# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_Chris_LOMeZn_DPA_0m _audit_creation_date 2013-07-12 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _chemical_formula_moiety 'C92 H64 N12 O2 S4 Zn2, 4(C F3 O3 S)(C H3 N O2) (C H3 C O2 C H2 C H3)' _chemical_formula_sum 'C101 H75 F12 N13 O18 S8 Zn2' _chemical_formula_weight 1926.81 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_dispersion_source C 0.00347 0.00161 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' F 0.01794 0.01033 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' H 0.00000 0.00000 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' Zn 0.31207 1.46666 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' O 0.01158 0.00611 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' N 0.00653 0.00323 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' S 0.12424 0.12443 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,-z+1/2 3 -x,-y,-z 4 x,-y,z-1/2 5 x+1/2,y+1/2,z 6 -x+1/2,y+1/2,-z+1/2 7 -x+1/2,-y+1/2,-z 8 x+1/2,-y+1/2,z-1/2 _cell_length_a 40.525(4) _cell_length_b 24.073(2) _cell_length_c 12.188(1) _cell_angle_alpha 90 _cell_angle_beta 105.746(2) _cell_angle_gamma 90 _cell_volume 11443.7(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6298 _cell_measurement_temperature 150.01 _cell_measurement_theta_max 22.38 _cell_measurement_theta_min 2.59 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.1183 _exptl_crystal_density_meas . _exptl_crystal_F_000 3951.1988 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_unetI/netI 0.0978 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 53010 _diffrn_reflns_theta_full 28.4588 _diffrn_reflns_theta_max 28.46 _diffrn_reflns_theta_min 1.74 _diffrn_ambient_temperature 150.01 _diffrn_measured_fraction_theta_full 0.9829 _diffrn_measured_fraction_theta_max 0.9829 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 52 _reflns_limit_h_min -54 _reflns_limit_k_max 32 _reflns_limit_k_min 0 _reflns_limit_l_max 16 _reflns_limit_l_min 0 _reflns_number_gt 6799 _reflns_number_total 14217 _reflns_threshold_expression I>=2u(I) _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; olex2.refine (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation, 2011) ; _refine_diff_density_max 0.7376 _refine_diff_density_min -0.9178 _refine_diff_density_rms 0.1531 _refine_ls_d_res_high 0.7457 _refine_ls_d_res_low 11.4396 _refine_ls_goodness_of_fit_ref 0.9833 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 60 _refine_ls_number_parameters 578 _refine_ls_number_reflns 14217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1291 _refine_ls_R_factor_gt 0.0635 _refine_ls_restrained_S_all 0.9833 _refine_ls_shift/su_max 0.0033 _refine_ls_shift/su_mean 0.0005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1321P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.2419 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C13(H13), C16(H16), C17(H17), C22(H22), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46) 2.b Idealised Me refined as rotating group: C34(H34a,H34b,H34c), C35(H35a,H35b,H35c) ; 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_refinement_flags_posn Zn1 Zn 0.112665(13) 0.27832(2) 0.23962(4) 0.04153(17) Uani 1.000000 . S1 S 0.17287(4) 0.12519(6) 0.18624(14) 0.0772(5) Uani 1.000000 . S2 S 0.19943(3) 0.42133(5) 0.73519(8) 0.0466(3) Uani 1.000000 . S3 S 0.16790(4) 0.40253(5) 0.06799(10) 0.0557(3) Uani 1.000000 . F1 F 0.23408(8) 0.38652(13) 0.9362(2) 0.0711(9) Uani 1.000000 . F2 F 0.22196(8) 0.47264(14) 0.9296(2) 0.0780(10) Uani 1.000000 . F3 F 0.26141(8) 0.44329(14) 0.8600(2) 0.0715(8) Uani 1.000000 . N1 N 0.10637(9) 0.27249(16) 0.4155(3) 0.0455(9) Uani 1.000000 . N2 N 0.12860(9) 0.35440(15) 0.3153(3) 0.0403(8) Uani 1.000000 . N3 N 0.13308(9) 0.32126(15) 0.1120(3) 0.0393(8) Uani 1.000000 . N4 N 0.08749(11) 0.20465(16) 0.1791(3) 0.0521(10) Uani 1.000000 . N5 N 0.15449(11) 0.21788(16) 0.2527(3) 0.0523(10) Uani 1.000000 . N6 N 0.05841(9) 0.30159(17) 0.1719(3) 0.0478(9) Uani 1.000000 . O1 O 0.20036(9) 0.47217(13) 0.6758(3) 0.0576(9) Uani 1.000000 . O2 O 0.16840(9) 0.41273(17) 0.7665(3) 0.0738(11) Uani 1.000000 . O3 O 0.21250(13) 0.37347(16) 0.6922(3) 0.0933(15) Uani 1.000000 . O4 O 0.29649(8) 0.28267(13) 0.2164(2) 0.0529(8) Uani 1.000000 . C1 C 0.09489(12) 0.2293(2) 0.4606(4) 0.0557(13) Uani 1.000000 . H1 H 0.09027(12) 0.1959(2) 0.4176(4) 0.0668(15) Uiso 1.000000 R C2 C 0.08925(14) 0.2302(3) 0.5676(5) 0.0700(16) Uani 1.000000 . H2 H 0.08005(14) 0.1987(3) 0.5961(5) 0.0840(19) Uiso 1.000000 R C3 C 0.09726(15) 0.2773(3) 0.6308(5) 0.0777(18) Uani 1.000000 . H3 H 0.09481(15) 0.2785(3) 0.7061(5) 0.093(2) Uiso 1.000000 R C4 C 0.11330(11) 0.3192(2) 0.4754(3) 0.0465(11) Uani 1.000000 . C5 C 0.10889(13) 0.3232(3) 0.5856(4) 0.0622(14) Uani 1.000000 . H5 H 0.11384(13) 0.3568(3) 0.6279(4) 0.0747(17) Uiso 1.000000 R C6 C 0.12594(11) 0.3662(2) 0.4197(3) 0.0467(11) Uani 1.000000 . C7 C 0.13579(13) 0.4178(2) 0.4683(4) 0.0608(14) Uani 1.000000 . H7 H 0.13348(13) 0.4264(2) 0.5420(4) 0.0730(16) Uiso 1.000000 R C8 C 0.14879(14) 0.4560(2) 0.4093(4) 0.0641(14) Uani 1.000000 . H8 H 0.15595(14) 0.4912(2) 0.4426(4) 0.0769(17) Uiso 1.000000 R C9 C 0.15178(13) 0.4440(2) 0.2994(4) 0.0576(13) Uani 1.000000 . H9 H 0.16056(13) 0.4704(2) 0.2567(4) 0.0692(15) Uiso 1.000000 R C10 C 0.14136(11) 0.39215(18) 0.2570(3) 0.0411(10) Uani 1.000000 . C11 C 0.14505(11) 0.37078(17) 0.1477(3) 0.0409(10) Uani 1.000000 . C12 C 0.14305(11) 0.30650(19) 0.0155(3) 0.0439(10) Uani 1.000000 . C13 C 0.16171(13) 0.3456(2) -0.0187(4) 0.0566(13) Uani 1.000000 . H13 H 0.17041(13) 0.3421(2) -0.0833(4) 0.0679(15) Uiso 1.000000 R C14 C 0.18921(13) 0.2220(2) 0.2670(4) 0.0544(13) Uani 1.000000 . C15 C 0.20708(12) 0.2732(2) 0.3071(4) 0.0542(13) Uani 1.000000 . C16 C 0.20255(13) 0.3011(3) 0.4035(4) 0.0659(15) Uani 1.000000 . H16 H 0.18792(13) 0.2858(3) 0.4448(4) 0.0791(18) Uiso 1.000000 R C17 C 0.22903(12) 0.2971(2) 0.2493(4) 0.0490(12) Uani 1.000000 . H17 H 0.23250(12) 0.2790(2) 0.1841(4) 0.0588(14) Uiso 1.000000 R C18 C 0.24579(12) 0.3467(2) 0.2853(4) 0.0497(12) Uani 1.000000 . C19 C 0.26984(12) 0.3712(2) 0.2248(3) 0.0458(11) Uani 1.000000 . C20 C 0.29510(12) 0.3390(2) 0.1958(3) 0.0469(11) Uani 1.000000 . C21 C 0.31880(12) 0.3636(2) 0.1457(4) 0.0480(11) Uani 1.000000 . C22 C 0.31605(13) 0.4197(2) 0.1228(4) 0.0541(12) Uani 1.000000 . H22 H 0.33210(13) 0.4365(2) 0.0888(4) 0.0649(15) Uiso 1.000000 R C23 C 0.29059(13) 0.4532(2) 0.1473(4) 0.0537(12) Uani 1.000000 . C24 C 0.26804(13) 0.4271(2) 0.1990(4) 0.0543(12) Uani 1.000000 . H24 H 0.25066(13) 0.4488(2) 0.2172(4) 0.0652(15) Uiso 1.000000 R C25 C 0.34611(13) 0.3301(2) 0.1179(4) 0.0512(12) Uani 1.000000 . C26 C 0.33964(12) 0.27799(19) 0.0640(3) 0.0450(11) Uani 1.000000 . H26 H 0.31705(12) 0.26324(19) 0.0449(3) 0.0540(13) Uiso 1.000000 R C27 C 0.39833(13) 0.2696(2) 0.0633(4) 0.0574(13) Uani 1.000000 . H27 H 0.41616(13) 0.2491(2) 0.0451(4) 0.0688(15) Uiso 1.000000 R C28 C 0.36564(12) 0.2480(2) 0.0384(3) 0.0459(11) Uani 1.000000 . C29 C 0.37910(14) 0.3516(2) 0.1420(4) 0.0624(14) Uani 1.000000 . H29 H 0.38388(14) 0.3870(2) 0.1771(4) 0.0748(16) Uiso 1.000000 R C30 C 0.21908(14) 0.3501(3) 0.4377(4) 0.0750(18) Uani 1.000000 . H30 H 0.21577(14) 0.3686(3) 0.5028(4) 0.090(2) Uiso 1.000000 R C31 C 0.24046(12) 0.3730(2) 0.3796(4) 0.0614(14) Uani 1.000000 . H31 H 0.25164(12) 0.4073(2) 0.4046(4) 0.0737(17) Uiso 1.000000 R C32 C 0.23083(13) 0.4313(2) 0.8711(4) 0.0501(11) Uani 1.000000 . C34 C 0.31316(14) 0.2679(2) 0.3316(4) 0.0722(16) Uani 1.000000 . H34a H 0.3363(4) 0.2838(14) 0.3537(11) 0.108(2) Uiso 1.000000 GR H34b H 0.2999(6) 0.2823(14) 0.3819(6) 0.108(2) Uiso 1.000000 GR H34c H 0.3147(9) 0.2273(2) 0.3384(8) 0.108(2) Uiso 1.000000 GR C35 C 0.28736(16) 0.5137(2) 0.1185(5) 0.0677(15) Uani 1.000000 . H35a H 0.2675(6) 0.5291(4) 0.139(3) 0.102(2) Uiso 1.000000 GR H35b H 0.3082(4) 0.5331(3) 0.161(2) 0.102(2) Uiso 1.000000 GR H35c H 0.2843(10) 0.5185(2) 0.0365(7) 0.102(2) Uiso 1.000000 GR C36 C 0.04544(13) 0.3525(2) 0.1653(4) 0.0630(14) Uani 1.000000 . H36 H 0.06057(13) 0.3830(2) 0.1894(4) 0.0756(16) Uiso 1.000000 R C37 C 0.03701(13) 0.2577(2) 0.1395(4) 0.0569(13) Uani 1.000000 . C38 C 0.05397(14) 0.2030(2) 0.1460(5) 0.0626(14) Uani 1.000000 . C39 C 0.20307(15) 0.1745(2) 0.2350(5) 0.0698(16) Uani 1.000000 . H39 H 0.22670(15) 0.1699(2) 0.2398(5) 0.0838(19) Uiso 1.000000 R C40 C 0.40528(14) 0.3215(2) 0.1151(4) 0.0655(14) Uani 1.000000 . H40 H 0.42781(14) 0.3364(2) 0.1320(4) 0.0786(17) Uiso 1.000000 R C41 C 0.01098(15) 0.3627(3) 0.1249(6) 0.0862(19) Uani 1.000000 . H41 H 0.00223(15) 0.3996(3) 0.1193(6) 0.103(2) Uiso 1.000000 R C42 C -0.01087(16) 0.3171(4) 0.0923(6) 0.097(2) Uani 1.000000 . H42 H -0.03488(16) 0.3229(4) 0.0647(6) 0.117(3) Uiso 1.000000 R C43 C 0.00181(15) 0.2647(3) 0.0997(5) 0.0778(17) Uani 1.000000 . H43 H -0.01300(15) 0.2336(3) 0.0783(5) 0.093(2) Uiso 1.000000 R C44 C 0.03650(19) 0.1529(3) 0.1116(8) 0.116(3) Uani 1.000000 . H44 H 0.01215(19) 0.1518(3) 0.0899(8) 0.139(3) Uiso 1.000000 R C45 C 0.0547(2) 0.1069(3) 0.1101(9) 0.137(4) Uani 1.000000 . H45 H 0.0431(2) 0.0732(3) 0.0830(9) 0.165(4) Uiso 1.000000 R C46 C 0.0903(2) 0.1071(3) 0.1473(8) 0.117(3) Uani 1.000000 . H46 H 0.1033(2) 0.0740(3) 0.1499(8) 0.141(3) Uiso 1.000000 R C47 C 0.10617(16) 0.1588(2) 0.1811(5) 0.0689(15) Uani 1.000000 . C48 C 0.14231(15) 0.1689(2) 0.2112(5) 0.0625(14) Uani 1.000000 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.0350(3) 0.0435(3) 0.0482(3) 0.0025(2) 0.0150(2) 0.0061(2) S1 0.0861(12) 0.0517(8) 0.1082(11) 0.0286(8) 0.0508(9) 0.0222(8) S2 0.0618(8) 0.0437(6) 0.0357(5) 0.0010(6) 0.0156(5) 0.0017(4) S3 0.0651(9) 0.0491(7) 0.0619(7) -0.0008(6) 0.0327(6) 0.0119(6) F1 0.080(2) 0.081(2) 0.0465(15) -0.0003(17) 0.0080(14) 0.0214(14) F2 0.068(2) 0.092(2) 0.0648(17) 0.0157(18) 0.0025(15) -0.0335(16) F3 0.0494(19) 0.098(2) 0.0687(18) -0.0001(17) 0.0188(14) 0.0159(16) N1 0.030(2) 0.060(2) 0.0478(19) 0.0074(18) 0.0134(16) 0.0144(18) N2 0.034(2) 0.050(2) 0.0367(17) 0.0037(17) 0.0097(14) 0.0031(15) N3 0.034(2) 0.045(2) 0.0407(17) 0.0026(17) 0.0132(15) 0.0060(15) N4 0.051(3) 0.049(2) 0.063(2) -0.000(2) 0.028(2) 0.0050(18) N5 0.053(3) 0.051(2) 0.062(2) 0.017(2) 0.031(2) 0.0185(19) N6 0.034(2) 0.056(2) 0.051(2) -0.0018(19) 0.0076(16) 0.0031(18) O1 0.065(2) 0.055(2) 0.0529(18) -0.0035(17) 0.0161(16) 0.0156(15) O2 0.057(2) 0.112(3) 0.0484(18) -0.027(2) 0.0061(16) 0.0164(18) O3 0.155(4) 0.070(3) 0.050(2) 0.043(3) 0.019(2) -0.0108(18) O4 0.055(2) 0.059(2) 0.0494(17) 0.0121(16) 0.0229(15) 0.0073(14) C1 0.041(3) 0.063(3) 0.066(3) 0.005(2) 0.018(2) 0.025(3) C2 0.052(3) 0.098(5) 0.063(3) 0.001(3) 0.020(3) 0.038(3) C3 0.065(4) 0.122(6) 0.052(3) 0.007(4) 0.025(3) 0.030(3) C4 0.031(2) 0.069(3) 0.040(2) 0.004(2) 0.0111(18) 0.007(2) C5 0.051(3) 0.091(4) 0.046(3) 0.003(3) 0.015(2) 0.001(3) C6 0.032(2) 0.063(3) 0.044(2) 0.001(2) 0.0095(19) -0.004(2) C7 0.061(3) 0.076(4) 0.047(3) -0.010(3) 0.016(2) -0.017(2) C8 0.071(4) 0.062(3) 0.063(3) -0.018(3) 0.024(3) -0.020(3) C9 0.059(3) 0.052(3) 0.065(3) -0.013(3) 0.022(2) -0.004(2) C10 0.038(3) 0.043(2) 0.044(2) -0.002(2) 0.0125(19) 0.0011(19) C11 0.039(3) 0.040(2) 0.044(2) 0.005(2) 0.0108(19) 0.0094(18) C12 0.044(3) 0.049(3) 0.042(2) 0.008(2) 0.0174(19) 0.007(2) C13 0.067(3) 0.062(3) 0.051(3) 0.001(3) 0.034(2) 0.006(2) C14 0.045(3) 0.068(3) 0.058(3) 0.019(3) 0.027(2) 0.018(2) C15 0.036(3) 0.081(4) 0.046(2) 0.027(3) 0.012(2) 0.017(2) C16 0.042(3) 0.111(5) 0.045(3) 0.020(3) 0.012(2) 0.015(3) C17 0.040(3) 0.066(3) 0.042(2) 0.021(2) 0.0116(19) 0.010(2) C18 0.036(3) 0.068(3) 0.044(2) 0.017(2) 0.0094(19) 0.003(2) C19 0.045(3) 0.055(3) 0.038(2) 0.005(2) 0.0115(19) -0.0037(19) C20 0.046(3) 0.055(3) 0.040(2) 0.005(2) 0.012(2) -0.005(2) C21 0.043(3) 0.060(3) 0.043(2) 0.004(2) 0.015(2) -0.005(2) C22 0.057(3) 0.059(3) 0.048(2) -0.009(3) 0.018(2) -0.015(2) C23 0.059(3) 0.057(3) 0.043(2) 0.002(3) 0.011(2) -0.011(2) C24 0.048(3) 0.069(3) 0.044(2) 0.009(3) 0.009(2) -0.012(2) C25 0.048(3) 0.063(3) 0.047(2) -0.001(2) 0.019(2) -0.002(2) C26 0.044(3) 0.057(3) 0.038(2) 0.001(2) 0.0175(19) 0.0024(19) C27 0.052(3) 0.072(4) 0.055(3) 0.003(3) 0.027(2) -0.006(2) C28 0.045(3) 0.057(3) 0.041(2) 0.000(2) 0.0226(19) -0.002(2) C29 0.059(4) 0.067(4) 0.066(3) -0.005(3) 0.025(3) -0.014(3) C30 0.045(3) 0.136(6) 0.043(3) 0.015(4) 0.010(2) -0.014(3) C31 0.043(3) 0.097(4) 0.042(2) 0.008(3) 0.009(2) -0.013(2) C32 0.049(3) 0.055(3) 0.049(2) 0.005(2) 0.017(2) 0.003(2) C34 0.059(4) 0.087(4) 0.067(3) 0.024(3) 0.013(3) 0.022(3) C35 0.081(4) 0.047(3) 0.078(3) -0.004(3) 0.025(3) -0.015(3) C36 0.045(3) 0.059(3) 0.084(3) 0.008(3) 0.016(3) 0.006(3) C37 0.039(3) 0.074(4) 0.059(3) -0.007(3) 0.016(2) -0.006(3) C38 0.053(4) 0.055(3) 0.084(4) -0.013(3) 0.027(3) -0.015(3) C39 0.061(4) 0.070(4) 0.087(4) 0.026(3) 0.036(3) 0.026(3) C40 0.053(3) 0.072(4) 0.079(3) -0.011(3) 0.031(3) -0.022(3) C41 0.043(4) 0.086(5) 0.118(5) 0.018(3) 0.002(3) -0.002(4) C42 0.037(3) 0.136(7) 0.110(5) 0.014(4) 0.006(3) -0.006(5) C43 0.042(3) 0.084(4) 0.105(4) -0.005(3) 0.014(3) -0.019(4) C44 0.068(5) 0.078(5) 0.210(8) -0.027(4) 0.055(5) -0.042(5) C45 0.103(7) 0.054(4) 0.273(11) -0.032(4) 0.082(7) -0.045(6) C46 0.124(7) 0.042(4) 0.215(9) -0.007(4) 0.096(7) -0.007(4) C47 0.072(4) 0.044(3) 0.103(4) 0.003(3) 0.044(3) 0.001(3) C48 0.072(4) 0.048(3) 0.083(3) 0.014(3) 0.045(3) 0.018(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zn1 N1 2.231(3) . Zn1 N2 2.073(4) . Zn1 N3 2.207(3) . Zn1 N4 2.079(4) . Zn1 N5 2.206(4) . Zn1 N6 2.201(4) . S1 C39 1.693(6) . S1 C48 1.713(5) . S2 O1 1.427(3) . S2 O2 1.425(4) . S2 O3 1.426(4) . S2 C32 1.810(5) . S3 C11 1.696(4) . S3 C13 1.706(5) . F1 C32 1.324(5) . F2 C32 1.330(5) . F3 C32 1.315(5) . N1 C1 1.319(5) . N1 C4 1.329(6) . N2 C6 1.337(5) . N2 C10 1.341(5) . N3 C11 1.316(5) . N3 C12 1.390(5) . N4 C38 1.309(6) . N4 C47 1.334(6) . N5 C14 1.374(6) . N5 C48 1.325(7) . N6 C36 1.328(6) . N6 C37 1.355(6) . O4 C20 1.378(5) . O4 C34 1.429(6) . C1 C2 1.383(7) . C2 C3 1.360(8) . C3 C5 1.373(8) . C4 C5 1.406(6) . C4 C6 1.480(6) . C6 C7 1.388(6) . C7 C8 1.358(7) . C8 C9 1.408(6) . C9 C10 1.372(6) . C10 C11 1.472(6) . C12 C13 1.343(6) . C12 C28 1.467(6) 7 C14 C15 1.446(7) . C14 C39 1.376(7) . C15 C16 1.407(7) . C15 C17 1.400(6) . C16 C30 1.364(8) . C17 C18 1.386(7) . C18 C19 1.493(6) . C18 C31 1.380(6) . C19 C20 1.403(6) . C19 C24 1.380(6) . C20 C21 1.401(6) . C21 C22 1.379(6) . C21 C25 1.480(6) . C22 C23 1.404(7) . C23 C24 1.392(7) . C23 C35 1.495(7) . C25 C26 1.408(6) . C25 C29 1.388(7) . C26 C28 1.381(6) . C27 C28 1.378(6) . C27 C40 1.395(7) . C29 C40 1.395(7) . C30 C31 1.375(7) . C36 C41 1.371(7) . C37 C38 1.479(7) . C37 C43 1.387(7) . C38 C44 1.403(8) . C41 C42 1.399(9) . C42 C43 1.357(9) . C44 C45 1.335(10) . C45 C46 1.388(11) . C46 C47 1.411(8) . C47 C48 1.431(8) . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N2 Zn1 N1 74.40(14) . . N3 Zn1 N1 150.36(14) . . N3 Zn1 N2 76.63(13) . . N4 Zn1 N1 96.55(14) . . N4 Zn1 N2 167.17(14) . . N4 Zn1 N3 113.04(14) . . N5 Zn1 N1 100.10(13) . . N5 Zn1 N2 114.20(15) . . N5 Zn1 N3 86.11(13) . . N5 Zn1 N4 75.90(16) . . N6 Zn1 N1 90.76(13) . . N6 Zn1 N2 95.79(14) . . N6 Zn1 N3 98.26(13) . . N6 Zn1 N4 74.93(16) . . N6 Zn1 N5 149.82(16) . . C48 S1 C39 89.8(3) . . O2 S2 O1 114.0(2) . . O3 S2 O1 116.3(2) . . O3 S2 O2 115.1(3) . . C32 S2 O1 104.0(2) . . C32 S2 O2 103.1(2) . . C32 S2 O3 101.8(2) . . C13 S3 C11 88.9(2) . . C1 N1 Zn1 126.6(3) . . C4 N1 Zn1 114.3(3) . . C4 N1 C1 119.0(4) . . C6 N2 Zn1 121.0(3) . . C10 N2 Zn1 118.8(3) . . C10 N2 C6 120.2(4) . . C11 N3 Zn1 111.5(3) . . C12 N3 Zn1 136.7(3) . . C12 N3 C11 110.2(4) . . C38 N4 Zn1 120.3(3) . . C47 N4 Zn1 118.5(4) . . C47 N4 C38 121.1(5) . . C14 N5 Zn1 134.6(3) . . C48 N5 Zn1 111.1(3) . . C48 N5 C14 112.1(4) . . C36 N6 Zn1 126.6(3) . . C37 N6 Zn1 114.0(3) . . C37 N6 C36 119.3(4) . . C34 O4 C20 114.2(4) . . C2 C1 N1 123.3(5) . . C3 C2 C1 118.1(5) . . C5 C3 C2 119.9(5) . . C5 C4 N1 121.3(4) . . C6 C4 N1 116.3(4) . . C6 C4 C5 122.4(5) . . C4 C5 C3 118.4(5) . . C4 C6 N2 113.6(4) . . C7 C6 N2 120.5(4) . . C7 C6 C4 125.8(4) . . C8 C7 C6 119.2(4) . . C9 C8 C7 120.7(5) . . C10 C9 C8 116.6(4) . . C9 C10 N2 122.7(4) . . C11 C10 N2 113.0(4) . . C11 C10 C9 124.2(4) . . N3 C11 S3 115.3(3) . . C10 C11 S3 124.5(3) . . C10 C11 N3 119.8(4) . . C13 C12 N3 113.6(4) . . C28 C12 N3 121.2(4) 7 . C28 C12 C13 125.2(4) 7 . C12 C13 S3 111.8(3) . . C15 C14 N5 120.4(4) . . C39 C14 N5 112.7(5) . . C39 C14 C15 126.8(5) . . C16 C15 C14 121.5(5) . . C17 C15 C14 120.5(4) . . C17 C15 C16 118.0(5) . . C30 C16 C15 120.2(5) . . C18 C17 C15 121.2(4) . . C19 C18 C17 120.9(4) . . C31 C18 C17 119.1(5) . . C31 C18 C19 120.1(5) . . C20 C19 C18 121.7(4) . . C24 C19 C18 119.8(4) . . C24 C19 C20 118.5(4) . . C19 C20 O4 119.6(4) . . C21 C20 O4 119.7(4) . . C21 C20 C19 120.7(4) . . C22 C21 C20 118.3(4) . . C25 C21 C20 121.0(4) . . C25 C21 C22 120.7(4) . . C23 C22 C21 122.9(5) . . C24 C23 C22 116.6(5) . . C35 C23 C22 122.1(5) . . C35 C23 C24 121.2(5) . . C23 C24 C19 122.8(5) . . C26 C25 C21 122.4(4) . . C29 C25 C21 119.1(4) . . C29 C25 C26 118.5(4) . . C28 C26 C25 121.0(4) . . C40 C27 C28 120.1(5) . . C26 C28 C12 117.6(4) . 7 C27 C28 C12 122.4(4) . 7 C27 C28 C26 120.0(4) . . C40 C29 C25 120.5(5) . . C31 C30 C16 121.0(5) . . C30 C31 C18 120.5(6) . . F1 C32 S2 111.8(3) . . F2 C32 S2 111.4(3) . . F2 C32 F1 106.6(4) . . F3 C32 S2 112.6(3) . . F3 C32 F1 107.3(4) . . F3 C32 F2 106.9(4) . . C41 C36 N6 122.4(5) . . C38 C37 N6 115.3(4) . . C43 C37 N6 121.6(5) . . C43 C37 C38 123.0(5) . . C37 C38 N4 114.7(4) . . C44 C38 N4 121.1(6) . . C44 C38 C37 124.1(6) . . C14 C39 S1 111.7(4) . . C29 C40 C27 119.9(5) . . C42 C41 C36 117.7(6) . . C43 C42 C41 120.9(6) . . C42 C43 C37 118.0(6) . . C45 C44 C38 118.8(7) . . C46 C45 C44 121.4(7) . . C47 C46 C45 116.7(6) . . C46 C47 N4 120.8(6) . . C48 C47 N4 113.7(5) . . C48 C47 C46 125.3(6) . . N5 C48 S1 113.7(4) . . C47 C48 S1 126.1(4) . . C47 C48 N5 119.8(5) . . _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.454 -0.329 1997.8 306.3 ? 2 0.250 0.250 0.000 25.1 0.0 ? 3 0.250 0.750 0.500 25.1 0.0 ? 4 0.500 -0.696 -0.180 1997.8 306.3 ? 5 0.750 0.250 0.500 25.1 0.0 ? 6 0.750 0.750 0.000 25.1 0.0 ? _database_code_depnum_ccdc_archive 'CCDC 945475' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_chris_lome_cd_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H64 Cd2 N12 O2 S4, 4(Cl O4), 0.77(C2 N), 4(C2 H3 N), 0.23(O)' _chemical_formula_sum 'C101.53 H78 Cd2 Cl4 N16.76 O18.24 S4' _chemical_formula_weight 2319.48 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 ' _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6829(8) _cell_length_b 16.4451(10) _cell_length_c 25.0185(14) _cell_angle_alpha 94.6030(10) _cell_angle_beta 101.5490(10) _cell_angle_gamma 97.467(2) _cell_volume 5038.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 23.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2357 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.8387 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 112792 _diffrn_reflns_av_R_equivalents 0.0807 _diffrn_reflns_av_sigmaI/netI 0.0989 _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 -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.03 _reflns_number_total 29420 _reflns_number_gt 16062 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+1.6475P] 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 29420 _refine_ls_number_parameters 1361 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1518 _refine_ls_wR_factor_gt 0.1237 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.016 _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 Cd1 Cd 0.57422(2) -0.134970(16) 0.280897(11) 0.02892(7) Uani 1 1 d . . . Cd2 Cd 1.20415(2) 0.382203(17) 0.253987(11) 0.03365(8) Uani 1 1 d . . . S1 S 1.22584(9) 0.19186(7) 0.38958(5) 0.0451(3) Uani 1 1 d . . . S2 S 0.51393(10) 0.10245(7) 0.38356(5) 0.0475(3) Uani 1 1 d . . . S3 S 0.90559(16) 0.38278(11) 0.10511(7) 0.0944(6) Uani 1 1 d . . . S4 S 0.90693(10) -0.15165(8) 0.22058(5) 0.0493(3) Uani 1 1 d . . . Cl1 Cl 0.23892(10) 0.91992(7) 0.38666(5) 0.0515(3) Uani 1 1 d . . . Cl2 Cl 0.56734(9) 0.33184(7) 0.43369(5) 0.0499(3) Uani 1 1 d . . . Cl3 Cl 0.40595(10) 0.72696(8) 0.95991(5) 0.0549(3) Uani 1 1 d . . . Cl4 Cl 0.9540(5) 0.6498(5) 0.0961(3) 0.0715(15) Uani 0.598(9) 1 d P A 1 O16 O 1.0102(6) 0.6848(5) 0.0569(3) 0.094(3) Uani 0.598(9) 1 d P A 1 N1 N 1.2310(3) 0.5267(2) 0.27280(14) 0.0395(8) Uani 1 1 d . . . N2 N 1.2526(2) 0.4206(2) 0.34756(13) 0.0328(7) Uani 1 1 d . . . N3 N 1.1971(3) 0.2618(2) 0.30180(13) 0.0335(7) Uani 1 1 d . . . N4 N 0.5495(2) -0.00242(18) 0.31201(13) 0.0282(7) Uani 1 1 d . . . N5 N 0.5649(2) -0.12951(19) 0.37244(13) 0.0317(7) Uani 1 1 d . . . N6 N 0.5605(3) -0.2698(2) 0.31004(15) 0.0396(8) Uani 1 1 d . . . N7 N 1.3849(3) 0.3676(2) 0.24528(16) 0.0449(9) Uani 1 1 d . . . N8 N 1.2157(4) 0.3632(2) 0.16228(15) 0.0505(10) Uani 1 1 d . . . N9 N 1.0309(3) 0.3832(2) 0.19843(14) 0.0450(9) Uani 1 1 d . . . N10 N 0.7638(3) -0.12121(19) 0.27494(13) 0.0315(7) Uani 1 1 d . . . N11 N 0.5859(3) -0.1833(2) 0.19406(14) 0.0366(8) Uani 1 1 d . . . N12 N 0.4011(3) -0.1490(2) 0.21969(14) 0.0390(8) Uani 1 1 d . . . N13 N 0.8177(4) 0.7081(3) 0.3226(2) 0.0703(14) Uani 1 1 d . . . O1 O 0.8111(2) 0.10179(17) 0.19465(11) 0.0388(7) Uani 1 1 d . . . O2 O 0.8831(2) 0.20008(16) 0.33545(11) 0.0364(6) Uani 1 1 d . . . O3 O 0.3179(4) 0.8677(4) 0.3968(3) 0.133(2) Uani 1 1 d . . . O4 O 0.2166(4) 0.9385(3) 0.33123(17) 0.0985(15) Uani 1 1 d . . . O5 O 0.2672(7) 0.9924(3) 0.4201(2) 0.178(3) Uani 1 1 d . . . O6 O 0.1386(4) 0.8808(3) 0.3971(2) 0.1080(17) Uani 1 1 d . . . O7 O 0.5602(3) 0.41521(19) 0.42243(15) 0.0690(10) Uani 1 1 d . . . O8 O 0.6656(3) 0.3085(3) 0.42276(17) 0.0781(12) Uani 1 1 d . . . O9 O 0.4763(3) 0.27818(19) 0.39898(15) 0.0621(10) Uani 1 1 d . . . O10 O 0.5637(3) 0.3237(2) 0.48988(15) 0.0644(10) Uani 1 1 d . . . O11 O 0.3613(3) 0.7127(4) 0.90308(16) 0.118(2) Uani 1 1 d . . . O12 O 0.4932(3) 0.6808(3) 0.97384(19) 0.0993(15) Uani 1 1 d . . . O13 O 0.3230(3) 0.7042(3) 0.98769(17) 0.1010(16) Uani 1 1 d . . . O14 O 0.4472(4) 0.8116(3) 0.9774(2) 0.1181(18) Uani 1 1 d . . . C1 C 1.2157(4) 0.5772(3) 0.2338(2) 0.0525(12) Uani 1 1 d . . . H1 H 1.1903 0.5535 0.1968 0.063 Uiso 1 1 calc R . . C2 C 1.2348(4) 0.6625(3) 0.2444(2) 0.0586(13) Uani 1 1 d . . . H2 H 1.2215 0.6967 0.2157 0.070 Uiso 1 1 calc R . . C3 C 1.2738(4) 0.6958(3) 0.2981(2) 0.0548(13) Uani 1 1 d . . . H3 H 1.2896 0.7539 0.3070 0.066 Uiso 1 1 calc R . . C4 C 1.2899(3) 0.6442(3) 0.3387(2) 0.0480(12) Uani 1 1 d . . . H4 H 1.3158 0.6665 0.3760 0.058 Uiso 1 1 calc R . . C5 C 1.2681(3) 0.5600(2) 0.32504(17) 0.0365(9) Uani 1 1 d . . . C6 C 1.2832(3) 0.5000(3) 0.36673(17) 0.0380(9) Uani 1 1 d . . . C7 C 1.3257(4) 0.5232(3) 0.42193(18) 0.0478(11) Uani 1 1 d . . . H7 H 1.3492 0.5797 0.4352 0.057 Uiso 1 1 calc R . . C8 C 1.3339(4) 0.4640(3) 0.45745(19) 0.0541(13) Uani 1 1 d . . . H8 H 1.3622 0.4794 0.4956 0.065 Uiso 1 1 calc R . . C9 C 1.3011(4) 0.3825(3) 0.43794(18) 0.0481(11) Uani 1 1 d . . . H9 H 1.3056 0.3408 0.4621 0.058 Uiso 1 1 calc R . . C10 C 1.2613(3) 0.3623(3) 0.38178(16) 0.0353(9) Uani 1 1 d . . . C11 C 1.2279(3) 0.2774(3) 0.35541(16) 0.0346(9) Uani 1 1 d . . . C12 C 1.1809(3) 0.1310(3) 0.32887(17) 0.0402(10) Uani 1 1 d . . . H12 H 1.1656 0.0725 0.3253 0.048 Uiso 1 1 calc R . . C13 C 1.1697(3) 0.1777(2) 0.28604(16) 0.0328(9) Uani 1 1 d . . . C14 C 1.1332(3) 0.1473(2) 0.22720(16) 0.0316(8) Uani 1 1 d . . . C15 C 1.1937(3) 0.1741(2) 0.18958(17) 0.0360(9) Uani 1 1 d . . . H15 H 1.2602 0.2107 0.2019 0.043 Uiso 1 1 calc R . . C16 C 1.1575(3) 0.1478(2) 0.13467(17) 0.0378(9) Uani 1 1 d . . . H16 H 1.1998 0.1654 0.1092 0.045 Uiso 1 1 calc R . . C17 C 1.0595(3) 0.0959(2) 0.11631(17) 0.0375(9) Uani 1 1 d . . . H17 H 1.0348 0.0785 0.0782 0.045 Uiso 1 1 calc R . . C18 C 0.9965(3) 0.0687(2) 0.15311(16) 0.0324(8) Uani 1 1 d . . . C19 C 1.0356(3) 0.0939(2) 0.20869(17) 0.0359(9) Uani 1 1 d . . . H19 H 0.9952 0.0744 0.2344 0.043 Uiso 1 1 calc R . . C20 C 0.8869(3) 0.0204(2) 0.13158(16) 0.0334(9) Uani 1 1 d . . . C21 C 0.7968(3) 0.0404(2) 0.15161(16) 0.0319(8) Uani 1 1 d . . . C22 C 0.6917(3) -0.0003(3) 0.12744(16) 0.0357(9) Uani 1 1 d . . . C23 C 0.6781(3) -0.0611(3) 0.08435(17) 0.0436(10) Uani 1 1 d . . . H23 H 0.6068 -0.0880 0.0677 0.052 Uiso 1 1 calc R . . C24 C 0.7665(4) -0.0840(3) 0.06463(17) 0.0419(10) Uani 1 1 d . . . C25 C 0.8702(3) -0.0425(3) 0.08887(16) 0.0382(9) Uani 1 1 d . . . H25 H 0.9310 -0.0576 0.0758 0.046 Uiso 1 1 calc R . . C26 C 0.7524(4) -0.1521(3) 0.0180(2) 0.0645(15) Uani 1 1 d . . . H26A H 0.7787 -0.1295 -0.0128 0.097 Uiso 1 1 calc R . . H26B H 0.6752 -0.1753 0.0061 0.097 Uiso 1 1 calc R . . H26C H 0.7943 -0.1956 0.0306 0.097 Uiso 1 1 calc R . . C27 C 0.8063(5) 0.1819(3) 0.1778(2) 0.0645(15) Uani 1 1 d . . . H27A H 0.8625 0.1952 0.1568 0.097 Uiso 1 1 calc R . . H27B H 0.8188 0.2223 0.2103 0.097 Uiso 1 1 calc R . . H27C H 0.7345 0.1834 0.1548 0.097 Uiso 1 1 calc R . . C28 C 0.5968(3) 0.0237(3) 0.14805(17) 0.0385(10) Uani 1 1 d . . . C29 C 0.5062(4) 0.0412(4) 0.1129(2) 0.0705(17) Uani 1 1 d . . . H29 H 0.5031 0.0364 0.0745 0.085 Uiso 1 1 calc R . . C30 C 0.4197(5) 0.0657(5) 0.1329(2) 0.086(2) Uani 1 1 d . . . H30 H 0.3573 0.0765 0.1080 0.103 Uiso 1 1 calc R . . C31 C 0.4230(4) 0.0745(4) 0.1884(2) 0.0623(15) Uani 1 1 d . . . H31 H 0.3637 0.0921 0.2016 0.075 Uiso 1 1 calc R . . C32 C 0.5135(3) 0.0575(2) 0.22506(16) 0.0332(9) Uani 1 1 d . . . C33 C 0.5985(3) 0.0311(2) 0.20422(16) 0.0315(8) Uani 1 1 d . . . H33 H 0.6595 0.0177 0.2289 0.038 Uiso 1 1 calc R . . C34 C 0.5182(3) 0.0626(2) 0.28410(16) 0.0312(8) Uani 1 1 d . . . C35 C 0.4959(4) 0.1249(3) 0.31727(19) 0.0434(11) Uani 1 1 d . . . H35 H 0.4733 0.1744 0.3051 0.052 Uiso 1 1 calc R . . C36 C 0.5491(3) 0.0099(2) 0.36403(16) 0.0331(9) Uani 1 1 d . . . C37 C 0.5666(3) -0.0558(3) 0.39999(16) 0.0334(9) Uani 1 1 d . . . C38 C 0.5806(3) -0.0457(3) 0.45640(17) 0.0437(11) Uani 1 1 d . . . H38 H 0.5842 0.0071 0.4756 0.052 Uiso 1 1 calc R . . C39 C 0.5894(4) -0.1143(4) 0.4840(2) 0.0572(14) Uani 1 1 d . . . H39 H 0.5995 -0.1092 0.5228 0.069 Uiso 1 1 calc R . . C40 C 0.5834(4) -0.1910(3) 0.45527(19) 0.0507(13) Uani 1 1 d . . . H40 H 0.5865 -0.2388 0.4742 0.061 Uiso 1 1 calc R . . C41 C 0.5730(3) -0.1975(3) 0.39890(17) 0.0369(9) Uani 1 1 d . . . C42 C 0.5677(3) -0.2752(3) 0.36388(19) 0.0411(10) Uani 1 1 d . . . C43 C 0.5689(4) -0.3516(3) 0.3849(2) 0.0517(13) Uani 1 1 d . . . H43 H 0.5733 -0.3549 0.4230 0.062 Uiso 1 1 calc R . . C44 C 0.5637(4) -0.4213(3) 0.3503(3) 0.0656(17) Uani 1 1 d . . . H44 H 0.5655 -0.4732 0.3642 0.079 Uiso 1 1 calc R . . C45 C 0.5557(4) -0.4156(3) 0.2957(3) 0.0637(16) Uani 1 1 d . . . H45 H 0.5508 -0.4637 0.2711 0.076 Uiso 1 1 calc R . . C46 C 0.5549(4) -0.3390(3) 0.2764(2) 0.0529(12) Uani 1 1 d . . . H46 H 0.5502 -0.3352 0.2384 0.063 Uiso 1 1 calc R . . C47 C 1.4664(4) 0.3666(2) 0.2885(2) 0.0490(12) Uani 1 1 d . . . H47 H 1.4533 0.3766 0.3244 0.059 Uiso 1 1 calc R . . C48 C 1.5688(4) 0.3515(3) 0.2831(3) 0.0683(16) Uani 1 1 d . . . H48 H 1.6256 0.3519 0.3143 0.082 Uiso 1 1 calc R . . C49 C 1.5854(6) 0.3357(4) 0.2304(4) 0.096(3) Uani 1 1 d . . . H49 H 1.6546 0.3249 0.2251 0.115 Uiso 1 1 calc R . . C50 C 1.5026(6) 0.3356(4) 0.1864(3) 0.088(2) Uani 1 1 d . . . H50 H 1.5136 0.3236 0.1503 0.105 Uiso 1 1 calc R . . C51 C 1.4026(4) 0.3528(3) 0.1940(2) 0.0571(14) Uani 1 1 d . . . C52 C 1.3080(5) 0.3532(3) 0.1483(2) 0.0611(15) Uani 1 1 d . . . C53 C 1.3135(7) 0.3426(3) 0.0920(3) 0.090(2) Uani 1 1 d . . . H53 H 1.3804 0.3364 0.0817 0.108 Uiso 1 1 calc R . . C54 C 1.2208(9) 0.3415(4) 0.0531(3) 0.108(3) Uani 1 1 d . . . H54 H 1.2227 0.3354 0.0152 0.130 Uiso 1 1 calc R . . C55 C 1.1271(7) 0.3491(3) 0.0687(2) 0.089(2) Uani 1 1 d . . . H55 H 1.0618 0.3462 0.0418 0.107 Uiso 1 1 calc R . . C56 C 1.1250(5) 0.3613(3) 0.12405(19) 0.0612(16) Uani 1 1 d . . . C57 C 0.8562(5) 0.4019(4) 0.1618(2) 0.0780(19) Uani 1 1 d . . . H57 H 0.7842 0.4124 0.1613 0.094 Uiso 1 1 calc R . . C58 C 0.9321(4) 0.4004(3) 0.2082(2) 0.0512(13) Uani 1 1 d . . . C59 C 0.9148(3) 0.4135(3) 0.26437(19) 0.0436(11) Uani 1 1 d . . . C60 C 0.8555(4) 0.4750(3) 0.2797(3) 0.0588(15) Uani 1 1 d . . . H60 H 0.8266 0.5092 0.2533 0.071 Uiso 1 1 calc R . . C61 C 0.8389(4) 0.4861(3) 0.3316(3) 0.0625(15) Uani 1 1 d . . . H61 H 0.8001 0.5286 0.3415 0.075 Uiso 1 1 calc R . . C62 C 0.8784(3) 0.4357(3) 0.3699(2) 0.0485(12) Uani 1 1 d . . . H62 H 0.8658 0.4435 0.4060 0.058 Uiso 1 1 calc R . . C63 C 0.9363(3) 0.3735(2) 0.35642(19) 0.0386(10) Uani 1 1 d . . . C64 C 0.9546(3) 0.3625(2) 0.30345(18) 0.0373(10) Uani 1 1 d . . . H64 H 0.9941 0.3204 0.2938 0.045 Uiso 1 1 calc R . . C65 C 0.9749(3) 0.3177(2) 0.39787(18) 0.0375(9) Uani 1 1 d . . . C66 C 1.0389(3) 0.3510(3) 0.44885(18) 0.0408(10) Uani 1 1 d . . . H66 H 1.0595 0.4091 0.4564 0.049 Uiso 1 1 calc R . . C67 C 1.0728(3) 0.3006(3) 0.48850(18) 0.0417(10) Uani 1 1 d . . . C68 C 1.0373(3) 0.2164(3) 0.47749(18) 0.0414(10) Uani 1 1 d . . . H68 H 1.0585 0.1821 0.5053 0.050 Uiso 1 1 calc R . . C69 C 0.9721(3) 0.1800(2) 0.42773(17) 0.0333(9) Uani 1 1 d . . . C70 C 0.9435(3) 0.2325(2) 0.38707(17) 0.0330(9) Uani 1 1 d . . . C71 C 0.7679(3) 0.1885(3) 0.3312(2) 0.0478(11) Uani 1 1 d . . . H71A H 0.7492 0.1517 0.3580 0.072 Uiso 1 1 calc R . . H71B H 0.7313 0.1638 0.2941 0.072 Uiso 1 1 calc R . . H71C H 0.7444 0.2419 0.3387 0.072 Uiso 1 1 calc R . . C72 C 1.1431(4) 0.3380(3) 0.54374(19) 0.0561(13) Uani 1 1 d . . . H72A H 1.1888 0.3886 0.5390 0.084 Uiso 1 1 calc R . . H72B H 1.1895 0.2985 0.5588 0.084 Uiso 1 1 calc R . . H72C H 1.0963 0.3511 0.5690 0.084 Uiso 1 1 calc R . . C73 C 0.9282(3) 0.0905(2) 0.41926(17) 0.0361(9) Uani 1 1 d . . . C74 C 0.8928(3) 0.0513(2) 0.46181(17) 0.0369(9) Uani 1 1 d . . . H74 H 0.8981 0.0820 0.4963 0.044 Uiso 1 1 calc R . . C75 C 0.8503(3) -0.0314(3) 0.45391(18) 0.0408(10) Uani 1 1 d . . . H75 H 0.8290 -0.0574 0.4835 0.049 Uiso 1 1 calc R . . C76 C 0.8382(3) -0.0771(2) 0.40382(18) 0.0380(10) Uani 1 1 d . . . H76 H 0.8065 -0.1335 0.3985 0.046 Uiso 1 1 calc R . . C77 C 0.8728(3) -0.0398(2) 0.36121(17) 0.0327(9) Uani 1 1 d . . . C78 C 0.9189(3) 0.0427(2) 0.36927(17) 0.0343(9) Uani 1 1 d . . . H78 H 0.9445 0.0672 0.3402 0.041 Uiso 1 1 calc R . . C79 C 0.8635(3) -0.0859(2) 0.30734(17) 0.0352(9) Uani 1 1 d . . . C80 C 0.9497(4) -0.0968(3) 0.28326(19) 0.0433(10) Uani 1 1 d . . . H80 H 1.0236 -0.0763 0.2996 0.052 Uiso 1 1 calc R . . C81 C 0.7751(3) -0.1585(2) 0.22813(17) 0.0365(9) Uani 1 1 d . . . C82 C 0.6829(4) -0.1980(2) 0.18572(17) 0.0382(10) Uani 1 1 d . . . C83 C 0.6931(5) -0.2451(3) 0.1390(2) 0.0562(13) Uani 1 1 d . . . H83 H 0.7623 -0.2559 0.1337 0.067 Uiso 1 1 calc R . . C84 C 0.5996(5) -0.2755(3) 0.1007(2) 0.0672(15) Uani 1 1 d . . . H84 H 0.6038 -0.3081 0.0683 0.081 Uiso 1 1 calc R . . C85 C 0.5004(5) -0.2593(3) 0.1088(2) 0.0581(13) Uani 1 1 d . . . H85 H 0.4360 -0.2803 0.0821 0.070 Uiso 1 1 calc R . . C86 C 0.4950(4) -0.2116(2) 0.15654(18) 0.0408(10) Uani 1 1 d . . . C87 C 0.3935(4) -0.1872(3) 0.16887(18) 0.0409(10) Uani 1 1 d . . . C88 C 0.2951(4) -0.1992(3) 0.1298(2) 0.0532(12) Uani 1 1 d . . . H88 H 0.2901 -0.2266 0.0943 0.064 Uiso 1 1 calc R . . C89 C 0.2067(4) -0.1710(3) 0.1438(2) 0.0616(15) Uani 1 1 d . . . H89 H 0.1392 -0.1792 0.1180 0.074 Uiso 1 1 calc R . . C90 C 0.2154(4) -0.1303(3) 0.1953(2) 0.0560(13) Uani 1 1 d . . . H90 H 0.1548 -0.1093 0.2052 0.067 Uiso 1 1 calc R . . C91 C 0.3142(3) -0.1207(3) 0.2323(2) 0.0472(11) Uani 1 1 d . . . H91 H 0.3204 -0.0930 0.2679 0.057 Uiso 1 1 calc R . . C92 C 1.0293(5) 0.3738(3) 0.1454(2) 0.0567(14) Uani 1 1 d . . . C93 C 0.8981(4) 0.6961(3) 0.3128(2) 0.0613(14) Uani 1 1 d . . . C94 C 1.0025(5) 0.6831(4) 0.3015(3) 0.087(2) Uani 1 1 d . . . H94A H 1.0560 0.7326 0.3156 0.131 Uiso 1 1 calc R . . H94B H 0.9957 0.6721 0.2618 0.131 Uiso 1 1 calc R . . H94C H 1.0265 0.6359 0.3194 0.131 Uiso 1 1 calc R . . C95 C 0.2633(8) 0.5598(4) 0.0834(4) 0.087(2) Uani 1 1 d . . . C96 C 0.1795(7) 0.5592(5) 0.0352(3) 0.108(3) Uani 1 1 d . . . H96A H 0.1095 0.5608 0.0459 0.162 Uiso 1 1 calc R . . H96B H 0.1751 0.5089 0.0106 0.162 Uiso 1 1 calc R . . H96C H 0.1966 0.6076 0.0163 0.162 Uiso 1 1 calc R . . N14 N 0.3308(6) 0.5612(4) 0.1223(3) 0.112(2) Uani 1 1 d . . . Cl4' Cl 0.9399(8) 0.6364(6) 0.1166(4) 0.068(2) Uani 0.402(9) 1 d P A 2 O16' O 0.8857(12) 0.6178(8) 0.1596(5) 0.121(6) Uani 0.402(9) 1 d P A 2 O17 O 0.9506(6) 0.7153(4) 0.1257(4) 0.234(5) Uani 1 1 d . . . O15 O 0.8608(7) 0.6080(6) 0.0716(3) 0.247(5) Uani 1 1 d . . . O18 O 1.0180(7) 0.5992(7) 0.1242(4) 0.246(5) Uani 1 1 d . . . C97 C 0.6138(9) 0.5214(6) 0.1264(6) 0.132(4) Uani 1 1 d . . . C98 C 0.5946(10) 0.5167(5) 0.0686(4) 0.172(5) Uani 1 1 d . . . H98A H 0.5292 0.5410 0.0548 0.258 Uiso 1 1 calc R . . H98B H 0.5841 0.4588 0.0533 0.258 Uiso 1 1 calc R . . H98C H 0.6572 0.5470 0.0576 0.258 Uiso 1 1 calc R . . N15 N 0.6310(9) 0.5290(6) 0.1740(4) 0.166(4) Uani 1 1 d . . . C100 C 0.8209(5) 0.2703(4) 0.5303(3) 0.085(2) Uani 1 1 d . . . H10A H 0.7432 0.2606 0.5309 0.127 Uiso 1 1 calc R . . H10B H 0.8603 0.2374 0.5562 0.127 Uiso 1 1 calc R . . H10C H 0.8308 0.2543 0.4933 0.127 Uiso 1 1 calc R . . C99 C 0.8617(5) 0.3549(5) 0.5456(3) 0.0825(19) Uani 1 1 d . . . N16 N 0.8925(6) 0.4223(5) 0.5540(4) 0.171(4) Uani 1 1 d . . . C1S C 0.8434(10) 0.0989(9) 0.9883(4) 0.128(3) Uani 0.766(7) 1 d PDU B 1 N1S N 0.8997(8) 0.0664(7) 0.9692(4) 0.141(3) Uani 0.766(7) 1 d PDU B 1 C2S C 0.7386(9) 0.0991(8) 1.0001(4) 0.131(3) Uani 0.766(7) 1 d PDU B 1 O1R O 0.861(2) 0.1771(19) 1.0081(9) 0.131(3) Uani 0.234(7) 1 d PU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03250(15) 0.02672(14) 0.03000(16) 0.00289(11) 0.01232(12) 0.00479(11) Cd2 0.04012(17) 0.03416(16) 0.02339(15) -0.00103(11) 0.00559(12) -0.00203(12) S1 0.0401(6) 0.0582(7) 0.0352(6) 0.0162(5) 0.0013(5) 0.0040(5) S2 0.0665(8) 0.0356(6) 0.0494(7) -0.0021(5) 0.0321(6) 0.0145(5) S3 0.1145(14) 0.0918(12) 0.0501(9) 0.0256(8) -0.0385(9) -0.0064(10) S4 0.0485(7) 0.0550(7) 0.0577(8) 0.0134(6) 0.0328(6) 0.0181(5) Cl1 0.0563(7) 0.0495(7) 0.0455(7) 0.0056(5) 0.0091(5) -0.0014(5) Cl2 0.0411(6) 0.0412(6) 0.0626(8) -0.0177(5) 0.0150(5) -0.0027(4) Cl3 0.0420(7) 0.0740(8) 0.0470(7) -0.0035(6) 0.0109(5) 0.0064(6) Cl4 0.056(2) 0.092(3) 0.056(3) -0.032(2) 0.000(2) 0.013(2) O16 0.082(6) 0.135(7) 0.066(5) -0.005(5) 0.020(4) 0.021(5) N1 0.044(2) 0.0378(19) 0.035(2) -0.0006(15) 0.0117(16) -0.0005(15) N2 0.0257(17) 0.0442(19) 0.0254(18) -0.0053(14) 0.0039(13) 0.0022(14) N3 0.0310(18) 0.0408(19) 0.0268(18) 0.0031(14) 0.0038(13) 0.0029(14) N4 0.0277(16) 0.0284(16) 0.0322(18) 0.0049(13) 0.0132(13) 0.0058(12) N5 0.0294(17) 0.0348(18) 0.0356(19) 0.0102(14) 0.0134(14) 0.0081(13) N6 0.039(2) 0.0319(19) 0.053(2) 0.0102(16) 0.0205(17) 0.0053(14) N7 0.053(2) 0.0316(19) 0.051(2) -0.0071(16) 0.025(2) -0.0048(16) N8 0.086(3) 0.035(2) 0.029(2) -0.0020(15) 0.022(2) -0.0092(19) N9 0.058(3) 0.0343(19) 0.031(2) 0.0086(15) -0.0106(17) -0.0093(16) N10 0.0360(18) 0.0292(17) 0.0351(19) 0.0098(14) 0.0150(15) 0.0113(13) N11 0.045(2) 0.0334(18) 0.034(2) 0.0025(14) 0.0148(16) 0.0060(15) N12 0.0339(19) 0.041(2) 0.042(2) 0.0050(16) 0.0101(16) -0.0012(15) N13 0.065(3) 0.064(3) 0.093(4) 0.040(3) 0.024(3) 0.021(2) O1 0.0365(16) 0.0396(16) 0.0394(17) -0.0051(13) 0.0146(13) -0.0015(12) O2 0.0369(16) 0.0303(14) 0.0410(17) 0.0062(12) 0.0070(13) 0.0022(11) O3 0.058(3) 0.144(5) 0.208(6) 0.070(4) 0.017(3) 0.036(3) O4 0.119(4) 0.137(4) 0.056(3) 0.012(3) 0.036(3) 0.051(3) O5 0.336(10) 0.099(4) 0.075(4) -0.029(3) 0.037(5) -0.017(5) O6 0.068(3) 0.139(4) 0.125(4) 0.064(3) 0.022(3) 0.014(3) O7 0.090(3) 0.0360(18) 0.074(3) -0.0132(17) 0.021(2) -0.0065(17) O8 0.041(2) 0.103(3) 0.088(3) -0.018(2) 0.0207(19) 0.0093(19) O9 0.0439(19) 0.0417(18) 0.087(3) -0.0228(17) -0.0037(17) 0.0027(14) O10 0.071(2) 0.056(2) 0.062(2) -0.0088(17) 0.0259(19) -0.0110(17) O11 0.064(3) 0.245(6) 0.040(2) -0.016(3) 0.007(2) 0.035(3) O12 0.075(3) 0.110(4) 0.104(4) -0.025(3) -0.007(2) 0.044(3) O13 0.048(2) 0.178(5) 0.073(3) 0.020(3) 0.020(2) -0.018(3) O14 0.102(4) 0.071(3) 0.164(5) 0.015(3) 0.003(3) -0.013(3) C1 0.069(3) 0.043(3) 0.045(3) 0.000(2) 0.019(2) -0.002(2) C2 0.072(4) 0.041(3) 0.066(4) 0.007(2) 0.032(3) -0.005(2) C3 0.053(3) 0.035(2) 0.078(4) -0.003(2) 0.029(3) -0.003(2) C4 0.037(2) 0.044(3) 0.059(3) -0.020(2) 0.020(2) -0.0072(19) C5 0.030(2) 0.038(2) 0.039(2) -0.0099(18) 0.0109(17) -0.0014(16) C6 0.028(2) 0.050(3) 0.034(2) -0.0115(19) 0.0084(17) 0.0051(17) C7 0.041(3) 0.058(3) 0.038(3) -0.020(2) 0.005(2) 0.009(2) C8 0.049(3) 0.082(4) 0.026(2) -0.013(2) 0.001(2) 0.015(3) C9 0.044(3) 0.072(3) 0.028(2) 0.001(2) 0.0037(19) 0.015(2) C10 0.026(2) 0.054(3) 0.024(2) -0.0011(18) 0.0001(15) 0.0087(17) C11 0.027(2) 0.049(2) 0.026(2) 0.0063(18) 0.0026(16) 0.0031(17) C12 0.036(2) 0.042(2) 0.043(3) 0.013(2) 0.0064(19) 0.0031(18) C13 0.027(2) 0.036(2) 0.035(2) 0.0056(17) 0.0038(16) 0.0042(15) C14 0.029(2) 0.033(2) 0.034(2) 0.0069(16) 0.0057(16) 0.0055(15) C15 0.030(2) 0.035(2) 0.043(3) 0.0012(18) 0.0098(18) 0.0015(16) C16 0.035(2) 0.040(2) 0.041(3) 0.0038(18) 0.0175(18) -0.0006(17) C17 0.039(2) 0.040(2) 0.033(2) -0.0011(18) 0.0116(18) 0.0026(17) C18 0.033(2) 0.037(2) 0.028(2) 0.0018(16) 0.0091(16) 0.0034(16) C19 0.032(2) 0.041(2) 0.038(2) 0.0108(18) 0.0143(17) 0.0022(17) C20 0.033(2) 0.039(2) 0.028(2) 0.0044(17) 0.0082(16) 0.0000(16) C21 0.032(2) 0.037(2) 0.027(2) 0.0037(16) 0.0101(16) 0.0005(16) C22 0.034(2) 0.048(2) 0.027(2) 0.0100(18) 0.0090(17) 0.0032(17) C23 0.035(2) 0.058(3) 0.031(2) -0.002(2) 0.0065(18) -0.0082(19) C24 0.043(3) 0.050(3) 0.027(2) -0.0039(19) 0.0088(18) -0.0073(19) C25 0.036(2) 0.045(2) 0.032(2) 0.0000(18) 0.0096(18) -0.0007(18) C26 0.056(3) 0.081(4) 0.048(3) -0.023(3) 0.019(2) -0.015(3) C27 0.078(4) 0.042(3) 0.082(4) 0.005(3) 0.039(3) 0.006(2) C28 0.033(2) 0.047(2) 0.035(2) 0.0120(19) 0.0075(18) 0.0020(18) C29 0.049(3) 0.134(5) 0.039(3) 0.032(3) 0.014(2) 0.032(3) C30 0.053(3) 0.171(7) 0.049(4) 0.042(4) 0.012(3) 0.055(4) C31 0.048(3) 0.099(4) 0.055(3) 0.029(3) 0.022(2) 0.035(3) C32 0.031(2) 0.035(2) 0.038(2) 0.0151(17) 0.0120(17) 0.0062(16) C33 0.028(2) 0.032(2) 0.036(2) 0.0084(17) 0.0082(16) 0.0034(15) C34 0.028(2) 0.030(2) 0.039(2) 0.0069(17) 0.0148(17) 0.0055(15) C35 0.050(3) 0.033(2) 0.057(3) 0.010(2) 0.028(2) 0.0135(19) C36 0.034(2) 0.033(2) 0.034(2) 0.0005(17) 0.0144(17) 0.0039(16) C37 0.028(2) 0.046(2) 0.030(2) 0.0037(18) 0.0128(16) 0.0086(16) C38 0.038(2) 0.067(3) 0.032(2) 0.005(2) 0.0140(19) 0.017(2) C39 0.045(3) 0.098(4) 0.040(3) 0.028(3) 0.021(2) 0.021(3) C40 0.043(3) 0.073(3) 0.049(3) 0.036(3) 0.022(2) 0.019(2) C41 0.031(2) 0.042(2) 0.043(3) 0.0187(19) 0.0152(18) 0.0060(17) C42 0.026(2) 0.042(2) 0.060(3) 0.021(2) 0.0153(19) 0.0048(17) C43 0.037(3) 0.043(3) 0.076(4) 0.029(3) 0.010(2) 0.0042(19) C44 0.047(3) 0.034(3) 0.120(5) 0.035(3) 0.016(3) 0.005(2) C45 0.061(3) 0.026(2) 0.112(5) 0.011(3) 0.034(3) 0.009(2) C46 0.061(3) 0.032(2) 0.073(4) 0.005(2) 0.031(3) 0.006(2) C47 0.051(3) 0.031(2) 0.070(4) -0.002(2) 0.031(3) -0.0005(19) C48 0.054(3) 0.039(3) 0.120(5) 0.006(3) 0.038(3) 0.006(2) C49 0.080(5) 0.061(4) 0.171(8) 0.000(5) 0.095(5) 0.005(3) C50 0.095(5) 0.069(4) 0.111(6) -0.015(4) 0.076(5) -0.009(4) C51 0.074(4) 0.033(2) 0.072(4) -0.009(2) 0.051(3) -0.010(2) C52 0.104(5) 0.036(3) 0.045(3) -0.011(2) 0.042(3) -0.017(3) C53 0.161(7) 0.051(3) 0.065(4) -0.014(3) 0.072(5) -0.015(4) C54 0.227(11) 0.056(4) 0.034(4) -0.013(3) 0.046(5) -0.025(5) C55 0.174(8) 0.051(3) 0.028(3) -0.002(2) 0.010(4) -0.017(4) C56 0.110(5) 0.036(3) 0.024(2) 0.0007(19) 0.000(3) -0.016(3) C57 0.073(4) 0.087(4) 0.058(4) 0.031(3) -0.024(3) -0.001(3) C58 0.045(3) 0.040(2) 0.056(3) 0.019(2) -0.017(2) -0.005(2) C59 0.030(2) 0.039(2) 0.054(3) 0.017(2) -0.0091(19) -0.0029(17) C60 0.043(3) 0.040(3) 0.087(4) 0.024(3) -0.010(3) 0.010(2) C61 0.044(3) 0.040(3) 0.107(5) 0.021(3) 0.014(3) 0.014(2) C62 0.039(3) 0.034(2) 0.076(4) 0.010(2) 0.017(2) 0.0062(18) C63 0.031(2) 0.029(2) 0.056(3) 0.0096(19) 0.0085(19) 0.0032(16) C64 0.022(2) 0.033(2) 0.055(3) 0.0097(19) 0.0016(18) 0.0041(15) C65 0.033(2) 0.031(2) 0.052(3) 0.0074(19) 0.0129(19) 0.0078(16) C66 0.037(2) 0.033(2) 0.052(3) 0.0007(19) 0.012(2) 0.0027(17) C67 0.039(2) 0.042(2) 0.045(3) 0.004(2) 0.012(2) 0.0065(18) C68 0.042(2) 0.047(3) 0.040(3) 0.011(2) 0.014(2) 0.0106(19) C69 0.034(2) 0.032(2) 0.036(2) 0.0061(17) 0.0103(17) 0.0084(16) C70 0.029(2) 0.033(2) 0.037(2) 0.0065(17) 0.0083(17) 0.0042(15) C71 0.037(3) 0.049(3) 0.057(3) 0.006(2) 0.007(2) 0.0091(19) C72 0.055(3) 0.066(3) 0.042(3) -0.002(2) 0.004(2) 0.007(2) C73 0.034(2) 0.035(2) 0.043(3) 0.0126(18) 0.0088(18) 0.0126(17) C74 0.037(2) 0.041(2) 0.037(2) 0.0099(18) 0.0096(18) 0.0133(18) C75 0.038(2) 0.046(3) 0.046(3) 0.022(2) 0.0143(19) 0.0121(18) C76 0.031(2) 0.034(2) 0.051(3) 0.015(2) 0.0094(19) 0.0053(16) C77 0.029(2) 0.033(2) 0.041(2) 0.0101(17) 0.0107(17) 0.0127(16) C78 0.034(2) 0.033(2) 0.042(2) 0.0132(18) 0.0146(18) 0.0094(16) C79 0.035(2) 0.031(2) 0.044(3) 0.0147(18) 0.0122(18) 0.0096(16) C80 0.038(2) 0.042(2) 0.056(3) 0.008(2) 0.021(2) 0.0077(18) C81 0.043(2) 0.035(2) 0.041(3) 0.0103(18) 0.022(2) 0.0139(18) C82 0.052(3) 0.037(2) 0.034(2) 0.0056(18) 0.021(2) 0.0161(19) C83 0.075(4) 0.053(3) 0.049(3) -0.002(2) 0.031(3) 0.021(3) C84 0.094(5) 0.060(3) 0.054(4) -0.010(3) 0.039(3) 0.010(3) C85 0.077(4) 0.053(3) 0.038(3) -0.008(2) 0.012(3) -0.006(3) C86 0.051(3) 0.034(2) 0.036(2) 0.0021(18) 0.010(2) -0.0003(18) C87 0.045(3) 0.036(2) 0.037(3) 0.0037(18) 0.0060(19) -0.0067(18) C88 0.048(3) 0.059(3) 0.044(3) 0.009(2) -0.001(2) -0.007(2) C89 0.040(3) 0.076(4) 0.059(4) 0.019(3) -0.004(2) -0.011(2) C90 0.032(3) 0.063(3) 0.075(4) 0.021(3) 0.013(2) 0.005(2) C91 0.034(2) 0.046(3) 0.063(3) 0.007(2) 0.016(2) 0.0000(19) C92 0.079(4) 0.039(3) 0.035(3) 0.008(2) -0.015(2) -0.015(2) C93 0.051(3) 0.050(3) 0.084(4) 0.025(3) 0.010(3) 0.010(2) C94 0.052(4) 0.078(4) 0.140(6) 0.028(4) 0.026(4) 0.019(3) C95 0.121(7) 0.060(4) 0.099(6) 0.015(4) 0.066(5) 0.010(4) C96 0.154(8) 0.106(6) 0.073(5) 0.026(4) 0.041(5) 0.017(5) N14 0.116(6) 0.103(5) 0.125(6) 0.029(5) 0.041(5) 0.011(4) Cl4' 0.055(3) 0.062(3) 0.076(6) -0.015(4) -0.004(4) 0.018(2) O16' 0.161(14) 0.117(11) 0.091(10) 0.017(8) 0.046(9) 0.008(9) O17 0.191(7) 0.108(5) 0.433(14) -0.088(7) 0.208(9) -0.019(5) O15 0.268(10) 0.294(10) 0.085(5) 0.003(5) -0.048(5) -0.162(8) O18 0.198(8) 0.379(13) 0.256(10) 0.177(10) 0.119(7) 0.197(9) C97 0.120(8) 0.086(6) 0.174(11) 0.046(8) -0.017(9) 0.015(5) C98 0.273(15) 0.062(5) 0.153(10) -0.015(6) -0.007(10) 0.020(7) N15 0.185(9) 0.133(7) 0.186(10) 0.039(8) 0.013(8) 0.073(6) C100 0.082(4) 0.084(5) 0.115(6) 0.049(4) 0.052(4) 0.037(4) C99 0.054(4) 0.078(5) 0.125(6) 0.005(4) 0.037(4) 0.022(3) N16 0.087(5) 0.099(5) 0.330(13) -0.042(7) 0.079(6) 0.004(4) C1S 0.159(6) 0.197(8) 0.075(5) 0.074(5) 0.052(4) 0.120(6) N1S 0.165(7) 0.212(8) 0.091(5) 0.063(5) 0.060(4) 0.110(6) C2S 0.165(7) 0.190(8) 0.091(5) 0.080(5) 0.068(5) 0.116(6) O1R 0.161(7) 0.195(8) 0.078(5) 0.072(6) 0.044(5) 0.123(6) _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 N11 2.293(3) . ? Cd1 N5 2.312(3) . ? Cd1 N4 2.337(3) . ? Cd1 N12 2.385(3) . ? Cd1 N6 2.386(3) . ? Cd1 N10 2.421(3) . ? Cd2 N2 2.311(3) . ? Cd2 N8 2.327(4) . ? Cd2 N1 2.352(3) . ? Cd2 N9 2.356(4) . ? Cd2 N7 2.386(4) . ? Cd2 N3 2.395(3) . ? S1 C12 1.701(5) . ? S1 C11 1.704(4) . ? S2 C36 1.702(4) . ? S2 C35 1.705(5) . ? S3 C57 1.685(7) . ? S3 C92 1.717(5) . ? S4 C80 1.695(5) . ? S4 C81 1.710(4) . ? Cl1 O5 1.363(5) . ? Cl1 O3 1.401(5) . ? Cl1 O4 1.425(4) . ? Cl1 O6 1.432(4) . ? Cl2 O8 1.421(4) . ? Cl2 O10 1.432(4) . ? Cl2 O7 1.432(4) . ? Cl2 O9 1.441(3) . ? Cl3 O13 1.401(4) . ? Cl3 O11 1.410(4) . ? Cl3 O14 1.423(5) . ? Cl3 O12 1.424(4) . ? Cl4 O17 1.267(9) . ? Cl4 O15 1.295(9) . ? Cl4 O18 1.373(9) . ? Cl4 O16 1.438(10) . ? N1 C1 1.332(5) . ? N1 C5 1.342(5) . ? N2 C6 1.335(5) . ? N2 C10 1.335(5) . ? N3 C11 1.314(5) . ? N3 C13 1.386(5) . ? N4 C36 1.302(5) . ? N4 C34 1.382(4) . ? N5 C37 1.341(5) . ? N5 C41 1.349(5) . ? N6 C42 1.342(5) . ? N6 C46 1.344(6) . ? N7 C47 1.341(6) . ? N7 C51 1.354(6) . ? N8 C52 1.314(7) . ? N8 C56 1.335(6) . ? N9 C92 1.320(6) . ? N9 C58 1.384(6) . ? N10 C81 1.320(5) . ? N10 C79 1.385(5) . ? N11 C82 1.336(5) . ? N11 C86 1.336(5) . ? N12 C91 1.334(5) . ? N12 C87 1.352(5) . ? N13 C93 1.133(6) . ? O1 C21 1.383(5) . ? O1 C27 1.419(5) . ? O2 C70 1.388(5) . ? O2 C71 1.430(5) . ? C1 C2 1.387(6) . ? C1 H1 0.9500 . ? C2 C3 1.375(7) . ? C2 H2 0.9500 . ? C3 C4 1.377(7) . ? C3 H3 0.9500 . ? C4 C5 1.377(6) . ? C4 H4 0.9500 . ? C5 C6 1.494(6) . ? C6 C7 1.381(6) . ? C7 C8 1.370(7) . ? C7 H7 0.9500 . ? C8 C9 1.370(7) . ? C8 H8 0.9500 . ? C9 C10 1.392(6) . ? C9 H9 0.9500 . ? C10 C11 1.467(6) . ? C12 C13 1.363(5) . ? C12 H12 0.9500 . ? C13 C14 1.477(5) . ? C14 C15 1.392(5) . ? C14 C19 1.393(5) . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.385(5) . ? C16 H16 0.9500 . ? C17 C18 1.398(5) . ? C17 H17 0.9500 . ? C18 C19 1.389(5) . ? C18 C20 1.483(5) . ? C19 H19 0.9500 . ? C20 C25 1.389(5) . ? C20 C21 1.402(5) . ? C21 C22 1.404(5) . ? C22 C23 1.378(6) . ? C22 C28 1.486(6) . ? C23 C24 1.394(6) . ? C23 H23 0.9500 . ? C24 C25 1.395(5) . ? C24 C26 1.517(6) . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.377(6) . ? C28 C33 1.396(5) . ? C29 C30 1.386(7) . ? C29 H29 0.9500 . ? C30 C31 1.374(7) . ? C30 H30 0.9500 . ? C31 C32 1.393(6) . ? C31 H31 0.9500 . ? C32 C33 1.391(5) . ? C32 C34 1.461(5) . ? C33 H33 0.9500 . ? C34 C35 1.360(5) . ? C35 H35 0.9500 . ? C36 C37 1.471(5) . ? C37 C38 1.380(6) . ? C38 C39 1.374(6) . ? C38 H38 0.9500 . ? C39 C40 1.386(7) . ? C39 H39 0.9500 . ? C40 C41 1.384(6) . ? C40 H40 0.9500 . ? C41 C42 1.476(6) . ? C42 C43 1.402(6) . ? C43 C44 1.366(7) . ? C43 H43 0.9500 . ? C44 C45 1.362(8) . ? C44 H44 0.9500 . ? C45 C46 1.386(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.384(6) . ? C47 H47 0.9500 . ? C48 C49 1.384(9) . ? C48 H48 0.9500 . ? C49 C50 1.362(10) . ? C49 H49 0.9500 . ? C50 C51 1.381(8) . ? C50 H50 0.9500 . ? C51 C52 1.484(8) . ? C52 C53 1.420(7) . ? C53 C54 1.365(11) . ? C53 H53 0.9500 . ? C54 C55 1.341(11) . ? C54 H54 0.9500 . ? C55 C56 1.389(7) . ? C55 H55 0.9500 . ? C56 C92 1.451(8) . ? C57 C58 1.355(6) . ? C57 H57 0.9500 . ? C58 C59 1.469(7) . ? C59 C64 1.399(5) . ? C59 C60 1.410(7) . ? C60 C61 1.358(7) . ? C60 H60 0.9500 . ? C61 C62 1.377(6) . ? C61 H61 0.9500 . ? C62 C63 1.392(6) . ? C62 H62 0.9500 . ? C63 C64 1.392(6) . ? C63 C65 1.491(5) . ? C64 H64 0.9500 . ? C65 C66 1.394(6) . ? C65 C70 1.396(5) . ? C66 C67 1.381(6) . ? C66 H66 0.9500 . ? C67 C68 1.387(6) . ? C67 C72 1.520(6) . ? C68 C69 1.390(6) . ? C68 H68 0.9500 . ? C69 C70 1.409(5) . ? C69 C73 1.487(5) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C78 1.398(6) . ? C73 C74 1.406(5) . ? C74 C75 1.379(6) . ? C74 H74 0.9500 . ? C75 C76 1.378(6) . ? C75 H75 0.9500 . ? C76 C77 1.388(5) . ? C76 H76 0.9500 . ? C77 C78 1.387(5) . ? C77 C79 1.468(6) . ? C78 H78 0.9500 . ? C79 C80 1.374(5) . ? C80 H80 0.9500 . ? C81 C82 1.453(6) . ? C82 C83 1.386(6) . ? C83 C84 1.375(7) . ? C83 H83 0.9500 . ? C84 C85 1.369(7) . ? C84 H84 0.9500 . ? C85 C86 1.395(6) . ? C85 H85 0.9500 . ? C86 C87 1.479(6) . ? C87 C88 1.402(6) . ? C88 C89 1.364(7) . ? C88 H88 0.9500 . ? C89 C90 1.382(7) . ? C89 H89 0.9500 . ? C90 C91 1.382(6) . ? C90 H90 0.9500 . ? C91 H91 0.9500 . ? C93 C94 1.447(8) . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 0.9800 . ? C95 N14 1.156(9) . ? C95 C96 1.438(10) . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? Cl4' O18 1.222(11) . ? Cl4' O17 1.283(11) . ? Cl4' O15 1.354(11) . ? Cl4' O16' 1.420(16) . ? C97 N15 1.161(13) . ? C97 C98 1.411(13) . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? C100 C99 1.413(9) . ? C100 H10A 0.9800 . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C99 N16 1.115(8) . ? C1S N1S 1.104(10) . ? C1S C2S 1.417(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Cd1 N5 161.81(11) . . ? N11 Cd1 N4 127.70(11) . . ? N5 Cd1 N4 70.43(11) . . ? N11 Cd1 N12 69.51(12) . . ? N5 Cd1 N12 113.76(11) . . ? N4 Cd1 N12 88.61(11) . . ? N11 Cd1 N6 92.71(12) . . ? N5 Cd1 N6 69.20(12) . . ? N4 Cd1 N6 138.42(11) . . ? N12 Cd1 N6 98.62(12) . . ? N11 Cd1 N10 70.81(12) . . ? N5 Cd1 N10 108.51(11) . . ? N4 Cd1 N10 104.55(10) . . ? N12 Cd1 N10 137.71(11) . . ? N6 Cd1 N10 97.23(10) . . ? N2 Cd2 N8 160.74(13) . . ? N2 Cd2 N1 69.49(12) . . ? N8 Cd2 N1 102.80(12) . . ? N2 Cd2 N9 125.31(13) . . ? N8 Cd2 N9 71.13(15) . . ? N1 Cd2 N9 91.26(12) . . ? N2 Cd2 N7 94.29(12) . . ? N8 Cd2 N7 68.70(15) . . ? N1 Cd2 N7 97.57(12) . . ? N9 Cd2 N7 139.83(14) . . ? N2 Cd2 N3 70.28(11) . . ? N8 Cd2 N3 116.82(12) . . ? N1 Cd2 N3 139.52(12) . . ? N9 Cd2 N3 108.43(11) . . ? N7 Cd2 N3 89.67(11) . . ? C12 S1 C11 90.1(2) . . ? C36 S2 C35 89.6(2) . . ? C57 S3 C92 90.1(3) . . ? C80 S4 C81 90.1(2) . . ? O5 Cl1 O3 112.2(4) . . ? O5 Cl1 O4 108.3(3) . . ? O3 Cl1 O4 113.0(3) . . ? O5 Cl1 O6 106.8(4) . . ? O3 Cl1 O6 109.6(3) . . ? O4 Cl1 O6 106.8(3) . . ? O8 Cl2 O10 109.6(2) . . ? O8 Cl2 O7 110.2(2) . . ? O10 Cl2 O7 110.1(2) . . ? O8 Cl2 O9 109.1(2) . . ? O10 Cl2 O9 108.9(2) . . ? O7 Cl2 O9 109.0(2) . . ? O13 Cl3 O11 108.1(3) . . ? O13 Cl3 O14 107.5(3) . . ? O11 Cl3 O14 112.3(4) . . ? O13 Cl3 O12 111.0(3) . . ? O11 Cl3 O12 110.2(3) . . ? O14 Cl3 O12 107.8(3) . . ? O17 Cl4 O15 115.9(8) . . ? O17 Cl4 O18 112.1(8) . . ? O15 Cl4 O18 110.1(9) . . ? O17 Cl4 O16 99.3(7) . . ? O15 Cl4 O16 110.6(6) . . ? O18 Cl4 O16 108.1(6) . . ? C1 N1 C5 118.4(4) . . ? C1 N1 Cd2 123.1(3) . . ? C5 N1 Cd2 118.5(3) . . ? C6 N2 C10 120.3(3) . . ? C6 N2 Cd2 119.9(3) . . ? C10 N2 Cd2 119.4(3) . . ? C11 N3 C13 111.2(3) . . ? C11 N3 Cd2 114.0(3) . . ? C13 N3 Cd2 134.8(3) . . ? C36 N4 C34 112.1(3) . . ? C36 N4 Cd1 115.5(2) . . ? C34 N4 Cd1 131.6(3) . . ? C37 N5 C41 120.9(3) . . ? C37 N5 Cd1 118.5(2) . . ? C41 N5 Cd1 119.9(3) . . ? C42 N6 C46 119.0(4) . . ? C42 N6 Cd1 117.2(3) . . ? C46 N6 Cd1 123.6(3) . . ? C47 N7 C51 119.0(4) . . ? C47 N7 Cd2 123.0(3) . . ? C51 N7 Cd2 117.7(3) . . ? C52 N8 C56 120.7(5) . . ? C52 N8 Cd2 121.3(4) . . ? C56 N8 Cd2 118.0(4) . . ? C92 N9 C58 111.4(4) . . ? C92 N9 Cd2 113.5(4) . . ? C58 N9 Cd2 134.7(3) . . ? C81 N10 C79 111.4(3) . . ? C81 N10 Cd1 111.1(3) . . ? C79 N10 Cd1 137.5(3) . . ? C82 N11 C86 120.9(4) . . ? C82 N11 Cd1 118.1(3) . . ? C86 N11 Cd1 119.6(3) . . ? C91 N12 C87 119.3(4) . . ? C91 N12 Cd1 124.3(3) . . ? C87 N12 Cd1 116.4(3) . . ? C21 O1 C27 113.8(3) . . ? C70 O2 C71 114.4(3) . . ? N1 C1 C2 123.4(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 117.6(5) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 119.5(4) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.6(4) . . ? N1 C5 C6 115.7(3) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C7 120.6(4) . . ? N2 C6 C5 115.8(3) . . ? C7 C6 C5 123.5(4) . . ? C8 C7 C6 119.5(4) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 118.3(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 121.3(4) . . ? N2 C10 C11 114.9(3) . . ? C9 C10 C11 123.7(4) . . ? N3 C11 C10 121.1(4) . . ? N3 C11 S1 114.3(3) . . ? C10 C11 S1 124.6(3) . . ? C13 C12 S1 110.7(3) . . ? C13 C12 H12 124.6 . . ? S1 C12 H12 124.6 . . ? C12 C13 N3 113.8(4) . . ? C12 C13 C14 126.7(4) . . ? N3 C13 C14 119.5(3) . . ? C15 C14 C19 119.5(4) . . ? C15 C14 C13 120.4(3) . . ? C19 C14 C13 120.1(3) . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 120.9(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 118.3(4) . . ? C19 C18 C20 122.1(3) . . ? C17 C18 C20 119.4(4) . . ? C18 C19 C14 120.9(4) . . ? C18 C19 H19 119.5 . . ? C14 C19 H19 119.5 . . ? C25 C20 C21 118.6(4) . . ? C25 C20 C18 120.7(4) . . ? C21 C20 C18 120.7(4) . . ? O1 C21 C20 119.9(3) . . ? O1 C21 C22 119.7(3) . . ? C20 C21 C22 120.4(4) . . ? C23 C22 C21 119.3(4) . . ? C23 C22 C28 121.0(4) . . ? C21 C22 C28 119.6(4) . . ? C22 C23 C24 121.5(4) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C24 C25 118.3(4) . . ? C23 C24 C26 121.9(4) . . ? C25 C24 C26 119.8(4) . . ? C20 C25 C24 121.8(4) . . ? C20 C25 H25 119.1 . . ? C24 C25 H25 119.1 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.1(4) . . ? C29 C28 C22 121.5(4) . . ? C33 C28 C22 120.4(4) . . ? C28 C29 C30 120.8(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 120.8(5) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 119.9(4) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 118.5(4) . . ? C33 C32 C34 119.8(3) . . ? C31 C32 C34 121.6(4) . . ? C32 C33 C28 121.9(4) . . ? C32 C33 H33 119.1 . . ? C28 C33 H33 119.1 . . ? C35 C34 N4 113.0(4) . . ? C35 C34 C32 128.5(4) . . ? N4 C34 C32 118.5(3) . . ? C34 C35 S2 111.1(3) . . ? C34 C35 H35 124.5 . . ? S2 C35 H35 124.5 . . ? N4 C36 C37 120.9(3) . . ? N4 C36 S2 114.2(3) . . ? C37 C36 S2 124.5(3) . . ? N5 C37 C38 121.6(4) . . ? N5 C37 C36 113.3(3) . . ? C38 C37 C36 125.1(4) . . ? C39 C38 C37 118.1(5) . . ? C39 C38 H38 120.9 . . ? C37 C38 H38 120.9 . . ? C38 C39 C40 120.2(4) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 119.5(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? N5 C41 C40 119.5(4) . . ? N5 C41 C42 115.7(4) . . ? C40 C41 C42 124.7(4) . . ? N6 C42 C43 120.7(4) . . ? N6 C42 C41 116.8(3) . . ? C43 C42 C41 122.4(4) . . ? C44 C43 C42 119.6(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 119.5(4) . . ? C45 C44 H44 120.3 . . ? C43 C44 H44 120.3 . . ? C44 C45 C46 119.3(5) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? N6 C46 C45 121.9(5) . . ? N6 C46 H46 119.0 . . ? C45 C46 H46 119.0 . . ? N7 C47 C48 122.7(5) . . ? N7 C47 H47 118.6 . . ? C48 C47 H47 118.6 . . ? C47 C48 C49 117.6(6) . . ? C47 C48 H48 121.2 . . ? C49 C48 H48 121.2 . . ? C50 C49 C48 120.0(6) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.1(6) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? N7 C51 C50 120.5(6) . . ? N7 C51 C52 116.0(4) . . ? C50 C51 C52 123.5(5) . . ? N8 C52 C53 120.4(6) . . ? N8 C52 C51 116.2(4) . . ? C53 C52 C51 123.4(6) . . ? C54 C53 C52 118.7(7) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C55 C54 C53 119.5(6) . . ? C55 C54 H54 120.2 . . ? C53 C54 H54 120.2 . . ? C54 C55 C56 120.3(7) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? N8 C56 C55 120.4(6) . . ? N8 C56 C92 114.8(4) . . ? C55 C56 C92 124.8(6) . . ? C58 C57 S3 111.6(5) . . ? C58 C57 H57 124.2 . . ? S3 C57 H57 124.2 . . ? C57 C58 N9 113.6(5) . . ? C57 C58 C59 125.3(5) . . ? N9 C58 C59 121.1(4) . . ? C64 C59 C60 118.6(5) . . ? C64 C59 C58 119.8(4) . . ? C60 C59 C58 121.5(4) . . ? C61 C60 C59 121.0(4) . . ? C61 C60 H60 119.5 . . ? C59 C60 H60 119.5 . . ? C60 C61 C62 120.0(5) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 121.0(5) . . ? C61 C62 H62 119.5 . . ? C63 C62 H62 119.5 . . ? C62 C63 C64 119.3(4) . . ? C62 C63 C65 120.1(4) . . ? C64 C63 C65 120.6(4) . . ? C63 C64 C59 120.1(4) . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C66 C65 C70 119.5(4) . . ? C66 C65 C63 119.9(4) . . ? C70 C65 C63 120.6(4) . . ? C67 C66 C65 120.9(4) . . ? C67 C66 H66 119.6 . . ? C65 C66 H66 119.6 . . ? C66 C67 C68 118.5(4) . . ? C66 C67 C72 120.1(4) . . ? C68 C67 C72 121.3(4) . . ? C67 C68 C69 123.1(4) . . ? C67 C68 H68 118.5 . . ? C69 C68 H68 118.5 . . ? C68 C69 C70 117.1(4) . . ? C68 C69 C73 121.3(4) . . ? C70 C69 C73 121.5(4) . . ? O2 C70 C65 118.8(3) . . ? O2 C70 C69 120.4(3) . . ? C65 C70 C69 120.9(4) . . ? O2 C71 H71A 109.5 . . ? O2 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? O2 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C67 C72 H72A 109.5 . . ? C67 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C67 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C78 C73 C74 117.7(4) . . ? C78 C73 C69 122.0(4) . . ? C74 C73 C69 120.3(4) . . ? C75 C74 C73 120.6(4) . . ? C75 C74 H74 119.7 . . ? C73 C74 H74 119.7 . . ? C76 C75 C74 121.1(4) . . ? C76 C75 H75 119.5 . . ? C74 C75 H75 119.5 . . ? C75 C76 C77 119.4(4) . . ? C75 C76 H76 120.3 . . ? C77 C76 H76 120.3 . . ? C78 C77 C76 120.0(4) . . ? C78 C77 C79 118.4(3) . . ? C76 C77 C79 121.6(4) . . ? C77 C78 C73 121.3(4) . . ? C77 C78 H78 119.4 . . ? C73 C78 H78 119.4 . . ? C80 C79 N10 113.3(4) . . ? C80 C79 C77 124.7(4) . . ? N10 C79 C77 122.0(3) . . ? C79 C80 S4 111.2(3) . . ? C79 C80 H80 124.4 . . ? S4 C80 H80 124.4 . . ? N10 C81 C82 122.6(4) . . ? N10 C81 S4 114.1(3) . . ? C82 C81 S4 123.2(3) . . ? N11 C82 C83 121.8(4) . . ? N11 C82 C81 114.7(4) . . ? C83 C82 C81 123.4(4) . . ? C84 C83 C82 117.6(5) . . ? C84 C83 H83 121.2 . . ? C82 C83 H83 121.2 . . ? C85 C84 C83 120.7(5) . . ? C85 C84 H84 119.7 . . ? C83 C84 H84 119.7 . . ? C84 C85 C86 119.2(5) . . ? C84 C85 H85 120.4 . . ? C86 C85 H85 120.4 . . ? N11 C86 C85 119.8(4) . . ? N11 C86 C87 115.9(4) . . ? C85 C86 C87 124.3(4) . . ? N12 C87 C88 121.0(4) . . ? N12 C87 C86 116.3(4) . . ? C88 C87 C86 122.6(4) . . ? C89 C88 C87 118.8(5) . . ? C89 C88 H88 120.6 . . ? C87 C88 H88 120.6 . . ? C88 C89 C90 120.0(5) . . ? C88 C89 H89 120.0 . . ? C90 C89 H89 120.0 . . ? C91 C90 C89 118.6(5) . . ? C91 C90 H90 120.7 . . ? C89 C90 H90 120.7 . . ? N12 C91 C90 122.2(5) . . ? N12 C91 H91 118.9 . . ? C90 C91 H91 118.9 . . ? N9 C92 C56 122.5(4) . . ? N9 C92 S3 113.3(5) . . ? C56 C92 S3 124.1(4) . . ? N13 C93 C94 178.2(7) . . ? C93 C94 H94A 109.5 . . ? C93 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C93 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? N14 C95 C96 179.2(9) . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? O18 Cl4' O17 122.0(10) . . ? O18 Cl4' O15 116.1(10) . . ? O17 Cl4' O15 110.8(9) . . ? O18 Cl4' O16' 104.5(9) . . ? O17 Cl4' O16' 97.3(9) . . ? O15 Cl4' O16' 101.6(9) . . ? Cl4 O17 Cl4' 28.3(4) . . ? Cl4 O15 Cl4' 27.1(4) . . ? Cl4' O18 Cl4 27.0(4) . . ? N15 C97 C98 177.0(12) . . ? C97 C98 H98A 109.5 . . ? C97 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C97 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C99 C100 H10A 109.5 . . ? C99 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N16 C99 C100 175.3(10) . . ? N1S C1S C2S 148.9(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.073 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 945476' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_chris_fe_0ma _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H56 Fe2 N12 S4, 4(Cl O4), 2(C H3 N O2)' _chemical_formula_sum 'C90 H62 Cl4 Fe2 N14 O20 S4' _chemical_formula_weight 2041.28 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 45.5093(11) _cell_length_b 22.2219(5) _cell_length_c 17.1211(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17314.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8079 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.42 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8352 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7408 _exptl_absorpt_correction_T_max 0.8829 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 46105 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.42 _reflns_number_total 10977 _reflns_number_gt 6702 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. least-squares restraints used in the refinement DELU 0.003 0.006 C40 C41 C42 C43 C44 simu 0.003 0.006 C40 C41 C42 C43 C44 ISOR 0.1 C43 ; _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^)+(0.0708P)^2^+34.5010P] 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 10977 _refine_ls_number_parameters 620 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1586 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _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 Fe1 Fe 0.136448(10) 0.37231(2) 0.19925(3) 0.02611(13) Uani 1 1 d . . . Cl1 Cl 0.5000 0.13307(6) 0.21547(7) 0.0326(3) Uani 1 2 d S . . Cl2 Cl 0.216468(19) 0.15195(4) 0.08855(5) 0.0333(2) Uani 1 1 d . . . Cl3 Cl 0.08049(4) 0.5000 0.5000 0.0561(4) Uani 1 2 d S . . S1 S 0.08008(2) 0.54130(5) 0.24980(6) 0.0451(3) Uani 1 1 d . . . S2 S 0.18647(2) 0.29602(4) -0.01150(5) 0.0425(3) Uani 1 1 d . . . N1 N 0.09962(6) 0.33507(13) 0.26874(16) 0.0312(7) Uani 1 1 d . . . N2 N 0.11970(6) 0.29624(13) 0.13591(16) 0.0307(6) Uani 1 1 d . . . N3 N 0.16419(6) 0.36351(12) 0.09311(15) 0.0280(6) Uani 1 1 d . . . N4 N 0.17607(6) 0.33579(13) 0.25749(15) 0.0282(6) Uani 1 1 d . . . N5 N 0.14863(6) 0.43639(13) 0.28690(14) 0.0265(6) Uani 1 1 d . . . N6 N 0.10519(6) 0.45123(13) 0.18562(15) 0.0289(6) Uani 1 1 d . . . N7 N 1.0000 0.4234(3) 0.3056(4) 0.0719(17) Uani 1 2 d S . . N8 N 0.0000 0.3307(3) 0.5332(3) 0.0657(16) Uani 1 2 d S . . O1 O 0.5000 0.18605(16) 0.1679(2) 0.0425(9) Uani 1 2 d S . . O2 O 0.5000 0.08058(17) 0.1666(2) 0.0479(10) Uani 1 2 d S . . O3 O 0.52590(6) 0.13216(13) 0.26302(16) 0.0504(7) Uani 1 1 d . . . O4 O 0.18601(6) 0.16764(13) 0.0853(2) 0.0572(8) Uani 1 1 d . . . O5 O 0.22462(8) 0.14198(16) 0.16780(16) 0.0697(10) Uani 1 1 d . . . O6 O 0.22185(6) 0.09831(12) 0.04435(14) 0.0425(6) Uani 1 1 d . . . O7 O 0.23377(6) 0.19980(13) 0.05629(19) 0.0553(8) Uani 1 1 d . . . O8 O 0.09965(12) 0.54898(18) 0.5121(3) 0.1172(17) Uani 1 1 d . . . O9 O 0.06612(17) 0.5042(4) 0.4338(3) 0.214(4) Uani 1 1 d . . . O10 O 1.0000 0.3867(3) 0.3628(4) 0.099(2) Uani 1 2 d S . . O11 O 1.0000 0.4083(4) 0.2405(4) 0.141(3) Uani 1 2 d S . . O12 O 0.02362(9) 0.3053(2) 0.5270(3) 0.0993(14) Uani 1 1 d . . . C1 C 0.08997(8) 0.35779(17) 0.3363(2) 0.0384(9) Uani 1 1 d . . . H1 H 0.1014 0.3882 0.3608 0.046 Uiso 1 1 calc R . . C2 C 0.06436(9) 0.33962(19) 0.3724(2) 0.0452(10) Uani 1 1 d . . . H2 H 0.0583 0.3571 0.4204 0.054 Uiso 1 1 calc R . . C3 C 0.04793(9) 0.29548(19) 0.3368(3) 0.0495(11) Uani 1 1 d . . . H3 H 0.0302 0.2818 0.3603 0.059 Uiso 1 1 calc R . . C4 C 0.05715(9) 0.27143(18) 0.2677(3) 0.0456(10) Uani 1 1 d . . . H4 H 0.0458 0.2413 0.2423 0.055 Uiso 1 1 calc R . . C5 C 0.08334(8) 0.29153(16) 0.2347(2) 0.0349(8) Uani 1 1 d . . . C6 C 0.09603(8) 0.26661(16) 0.1622(2) 0.0355(8) Uani 1 1 d . . . C7 C 0.08589(9) 0.21504(18) 0.1244(3) 0.0465(10) Uani 1 1 d . . . H7 H 0.0689 0.1945 0.1425 0.056 Uiso 1 1 calc R . . C8 C 0.10110(10) 0.19447(18) 0.0600(3) 0.0505(11) Uani 1 1 d . . . H8 H 0.0948 0.1589 0.0342 0.061 Uiso 1 1 calc R . . C9 C 0.12518(10) 0.22485(17) 0.0331(2) 0.0429(10) Uani 1 1 d . . . H9 H 0.1356 0.2109 -0.0115 0.051 Uiso 1 1 calc R . . C10 C 0.13401(8) 0.27647(16) 0.0722(2) 0.0332(8) Uani 1 1 d . . . C11 C 0.15948(8) 0.31365(16) 0.05354(18) 0.0316(8) Uani 1 1 d . . . C12 C 0.20522(9) 0.35890(17) 0.0155(2) 0.0386(9) Uani 1 1 d . . . H12 H 0.2236 0.3709 -0.0058 0.046 Uiso 1 1 calc R . . C13 C 0.19039(8) 0.38979(16) 0.07174(19) 0.0312(8) Uani 1 1 d . . . C14 C 0.19886(8) 0.44735(16) 0.10679(18) 0.0299(7) Uani 1 1 d . . . C15 C 0.22798(8) 0.46126(18) 0.1244(2) 0.0397(9) Uani 1 1 d . . . H15 H 0.2431 0.4326 0.1152 0.048 Uiso 1 1 calc R . . C16 C 0.23474(8) 0.51711(19) 0.1553(2) 0.0422(9) Uani 1 1 d . . . H16 H 0.2546 0.5263 0.1680 0.051 Uiso 1 1 calc R . . C17 C 0.21310(8) 0.55972(17) 0.1680(2) 0.0351(8) Uani 1 1 d . . . H17 H 0.2181 0.5978 0.1893 0.042 Uiso 1 1 calc R . . C18 C 0.18397(8) 0.54689(15) 0.14957(18) 0.0289(7) Uani 1 1 d . . . C19 C 0.17738(7) 0.48995(15) 0.12076(18) 0.0282(7) Uani 1 1 d . . . H19 H 0.1575 0.4800 0.1104 0.034 Uiso 1 1 calc R . . C20 C 0.16049(8) 0.59287(16) 0.15379(19) 0.0301(7) Uani 1 1 d . . . C21 C 0.16060(8) 0.63988(17) 0.2073(2) 0.0378(9) Uani 1 1 d . . . H21 H 0.1758 0.6429 0.2450 0.045 Uiso 1 1 calc R . . C22 C 0.13832(9) 0.68224(19) 0.2051(2) 0.0456(10) Uani 1 1 d . . . H22 H 0.1385 0.7143 0.2417 0.055 Uiso 1 1 calc R . . C23 C 0.11585(9) 0.67915(19) 0.1513(2) 0.0427(9) Uani 1 1 d . . . H23 H 0.1010 0.7093 0.1505 0.051 Uiso 1 1 calc R . . C24 C 0.11491(8) 0.63198(17) 0.0983(2) 0.0327(8) Uani 1 1 d . . . C25 C 0.13734(8) 0.59022(16) 0.10033(19) 0.0306(8) Uani 1 1 d . . . H25 H 0.1370 0.5582 0.0636 0.037 Uiso 1 1 calc R . . C26 C 0.18979(8) 0.28426(16) 0.2394(2) 0.0325(8) Uani 1 1 d . . . H26 H 0.1831 0.2622 0.1954 0.039 Uiso 1 1 calc R . . C27 C 0.21317(8) 0.26160(18) 0.2814(2) 0.0380(9) Uani 1 1 d . . . H27 H 0.2225 0.2253 0.2659 0.046 Uiso 1 1 calc R . . C28 C 0.22264(8) 0.29281(18) 0.3463(2) 0.0380(9) Uani 1 1 d . . . H28 H 0.2383 0.2776 0.3774 0.046 Uiso 1 1 calc R . . C29 C 0.20912(8) 0.34642(17) 0.3654(2) 0.0340(8) Uani 1 1 d . . . H29 H 0.2154 0.3688 0.4097 0.041 Uiso 1 1 calc R . . C30 C 0.18635(7) 0.36718(16) 0.31967(18) 0.0278(7) Uani 1 1 d . . . C31 C 0.17170(7) 0.42567(16) 0.33345(18) 0.0284(7) Uani 1 1 d . . . C32 C 0.18051(8) 0.46749(17) 0.3891(2) 0.0363(9) Uani 1 1 d . . . H32 H 0.1970 0.4597 0.4217 0.044 Uiso 1 1 calc R . . C33 C 0.16499(9) 0.52054(17) 0.3962(2) 0.0404(9) Uani 1 1 d . . . H33 H 0.1709 0.5498 0.4335 0.049 Uiso 1 1 calc R . . C34 C 0.14098(9) 0.53107(17) 0.3492(2) 0.0370(9) Uani 1 1 d . . . H34 H 0.1300 0.5672 0.3539 0.044 Uiso 1 1 calc R . . C35 C 0.13329(8) 0.48783(16) 0.29510(18) 0.0311(8) Uani 1 1 d . . . C36 C 0.10815(8) 0.49087(16) 0.24199(19) 0.0319(8) Uani 1 1 d . . . C37 C 0.06305(9) 0.5072(2) 0.1728(2) 0.0481(11) Uani 1 1 d . . . H37 H 0.0447 0.5195 0.1518 0.058 Uiso 1 1 calc R . . C38 C 0.07929(8) 0.46005(18) 0.1455(2) 0.0357(8) Uani 1 1 d . . . C39 C 0.07266(8) 0.4216(2) 0.0779(2) 0.0422(10) Uani 1 1 d . . . C40 C 0.09489(8) 0.40918(17) 0.02630(19) 0.0345(7) Uani 1 1 d U . . H40 H 0.1140 0.4239 0.0375 0.041 Uiso 1 1 calc R . . C41 C 0.09072(8) 0.37601(19) -0.0416(2) 0.0393(8) Uani 1 1 d U . . C42 C 0.06318(10) 0.3524(3) -0.0550(3) 0.0748(10) Uani 1 1 d U . . H42 H 0.0597 0.3289 -0.1005 0.090 Uiso 1 1 calc R . . C43 C 0.04083(11) 0.3626(3) -0.0030(3) 0.0900(12) Uani 1 1 d U . . H43 H 0.0221 0.3452 -0.0124 0.108 Uiso 1 1 calc R . . C44 C 0.04496(10) 0.3982(3) 0.0637(3) 0.0899(14) Uani 1 1 d U . . H44 H 0.0291 0.4060 0.0984 0.108 Uiso 1 1 calc R . . C45 C 1.0000 0.4838(3) 0.3299(4) 0.075(2) Uani 1 2 d S . . H45A H 1.0157 0.4900 0.3681 0.113 Uiso 0.50 1 calc PR . . H45B H 0.9810 0.4934 0.3539 0.113 Uiso 0.50 1 calc PR . . H45C H 1.0032 0.5099 0.2846 0.113 Uiso 0.50 1 calc PR . . C46 C 0.0000 0.3952(4) 0.5508(4) 0.081(2) Uani 1 2 d S . . H46A H 0.0202 0.4102 0.5506 0.122 Uiso 0.50 1 calc PR . . H46B H -0.0087 0.4018 0.6025 0.122 Uiso 0.50 1 calc PR . . H46C H -0.0115 0.4166 0.5113 0.122 Uiso 0.50 1 calc PR . . 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 Fe1 0.0239(3) 0.0233(3) 0.0311(2) -0.00013(19) -0.00283(18) -0.0018(2) Cl1 0.0248(6) 0.0263(6) 0.0468(6) 0.0049(5) 0.000 0.000 Cl2 0.0291(5) 0.0325(5) 0.0385(4) 0.0025(4) -0.0008(3) 0.0028(4) Cl3 0.0701(11) 0.0566(10) 0.0416(7) 0.0064(7) 0.000 0.000 S1 0.0415(6) 0.0483(6) 0.0455(5) 0.0021(5) 0.0092(4) 0.0195(5) S2 0.0570(7) 0.0325(5) 0.0380(5) -0.0005(4) 0.0060(4) 0.0141(5) N1 0.0254(15) 0.0276(16) 0.0407(15) 0.0054(13) -0.0053(12) -0.0053(13) N2 0.0287(16) 0.0222(15) 0.0411(15) 0.0036(12) -0.0089(12) 0.0004(13) N3 0.0289(16) 0.0254(15) 0.0297(13) 0.0034(12) -0.0014(11) 0.0054(13) N4 0.0269(15) 0.0254(15) 0.0323(14) 0.0007(12) -0.0044(12) -0.0008(13) N5 0.0248(14) 0.0246(15) 0.0300(13) -0.0003(11) 0.0012(11) -0.0036(12) N6 0.0234(15) 0.0297(16) 0.0335(14) 0.0044(12) 0.0018(11) 0.0026(13) N7 0.060(4) 0.057(4) 0.098(5) 0.005(4) 0.000 0.000 N8 0.054(4) 0.090(5) 0.054(3) 0.001(3) 0.000 0.000 O1 0.041(2) 0.031(2) 0.056(2) 0.0140(17) 0.000 0.000 O2 0.042(2) 0.032(2) 0.070(3) -0.0069(19) 0.000 0.000 O3 0.0419(17) 0.0493(18) 0.0600(17) 0.0068(14) -0.0177(13) -0.0036(15) O4 0.0278(15) 0.0423(17) 0.101(2) 0.0173(17) 0.0018(15) 0.0065(14) O5 0.096(3) 0.079(2) 0.0340(14) -0.0045(15) -0.0043(16) 0.044(2) O6 0.0489(17) 0.0354(15) 0.0432(13) -0.0052(12) -0.0050(12) 0.0019(13) O7 0.0398(17) 0.0409(17) 0.085(2) 0.0026(16) 0.0043(15) -0.0132(14) O8 0.144(4) 0.049(2) 0.158(4) -0.023(3) 0.038(4) -0.007(3) O9 0.250(8) 0.290(9) 0.102(4) -0.020(5) -0.107(5) 0.109(7) O10 0.077(4) 0.068(4) 0.151(6) 0.030(4) 0.000 0.000 O11 0.202(9) 0.146(7) 0.075(4) -0.042(4) 0.000 0.000 O12 0.060(3) 0.110(4) 0.128(4) 0.000(3) 0.010(2) 0.019(3) C1 0.031(2) 0.037(2) 0.047(2) 0.0015(17) 0.0028(16) -0.0060(18) C2 0.035(2) 0.041(2) 0.059(2) 0.007(2) 0.0080(18) -0.003(2) C3 0.030(2) 0.036(2) 0.082(3) 0.005(2) 0.010(2) -0.0046(19) C4 0.029(2) 0.029(2) 0.079(3) 0.002(2) -0.0038(19) -0.0049(18) C5 0.0276(19) 0.0249(18) 0.052(2) 0.0055(16) -0.0072(16) -0.0032(16) C6 0.031(2) 0.0207(18) 0.055(2) 0.0030(16) -0.0115(17) -0.0003(16) C7 0.041(2) 0.031(2) 0.068(3) -0.006(2) -0.015(2) -0.0057(19) C8 0.056(3) 0.029(2) 0.067(3) -0.010(2) -0.023(2) -0.004(2) C9 0.055(3) 0.029(2) 0.045(2) -0.0061(17) -0.0128(18) 0.004(2) C10 0.040(2) 0.0230(18) 0.0361(17) 0.0014(14) -0.0112(15) 0.0069(17) C11 0.037(2) 0.0282(18) 0.0295(16) 0.0028(14) -0.0048(14) 0.0103(16) C12 0.040(2) 0.036(2) 0.0401(19) 0.0064(16) 0.0053(16) 0.0073(18) C13 0.0312(19) 0.0290(18) 0.0334(16) 0.0057(15) 0.0018(14) 0.0068(16) C14 0.0286(19) 0.0295(19) 0.0316(16) 0.0070(14) 0.0030(14) -0.0002(16) C15 0.027(2) 0.039(2) 0.053(2) 0.0066(18) 0.0023(16) 0.0036(18) C16 0.0242(19) 0.048(2) 0.054(2) 0.0066(19) -0.0030(17) -0.0046(18) C17 0.033(2) 0.032(2) 0.0404(18) 0.0027(16) -0.0022(15) -0.0068(17) C18 0.0281(18) 0.0269(18) 0.0317(16) 0.0046(14) 0.0020(14) -0.0032(15) C19 0.0231(17) 0.0296(19) 0.0319(16) 0.0047(14) 0.0018(13) -0.0007(15) C20 0.0272(18) 0.0279(18) 0.0351(17) 0.0025(15) 0.0048(14) -0.0059(15) C21 0.032(2) 0.038(2) 0.0431(19) -0.0087(17) 0.0022(16) -0.0029(18) C22 0.041(2) 0.042(2) 0.054(2) -0.0193(19) 0.0059(18) 0.003(2) C23 0.034(2) 0.040(2) 0.053(2) -0.0103(19) 0.0072(18) 0.0059(19) C24 0.0271(18) 0.0328(19) 0.0381(17) 0.0041(15) 0.0080(14) 0.0018(16) C25 0.0306(19) 0.0280(18) 0.0332(16) 0.0004(14) 0.0041(14) -0.0050(16) C26 0.034(2) 0.0284(19) 0.0355(17) 0.0011(15) -0.0004(15) -0.0022(16) C27 0.034(2) 0.033(2) 0.047(2) 0.0047(17) -0.0023(16) 0.0067(17) C28 0.0275(19) 0.042(2) 0.0441(19) 0.0107(18) -0.0082(16) 0.0023(18) C29 0.0296(19) 0.038(2) 0.0340(17) 0.0037(16) -0.0051(14) -0.0052(17) C30 0.0229(17) 0.0293(18) 0.0313(15) 0.0033(14) -0.0012(13) -0.0056(15) C31 0.0256(18) 0.0289(18) 0.0307(15) 0.0025(14) 0.0023(13) -0.0068(15) C32 0.035(2) 0.039(2) 0.0357(17) -0.0037(16) -0.0051(15) -0.0102(18) C33 0.046(2) 0.033(2) 0.0422(19) -0.0089(17) -0.0009(17) -0.0119(19) C34 0.046(2) 0.0271(19) 0.0374(18) -0.0016(15) 0.0080(17) -0.0024(17) C35 0.035(2) 0.0264(18) 0.0318(16) 0.0018(14) 0.0071(14) -0.0024(16) C36 0.0309(19) 0.0298(19) 0.0349(17) 0.0060(15) 0.0058(14) 0.0053(16) C37 0.035(2) 0.065(3) 0.044(2) 0.006(2) 0.0030(17) 0.017(2) C38 0.0224(18) 0.046(2) 0.0382(18) 0.0086(17) 0.0047(14) 0.0044(17) C39 0.027(2) 0.061(3) 0.0390(19) 0.0076(19) -0.0024(15) 0.0040(19) C40 0.0248(16) 0.0398(19) 0.0388(15) 0.0072(14) -0.0048(13) -0.0019(15) C41 0.0260(15) 0.052(2) 0.0401(15) 0.0005(14) -0.0062(13) -0.0068(15) C42 0.0324(17) 0.136(3) 0.0564(18) -0.026(2) -0.0027(15) -0.0212(19) C43 0.0342(18) 0.164(3) 0.072(2) -0.039(2) 0.0026(16) -0.025(2) C44 0.030(2) 0.171(4) 0.069(2) -0.041(3) 0.0039(18) -0.018(3) C45 0.106(7) 0.052(5) 0.068(4) 0.002(4) 0.000 0.000 C46 0.111(7) 0.066(5) 0.065(4) -0.013(4) 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N5 2.142(3) . ? Fe1 N2 2.148(3) . ? Fe1 N4 2.215(3) . ? Fe1 N1 2.216(3) . ? Fe1 N3 2.221(3) . ? Fe1 N6 2.270(3) . ? Cl1 O1 1.431(4) . ? Cl1 O3 1.432(3) 12_655 ? Cl1 O3 1.432(3) . ? Cl1 O2 1.436(4) . ? Cl2 O5 1.424(3) . ? Cl2 O4 1.430(3) . ? Cl2 O6 1.433(3) . ? Cl2 O7 1.434(3) . ? Cl3 O9 1.312(5) . ? Cl3 O9 1.312(5) 4_566 ? Cl3 O8 1.410(5) 4_566 ? Cl3 O8 1.410(5) . ? S1 C36 1.705(4) . ? S1 C37 1.706(4) . ? S2 C12 1.701(4) . ? S2 C11 1.703(4) . ? N1 C1 1.336(5) . ? N1 C5 1.351(4) . ? N2 C6 1.340(5) . ? N2 C10 1.345(5) . ? N3 C11 1.316(4) . ? N3 C13 1.377(5) . ? N4 C26 1.340(4) . ? N4 C30 1.356(4) . ? N5 C31 1.340(4) . ? N5 C35 1.347(4) . ? N6 C36 1.314(4) . ? N6 C38 1.378(4) . ? N7 O11 1.164(8) . ? N7 O10 1.274(8) . ? N7 C45 1.404(9) . ? N8 O12 1.218(5) 12 ? N8 O12 1.218(5) . ? N8 C46 1.464(10) . ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? C2 C3 1.375(6) . ? C2 H2 0.9500 . ? C3 C4 1.366(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(5) . ? C4 H4 0.9500 . ? C5 C6 1.477(5) . ? C6 C7 1.395(5) . ? C7 C8 1.379(6) . ? C7 H7 0.9500 . ? C8 C9 1.367(6) . ? C8 H8 0.9500 . ? C9 C10 1.388(5) . ? C9 H9 0.9500 . ? C10 C11 1.459(5) . ? C12 C13 1.361(5) . ? C12 H12 0.9500 . ? C13 C14 1.464(5) . ? C14 C19 1.382(5) . ? C14 C15 1.394(5) . ? C15 C16 1.384(6) . ? C15 H15 0.9500 . ? C16 C17 1.384(5) . ? C16 H16 0.9500 . ? C17 C18 1.392(5) . ? C17 H17 0.9500 . ? C18 C19 1.391(5) . ? C18 C20 1.480(5) . ? C19 H19 0.9500 . ? C20 C21 1.389(5) . ? C20 C25 1.397(5) . ? C21 C22 1.384(5) . ? C21 H21 0.9500 . ? C22 C23 1.378(6) . ? C22 H22 0.9500 . ? C23 C24 1.387(5) . ? C23 H23 0.9500 . ? C24 C25 1.380(5) . ? C24 C41 1.479(5) 4_565 ? C25 H25 0.9500 . ? C26 C27 1.379(5) . ? C26 H26 0.9500 . ? C27 C28 1.379(5) . ? C27 H27 0.9500 . ? C28 C29 1.380(5) . ? C28 H28 0.9500 . ? C29 C30 1.379(5) . ? C29 H29 0.9500 . ? C30 C31 1.480(5) . ? C31 C32 1.389(5) . ? C32 C33 1.380(5) . ? C32 H32 0.9500 . ? C33 C34 1.377(5) . ? C33 H33 0.9500 . ? C34 C35 1.380(5) . ? C34 H34 0.9500 . ? C35 C36 1.463(5) . ? C37 C38 1.365(5) . ? C37 H37 0.9500 . ? C38 C39 1.470(5) . ? C39 C40 1.371(5) . ? C39 C44 1.386(6) . ? C40 C41 1.389(5) . ? C40 H40 0.9500 . ? C41 C42 1.378(6) . ? C41 C24 1.478(5) 4_565 ? C42 C43 1.371(7) . ? C42 H42 0.9500 . ? C43 C44 1.401(7) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? 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 N5 Fe1 N2 165.64(11) . . ? N5 Fe1 N4 73.58(10) . . ? N2 Fe1 N4 103.18(10) . . ? N5 Fe1 N1 93.89(10) . . ? N2 Fe1 N1 73.07(11) . . ? N4 Fe1 N1 103.73(10) . . ? N5 Fe1 N3 118.98(11) . . ? N2 Fe1 N3 73.71(11) . . ? N4 Fe1 N3 82.72(10) . . ? N1 Fe1 N3 146.76(11) . . ? N5 Fe1 N6 73.77(10) . . ? N2 Fe1 N6 109.49(11) . . ? N4 Fe1 N6 147.09(10) . . ? N1 Fe1 N6 82.51(10) . . ? N3 Fe1 N6 109.88(10) . . ? O1 Cl1 O3 109.56(15) . 12_655 ? O1 Cl1 O3 109.56(15) . . ? O3 Cl1 O3 110.7(3) 12_655 . ? O1 Cl1 O2 109.7(2) . . ? O3 Cl1 O2 108.65(16) 12_655 . ? O3 Cl1 O2 108.65(16) . . ? O5 Cl2 O4 109.1(2) . . ? O5 Cl2 O6 109.22(17) . . ? O4 Cl2 O6 110.35(18) . . ? O5 Cl2 O7 109.8(2) . . ? O4 Cl2 O7 109.66(18) . . ? O6 Cl2 O7 108.65(17) . . ? O9 Cl3 O9 120.2(8) . 4_566 ? O9 Cl3 O8 103.7(4) . 4_566 ? O9 Cl3 O8 112.3(5) 4_566 4_566 ? O9 Cl3 O8 112.3(5) . . ? O9 Cl3 O8 103.7(4) 4_566 . ? O8 Cl3 O8 103.6(4) 4_566 . ? C36 S1 C37 89.32(19) . . ? C12 S2 C11 89.71(18) . . ? C1 N1 C5 117.6(3) . . ? C1 N1 Fe1 124.9(2) . . ? C5 N1 Fe1 116.8(2) . . ? C6 N2 C10 120.1(3) . . ? C6 N2 Fe1 120.1(2) . . ? C10 N2 Fe1 119.7(2) . . ? C11 N3 C13 111.2(3) . . ? C11 N3 Fe1 113.7(2) . . ? C13 N3 Fe1 132.2(2) . . ? C26 N4 C30 117.4(3) . . ? C26 N4 Fe1 126.0(2) . . ? C30 N4 Fe1 116.5(2) . . ? C31 N5 C35 119.7(3) . . ? C31 N5 Fe1 120.1(2) . . ? C35 N5 Fe1 120.2(2) . . ? C36 N6 C38 111.0(3) . . ? C36 N6 Fe1 112.2(2) . . ? C38 N6 Fe1 134.2(2) . . ? O11 N7 O10 123.4(8) . . ? O11 N7 C45 124.0(8) . . ? O10 N7 C45 112.6(7) . . ? O12 N8 O12 123.8(8) 12 . ? O12 N8 C46 118.1(4) 12 . ? O12 N8 C46 118.1(4) . . ? N1 C1 C2 123.7(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C2 C1 118.0(4) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 114.6(3) . . ? C4 C5 C6 123.7(3) . . ? N2 C6 C7 120.9(4) . . ? N2 C6 C5 114.4(3) . . ? C7 C6 C5 124.7(4) . . ? C8 C7 C6 118.5(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.5(4) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? N2 C10 C9 121.4(4) . . ? N2 C10 C11 112.2(3) . . ? C9 C10 C11 126.3(4) . . ? N3 C11 C10 119.6(3) . . ? N3 C11 S2 114.4(3) . . ? C10 C11 S2 125.9(3) . . ? C13 C12 S2 111.0(3) . . ? C13 C12 H12 124.5 . . ? S2 C12 H12 124.5 . . ? C12 C13 N3 113.8(3) . . ? C12 C13 C14 126.9(3) . . ? N3 C13 C14 119.3(3) . . ? C19 C14 C15 118.9(3) . . ? C19 C14 C13 118.9(3) . . ? C15 C14 C13 122.2(3) . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 121.0(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 118.2(3) . . ? C19 C18 C20 119.3(3) . . ? C17 C18 C20 122.3(3) . . ? C14 C19 C18 122.2(3) . . ? C14 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? C21 C20 C25 117.8(3) . . ? C21 C20 C18 123.3(3) . . ? C25 C20 C18 118.9(3) . . ? C22 C21 C20 119.4(4) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 121.8(4) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 117.9(3) . . ? C25 C24 C41 119.1(3) . 4_565 ? C23 C24 C41 122.9(3) . 4_565 ? C24 C25 C20 123.1(3) . . ? C24 C25 H25 118.4 . . ? C20 C25 H25 118.4 . . ? N4 C26 C27 123.4(3) . . ? N4 C26 H26 118.3 . . ? C27 C26 H26 118.3 . . ? C26 C27 C28 118.5(4) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C27 C28 C29 119.1(3) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 119.3(3) . . ? C30 C29 H29 120.4 . . ? C28 C29 H29 120.4 . . ? N4 C30 C29 122.2(3) . . ? N4 C30 C31 114.9(3) . . ? C29 C30 C31 122.8(3) . . ? N5 C31 C32 121.0(3) . . ? N5 C31 C30 114.5(3) . . ? C32 C31 C30 124.5(3) . . ? C33 C32 C31 119.0(3) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 118.4(4) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N5 C35 C34 122.0(3) . . ? N5 C35 C36 112.3(3) . . ? C34 C35 C36 125.7(3) . . ? N6 C36 C35 120.4(3) . . ? N6 C36 S1 114.9(3) . . ? C35 C36 S1 124.6(3) . . ? C38 C37 S1 111.1(3) . . ? C38 C37 H37 124.5 . . ? S1 C37 H37 124.5 . . ? C37 C38 N6 113.7(3) . . ? C37 C38 C39 127.2(3) . . ? N6 C38 C39 119.0(3) . . ? C40 C39 C44 118.8(4) . . ? C40 C39 C38 118.3(3) . . ? C44 C39 C38 122.9(4) . . ? C39 C40 C41 123.0(4) . . ? C39 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C42 C41 C40 117.8(4) . . ? C42 C41 C24 121.4(4) . 4_565 ? C40 C41 C24 120.8(3) . 4_565 ? C43 C42 C41 120.2(4) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C42 C43 C44 121.6(5) . . ? C42 C43 H43 119.2 . . ? C44 C43 H43 119.2 . . ? C39 C44 C43 118.5(4) . . ? C39 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? N7 C45 H45A 109.5 . . ? N7 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N7 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N8 C46 H46A 109.5 . . ? N8 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N8 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.129 _refine_diff_density_min -0.792 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 945477' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_I _chemical_name_systematic ? _chemical_name_common 'LOMe_CoBF4_MeNO2_CHCl3 ' _chemical_formula_moiety 'C92 H64 Co2 N12 O2 S4, 4(B F4), 4(C H Cl3)' _chemical_formula_sum 'C96 H68 B4 Cl12 Co2 F16 N12 O2 S4' _chemical_formula_iupac ? _chemical_formula_weight 2440.36 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2403(4) _cell_length_b 14.2668(6) _cell_length_c 15.9890(6) _cell_angle_alpha 97.9160(10) _cell_angle_beta 102.7040(10) _cell_angle_gamma 91.6320(10) _cell_volume 2472.85(16) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.5134 _cell_measurement_theta_max 29.1089 _cell_measurement_temperature 150.(2) _exptl_crystal_description plate _exptl_crystal_colour 'clear orange' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1230 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.89 _exptl_special_details ; ; _diffrn_ambient_temperature 150.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 56159 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _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. ; _reflns_number_total 14975 _reflns_number_gt 9866 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_gt 0.1684 _refine_ls_wR_factor_ref 0.1935 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_number_reflns 14975 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+3.7684P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.469 _refine_diff_density_min -1.185 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service v2011.6.0.0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co Co1 0.30545(4) 0.22623(3) 0.22063(3) 0.01579(10) Uani d . 1 . . B B1 0.1072(4) 0.6881(3) 0.0223(3) 0.0320(9) Uani d . 1 . . B B2 0.6800(4) 0.9579(3) 0.3626(3) 0.0324(9) Uani d . 1 . . S S1 0.02264(8) 0.45129(6) 0.18460(6) 0.02546(18) Uani d . 1 . . S S2 0.40406(11) 0.23768(7) 0.51300(6) 0.0347(2) Uani d . 1 . . Cl Cl1 0.71705(10) 0.70495(7) 0.31680(8) 0.0423(2) Uani d . 1 . . Cl Cl2 0.74121(13) 0.53849(10) 0.19881(8) 0.0595(4) Uani d . 1 . . Cl Cl3 0.80444(13) 0.53372(10) 0.38252(9) 0.0565(3) Uani d . 1 . . Cl Cl4 0.52919(19) 0.92424(13) 0.07237(15) 0.0927(6) Uani d . 1 . . Cl Cl5 0.42673(13) 0.76007(12) 0.12267(10) 0.0651(4) Uani d . 1 . . Cl Cl6 0.67086(13) 0.76233(12) 0.09678(10) 0.0644(4) Uani d . 1 . . F F1 0.1623(3) 0.73441(19) 0.10461(16) 0.0460(6) Uani d . 1 . . F F2 0.0615(3) 0.75290(18) -0.03140(18) 0.0494(7) Uani d . 1 . . F F3 0.0165(3) 0.6240(2) 0.0294(2) 0.0583(8) Uani d . 1 . . F F4 0.1943(2) 0.63870(18) -0.01267(17) 0.0425(6) Uani d . 1 . . F F5 0.5824(2) 0.8896(2) 0.33666(19) 0.0492(7) Uani d . 1 . . F F6 0.7303(3) 0.9644(2) 0.29190(18) 0.0505(7) Uani d . 1 . . F F7 0.6377(3) 1.0443(2) 0.3917(2) 0.0552(7) Uani d . 1 . . F F8 0.7665(2) 0.93010(19) 0.42903(18) 0.0463(6) Uani d . 1 . . N N1 0.4888(2) 0.2147(2) 0.19564(18) 0.0215(5) Uani d . 1 . . N N2 0.3235(2) 0.33336(19) 0.14935(18) 0.0197(5) Uani d . 1 . . N N3 0.1395(2) 0.30554(18) 0.22301(17) 0.0167(5) Uani d . 1 . . N N4 0.2194(2) 0.1192(2) 0.11391(18) 0.0212(5) Uani d . 1 . . N N5 0.3077(2) 0.10213(18) 0.27420(17) 0.0175(5) Uani d . 1 . . N N6 0.3602(2) 0.27445(18) 0.35792(17) 0.0174(5) Uani d . 1 . . O O1 -0.2043(2) 0.34885(16) 0.47900(15) 0.0223(5) Uani d . 1 . . C C1 0.5715(3) 0.1540(3) 0.2241(2) 0.0268(7) Uani d . 1 . . H H1 0.5509 0.11 0.2589 0.032 Uiso calc R 1 . . C C2 0.6868(3) 0.1527(3) 0.2049(3) 0.0313(8) Uani d . 1 . . H H2 0.7437 0.109 0.2265 0.038 Uiso calc R 1 . . C C3 0.7162(3) 0.2157(3) 0.1541(3) 0.0322(8) Uani d . 1 . . H H3 0.7939 0.2162 0.1399 0.039 Uiso calc R 1 . . C C4 0.6317(3) 0.2784(3) 0.1240(3) 0.0304(8) Uani d . 1 . . H H4 0.6506 0.3224 0.0886 0.037 Uiso calc R 1 . . C C5 0.5188(3) 0.2768(2) 0.1456(2) 0.0226(6) Uani d . 1 . . C C6 0.4245(3) 0.3434(3) 0.1186(2) 0.0248(7) Uani d . 1 . . C C7 0.4345(4) 0.4134(3) 0.0675(3) 0.0393(10) Uani d . 1 . . H H7 0.5062 0.4212 0.0463 0.047 Uiso calc R 1 . . C C8 0.3391(4) 0.4715(3) 0.0481(3) 0.0412(10) Uani d . 1 . . H H8 0.3446 0.5186 0.0122 0.049 Uiso calc R 1 . . C C9 0.2361(3) 0.4616(3) 0.0801(3) 0.0323(8) Uani d . 1 . . H H9 0.1699 0.5011 0.0671 0.039 Uiso calc R 1 . . C C10 0.2328(3) 0.3918(2) 0.1322(2) 0.0206(6) Uani d . 1 . . C C11 0.1366(3) 0.3764(2) 0.1775(2) 0.0193(6) Uani d . 1 . . C C12 -0.0249(3) 0.3849(2) 0.2533(2) 0.0243(7) Uani d . 1 . . H H12 -0.0931 0.3978 0.2783 0.029 Uiso calc R 1 . . C C13 0.0477(3) 0.3105(2) 0.2678(2) 0.0195(6) Uani d . 1 . . C C14 0.0278(3) 0.2407(2) 0.3235(2) 0.0191(6) Uani d . 1 . . C C15 0.0336(3) 0.1440(2) 0.2970(2) 0.0223(6) Uani d . 1 . . H H15 0.0558 0.1225 0.2439 0.027 Uiso calc R 1 . . C C16 0.0069(3) 0.0794(2) 0.3487(2) 0.0253(7) Uani d . 1 . . H H16 0.0112 0.0135 0.331 0.03 Uiso calc R 1 . . C C17 -0.0260(3) 0.1102(2) 0.4259(2) 0.0237(7) Uani d . 1 . . H H17 -0.0448 0.0652 0.4604 0.028 Uiso calc R 1 . . C C18 -0.0318(3) 0.2066(2) 0.4536(2) 0.0189(6) Uani d . 1 . . C C19 -0.0043(3) 0.2715(2) 0.4019(2) 0.0194(6) Uani d . 1 . . H H19 -0.0074 0.3374 0.4203 0.023 Uiso calc R 1 . . C C20 -0.0633(3) 0.2378(2) 0.5388(2) 0.0191(6) Uani d . 1 . . C C21 -0.0077(3) 0.1966(2) 0.6106(2) 0.0210(6) Uani d . 1 . . H H21 0.0487 0.1493 0.6039 0.025 Uiso calc R 1 . . C C22 -0.0326(3) 0.2231(2) 0.6918(2) 0.0227(6) Uani d . 1 . . C C23 -0.1169(3) 0.2911(2) 0.7003(2) 0.0213(6) Uani d . 1 . . H H23 -0.134 0.3098 0.7556 0.026 Uiso calc R 1 . . C C24 -0.1774(3) 0.3329(2) 0.6296(2) 0.0184(6) Uani d . 1 . . C C25 -0.1483(3) 0.3065(2) 0.5491(2) 0.0178(6) Uani d . 1 . . C C26 0.0310(3) 0.1799(3) 0.7694(2) 0.0308(8) Uani d . 1 . . H H26A 0.0521 0.2291 0.8203 0.046 Uiso calc R 1 . . H H26B 0.1056 0.1521 0.758 0.046 Uiso calc R 1 . . H H26C -0.0235 0.1303 0.7802 0.046 Uiso calc R 1 . . C C27 -0.3016(4) 0.2916(3) 0.4214(3) 0.0382(9) Uani d . 1 . . H H27A -0.2731 0.229 0.4044 0.057 Uiso calc R 1 . . H H27B -0.33 0.3217 0.3697 0.057 Uiso calc R 1 . . H H27C -0.3691 0.2844 0.4503 0.057 Uiso calc R 1 . . C C28 -0.2717(3) 0.4008(2) 0.6434(2) 0.0179(6) Uani d . 1 . . C C29 -0.3496(3) 0.3822(2) 0.6972(2) 0.0221(6) Uani d . 1 . . H H29 -0.3444 0.3249 0.7214 0.027 Uiso calc R 1 . . C C30 0.1735(3) 0.1340(3) 0.0324(2) 0.0284(7) Uani d . 1 . . H H30 0.1656 0.1974 0.0211 0.034 Uiso calc R 1 . . C C31 0.1372(4) 0.0610(3) -0.0358(3) 0.0355(9) Uani d . 1 . . H H31 0.1076 0.074 -0.0932 0.043 Uiso calc R 1 . . C C32 0.1449(4) -0.0306(3) -0.0189(3) 0.0375(9) Uani d . 1 . . H H32 0.1192 -0.0821 -0.0645 0.045 Uiso calc R 1 . . C C33 0.1905(4) -0.0478(3) 0.0654(2) 0.0313(8) Uani d . 1 . . H H33 0.1968 -0.1107 0.0783 0.038 Uiso calc R 1 . . C C34 0.2265(3) 0.0293(2) 0.1301(2) 0.0209(6) Uani d . 1 . . C C35 0.2728(3) 0.0191(2) 0.2226(2) 0.0193(6) Uani d . 1 . . C C36 0.2758(3) -0.0649(2) 0.2572(2) 0.0257(7) Uani d . 1 . . H H36 0.2525 -0.1239 0.2206 0.031 Uiso calc R 1 . . C C37 0.3136(3) -0.0612(2) 0.3467(2) 0.0276(7) Uani d . 1 . . H H37 0.316 -0.1181 0.3715 0.033 Uiso calc R 1 . . C C38 0.3474(3) 0.0243(2) 0.3995(2) 0.0242(7) Uani d . 1 . . H H38 0.3724 0.0276 0.4606 0.029 Uiso calc R 1 . . C C39 0.3436(3) 0.1059(2) 0.3602(2) 0.0188(6) Uani d . 1 . . C C40 0.3701(3) 0.2035(2) 0.4042(2) 0.0200(6) Uani d . 1 . . C C41 0.4025(4) 0.3538(3) 0.4962(2) 0.0309(8) Uani d . 1 . . H H41 0.4175 0.4066 0.5412 0.037 Uiso calc R 1 . . C C42 0.3773(3) 0.3607(2) 0.4105(2) 0.0203(6) Uani d . 1 . . C C43 0.3678(3) 0.4500(2) 0.3732(2) 0.0197(6) Uani d . 1 . . C C44 0.4434(3) 0.4702(2) 0.3186(2) 0.0218(6) Uani d . 1 . . H H44 0.5009 0.4263 0.3052 0.026 Uiso calc R 1 . . C C45 0.4346(3) 0.5540(2) 0.2842(2) 0.0231(6) Uani d . 1 . . H H45 0.4868 0.5681 0.2477 0.028 Uiso calc R 1 . . C C46 0.2823(3) 0.5143(2) 0.3924(2) 0.0190(6) Uani d . 1 . . H H46 0.2313 0.5004 0.4297 0.023 Uiso calc R 1 . . C C47 0.8009(4) 0.6058(3) 0.3009(3) 0.0380(9) Uani d . 1 . . H H47 0.8867 0.6282 0.303 0.046 Uiso calc R 1 . . C C48 0.5609(4) 0.8309(4) 0.1327(3) 0.0496(11) Uani d . 1 . . H H48 0.5929 0.8576 0.1951 0.06 Uiso calc R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.01948(19) 0.01326(19) 0.0182(2) 0.00441(14) 0.00930(15) 0.00588(15) B1 0.040(2) 0.025(2) 0.034(2) 0.0022(17) 0.0125(18) 0.0049(17) B2 0.035(2) 0.031(2) 0.037(2) 0.0081(17) 0.0139(18) 0.0154(19) S1 0.0298(4) 0.0215(4) 0.0297(4) 0.0123(3) 0.0105(3) 0.0117(3) S2 0.0651(7) 0.0216(4) 0.0181(4) 0.0055(4) 0.0085(4) 0.0065(3) Cl1 0.0477(6) 0.0310(5) 0.0556(7) 0.0076(4) 0.0269(5) 0.0071(5) Cl2 0.0655(8) 0.0570(8) 0.0488(7) 0.0303(6) 0.0038(6) -0.0071(6) Cl3 0.0744(8) 0.0545(7) 0.0553(7) 0.0289(6) 0.0343(6) 0.0217(6) Cl4 0.0938(13) 0.0639(10) 0.1139(15) -0.0037(9) -0.0017(11) 0.0331(10) Cl5 0.0501(7) 0.0780(10) 0.0679(9) -0.0124(6) 0.0221(6) 0.0027(7) Cl6 0.0526(7) 0.0850(10) 0.0584(8) 0.0037(7) 0.0184(6) 0.0113(7) F1 0.0601(16) 0.0476(15) 0.0302(13) -0.0050(12) 0.0127(11) 0.0034(11) F2 0.0642(17) 0.0320(13) 0.0470(15) 0.0113(12) -0.0010(13) 0.0086(11) F3 0.0595(18) 0.0582(18) 0.0617(19) -0.0204(14) 0.0295(15) 0.0039(15) F4 0.0508(14) 0.0369(13) 0.0473(15) 0.0104(11) 0.0223(12) 0.0120(11) F5 0.0395(14) 0.0495(16) 0.0619(18) 0.0012(11) 0.0115(12) 0.0196(14) F6 0.0584(17) 0.0550(17) 0.0442(15) -0.0058(13) 0.0227(13) 0.0118(13) F7 0.0721(19) 0.0416(15) 0.0574(18) 0.0233(14) 0.0201(15) 0.0133(13) F8 0.0431(14) 0.0499(16) 0.0482(15) 0.0158(12) 0.0076(11) 0.0171(12) N1 0.0215(12) 0.0215(14) 0.0251(14) 0.0046(10) 0.0104(11) 0.0068(11) N2 0.0230(12) 0.0198(13) 0.0212(13) 0.0050(10) 0.0113(10) 0.0087(11) N3 0.0183(11) 0.0156(12) 0.0188(12) 0.0040(9) 0.0075(9) 0.0054(10) N4 0.0244(13) 0.0192(13) 0.0227(13) 0.0053(10) 0.0080(10) 0.0068(11) N5 0.0197(12) 0.0147(12) 0.0211(13) 0.0049(9) 0.0087(10) 0.0052(10) N6 0.0211(12) 0.0135(12) 0.0198(13) 0.0041(9) 0.0072(10) 0.0052(10) O1 0.0309(12) 0.0211(11) 0.0186(11) 0.0107(9) 0.0088(9) 0.0092(9) C1 0.0251(16) 0.0251(17) 0.0334(19) 0.0068(13) 0.0109(14) 0.0078(14) C2 0.0245(16) 0.0299(19) 0.042(2) 0.0100(14) 0.0117(15) 0.0045(16) C3 0.0228(16) 0.032(2) 0.046(2) 0.0038(14) 0.0185(15) 0.0005(17) C4 0.0305(17) 0.033(2) 0.035(2) 0.0024(14) 0.0194(15) 0.0083(16) C5 0.0230(14) 0.0234(16) 0.0248(16) 0.0021(12) 0.0119(12) 0.0044(13) C6 0.0239(15) 0.0286(18) 0.0266(17) 0.0019(13) 0.0120(13) 0.0100(14) C7 0.041(2) 0.045(2) 0.046(2) 0.0068(18) 0.0256(19) 0.029(2) C8 0.043(2) 0.044(2) 0.050(3) 0.0065(18) 0.0214(19) 0.033(2) C9 0.0323(18) 0.033(2) 0.038(2) 0.0041(15) 0.0106(15) 0.0222(17) C10 0.0223(14) 0.0196(15) 0.0231(15) 0.0039(11) 0.0070(12) 0.0104(12) C11 0.0214(14) 0.0192(15) 0.0192(14) 0.0061(11) 0.0055(11) 0.0070(12) C12 0.0272(16) 0.0238(16) 0.0268(17) 0.0100(13) 0.0133(13) 0.0078(13) C13 0.0215(14) 0.0199(15) 0.0197(15) 0.0058(11) 0.0088(11) 0.0041(12) C14 0.0179(13) 0.0192(15) 0.0230(15) 0.0053(11) 0.0087(11) 0.0057(12) C15 0.0220(14) 0.0214(16) 0.0266(16) 0.0058(12) 0.0127(12) 0.0010(13) C16 0.0305(16) 0.0174(15) 0.0316(18) 0.0061(13) 0.0146(14) 0.0034(13) C17 0.0299(16) 0.0177(15) 0.0297(17) 0.0054(12) 0.0158(14) 0.0089(13) C18 0.0183(13) 0.0182(15) 0.0239(15) 0.0066(11) 0.0104(11) 0.0055(12) C19 0.0225(14) 0.0160(14) 0.0236(15) 0.0069(11) 0.0115(12) 0.0056(12) C20 0.0213(14) 0.0193(15) 0.0202(15) 0.0028(11) 0.0097(11) 0.0069(12) C21 0.0232(14) 0.0201(15) 0.0241(16) 0.0076(12) 0.0104(12) 0.0082(13) C22 0.0248(15) 0.0235(16) 0.0225(16) 0.0061(12) 0.0069(12) 0.0096(13) C23 0.0254(15) 0.0212(15) 0.0202(15) 0.0039(12) 0.0081(12) 0.0074(12) C24 0.0221(14) 0.0167(14) 0.0202(14) 0.0045(11) 0.0100(11) 0.0066(12) C25 0.0225(14) 0.0153(14) 0.0182(14) 0.0048(11) 0.0070(11) 0.0072(11) C26 0.0352(18) 0.035(2) 0.0247(17) 0.0125(15) 0.0064(14) 0.0118(15) C27 0.0333(19) 0.042(2) 0.035(2) 0.0079(17) -0.0038(16) 0.0084(18) C28 0.0230(14) 0.0149(14) 0.0171(14) 0.0033(11) 0.0066(11) 0.0032(11) C29 0.0268(15) 0.0203(16) 0.0223(16) 0.0017(12) 0.0103(12) 0.0056(13) C30 0.0355(18) 0.0244(17) 0.0269(18) 0.0045(14) 0.0062(14) 0.0096(14) C31 0.045(2) 0.038(2) 0.0229(18) 0.0034(17) 0.0035(15) 0.0063(16) C32 0.048(2) 0.032(2) 0.028(2) 0.0048(17) 0.0045(17) -0.0036(16) C33 0.043(2) 0.0213(17) 0.0280(18) 0.0073(15) 0.0055(15) 0.0005(14) C34 0.0222(14) 0.0177(15) 0.0245(16) 0.0046(11) 0.0081(12) 0.0044(12) C35 0.0205(14) 0.0166(14) 0.0233(15) 0.0044(11) 0.0090(12) 0.0041(12) C36 0.0312(17) 0.0154(15) 0.0308(18) 0.0042(12) 0.0073(14) 0.0035(13) C37 0.0367(18) 0.0171(16) 0.0323(19) 0.0052(13) 0.0091(15) 0.0120(14) C38 0.0293(16) 0.0201(16) 0.0266(17) 0.0052(13) 0.0082(13) 0.0119(13) C39 0.0222(14) 0.0162(14) 0.0202(15) 0.0038(11) 0.0074(11) 0.0053(12) C40 0.0232(14) 0.0198(15) 0.0187(15) 0.0037(11) 0.0060(11) 0.0069(12) C41 0.052(2) 0.0187(16) 0.0215(17) 0.0028(15) 0.0077(15) 0.0025(13) C42 0.0253(15) 0.0170(15) 0.0203(15) 0.0047(11) 0.0072(12) 0.0051(12) C43 0.0254(15) 0.0144(14) 0.0195(15) 0.0026(11) 0.0051(12) 0.0027(12) C44 0.0215(14) 0.0213(16) 0.0237(16) 0.0046(12) 0.0084(12) 0.0014(13) C45 0.0269(15) 0.0222(16) 0.0247(16) 0.0021(12) 0.0145(13) 0.0047(13) C46 0.0256(14) 0.0158(14) 0.0183(14) 0.0021(11) 0.0097(11) 0.0041(11) C47 0.040(2) 0.035(2) 0.045(2) 0.0071(17) 0.0207(18) 0.0081(18) C48 0.045(2) 0.055(3) 0.045(3) -0.004(2) 0.006(2) -0.001(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 N2 . 2.059(3) ? Co1 N5 . 2.069(3) ? Co1 N6 . 2.153(3) ? Co1 N4 . 2.157(3) ? Co1 N1 . 2.191(3) ? Co1 N3 . 2.213(2) ? B1 F2 . 1.381(5) ? B1 F3 . 1.384(5) ? B1 F1 . 1.390(5) ? B1 F4 . 1.393(5) ? B2 F8 . 1.383(5) ? B2 F6 . 1.383(5) ? B2 F7 . 1.392(5) ? B2 F5 . 1.398(5) ? S1 C11 . 1.704(3) ? S1 C12 . 1.705(3) ? S2 C40 . 1.695(3) ? S2 C41 . 1.715(4) ? Cl1 C47 . 1.743(4) ? Cl2 C47 . 1.757(5) ? Cl3 C47 . 1.764(4) ? Cl4 C48 . 1.750(6) ? Cl5 C48 . 1.756(5) ? Cl6 C48 . 1.743(5) ? N1 C1 . 1.337(4) ? N1 C5 . 1.354(4) ? N2 C10 . 1.341(4) ? N2 C6 . 1.344(4) ? N3 C11 . 1.321(4) ? N3 C13 . 1.378(4) ? N4 C30 . 1.339(4) ? N4 C34 . 1.344(4) ? N5 C39 . 1.339(4) ? N5 C35 . 1.342(4) ? N6 C40 . 1.327(4) ? N6 C42 . 1.374(4) ? O1 C25 . 1.384(4) ? O1 C27 . 1.419(5) ? C1 C2 . 1.397(5) ? C1 H1 . 0.95 ? C2 C3 . 1.371(6) ? C2 H2 . 0.95 ? C3 C4 . 1.378(5) ? C3 H3 . 0.95 ? C4 C5 . 1.388(4) ? C4 H4 . 0.95 ? C5 C6 . 1.478(5) ? C6 C7 . 1.391(5) ? C7 C8 . 1.381(6) ? C7 H7 . 0.95 ? C8 C9 . 1.376(5) ? C8 H8 . 0.95 ? C9 C10 . 1.387(5) ? C9 H9 . 0.95 ? C10 C11 . 1.455(4) ? C12 C13 . 1.371(4) ? C12 H12 . 0.95 ? C13 C14 . 1.468(4) ? C14 C15 . 1.394(4) ? C14 C19 . 1.397(4) ? C15 C16 . 1.388(5) ? C15 H15 . 0.95 ? C16 C17 . 1.383(5) ? C16 H16 . 0.95 ? C17 C18 . 1.393(4) ? C17 H17 . 0.95 ? C18 C19 . 1.394(4) ? C18 C20 . 1.494(4) ? C19 H19 . 0.95 ? C20 C21 . 1.395(4) ? C20 C25 . 1.407(4) ? C21 C22 . 1.392(5) ? C21 H21 . 0.95 ? C22 C23 . 1.390(4) ? C22 C26 . 1.508(5) ? C23 C24 . 1.403(4) ? C23 H23 . 0.95 ? C24 C25 . 1.402(4) ? C24 C28 . 1.486(4) ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 C29 . 1.400(4) ? C28 C46 2_566 1.407(4) ? C29 C45 2_566 1.389(4) ? C29 H29 . 0.95 ? C30 C31 . 1.381(6) ? C30 H30 . 0.95 ? C31 C32 . 1.372(6) ? C31 H31 . 0.95 ? C32 C33 . 1.390(5) ? C32 H32 . 0.95 ? C33 C34 . 1.386(5) ? C33 H33 . 0.95 ? C34 C35 . 1.484(5) ? C35 C36 . 1.386(4) ? C36 C37 . 1.393(5) ? C36 H36 . 0.95 ? C37 C38 . 1.376(5) ? C37 H37 . 0.95 ? C38 C39 . 1.395(4) ? C38 H38 . 0.95 ? C39 C40 . 1.462(5) ? C41 C42 . 1.355(5) ? C41 H41 . 0.95 ? C42 C43 . 1.476(4) ? C43 C44 . 1.396(4) ? C43 C46 . 1.401(4) ? C44 C45 . 1.381(5) ? C44 H44 . 0.95 ? C45 C29 2_566 1.389(4) ? C45 H45 . 0.95 ? C46 C28 2_566 1.407(4) ? C46 H46 . 0.95 ? C47 H47 . 1.0 ? C48 H48 . 1.0 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Co1 N5 . . 167.44(10) ? N2 Co1 N6 . . 111.90(11) ? N5 Co1 N6 . . 76.57(10) ? N2 Co1 N4 . . 97.52(11) ? N5 Co1 N4 . . 75.39(10) ? N6 Co1 N4 . . 150.07(10) ? N2 Co1 N1 . . 75.53(10) ? N5 Co1 N1 . . 94.54(10) ? N6 Co1 N1 . . 97.47(10) ? N4 Co1 N1 . . 94.98(10) ? N2 Co1 N3 . . 76.26(10) ? N5 Co1 N3 . . 114.33(10) ? N6 Co1 N3 . . 86.62(9) ? N4 Co1 N3 . . 95.49(10) ? N1 Co1 N3 . . 150.94(10) ? F2 B1 F3 . . 111.8(4) ? F2 B1 F1 . . 110.4(3) ? F3 B1 F1 . . 108.7(4) ? F2 B1 F4 . . 108.2(3) ? F3 B1 F4 . . 108.8(3) ? F1 B1 F4 . . 109.0(4) ? F8 B2 F6 . . 109.9(3) ? F8 B2 F7 . . 109.4(4) ? F6 B2 F7 . . 111.0(3) ? F8 B2 F5 . . 109.4(3) ? F6 B2 F5 . . 107.8(4) ? F7 B2 F5 . . 109.3(3) ? C11 S1 C12 . . 89.11(15) ? C40 S2 C41 . . 89.34(17) ? C1 N1 C5 . . 118.2(3) ? C1 N1 Co1 . . 127.1(2) ? C5 N1 Co1 . . 114.7(2) ? C10 N2 C6 . . 120.1(3) ? C10 N2 Co1 . . 119.6(2) ? C6 N2 Co1 . . 120.2(2) ? C11 N3 C13 . . 110.5(2) ? C11 N3 Co1 . . 110.88(19) ? C13 N3 Co1 . . 137.8(2) ? C30 N4 C34 . . 118.3(3) ? C30 N4 Co1 . . 125.8(2) ? C34 N4 Co1 . . 115.4(2) ? C39 N5 C35 . . 120.8(3) ? C39 N5 Co1 . . 119.4(2) ? C35 N5 Co1 . . 119.8(2) ? C40 N6 C42 . . 111.2(3) ? C40 N6 Co1 . . 112.5(2) ? C42 N6 Co1 . . 135.9(2) ? C25 O1 C27 . . 113.6(3) ? N1 C1 C2 . . 122.8(3) ? N1 C1 H1 . . 118.6 ? C2 C1 H1 . . 118.6 ? C3 C2 C1 . . 118.6(3) ? C3 C2 H2 . . 120.7 ? C1 C2 H2 . . 120.7 ? C2 C3 C4 . . 119.2(3) ? C2 C3 H3 . . 120.4 ? C4 C3 H3 . . 120.4 ? C3 C4 C5 . . 119.6(3) ? C3 C4 H4 . . 120.2 ? C5 C4 H4 . . 120.2 ? N1 C5 C4 . . 121.6(3) ? N1 C5 C6 . . 115.2(3) ? C4 C5 C6 . . 123.1(3) ? N2 C6 C7 . . 120.2(3) ? N2 C6 C5 . . 114.2(3) ? C7 C6 C5 . . 125.6(3) ? C8 C7 C6 . . 119.3(3) ? C8 C7 H7 . . 120.4 ? C6 C7 H7 . . 120.4 ? C9 C8 C7 . . 120.5(3) ? C9 C8 H8 . . 119.7 ? C7 C8 H8 . . 119.7 ? C8 C9 C10 . . 117.4(3) ? C8 C9 H9 . . 121.3 ? C10 C9 H9 . . 121.3 ? N2 C10 C9 . . 122.4(3) ? N2 C10 C11 . . 112.4(3) ? C9 C10 C11 . . 125.1(3) ? N3 C11 C10 . . 120.4(3) ? N3 C11 S1 . . 115.4(2) ? C10 C11 S1 . . 123.9(2) ? C13 C12 S1 . . 111.3(2) ? C13 C12 H12 . . 124.3 ? S1 C12 H12 . . 124.3 ? C12 C13 N3 . . 113.6(3) ? C12 C13 C14 . . 123.5(3) ? N3 C13 C14 . . 122.8(3) ? C15 C14 C19 . . 119.7(3) ? C15 C14 C13 . . 120.9(3) ? C19 C14 C13 . . 119.2(3) ? C16 C15 C14 . . 119.5(3) ? C16 C15 H15 . . 120.3 ? C14 C15 H15 . . 120.3 ? C17 C16 C15 . . 120.6(3) ? C17 C16 H16 . . 119.7 ? C15 C16 H16 . . 119.7 ? C16 C17 C18 . . 120.7(3) ? C16 C17 H17 . . 119.6 ? C18 C17 H17 . . 119.6 ? C17 C18 C19 . . 118.7(3) ? C17 C18 C20 . . 119.5(3) ? C19 C18 C20 . . 121.8(3) ? C18 C19 C14 . . 120.8(3) ? C18 C19 H19 . . 119.6 ? C14 C19 H19 . . 119.6 ? C21 C20 C25 . . 118.7(3) ? C21 C20 C18 . . 118.9(3) ? C25 C20 C18 . . 122.4(3) ? C22 C21 C20 . . 121.7(3) ? C22 C21 H21 . . 119.2 ? C20 C21 H21 . . 119.2 ? C23 C22 C21 . . 118.6(3) ? C23 C22 C26 . . 120.4(3) ? C21 C22 C26 . . 121.1(3) ? C22 C23 C24 . . 121.9(3) ? C22 C23 H23 . . 119.1 ? C24 C23 H23 . . 119.1 ? C25 C24 C23 . . 118.2(3) ? C25 C24 C28 . . 123.4(3) ? C23 C24 C28 . . 118.3(3) ? O1 C25 C24 . . 119.2(3) ? O1 C25 C20 . . 119.8(3) ? C24 C25 C20 . . 120.9(3) ? C22 C26 H26A . . 109.5 ? C22 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? C22 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? O1 C27 H27A . . 109.5 ? O1 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? O1 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C29 C28 C46 . 2_566 118.2(3) ? C29 C28 C24 . . 119.2(3) ? C46 C28 C24 2_566 . 122.6(3) ? C45 C29 C28 2_566 . 121.3(3) ? C45 C29 H29 2_566 . 119.4 ? C28 C29 H29 . . 119.4 ? N4 C30 C31 . . 122.9(3) ? N4 C30 H30 . . 118.6 ? C31 C30 H30 . . 118.6 ? C32 C31 C30 . . 118.5(4) ? C32 C31 H31 . . 120.7 ? C30 C31 H31 . . 120.7 ? C31 C32 C33 . . 119.7(4) ? C31 C32 H32 . . 120.2 ? C33 C32 H32 . . 120.2 ? C34 C33 C32 . . 118.3(4) ? C34 C33 H33 . . 120.8 ? C32 C33 H33 . . 120.8 ? N4 C34 C33 . . 122.3(3) ? N4 C34 C35 . . 114.9(3) ? C33 C34 C35 . . 122.7(3) ? N5 C35 C36 . . 120.6(3) ? N5 C35 C34 . . 113.3(3) ? C36 C35 C34 . . 126.0(3) ? C35 C36 C37 . . 118.7(3) ? C35 C36 H36 . . 120.7 ? C37 C36 H36 . . 120.7 ? C38 C37 C36 . . 120.5(3) ? C38 C37 H37 . . 119.7 ? C36 C37 H37 . . 119.7 ? C37 C38 C39 . . 117.7(3) ? C37 C38 H38 . . 121.1 ? C39 C38 H38 . . 121.1 ? N5 C39 C38 . . 121.6(3) ? N5 C39 C40 . . 111.7(3) ? C38 C39 C40 . . 126.6(3) ? N6 C40 C39 . . 119.7(3) ? N6 C40 S2 . . 114.6(2) ? C39 C40 S2 . . 125.6(2) ? C42 C41 S2 . . 111.2(3) ? C42 C41 H41 . . 124.4 ? S2 C41 H41 . . 124.4 ? C41 C42 N6 . . 113.6(3) ? C41 C42 C43 . . 125.5(3) ? N6 C42 C43 . . 120.9(3) ? C44 C43 C46 . . 120.0(3) ? C44 C43 C42 . . 120.2(3) ? C46 C43 C42 . . 119.8(3) ? C45 C44 C43 . . 120.0(3) ? C45 C44 H44 . . 120.0 ? C43 C44 H44 . . 120.0 ? C44 C45 C29 . 2_566 120.2(3) ? C44 C45 H45 . . 119.9 ? C29 C45 H45 2_566 . 119.9 ? C43 C46 C28 . 2_566 120.4(3) ? C43 C46 H46 . . 119.8 ? C28 C46 H46 2_566 . 119.8 ? Cl1 C47 Cl2 . . 110.8(2) ? Cl1 C47 Cl3 . . 111.8(2) ? Cl2 C47 Cl3 . . 109.6(2) ? Cl1 C47 H47 . . 108.2 ? Cl2 C47 H47 . . 108.2 ? Cl3 C47 H47 . . 108.2 ? Cl6 C48 Cl4 . . 110.2(3) ? Cl6 C48 Cl5 . . 109.8(3) ? Cl4 C48 Cl5 . . 109.9(3) ? Cl6 C48 H48 . . 109.0 ? Cl4 C48 H48 . . 109.0 ? Cl5 C48 H48 . . 109.0 ? _database_code_depnum_ccdc_archive 'CCDC 945478' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_I _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C104 H72 Cd2 N12 O2 S4, 4(Cl O4), 3.48(C2 H3 N)' _chemical_formula_sum 'C110.95 H82.43 Cd2 Cl4 N15.48 O18 S4' _chemical_formula_iupac ? _chemical_formula_weight 2415.24 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.7000(11) _cell_length_b 12.4488(6) _cell_length_c 22.2200(11) _cell_angle_alpha 90 _cell_angle_beta 117.0500(10) _cell_angle_gamma 90 _cell_volume 5345.9(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7969 _cell_measurement_theta_min 2.4152 _cell_measurement_theta_max 26.8431 _cell_measurement_temperature 150.(2) _exptl_crystal_description block _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2457 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ; _diffrn_ambient_temperature 150.(2) _diffrn_source ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 53131 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.33 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _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. Rewstrains used in the least squares refinement sadi 0.005 o7 o8 o7 o6' o7 o9' o8 o6' o8 o9' o9' o6' sadi 0.005 cl2 o9 cl2 o6 cl2' o6' cl2' o9' DELU 0.003 0.006 O8 O9' O7 O6 O6' O9 DELU 0.003 0.006 N8 C55 C56 SIMU 0.003 0.006 O6 O6' O8 O7 O9' O9 SIMU 0.003 0.006 N8 C55 C56 ISOR 0.01 O9' ; _reflns_number_total 13301 _reflns_number_gt 8746 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_gt 0.1503 _refine_ls_wR_factor_ref 0.1743 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.038 _refine_ls_number_reflns 13301 _refine_ls_number_parameters 734 _refine_ls_number_restraints 60 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+5.0467P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.560 _refine_diff_density_min -0.920 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' _computing_data_collection 'Bruker Instrument Service v2011.6.0.0' _computing_cell_refinement 'SAINT V7.68A (Bruker AXS, 2009)' _computing_data_reduction 'SAINT V7.68A (Bruker AXS, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.687993(14) 0.87774(3) 0.207465(15) 0.02686(10) Uani d . 1.0 . . Cl Cl1 0.23346(5) 0.52234(10) 0.49964(6) 0.0382(3) Uani d . 1.0 . . Cl Cl2 0.50873(15) 0.2700(3) 0.19020(17) 0.0498(7) Uani d PD 0.738(5) A 1 Cl Cl2' 0.4901(4) 0.3088(5) 0.1834(4) 0.0391(17) Uani d PD 0.262(5) A 2 S S1 0.88288(5) 1.08814(10) 0.23830(6) 0.0370(3) Uani d . 1.0 . . S S2 0.76500(7) 0.77896(11) 0.43435(6) 0.0426(3) Uani d . 1.0 . . N N1 0.57186(17) 0.9343(3) 0.15131(19) 0.0343(9) Uani d . 1.0 . . N N2 0.68038(17) 1.0365(3) 0.15148(18) 0.0297(8) Uani d . 1.0 . . N N3 0.80129(16) 0.9370(3) 0.23319(17) 0.0274(8) Uani d . 1.0 . . N N4 0.66215(18) 0.7491(3) 0.12007(19) 0.0366(9) Uani d . 1.0 . . N N5 0.67071(17) 0.7088(3) 0.24047(19) 0.0301(8) Uani d . 1.0 . . N N6 0.71975(17) 0.8814(3) 0.32284(17) 0.0274(7) Uani d . 1.0 . . N N7 0.9641(3) 0.8297(6) 0.7089(5) 0.121(3) Uani d . 1.0 . . N N8 0.4471(5) 0.6383(7) 0.0504(5) 0.085(2) Uani d PU 0.738(5) A 1 O O1 1.06666(14) 0.7979(2) 0.48286(15) 0.0309(7) Uani d . 1.0 . . O O2 0.19567(18) 0.5012(4) 0.5372(2) 0.0608(11) Uani d . 1.0 . . O O3 0.2738(2) 0.4291(3) 0.5023(2) 0.0586(11) Uani d . 1.0 . . O O4 0.27926(18) 0.6112(3) 0.5287(2) 0.0551(10) Uani d . 1.0 . . O O5 0.18554(18) 0.5447(4) 0.43141(18) 0.0580(11) Uani d . 1.0 . . O O6 0.4378(3) 0.2825(8) 0.1670(4) 0.097(2) Uani d PDU 0.738(5) A 1 O O7 0.5275(3) 0.3148(5) 0.1416(2) 0.0916(18) Uani d D 1.0 . . O O8 0.5476(2) 0.3066(4) 0.25467(19) 0.0714(13) Uani d D 1.0 . . O O9 0.5218(5) 0.1591(5) 0.1972(5) 0.125(3) Uani d PDU 0.738(5) A 1 O O6' 0.4537(6) 0.2123(10) 0.1705(4) 0.102(4) Uani d PDU 0.262(5) A 2 O O9' 0.4511(6) 0.4012(10) 0.1749(4) 0.104(4) Uani d PDU 0.262(5) A 2 C C1 0.5198(2) 0.8792(4) 0.1516(2) 0.0398(11) Uani d . 1.0 . . H H1 0.53 0.8201 0.1817 0.048 Uiso calc R 1.0 . . C C2 0.4505(2) 0.9046(5) 0.1095(3) 0.0442(13) Uani d . 1.0 . . H H2 0.4141 0.8635 0.1107 0.053 Uiso calc R 1.0 . . C C3 0.4367(2) 0.9896(5) 0.0669(3) 0.0468(13) Uani d . 1.0 . . H H3 0.3901 1.0089 0.0378 0.056 Uiso calc R 1.0 . . C C4 0.4901(2) 1.0475(5) 0.0659(3) 0.0466(13) Uani d . 1.0 . . H H4 0.4809 1.1068 0.0361 0.056 Uiso calc R 1.0 . . C C5 0.5577(2) 1.0182(4) 0.1092(2) 0.0347(10) Uani d . 1.0 . . C C6 0.6184(2) 1.0816(4) 0.1126(2) 0.0340(10) Uani d . 1.0 . . C C7 0.6132(2) 1.1762(4) 0.0805(3) 0.0447(12) Uani d . 1.0 . . H H7 0.5691 1.207 0.0531 0.054 Uiso calc R 1.0 . . C C8 0.6725(3) 1.2271(5) 0.0881(3) 0.0502(14) Uani d . 1.0 . . H H8 0.6695 1.2926 0.065 0.06 Uiso calc R 1.0 . . C C9 0.7366(2) 1.1834(4) 0.1293(3) 0.0426(12) Uani d . 1.0 . . H H9 0.778 1.2186 0.1359 0.051 Uiso calc R 1.0 . . C C10 0.7384(2) 1.0866(4) 0.1607(2) 0.0312(9) Uani d . 1.0 . . C C11 0.80230(19) 1.0317(4) 0.2078(2) 0.0291(9) Uani d . 1.0 . . C C12 0.9168(2) 0.9783(4) 0.2885(2) 0.0353(10) Uani d . 1.0 . . H H12 0.9646 0.9693 0.3185 0.042 Uiso calc R 1.0 . . C C13 0.86663(19) 0.9047(4) 0.2802(2) 0.0278(9) Uani d . 1.0 . . C C14 0.87566(19) 0.8015(4) 0.3153(2) 0.0296(9) Uani d . 1.0 . . C C15 0.8366(2) 0.7120(4) 0.2817(2) 0.0332(10) Uani d . 1.0 . . H H15 0.8045 0.7168 0.2351 0.04 Uiso calc R 1.0 . . C C16 0.8445(2) 0.6161(4) 0.3161(2) 0.0353(10) Uani d . 1.0 . . H H16 0.8177 0.5554 0.2929 0.042 Uiso calc R 1.0 . . C C17 0.8911(2) 0.6081(4) 0.3840(2) 0.0340(10) Uani d . 1.0 . . H H17 0.8954 0.5421 0.407 0.041 Uiso calc R 1.0 . . C C18 0.9319(2) 0.6958(4) 0.4191(2) 0.0313(10) Uani d . 1.0 . . C C19 0.92262(19) 0.7921(4) 0.3834(2) 0.0310(10) Uani d . 1.0 . . H H19 0.9492 0.8531 0.4064 0.037 Uiso calc R 1.0 . . C C20 0.9802(2) 0.6858(4) 0.4927(2) 0.0312(10) Uani d . 1.0 . . C C21 0.9610(2) 0.6250(4) 0.5333(2) 0.0338(10) Uani d . 1.0 . . H H21 0.9171 0.5907 0.5135 0.041 Uiso calc R 1.0 . . C C22 1.0037(2) 0.6120(4) 0.6026(2) 0.0345(10) Uani d . 1.0 . . C C23 1.0674(2) 0.6650(4) 0.6309(2) 0.0345(10) Uani d . 1.0 . . H H23 1.0966 0.6584 0.6781 0.041 Uiso calc R 1.0 . . C C24 1.0896(2) 0.7273(4) 0.5923(2) 0.0324(10) Uani d . 1.0 . . C C25 1.0454(2) 0.7367(4) 0.5227(2) 0.0311(10) Uani d . 1.0 . . C C26 0.9825(2) 0.5438(4) 0.6469(3) 0.0422(12) Uani d . 1.0 . . H H26A 1.0126 0.4806 0.6628 0.063 Uiso calc R 1.0 . . H H26B 0.9344 0.5206 0.6206 0.063 Uiso calc R 1.0 . . H H26C 0.9868 0.5862 0.6858 0.063 Uiso calc R 1.0 . . C C27 1.1588(2) 0.7791(4) 0.6255(2) 0.0303(9) Uani d . 1.0 . . C C28 1.2155(2) 0.7229(4) 0.6733(2) 0.0379(11) Uani d . 1.0 . . H H28 1.2105 0.6496 0.6822 0.045 Uiso calc R 1.0 . . C C29 1.2793(2) 0.7734(4) 0.7082(3) 0.0410(12) Uani d . 1.0 . . H H29 1.3172 0.7349 0.7417 0.049 Uiso calc R 1.0 . . C C30 1.2879(2) 0.8794(4) 0.6945(2) 0.0338(10) Uani d . 1.0 . . H H30 1.3316 0.9134 0.7183 0.041 Uiso calc R 1.0 . . C C31 1.2320(2) 0.9359(4) 0.6457(2) 0.0282(9) Uani d . 1.0 . . C C32 1.1677(2) 0.8851(4) 0.6117(2) 0.0293(9) Uani d . 1.0 . . H H32 1.1295 0.9237 0.5787 0.035 Uiso calc R 1.0 . . C C33 1.1060(3) 0.7370(4) 0.4575(3) 0.0464(13) Uani d . 1.0 . . H H33A 1.0756 0.6853 0.4228 0.056 Uiso calc R 1.0 . . H H33B 1.1429 0.6962 0.4947 0.056 Uiso calc R 1.0 . . C C34 1.1374(2) 0.8146(4) 0.4271(2) 0.0362(10) Uani d . 1.0 . . C C35 1.2020(3) 0.8578(4) 0.4658(3) 0.0426(12) Uani d . 1.0 . . H H35 1.2271 0.8366 0.5117 0.051 Uiso calc R 1.0 . . C C36 1.2312(3) 0.9307(5) 0.4399(3) 0.0519(14) Uani d . 1.0 . . H H36 1.276 0.9587 0.4677 0.062 Uiso calc R 1.0 . . C C37 1.1953(4) 0.9630(5) 0.3736(4) 0.0623(17) Uani d . 1.0 . . H H37 1.215 1.0144 0.3558 0.075 Uiso calc R 1.0 . . C C38 1.1309(3) 0.9209(6) 0.3332(3) 0.0607(17) Uani d . 1.0 . . H H38 1.1064 0.9421 0.2872 0.073 Uiso calc R 1.0 . . C C39 1.1017(3) 0.8472(5) 0.3598(3) 0.0510(14) Uani d . 1.0 . . H H39 1.057 0.8187 0.3319 0.061 Uiso calc R 1.0 . . C C40 0.6570(3) 0.7769(5) 0.0597(2) 0.0479(13) Uani d . 1.0 . . H H40 0.676 0.8437 0.0557 0.058 Uiso calc R 1.0 . . C C41 0.6254(3) 0.7132(6) 0.0030(3) 0.0636(18) Uani d . 1.0 . . H H41 0.6227 0.7347 -0.0392 0.076 Uiso calc R 1.0 . . C C42 0.5981(3) 0.6176(6) 0.0100(3) 0.0657(19) Uani d . 1.0 . . H H42 0.5751 0.5721 -0.0281 0.079 Uiso calc R 1.0 . . C C43 0.6037(3) 0.5871(5) 0.0715(3) 0.0569(16) Uani d . 1.0 . . H H43 0.5856 0.52 0.0764 0.068 Uiso calc R 1.0 . . C C44 0.6360(2) 0.6551(4) 0.1263(2) 0.0382(11) Uani d . 1.0 . . C C45 0.6446(2) 0.6287(4) 0.1951(3) 0.0366(10) Uani d . 1.0 . . C C46 0.6298(3) 0.5301(5) 0.2141(3) 0.0572(16) Uani d . 1.0 . . H H46 0.6116 0.4731 0.1824 0.069 Uiso calc R 1.0 . . C C47 0.6422(4) 0.5161(5) 0.2811(4) 0.0679(19) Uani d . 1.0 . . H H47 0.6313 0.4495 0.2948 0.082 Uiso calc R 1.0 . . C C48 0.6702(3) 0.5983(4) 0.3273(3) 0.0475(13) Uani d . 1.0 . . H H48 0.6793 0.5893 0.3731 0.057 Uiso calc R 1.0 . . C C49 0.6843(2) 0.6933(4) 0.3050(2) 0.0323(10) Uani d . 1.0 . . C C50 0.7178(2) 0.7863(4) 0.3486(2) 0.0288(9) Uani d . 1.0 . . C C51 0.7878(3) 0.9103(4) 0.4357(2) 0.0393(11) Uani d . 1.0 . . H H51 0.8166 0.9488 0.4756 0.047 Uiso calc R 1.0 . . C C52 0.7599(2) 0.9529(4) 0.3727(2) 0.0289(9) Uani d . 1.0 . . C C53 0.9162(4) 0.7933(6) 0.6660(5) 0.075(2) Uani d . 1.0 B 4 C C54 0.8544(3) 0.7402(6) 0.6172(3) 0.076(2) Uani d . 1.0 . . H H54A 0.8478 0.673 0.6365 0.114 Uiso calc R 1.0 B 4 H H54B 0.8592 0.7244 0.5763 0.114 Uiso calc R 1.0 B 4 H H54C 0.8143 0.7871 0.6057 0.114 Uiso calc R 1.0 B 4 C C55 0.4325(5) 0.6200(9) 0.0884(7) 0.083(2) Uani d PU 0.738(5) A 1 C C56 0.4242(7) 0.5900(10) 0.1428(7) 0.108(3) Uani d PU 0.738(5) A 1 H H56A 0.469 0.5682 0.1794 0.163 Uiso calc PR 0.738(5) A 1 H H56B 0.3918 0.5295 0.1306 0.163 Uiso calc PR 0.738(5) A 1 H H56C 0.4058 0.6505 0.1579 0.163 Uiso calc PR 0.738(5) A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cd1 0.01981(14) 0.02884(17) 0.02704(16) -0.00287(12) 0.00638(11) 0.00099(13) Cl1 0.0239(5) 0.0442(7) 0.0443(6) -0.0007(4) 0.0135(4) 0.0040(5) Cl2 0.0501(15) 0.0550(19) 0.0423(13) -0.0173(12) 0.0193(12) -0.0176(14) Cl2' 0.043(4) 0.035(4) 0.035(3) -0.005(3) 0.013(3) -0.001(3) S1 0.0232(5) 0.0382(7) 0.0466(7) -0.0063(4) 0.0131(5) 0.0017(5) S2 0.0551(7) 0.0372(7) 0.0296(6) -0.0087(6) 0.0141(5) 0.0025(5) N1 0.0228(16) 0.042(2) 0.034(2) 0.0000(16) 0.0093(15) 0.0074(18) N2 0.0220(15) 0.032(2) 0.0315(19) 0.0011(14) 0.0089(14) 0.0018(16) N3 0.0194(15) 0.030(2) 0.0303(18) -0.0028(14) 0.0088(13) -0.0022(15) N4 0.0303(18) 0.044(3) 0.0297(19) -0.0024(17) 0.0083(15) -0.0024(18) N5 0.0236(16) 0.027(2) 0.037(2) -0.0047(14) 0.0113(14) -0.0035(16) N6 0.0244(15) 0.0269(19) 0.0289(17) -0.0042(14) 0.0103(14) -0.0007(16) N7 0.052(4) 0.093(5) 0.197(9) -0.015(4) 0.040(5) -0.058(6) N8 0.075(5) 0.064(5) 0.122(7) 0.000(4) 0.050(4) -0.027(5) O1 0.0232(13) 0.0314(17) 0.0366(16) -0.0027(12) 0.0123(12) 0.0002(14) O2 0.0376(19) 0.090(3) 0.060(2) 0.001(2) 0.0274(18) 0.015(2) O3 0.049(2) 0.046(2) 0.087(3) 0.0048(18) 0.036(2) 0.001(2) O4 0.0355(18) 0.050(2) 0.067(3) -0.0071(16) 0.0126(17) -0.006(2) O5 0.0408(19) 0.085(3) 0.042(2) -0.006(2) 0.0126(16) 0.003(2) O6 0.050(3) 0.152(6) 0.082(4) -0.008(4) 0.026(3) 0.019(4) O7 0.104(4) 0.126(5) 0.067(3) -0.054(4) 0.057(3) -0.025(3) O8 0.058(2) 0.100(4) 0.049(2) -0.019(2) 0.018(2) -0.018(2) O9 0.145(6) 0.100(6) 0.106(5) 0.000(5) 0.038(5) -0.014(5) O6' 0.089(5) 0.122(7) 0.089(5) -0.016(5) 0.034(5) 0.004(6) O9' 0.071(5) 0.141(7) 0.089(6) 0.006(6) 0.027(5) 0.013(6) C1 0.025(2) 0.050(3) 0.041(3) -0.003(2) 0.0126(19) 0.008(2) C2 0.023(2) 0.056(3) 0.052(3) -0.005(2) 0.016(2) 0.000(3) C3 0.0199(19) 0.066(4) 0.045(3) 0.004(2) 0.0062(19) 0.007(3) C4 0.026(2) 0.058(4) 0.047(3) 0.005(2) 0.009(2) 0.015(3) C5 0.0211(18) 0.046(3) 0.033(2) -0.0002(18) 0.0092(17) 0.004(2) C6 0.027(2) 0.036(3) 0.038(2) 0.0026(18) 0.0129(18) 0.003(2) C7 0.031(2) 0.047(3) 0.054(3) 0.009(2) 0.018(2) 0.017(3) C8 0.044(3) 0.045(3) 0.063(3) 0.006(2) 0.026(3) 0.022(3) C9 0.034(2) 0.042(3) 0.056(3) 0.002(2) 0.025(2) 0.010(2) C10 0.0268(19) 0.036(2) 0.033(2) -0.0015(18) 0.0156(18) 0.0011(19) C11 0.0208(17) 0.034(3) 0.032(2) -0.0042(17) 0.0120(16) -0.0036(19) C12 0.0214(18) 0.040(3) 0.037(2) -0.0010(18) 0.0074(17) 0.000(2) C13 0.0181(17) 0.033(2) 0.030(2) -0.0023(16) 0.0084(15) -0.0032(18) C14 0.0179(16) 0.034(2) 0.037(2) -0.0029(16) 0.0125(16) -0.0047(19) C15 0.0223(18) 0.040(3) 0.034(2) -0.0029(18) 0.0098(17) -0.005(2) C16 0.027(2) 0.036(3) 0.038(2) -0.0082(19) 0.0102(18) -0.008(2) C17 0.0265(19) 0.031(3) 0.042(3) -0.0027(17) 0.0137(18) -0.004(2) C18 0.0202(17) 0.035(3) 0.037(2) -0.0023(17) 0.0119(17) -0.004(2) C19 0.0193(17) 0.034(3) 0.035(2) -0.0024(17) 0.0081(16) -0.001(2) C20 0.0220(18) 0.029(2) 0.038(2) -0.0035(17) 0.0093(17) -0.0008(19) C21 0.0219(18) 0.035(2) 0.039(2) -0.0006(18) 0.0084(17) -0.001(2) C22 0.029(2) 0.032(3) 0.040(2) -0.0012(18) 0.0139(18) 0.002(2) C23 0.028(2) 0.034(3) 0.035(2) -0.0005(19) 0.0088(18) 0.006(2) C24 0.0243(19) 0.027(2) 0.041(2) -0.0016(17) 0.0105(18) 0.0019(19) C25 0.0215(18) 0.032(2) 0.033(2) -0.0017(17) 0.0065(16) 0.0027(19) C26 0.033(2) 0.042(3) 0.047(3) -0.006(2) 0.014(2) 0.006(2) C27 0.0212(18) 0.031(2) 0.034(2) -0.0026(17) 0.0089(16) 0.0001(19) C28 0.027(2) 0.031(3) 0.047(3) 0.0000(18) 0.0089(19) 0.005(2) C29 0.024(2) 0.036(3) 0.049(3) 0.0022(19) 0.0038(19) 0.007(2) C30 0.0207(18) 0.038(3) 0.038(2) -0.0018(18) 0.0088(17) -0.004(2) C31 0.0277(19) 0.028(2) 0.028(2) -0.0005(17) 0.0121(16) -0.0029(18) C32 0.0240(18) 0.029(2) 0.031(2) -0.0008(17) 0.0089(16) -0.0027(19) C33 0.047(3) 0.036(3) 0.062(3) -0.004(2) 0.030(3) -0.008(3) C34 0.037(2) 0.032(3) 0.044(3) 0.0028(19) 0.021(2) -0.007(2) C35 0.041(2) 0.045(3) 0.042(3) -0.001(2) 0.019(2) -0.010(2) C36 0.051(3) 0.048(3) 0.069(4) -0.010(3) 0.039(3) -0.019(3) C37 0.085(5) 0.050(4) 0.083(5) 0.011(3) 0.065(4) 0.008(3) C38 0.065(4) 0.075(4) 0.052(3) 0.027(3) 0.036(3) 0.016(3) C39 0.035(2) 0.062(4) 0.053(3) 0.012(2) 0.017(2) -0.004(3) C40 0.046(3) 0.060(4) 0.035(3) 0.007(3) 0.016(2) 0.000(3) C41 0.061(4) 0.082(5) 0.038(3) 0.017(4) 0.015(3) -0.010(3) C42 0.058(4) 0.075(5) 0.042(3) 0.010(3) 0.004(3) -0.026(3) C43 0.043(3) 0.056(4) 0.052(3) -0.002(3) 0.005(2) -0.023(3) C44 0.0220(19) 0.045(3) 0.038(2) 0.0007(19) 0.0052(17) -0.012(2) C45 0.030(2) 0.033(3) 0.045(3) -0.0087(19) 0.0162(19) -0.008(2) C46 0.070(4) 0.039(3) 0.068(4) -0.028(3) 0.037(3) -0.019(3) C47 0.094(5) 0.038(3) 0.087(5) -0.031(3) 0.055(4) -0.008(3) C48 0.059(3) 0.036(3) 0.053(3) -0.017(2) 0.031(3) -0.001(2) C49 0.0272(19) 0.031(2) 0.040(2) -0.0045(17) 0.0155(18) 0.001(2) C50 0.0249(18) 0.029(2) 0.032(2) -0.0039(17) 0.0131(16) 0.0000(18) C51 0.047(3) 0.038(3) 0.030(2) -0.010(2) 0.015(2) -0.004(2) C52 0.0241(18) 0.032(2) 0.029(2) -0.0050(17) 0.0111(16) -0.0043(18) C53 0.056(4) 0.056(4) 0.127(7) 0.001(3) 0.054(4) -0.012(4) C54 0.061(4) 0.087(5) 0.057(4) 0.016(4) 0.006(3) -0.012(4) C55 0.076(4) 0.067(5) 0.129(7) -0.019(4) 0.067(4) -0.060(5) C56 0.112(6) 0.094(6) 0.139(7) -0.043(5) 0.075(5) -0.055(6) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 N2 . 2.301(4) ? Cd1 N5 . 2.314(4) ? Cd1 N6 . 2.333(3) ? Cd1 N1 . 2.355(3) ? Cd1 N3 . 2.374(3) ? Cd1 N4 . 2.379(4) ? Cl1 O5 . 1.423(4) ? Cl1 O4 . 1.430(4) ? Cl1 O2 . 1.435(4) ? Cl1 O3 . 1.440(4) ? Cl2 O8 . 1.369(5) ? Cl2 O6 . 1.391(5) ? Cl2 O9 . 1.403(5) ? Cl2 O7 . 1.428(5) ? Cl2' O9' . 1.389(5) ? Cl2' O6' . 1.395(5) ? Cl2' O7 . 1.486(10) ? Cl2' O8 . 1.507(9) ? S1 C12 . 1.705(5) ? S1 C11 . 1.713(4) ? S2 C51 . 1.705(5) ? S2 C50 . 1.707(4) ? N1 C1 . 1.324(6) ? N1 C5 . 1.341(6) ? N2 C10 . 1.335(5) ? N2 C6 . 1.346(5) ? N3 C11 . 1.311(6) ? N3 C13 . 1.384(5) ? N4 C44 . 1.335(7) ? N4 C40 . 1.340(6) ? N5 C49 . 1.341(6) ? N5 C45 . 1.346(6) ? N6 C50 . 1.324(5) ? N6 C52 . 1.379(5) ? N7 C53 . 1.138(9) ? N8 C55 . 1.053(14) ? O1 C25 . 1.395(5) ? O1 C33 . 1.435(6) ? C1 C2 . 1.399(6) ? C1 H1 . 0.95 ? C2 C3 . 1.359(8) ? C2 H2 . 0.95 ? C3 C4 . 1.374(7) ? C3 H3 . 0.95 ? C4 C5 . 1.388(6) ? C4 H4 . 0.95 ? C5 C6 . 1.509(6) ? C6 C7 . 1.355(7) ? C7 C8 . 1.374(7) ? C7 H7 . 0.95 ? C8 C9 . 1.382(7) ? C8 H8 . 0.95 ? C9 C10 . 1.383(7) ? C9 H9 . 0.95 ? C10 C11 . 1.472(6) ? C12 C13 . 1.370(6) ? C12 H12 . 0.95 ? C13 C14 . 1.469(6) ? C14 C19 . 1.393(6) ? C14 C15 . 1.393(6) ? C15 C16 . 1.386(7) ? C15 H15 . 0.95 ? C16 C17 . 1.386(6) ? C16 H16 . 0.95 ? C17 C18 . 1.399(6) ? C17 H17 . 0.95 ? C18 C19 . 1.401(6) ? C18 C20 . 1.494(6) ? C19 H19 . 0.95 ? C20 C21 . 1.379(6) ? C20 C25 . 1.410(5) ? C21 C22 . 1.400(6) ? C21 H21 . 0.95 ? C22 C23 . 1.396(6) ? C22 C26 . 1.521(7) ? C23 C24 . 1.395(6) ? C23 H23 . 0.95 ? C24 C25 . 1.407(6) ? C24 C27 . 1.485(6) ? C26 H26A . 0.98 ? C26 H26B . 0.98 ? C26 H26C . 0.98 ? C27 C32 . 1.387(6) ? C27 C28 . 1.394(6) ? C28 C29 . 1.391(6) ? C28 H28 . 0.95 ? C29 C30 . 1.386(7) ? C29 H29 . 0.95 ? C30 C31 . 1.395(6) ? C30 H30 . 0.95 ? C31 C32 . 1.400(6) ? C31 C52 3_776 1.476(6) ? C32 H32 . 0.95 ? C33 C34 . 1.507(7) ? C33 H33A . 0.99 ? C33 H33B . 0.99 ? C34 C35 . 1.377(7) ? C34 C39 . 1.396(7) ? C35 C36 . 1.374(8) ? C35 H35 . 0.95 ? C36 C37 . 1.377(9) ? C36 H36 . 0.95 ? C37 C38 . 1.376(9) ? C37 H37 . 0.95 ? C38 C39 . 1.390(9) ? C38 H38 . 0.95 ? C39 H39 . 0.95 ? C40 C41 . 1.378(8) ? C40 H40 . 0.95 ? C41 C42 . 1.370(10) ? C41 H41 . 0.95 ? C42 C43 . 1.368(9) ? C42 H42 . 0.95 ? C43 C44 . 1.384(7) ? C43 H43 . 0.95 ? C44 C45 . 1.490(7) ? C45 C46 . 1.383(7) ? C46 C47 . 1.397(9) ? C46 H46 . 0.95 ? C47 C48 . 1.381(8) ? C47 H47 . 0.95 ? C48 C49 . 1.369(7) ? C48 H48 . 0.95 ? C49 C50 . 1.472(6) ? C51 C52 . 1.354(6) ? C51 H51 . 0.95 ? C52 C31 3_776 1.476(6) ? C53 C54 . 1.445(10) ? C54 H54A . 0.98 ? C54 H54B . 0.98 ? C54 H54C . 0.98 ? C55 C56 . 1.355(17) ? C56 H56A . 0.98 ? C56 H56B . 0.98 ? C56 H56C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 Cd1 N5 . . 165.97(12) ? N2 Cd1 N6 . . 119.33(13) ? N5 Cd1 N6 . . 71.27(13) ? N2 Cd1 N1 . . 70.13(12) ? N5 Cd1 N1 . . 98.70(13) ? N6 Cd1 N1 . . 106.65(13) ? N2 Cd1 N3 . . 71.05(12) ? N5 Cd1 N3 . . 120.36(12) ? N6 Cd1 N3 . . 88.47(12) ? N1 Cd1 N3 . . 140.92(13) ? N2 Cd1 N4 . . 101.82(14) ? N5 Cd1 N4 . . 68.57(14) ? N6 Cd1 N4 . . 138.79(13) ? N1 Cd1 N4 . . 88.32(13) ? N3 Cd1 N4 . . 103.86(13) ? O5 Cl1 O4 . . 110.6(3) ? O5 Cl1 O2 . . 108.7(2) ? O4 Cl1 O2 . . 110.0(3) ? O5 Cl1 O3 . . 109.7(3) ? O4 Cl1 O3 . . 108.7(2) ? O2 Cl1 O3 . . 109.0(3) ? O8 Cl2 O6 . . 113.7(5) ? O8 Cl2 O9 . . 102.4(5) ? O6 Cl2 O9 . . 106.6(6) ? O8 Cl2 O7 . . 114.1(3) ? O6 Cl2 O7 . . 108.8(4) ? O9 Cl2 O7 . . 110.8(5) ? O9' Cl2' O6' . . 115.6(5) ? O9' Cl2' O7 . . 110.3(5) ? O6' Cl2' O7 . . 109.5(5) ? O9' Cl2' O8 . . 108.7(5) ? O6' Cl2' O8 . . 108.7(5) ? O7 Cl2' O8 . . 103.3(4) ? C12 S1 C11 . . 89.4(2) ? C51 S2 C50 . . 89.4(2) ? C1 N1 C5 . . 118.8(4) ? C1 N1 Cd1 . . 123.5(3) ? C5 N1 Cd1 . . 117.0(3) ? C10 N2 C6 . . 120.0(4) ? C10 N2 Cd1 . . 119.2(3) ? C6 N2 Cd1 . . 120.7(3) ? C11 N3 C13 . . 111.9(3) ? C11 N3 Cd1 . . 113.2(2) ? C13 N3 Cd1 . . 133.2(3) ? C44 N4 C40 . . 119.0(4) ? C44 N4 Cd1 . . 117.3(3) ? C40 N4 Cd1 . . 121.6(4) ? C49 N5 C45 . . 120.5(4) ? C49 N5 Cd1 . . 118.8(3) ? C45 N5 Cd1 . . 120.6(3) ? C50 N6 C52 . . 111.2(4) ? C50 N6 Cd1 . . 113.9(3) ? C52 N6 Cd1 . . 131.2(3) ? C25 O1 C33 . . 112.8(4) ? Cl2 O7 Cl2' . . 23.8(2) ? Cl2 O8 Cl2' . . 23.6(2) ? N1 C1 C2 . . 122.7(5) ? N1 C1 H1 . . 118.7 ? C2 C1 H1 . . 118.7 ? C3 C2 C1 . . 118.1(5) ? C3 C2 H2 . . 121.0 ? C1 C2 H2 . . 121.0 ? C2 C3 C4 . . 120.0(4) ? C2 C3 H3 . . 120.0 ? C4 C3 H3 . . 120.0 ? C3 C4 C5 . . 119.0(5) ? C3 C4 H4 . . 120.5 ? C5 C4 H4 . . 120.5 ? N1 C5 C4 . . 121.5(4) ? N1 C5 C6 . . 117.1(4) ? C4 C5 C6 . . 121.4(4) ? N2 C6 C7 . . 121.3(4) ? N2 C6 C5 . . 114.1(4) ? C7 C6 C5 . . 124.6(4) ? C6 C7 C8 . . 119.1(4) ? C6 C7 H7 . . 120.4 ? C8 C7 H7 . . 120.4 ? C7 C8 C9 . . 120.3(5) ? C7 C8 H8 . . 119.9 ? C9 C8 H8 . . 119.9 ? C8 C9 C10 . . 117.8(4) ? C8 C9 H9 . . 121.1 ? C10 C9 H9 . . 121.1 ? N2 C10 C9 . . 121.4(4) ? N2 C10 C11 . . 114.2(4) ? C9 C10 C11 . . 124.4(4) ? N3 C11 C10 . . 122.0(4) ? N3 C11 S1 . . 114.4(3) ? C10 C11 S1 . . 123.5(3) ? C13 C12 S1 . . 111.5(3) ? C13 C12 H12 . . 124.2 ? S1 C12 H12 . . 124.2 ? C12 C13 N3 . . 112.8(4) ? C12 C13 C14 . . 127.4(4) ? N3 C13 C14 . . 119.8(3) ? C19 C14 C15 . . 118.8(4) ? C19 C14 C13 . . 120.3(4) ? C15 C14 C13 . . 120.9(4) ? C16 C15 C14 . . 120.1(4) ? C16 C15 H15 . . 120.0 ? C14 C15 H15 . . 120.0 ? C15 C16 C17 . . 120.6(4) ? C15 C16 H16 . . 119.7 ? C17 C16 H16 . . 119.7 ? C16 C17 C18 . . 120.9(5) ? C16 C17 H17 . . 119.5 ? C18 C17 H17 . . 119.5 ? C17 C18 C19 . . 117.4(4) ? C17 C18 C20 . . 119.8(4) ? C19 C18 C20 . . 122.7(4) ? C14 C19 C18 . . 122.2(4) ? C14 C19 H19 . . 118.9 ? C18 C19 H19 . . 118.9 ? C21 C20 C25 . . 118.4(4) ? C21 C20 C18 . . 119.5(4) ? C25 C20 C18 . . 122.2(4) ? C20 C21 C22 . . 122.5(4) ? C20 C21 H21 . . 118.8 ? C22 C21 H21 . . 118.8 ? C23 C22 C21 . . 117.7(4) ? C23 C22 C26 . . 120.1(4) ? C21 C22 C26 . . 122.2(4) ? C24 C23 C22 . . 122.3(4) ? C24 C23 H23 . . 118.8 ? C22 C23 H23 . . 118.8 ? C23 C24 C25 . . 118.0(4) ? C23 C24 C27 . . 119.3(4) ? C25 C24 C27 . . 122.7(4) ? O1 C25 C24 . . 119.1(4) ? O1 C25 C20 . . 119.8(4) ? C24 C25 C20 . . 121.2(4) ? C22 C26 H26A . . 109.5 ? C22 C26 H26B . . 109.5 ? H26A C26 H26B . . 109.5 ? C22 C26 H26C . . 109.5 ? H26A C26 H26C . . 109.5 ? H26B C26 H26C . . 109.5 ? C32 C27 C28 . . 118.8(4) ? C32 C27 C24 . . 120.9(4) ? C28 C27 C24 . . 120.2(4) ? C29 C28 C27 . . 120.5(4) ? C29 C28 H28 . . 119.7 ? C27 C28 H28 . . 119.7 ? C30 C29 C28 . . 120.5(4) ? C30 C29 H29 . . 119.8 ? C28 C29 H29 . . 119.8 ? C29 C30 C31 . . 119.7(4) ? C29 C30 H30 . . 120.2 ? C31 C30 H30 . . 120.2 ? C30 C31 C32 . . 119.5(4) ? C30 C31 C52 . 3_776 121.2(4) ? C32 C31 C52 . 3_776 119.3(4) ? C27 C32 C31 . . 121.0(4) ? C27 C32 H32 . . 119.5 ? C31 C32 H32 . . 119.5 ? O1 C33 C34 . . 107.9(4) ? O1 C33 H33A . . 110.1 ? C34 C33 H33A . . 110.1 ? O1 C33 H33B . . 110.1 ? C34 C33 H33B . . 110.1 ? H33A C33 H33B . . 108.4 ? C35 C34 C39 . . 117.8(5) ? C35 C34 C33 . . 120.7(5) ? C39 C34 C33 . . 121.5(5) ? C36 C35 C34 . . 121.9(5) ? C36 C35 H35 . . 119.0 ? C34 C35 H35 . . 119.0 ? C35 C36 C37 . . 119.8(5) ? C35 C36 H36 . . 120.1 ? C37 C36 H36 . . 120.1 ? C38 C37 C36 . . 119.9(6) ? C38 C37 H37 . . 120.0 ? C36 C37 H37 . . 120.0 ? C37 C38 C39 . . 119.9(6) ? C37 C38 H38 . . 120.0 ? C39 C38 H38 . . 120.0 ? C38 C39 C34 . . 120.6(5) ? C38 C39 H39 . . 119.7 ? C34 C39 H39 . . 119.7 ? N4 C40 C41 . . 123.1(6) ? N4 C40 H40 . . 118.4 ? C41 C40 H40 . . 118.4 ? C42 C41 C40 . . 117.2(6) ? C42 C41 H41 . . 121.4 ? C40 C41 H41 . . 121.4 ? C43 C42 C41 . . 120.6(6) ? C43 C42 H42 . . 119.7 ? C41 C42 H42 . . 119.7 ? C42 C43 C44 . . 119.2(6) ? C42 C43 H43 . . 120.4 ? C44 C43 H43 . . 120.4 ? N4 C44 C43 . . 121.0(5) ? N4 C44 C45 . . 116.0(4) ? C43 C44 C45 . . 123.0(5) ? N5 C45 C46 . . 120.4(5) ? N5 C45 C44 . . 114.8(4) ? C46 C45 C44 . . 124.8(5) ? C45 C46 C47 . . 118.5(5) ? C45 C46 H46 . . 120.7 ? C47 C46 H46 . . 120.7 ? C48 C47 C46 . . 120.5(5) ? C48 C47 H47 . . 119.8 ? C46 C47 H47 . . 119.8 ? C49 C48 C47 . . 117.8(5) ? C49 C48 H48 . . 121.1 ? C47 C48 H48 . . 121.1 ? N5 C49 C48 . . 122.3(4) ? N5 C49 C50 . . 113.1(4) ? C48 C49 C50 . . 124.5(4) ? N6 C50 C49 . . 121.5(4) ? N6 C50 S2 . . 114.2(3) ? C49 C50 S2 . . 123.9(3) ? C52 C51 S2 . . 111.6(4) ? C52 C51 H51 . . 124.2 ? S2 C51 H51 . . 124.2 ? C51 C52 N6 . . 113.6(4) ? C51 C52 C31 . 3_776 126.8(4) ? N6 C52 C31 . 3_776 119.6(4) ? N7 C53 C54 . . 173.6(10) ? N8 C55 C56 . . 170.7(15) ? _database_code_depnum_ccdc_archive 'CCDC 945479' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_becky_ph3cd_0ma _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H56 Cd2 N6 S4, 4(Cl O4), C H Cl3, 0.47(C N O2), 1.05(O)' _chemical_formula_sum 'C95.95 H60.51 Cd2 Cl7 N6.95 O18.95 S4' _chemical_formula_weight 2215.01 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 Orthorhombic _symmetry_space_group_name_H-M 'Cmca ' _symmetry_space_group_name_Hall '-C 2bc 2' 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' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y, z-1/2' _cell_length_a 47.3227(17) _cell_length_b 21.8469(8) _cell_length_c 17.0480(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 17625.2(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 29.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8923 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.8387 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56917 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0486 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 30.51 _reflns_number_total 13590 _reflns_number_gt 9178 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The hydrogen atoms for the disordered nitromethane and water molecules could not be located. However, the molecular formula includes these missing atoms. Least squares restraints used in refinement SADI 0.005 O21 O25 O4 O1 SADI 0.005 Cl2 O18 Cl6 O1 SADI 0.005 Cl2 O18 Cl6 O4 DELU O15 C76 O4 O1 DELU 0.003 C39 C17 SIMU O15 C76 O1 O4 SIMU 0.003 C39 C17 ISOR 0.01 O4 O1 ISOR 0.01 O2 ; _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^)+(0.0769P)^2^+78.7809P] 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 13590 _refine_ls_number_parameters 628 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1674 _refine_ls_wR_factor_gt 0.1451 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.004 _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 0.637878(6) 0.625138(11) 0.303699(14) 0.02193(8) Uani 1 1 d . . . Cl2 Cl 0.28054(2) 0.84173(4) 0.39904(5) 0.0298(2) Uani 1 1 d D . . Cl3 Cl 0.5000 0.62757(6) 0.70119(8) 0.0310(3) Uani 1 2 d S . . S4 S 0.58035(3) 0.45316(5) 0.24656(6) 0.0357(2) Uani 1 1 d . . . S5 S 0.68939(4) 0.29322(6) 0.48394(7) 0.0596(4) Uani 1 1 d . . . Cl6 Cl 0.59190(7) 0.5000 1.0000 0.1044(11) Uani 1 2 d SD . . O8 O 0.52482(7) 0.62885(14) 0.7501(2) 0.0452(8) Uani 1 1 d . . . N9 N 0.60600(7) 0.54138(13) 0.31399(17) 0.0225(6) Uani 1 1 d . . . C10 C 0.66649(8) 0.36219(15) 0.58552(18) 0.0203(7) Uani 1 1 d . . . O11 O 0.27734(7) 0.89846(14) 0.44103(18) 0.0409(7) Uani 1 1 d . . . N12 N 0.67901(7) 0.65509(14) 0.23486(18) 0.0262(6) Uani 1 1 d . . . N13 N 0.64835(7) 0.55475(14) 0.20748(17) 0.0239(6) Uani 1 1 d . . . O14 O 0.5000 0.6800(2) 0.6499(3) 0.0430(11) Uani 1 2 d S . . O15 O 0.5000 0.57246(19) 0.6548(3) 0.0409(10) Uani 1 2 d S . . C16 C 0.68681(8) 0.62049(17) 0.1735(2) 0.0258(7) Uani 1 1 d . . . C17 C 0.62289(9) 0.28979(14) 0.6256(2) 0.0267(7) Uani 1 1 d U . . O18 O 0.27139(10) 0.8496(2) 0.31946(18) 0.0638(12) Uani 1 1 d D . . C19 C 0.59914(8) 0.32758(15) 0.7592(2) 0.0230(7) Uani 1 1 d . . . C20 C 0.69359(9) 0.70636(18) 0.2495(2) 0.0295(8) Uani 1 1 d . . . H20 H 0.6884 0.7303 0.2938 0.035 Uiso 1 1 calc R . . O21 O 0.30944(7) 0.82321(15) 0.3999(2) 0.0482(8) Uani 1 1 d D . . C22 C 0.59657(8) 0.58847(16) 0.4720(2) 0.0232(7) Uani 1 1 d . . . H22 H 0.6151 0.5743 0.4604 0.028 Uiso 1 1 calc R . . C23 C 0.63289(8) 0.50289(17) 0.2032(2) 0.0259(7) Uani 1 1 d . . . C24 C 0.67124(8) 0.56183(17) 0.1625(2) 0.0257(7) Uani 1 1 d . . . O25 O 0.26397(8) 0.79581(16) 0.4373(2) 0.0558(10) Uani 1 1 d D . . C26 C 0.69905(9) 0.4484(2) 0.6022(2) 0.0340(9) Uani 1 1 d . . . C27 C 0.68362(8) 0.54829(19) 0.6459(2) 0.0291(8) Uani 1 1 d . . . C28 C 0.59240(8) 0.62330(16) 0.5391(2) 0.0242(7) Uani 1 1 d . . . C29 C 0.60851(8) 0.50139(16) 0.2561(2) 0.0259(7) Uani 1 1 d . . . C30 C 0.71593(9) 0.72629(19) 0.2032(2) 0.0337(9) Uani 1 1 d . . . H30 H 0.7259 0.7628 0.2156 0.040 Uiso 1 1 calc R . . C31 C 0.63977(10) 0.6876(2) 0.6987(2) 0.0370(10) Uani 1 1 d . . . H31 H 0.6402 0.7212 0.7341 0.044 Uiso 1 1 calc R . . C34 C 0.61609(8) 0.63274(16) 0.5948(2) 0.0263(7) Uani 1 1 d . . . C35 C 0.63789(8) 0.59021(17) 0.5977(2) 0.0246(7) Uani 1 1 d . . . H35 H 0.6373 0.5563 0.5629 0.029 Uiso 1 1 calc R . . C36 C 0.58075(8) 0.53445(17) 0.3530(2) 0.0272(8) Uani 1 1 d . . . C37 C 0.70856(9) 0.63804(19) 0.1232(2) 0.0314(8) Uani 1 1 d . . . H37 H 0.7133 0.6136 0.0790 0.038 Uiso 1 1 calc R . . C38 C 0.58749(10) 0.3503(2) 0.8241(3) 0.0422(11) Uani 1 1 d . . . H38 H 0.5972 0.3820 0.8510 0.051 Uiso 1 1 calc R . . C39 C 0.59988(11) 0.25934(18) 0.6485(3) 0.0388(9) Uani 1 1 d U . . C40 C 0.64024(9) 0.45533(18) 0.1525(2) 0.0326(9) Uani 1 1 d . . . H40 H 0.6293 0.4190 0.1502 0.039 Uiso 1 1 calc R . . C41 C 0.63791(12) 0.27195(18) 0.5640(3) 0.0418(12) Uani 1 1 d . . . C42 C 0.66065(8) 0.59513(18) 0.6498(2) 0.0270(7) Uani 1 1 d . . . C43 C 0.66117(10) 0.6448(2) 0.7011(2) 0.0332(9) Uani 1 1 d . . . H43 H 0.6762 0.6491 0.7376 0.040 Uiso 1 1 calc R . . C44 C 0.54768(10) 0.5960(2) 0.4365(3) 0.0419(11) Uani 1 1 d . . . H44 H 0.5324 0.5869 0.4022 0.050 Uiso 1 1 calc R . . C45 C 0.56536(9) 0.6459(2) 0.5533(3) 0.0377(9) Uani 1 1 d . . . H45 H 0.5620 0.6711 0.5978 0.045 Uiso 1 1 calc R . . C46 C 0.72320(9) 0.6915(2) 0.1386(3) 0.0361(9) Uani 1 1 d . . . H46 H 0.7381 0.7042 0.1050 0.043 Uiso 1 1 calc R . . C47 C 0.67954(9) 0.5160(2) 0.1109(2) 0.0348(9) Uani 1 1 d . . . H47 H 0.6958 0.5211 0.0791 0.042 Uiso 1 1 calc R . . C48 C 0.67790(8) 0.49064(18) 0.6148(2) 0.0282(8) Uani 1 1 d . . . H48 H 0.6590 0.4802 0.6019 0.034 Uiso 1 1 calc R . . C49 C 0.66241(12) 0.3103(2) 0.5470(2) 0.0411(12) Uani 1 1 d . . . C50 C 0.73265(11) 0.5196(2) 0.6559(3) 0.0516(13) Uani 1 1 d . . . H50 H 0.7515 0.5294 0.6709 0.062 Uiso 1 1 calc R . . C51 C 0.56415(10) 0.4879(2) 0.3244(2) 0.0343(9) Uani 1 1 d . . . H51 H 0.5462 0.4766 0.3449 0.041 Uiso 1 1 calc R . . C52 C 0.57461(8) 0.57360(18) 0.4209(2) 0.0279(8) Uani 1 1 d . . . C53 C 0.70700(12) 0.3578(2) 0.5108(3) 0.0498(13) Uani 1 1 d . . . H53 H 0.7248 0.3704 0.4907 0.060 Uiso 1 1 calc R . . C54 C 0.58559(10) 0.28290(19) 0.7203(3) 0.0416(11) Uani 1 1 d . . . C55 C 0.61755(9) 0.68279(19) 0.6459(2) 0.0331(8) Uani 1 1 d . . . H55 H 0.6033 0.7135 0.6444 0.040 Uiso 1 1 calc R . . C56 C 0.71141(10) 0.5617(2) 0.6673(3) 0.0407(10) Uani 1 1 d . . . H56 H 0.7157 0.6003 0.6901 0.049 Uiso 1 1 calc R . . C57 C 0.66366(10) 0.4624(2) 0.1062(3) 0.0393(10) Uani 1 1 d . . . H57 H 0.6691 0.4308 0.0710 0.047 Uiso 1 1 calc R . . C58 C 0.54331(10) 0.6318(3) 0.5025(3) 0.0499(13) Uani 1 1 d . . . H58 H 0.5249 0.6469 0.5133 0.060 Uiso 1 1 calc R . . C59 C 0.69145(10) 0.3890(2) 0.5660(2) 0.0357(10) Uani 1 1 d . . . C60 C 0.59194(15) 0.2057(2) 0.6080(4) 0.0634(18) Uani 1 1 d . . . H60 H 0.5759 0.1830 0.6246 0.076 Uiso 1 1 calc R . . C61 C 0.72681(10) 0.4633(3) 0.6228(3) 0.0494(13) Uani 1 1 d . . . H61 H 0.7416 0.4347 0.6140 0.059 Uiso 1 1 calc R . . C62 C 0.56223(12) 0.3304(3) 0.8540(4) 0.0587(15) Uani 1 1 d . . . H62 H 0.5547 0.3474 0.9009 0.070 Uiso 1 1 calc R . . C64 C 0.60732(18) 0.1865(2) 0.5453(4) 0.075(2) Uani 1 1 d . . . H64 H 0.6021 0.1504 0.5179 0.090 Uiso 1 1 calc R . . C65 C 0.63047(16) 0.2196(2) 0.5219(3) 0.0629(18) Uani 1 1 d . . . H65 H 0.6413 0.2071 0.4777 0.075 Uiso 1 1 calc R . . C66 C 0.55965(12) 0.2606(2) 0.7461(4) 0.0589(16) Uani 1 1 d . . . H66 H 0.5501 0.2294 0.7176 0.071 Uiso 1 1 calc R . . C68 C 0.54805(12) 0.2846(3) 0.8136(5) 0.070(2) Uani 1 1 d . . . H68 H 0.5304 0.2698 0.8324 0.084 Uiso 1 1 calc R . . C70 C 0.5000 0.1530(5) 0.5684(7) 0.087(3) Uani 1 2 d S . . H70 H 0.5000 0.1637 0.6255 0.105 Uiso 1 2 calc SR . . Cl1 Cl 0.53039(5) 0.10801(11) 0.54942(12) 0.0928(6) Uani 1 1 d . . . O72 O 0.5000 0.5902(6) 0.2617(5) 0.130(5) Uani 0.474(6) 1 d P A 1 C76 C 0.5000 0.5178(6) 0.1613(10) 0.110(5) Uani 0.474(6) 1 d P A 1 O63 O 0.5000 0.6198(4) 0.1511(7) 0.118(4) Uani 0.474(6) 1 d P A 1 N67 N 0.5000 0.5744(5) 0.2003(7) 0.082(3) Uani 0.474(6) 1 d P A 1 O2 O 0.4712(3) 0.5288(6) 0.1427(8) 0.125(5) Uani 0.526(6) 1 d PU A 2 O1 O 0.61093(12) 0.5471(2) 1.0304(3) 0.1042(19) Uani 1 1 d DU . . Cl7 Cl 0.5000 0.2180(2) 0.5174(3) 0.209(3) Uani 1 2 d S . . O4 O 0.57749(14) 0.5271(4) 0.9354(3) 0.156(3) Uani 1 1 d DU . . 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 0.02346(14) 0.02066(12) 0.02167(12) -0.00246(9) 0.00213(10) -0.00012(9) Cl2 0.0260(5) 0.0343(5) 0.0289(4) 0.0033(4) 0.0011(4) 0.0002(4) Cl3 0.0239(6) 0.0280(6) 0.0413(7) -0.0026(5) 0.000 0.000 S4 0.0403(6) 0.0353(5) 0.0315(5) -0.0061(4) -0.0036(4) -0.0138(5) S5 0.1037(12) 0.0468(7) 0.0282(5) 0.0011(5) 0.0143(6) 0.0440(7) Cl6 0.106(2) 0.159(3) 0.0488(12) 0.0536(17) 0.000 0.000 O8 0.0347(18) 0.0451(18) 0.056(2) -0.0056(15) -0.0142(16) -0.0005(14) N9 0.0222(15) 0.0231(13) 0.0222(13) -0.0007(11) -0.0007(12) -0.0018(11) C10 0.0292(19) 0.0190(14) 0.0126(13) -0.0005(11) -0.0008(13) 0.0120(13) O11 0.045(2) 0.0396(16) 0.0383(16) -0.0054(13) -0.0025(14) 0.0048(14) N12 0.0247(17) 0.0278(15) 0.0260(15) 0.0002(12) 0.0009(13) 0.0007(12) N13 0.0253(16) 0.0236(14) 0.0226(14) -0.0017(11) -0.0011(12) 0.0032(12) O14 0.042(3) 0.033(2) 0.054(3) 0.007(2) 0.000 0.000 O15 0.032(2) 0.032(2) 0.059(3) -0.010(2) 0.000 0.000 C16 0.0221(18) 0.0337(19) 0.0214(15) 0.0020(14) -0.0022(14) 0.0060(15) C17 0.040(2) 0.0130(13) 0.0275(15) 0.0000(11) -0.0207(14) 0.0027(12) O18 0.085(3) 0.076(3) 0.0295(16) -0.0048(17) -0.0112(18) 0.030(2) C19 0.0188(17) 0.0196(15) 0.0306(17) 0.0064(13) -0.0043(14) -0.0059(13) C20 0.028(2) 0.0313(18) 0.0294(18) 0.0006(15) -0.0018(16) -0.0024(16) O21 0.0306(18) 0.0383(17) 0.076(2) 0.0118(16) 0.0014(17) 0.0051(13) C22 0.0208(18) 0.0238(16) 0.0250(16) 0.0015(13) 0.0003(13) 0.0007(13) C23 0.030(2) 0.0263(17) 0.0214(16) -0.0010(13) -0.0041(14) 0.0020(14) C24 0.0252(19) 0.0305(18) 0.0214(16) -0.0006(13) -0.0005(14) 0.0049(15) O25 0.043(2) 0.050(2) 0.075(3) 0.0076(18) 0.0161(19) -0.0147(16) C26 0.029(2) 0.042(2) 0.0315(19) 0.0115(17) 0.0073(17) 0.0075(17) C27 0.024(2) 0.038(2) 0.0259(17) 0.0092(15) -0.0016(15) -0.0024(15) C28 0.0215(18) 0.0272(16) 0.0238(16) -0.0008(13) 0.0018(13) 0.0001(14) C29 0.030(2) 0.0227(16) 0.0245(16) 0.0004(13) -0.0050(15) -0.0031(14) C30 0.027(2) 0.035(2) 0.040(2) 0.0079(17) -0.0025(17) -0.0033(16) C31 0.040(3) 0.037(2) 0.034(2) -0.0122(17) 0.0032(19) -0.0045(18) C34 0.027(2) 0.0276(17) 0.0239(16) 0.0007(14) 0.0021(14) -0.0007(14) C35 0.0255(19) 0.0268(16) 0.0213(15) -0.0014(13) 0.0018(14) -0.0006(14) C36 0.025(2) 0.0313(18) 0.0249(17) 0.0011(14) -0.0015(15) -0.0057(15) C37 0.025(2) 0.041(2) 0.0283(18) 0.0043(16) 0.0044(15) 0.0057(16) C38 0.030(2) 0.042(2) 0.055(3) 0.012(2) 0.006(2) -0.0059(19) C39 0.050(2) 0.0222(15) 0.0439(19) 0.0041(14) -0.0247(17) -0.0013(14) C40 0.039(2) 0.0279(18) 0.0310(19) -0.0070(15) -0.0060(17) 0.0027(16) C41 0.072(4) 0.0203(17) 0.033(2) -0.0024(15) -0.021(2) 0.013(2) C42 0.0222(19) 0.0336(19) 0.0252(17) 0.0020(15) 0.0012(14) -0.0048(15) C43 0.034(2) 0.038(2) 0.0274(18) -0.0025(16) -0.0027(16) -0.0083(17) C44 0.022(2) 0.066(3) 0.038(2) -0.009(2) -0.0008(18) -0.001(2) C45 0.029(2) 0.048(2) 0.036(2) -0.0070(19) 0.0028(18) 0.0077(19) C46 0.026(2) 0.046(2) 0.036(2) 0.0099(18) 0.0072(17) 0.0037(17) C47 0.029(2) 0.043(2) 0.032(2) -0.0106(17) 0.0014(17) 0.0082(17) C48 0.0230(19) 0.0358(19) 0.0258(17) 0.0064(15) 0.0015(14) 0.0034(15) C49 0.069(3) 0.034(2) 0.0207(17) -0.0004(15) -0.0046(19) 0.026(2) C50 0.027(2) 0.060(3) 0.069(3) 0.021(3) -0.008(2) -0.006(2) C51 0.032(2) 0.041(2) 0.0298(18) -0.0013(17) -0.0035(17) -0.0122(18) C52 0.0240(19) 0.0315(18) 0.0282(18) 0.0019(15) -0.0011(15) -0.0035(15) C53 0.056(3) 0.057(3) 0.036(2) 0.013(2) 0.020(2) 0.033(2) C54 0.038(3) 0.0272(19) 0.059(3) 0.0168(19) -0.019(2) -0.0069(17) C55 0.030(2) 0.034(2) 0.035(2) -0.0090(16) 0.0023(17) 0.0001(17) C56 0.029(2) 0.047(2) 0.046(2) 0.013(2) -0.0071(19) -0.0089(19) C57 0.041(3) 0.040(2) 0.036(2) -0.0143(18) -0.0040(19) 0.0125(19) C58 0.020(2) 0.084(4) 0.045(3) -0.011(3) 0.0012(19) 0.011(2) C59 0.038(2) 0.043(2) 0.0256(18) 0.0100(16) 0.0075(17) 0.0218(19) C60 0.088(5) 0.027(2) 0.076(4) 0.005(2) -0.049(4) -0.012(2) C61 0.024(2) 0.062(3) 0.063(3) 0.023(3) 0.008(2) 0.013(2) C62 0.037(3) 0.058(3) 0.081(4) 0.024(3) 0.017(3) -0.001(2) C64 0.135(7) 0.023(2) 0.066(4) -0.012(2) -0.056(4) 0.002(3) C65 0.119(6) 0.028(2) 0.041(3) -0.010(2) -0.034(3) 0.019(3) C66 0.040(3) 0.041(3) 0.096(4) 0.022(3) -0.019(3) -0.017(2) C68 0.029(3) 0.061(3) 0.121(6) 0.042(4) 0.002(3) -0.010(3) C70 0.094(9) 0.094(8) 0.075(7) -0.011(6) 0.000 0.000 Cl1 0.0839(14) 0.1121(15) 0.0825(12) 0.0018(11) 0.0135(11) -0.0212(12) O72 0.157(10) 0.179(11) 0.054(5) -0.039(6) 0.000 0.000 C76 0.108(13) 0.077(8) 0.147(13) 0.046(9) 0.000 0.000 O63 0.093(7) 0.077(6) 0.183(11) 0.035(6) 0.000 0.000 N67 0.070(6) 0.067(6) 0.110(8) -0.015(5) 0.000 0.000 O2 0.122(8) 0.126(8) 0.126(8) 0.014(6) 0.001(7) -0.021(7) O1 0.154(5) 0.062(3) 0.097(4) -0.007(3) -0.007(4) 0.015(3) Cl7 0.378(10) 0.081(2) 0.169(5) 0.036(3) 0.000 0.000 O4 0.128(5) 0.254(8) 0.087(4) 0.043(5) -0.003(4) 0.045(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N13 2.302(3) . ? Cd1 C17 2.326(3) 3_566 ? Cd1 C10 2.340(3) 3_566 ? Cd1 C19 2.361(4) 3_566 ? Cd1 N12 2.365(3) . ? Cd1 N9 2.378(3) . ? Cl2 O21 1.427(3) . ? Cl2 O25 1.431(3) . ? Cl2 O18 1.435(3) . ? Cl2 O11 1.439(3) . ? Cl3 O15 1.440(4) . ? Cl3 O8 1.441(3) . ? Cl3 O8 1.441(3) 11_655 ? Cl3 O14 1.442(5) . ? S4 C29 1.707(4) . ? S4 C51 1.709(5) . ? S5 C53 1.701(7) . ? S5 C49 1.710(5) . ? Cl6 O4 1.424(4) . ? Cl6 O4 1.424(4) 3_567 ? Cl6 O1 1.463(4) . ? Cl6 O1 1.463(4) 3_567 ? N9 C29 1.324(5) . ? N9 C36 1.376(5) . ? C10 C49 1.323(5) . ? C10 C59 1.360(6) . ? C10 Cd1 2.340(3) 3_566 ? N12 C20 1.339(5) . ? N12 C16 1.343(5) . ? N13 C24 1.336(5) . ? N13 C23 1.351(5) . ? C16 C37 1.393(5) . ? C16 C24 1.490(5) . ? C17 C41 1.326(6) . ? C17 C39 1.335(6) . ? C17 Cd1 2.326(3) 3_566 ? C19 C38 1.332(6) . ? C19 C54 1.343(6) . ? C19 Cd1 2.361(4) 3_566 ? C20 C30 1.389(6) . ? C20 H20 0.9500 . ? C22 C28 1.389(5) . ? C22 C52 1.394(5) . ? C22 H22 0.9500 . ? C23 C40 1.395(5) . ? C23 C29 1.465(5) . ? C24 C47 1.391(5) . ? C26 C48 1.378(6) . ? C26 C61 1.398(7) . ? C26 C59 1.480(7) . ? C27 C48 1.393(6) . ? C27 C56 1.396(6) . ? C27 C42 1.494(6) . ? C28 C45 1.393(6) . ? C28 C34 1.483(5) . ? C30 C46 1.382(6) . ? C30 H30 0.9500 . ? C31 C43 1.380(6) . ? C31 C55 1.388(6) . ? C31 H31 0.9500 . ? C34 C35 1.389(5) . ? C34 C55 1.400(5) . ? C35 C42 1.400(5) . ? C35 H35 0.9500 . ? C36 C51 1.375(5) . ? C36 C52 1.469(5) . ? C37 C46 1.383(6) . ? C37 H37 0.9500 . ? C38 C62 1.371(7) . ? C38 H38 0.9500 . ? C39 C60 1.411(6) . ? C39 C54 1.490(7) . ? C40 C57 1.369(6) . ? C40 H40 0.9500 . ? C41 C65 1.395(6) . ? C41 C49 1.460(8) . ? C42 C43 1.393(6) . ? C43 H43 0.9500 . ? C44 C58 1.385(7) . ? C44 C52 1.391(6) . ? C44 H44 0.9500 . ? C45 C58 1.391(7) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C57 1.393(6) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C50 C56 1.376(7) . ? C50 C61 1.383(8) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C53 C59 1.376(6) . ? C53 H53 0.9500 . ? C54 C66 1.392(7) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C60 C64 1.360(10) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C68 1.387(9) . ? C62 H62 0.9500 . ? C64 C65 1.373(10) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 C68 1.380(10) . ? C66 H66 0.9500 . ? C68 H68 0.9500 . ? C70 Cl7 1.665(13) . ? C70 Cl1 1.772(7) 11_655 ? C70 Cl1 1.772(7) . ? C70 H70 1.0000 . ? O72 N67 1.102(12) . ? C76 N67 1.404(18) . ? O63 N67 1.299(13) . ? 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 N13 Cd1 C17 165.60(12) . 3_566 ? N13 Cd1 C10 121.97(12) . 3_566 ? C17 Cd1 C10 70.33(14) 3_566 3_566 ? N13 Cd1 C19 97.80(12) . 3_566 ? C17 Cd1 C19 69.47(14) 3_566 3_566 ? C10 Cd1 C19 139.80(13) 3_566 3_566 ? N13 Cd1 N12 69.77(11) . . ? C17 Cd1 N12 106.68(11) 3_566 . ? C10 Cd1 N12 83.77(11) 3_566 . ? C19 Cd1 N12 107.01(12) 3_566 . ? N13 Cd1 N9 71.04(11) . . ? C17 Cd1 N9 112.53(12) 3_566 . ? C10 Cd1 N9 113.48(10) 3_566 . ? C19 Cd1 N9 82.98(11) 3_566 . ? N12 Cd1 N9 140.49(10) . . ? O21 Cl2 O25 108.8(2) . . ? O21 Cl2 O18 109.5(2) . . ? O25 Cl2 O18 110.5(3) . . ? O21 Cl2 O11 109.9(2) . . ? O25 Cl2 O11 108.6(2) . . ? O18 Cl2 O11 109.6(2) . . ? O15 Cl3 O8 109.50(17) . . ? O15 Cl3 O8 109.50(17) . 11_655 ? O8 Cl3 O8 109.2(3) . 11_655 ? O15 Cl3 O14 109.4(3) . . ? O8 Cl3 O14 109.62(18) . . ? O8 Cl3 O14 109.62(18) 11_655 . ? C29 S4 C51 90.13(19) . . ? C53 S5 C49 90.9(2) . . ? O4 Cl6 O4 122.8(7) . 3_567 ? O4 Cl6 O1 106.0(4) . . ? O4 Cl6 O1 108.3(4) 3_567 . ? O4 Cl6 O1 108.3(4) . 3_567 ? O4 Cl6 O1 106.0(4) 3_567 3_567 ? O1 Cl6 O1 104.0(5) . 3_567 ? C29 N9 C36 111.5(3) . . ? C29 N9 Cd1 113.3(2) . . ? C36 N9 Cd1 132.2(2) . . ? C49 C10 C59 112.0(4) . . ? C49 C10 Cd1 114.7(3) . 3_566 ? C59 C10 Cd1 130.5(3) . 3_566 ? C20 N12 C16 118.3(3) . . ? C20 N12 Cd1 124.3(3) . . ? C16 N12 Cd1 117.2(3) . . ? C24 N13 C23 120.3(3) . . ? C24 N13 Cd1 120.4(2) . . ? C23 N13 Cd1 118.9(2) . . ? N12 C16 C37 121.8(4) . . ? N12 C16 C24 116.5(3) . . ? C37 C16 C24 121.7(3) . . ? C41 C17 C39 121.5(4) . . ? C41 C17 Cd1 118.8(3) . 3_566 ? C39 C17 Cd1 119.6(3) . 3_566 ? C38 C19 C54 118.9(4) . . ? C38 C19 Cd1 122.4(3) . 3_566 ? C54 C19 Cd1 117.7(3) . 3_566 ? N12 C20 C30 123.2(4) . . ? N12 C20 H20 118.4 . . ? C30 C20 H20 118.4 . . ? C28 C22 C52 122.4(4) . . ? C28 C22 H22 118.8 . . ? C52 C22 H22 118.8 . . ? N13 C23 C40 121.6(4) . . ? N13 C23 C29 114.3(3) . . ? C40 C23 C29 124.1(4) . . ? N13 C24 C47 120.6(4) . . ? N13 C24 C16 115.4(3) . . ? C47 C24 C16 124.0(4) . . ? C48 C26 C61 119.2(4) . . ? C48 C26 C59 118.4(4) . . ? C61 C26 C59 122.4(4) . . ? C48 C27 C56 118.2(4) . . ? C48 C27 C42 119.7(3) . . ? C56 C27 C42 122.0(4) . . ? C22 C28 C45 117.9(4) . . ? C22 C28 C34 119.7(3) . . ? C45 C28 C34 122.3(3) . . ? N9 C29 C23 121.0(3) . . ? N9 C29 S4 114.1(3) . . ? C23 C29 S4 124.8(3) . . ? C46 C30 C20 118.1(4) . . ? C46 C30 H30 121.0 . . ? C20 C30 H30 121.0 . . ? C43 C31 C55 121.6(4) . . ? C43 C31 H31 119.2 . . ? C55 C31 H31 119.2 . . ? C35 C34 C55 117.6(4) . . ? C35 C34 C28 119.4(3) . . ? C55 C34 C28 123.0(4) . . ? C34 C35 C42 122.9(3) . . ? C34 C35 H35 118.6 . . ? C42 C35 H35 118.6 . . ? C51 C36 N9 113.9(4) . . ? C51 C36 C52 126.7(4) . . ? N9 C36 C52 119.3(3) . . ? C46 C37 C16 119.1(4) . . ? C46 C37 H37 120.4 . . ? C16 C37 H37 120.4 . . ? C19 C38 C62 123.5(5) . . ? C19 C38 H38 118.3 . . ? C62 C38 H38 118.3 . . ? C17 C39 C60 119.2(5) . . ? C17 C39 C54 116.1(4) . . ? C60 C39 C54 124.6(5) . . ? C57 C40 C23 118.3(4) . . ? C57 C40 H40 120.8 . . ? C23 C40 H40 120.8 . . ? C17 C41 C65 120.8(5) . . ? C17 C41 C49 114.4(4) . . ? C65 C41 C49 124.7(5) . . ? C43 C42 C35 118.1(4) . . ? C43 C42 C27 123.2(4) . . ? C35 C42 C27 118.6(3) . . ? C31 C43 C42 119.8(4) . . ? C31 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C58 C44 C52 119.4(4) . . ? C58 C44 H44 120.3 . . ? C52 C44 H44 120.3 . . ? C58 C45 C28 120.1(4) . . ? C58 C45 H45 119.9 . . ? C28 C45 H45 119.9 . . ? C30 C46 C37 119.3(4) . . ? C30 C46 H46 120.3 . . ? C37 C46 H46 120.3 . . ? C24 C47 C57 119.3(4) . . ? C24 C47 H47 120.4 . . ? C57 C47 H47 120.4 . . ? C26 C48 C27 121.6(4) . . ? C26 C48 H48 119.2 . . ? C27 C48 H48 119.2 . . ? C10 C49 C41 120.6(4) . . ? C10 C49 S5 113.0(4) . . ? C41 C49 S5 126.3(3) . . ? C56 C50 C61 120.4(5) . . ? C56 C50 H50 119.8 . . ? C61 C50 H50 119.8 . . ? C36 C51 S4 110.4(3) . . ? C36 C51 H51 124.8 . . ? S4 C51 H51 124.8 . . ? C44 C52 C22 118.8(4) . . ? C44 C52 C36 122.5(4) . . ? C22 C52 C36 118.7(4) . . ? C59 C53 S5 109.5(4) . . ? C59 C53 H53 125.3 . . ? S5 C53 H53 125.3 . . ? C19 C54 C66 121.4(5) . . ? C19 C54 C39 116.1(4) . . ? C66 C54 C39 122.6(5) . . ? C31 C55 C34 120.0(4) . . ? C31 C55 H55 120.0 . . ? C34 C55 H55 120.0 . . ? C50 C56 C27 120.8(5) . . ? C50 C56 H56 119.6 . . ? C27 C56 H56 119.6 . . ? C40 C57 C47 119.9(4) . . ? C40 C57 H57 120.1 . . ? C47 C57 H57 120.1 . . ? C44 C58 C45 121.3(4) . . ? C44 C58 H58 119.4 . . ? C45 C58 H58 119.4 . . ? C10 C59 C53 114.7(5) . . ? C10 C59 C26 119.1(3) . . ? C53 C59 C26 126.1(5) . . ? C64 C60 C39 119.9(6) . . ? C64 C60 H60 120.1 . . ? C39 C60 H60 120.1 . . ? C50 C61 C26 119.8(5) . . ? C50 C61 H61 120.1 . . ? C26 C61 H61 120.1 . . ? C38 C62 C68 117.8(6) . . ? C38 C62 H62 121.1 . . ? C68 C62 H62 121.1 . . ? C60 C64 C65 119.6(5) . . ? C60 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C41 118.9(6) . . ? C64 C65 H65 120.5 . . ? C41 C65 H65 120.5 . . ? C68 C66 C54 118.7(5) . . ? C68 C66 H66 120.6 . . ? C54 C66 H66 120.6 . . ? C66 C68 C62 119.8(5) . . ? C66 C68 H68 120.1 . . ? C62 C68 H68 120.1 . . ? Cl7 C70 Cl1 112.2(5) . 11_655 ? Cl7 C70 Cl1 112.2(5) . . ? Cl1 C70 Cl1 108.5(6) 11_655 . ? Cl7 C70 H70 107.9 . . ? Cl1 C70 H70 107.9 11_655 . ? Cl1 C70 H70 107.9 . . ? O72 N67 O63 111.9(12) . . ? O72 N67 C76 136.6(14) . . ? O63 N67 C76 111.5(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.656 _refine_diff_density_min -1.489 _refine_diff_density_rms 0.127 _database_code_depnum_ccdc_archive 'CCDC 949899'