 0.0164(8) O3A 0.047(3) 0.049(3) 0.039(3) 0.029(3) 0.027(3) 0.032(3) O3B 0.079(5) 0.054(4) 0.056(4) 0.033(3) -0.012(4) -0.023(4) O3C 0.036(3) 0.061(4) 0.029(3) 0.016(3) 0.005(2) 0.022(3) O3D 0.055(4) 0.154(7) 0.052(4) 0.030(4) 0.037(3) 0.062(5) Cl4 0.0471(11) 0.0367(9) 0.0220(8) 0.0093(7) 0.0056(8) 0.0315(9) O4A 0.027(3) 0.035(3) 0.032(3) 0.021(2) 0.011(2) 0.014(2) O4B 0.049(3) 0.030(3) 0.031(3) 0.000(2) -0.001(2) 0.027(3) O4C 0.033(3) 0.027(3) 0.062(4) 0.004(3) -0.001(3) 0.023(2) O4D 0.118(6) 0.078(5) 0.029(3) 0.029(3) 0.025(3) 0.068(5) Cl5 0.0211(7) 0.0166(6) 0.0158(6) 0.0070(6) 0.0064(6) 0.0103(6) O5A 0.023(2) 0.017(2) 0.025(2) 0.0135(19) 0.0112(19) 0.0091(19) O5B 0.021(2) 0.023(2) 0.016(2) 0.0056(18) 0.0024(19) 0.0032(19) O5C 0.036(3) 0.041(3) 0.058(3) 0.027(3) 0.028(3) 0.026(3) O5D 0.033(3) 0.026(2) 0.019(2) 0.015(2) 0.006(2) 0.009(2) Cl6 0.0244(8) 0.0215(7) 0.0240(8) 0.0032(6) 0.0014(7) 0.0061(7) O6A 0.048(4) 0.052(3) 0.057(4) 0.013(3) 0.011(3) 0.034(3) O6B 0.042(3) 0.026(3) 0.035(3) 0.009(2) -0.002(2) 0.000(2) O6C 0.037(3) 0.033(3) 0.030(3) 0.007(2) -0.007(2) 0.000(2) O6D 0.044(3) 0.044(3) 0.033(3) 0.019(3) 0.013(2) 0.016(3) Cl7 0.0207(8) 0.0273(8) 0.0255(8) 0.0142(7) 0.0052(7) 0.0112(7) O7A 0.024(3) 0.043(3) 0.053(3) 0.031(3) 0.019(2) 0.019(2) O7B 0.044(4) 0.027(3) 0.084(5) 0.003(3) -0.003(3) 0.015(3) O7C 0.025(3) 0.068(4) 0.025(3) 0.020(3) 0.005(2) 0.008(3) O7D 0.035(3) 0.061(4) 0.049(3) 0.044(3) 0.018(3) 0.024(3) Cl8 0.0251(8) 0.0360(9) 0.0265(8) 0.0162(7) 0.0108(7) 0.0146(7) O8A 0.035(3) 0.053(3) 0.044(3) 0.028(3) 0.024(3) 0.018(3) O8B 0.052(4) 0.028(3) 0.037(3) 0.005(2) 0.000(3) 0.014(3) O8C 0.049(3) 0.064(4) 0.054(4) 0.034(3) 0.018(3) 0.040(3) O8D 0.027(3) 0.049(3) 0.030(3) 0.012(2) 0.011(2) 0.012(2) _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 N21 1.986(5) . ? Zn1 N81 1.989(5) . ? Zn1 N71 2.197(5) . ? Zn1 N11 2.286(5) . ? Zn1 N31 2.377(4) . ? Zn2 N111 1.985(5) . ? Zn2 N51 1.994(5) . ? Zn2 N61 2.173(5) . ? Zn2 N121 2.289(5) . ? Zn2 N101 2.368(5) . ? Zn2 N41 2.525(5) . ? Ba1 O1 2.677(5) . ? Ba1 O203 2.740(4) . ? Ba1 O212 2.750(4) . ? Ba1 O209 2.796(4) . ? Ba1 O2A 2.797(5) . ? Ba1 O206 2.835(5) . ? Ba1 O1A 2.844(5) . ? Ba1 O2B 2.861(5) . ? Ba1 O215 3.018(4) . ? Ba1 O200 3.089(4) . ? Ba1 Cl2 3.4433(18) . ? Ba2 O3A 2.691(5) . ? Ba2 O309 2.744(4) . ? Ba2 O303 2.811(4) . ? Ba2 O306 2.811(4) . ? Ba2 O5A 2.834(4) . ? Ba2 O4A 2.841(5) . ? Ba2 O312 2.851(4) . ? Ba2 O5B 2.873(4) . ? Ba2 O4B 2.892(5) . ? Ba2 O300 3.312(4) . ? Ba2 Cl5 3.4641(13) . ? Ba2 Cl4 3.4839(17) . ? N11 C16 1.329(8) . ? N11 C12 1.339(8) . ? C12 C13 1.392(8) . ? C12 C25 1.473(8) . ? C13 C14 1.395(9) . ? C14 C15 1.365(10) . ? C15 C16 1.364(9) . ? N21 C22 1.306(7) . ? N21 C25 1.360(7) . ? C22 C36 1.479(8) . ? C22 S23 1.713(6) . ? S23 C24 1.717(6) . ? C24 C25 1.355(9) . ? N31 C36 1.336(7) . ? N31 C32 1.340(7) . ? C32 C33 1.410(7) . ? C32 C42 1.496(8) . ? C33 O200 1.366(7) . ? C33 C34 1.395(8) . ? C34 C35 1.378(8) . ? C35 C36 1.384(7) . ? N41 C42 1.340(7) . ? N41 C46 1.348(7) . ? C42 C43 1.397(8) . ? C43 O215 1.371(6) . ? C43 C44 1.380(8) . ? C44 C45 1.396(8) . ? C45 C46 1.374(8) . ? C46 C52 1.464(8) . ? N51 C52 1.302(7) . ? N51 C55 1.376(7) . ? C52 S53 1.717(6) . ? S53 C54 1.705(6) . ? C54 C55 1.362(8) . ? C55 C62 1.484(8) . ? N61 C66 1.335(8) . ? N61 C62 1.341(7) . ? C62 C63 1.383(8) . ? C63 C64 1.375(9) . ? C64 C65 1.374(9) . ? C65 C66 1.381(9) . ? N71 C76 1.342(8) . ? N71 C72 1.354(8) . ? C72 C73 1.358(9) . ? C72 C85 1.492(8) . ? C73 C74 1.395(9) . ? C74 C75 1.368(10) . ? C75 C76 1.384(10) . ? N81 C82 1.318(7) . ? N81 C85 1.363(7) . ? C82 C96 1.462(8) . ? C82 S83 1.710(6) . ? S83 C84 1.713(6) . ? C84 C85 1.352(8) . ? N91 C92 1.337(7) . ? N91 C96 1.351(7) . ? C92 C93 1.425(8) . ? C92 C102 1.496(8) . ? C93 O300 1.366(7) . ? C93 C94 1.369(8) . ? C94 C95 1.386(9) . ? C95 C96 1.382(8) . ? N101 C102 1.330(7) . ? N101 C106 1.361(7) . ? C102 C103 1.414(8) . ? C103 O315 1.353(7) . ? C103 C104 1.380(8) . ? C104 C105 1.378(8) . ? C105 C106 1.380(8) . ? C106 C112 1.461(8) . ? N111 C112 1.313(8) . ? N111 C115 1.365(7) . ? C112 S113 1.709(6) . ? S113 C114 1.716(6) . ? C114 C115 1.367(8) . ? C115 C122 1.472(9) . ? N121 C126 1.336(8) . ? N121 C122 1.355(8) . ? C122 C123 1.382(8) . ? C123 C124 1.401(10) . ? C124 C125 1.388(10) . ? C125 C126 1.394(9) . ? O200 C201 1.464(6) . ? C201 C202 1.503(8) . ? C202 O203 1.423(7) . ? O203 C204 1.441(8) . ? C204 C205 1.498(11) . ? C205 O206 1.426(8) . ? O206 C207 1.451(9) . ? C207 C208 1.510(9) . ? C208 O209 1.415(8) . ? O209 C210 1.436(7) . ? C210 C211 1.495(9) . ? C211 O212 1.436(7) . ? O212 C213 1.429(7) . ? C213 C214 1.513(8) . ? C214 O215 1.463(7) . ? O300 C301 1.464(6) . ? C301 C302 1.477(9) . ? C302 O303 1.438(7) . ? O303 C304 1.428(7) . ? C304 C305 1.470(10) . ? C305 O306 1.425(8) . ? O306 C307 1.417(8) . ? C307 C308 1.482(10) . ? C308 O309 1.421(8) . ? O309 C310 1.422(8) . ? C310 C311 1.492(10) . ? C311 O312 1.439(7) . ? O312 C313 1.425(8) . ? C313 C314 1.506(8) . ? C314 O315 1.450(7) . ? N400 C401 1.133(11) . ? C401 C402 1.441(13) . ? N403 C404 1.07(2) . ? C404 C405 1.29(2) . ? N406 C407 1.165(13) . ? C407 C408 1.421(16) . ? N409 C410 1.227(16) . ? C410 C411 1.435(15) . ? Cl1 O1D 1.421(5) . ? Cl1 O1C 1.431(5) . ? Cl1 O1A 1.438(5) . ? Cl1 O1B 1.446(5) . ? Cl2 O2C 1.425(5) . ? Cl2 O2D 1.441(6) . ? Cl2 O2A 1.457(5) . ? Cl2 O2B 1.459(6) . ? Cl3 O3B 1.403(6) . ? Cl3 O3D 1.428(6) . ? Cl3 O3C 1.432(5) . ? Cl3 O3A 1.441(5) . ? Cl4 O4D 1.421(6) . ? Cl4 O4C 1.430(5) . ? Cl4 O4A 1.453(5) . ? Cl4 O4B 1.457(5) . ? Cl5 O5C 1.416(5) . ? Cl5 O5D 1.424(5) . ? Cl5 O5B 1.440(4) . ? Cl5 O5A 1.452(4) . ? Cl6 O6A 1.437(6) . ? Cl6 O6C 1.437(5) . ? Cl6 O6D 1.440(5) . ? Cl6 O6B 1.452(5) . ? Cl7 O7C 1.417(5) . ? Cl7 O7D 1.423(5) . ? Cl7 O7B 1.425(5) . ? Cl7 O7A 1.455(5) . ? Cl8 O8C 1.415(6) . ? Cl8 O8A 1.439(5) . ? Cl8 O8B 1.439(5) . ? Cl8 O8D 1.445(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 N21 Zn1 N81 167.39(19) . . ? N21 Zn1 N71 102.07(19) . . ? N81 Zn1 N71 76.69(19) . . ? N21 Zn1 N11 75.07(19) . . ? N81 Zn1 N11 92.56(18) . . ? N71 Zn1 N11 97.06(18) . . ? N21 Zn1 N31 73.49(18) . . ? N81 Zn1 N31 119.00(17) . . ? N71 Zn1 N31 92.97(17) . . ? N11 Zn1 N31 148.34(18) . . ? N111 Zn2 N51 171.29(19) . . ? N111 Zn2 N61 99.78(19) . . ? N51 Zn2 N61 77.65(19) . . ? N111 Zn2 N121 74.31(19) . . ? N51 Zn2 N121 97.45(18) . . ? N61 Zn2 N121 93.82(18) . . ? N111 Zn2 N101 74.03(17) . . ? N51 Zn2 N101 114.32(17) . . ? N61 Zn2 N101 94.33(17) . . ? N121 Zn2 N101 148.20(17) . . ? N111 Zn2 N41 112.62(17) . . ? N51 Zn2 N41 69.92(17) . . ? N61 Zn2 N41 147.49(16) . . ? N121 Zn2 N41 92.48(17) . . ? N101 Zn2 N41 96.91(15) . . ? O1 Ba1 O203 121.67(15) . . ? O1 Ba1 O212 69.80(15) . . ? O203 Ba1 O212 166.13(13) . . ? O1 Ba1 O209 81.33(17) . . ? O203 Ba1 O209 112.47(13) . . ? O212 Ba1 O209 59.11(12) . . ? O1 Ba1 O2A 137.15(16) . . ? O203 Ba1 O2A 100.59(14) . . ? O212 Ba1 O2A 69.59(14) . . ? O209 Ba1 O2A 89.40(13) . . ? O1 Ba1 O206 89.05(18) . . ? O203 Ba1 O206 59.23(13) . . ? O212 Ba1 O206 116.68(13) . . ? O209 Ba1 O206 59.03(13) . . ? O2A Ba1 O206 121.40(15) . . ? O1 Ba1 O1A 66.65(16) . . ? O203 Ba1 O1A 71.34(14) . . ? O212 Ba1 O1A 122.34(13) . . ? O209 Ba1 O1A 141.74(14) . . ? O2A Ba1 O1A 128.26(14) . . ? O206 Ba1 O1A 98.61(15) . . ? O1 Ba1 O2B 150.6(2) . . ? O203 Ba1 O2B 69.12(15) . . ? O212 Ba1 O2B 97.06(14) . . ? O209 Ba1 O2B 69.49(16) . . ? O2A Ba1 O2B 48.90(15) . . ? O206 Ba1 O2B 73.14(17) . . ? O1A Ba1 O2B 137.85(16) . . ? O1 Ba1 O215 79.24(16) . . ? O203 Ba1 O215 126.03(12) . . ? O212 Ba1 O215 60.95(11) . . ? O209 Ba1 O215 120.05(12) . . ? O2A Ba1 O215 69.58(12) . . ? O206 Ba1 O215 168.16(14) . . ? O1A Ba1 O215 75.21(12) . . ? O2B Ba1 O215 118.27(14) . . ? O1 Ba1 O200 127.12(16) . . ? O203 Ba1 O200 60.12(11) . . ? O212 Ba1 O200 121.01(11) . . ? O209 Ba1 O200 151.09(12) . . ? O2A Ba1 O200 66.57(12) . . ? O206 Ba1 O200 119.19(12) . . ? O1A Ba1 O200 65.61(12) . . ? O2B Ba1 O200 82.28(15) . . ? O215 Ba1 O200 67.90(10) . . ? O1 Ba1 Cl2 151.36(12) . . ? O203 Ba1 Cl2 84.96(10) . . ? O212 Ba1 Cl2 82.47(9) . . ? O209 Ba1 Cl2 78.29(10) . . ? O2A Ba1 Cl2 24.28(10) . . ? O206 Ba1 Cl2 97.39(12) . . ? O1A Ba1 Cl2 138.70(10) . . ? O2B Ba1 Cl2 24.62(12) . . ? O215 Ba1 Cl2 93.79(8) . . ? O200 Ba1 Cl2 73.32(8) . . ? O3A Ba2 O309 87.12(15) . . ? O3A Ba2 O303 87.96(14) . . ? O309 Ba2 O303 117.35(12) . . ? O3A Ba2 O306 77.52(15) . . ? O309 Ba2 O306 59.61(13) . . ? O303 Ba2 O306 58.38(12) . . ? O3A Ba2 O5A 123.89(14) . . ? O309 Ba2 O5A 128.66(13) . . ? O303 Ba2 O5A 104.76(12) . . ? O306 Ba2 O5A 154.35(13) . . ? O3A Ba2 O4A 143.29(14) . . ? O309 Ba2 O4A 66.82(14) . . ? O303 Ba2 O4A 82.26(13) . . ? O306 Ba2 O4A 67.21(14) . . ? O5A Ba2 O4A 92.82(12) . . ? O3A Ba2 O312 73.84(15) . . ? O309 Ba2 O312 59.54(13) . . ? O303 Ba2 O312 161.49(13) . . ? O306 Ba2 O312 112.84(12) . . ? O5A Ba2 O312 88.58(11) . . ? O4A Ba2 O312 110.30(13) . . ? O3A Ba2 O5B 127.72(14) . . ? O309 Ba2 O5B 142.17(14) . . ? O303 Ba2 O5B 58.44(12) . . ? O306 Ba2 O5B 108.94(12) . . ? O5A Ba2 O5B 48.02(11) . . ? O4A Ba2 O5B 75.51(13) . . ? O312 Ba2 O5B 136.56(11) . . ? O3A Ba2 O4B 143.61(16) . . ? O309 Ba2 O4B 66.83(15) . . ? O303 Ba2 O4B 125.97(14) . . ? O306 Ba2 O4B 107.37(13) . . ? O5A Ba2 O4B 65.02(13) . . ? O4A Ba2 O4B 48.07(13) . . ? O312 Ba2 O4B 71.14(15) . . ? O5B Ba2 O4B 85.76(14) . . ? O3A Ba2 O300 60.28(12) . . ? O309 Ba2 O300 146.81(13) . . ? O303 Ba2 O300 59.78(11) . . ? O306 Ba2 O300 103.75(12) . . ? O5A Ba2 O300 79.49(11) . . ? O4A Ba2 O300 137.04(11) . . ? O312 Ba2 O300 111.66(11) . . ? O5B Ba2 O300 68.03(11) . . ? O4B Ba2 O300 144.45(12) . . ? O3A Ba2 Cl5 131.52(11) . . ? O309 Ba2 Cl5 139.11(11) . . ? O303 Ba2 Cl5 81.95(9) . . ? O306 Ba2 Cl5 131.59(10) . . ? O5A Ba2 Cl5 24.11(8) . . ? O4A Ba2 Cl5 82.06(9) . . ? O312 Ba2 Cl5 112.53(9) . . ? O5B Ba2 Cl5 24.03(8) . . ? O4B Ba2 Cl5 72.72(11) . . ? O300 Ba2 Cl5 73.93(7) . . ? O3A Ba2 Cl4 150.66(11) . . ? O309 Ba2 Cl4 63.54(11) . . ? O303 Ba2 Cl4 104.58(10) . . ? O306 Ba2 Cl4 86.58(10) . . ? O5A Ba2 Cl4 79.06(9) . . ? O4A Ba2 Cl4 23.90(10) . . ? O312 Ba2 Cl4 90.34(10) . . ? O5B Ba2 Cl4 80.65(10) . . ? O4B Ba2 Cl4 24.21(10) . . ? O300 Ba2 Cl4 148.68(7) . . ? Cl5 Ba2 Cl4 77.16(4) . . ? C16 N11 C12 118.1(5) . . ? C16 N11 Zn1 129.3(5) . . ? C12 N11 Zn1 112.6(4) . . ? N11 C12 C13 122.0(6) . . ? N11 C12 C25 115.0(5) . . ? C13 C12 C25 123.0(6) . . ? C12 C13 C14 117.7(6) . . ? C15 C14 C13 119.9(6) . . ? C16 C15 C14 118.2(6) . . ? N11 C16 C15 124.0(6) . . ? C22 N21 C25 114.3(5) . . ? C22 N21 Zn1 123.0(4) . . ? C25 N21 Zn1 122.0(4) . . ? N21 C22 C36 118.3(5) . . ? N21 C22 S23 112.2(4) . . ? C36 C22 S23 129.4(4) . . ? C22 S23 C24 89.9(3) . . ? C25 C24 S23 110.8(5) . . ? C24 C25 N21 112.8(5) . . ? C24 C25 C12 132.3(6) . . ? N21 C25 C12 114.9(5) . . ? C36 N31 C32 118.4(5) . . ? C36 N31 Zn1 111.0(3) . . ? C32 N31 Zn1 130.2(4) . . ? N31 C32 C33 122.1(5) . . ? N31 C32 C42 114.9(4) . . ? C33 C32 C42 122.9(5) . . ? O200 C33 C34 124.3(5) . . ? O200 C33 C32 117.1(5) . . ? C34 C33 C32 118.6(5) . . ? C35 C34 C33 118.4(5) . . ? C34 C35 C36 119.5(5) . . ? N31 C36 C35 122.9(5) . . ? N31 C36 C22 113.3(5) . . ? C35 C36 C22 123.8(5) . . ? C42 N41 C46 118.3(5) . . ? C42 N41 Zn2 131.1(4) . . ? C46 N41 Zn2 110.1(3) . . ? N41 C42 C43 122.0(5) . . ? N41 C42 C32 115.8(5) . . ? C43 C42 C32 121.9(5) . . ? O215 C43 C44 124.5(5) . . ? O215 C43 C42 115.9(5) . . ? C44 C43 C42 119.6(5) . . ? C43 C44 C45 117.7(5) . . ? C46 C45 C44 119.7(5) . . ? N41 C46 C45 122.4(5) . . ? N41 C46 C52 112.9(5) . . ? C45 C46 C52 124.6(5) . . ? C52 N51 C55 113.8(5) . . ? C52 N51 Zn2 127.6(4) . . ? C55 N51 Zn2 118.5(4) . . ? N51 C52 C46 119.1(5) . . ? N51 C52 S53 112.4(4) . . ? C46 C52 S53 128.4(4) . . ? C54 S53 C52 90.2(3) . . ? C55 C54 S53 110.9(4) . . ? C54 C55 N51 112.6(5) . . ? C54 C55 C62 132.2(5) . . ? N51 C55 C62 115.2(5) . . ? C66 N61 C62 118.8(5) . . ? C66 N61 Zn2 126.5(4) . . ? C62 N61 Zn2 114.4(4) . . ? N61 C62 C63 121.9(6) . . ? N61 C62 C55 114.0(5) . . ? C63 C62 C55 124.0(5) . . ? C64 C63 C62 119.0(6) . . ? C65 C64 C63 119.0(6) . . ? C64 C65 C66 119.2(6) . . ? N61 C66 C65 122.0(6) . . ? C76 N71 C72 117.1(6) . . ? C76 N71 Zn1 128.5(5) . . ? C72 N71 Zn1 114.1(4) . . ? N71 C72 C73 123.3(6) . . ? N71 C72 C85 113.2(5) . . ? C73 C72 C85 123.5(6) . . ? C72 C73 C74 119.3(6) . . ? C75 C74 C73 117.8(6) . . ? C74 C75 C76 120.1(6) . . ? N71 C76 C75 122.3(7) . . ? C82 N81 C85 112.5(5) . . ? C82 N81 Zn1 126.9(4) . . ? C85 N81 Zn1 120.1(4) . . ? N81 C82 C96 118.9(5) . . ? N81 C82 S83 112.7(5) . . ? C96 C82 S83 128.4(4) . . ? C82 S83 C84 90.3(3) . . ? C85 C84 S83 109.9(5) . . ? C84 C85 N81 114.5(5) . . ? C84 C85 C72 130.4(6) . . ? N81 C85 C72 115.0(5) . . ? C92 N91 C96 118.4(5) . . ? N91 C92 C93 121.6(5) . . ? N91 C92 C102 114.3(5) . . ? C93 C92 C102 124.1(5) . . ? O300 C93 C94 123.2(5) . . ? O300 C93 C92 118.2(5) . . ? C94 C93 C92 118.5(6) . . ? C93 C94 C95 120.0(5) . . ? C96 C95 C94 118.3(5) . . ? N91 C96 C95 123.2(5) . . ? N91 C96 C82 114.7(5) . . ? C95 C96 C82 122.1(5) . . ? C102 N101 C106 118.5(5) . . ? C102 N101 Zn2 130.9(4) . . ? C106 N101 Zn2 110.3(3) . . ? N101 C102 C103 122.1(5) . . ? N101 C102 C92 115.8(5) . . ? C103 C102 C92 121.9(5) . . ? O315 C103 C104 125.4(5) . . ? O315 C103 C102 116.1(5) . . ? C104 C103 C102 118.5(5) . . ? C105 C104 C103 119.2(5) . . ? C104 C105 C106 119.5(5) . . ? N101 C106 C105 122.0(5) . . ? N101 C106 C112 114.1(5) . . ? C105 C106 C112 123.9(5) . . ? C112 N111 C115 113.4(5) . . ? C112 N111 Zn2 123.3(4) . . ? C115 N111 Zn2 123.1(4) . . ? N111 C112 C106 118.1(5) . . ? N111 C112 S113 112.9(4) . . ? C106 C112 S113 129.0(5) . . ? C112 S113 C114 90.1(3) . . ? C115 C114 S113 110.5(4) . . ? N111 C115 C114 113.1(5) . . ? N111 C115 C122 114.9(5) . . ? C114 C115 C122 132.0(5) . . ? C126 N121 C122 118.3(5) . . ? C126 N121 Zn2 128.1(4) . . ? C122 N121 Zn2 113.3(4) . . ? N121 C122 C123 123.7(6) . . ? N121 C122 C115 113.7(5) . . ? C123 C122 C115 122.6(6) . . ? C122 C123 C124 117.6(6) . . ? C125 C124 C123 119.0(6) . . ? C124 C125 C126 119.6(7) . . ? N121 C126 C125 121.8(6) . . ? C33 O200 C201 115.1(4) . . ? C33 O200 Ba1 121.3(3) . . ? C201 O200 Ba1 102.8(3) . . ? O200 C201 C202 107.9(5) . . ? O203 C202 C201 108.4(5) . . ? C202 O203 C204 114.6(5) . . ? C202 O203 Ba1 118.3(3) . . ? C204 O203 Ba1 113.2(4) . . ? O203 C204 C205 106.7(6) . . ? O206 C205 C204 109.3(6) . . ? C205 O206 C207 110.7(6) . . ? C205 O206 Ba1 117.5(4) . . ? C207 O206 Ba1 116.6(4) . . ? O206 C207 C208 108.1(6) . . ? O209 C208 C207 108.2(6) . . ? C208 O209 C210 111.7(5) . . ? C208 O209 Ba1 118.2(4) . . ? C210 O209 Ba1 119.1(3) . . ? O209 C210 C211 107.8(5) . . ? O212 C211 C210 107.4(5) . . ? C213 O212 C211 113.7(4) . . ? C213 O212 Ba1 116.9(3) . . ? C211 O212 Ba1 114.8(3) . . ? O212 C213 C214 106.9(5) . . ? O215 C214 C213 108.1(5) . . ? C43 O215 C214 116.6(4) . . ? C43 O215 Ba1 115.7(3) . . ? C214 O215 Ba1 103.3(3) . . ? C93 O300 C301 113.1(4) . . ? C93 O300 Ba2 122.6(3) . . ? C301 O300 Ba2 97.9(3) . . ? O300 C301 C302 110.8(5) . . ? O303 C302 C301 112.0(5) . . ? C304 O303 C302 111.4(5) . . ? C304 O303 Ba2 120.1(4) . . ? C302 O303 Ba2 116.4(3) . . ? O303 C304 C305 108.1(5) . . ? O306 C305 C304 109.7(6) . . ? C307 O306 C305 112.7(5) . . ? C307 O306 Ba2 115.8(4) . . ? C305 O306 Ba2 114.6(4) . . ? O306 C307 C308 109.1(6) . . ? O309 C308 C307 107.5(6) . . ? C308 O309 C310 114.7(5) . . ? C308 O309 Ba2 116.1(4) . . ? C310 O309 Ba2 117.9(3) . . ? O309 C310 C311 109.7(6) . . ? O312 C311 C310 106.2(6) . . ? C313 O312 C311 112.7(5) . . ? C313 O312 Ba2 125.2(3) . . ? C311 O312 Ba2 113.9(4) . . ? O312 C313 C314 107.3(5) . . ? O315 C314 C313 106.9(5) . . ? C103 O315 C314 114.9(4) . . ? N400 C401 C402 177.4(11) . . ? N403 C404 C405 174.3(18) . . ? N406 C407 C408 174.2(13) . . ? N409 C410 C411 171.7(15) . . ? O1D Cl1 O1C 109.9(3) . . ? O1D Cl1 O1A 109.2(3) . . ? O1C Cl1 O1A 109.8(3) . . ? O1D Cl1 O1B 109.6(4) . . ? O1C Cl1 O1B 109.2(3) . . ? O1A Cl1 O1B 109.2(3) . . ? Cl1 O1A Ba1 145.3(3) . . ? O2C Cl2 O2D 111.3(3) . . ? O2C Cl2 O2A 109.5(3) . . ? O2D Cl2 O2A 109.6(3) . . ? O2C Cl2 O2B 110.1(4) . . ? O2D Cl2 O2B 109.3(4) . . ? O2A Cl2 O2B 106.9(3) . . ? O2C Cl2 Ba1 123.5(2) . . ? O2D Cl2 Ba1 125.2(2) . . ? O2A Cl2 Ba1 52.1(2) . . ? O2B Cl2 Ba1 54.7(2) . . ? Cl2 O2A Ba1 103.6(3) . . ? Cl2 O2B Ba1 100.6(3) . . ? O3B Cl3 O3D 111.9(5) . . ? O3B Cl3 O3C 109.0(4) . . ? O3D Cl3 O3C 108.9(4) . . ? O3B Cl3 O3A 109.2(4) . . ? O3D Cl3 O3A 109.3(4) . . ? O3C Cl3 O3A 108.5(3) . . ? Cl3 O3A Ba2 157.2(3) . . ? O4D Cl4 O4C 110.6(4) . . ? O4D Cl4 O4A 109.2(4) . . ? O4C Cl4 O4A 110.0(3) . . ? O4D Cl4 O4B 110.7(3) . . ? O4C Cl4 O4B 109.5(3) . . ? O4A Cl4 O4B 106.8(3) . . ? O4D Cl4 Ba2 127.6(3) . . ? O4C Cl4 Ba2 121.7(3) . . ? O4A Cl4 Ba2 52.39(19) . . ? O4B Cl4 Ba2 54.5(2) . . ? Cl4 O4A Ba2 103.7(2) . . ? Cl4 O4B Ba2 101.3(2) . . ? O5C Cl5 O5D 110.4(3) . . ? O5C Cl5 O5B 111.9(3) . . ? O5D Cl5 O5B 109.2(3) . . ? O5C Cl5 O5A 109.5(3) . . ? O5D Cl5 O5A 108.9(3) . . ? O5B Cl5 O5A 106.8(2) . . ? O5C Cl5 Ba2 131.6(2) . . ? O5D Cl5 Ba2 117.99(19) . . ? O5B Cl5 Ba2 54.33(17) . . ? O5A Cl5 Ba2 52.86(16) . . ? Cl5 O5A Ba2 103.0(2) . . ? Cl5 O5B Ba2 101.6(2) . . ? O6A Cl6 O6C 109.2(3) . . ? O6A Cl6 O6D 109.4(4) . . ? O6C Cl6 O6D 110.1(3) . . ? O6A Cl6 O6B 109.2(3) . . ? O6C Cl6 O6B 109.1(3) . . ? O6D Cl6 O6B 109.8(3) . . ? O7C Cl7 O7D 110.0(3) . . ? O7C Cl7 O7B 109.9(4) . . ? O7D Cl7 O7B 110.1(4) . . ? O7C Cl7 O7A 108.0(3) . . ? O7D Cl7 O7A 109.9(3) . . ? O7B Cl7 O7A 108.9(3) . . ? O8C Cl8 O8A 110.0(3) . . ? O8C Cl8 O8B 109.7(3) . . ? O8A Cl8 O8B 109.5(3) . . ? O8C Cl8 O8D 110.1(3) . . ? O8A Cl8 O8D 109.2(3) . . ? O8B Cl8 O8D 108.3(3) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 70.12 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 2.031 _refine_diff_density_min -1.851 _refine_diff_density_rms 0.141