# 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 loop_ _publ_author_name _publ_author_address 'Craig Rice' ; Thomas Riis-Johannesen Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30, quai E. Ansermet CH - 1211 Geneva 4 Switzerland ; 'Georgios Bokolinis' ; Department of Chemical and Biological Sciences, University of Huddersfield ; 'J. Jeffery' ; Department of Chemical and Biological Sciences, University of Huddersfield ; 'T. Riis-Johannessen' ; School of Chemistry, University of Bristol, Cantocks Close, Bristol BS8 1TS, U.K ; _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 ; Synthesis and X-Ray Structures of Cadmium-Containing Dinuclear Double Helicates Derived from Ligands Containing N-Oxide Units. ; # Attachment 'CRRCIF2.cif' #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Dr. Craig Rice Department of Chemistry and Biological Sciences University of Huddersfield Huddersfield HD1 3DH ; _publ_contact_author_fax '01484 472182' _publ_contact_letter ; This CIF file contains details one crystal structure for the paper by Craig Rice, et al, submitted to NJC for publication (Two structures submitted separately craigz1 and craigzm). ; data_CRRCIF1 _database_code_depnum_ccdc_archive 'CCDC 654463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H42 Cd2 Cl4 N10 O20 S4' _chemical_formula_weight 1597.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.568(4) _cell_length_b 12.894(2) _cell_length_c 21.345(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.065(4) _cell_angle_gamma 90.00 _cell_volume 6093(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12765 _cell_measurement_theta_min 4.449 _cell_measurement_theta_max 48.838 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3200 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.658630 _exptl_absorpt_correction_T_max 0.789877 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 64281 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.52 _reflns_number_total 13984 _reflns_number_gt 8783 _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. Non-hydrogen atoms Cl(2), O(2A), O(2B), O(2C), O(2D), Cl(3), O(3A), O(3B), O(3C), O(3D), O(3E), O(3F), O(3G) and O(3H) were refined with isotropic thermal parameters due to unstable anisotropic behavior. The crystal sustained rapid solvent loss on removal from the mother liquor resulting in one poorly defined ethyl acetate solvate in the asymmetric unit. As attempts at modeling unsuccessful scattering contributions from the affected region were removed using the SQUEEZE routine in PLATON (Spek, A. L. Acta. Cryst. 1990, A46, C-34). The estimated solvent content per asymmetric unit is thus one EtCO2Me molecule per asymmetric unit. ; _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^)+(0.1103P)^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 13984 _refine_ls_number_parameters 812 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1615 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.237380(15) 0.73233(3) 0.138631(17) 0.03619(10) Uani 1 1 d . . . Cd2 Cd 0.233978(15) 0.67561(3) 0.322830(17) 0.03806(10) Uani 1 1 d . . . N11 N 0.32753(18) 0.6682(3) 0.1390(2) 0.0446(10) Uani 1 1 d . . . C12 C 0.3310(2) 0.5676(5) 0.1370(2) 0.0507(14) Uani 1 1 d . . . S13 S 0.39811(8) 0.52319(17) 0.13350(9) 0.0823(6) Uani 1 1 d . . . C14 C 0.4220(3) 0.6476(6) 0.1342(3) 0.080(2) Uani 1 1 d . . . H25 H 0.4596 0.6665 0.1327 0.095 Uiso 1 1 calc R . . C15 C 0.3794(3) 0.7156(5) 0.1372(3) 0.0603(16) Uani 1 1 d . . . C16 C 0.3853(3) 0.8299(6) 0.1373(4) 0.081(2) Uani 1 1 d . . . H40A H 0.4140 0.8520 0.1791 0.121 Uiso 1 1 calc R . . H40B H 0.3468 0.8611 0.1311 0.121 Uiso 1 1 calc R . . H40C H 0.3990 0.8506 0.1016 0.121 Uiso 1 1 calc R . . N21 N 0.22954(18) 0.5423(3) 0.13533(19) 0.0406(10) Uani 1 1 d . . . C22 C 0.2822(2) 0.4968(4) 0.1407(2) 0.0463(12) Uani 1 1 d . . . C23 C 0.2922(3) 0.3918(5) 0.1524(3) 0.0611(16) Uani 1 1 d . . . H41 H 0.3292 0.3622 0.1562 0.073 Uiso 1 1 calc R . . C24 C 0.2456(3) 0.3323(5) 0.1581(3) 0.0650(17) Uani 1 1 d . . . H28 H 0.2505 0.2610 0.1646 0.078 Uiso 1 1 calc R . . C25 C 0.1924(3) 0.3778(4) 0.1542(3) 0.0566(14) Uani 1 1 d . . . H20 H 0.1610 0.3384 0.1587 0.068 Uiso 1 1 calc R . . C26 C 0.1856(2) 0.4841(4) 0.1433(2) 0.0412(11) Uani 1 1 d . . . N31 N 0.13217(16) 0.6219(3) 0.17946(18) 0.0350(9) Uani 1 1 d . . . O31 O 0.18674(13) 0.6658(2) 0.20773(15) 0.0350(7) Uani 1 1 d . . . C32 C 0.1289(2) 0.5320(4) 0.1438(2) 0.0399(11) Uani 1 1 d . . . C33 C 0.0726(2) 0.4888(4) 0.1133(3) 0.0546(14) Uani 1 1 d . . . H42 H 0.0686 0.4288 0.0880 0.066 Uiso 1 1 calc R . . C34 C 0.0219(3) 0.5350(5) 0.1204(3) 0.0606(16) Uani 1 1 d . . . H33 H -0.0161 0.5065 0.0993 0.073 Uiso 1 1 calc R . . C35 C 0.0279(2) 0.6224(4) 0.1584(3) 0.0522(14) Uani 1 1 d . . . H31 H -0.0061 0.6510 0.1644 0.063 Uiso 1 1 calc R . . C36 C 0.0836(2) 0.6687(4) 0.1880(3) 0.0404(11) Uani 1 1 d . . . N41 N 0.14102(18) 0.7822(3) 0.2805(2) 0.0450(10) Uani 1 1 d . . . C42 C 0.1474(2) 0.8751(4) 0.3110(3) 0.0566(15) Uani 1 1 d . . . C43 C 0.1052(3) 0.9523(5) 0.2912(4) 0.077(2) Uani 1 1 d . . . H39 H 0.1109 1.0148 0.3143 0.092 Uiso 1 1 calc R . . C44 C 0.0547(3) 0.9357(5) 0.2368(4) 0.071(2) Uani 1 1 d . . . H56 H 0.0249 0.9866 0.2232 0.085 Uiso 1 1 calc R . . C45 C 0.0475(2) 0.8422(4) 0.2016(3) 0.0600(16) Uani 1 1 d . . . H52 H 0.0141 0.8305 0.1634 0.072 Uiso 1 1 calc R . . C46 C 0.0924(2) 0.7671(4) 0.2259(3) 0.0447(12) Uani 1 1 d . . . N51 N 0.2536(2) 0.8310(4) 0.3788(2) 0.0614(13) Uani 1 1 d . . . C52 C 0.2066(3) 0.8938(5) 0.3664(3) 0.0627(16) Uani 1 1 d . . . S53 S 0.22054(10) 1.00314(15) 0.41348(10) 0.0866(6) Uani 1 1 d . . . C54 C 0.2936(4) 0.9637(6) 0.4516(4) 0.095(3) Uani 1 1 d . . . H57 H 0.3228 1.0015 0.4842 0.114 Uiso 1 1 calc R . . C55 C 0.3036(3) 0.8706(6) 0.4282(3) 0.078(2) Uani 1 1 d . . . C56 C 0.3616(3) 0.8148(8) 0.4525(4) 0.109(3) Uani 1 1 d . . . H59A H 0.3627 0.7636 0.4203 0.164 Uiso 1 1 calc R . . H59B H 0.3658 0.7813 0.4940 0.164 Uiso 1 1 calc R . . H59C H 0.3942 0.8630 0.4591 0.164 Uiso 1 1 calc R . . N61 N 0.14982(18) 0.8085(3) 0.0770(2) 0.0394(9) Uani 1 1 d . . . C62 C 0.1425(2) 0.9041(4) 0.0944(3) 0.0495(13) Uani 1 1 d . . . S63 S 0.07801(8) 0.96058(15) 0.04217(12) 0.0978(8) Uani 1 1 d . . . C64 C 0.0616(3) 0.8519(6) -0.0059(4) 0.087(2) Uani 1 1 d . . . H58 H 0.0279 0.8443 -0.0443 0.104 Uiso 1 1 calc R . . C65 C 0.1048(2) 0.7769(5) 0.0195(3) 0.0527(14) Uani 1 1 d . . . C66 C 0.1064(3) 0.6740(5) -0.0103(3) 0.0624(16) Uani 1 1 d . . . H30A H 0.1475 0.6514 0.0015 0.094 Uiso 1 1 calc R . . H30B H 0.0884 0.6787 -0.0579 0.094 Uiso 1 1 calc R . . H30C H 0.0842 0.6252 0.0063 0.094 Uiso 1 1 calc R . . N71 N 0.23856(17) 0.9091(3) 0.1814(2) 0.0414(10) Uani 1 1 d . . . C72 C 0.1862(2) 0.9577(4) 0.1523(3) 0.0480(13) Uani 1 1 d . . . C73 C 0.1716(3) 1.0509(4) 0.1752(3) 0.0603(16) Uani 1 1 d . . . H35 H 0.1347 1.0828 0.1533 0.072 Uiso 1 1 calc R . . C74 C 0.2120(3) 1.0945(5) 0.2298(3) 0.0649(17) Uani 1 1 d . . . H32 H 0.2031 1.1570 0.2461 0.078 Uiso 1 1 calc R . . C75 C 0.2667(3) 1.0461(4) 0.2615(3) 0.0574(15) Uani 1 1 d . . . H27 H 0.2952 1.0759 0.2988 0.069 Uiso 1 1 calc R . . C76 C 0.2785(2) 0.9517(4) 0.2364(3) 0.0444(12) Uani 1 1 d . . . N81 N 0.33553(17) 0.7934(3) 0.2793(2) 0.0433(10) Uani 1 1 d . . . O81 O 0.28330(13) 0.7440(2) 0.25424(15) 0.0374(7) Uani 1 1 d . . . C82 C 0.3360(2) 0.8984(4) 0.2720(3) 0.0468(12) Uani 1 1 d . . . C83 C 0.3908(2) 0.9485(5) 0.2987(3) 0.0636(17) Uani 1 1 d . . . H43 H 0.3928 1.0202 0.2955 0.076 Uiso 1 1 calc R . . C84 C 0.4427(3) 0.8920(6) 0.3301(4) 0.079(2) Uani 1 1 d . . . H36 H 0.4795 0.9263 0.3467 0.095 Uiso 1 1 calc R . . C85 C 0.4408(3) 0.7868(6) 0.3370(3) 0.0694(19) Uani 1 1 d . . . H44 H 0.4761 0.7497 0.3578 0.083 Uiso 1 1 calc R . . C86 C 0.3855(2) 0.7357(5) 0.3127(3) 0.0494(13) Uani 1 1 d . . . N91 N 0.33126(18) 0.5843(3) 0.32961(19) 0.0413(10) Uani 1 1 d . . . C92 C 0.3800(2) 0.6236(5) 0.3187(3) 0.0480(13) Uani 1 1 d . . . C93 C 0.4255(3) 0.5572(5) 0.3123(3) 0.0603(16) Uani 1 1 d . . . H34 H 0.4590 0.5845 0.3047 0.072 Uiso 1 1 calc R . . C94 C 0.4197(3) 0.4530(6) 0.3174(3) 0.075(2) Uani 1 1 d . . . H38 H 0.4496 0.4088 0.3139 0.089 Uiso 1 1 calc R . . C95 C 0.3703(3) 0.4134(5) 0.3275(3) 0.0644(17) Uani 1 1 d . . . H24 H 0.3661 0.3421 0.3309 0.077 Uiso 1 1 calc R . . C96 C 0.3260(3) 0.4809(4) 0.3327(2) 0.0493(13) Uani 1 1 d . . . N101 N 0.22133(19) 0.4996(3) 0.32921(19) 0.0433(10) Uani 1 1 d . . . C102 C 0.2690(3) 0.4424(4) 0.3385(2) 0.0458(12) Uani 1 1 d . . . S103 S 0.25980(9) 0.31607(13) 0.35718(9) 0.0715(5) Uani 1 1 d . . . C104 C 0.1878(3) 0.3433(5) 0.3517(3) 0.073(2) Uani 1 1 d . . . H54 H 0.1612 0.2950 0.3587 0.087 Uiso 1 1 calc R . . C105 C 0.1740(3) 0.4432(5) 0.3361(3) 0.0567(15) Uani 1 1 d . . . C106 C 0.1128(3) 0.4938(5) 0.3249(3) 0.0677(18) Uani 1 1 d . . . H37A H 0.0859 0.4777 0.2808 0.102 Uiso 1 1 calc R . . H37B H 0.1178 0.5676 0.3297 0.102 Uiso 1 1 calc R . . H37C H 0.0963 0.4679 0.3572 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.23800(7) 0.86445(17) -0.01871(8) 0.0801(5) Uani 1 1 d . . . O1A O 0.2229(3) 0.9484(5) 0.0134(3) 0.111(2) Uani 1 1 d . . . O1B O 0.2530(2) 0.7756(4) 0.0246(2) 0.0827(15) Uani 1 1 d . . . O1C O 0.1880(2) 0.8385(4) -0.0771(2) 0.0933(17) Uani 1 1 d . . . O1D O 0.2869(2) 0.8904(5) -0.0408(2) 0.0991(19) Uani 1 1 d . . . Cl2 Cl 0.44236(16) 0.3606(3) 0.95323(18) 0.0746(9) Uiso 0.50 1 d PD . . O2A O 0.4731(7) 0.2594(10) 0.9719(9) 0.199(8) Uiso 0.50 1 d PD . . O2B O 0.4819(5) 0.4226(9) 0.9256(6) 0.119(4) Uiso 0.50 1 d PD . . O2C O 0.4432(5) 0.4006(9) 1.0123(5) 0.115(4) Uiso 0.50 1 d PD . . O2D O 0.3851(3) 0.3473(6) 0.9040(4) 0.067(2) Uiso 0.50 1 d PD . . Cl3A Cl 0.42192(12) 0.1852(2) 0.20380(15) 0.0576(7) Uiso 0.60 1 d PD A 1 O3A O 0.4214(6) 0.2529(9) 0.1514(6) 0.151(5) Uiso 0.60 1 d PD A 1 O3B O 0.3642(3) 0.1854(6) 0.2172(4) 0.077(2) Uiso 0.60 1 d PD A 1 O3C O 0.4648(6) 0.2420(11) 0.2633(7) 0.201(7) Uiso 0.60 1 d PD A 1 O3D O 0.4441(5) 0.0872(7) 0.2002(6) 0.116(4) Uiso 0.60 1 d PD A 1 Cl3B Cl 0.4191(2) 0.1856(4) 0.2288(3) 0.0682(12) Uiso 0.40 1 d PD B 2 O3E O 0.4262(7) 0.1961(12) 0.2970(5) 0.120(5) Uiso 0.40 1 d PD B 2 O3F O 0.4340(5) 0.2791(7) 0.1998(5) 0.067(3) Uiso 0.40 1 d PD B 2 O3G O 0.3556(4) 0.1549(8) 0.1902(5) 0.059(3) Uiso 0.40 1 d PD B 2 O3H O 0.4601(4) 0.0989(7) 0.2328(5) 0.057(3) Uiso 0.40 1 d PD B 2 Cl4 Cl 0.04087(7) 0.22990(11) 0.19478(8) 0.0613(4) Uani 1 1 d . . . O4A O 0.0790(5) 0.1913(9) 0.2553(5) 0.084(3) Uani 0.50 1 d P C 1 O4B O 0.0344(6) 0.3379(8) 0.1982(7) 0.090(4) Uani 0.50 1 d P C 1 O4C O 0.0626(4) 0.2135(7) 0.1380(5) 0.067(2) Uani 0.50 1 d P C 1 O4D O -0.0176(4) 0.1779(8) 0.1809(5) 0.070(2) Uani 0.50 1 d P C 1 O4E O 0.0988(5) 0.2688(11) 0.2046(8) 0.125(5) Uani 0.50 1 d P C 2 O4F O -0.0024(6) 0.3106(12) 0.1752(8) 0.114(5) Uani 0.50 1 d P C 2 O4G O 0.0322(9) 0.1448(10) 0.1541(7) 0.176(9) Uani 0.50 1 d P C 2 O4H O 0.0502(8) 0.2021(14) 0.2648(9) 0.181(7) Uani 0.50 1 d P C 2 Cl5 Cl 0.89818(15) 0.7328(2) 0.01973(13) 0.0616(8) Uani 0.50 1 d PD . . O5A O 0.8594(4) 0.7920(7) -0.0342(5) 0.106(4) Uani 0.50 1 d PD . . O5B O 0.8784(5) 0.6521(10) 0.0411(7) 0.155(6) Uani 0.50 1 d PD . . O5C O 0.9493(5) 0.6881(10) 0.0042(5) 0.149(6) Uani 0.50 1 d PD . . O5D O 0.9293(5) 0.8107(8) 0.0710(5) 0.126(5) Uani 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03390(18) 0.03787(19) 0.03841(19) 0.00511(15) 0.01450(15) 0.00367(14) Cd2 0.03467(19) 0.0448(2) 0.03741(18) -0.00603(15) 0.01581(15) -0.00482(15) N11 0.039(2) 0.061(3) 0.037(2) 0.011(2) 0.0176(18) 0.011(2) C12 0.042(3) 0.077(4) 0.034(3) 0.010(3) 0.014(2) 0.022(3) S13 0.0648(10) 0.1128(15) 0.0842(11) 0.0308(11) 0.0450(9) 0.0471(10) C14 0.046(3) 0.128(6) 0.076(4) 0.030(4) 0.035(3) 0.015(4) C15 0.043(3) 0.090(5) 0.052(3) 0.018(3) 0.022(3) 0.005(3) C16 0.060(4) 0.109(6) 0.083(5) 0.015(4) 0.036(4) -0.017(4) N21 0.046(2) 0.041(2) 0.035(2) 0.0021(17) 0.0141(18) 0.0080(18) C22 0.053(3) 0.056(3) 0.031(2) 0.006(2) 0.017(2) 0.017(3) C23 0.076(4) 0.056(4) 0.051(3) 0.001(3) 0.021(3) 0.027(3) C24 0.086(5) 0.037(3) 0.067(4) -0.001(3) 0.021(3) 0.012(3) C25 0.065(4) 0.044(3) 0.056(3) -0.006(3) 0.014(3) -0.003(3) C26 0.044(3) 0.039(3) 0.038(3) -0.002(2) 0.010(2) 0.004(2) N31 0.0289(19) 0.036(2) 0.038(2) 0.0044(17) 0.0092(16) -0.0039(16) O31 0.0275(15) 0.0409(18) 0.0367(16) -0.0031(14) 0.0111(13) -0.0059(13) C32 0.044(3) 0.035(3) 0.038(2) 0.004(2) 0.011(2) -0.007(2) C33 0.052(3) 0.044(3) 0.057(3) 0.002(3) 0.005(3) -0.013(3) C34 0.038(3) 0.057(4) 0.077(4) 0.002(3) 0.006(3) -0.015(3) C35 0.032(3) 0.052(3) 0.067(4) 0.006(3) 0.011(3) -0.004(2) C36 0.026(2) 0.041(3) 0.055(3) 0.005(2) 0.014(2) 0.0013(19) N41 0.039(2) 0.044(2) 0.060(3) -0.007(2) 0.026(2) -0.0012(19) C42 0.052(3) 0.050(3) 0.083(4) -0.013(3) 0.043(3) -0.002(3) C43 0.061(4) 0.041(3) 0.150(7) -0.015(4) 0.065(4) -0.001(3) C44 0.041(3) 0.048(3) 0.130(6) 0.000(4) 0.037(4) 0.008(3) C45 0.040(3) 0.043(3) 0.102(5) 0.010(3) 0.031(3) -0.002(2) C46 0.033(2) 0.039(3) 0.070(3) 0.005(2) 0.027(2) 0.000(2) N51 0.051(3) 0.077(3) 0.060(3) -0.033(3) 0.023(2) -0.012(2) C52 0.066(4) 0.063(4) 0.073(4) -0.028(3) 0.042(3) -0.022(3) S53 0.1044(14) 0.0733(11) 0.0997(13) -0.0467(10) 0.0576(11) -0.0230(10) C54 0.092(5) 0.113(6) 0.091(5) -0.060(5) 0.046(4) -0.040(5) C55 0.072(4) 0.109(6) 0.061(4) -0.044(4) 0.034(3) -0.024(4) C56 0.048(4) 0.193(10) 0.078(5) -0.060(6) 0.011(4) -0.014(5) N61 0.035(2) 0.041(2) 0.041(2) 0.0037(18) 0.0108(18) 0.0007(17) C62 0.039(3) 0.047(3) 0.059(3) 0.004(3) 0.011(2) 0.011(2) S63 0.0623(11) 0.0705(11) 0.1151(16) -0.0243(11) -0.0282(11) 0.0333(9) C64 0.049(4) 0.085(5) 0.088(5) -0.022(4) -0.025(4) 0.016(3) C65 0.045(3) 0.059(3) 0.048(3) 0.004(3) 0.008(3) -0.004(3) C66 0.069(4) 0.056(4) 0.052(3) -0.009(3) 0.008(3) -0.002(3) N71 0.033(2) 0.041(2) 0.050(2) 0.0007(19) 0.0133(19) -0.0015(17) C72 0.039(3) 0.044(3) 0.059(3) -0.001(2) 0.014(2) 0.003(2) C73 0.045(3) 0.050(3) 0.078(4) -0.011(3) 0.010(3) 0.005(3) C74 0.055(4) 0.047(3) 0.089(5) -0.014(3) 0.021(3) -0.003(3) C75 0.054(3) 0.048(3) 0.065(4) -0.015(3) 0.014(3) -0.016(3) C76 0.033(3) 0.038(3) 0.061(3) 0.002(2) 0.015(2) -0.008(2) N81 0.026(2) 0.058(3) 0.046(2) 0.004(2) 0.0135(18) -0.0056(18) O81 0.0239(15) 0.0490(19) 0.0368(17) -0.0004(14) 0.0072(13) -0.0070(14) C82 0.035(3) 0.050(3) 0.053(3) -0.002(2) 0.012(2) -0.011(2) C83 0.038(3) 0.066(4) 0.077(4) 0.007(3) 0.008(3) -0.018(3) C84 0.035(3) 0.089(5) 0.101(5) 0.009(4) 0.008(3) -0.026(3) C85 0.033(3) 0.085(5) 0.084(5) 0.020(4) 0.012(3) -0.003(3) C86 0.027(2) 0.070(4) 0.051(3) 0.004(3) 0.014(2) -0.001(2) N91 0.041(2) 0.052(3) 0.032(2) -0.0019(18) 0.0139(18) 0.0058(19) C92 0.037(3) 0.065(4) 0.044(3) 0.009(3) 0.016(2) 0.008(3) C93 0.043(3) 0.080(4) 0.058(3) 0.010(3) 0.018(3) 0.013(3) C94 0.070(4) 0.094(5) 0.060(4) 0.012(4) 0.022(3) 0.042(4) C95 0.066(4) 0.065(4) 0.057(4) -0.006(3) 0.015(3) 0.022(3) C96 0.058(3) 0.057(3) 0.032(3) -0.004(2) 0.014(2) 0.007(3) N101 0.050(2) 0.046(2) 0.032(2) 0.0012(18) 0.0121(19) -0.010(2) C102 0.059(3) 0.046(3) 0.029(2) -0.005(2) 0.010(2) -0.001(3) S103 0.0925(13) 0.0456(9) 0.0664(10) 0.0062(8) 0.0144(9) -0.0042(8) C104 0.082(5) 0.062(4) 0.058(4) 0.011(3) 0.005(3) -0.025(3) C105 0.063(4) 0.060(4) 0.041(3) 0.001(3) 0.010(3) -0.021(3) C106 0.049(3) 0.090(5) 0.059(4) 0.015(3) 0.012(3) -0.021(3) Cl1 0.0586(9) 0.1273(16) 0.0582(9) 0.0385(10) 0.0249(8) 0.0048(10) O1A 0.126(5) 0.127(5) 0.101(4) 0.029(4) 0.068(4) -0.008(4) O1B 0.068(3) 0.127(4) 0.062(3) 0.049(3) 0.034(2) 0.021(3) O1C 0.073(3) 0.130(5) 0.070(3) 0.040(3) 0.015(3) 0.006(3) O1D 0.069(3) 0.166(5) 0.070(3) 0.048(3) 0.034(2) -0.002(3) Cl4 0.0554(8) 0.0501(8) 0.0802(10) 0.0128(7) 0.0256(8) 0.0070(7) O4A 0.092(8) 0.080(7) 0.049(5) 0.003(5) -0.015(6) -0.011(6) O4B 0.134(10) 0.047(5) 0.122(10) 0.011(6) 0.087(9) 0.025(7) O4C 0.046(4) 0.057(5) 0.109(7) -0.021(5) 0.040(5) 0.000(4) O4D 0.060(5) 0.080(6) 0.078(6) -0.009(5) 0.035(5) -0.022(5) O4E 0.080(8) 0.124(11) 0.164(12) 0.024(10) 0.034(8) 0.005(7) O4F 0.088(8) 0.120(11) 0.147(12) 0.066(9) 0.059(9) 0.067(8) O4G 0.234(18) 0.067(8) 0.117(11) -0.012(8) -0.081(12) 0.032(10) O4H 0.260(15) 0.182(13) 0.193(13) 0.122(10) 0.198(12) 0.158(12) Cl5 0.073(2) 0.0622(18) 0.0395(14) -0.0100(13) 0.0057(14) 0.0183(15) O5A 0.080(7) 0.077(7) 0.104(8) 0.012(6) -0.041(6) -0.008(6) O5B 0.060(7) 0.189(14) 0.179(14) 0.057(12) -0.007(8) -0.048(8) O5C 0.213(15) 0.154(12) 0.061(6) -0.009(7) 0.025(8) 0.112(11) O5D 0.148(11) 0.114(9) 0.066(6) -0.019(6) -0.027(7) 0.059(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 Cd1 N61 2.256(4) . ? Cd1 N11 2.277(4) . ? Cd1 O81 2.335(3) . ? Cd1 O31 2.355(3) . ? Cd1 N71 2.452(4) . ? Cd1 N21 2.456(4) . ? Cd1 O1B 2.644(4) . ? Cd2 N51 2.297(5) . ? Cd2 N101 2.300(4) . ? Cd2 O31 2.327(3) . ? Cd2 O81 2.332(3) . ? Cd2 N41 2.480(4) . ? Cd2 N91 2.537(4) . ? N11 C12 1.301(7) . ? N11 C15 1.380(7) . ? C12 C22 1.493(8) . ? C12 S13 1.708(5) . ? S13 C14 1.699(8) . ? C14 C15 1.349(9) . ? C15 C16 1.480(10) . ? N21 C26 1.336(6) . ? N21 C22 1.341(6) . ? C22 C23 1.382(8) . ? C23 C24 1.379(9) . ? C24 C25 1.362(8) . ? C25 C26 1.391(7) . ? C26 C32 1.476(7) . ? N31 O31 1.344(4) . ? N31 C36 1.362(6) . ? N31 C32 1.374(6) . ? C32 C33 1.379(7) . ? C33 C34 1.388(8) . ? C34 C35 1.367(8) . ? C35 C36 1.383(7) . ? C36 C46 1.480(7) . ? N41 C46 1.338(7) . ? N41 C42 1.346(7) . ? C42 C43 1.367(8) . ? C42 C52 1.507(8) . ? C43 C44 1.365(9) . ? C44 C45 1.401(9) . ? C45 C46 1.397(7) . ? N51 C52 1.323(8) . ? N51 C55 1.382(8) . ? C52 S53 1.697(6) . ? S53 C54 1.711(8) . ? C54 C55 1.352(10) . ? C55 C56 1.473(10) . ? N61 C62 1.315(7) . ? N61 C65 1.381(7) . ? C62 C72 1.481(7) . ? C62 S63 1.709(5) . ? S63 C64 1.702(7) . ? C64 C65 1.373(8) . ? C65 C66 1.477(8) . ? N71 C72 1.332(6) . ? N71 C76 1.345(6) . ? C72 C73 1.385(8) . ? C73 C74 1.350(8) . ? C74 C75 1.383(8) . ? C75 C76 1.394(7) . ? C76 C82 1.476(7) . ? N81 O81 1.325(5) . ? N81 C82 1.364(7) . ? N81 C86 1.368(7) . ? C82 C83 1.380(7) . ? C83 C84 1.383(9) . ? C84 C85 1.368(10) . ? C85 C86 1.391(8) . ? C86 C92 1.461(8) . ? N91 C96 1.343(7) . ? N91 C92 1.347(6) . ? C92 C93 1.415(8) . ? C93 C94 1.358(10) . ? C94 C95 1.353(9) . ? C95 C96 1.393(8) . ? C96 C102 1.477(8) . ? N101 C102 1.300(7) . ? N101 C105 1.380(7) . ? C102 S103 1.708(5) . ? S103 C104 1.697(8) . ? C104 C105 1.343(9) . ? C105 C106 1.525(8) . ? Cl1 O1A 1.392(7) . ? Cl1 O1D 1.426(5) . ? Cl1 O1C 1.431(5) . ? Cl1 O1B 1.437(5) . ? Cl2 O2C 1.357(9) . ? Cl2 O2D 1.408(8) . ? Cl2 O2A 1.478(11) . ? Cl2 O2B 1.494(10) . ? Cl3A O3D 1.380(9) . ? Cl3A O3A 1.414(10) . ? Cl3A O3B 1.483(8) . ? Cl3A O3C 1.513(11) . ? Cl3B O3E 1.412(11) . ? Cl3B O3F 1.452(9) . ? Cl3B O3H 1.462(9) . ? Cl3B O3G 1.493(9) . ? Cl4 O4G 1.370(13) . ? Cl4 O4A 1.388(10) . ? Cl4 O4E 1.401(12) . ? Cl4 O4B 1.406(11) . ? Cl4 O4F 1.417(12) . ? Cl4 O4D 1.468(8) . ? Cl4 O4H 1.479(15) . ? Cl4 O4C 1.484(9) . ? Cl5 O5B 1.286(10) . ? Cl5 O5A 1.422(8) . ? Cl5 O5C 1.472(10) . ? Cl5 O5D 1.481(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 N61 Cd1 N11 145.68(14) . . ? N61 Cd1 O81 125.98(13) . . ? N11 Cd1 O81 85.76(13) . . ? N61 Cd1 O31 87.99(13) . . ? N11 Cd1 O31 122.56(13) . . ? O81 Cd1 O31 60.81(10) . . ? N61 Cd1 N71 72.75(14) . . ? N11 Cd1 N71 116.41(15) . . ? O81 Cd1 N71 66.72(12) . . ? O31 Cd1 N71 92.82(12) . . ? N61 Cd1 N21 111.88(14) . . ? N11 Cd1 N21 72.47(15) . . ? O81 Cd1 N21 95.60(12) . . ? O31 Cd1 N21 66.73(12) . . ? N71 Cd1 N21 158.30(13) . . ? N61 Cd1 O1B 76.12(14) . . ? N11 Cd1 O1B 69.84(14) . . ? O81 Cd1 O1B 143.05(13) . . ? O31 Cd1 O1B 156.13(13) . . ? N71 Cd1 O1B 99.16(15) . . ? N21 Cd1 O1B 102.54(15) . . ? N51 Cd2 N101 146.86(17) . . ? N51 Cd2 O31 122.32(16) . . ? N101 Cd2 O31 89.07(12) . . ? N51 Cd2 O81 86.68(15) . . ? N101 Cd2 O81 120.86(13) . . ? O31 Cd2 O81 61.24(10) . . ? N51 Cd2 N41 72.60(16) . . ? N101 Cd2 N41 116.91(15) . . ? O31 Cd2 N41 66.57(13) . . ? O81 Cd2 N41 97.46(13) . . ? N51 Cd2 N91 111.01(15) . . ? N101 Cd2 N91 70.82(15) . . ? O31 Cd2 N91 97.50(11) . . ? O81 Cd2 N91 64.90(12) . . ? N41 Cd2 N91 161.13(13) . . ? C12 N11 C15 112.0(5) . . ? C12 N11 Cd1 115.5(4) . . ? C15 N11 Cd1 132.4(4) . . ? N11 C12 C22 123.3(5) . . ? N11 C12 S13 113.9(4) . . ? C22 C12 S13 122.7(4) . . ? C14 S13 C12 89.5(3) . . ? C15 C14 S13 111.4(5) . . ? C14 C15 N11 113.2(6) . . ? C14 C15 C16 125.2(6) . . ? N11 C15 C16 121.6(5) . . ? C26 N21 C22 118.5(4) . . ? C26 N21 Cd1 127.6(3) . . ? C22 N21 Cd1 112.1(3) . . ? N21 C22 C23 122.7(5) . . ? N21 C22 C12 115.8(5) . . ? C23 C22 C12 121.4(5) . . ? C24 C23 C22 117.9(6) . . ? C25 C24 C23 120.0(6) . . ? C24 C25 C26 119.1(6) . . ? N21 C26 C25 121.7(5) . . ? N21 C26 C32 120.6(4) . . ? C25 C26 C32 117.6(5) . . ? O31 N31 C36 118.2(4) . . ? O31 N31 C32 117.9(4) . . ? C36 N31 C32 123.9(4) . . ? N31 O31 Cd2 122.3(2) . . ? N31 O31 Cd1 119.0(2) . . ? Cd2 O31 Cd1 118.66(12) . . ? N31 C32 C33 117.7(5) . . ? N31 C32 C26 118.5(4) . . ? C33 C32 C26 123.7(5) . . ? C32 C33 C34 119.9(5) . . ? C35 C34 C33 120.1(5) . . ? C34 C35 C36 121.1(5) . . ? N31 C36 C35 117.2(5) . . ? N31 C36 C46 119.1(4) . . ? C35 C36 C46 123.6(5) . . ? C46 N41 C42 118.1(5) . . ? C46 N41 Cd2 128.5(3) . . ? C42 N41 Cd2 112.2(3) . . ? N41 C42 C43 123.3(6) . . ? N41 C42 C52 116.2(5) . . ? C43 C42 C52 120.3(6) . . ? C44 C43 C42 118.6(6) . . ? C43 C44 C45 120.1(6) . . ? C46 C45 C44 117.4(6) . . ? N41 C46 C45 122.4(5) . . ? N41 C46 C36 121.2(4) . . ? C45 C46 C36 116.4(5) . . ? C52 N51 C55 111.3(5) . . ? C52 N51 Cd2 115.1(4) . . ? C55 N51 Cd2 133.3(5) . . ? N51 C52 C42 123.0(5) . . ? N51 C52 S53 114.3(5) . . ? C42 C52 S53 122.5(5) . . ? C52 S53 C54 89.6(3) . . ? C55 C54 S53 111.2(5) . . ? C54 C55 N51 113.6(7) . . ? C54 C55 C56 124.2(7) . . ? N51 C55 C56 122.3(6) . . ? C62 N61 C65 113.1(4) . . ? C62 N61 Cd1 115.2(3) . . ? C65 N61 Cd1 131.3(4) . . ? N61 C62 C72 123.5(4) . . ? N61 C62 S63 112.9(4) . . ? C72 C62 S63 123.6(4) . . ? C64 S63 C62 90.6(3) . . ? C65 C64 S63 110.9(5) . . ? C64 C65 N61 112.5(5) . . ? C64 C65 C66 125.9(5) . . ? N61 C65 C66 121.5(5) . . ? C72 N71 C76 118.3(4) . . ? C72 N71 Cd1 111.9(3) . . ? C76 N71 Cd1 128.3(3) . . ? N71 C72 C73 123.2(5) . . ? N71 C72 C62 115.9(5) . . ? C73 C72 C62 120.9(5) . . ? C74 C73 C72 118.6(5) . . ? C73 C74 C75 119.9(6) . . ? C74 C75 C76 118.8(5) . . ? N71 C76 C75 121.3(5) . . ? N71 C76 C82 120.2(5) . . ? C75 C76 C82 118.5(5) . . ? O81 N81 C82 118.3(4) . . ? O81 N81 C86 117.6(4) . . ? C82 N81 C86 124.1(4) . . ? N81 O81 Cd2 121.5(3) . . ? N81 O81 Cd1 119.2(3) . . ? Cd2 O81 Cd1 119.27(12) . . ? N81 C82 C83 117.4(5) . . ? N81 C82 C76 118.7(4) . . ? C83 C82 C76 123.9(5) . . ? C82 C83 C84 120.0(6) . . ? C85 C84 C83 121.2(5) . . ? C84 C85 C86 119.3(6) . . ? N81 C86 C85 117.8(5) . . ? N81 C86 C92 119.8(4) . . ? C85 C86 C92 122.3(5) . . ? C96 N91 C92 118.7(5) . . ? C96 N91 Cd2 111.5(3) . . ? C92 N91 Cd2 128.6(3) . . ? N91 C92 C93 120.5(5) . . ? N91 C92 C86 119.6(5) . . ? C93 C92 C86 119.8(5) . . ? C94 C93 C92 119.4(6) . . ? C95 C94 C93 120.1(6) . . ? C94 C95 C96 119.1(6) . . ? N91 C96 C95 122.2(5) . . ? N91 C96 C102 116.1(5) . . ? C95 C96 C102 121.7(5) . . ? C102 N101 C105 111.9(5) . . ? C102 N101 Cd2 116.5(3) . . ? C105 N101 Cd2 130.7(4) . . ? N101 C102 C96 124.0(5) . . ? N101 C102 S103 113.8(4) . . ? C96 C102 S103 122.1(4) . . ? C104 S103 C102 89.5(3) . . ? C105 C104 S103 111.5(5) . . ? C104 C105 N101 113.3(6) . . ? C104 C105 C106 125.8(6) . . ? N101 C105 C106 120.9(5) . . ? O1A Cl1 O1D 110.6(4) . . ? O1A Cl1 O1C 109.7(4) . . ? O1D Cl1 O1C 106.6(3) . . ? O1A Cl1 O1B 110.6(3) . . ? O1D Cl1 O1B 110.5(3) . . ? O1C Cl1 O1B 108.7(3) . . ? Cl1 O1B Cd1 132.7(3) . . ? O2C Cl2 O2D 116.4(6) . . ? O2C Cl2 O2A 103.6(8) . . ? O2D Cl2 O2A 110.5(8) . . ? O2C Cl2 O2B 110.5(7) . . ? O2D Cl2 O2B 109.8(6) . . ? O2A Cl2 O2B 105.3(8) . . ? O3D Cl3A O3A 115.0(7) . . ? O3D Cl3A O3B 113.7(6) . . ? O3A Cl3A O3B 113.0(6) . . ? O3D Cl3A O3C 109.4(7) . . ? O3A Cl3A O3C 100.8(7) . . ? O3B Cl3A O3C 103.4(7) . . ? O3E Cl3B O3F 113.5(8) . . ? O3E Cl3B O3H 99.9(7) . . ? O3F Cl3B O3H 114.0(6) . . ? O3E Cl3B O3G 109.6(8) . . ? O3F Cl3B O3G 109.2(6) . . ? O3H Cl3B O3G 110.3(6) . . ? O4G Cl4 O4A 102.2(7) . . ? O4G Cl4 O4E 107.9(12) . . ? O4A Cl4 O4E 72.7(8) . . ? O4G Cl4 O4B 146.2(8) . . ? O4A Cl4 O4B 110.7(7) . . ? O4E Cl4 O4B 75.8(7) . . ? O4G Cl4 O4F 117.7(9) . . ? O4A Cl4 O4F 135.1(9) . . ? O4E Cl4 O4F 110.3(8) . . ? O4B Cl4 O4F 37.5(7) . . ? O4G Cl4 O4D 65.2(10) . . ? O4A Cl4 O4D 106.7(6) . . ? O4E Cl4 O4D 173.0(7) . . ? O4B Cl4 O4D 110.6(6) . . ? O4F Cl4 O4D 75.2(7) . . ? O4G Cl4 O4H 112.6(10) . . ? O4A Cl4 O4H 31.5(7) . . ? O4E Cl4 O4H 97.8(10) . . ? O4B Cl4 O4H 99.7(9) . . ? O4F Cl4 O4H 108.6(8) . . ? O4D Cl4 O4H 84.1(9) . . ? O4G Cl4 O4C 52.2(9) . . ? O4A Cl4 O4C 114.5(7) . . ? O4E Cl4 O4C 65.3(7) . . ? O4B Cl4 O4C 104.9(6) . . ? O4F Cl4 O4C 106.2(8) . . ? O4D Cl4 O4C 109.5(5) . . ? O4H Cl4 O4C 144.9(6) . . ? O5B Cl5 O5A 120.7(7) . . ? O5B Cl5 O5C 100.8(8) . . ? O5A Cl5 O5C 112.1(7) . . ? O5B Cl5 O5D 115.7(8) . . ? O5A Cl5 O5D 104.6(6) . . ? O5C Cl5 O5D 101.3(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.603 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.125 #======================================================== data_craigzm _database_code_depnum_ccdc_archive 'CCDC 654464' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H47 Cd2 Cl4 N17 O24 S4' _chemical_formula_weight 1945.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4892(8) _cell_length_b 13.6419(9) _cell_length_c 23.7577(16) _cell_angle_alpha 93.2420(10) _cell_angle_beta 99.9830(10) _cell_angle_gamma 97.9550(10) _cell_volume 3619.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8475 _cell_measurement_theta_min 4.369 _cell_measurement_theta_max 48.302 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653110 _exptl_absorpt_correction_T_max 0.843338 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; Perchlorates 2 and 4 are disordered over two positions (60:40 population parameters). In both cases, the geometries of each component were modelled using geometric restraints (DFIX). ; _diffrn_ambient_temperature 173(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 27891 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.62 _reflns_number_total 15653 _reflns_number_gt 9053 _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^)+(0.0525P)^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 15653 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 0.906 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.03785(3) 0.74979(2) 0.270231(13) 0.02892(9) Uani 1 1 d . . . Cd2 Cd 0.37171(3) 0.82880(2) 0.235602(14) 0.02772(9) Uani 1 1 d . . . N11 N -0.0044(3) 0.6318(3) 0.34669(16) 0.0399(10) Uani 1 1 d . . . C12 C -0.0236(4) 0.5325(4) 0.3390(2) 0.0483(14) Uani 1 1 d . . . H12 H -0.0562 0.5030 0.3024 0.058 Uiso 1 1 calc R . . C13 C 0.0023(5) 0.4713(5) 0.3824(3) 0.0602(16) Uani 1 1 d . . . H13 H -0.0127 0.4026 0.3755 0.072 Uiso 1 1 calc R . . C14 C 0.0516(6) 0.5165(5) 0.4368(3) 0.0657(18) Uani 1 1 d . . . H14 H 0.0746 0.4779 0.4666 0.079 Uiso 1 1 calc R . . C15 C 0.0664(5) 0.6177(5) 0.4467(2) 0.0585(16) Uani 1 1 d . . . H15 H 0.0955 0.6482 0.4834 0.070 Uiso 1 1 calc R . . C16 C 0.0370(4) 0.6738(4) 0.4007(2) 0.0387(12) Uani 1 1 d . . . N21 N 0.0544(3) 0.8338(3) 0.35939(15) 0.0334(9) Uani 1 1 d . . . C22 C 0.0487(4) 0.7824(4) 0.4073(2) 0.0376(12) Uani 1 1 d . . . C23 C 0.0520(4) 0.8435(4) 0.4558(2) 0.0444(13) Uani 1 1 d . . . H23 H 0.0490 0.8212 0.4919 0.053 Uiso 1 1 calc R . . S24 S 0.06218(12) 0.96449(11) 0.44148(5) 0.0476(4) Uani 1 1 d . . . C25 C 0.0622(4) 0.9301(4) 0.37005(19) 0.0346(11) Uani 1 1 d . . . N31 N 0.0718(3) 0.9524(3) 0.27385(15) 0.0308(9) Uani 1 1 d . . . C32 C 0.0736(4) 0.9989(3) 0.32570(19) 0.0331(11) Uani 1 1 d . . . C33 C 0.0820(4) 1.1017(4) 0.3353(2) 0.0440(13) Uani 1 1 d . . . H33 H 0.0811 1.1312 0.3714 0.053 Uiso 1 1 calc R . . C34 C 0.0917(4) 1.1585(4) 0.2895(2) 0.0497(14) Uani 1 1 d . . . H34 H 0.0990 1.2274 0.2944 0.060 Uiso 1 1 calc R . . C35 C 0.0904(4) 1.1108(4) 0.2356(2) 0.0402(12) Uani 1 1 d . . . H35 H 0.0961 1.1477 0.2042 0.048 Uiso 1 1 calc R . . C36 C 0.0804(4) 1.0081(3) 0.22927(19) 0.0304(10) Uani 1 1 d . . . N41 N 0.1116(3) 0.8686(3) 0.16395(15) 0.0275(8) Uani 1 1 d . . . O41 O 0.1612(2) 0.8280(2) 0.21004(12) 0.0313(7) Uani 1 1 d . . . C42 C 0.0684(4) 0.9565(3) 0.17110(19) 0.0287(10) Uani 1 1 d . . . C43 C 0.0103(4) 0.9948(4) 0.1235(2) 0.0364(11) Uani 1 1 d . . . H43 H -0.0209 1.0536 0.1277 0.044 Uiso 1 1 calc R . . C44 C -0.0019(4) 0.9469(4) 0.0699(2) 0.0394(12) Uani 1 1 d . . . H44 H -0.0422 0.9729 0.0382 0.047 Uiso 1 1 calc R . . C45 C 0.0453(4) 0.8606(3) 0.0631(2) 0.0357(11) Uani 1 1 d . . . H45 H 0.0390 0.8296 0.0266 0.043 Uiso 1 1 calc R . . C46 C 0.1021(4) 0.8199(3) 0.11040(19) 0.0308(10) Uani 1 1 d . . . N51 N 0.2455(3) 0.7085(3) 0.14128(15) 0.0307(9) Uani 1 1 d . . . C52 C 0.1490(4) 0.7246(3) 0.10428(18) 0.0289(10) Uani 1 1 d . . . C53 C 0.0935(4) 0.6546(4) 0.0583(2) 0.0383(12) Uani 1 1 d . . . H53 H 0.0270 0.6672 0.0330 0.046 Uiso 1 1 calc R . . C54 C 0.1384(5) 0.5684(4) 0.0514(2) 0.0430(13) Uani 1 1 d . . . H54 H 0.1026 0.5219 0.0210 0.052 Uiso 1 1 calc R . . C55 C 0.2365(4) 0.5497(4) 0.0891(2) 0.0403(12) Uani 1 1 d . . . H55 H 0.2671 0.4904 0.0855 0.048 Uiso 1 1 calc R . . C56 C 0.2885(4) 0.6233(3) 0.13309(19) 0.0330(11) Uani 1 1 d . . . N61 N 0.4429(3) 0.6809(3) 0.21723(15) 0.0302(9) Uani 1 1 d . . . C62 C 0.3967(4) 0.6137(3) 0.17392(19) 0.0309(11) Uani 1 1 d . . . S63 S 0.47557(12) 0.51603(10) 0.17107(6) 0.0440(3) Uani 1 1 d . . . C64 C 0.5727(4) 0.5677(4) 0.2306(2) 0.0423(13) Uani 1 1 d . . . H64 H 0.6381 0.5399 0.2478 0.051 Uiso 1 1 calc R . . C65 C 0.5428(4) 0.6557(3) 0.25041(19) 0.0331(11) Uani 1 1 d . . . N71 N 0.5695(3) 0.8135(3) 0.30260(16) 0.0332(9) Uani 1 1 d . . . C72 C 0.6032(4) 0.7231(3) 0.29979(19) 0.0319(11) Uani 1 1 d . . . C73 C 0.6897(4) 0.6940(4) 0.3420(2) 0.0383(12) Uani 1 1 d . . . H73 H 0.7112 0.6309 0.3390 0.046 Uiso 1 1 calc R . . C74 C 0.7427(4) 0.7609(4) 0.3885(2) 0.0469(13) Uani 1 1 d . . . H74 H 0.7981 0.7425 0.4178 0.056 Uiso 1 1 calc R . . C75 C 0.7121(4) 0.8542(4) 0.3905(2) 0.0429(13) Uani 1 1 d . . . H75 H 0.7489 0.9012 0.4204 0.051 Uiso 1 1 calc R . . C76 C 0.6258(4) 0.8778(4) 0.3473(2) 0.0390(12) Uani 1 1 d . . . H76 H 0.6055 0.9415 0.3492 0.047 Uiso 1 1 calc R . . N81 N -0.1581(3) 0.8152(3) 0.22872(17) 0.0398(10) Uani 1 1 d . . . C82 C -0.1917(4) 0.9001(4) 0.2476(2) 0.0436(13) Uani 1 1 d . . . H82 H -0.1696 0.9211 0.2864 0.052 Uiso 1 1 calc R . . C83 C -0.2577(4) 0.9577(4) 0.2119(3) 0.0508(14) Uani 1 1 d . . . H83 H -0.2789 1.0160 0.2266 0.061 Uiso 1 1 calc R . . C84 C -0.2914(4) 0.9266(4) 0.1539(2) 0.0525(15) Uani 1 1 d . . . H84 H -0.3329 0.9651 0.1288 0.063 Uiso 1 1 calc R . . C85 C -0.2626(4) 0.8385(4) 0.1341(2) 0.0463(13) Uani 1 1 d . . . H85 H -0.2870 0.8152 0.0957 0.056 Uiso 1 1 calc R . . C86 C -0.1957(4) 0.7837(4) 0.1726(2) 0.0373(12) Uani 1 1 d . . . N91 N -0.0679(3) 0.6550(3) 0.18974(16) 0.0371(10) Uani 1 1 d . . . C92 C -0.1622(4) 0.6889(4) 0.1552(2) 0.0394(12) Uani 1 1 d . . . C93 C -0.2120(5) 0.6264(4) 0.1076(2) 0.0509(14) Uani 1 1 d . . . H93 H -0.2741 0.6388 0.0794 0.061 Uiso 1 1 calc R . . S94 S -0.14473(13) 0.52222(11) 0.10669(6) 0.0547(4) Uani 1 1 d . . . C95 C -0.0491(4) 0.5686(4) 0.16930(19) 0.0358(12) Uani 1 1 d . . . N101 N 0.1157(3) 0.5717(3) 0.24495(16) 0.0350(9) Uani 1 1 d . . . C102 C 0.0500(4) 0.5200(4) 0.1973(2) 0.0396(12) Uani 1 1 d . . . C103 C 0.0753(5) 0.4300(4) 0.1769(2) 0.0481(14) Uani 1 1 d . . . H103 H 0.0276 0.3950 0.1444 0.058 Uiso 1 1 calc R . . C104 C 0.1726(5) 0.3933(4) 0.2058(2) 0.0539(16) Uani 1 1 d . . . H104 H 0.1918 0.3332 0.1925 0.065 Uiso 1 1 calc R . . C105 C 0.2420(5) 0.4462(4) 0.2548(2) 0.0478(14) Uani 1 1 d . . . H105 H 0.3081 0.4223 0.2746 0.057 Uiso 1 1 calc R . . C106 C 0.2103(4) 0.5364(3) 0.2736(2) 0.0365(12) Uani 1 1 d . . . N111 N 0.2920(3) 0.6917(3) 0.33504(15) 0.0312(9) Uani 1 1 d . . . O111 O 0.2455(3) 0.7414(2) 0.29248(12) 0.0327(7) Uani 1 1 d . . . C112 C 0.2791(4) 0.5897(3) 0.3283(2) 0.0336(11) Uani 1 1 d . . . C113 C 0.3294(5) 0.5407(4) 0.3731(2) 0.0483(14) Uani 1 1 d . . . H113 H 0.3178 0.4716 0.3701 0.058 Uiso 1 1 calc R . . C114 C 0.3967(5) 0.5917(4) 0.4224(2) 0.0516(15) Uani 1 1 d . . . H114 H 0.4343 0.5577 0.4514 0.062 Uiso 1 1 calc R . . C115 C 0.4078(4) 0.6941(4) 0.4281(2) 0.0465(13) Uani 1 1 d . . . H115 H 0.4520 0.7289 0.4616 0.056 Uiso 1 1 calc R . . C116 C 0.3538(4) 0.7453(4) 0.38489(19) 0.0337(11) Uani 1 1 d . . . N121 N 0.3709(3) 0.9070(3) 0.34515(15) 0.0318(9) Uani 1 1 d . . . C122 C 0.3599(4) 0.8551(4) 0.3908(2) 0.0353(11) Uani 1 1 d . . . C123 C 0.3592(4) 0.9032(4) 0.4446(2) 0.0437(13) Uani 1 1 d . . . H123 H 0.3525 0.8667 0.4760 0.052 Uiso 1 1 calc R . . C124 C 0.3686(4) 1.0051(4) 0.4500(2) 0.0481(14) Uani 1 1 d . . . H124 H 0.3671 1.0375 0.4853 0.058 Uiso 1 1 calc R . . C125 C 0.3803(4) 1.0595(4) 0.4037(2) 0.0453(13) Uani 1 1 d . . . H125 H 0.3872 1.1284 0.4068 0.054 Uiso 1 1 calc R . . C126 C 0.3812(4) 1.0059(4) 0.3515(2) 0.0350(11) Uani 1 1 d . . . N131 N 0.3922(3) 1.0012(3) 0.25041(16) 0.0300(9) Uani 1 1 d . . . C132 C 0.3922(4) 1.0536(3) 0.2987(2) 0.0344(11) Uani 1 1 d . . . S133 S 0.40460(13) 1.17959(10) 0.29112(7) 0.0522(4) Uani 1 1 d . . . C134 C 0.4070(4) 1.1580(4) 0.2203(2) 0.0493(14) Uani 1 1 d . . . H134 H 0.4117 1.2069 0.1947 0.059 Uiso 1 1 calc R . . C135 C 0.4009(4) 1.0585(3) 0.2060(2) 0.0347(11) Uani 1 1 d . . . N141 N 0.4116(3) 0.9106(3) 0.14891(16) 0.0326(9) Uani 1 1 d . . . C142 C 0.4024(4) 1.0082(3) 0.1494(2) 0.0338(11) Uani 1 1 d . . . C143 C 0.3943(5) 1.0575(4) 0.0991(2) 0.0506(14) Uani 1 1 d . . . H143 H 0.3897 1.1251 0.1004 0.061 Uiso 1 1 calc R . . C144 C 0.3934(5) 1.0056(4) 0.0484(2) 0.0542(15) Uani 1 1 d . . . H144 H 0.3831 1.0365 0.0144 0.065 Uiso 1 1 calc R . . C145 C 0.4078(4) 0.9059(4) 0.0478(2) 0.0487(14) Uani 1 1 d . . . H145 H 0.4115 0.8701 0.0138 0.058 Uiso 1 1 calc R . . C146 C 0.4165(4) 0.8619(4) 0.0988(2) 0.0364(11) Uani 1 1 d . . . H146 H 0.4263 0.7954 0.0985 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.21165(11) 0.25611(9) 0.05748(6) 0.0457(3) Uani 1 1 d . . . O1A O 0.1427(4) 0.3291(3) 0.0366(2) 0.0984(17) Uani 1 1 d . . . O1B O 0.2661(4) 0.2183(3) 0.01263(16) 0.0809(13) Uani 1 1 d . . . O1C O 0.3037(3) 0.2995(3) 0.10472(14) 0.0532(10) Uani 1 1 d . . . O1D O 0.1405(4) 0.1766(3) 0.0753(2) 0.1023(17) Uani 1 1 d . . . Cl2 Cl 0.76215(13) 0.14964(11) 0.39314(6) 0.0550(4) Uani 1 1 d D . . O2A O 0.8405(5) 0.2382(3) 0.4081(2) 0.1157(19) Uani 1 1 d D A . O2B O 0.8008(10) 0.0979(6) 0.3470(4) 0.114(4) Uani 0.60 1 d PD A 1 O2C O 0.7443(9) 0.0863(5) 0.4371(3) 0.072(2) Uani 0.60 1 d PD A 1 O2D O 0.6519(6) 0.1800(8) 0.3706(5) 0.124(4) Uani 0.60 1 d PD A 1 O2E O 0.8410(14) 0.0800(8) 0.4153(6) 0.118(5) Uani 0.40 1 d PD A 2 O2F O 0.7062(12) 0.1176(9) 0.3363(4) 0.074(3) Uani 0.40 1 d PD A 2 O2G O 0.6688(11) 0.1529(16) 0.4237(6) 0.175(10) Uani 0.40 1 d PD A 2 Cl3 Cl 0.80741(12) 0.19556(10) 0.09157(6) 0.0502(3) Uani 1 1 d . . . O3A O 0.8955(3) 0.2078(3) 0.14376(16) 0.0673(11) Uani 1 1 d . . . O3B O 0.8261(4) 0.1150(3) 0.05543(17) 0.0743(13) Uani 1 1 d . . . O3C O 0.8167(4) 0.2845(3) 0.0629(2) 0.0934(15) Uani 1 1 d . . . O3D O 0.6896(3) 0.1748(3) 0.10503(18) 0.0714(12) Uani 1 1 d . . . Cl4 Cl 0.26526(13) 0.30368(10) 0.45834(5) 0.0474(3) Uani 1 1 d D . . O4A O 0.2699(10) 0.3028(8) 0.3985(3) 0.078(4) Uani 0.60 1 d PD B 1 O4B O 0.3323(9) 0.2300(6) 0.4827(3) 0.076(2) Uani 0.60 1 d PD B 1 O4C O 0.3285(10) 0.3980(5) 0.4860(3) 0.083(3) Uani 0.60 1 d PD B 1 O4D O 0.1533(6) 0.2878(9) 0.4684(4) 0.107(3) Uani 0.60 1 d PD B 1 O4E O 0.2065(13) 0.3188(12) 0.4011(5) 0.070(5) Uani 0.40 1 d PD B 2 O4F O 0.3844(8) 0.3138(16) 0.4638(6) 0.138(7) Uani 0.40 1 d PD B 2 O4G O 0.2276(19) 0.3724(10) 0.4970(5) 0.110(6) Uani 0.40 1 d PD B 2 O4H O 0.2137(13) 0.2052(7) 0.4711(4) 0.071(3) Uani 0.40 1 d PD B 2 C200 C 0.4521(5) 0.6497(5) 0.9485(2) 0.0652(17) Uani 1 1 d . . . H20A H 0.4132 0.6023 0.9172 0.098 Uiso 1 1 calc R . . H20B H 0.5343 0.6682 0.9455 0.098 Uiso 1 1 calc R . . H20C H 0.4130 0.7075 0.9473 0.098 Uiso 1 1 calc R . . N201 N 0.4459(7) 0.6075(5) 1.0004(2) 0.0860(19) Uani 1 1 d . . . O202 O 0.3750(4) 0.5191(4) 0.9965(2) 0.0970(16) Uani 1 1 d . . . O203 O 0.4920(4) 0.6525(3) 1.04669(18) 0.0738(13) Uani 1 1 d . . . C204 C 0.6322(8) 0.4074(6) 0.4222(3) 0.115(3) Uani 1 1 d . . . H20D H 0.6707 0.3508 0.4316 0.173 Uiso 1 1 calc R . . H20E H 0.5549 0.3989 0.4330 0.173 Uiso 1 1 calc R . . H20F H 0.6800 0.4662 0.4426 0.173 Uiso 1 1 calc R . . N205 N 0.6188(5) 0.4169(3) 0.3617(2) 0.0582(14) Uani 1 1 d . . . O206 O 0.7066(4) 0.4373(4) 0.3411(2) 0.1062(18) Uani 1 1 d . . . O207 O 0.5211(5) 0.4060(4) 0.3323(2) 0.0995(16) Uani 1 1 d . . . C208 C 0.7479(6) 0.2559(5) 0.2454(3) 0.075(2) Uani 1 1 d . . . H20G H 0.8307 0.2691 0.2632 0.112 Uiso 1 1 calc R . . H20H H 0.7358 0.2013 0.2166 0.112 Uiso 1 1 calc R . . H20I H 0.7000 0.2393 0.2738 0.112 Uiso 1 1 calc R . . N209 N 0.7136(4) 0.3431(4) 0.2190(2) 0.0512(12) Uani 1 1 d . . . O210 O 0.7876(4) 0.4162(3) 0.22033(19) 0.0810(14) Uani 1 1 d . . . O211 O 0.6093(4) 0.3409(3) 0.19684(18) 0.0674(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03130(19) 0.0305(2) 0.02361(19) 0.00129(14) 0.00463(15) 0.00065(14) Cd2 0.02965(18) 0.02380(19) 0.0291(2) 0.00262(14) 0.00397(15) 0.00333(14) N11 0.040(2) 0.049(3) 0.033(2) 0.008(2) 0.015(2) -0.001(2) C12 0.049(3) 0.046(4) 0.050(3) 0.006(3) 0.018(3) -0.007(3) C13 0.062(4) 0.054(4) 0.072(4) 0.016(3) 0.036(4) 0.001(3) C14 0.087(5) 0.067(5) 0.059(4) 0.034(4) 0.035(4) 0.025(4) C15 0.064(4) 0.072(5) 0.048(4) 0.022(3) 0.024(3) 0.014(3) C16 0.033(3) 0.053(3) 0.034(3) 0.012(3) 0.014(2) 0.007(2) N21 0.030(2) 0.045(3) 0.025(2) 0.0017(19) 0.0057(17) 0.0078(18) C22 0.028(2) 0.058(4) 0.028(3) 0.006(2) 0.008(2) 0.005(2) C23 0.035(3) 0.070(4) 0.026(3) 0.002(3) 0.007(2) 0.000(3) S24 0.0496(8) 0.0612(10) 0.0307(7) -0.0083(6) 0.0102(6) 0.0055(7) C25 0.030(2) 0.046(3) 0.025(3) -0.006(2) 0.002(2) 0.006(2) N31 0.028(2) 0.034(2) 0.030(2) 0.0004(18) 0.0048(17) 0.0032(17) C32 0.027(2) 0.037(3) 0.034(3) 0.001(2) 0.003(2) 0.004(2) C33 0.047(3) 0.045(3) 0.039(3) -0.010(3) 0.005(3) 0.013(3) C34 0.054(3) 0.034(3) 0.056(4) -0.006(3) 0.004(3) 0.002(3) C35 0.043(3) 0.035(3) 0.041(3) 0.006(2) 0.004(2) 0.003(2) C36 0.025(2) 0.032(3) 0.035(3) 0.008(2) 0.004(2) 0.0068(19) N41 0.0251(19) 0.029(2) 0.029(2) 0.0110(17) 0.0048(17) 0.0028(16) O41 0.0327(17) 0.0328(18) 0.0278(17) 0.0107(14) 0.0025(14) 0.0037(14) C42 0.026(2) 0.028(3) 0.032(3) 0.008(2) 0.006(2) -0.0004(19) C43 0.037(3) 0.036(3) 0.038(3) 0.009(2) 0.007(2) 0.010(2) C44 0.046(3) 0.045(3) 0.029(3) 0.017(2) 0.005(2) 0.010(2) C45 0.041(3) 0.038(3) 0.031(3) 0.009(2) 0.009(2) 0.007(2) C46 0.025(2) 0.037(3) 0.029(3) 0.005(2) 0.005(2) 0.000(2) N51 0.033(2) 0.028(2) 0.030(2) 0.0036(17) 0.0052(18) -0.0006(17) C52 0.033(2) 0.030(3) 0.023(2) 0.006(2) 0.005(2) 0.003(2) C53 0.030(2) 0.046(3) 0.036(3) 0.000(2) -0.002(2) 0.003(2) C54 0.054(3) 0.036(3) 0.035(3) -0.010(2) 0.004(3) 0.004(2) C55 0.044(3) 0.033(3) 0.042(3) -0.002(2) 0.006(3) 0.007(2) C56 0.040(3) 0.029(3) 0.032(3) 0.005(2) 0.010(2) 0.005(2) N61 0.032(2) 0.028(2) 0.033(2) 0.0062(18) 0.0066(18) 0.0082(17) C62 0.039(3) 0.024(3) 0.030(3) 0.002(2) 0.008(2) 0.005(2) S63 0.0499(8) 0.0367(8) 0.0454(8) -0.0043(6) 0.0037(6) 0.0165(6) C64 0.047(3) 0.041(3) 0.041(3) 0.003(2) 0.004(3) 0.018(2) C65 0.033(3) 0.034(3) 0.033(3) 0.007(2) 0.010(2) 0.001(2) N71 0.026(2) 0.038(2) 0.034(2) 0.0010(19) 0.0020(18) 0.0042(17) C72 0.029(2) 0.034(3) 0.034(3) 0.005(2) 0.008(2) 0.006(2) C73 0.034(3) 0.043(3) 0.038(3) 0.003(2) 0.005(2) 0.008(2) C74 0.036(3) 0.063(4) 0.041(3) 0.007(3) 0.001(3) 0.009(3) C75 0.029(3) 0.051(4) 0.042(3) -0.008(3) -0.002(2) -0.003(2) C76 0.035(3) 0.034(3) 0.046(3) -0.008(2) 0.009(2) 0.002(2) N81 0.035(2) 0.044(3) 0.037(3) 0.004(2) 0.006(2) -0.0064(19) C82 0.034(3) 0.048(3) 0.044(3) -0.006(3) 0.008(2) -0.006(2) C83 0.033(3) 0.045(3) 0.071(4) 0.003(3) 0.011(3) -0.004(2) C84 0.035(3) 0.064(4) 0.058(4) 0.020(3) 0.004(3) 0.005(3) C85 0.037(3) 0.056(4) 0.040(3) 0.007(3) -0.002(2) -0.001(3) C86 0.026(2) 0.048(3) 0.031(3) 0.002(2) 0.000(2) -0.009(2) N91 0.035(2) 0.040(3) 0.033(2) -0.0006(19) 0.0102(19) -0.0097(19) C92 0.036(3) 0.047(3) 0.030(3) 0.004(2) 0.003(2) -0.010(2) C93 0.048(3) 0.060(4) 0.037(3) 0.001(3) -0.002(3) -0.007(3) S94 0.0578(9) 0.0555(10) 0.0405(8) -0.0133(7) 0.0022(7) -0.0117(7) C95 0.037(3) 0.040(3) 0.026(3) -0.005(2) 0.008(2) -0.011(2) N101 0.039(2) 0.034(2) 0.032(2) 0.0006(19) 0.0097(19) -0.0004(19) C102 0.044(3) 0.035(3) 0.039(3) -0.001(2) 0.017(3) -0.008(2) C103 0.065(4) 0.033(3) 0.044(3) -0.003(3) 0.015(3) -0.005(3) C104 0.085(4) 0.029(3) 0.055(4) 0.002(3) 0.036(4) 0.006(3) C105 0.057(3) 0.038(3) 0.053(4) 0.007(3) 0.019(3) 0.006(3) C106 0.049(3) 0.023(3) 0.041(3) 0.007(2) 0.022(3) 0.001(2) N111 0.032(2) 0.038(2) 0.026(2) 0.0096(19) 0.0080(18) 0.0060(18) O111 0.0349(17) 0.0337(19) 0.0291(18) 0.0072(15) 0.0031(15) 0.0058(14) C112 0.042(3) 0.029(3) 0.034(3) 0.010(2) 0.015(2) 0.007(2) C113 0.063(4) 0.040(3) 0.048(3) 0.014(3) 0.017(3) 0.015(3) C114 0.059(4) 0.055(4) 0.048(4) 0.028(3) 0.008(3) 0.024(3) C115 0.044(3) 0.063(4) 0.032(3) 0.007(3) 0.001(2) 0.010(3) C116 0.032(3) 0.042(3) 0.027(3) 0.005(2) 0.007(2) 0.003(2) N121 0.028(2) 0.036(2) 0.031(2) 0.0000(18) 0.0056(17) 0.0019(17) C122 0.028(2) 0.042(3) 0.033(3) -0.004(2) 0.002(2) 0.004(2) C123 0.032(3) 0.064(4) 0.033(3) 0.001(3) -0.001(2) 0.010(3) C124 0.041(3) 0.062(4) 0.037(3) -0.014(3) -0.002(3) 0.013(3) C125 0.040(3) 0.047(3) 0.045(3) -0.011(3) 0.002(3) 0.007(2) C126 0.027(2) 0.039(3) 0.036(3) -0.010(2) 0.001(2) 0.006(2) N131 0.028(2) 0.025(2) 0.035(2) 0.0003(18) 0.0059(18) 0.0002(16) C132 0.030(2) 0.027(3) 0.045(3) -0.001(2) 0.006(2) 0.000(2) S133 0.0600(9) 0.0265(7) 0.0680(10) -0.0064(7) 0.0151(8) -0.0011(6) C134 0.053(3) 0.031(3) 0.068(4) 0.015(3) 0.022(3) 0.003(2) C135 0.029(2) 0.025(3) 0.052(3) 0.012(2) 0.012(2) 0.002(2) N141 0.030(2) 0.033(2) 0.035(2) 0.0057(18) 0.0066(18) 0.0036(17) C142 0.020(2) 0.034(3) 0.049(3) 0.009(2) 0.008(2) 0.003(2) C143 0.054(3) 0.048(3) 0.058(4) 0.024(3) 0.018(3) 0.015(3) C144 0.057(4) 0.069(4) 0.043(3) 0.024(3) 0.018(3) 0.015(3) C145 0.050(3) 0.060(4) 0.038(3) 0.007(3) 0.013(3) 0.009(3) C146 0.035(3) 0.034(3) 0.041(3) 0.005(2) 0.013(2) -0.001(2) Cl1 0.0437(7) 0.0349(7) 0.0548(9) 0.0044(6) -0.0013(7) 0.0056(6) O1A 0.091(3) 0.044(3) 0.134(4) -0.014(3) -0.060(3) 0.028(2) O1B 0.097(3) 0.095(4) 0.047(3) -0.015(2) 0.005(2) 0.021(3) O1C 0.050(2) 0.064(3) 0.040(2) -0.0041(18) -0.0054(18) 0.0138(19) O1D 0.077(3) 0.075(3) 0.156(5) 0.032(3) 0.040(3) -0.017(3) Cl2 0.0606(9) 0.0544(9) 0.0431(9) 0.0108(7) -0.0046(7) -0.0003(7) O2A 0.120(4) 0.080(4) 0.127(5) -0.006(3) 0.022(4) -0.045(3) O2B 0.167(10) 0.090(7) 0.109(8) -0.009(6) 0.100(8) 0.022(7) O2C 0.110(7) 0.063(5) 0.035(4) 0.001(3) 0.021(5) -0.020(5) O2D 0.057(5) 0.152(10) 0.167(11) 0.052(9) 0.008(6) 0.032(6) O2E 0.153(14) 0.086(10) 0.096(11) 0.008(8) -0.051(10) 0.048(10) O2F 0.089(9) 0.088(10) 0.039(7) 0.020(6) -0.002(7) 0.005(8) O2G 0.088(12) 0.37(3) 0.059(10) 0.049(15) 0.017(9) -0.001(15) Cl3 0.0513(8) 0.0463(8) 0.0569(9) 0.0063(7) 0.0109(7) 0.0183(6) O3A 0.062(3) 0.076(3) 0.057(3) -0.020(2) -0.004(2) 0.018(2) O3B 0.075(3) 0.073(3) 0.069(3) -0.022(2) -0.016(2) 0.041(2) O3C 0.102(4) 0.064(3) 0.127(4) 0.052(3) 0.039(3) 0.018(3) O3D 0.055(2) 0.085(3) 0.082(3) 0.031(2) 0.019(2) 0.018(2) Cl4 0.0633(9) 0.0363(8) 0.0398(8) 0.0027(6) 0.0005(7) 0.0086(7) O4A 0.146(11) 0.050(6) 0.032(5) 0.005(4) 0.007(6) 0.010(7) O4B 0.124(7) 0.054(5) 0.053(5) -0.005(4) -0.003(5) 0.051(5) O4C 0.141(9) 0.039(5) 0.055(5) -0.010(4) 0.004(5) -0.007(5) O4D 0.066(6) 0.157(10) 0.107(8) 0.064(7) 0.028(5) 0.007(6) O4E 0.111(13) 0.040(8) 0.043(8) 0.008(6) -0.030(8) 0.009(8) O4F 0.040(7) 0.23(2) 0.130(14) 0.058(15) -0.017(8) -0.014(10) O4G 0.23(2) 0.048(9) 0.062(9) -0.004(7) 0.012(12) 0.070(11) O4H 0.126(11) 0.045(7) 0.032(6) 0.012(5) 0.001(7) -0.004(7) C200 0.071(4) 0.079(5) 0.055(4) 0.022(3) 0.020(3) 0.025(3) N201 0.145(6) 0.073(4) 0.043(4) -0.009(3) 0.006(4) 0.049(4) O202 0.070(3) 0.115(5) 0.098(4) -0.021(3) 0.018(3) -0.006(3) O203 0.095(3) 0.078(3) 0.046(3) -0.019(2) 0.011(2) 0.020(3) C204 0.169(9) 0.138(8) 0.053(5) -0.005(5) 0.020(5) 0.079(7) N205 0.048(3) 0.040(3) 0.091(4) 0.003(3) 0.026(3) 0.007(2) O206 0.086(4) 0.103(4) 0.157(5) 0.056(4) 0.065(4) 0.037(3) O207 0.084(4) 0.090(4) 0.116(4) 0.012(3) -0.002(3) 0.005(3) C208 0.090(5) 0.080(5) 0.073(4) 0.031(4) 0.033(4) 0.046(4) N209 0.052(3) 0.053(3) 0.051(3) 0.003(2) 0.020(3) 0.005(3) O210 0.071(3) 0.079(3) 0.091(3) 0.004(3) 0.035(3) -0.017(3) O211 0.063(3) 0.055(3) 0.081(3) 0.002(2) 0.003(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 Cd1 N91 2.299(4) . ? Cd1 N21 2.315(4) . ? Cd1 O111 2.373(3) . ? Cd1 O41 2.377(3) . ? Cd1 N11 2.558(4) . ? Cd1 N81 2.593(4) . ? Cd2 N61 2.326(3) . ? Cd2 N131 2.331(4) . ? Cd2 O41 2.388(3) . ? Cd2 O111 2.395(3) . ? Cd2 N141 2.478(4) . ? Cd2 N71 2.580(4) . ? N11 C12 1.339(6) . ? N11 C16 1.353(6) . ? C12 C13 1.382(7) . ? C12 H12 0.9300 . ? C13 C14 1.390(8) . ? C13 H13 0.9300 . ? C14 C15 1.368(8) . ? C14 H14 0.9300 . ? C15 C16 1.391(7) . ? C15 H15 0.9300 . ? C16 C22 1.466(7) . ? N21 C25 1.312(6) . ? N21 C22 1.376(6) . ? C22 C23 1.375(6) . ? C23 S24 1.697(5) . ? C23 H23 0.9300 . ? S24 C25 1.735(4) . ? C25 C32 1.461(6) . ? N31 C36 1.347(5) . ? N31 C32 1.349(5) . ? C32 C33 1.395(6) . ? C33 C34 1.382(7) . ? C33 H33 0.9300 . ? C34 C35 1.401(7) . ? C34 H34 0.9300 . ? C35 C36 1.387(6) . ? C35 H35 0.9300 . ? C36 C42 1.491(6) . ? N41 O41 1.331(4) . ? N41 C42 1.371(5) . ? N41 C46 1.382(5) . ? C42 C43 1.379(6) . ? C43 C44 1.372(6) . ? C43 H43 0.9300 . ? C44 C45 1.376(6) . ? C44 H44 0.9300 . ? C45 C46 1.384(6) . ? C45 H45 0.9300 . ? C46 C52 1.484(6) . ? N51 C56 1.341(5) . ? N51 C52 1.342(5) . ? C52 C53 1.408(6) . ? C53 C54 1.361(6) . ? C53 H53 0.9300 . ? C54 C55 1.377(7) . ? C54 H54 0.9300 . ? C55 C56 1.399(6) . ? C55 H55 0.9300 . ? C56 C62 1.465(6) . ? N61 C62 1.323(5) . ? N61 C65 1.373(6) . ? C62 S63 1.717(4) . ? S63 C64 1.693(5) . ? C64 C65 1.373(6) . ? C64 H64 0.9300 . ? C65 C72 1.457(6) . ? N71 C72 1.344(6) . ? N71 C76 1.348(6) . ? C72 C73 1.400(6) . ? C73 C74 1.385(7) . ? C73 H73 0.9300 . ? C74 C75 1.368(7) . ? C74 H74 0.9300 . ? C75 C76 1.383(7) . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? N81 C82 1.348(6) . ? N81 C86 1.353(6) . ? C82 C83 1.388(7) . ? C82 H82 0.9300 . ? C83 C84 1.391(7) . ? C83 H83 0.9300 . ? C84 C85 1.368(7) . ? C84 H84 0.9300 . ? C85 C86 1.408(7) . ? C85 H85 0.9300 . ? C86 C92 1.457(7) . ? N91 C95 1.309(6) . ? N91 C92 1.391(6) . ? C92 C93 1.366(7) . ? C93 S94 1.710(6) . ? C93 H93 0.9300 . ? S94 C95 1.719(5) . ? C95 C102 1.475(7) . ? N101 C106 1.342(6) . ? N101 C102 1.347(6) . ? C102 C103 1.380(7) . ? C103 C104 1.379(7) . ? C103 H103 0.9300 . ? C104 C105 1.392(7) . ? C104 H104 0.9300 . ? C105 C106 1.402(6) . ? C105 H105 0.9300 . ? C106 C112 1.489(7) . ? N111 O111 1.325(4) . ? N111 C112 1.376(6) . ? N111 C116 1.381(6) . ? C112 C113 1.374(7) . ? C113 C114 1.378(7) . ? C113 H113 0.9300 . ? C114 C115 1.381(7) . ? C114 H114 0.9300 . ? C115 C116 1.382(6) . ? C115 H115 0.9300 . ? C116 C122 1.488(6) . ? N121 C126 1.336(6) . ? N121 C122 1.343(6) . ? C122 C123 1.404(6) . ? C123 C124 1.377(7) . ? C123 H123 0.9300 . ? C124 C125 1.375(7) . ? C124 H124 0.9300 . ? C125 C126 1.407(6) . ? C125 H125 0.9300 . ? C126 C132 1.461(6) . ? N131 C132 1.318(5) . ? N131 C135 1.357(5) . ? C132 S133 1.727(5) . ? S133 C134 1.697(5) . ? C134 C135 1.370(6) . ? C134 H134 0.9300 . ? C135 C142 1.479(6) . ? N141 C146 1.344(5) . ? N141 C142 1.349(5) . ? C142 C143 1.399(6) . ? C143 C144 1.360(7) . ? C143 H143 0.9300 . ? C144 C145 1.392(7) . ? C144 H144 0.9300 . ? C145 C146 1.377(6) . ? C145 H145 0.9300 . ? C146 H146 0.9300 . ? Cl1 O1D 1.397(4) . ? Cl1 O1A 1.415(4) . ? Cl1 O1B 1.433(4) . ? Cl1 O1C 1.439(4) . ? Cl2 O2A 1.392(4) . ? Cl2 O2F 1.409(8) . ? Cl2 O2G 1.400(10) . ? Cl2 O2D 1.413(7) . ? Cl2 O2C 1.417(6) . ? Cl2 O2B 1.437(6) . ? Cl2 O2E 1.460(9) . ? Cl3 O3B 1.419(4) . ? Cl3 O3C 1.425(4) . ? Cl3 O3D 1.439(4) . ? Cl3 O3A 1.444(4) . ? Cl4 O4F 1.339(9) . ? Cl4 O4D 1.340(7) . ? Cl4 O4A 1.432(8) . ? Cl4 O4B 1.436(6) . ? Cl4 O4G 1.436(9) . ? Cl4 O4C 1.447(7) . ? Cl4 O4E 1.450(10) . ? Cl4 O4H 1.462(8) . ? C200 N201 1.398(7) . ? C200 H20A 0.9600 . ? C200 H20B 0.9600 . ? C200 H20C 0.9600 . ? N201 O203 1.224(6) . ? N201 O202 1.348(7) . ? C204 N205 1.436(8) . ? C204 H20D 0.9600 . ? C204 H20E 0.9600 . ? C204 H20F 0.9600 . ? N205 O207 1.199(6) . ? N205 O206 1.202(5) . ? C208 N209 1.447(7) . ? C208 H20G 0.9600 . ? C208 H20H 0.9600 . ? C208 H20I 0.9600 . ? N209 O210 1.213(5) . ? N209 O211 1.218(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 N91 Cd1 N21 153.11(12) . . ? N91 Cd1 O111 116.40(12) . . ? N21 Cd1 O111 88.43(11) . . ? N91 Cd1 O41 87.43(11) . . ? N21 Cd1 O41 114.70(12) . . ? O111 Cd1 O41 62.63(10) . . ? N91 Cd1 N11 99.59(13) . . ? N21 Cd1 N11 67.93(13) . . ? O111 Cd1 N11 91.28(11) . . ? O41 Cd1 N11 153.09(11) . . ? N91 Cd1 N81 67.44(13) . . ? N21 Cd1 N81 93.29(12) . . ? O111 Cd1 N81 159.03(11) . . ? O41 Cd1 N81 97.98(11) . . ? N11 Cd1 N81 108.73(12) . . ? N61 Cd2 N131 153.21(12) . . ? N61 Cd2 O41 117.11(11) . . ? N131 Cd2 O41 87.61(11) . . ? N61 Cd2 O111 88.09(11) . . ? N131 Cd2 O111 114.15(11) . . ? O41 Cd2 O111 62.15(10) . . ? N61 Cd2 N141 98.55(12) . . ? N131 Cd2 N141 68.38(12) . . ? O41 Cd2 N141 92.64(10) . . ? O111 Cd2 N141 153.86(11) . . ? N61 Cd2 N71 66.78(13) . . ? N131 Cd2 N71 95.16(12) . . ? O41 Cd2 N71 155.98(10) . . ? O111 Cd2 N71 95.29(11) . . ? N141 Cd2 N71 110.59(11) . . ? C12 N11 C16 117.7(4) . . ? C12 N11 Cd1 125.5(3) . . ? C16 N11 Cd1 112.7(3) . . ? N11 C12 C13 123.7(5) . . ? N11 C12 H12 118.2 . . ? C13 C12 H12 118.2 . . ? C12 C13 C14 117.4(6) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C15 C14 C13 120.2(6) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 118.6(6) . . ? C14 C15 H15 120.7 . . ? C16 C15 H15 120.7 . . ? N11 C16 C15 122.2(5) . . ? N11 C16 C22 115.4(4) . . ? C15 C16 C22 122.4(5) . . ? C25 N21 C22 113.1(4) . . ? C25 N21 Cd1 126.2(3) . . ? C22 N21 Cd1 120.6(3) . . ? C23 C22 N21 112.9(5) . . ? C23 C22 C16 128.8(5) . . ? N21 C22 C16 118.3(4) . . ? C22 C23 S24 111.4(4) . . ? C22 C23 H23 124.3 . . ? S24 C23 H23 124.3 . . ? C23 S24 C25 89.9(2) . . ? N21 C25 C32 122.1(4) . . ? N21 C25 S24 112.8(4) . . ? C32 C25 S24 125.1(4) . . ? C36 N31 C32 118.4(4) . . ? N31 C32 C33 123.2(4) . . ? N31 C32 C25 112.9(4) . . ? C33 C32 C25 123.9(4) . . ? C34 C33 C32 118.1(5) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C33 C34 C35 118.9(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C36 C35 C34 119.6(5) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? N31 C36 C35 121.7(4) . . ? N31 C36 C42 118.4(4) . . ? C35 C36 C42 119.7(4) . . ? O41 N41 C42 119.0(3) . . ? O41 N41 C46 119.1(3) . . ? C42 N41 C46 121.9(4) . . ? N41 O41 Cd1 119.6(2) . . ? N41 O41 Cd2 122.8(2) . . ? Cd1 O41 Cd2 117.56(12) . . ? N41 C42 C43 118.6(4) . . ? N41 C42 C36 120.9(4) . . ? C43 C42 C36 120.4(4) . . ? C44 C43 C42 120.6(4) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 120.3(4) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C46 120.1(4) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? N41 C46 C45 118.5(4) . . ? N41 C46 C52 120.4(4) . . ? C45 C46 C52 121.0(4) . . ? C56 N51 C52 117.9(4) . . ? N51 C52 C53 121.5(4) . . ? N51 C52 C46 119.5(4) . . ? C53 C52 C46 119.0(4) . . ? C54 C53 C52 119.3(4) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C53 C54 C55 120.3(5) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C54 C55 C56 117.3(4) . . ? C54 C55 H55 121.3 . . ? C56 C55 H55 121.3 . . ? N51 C56 C55 123.6(4) . . ? N51 C56 C62 114.3(4) . . ? C55 C56 C62 122.1(4) . . ? C62 N61 C65 112.2(4) . . ? C62 N61 Cd2 125.5(3) . . ? C65 N61 Cd2 122.3(3) . . ? N61 C62 C56 122.3(4) . . ? N61 C62 S63 113.4(3) . . ? C56 C62 S63 124.3(3) . . ? C64 S63 C62 89.9(2) . . ? C65 C64 S63 111.6(4) . . ? C65 C64 H64 124.2 . . ? S63 C64 H64 124.2 . . ? C64 C65 N61 112.9(4) . . ? C64 C65 C72 128.9(4) . . ? N61 C65 C72 118.2(4) . . ? C72 N71 C76 117.1(4) . . ? C72 N71 Cd2 114.9(3) . . ? C76 N71 Cd2 126.2(3) . . ? N71 C72 C73 122.5(4) . . ? N71 C72 C65 116.1(4) . . ? C73 C72 C65 121.4(4) . . ? C74 C73 C72 118.8(5) . . ? C74 C73 H73 120.6 . . ? C72 C73 H73 120.6 . . ? C75 C74 C73 119.0(5) . . ? C75 C74 H74 120.5 . . ? C73 C74 H74 120.5 . . ? C74 C75 C76 119.1(5) . . ? C74 C75 H75 120.5 . . ? C76 C75 H75 120.5 . . ? N71 C76 C75 123.4(5) . . ? N71 C76 H76 118.3 . . ? C75 C76 H76 118.3 . . ? C82 N81 C86 117.4(4) . . ? C82 N81 Cd1 125.3(3) . . ? C86 N81 Cd1 111.3(3) . . ? N81 C82 C83 123.2(5) . . ? N81 C82 H82 118.4 . . ? C83 C82 H82 118.4 . . ? C82 C83 C84 118.7(5) . . ? C82 C83 H83 120.6 . . ? C84 C83 H83 120.6 . . ? C85 C84 C83 119.2(5) . . ? C85 C84 H84 120.4 . . ? C83 C84 H84 120.4 . . ? C84 C85 C86 119.1(5) . . ? C84 C85 H85 120.5 . . ? C86 C85 H85 120.5 . . ? N81 C86 C85 122.3(5) . . ? N81 C86 C92 115.1(4) . . ? C85 C86 C92 122.5(5) . . ? C95 N91 C92 111.7(4) . . ? C95 N91 Cd1 127.6(3) . . ? C92 N91 Cd1 120.7(3) . . ? C93 C92 N91 113.5(5) . . ? C93 C92 C86 128.0(5) . . ? N91 C92 C86 118.4(4) . . ? C92 C93 S94 110.8(4) . . ? C92 C93 H93 124.6 . . ? S94 C93 H93 124.6 . . ? C93 S94 C95 89.9(3) . . ? N91 C95 C102 121.4(4) . . ? N91 C95 S94 114.1(4) . . ? C102 C95 S94 124.4(4) . . ? C106 N101 C102 119.8(4) . . ? N101 C102 C103 122.2(5) . . ? N101 C102 C95 114.0(4) . . ? C103 C102 C95 123.8(5) . . ? C104 C103 C102 118.6(5) . . ? C104 C103 H103 120.7 . . ? C102 C103 H103 120.7 . . ? C103 C104 C105 119.9(5) . . ? C103 C104 H104 120.1 . . ? C105 C104 H104 120.1 . . ? C104 C105 C106 118.5(5) . . ? C104 C105 H105 120.7 . . ? C106 C105 H105 120.7 . . ? N101 C106 C105 121.0(5) . . ? N101 C106 C112 120.3(4) . . ? C105 C106 C112 118.6(5) . . ? O111 N111 C112 119.7(4) . . ? O111 N111 C116 118.2(4) . . ? C112 N111 C116 122.1(4) . . ? N111 O111 Cd1 122.2(2) . . ? N111 O111 Cd2 120.3(2) . . ? Cd1 O111 Cd2 117.44(12) . . ? C113 C112 N111 118.2(5) . . ? C113 C112 C106 122.5(4) . . ? N111 C112 C106 119.4(4) . . ? C114 C113 C112 121.4(5) . . ? C114 C113 H113 119.3 . . ? C112 C113 H113 119.3 . . ? C113 C114 C115 119.1(5) . . ? C113 C114 H114 120.4 . . ? C115 C114 H114 120.4 . . ? C114 C115 C116 120.8(5) . . ? C114 C115 H115 119.6 . . ? C116 C115 H115 119.6 . . ? N111 C116 C115 118.3(4) . . ? N111 C116 C122 119.7(4) . . ? C115 C116 C122 122.0(5) . . ? C126 N121 C122 119.0(4) . . ? N121 C122 C123 121.1(5) . . ? N121 C122 C116 119.4(4) . . ? C123 C122 C116 119.5(4) . . ? C124 C123 C122 119.0(5) . . ? C124 C123 H123 120.5 . . ? C122 C123 H123 120.5 . . ? C125 C124 C123 120.7(5) . . ? C125 C124 H124 119.6 . . ? C123 C124 H124 119.6 . . ? C124 C125 C126 116.8(5) . . ? C124 C125 H125 121.6 . . ? C126 C125 H125 121.6 . . ? N121 C126 C125 123.4(5) . . ? N121 C126 C132 113.7(4) . . ? C125 C126 C132 122.9(5) . . ? C132 N131 C135 112.7(4) . . ? C132 N131 Cd2 127.0(3) . . ? C135 N131 Cd2 120.3(3) . . ? N131 C132 C126 121.4(4) . . ? N131 C132 S133 112.6(4) . . ? C126 C132 S133 126.0(3) . . ? C134 S133 C132 90.1(2) . . ? C135 C134 S133 110.6(4) . . ? C135 C134 H134 124.7 . . ? S133 C134 H134 124.7 . . ? N131 C135 C134 114.1(4) . . ? N131 C135 C142 117.8(4) . . ? C134 C135 C142 128.2(4) . . ? C146 N141 C142 118.1(4) . . ? C146 N141 Cd2 124.5(3) . . ? C142 N141 Cd2 115.9(3) . . ? N141 C142 C143 121.5(4) . . ? N141 C142 C135 115.8(4) . . ? C143 C142 C135 122.7(4) . . ? C144 C143 C142 119.3(5) . . ? C144 C143 H143 120.4 . . ? C142 C143 H143 120.4 . . ? C143 C144 C145 119.6(5) . . ? C143 C144 H144 120.2 . . ? C145 C144 H144 120.2 . . ? C146 C145 C144 118.2(5) . . ? C146 C145 H145 120.9 . . ? C144 C145 H145 120.9 . . ? N141 C146 C145 123.1(5) . . ? N141 C146 H146 118.4 . . ? C145 C146 H146 118.4 . . ? O1D Cl1 O1A 111.2(3) . . ? O1D Cl1 O1B 108.0(3) . . ? O1A Cl1 O1B 109.4(3) . . ? O1D Cl1 O1C 109.5(3) . . ? O1A Cl1 O1C 109.8(2) . . ? O1B Cl1 O1C 109.0(2) . . ? O2A Cl2 O2F 123.2(5) . . ? O2A Cl2 O2G 107.3(8) . . ? O2F Cl2 O2G 105.4(7) . . ? O2A Cl2 O2D 104.1(5) . . ? O2F Cl2 O2D 60.5(6) . . ? O2G Cl2 O2D 56.2(7) . . ? O2A Cl2 O2C 117.8(4) . . ? O2F Cl2 O2C 118.9(5) . . ? O2G Cl2 O2C 57.5(8) . . ? O2D Cl2 O2C 108.6(5) . . ? O2A Cl2 O2B 107.3(4) . . ? O2F Cl2 O2B 47.4(6) . . ? O2G Cl2 O2B 144.6(8) . . ? O2D Cl2 O2B 107.5(6) . . ? O2C Cl2 O2B 110.9(5) . . ? O2A Cl2 O2E 99.5(6) . . ? O2F Cl2 O2E 109.8(7) . . ? O2G Cl2 O2E 111.7(9) . . ? O2D Cl2 O2E 155.9(7) . . ? O2C Cl2 O2E 54.4(6) . . ? O2B Cl2 O2E 69.5(7) . . ? O3B Cl3 O3C 109.9(3) . . ? O3B Cl3 O3D 108.8(3) . . ? O3C Cl3 O3D 109.2(3) . . ? O3B Cl3 O3A 109.8(2) . . ? O3C Cl3 O3A 109.5(3) . . ? O3D Cl3 O3A 109.7(2) . . ? O4F Cl4 O4D 163.7(7) . . ? O4F Cl4 O4A 83.0(8) . . ? O4D Cl4 O4A 112.8(6) . . ? O4F Cl4 O4B 58.2(7) . . ? O4D Cl4 O4B 110.4(5) . . ? O4A Cl4 O4B 108.7(5) . . ? O4F Cl4 O4G 112.4(9) . . ? O4D Cl4 O4G 60.4(8) . . ? O4A Cl4 O4G 132.4(6) . . ? O4B Cl4 O4G 117.8(6) . . ? O4F Cl4 O4C 65.2(8) . . ? O4D Cl4 O4C 111.1(6) . . ? O4A Cl4 O4C 108.1(6) . . ? O4B Cl4 O4C 105.5(5) . . ? O4G Cl4 O4C 50.9(7) . . ? O4F Cl4 O4E 112.8(8) . . ? O4D Cl4 O4E 83.5(7) . . ? O4A Cl4 O4E 32.2(6) . . ? O4B Cl4 O4E 134.8(6) . . ? O4G Cl4 O4E 106.7(7) . . ? O4C Cl4 O4E 108.9(8) . . ? O4F Cl4 O4H 112.3(8) . . ? O4D Cl4 O4H 59.9(6) . . ? O4A Cl4 O4H 109.4(6) . . ? O4B Cl4 O4H 54.8(5) . . ? O4G Cl4 O4H 105.4(8) . . ? O4C Cl4 O4H 141.8(5) . . ? O4E Cl4 O4H 106.7(8) . . ? N201 C200 H20A 109.5 . . ? N201 C200 H20B 109.5 . . ? H20A C200 H20B 109.5 . . ? N201 C200 H20C 109.5 . . ? H20A C200 H20C 109.5 . . ? H20B C200 H20C 109.5 . . ? O203 N201 O202 122.0(6) . . ? O203 N201 C200 121.9(7) . . ? O202 N201 C200 115.6(6) . . ? N205 C204 H20D 109.5 . . ? N205 C204 H20E 109.5 . . ? H20D C204 H20E 109.5 . . ? N205 C204 H20F 109.5 . . ? H20D C204 H20F 109.5 . . ? H20E C204 H20F 109.5 . . ? O207 N205 O206 120.7(6) . . ? O207 N205 C204 120.3(6) . . ? O206 N205 C204 119.1(7) . . ? N209 C208 H20G 109.5 . . ? N209 C208 H20H 109.5 . . ? H20G C208 H20H 109.5 . . ? N209 C208 H20I 109.5 . . ? H20G C208 H20I 109.5 . . ? H20H C208 H20I 109.5 . . ? O210 N209 O211 122.1(5) . . ? O210 N209 C208 119.8(6) . . ? O211 N209 C208 118.1(5) . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.62 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 1.902 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.094