# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Alan H. Cowley' _publ_contact_author_address ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_phone 512-471-7710 _publ_contact_author_fax 512-471-6822 _publ_contact_author_email cowley@mail.utexas.edu # 2. TITLE AND AUTHOR LIST _publ_section_title ; Controlling the oxidation state of arsenic in cyclic arsenic cations ; loop_ _publ_author_name _publ_author_address 'Alan H. Cowley' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; 'Gregor Reeske' ; Department of Chemistry and Biochemistry University of Texas-Austin 1 University Station, A5300 Austin, TX 78701 USA ; _publ_section_exptl_prep ; ; data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 295977' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H43 As N3, As I4' _chemical_formula_sum 'C33 H43 As2 I4 N3 ' _chemical_formula_weight 1139.14 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 10.668(2) _cell_length_b 14.692(3) _cell_length_c 17.074(3) _cell_angle_alpha 105.32(3) _cell_angle_beta 98.94(3) _cell_angle_gamma 107.50(3) _cell_volume 2380.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 4.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.886 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17234 _diffrn_reflns_av_R_equivalents 0.0762 _diffrn_reflns_av_sigmaI/netI 0.2814 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.56 _reflns_number_total 10689 _reflns_number_gt 3873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. One molecule of what appeared to be dichloromethane was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.0782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00095(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10689 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1784 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6744(10) 0.5716(7) 0.8427(7) 0.038(3) Uani 1 1 d . . . H7A H 0.7111 0.6024 0.9024 0.056 Uiso 1 1 calc R . . H7B H 0.7061 0.5173 0.8226 0.056 Uiso 1 1 calc R . . H7C H 0.5769 0.5455 0.8301 0.056 Uiso 1 1 calc R . . C2 C 0.7195(10) 0.6487(8) 0.8008(7) 0.034(3) Uani 1 1 d . . . C3 C 0.7088(10) 0.6256(7) 0.7130(7) 0.031(3) Uani 1 1 d . . . C4 C 0.6531(10) 0.5272(8) 0.6533(7) 0.036(3) Uani 1 1 d . . . H2 H 0.6179 0.4709 0.6693 0.043 Uiso 1 1 calc R . . C5 C 0.6523(10) 0.5170(8) 0.5692(7) 0.035(3) Uani 1 1 d . . . H3 H 0.6171 0.4527 0.5293 0.042 Uiso 1 1 calc R . . C6 C 0.7029(10) 0.6007(8) 0.5436(6) 0.032(3) Uani 1 1 d . . . H4 H 0.6994 0.5928 0.4874 0.039 Uiso 1 1 calc R . . C7 C 0.7588(10) 0.6962(8) 0.6046(6) 0.029(3) Uani 1 1 d . . . C8 C 0.8161(10) 0.7921(8) 0.5894(7) 0.032(3) Uani 1 1 d . . . C9 C 0.8151(11) 0.7959(9) 0.5035(6) 0.040(3) Uani 1 1 d . . . H9A H 0.8360 0.8645 0.5043 0.060 Uiso 1 1 calc R . . H9B H 0.7268 0.7548 0.4666 0.060 Uiso 1 1 calc R . . H9C H 0.8819 0.7709 0.4839 0.060 Uiso 1 1 calc R . . C10 C 0.7991(11) 0.7886(8) 0.9292(7) 0.037(3) Uani 1 1 d . . . C11 C 0.9284(11) 0.8130(8) 0.9830(7) 0.041(3) Uani 1 1 d . . . C12 C 0.9468(11) 0.8543(8) 1.0683(7) 0.044(3) Uani 1 1 d . . . H12 H 1.0298 0.8686 1.1048 0.053 Uiso 1 1 calc R . . C13 C 0.8431(13) 0.8749(9) 1.1001(7) 0.050(3) Uani 1 1 d . . . H13 H 0.8582 0.9029 1.1578 0.060 Uiso 1 1 calc R . . C14 C 0.7190(12) 0.8553(9) 1.0492(6) 0.044(3) Uani 1 1 d . . . H14 H 0.6517 0.8713 1.0721 0.053 Uiso 1 1 calc R . . C15 C 0.6940(10) 0.8106(8) 0.9616(7) 0.032(3) Uani 1 1 d . . . C16 C 1.0439(11) 0.7902(9) 0.9484(7) 0.047(3) Uani 1 1 d . . . H16 H 1.0116 0.7636 0.8870 0.056 Uiso 1 1 calc R . . C17 C 1.1700(13) 0.8838(10) 0.9710(9) 0.076(5) Uani 1 1 d . . . H17A H 1.1447 0.9374 0.9598 0.114 Uiso 1 1 calc R . . H17B H 1.2310 0.8691 0.9380 0.114 Uiso 1 1 calc R . . H17C H 1.2143 0.9041 1.0296 0.114 Uiso 1 1 calc R . . C18 C 1.0794(14) 0.7060(11) 0.9780(10) 0.075(5) Uani 1 1 d . . . H18A H 1.1414 0.6855 0.9486 0.112 Uiso 1 1 calc R . . H18B H 0.9977 0.6487 0.9660 0.112 Uiso 1 1 calc R . . H18C H 1.1208 0.7324 1.0373 0.112 Uiso 1 1 calc R . . C19 C 0.5518(10) 0.7864(9) 0.9033(7) 0.045(3) Uani 1 1 d . . . H19 H 0.5484 0.7467 0.8465 0.054 Uiso 1 1 calc R . . C20 C 0.5336(13) 0.8832(10) 0.9003(9) 0.067(4) Uani 1 1 d . . . H20A H 0.4490 0.8679 0.8612 0.100 Uiso 1 1 calc R . . H20B H 0.6071 0.9216 0.8826 0.100 Uiso 1 1 calc R . . H20C H 0.5331 0.9220 0.9551 0.100 Uiso 1 1 calc R . . C21 C 0.4380(11) 0.7226(10) 0.9336(9) 0.071(4) Uani 1 1 d . . . H21A H 0.4409 0.7599 0.9897 0.106 Uiso 1 1 calc R . . H21B H 0.4512 0.6606 0.9331 0.106 Uiso 1 1 calc R . . H21C H 0.3514 0.7077 0.8969 0.106 Uiso 1 1 calc R . . C22 C 0.9290(11) 0.9705(8) 0.6614(6) 0.032(3) Uani 1 1 d . . . C23 C 1.0657(10) 1.0036(8) 0.6586(7) 0.032(3) Uani 1 1 d . . . C24 C 1.1235(11) 1.1065(8) 0.6678(6) 0.038(3) Uani 1 1 d . . . H24 H 1.2141 1.1323 0.6669 0.045 Uiso 1 1 calc R . . C25 C 1.0533(11) 1.1701(8) 0.6780(7) 0.036(3) Uani 1 1 d . . . H25 H 1.0965 1.2378 0.6845 0.043 Uiso 1 1 calc R . . C26 C 0.9213(11) 1.1359(9) 0.6788(7) 0.039(3) Uani 1 1 d . . . H26 H 0.8739 1.1801 0.6842 0.047 Uiso 1 1 calc R . . C27 C 0.8561(10) 1.0372(8) 0.6715(6) 0.033(3) Uani 1 1 d . . . C28 C 1.1484(11) 0.9354(9) 0.6508(8) 0.052(4) Uani 1 1 d . . . H28 H 1.0853 0.8661 0.6377 0.062 Uiso 1 1 calc R . . C29 C 1.2175(13) 0.9387(9) 0.5720(9) 0.070(4) Uani 1 1 d . . . H29A H 1.1478 0.9203 0.5217 0.105 Uiso 1 1 calc R . . H29B H 1.2646 0.8920 0.5648 0.105 Uiso 1 1 calc R . . H29C H 1.2806 1.0058 0.5832 0.105 Uiso 1 1 calc R . . C30 C 1.2553(12) 0.9613(10) 0.7338(8) 0.062(4) Uani 1 1 d . . . H30A H 1.3212 1.0278 0.7472 0.093 Uiso 1 1 calc R . . H30B H 1.3000 0.9130 0.7273 0.093 Uiso 1 1 calc R . . H30C H 1.2108 0.9591 0.7784 0.093 Uiso 1 1 calc R . . C31 C 0.7050(11) 0.9960(9) 0.6700(7) 0.042(3) Uani 1 1 d . . . H31 H 0.6805 0.9249 0.6664 0.050 Uiso 1 1 calc R . . C32 C 0.6159(12) 1.0011(11) 0.5915(8) 0.071(4) Uani 1 1 d . . . H32A H 0.5220 0.9649 0.5861 0.106 Uiso 1 1 calc R . . H32B H 0.6415 0.9713 0.5422 0.106 Uiso 1 1 calc R . . H32C H 0.6292 1.0705 0.5975 0.106 Uiso 1 1 calc R . . C33 C 0.6754(12) 1.0523(10) 0.7486(8) 0.063(4) Uani 1 1 d . . . H33A H 0.7359 1.0536 0.7971 0.095 Uiso 1 1 calc R . . H33B H 0.5831 1.0188 0.7487 0.095 Uiso 1 1 calc R . . H33C H 0.6886 1.1203 0.7498 0.095 Uiso 1 1 calc R . . N1 N 0.7647(7) 0.7089(6) 0.6883(5) 0.024(2) Uani 1 1 d . . . N2 N 0.7776(8) 0.7461(6) 0.8405(5) 0.026(2) Uani 1 1 d . . . N3 N 0.8629(8) 0.8685(6) 0.6590(5) 0.0230(19) Uani 1 1 d . . . As1 As 0.84064(11) 0.83818(8) 0.76954(7) 0.0316(3) Uani 1 1 d . . . As2 As 0.81410(11) 0.42918(8) 0.39101(7) 0.0371(3) Uani 1 1 d . . . I1 I 0.57739(7) 0.27429(6) 0.35584(5) 0.0429(3) Uani 1 1 d . . . I2 I 0.94120(8) 0.36641(6) 0.52359(5) 0.0496(3) Uani 1 1 d . . . I3 I 0.70270(8) 0.52683(6) 0.29622(5) 0.0473(3) Uani 1 1 d . . . I4 I 0.91968(8) 0.34482(7) 0.27947(5) 0.0552(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(6) 0.017(6) 0.046(7) 0.000(5) -0.009(6) 0.003(5) C2 0.022(6) 0.026(7) 0.044(7) 0.001(6) -0.018(5) 0.014(5) C3 0.021(6) 0.026(6) 0.036(7) -0.004(5) -0.004(5) 0.012(5) C4 0.036(7) 0.025(6) 0.041(7) 0.003(6) 0.004(6) 0.012(5) C5 0.035(7) 0.027(6) 0.036(7) -0.001(6) -0.001(5) 0.015(5) C6 0.033(7) 0.046(7) 0.024(6) 0.017(6) 0.013(5) 0.015(6) C7 0.037(6) 0.046(7) 0.019(6) 0.013(6) 0.014(5) 0.030(6) C8 0.021(6) 0.041(7) 0.051(8) 0.030(7) 0.022(5) 0.017(5) C9 0.056(8) 0.066(8) 0.018(6) 0.028(6) 0.017(5) 0.034(7) C10 0.048(8) 0.034(7) 0.043(7) 0.018(6) 0.021(6) 0.025(6) C11 0.041(7) 0.046(7) 0.038(7) 0.008(6) 0.006(6) 0.026(6) C12 0.032(7) 0.048(8) 0.034(7) -0.006(6) -0.002(6) 0.010(6) C13 0.071(9) 0.053(8) 0.028(7) 0.001(6) 0.017(7) 0.034(7) C14 0.058(8) 0.063(8) 0.015(6) 0.005(6) 0.010(6) 0.032(7) C15 0.027(6) 0.032(6) 0.041(7) 0.018(6) 0.010(5) 0.009(5) C16 0.043(7) 0.063(9) 0.039(7) 0.018(6) 0.011(6) 0.024(7) C17 0.046(9) 0.078(11) 0.100(12) 0.035(9) 0.029(8) 0.006(8) C18 0.078(10) 0.086(11) 0.115(13) 0.063(10) 0.056(9) 0.063(9) C19 0.024(6) 0.062(8) 0.034(7) -0.001(6) 0.000(5) 0.014(6) C20 0.059(9) 0.077(10) 0.070(10) 0.025(8) 0.009(7) 0.036(8) C21 0.027(7) 0.084(11) 0.088(11) 0.010(9) 0.016(7) 0.016(7) C22 0.045(7) 0.027(6) 0.022(6) 0.000(5) 0.007(5) 0.016(5) C23 0.022(6) 0.034(7) 0.049(7) 0.018(6) 0.028(5) 0.010(5) C24 0.043(7) 0.033(7) 0.038(7) 0.017(6) 0.027(6) 0.001(6) C25 0.041(7) 0.026(6) 0.043(7) 0.016(6) 0.016(6) 0.007(6) C26 0.034(7) 0.044(7) 0.042(7) 0.018(6) 0.006(6) 0.015(6) C27 0.031(6) 0.034(7) 0.032(6) 0.006(5) 0.010(5) 0.013(5) C28 0.039(7) 0.043(8) 0.063(9) 0.014(7) 0.028(7) -0.006(6) C29 0.056(9) 0.050(9) 0.086(11) 0.014(8) 0.031(8) -0.005(7) C30 0.055(9) 0.086(11) 0.057(9) 0.024(8) 0.016(7) 0.042(8) C31 0.046(7) 0.047(7) 0.039(7) 0.010(6) 0.016(6) 0.027(6) C32 0.039(8) 0.120(13) 0.067(10) 0.046(9) 0.011(7) 0.037(8) C33 0.046(8) 0.062(9) 0.087(11) 0.020(8) 0.015(7) 0.031(7) N1 0.009(4) 0.030(5) 0.038(6) 0.014(4) 0.008(4) 0.011(4) N2 0.026(5) 0.045(6) 0.012(4) 0.006(4) 0.003(4) 0.023(4) N3 0.027(5) 0.027(5) 0.026(5) 0.016(4) 0.016(4) 0.013(4) As1 0.0364(7) 0.0284(6) 0.0306(6) 0.0084(5) 0.0092(5) 0.0135(5) As2 0.0308(7) 0.0384(7) 0.0405(7) 0.0086(6) 0.0080(6) 0.0147(5) I1 0.0310(4) 0.0390(5) 0.0528(5) 0.0087(4) 0.0087(4) 0.0110(3) I2 0.0411(5) 0.0416(5) 0.0594(6) 0.0188(4) 0.0004(4) 0.0102(4) I3 0.0463(5) 0.0485(5) 0.0456(5) 0.0165(4) 0.0044(4) 0.0178(4) I4 0.0448(5) 0.0656(6) 0.0555(6) 0.0081(5) 0.0185(4) 0.0276(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.495(15) . ? C1 H7A 0.9600 . ? C1 H7B 0.9600 . ? C1 H7C 0.9600 . ? C2 N2 1.310(12) . ? C2 C3 1.424(15) . ? C3 N1 1.395(13) . ? C3 C4 1.413(13) . ? C4 C5 1.402(14) . ? C4 H2 0.9300 . ? C5 C6 1.396(14) . ? C5 H3 0.9300 . ? C6 C7 1.394(14) . ? C6 H4 0.9300 . ? C7 N1 1.380(12) . ? C7 C8 1.466(14) . ? C8 N3 1.302(12) . ? C8 C9 1.482(14) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.409(14) . ? C10 C11 1.418(14) . ? C10 N2 1.428(13) . ? C11 C12 1.378(15) . ? C11 C16 1.533(15) . ? C12 C13 1.381(15) . ? C12 H12 0.9300 . ? C13 C14 1.368(15) . ? C13 H13 0.9300 . ? C14 C15 1.410(14) . ? C14 H14 0.9300 . ? C15 C19 1.561(13) . ? C16 C17 1.515(16) . ? C16 C18 1.575(16) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.506(16) . ? C19 C21 1.544(17) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.405(14) . ? C22 C27 1.417(14) . ? C22 N3 1.437(13) . ? C23 C24 1.406(14) . ? C23 C28 1.515(15) . ? C24 C25 1.356(14) . ? C24 H24 0.9300 . ? C25 C26 1.348(14) . ? C25 H25 0.9300 . ? C26 C27 1.369(15) . ? C26 H26 0.9300 . ? C27 C31 1.534(15) . ? C28 C30 1.551(16) . ? C28 C29 1.637(17) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C33 1.513(15) . ? C31 C32 1.552(15) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N1 As1 1.877(8) . ? N2 As1 2.080(9) . ? N3 As1 2.083(8) . ? As2 I4 2.5865(16) . ? As2 I1 2.6956(18) . ? As2 I3 2.7829(16) . ? As2 I2 2.9519(16) . ? 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 C2 C1 H7A 109.5 . . ? C2 C1 H7B 109.5 . . ? H7A C1 H7B 109.5 . . ? C2 C1 H7C 109.5 . . ? H7A C1 H7C 109.5 . . ? H7B C1 H7C 109.5 . . ? N2 C2 C3 111.3(10) . . ? N2 C2 C1 124.2(10) . . ? C3 C2 C1 124.5(9) . . ? N1 C3 C4 120.2(10) . . ? N1 C3 C2 114.7(9) . . ? C4 C3 C2 125.1(11) . . ? C5 C4 C3 118.1(11) . . ? C5 C4 H2 121.0 . . ? C3 C4 H2 121.0 . . ? C6 C5 C4 121.9(10) . . ? C6 C5 H3 119.0 . . ? C4 C5 H3 119.0 . . ? C7 C6 C5 118.3(10) . . ? C7 C6 H4 120.9 . . ? C5 C6 H4 120.9 . . ? N1 C7 C6 121.4(10) . . ? N1 C7 C8 112.8(9) . . ? C6 C7 C8 125.8(10) . . ? N3 C8 C7 111.6(9) . . ? N3 C8 C9 126.9(10) . . ? C7 C8 C9 121.6(10) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 120.8(10) . . ? C15 C10 N2 119.6(9) . . ? C11 C10 N2 119.4(9) . . ? C12 C11 C10 118.4(10) . . ? C12 C11 C16 120.2(10) . . ? C10 C11 C16 121.4(10) . . ? C11 C12 C13 120.7(11) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 122.1(11) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.4(11) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 118.6(10) . . ? C10 C15 C19 121.7(10) . . ? C14 C15 C19 119.7(10) . . ? C17 C16 C11 112.6(10) . . ? C17 C16 C18 110.6(10) . . ? C11 C16 C18 111.1(10) . . ? C17 C16 H16 107.4 . . ? C11 C16 H16 107.4 . . ? C18 C16 H16 107.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 111.7(10) . . ? C20 C19 C15 109.8(9) . . ? C21 C19 C15 110.4(10) . . ? C20 C19 H19 108.3 . . ? C21 C19 H19 108.3 . . ? C15 C19 H19 108.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 121.4(10) . . ? C23 C22 N3 119.8(9) . . ? C27 C22 N3 118.7(10) . . ? C22 C23 C24 115.2(10) . . ? C22 C23 C28 123.0(9) . . ? C24 C23 C28 121.8(9) . . ? C25 C24 C23 123.0(10) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C26 C25 C24 120.6(11) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 121.0(11) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 118.8(10) . . ? C26 C27 C31 121.9(10) . . ? C22 C27 C31 119.2(10) . . ? C23 C28 C30 112.4(10) . . ? C23 C28 C29 109.7(10) . . ? C30 C28 C29 112.2(10) . . ? C23 C28 H28 107.4 . . ? C30 C28 H28 107.4 . . ? C29 C28 H28 107.4 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C27 112.0(9) . . ? C33 C31 C32 109.8(10) . . ? C27 C31 C32 110.4(10) . . ? C33 C31 H31 108.2 . . ? C27 C31 H31 108.2 . . ? C32 C31 H31 108.2 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C7 N1 C3 120.1(9) . . ? C7 N1 As1 120.8(7) . . ? C3 N1 As1 119.1(7) . . ? C2 N2 C10 122.1(9) . . ? C2 N2 As1 117.3(7) . . ? C10 N2 As1 120.6(7) . . ? C8 N3 C22 122.4(8) . . ? C8 N3 As1 117.4(7) . . ? C22 N3 As1 120.2(6) . . ? N1 As1 N2 77.6(3) . . ? N1 As1 N3 77.4(3) . . ? N2 As1 N3 154.9(3) . . ? I4 As2 I1 98.53(5) . . ? I4 As2 I3 96.70(5) . . ? I1 As2 I3 93.88(5) . . ? I4 As2 I2 94.06(5) . . ? I1 As2 I2 91.64(5) . . ? I3 As2 I2 167.04(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N1 1.8(12) . . . . ? C1 C2 C3 N1 -176.4(9) . . . . ? N2 C2 C3 C4 178.9(9) . . . . ? C1 C2 C3 C4 0.7(16) . . . . ? N1 C3 C4 C5 -1.9(14) . . . . ? C2 C3 C4 C5 -178.8(10) . . . . ? C3 C4 C5 C6 -0.9(15) . . . . ? C4 C5 C6 C7 1.8(15) . . . . ? C5 C6 C7 N1 0.0(15) . . . . ? C5 C6 C7 C8 -179.8(9) . . . . ? N1 C7 C8 N3 1.3(12) . . . . ? C6 C7 C8 N3 -178.8(10) . . . . ? N1 C7 C8 C9 -177.7(9) . . . . ? C6 C7 C8 C9 2.2(16) . . . . ? C15 C10 C11 C12 3.1(17) . . . . ? N2 C10 C11 C12 179.7(10) . . . . ? C15 C10 C11 C16 -179.5(10) . . . . ? N2 C10 C11 C16 -2.9(16) . . . . ? C10 C11 C12 C13 -2.4(18) . . . . ? C16 C11 C12 C13 -179.8(11) . . . . ? C11 C12 C13 C14 0.1(19) . . . . ? C12 C13 C14 C15 1.5(19) . . . . ? C11 C10 C15 C14 -1.5(16) . . . . ? N2 C10 C15 C14 -178.1(10) . . . . ? C11 C10 C15 C19 178.7(10) . . . . ? N2 C10 C15 C19 2.1(15) . . . . ? C13 C14 C15 C10 -0.7(17) . . . . ? C13 C14 C15 C19 179.0(11) . . . . ? C12 C11 C16 C17 -60.0(15) . . . . ? C10 C11 C16 C17 122.6(12) . . . . ? C12 C11 C16 C18 64.6(15) . . . . ? C10 C11 C16 C18 -112.7(13) . . . . ? C10 C15 C19 C20 -109.8(12) . . . . ? C14 C15 C19 C20 70.5(14) . . . . ? C10 C15 C19 C21 126.6(11) . . . . ? C14 C15 C19 C21 -53.1(14) . . . . ? C27 C22 C23 C24 0.9(15) . . . . ? N3 C22 C23 C24 -175.3(9) . . . . ? C27 C22 C23 C28 177.9(10) . . . . ? N3 C22 C23 C28 1.6(16) . . . . ? C22 C23 C24 C25 -0.5(16) . . . . ? C28 C23 C24 C25 -177.5(11) . . . . ? C23 C24 C25 C26 -0.8(18) . . . . ? C24 C25 C26 C27 1.8(17) . . . . ? C25 C26 C27 C22 -1.4(16) . . . . ? C25 C26 C27 C31 -178.4(10) . . . . ? C23 C22 C27 C26 0.0(16) . . . . ? N3 C22 C27 C26 176.2(9) . . . . ? C23 C22 C27 C31 177.1(9) . . . . ? N3 C22 C27 C31 -6.6(14) . . . . ? C22 C23 C28 C30 -107.4(12) . . . . ? C24 C23 C28 C30 69.4(14) . . . . ? C22 C23 C28 C29 127.1(11) . . . . ? C24 C23 C28 C29 -56.1(14) . . . . ? C26 C27 C31 C33 -59.0(14) . . . . ? C22 C27 C31 C33 124.0(11) . . . . ? C26 C27 C31 C32 63.7(14) . . . . ? C22 C27 C31 C32 -113.3(12) . . . . ? C6 C7 N1 C3 -2.8(14) . . . . ? C8 C7 N1 C3 177.1(8) . . . . ? C6 C7 N1 As1 179.9(7) . . . . ? C8 C7 N1 As1 -0.2(11) . . . . ? C4 C3 N1 C7 3.7(13) . . . . ? C2 C3 N1 C7 -179.1(8) . . . . ? C4 C3 N1 As1 -178.9(7) . . . . ? C2 C3 N1 As1 -1.7(11) . . . . ? C3 C2 N2 C10 179.5(8) . . . . ? C1 C2 N2 C10 -2.3(15) . . . . ? C3 C2 N2 As1 -1.3(11) . . . . ? C1 C2 N2 As1 177.0(7) . . . . ? C15 C10 N2 C2 -84.9(12) . . . . ? C11 C10 N2 C2 98.4(12) . . . . ? C15 C10 N2 As1 95.8(10) . . . . ? C11 C10 N2 As1 -80.8(11) . . . . ? C7 C8 N3 C22 177.6(8) . . . . ? C9 C8 N3 C22 -3.5(15) . . . . ? C7 C8 N3 As1 -1.8(10) . . . . ? C9 C8 N3 As1 177.1(8) . . . . ? C23 C22 N3 C8 -79.7(12) . . . . ? C27 C22 N3 C8 104.0(11) . . . . ? C23 C22 N3 As1 99.7(10) . . . . ? C27 C22 N3 As1 -76.6(10) . . . . ? C7 N1 As1 N2 178.1(7) . . . . ? C3 N1 As1 N2 0.8(6) . . . . ? C7 N1 As1 N3 -0.5(7) . . . . ? C3 N1 As1 N3 -177.9(7) . . . . ? C2 N2 As1 N1 0.3(7) . . . . ? C10 N2 As1 N1 179.6(8) . . . . ? C2 N2 As1 N3 3.4(12) . . . . ? C10 N2 As1 N3 -177.3(7) . . . . ? C8 N3 As1 N1 1.4(7) . . . . ? C22 N3 As1 N1 -178.0(8) . . . . ? C8 N3 As1 N2 -1.7(12) . . . . ? C22 N3 As1 N2 178.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.996 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.208 # Attachment '295978.cif' data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 295978' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H43 As N3, C4 H8 Cl5 O Sn' _chemical_formula_sum 'C37 H51 As Cl5 N3 O Sn' _chemical_formula_weight 924.69 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall -P2ac2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 25.951(5) _cell_length_b 23.306(5) _cell_length_c 17.579(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10632(4) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3760 _exptl_absorpt_coefficient_mu 1.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.934 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22700 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12396 _reflns_number_gt 5981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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. One molecule of what appeared to be thf was found to be badly disordered. Attempts to model the disorder were unsatisfactory. The contributions to the scattering factors due to these solvent molecules were removed by use of the utility SQUEEZE (Sluis and Spek, 1990) in PLATON98 (Spek, 1998). PLATON98 was used as incorporated in WinGX (Farrugia, 1999). ; _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^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12396 _refine_ls_number_parameters 452 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1639 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3718(2) 0.0900(2) 0.5463(3) 0.0612(16) Uani 1 1 d . . . H1A H 0.3552 0.0634 0.5127 0.092 Uiso 1 1 calc R . . H1B H 0.3581 0.0857 0.5967 0.092 Uiso 1 1 calc R . . H1C H 0.4082 0.0826 0.5470 0.092 Uiso 1 1 calc R . . C2 C 0.3625(2) 0.1495(2) 0.5193(3) 0.0475(13) Uani 1 1 d . . . C3 C 0.37849(18) 0.1987(2) 0.5612(3) 0.0420(12) Uani 1 1 d . . . C4 C 0.40391(19) 0.1987(2) 0.6293(3) 0.0456(13) Uani 1 1 d . . . H4 H 0.4126 0.1641 0.6523 0.055 Uiso 1 1 calc R . . C5 C 0.4168(3) 0.2500 0.6642(4) 0.054(2) Uani 1 2 d S . . H5 H 0.4339 0.2500 0.7107 0.065 Uiso 1 2 calc SR . . C6 C 0.3184(2) 0.1194(2) 0.4032(3) 0.0505(14) Uani 1 1 d . . . C7 C 0.2680(2) 0.1019(2) 0.4135(4) 0.0602(16) Uani 1 1 d . . . C8 C 0.2493(3) 0.0611(3) 0.3614(4) 0.0696(18) Uani 1 1 d . . . H8 H 0.2158 0.0475 0.3670 0.084 Uiso 1 1 calc R . . C9 C 0.2784(3) 0.0411(3) 0.3037(4) 0.079(2) Uani 1 1 d . . . H11 H 0.2649 0.0141 0.2702 0.095 Uiso 1 1 calc R . . C10 C 0.3279(3) 0.0606(2) 0.2942(4) 0.0679(18) Uani 1 1 d . . . H10 H 0.3474 0.0464 0.2541 0.081 Uiso 1 1 calc R . . C11 C 0.3502(2) 0.1020(2) 0.3441(3) 0.0529(14) Uani 1 1 d . . . C12 C 0.2338(2) 0.1229(3) 0.4768(4) 0.0711(18) Uani 1 1 d . . . H32 H 0.2546 0.1489 0.5081 0.085 Uiso 1 1 calc R . . C13 C 0.1886(3) 0.1570(3) 0.4479(5) 0.099(2) Uani 1 1 d . . . H34A H 0.2003 0.1845 0.4111 0.148 Uiso 1 1 calc R . . H34B H 0.1725 0.1767 0.4896 0.148 Uiso 1 1 calc R . . H34C H 0.1641 0.1315 0.4247 0.148 Uiso 1 1 calc R . . C14 C 0.2152(3) 0.0753(3) 0.5284(5) 0.110(3) Uani 1 1 d . . . H33A H 0.2007 0.0450 0.4982 0.165 Uiso 1 1 calc R . . H33B H 0.1895 0.0900 0.5624 0.165 Uiso 1 1 calc R . . H33C H 0.2437 0.0606 0.5574 0.165 Uiso 1 1 calc R . . C15 C 0.4049(2) 0.1222(3) 0.3318(3) 0.0646(16) Uani 1 1 d . . . H12 H 0.4114 0.1521 0.3698 0.078 Uiso 1 1 calc R . . C16 C 0.4155(3) 0.1493(4) 0.2542(5) 0.112(3) Uani 1 1 d . . . H31A H 0.4106 0.1212 0.2150 0.167 Uiso 1 1 calc R . . H31B H 0.4504 0.1631 0.2526 0.167 Uiso 1 1 calc R . . H31C H 0.3923 0.1808 0.2462 0.167 Uiso 1 1 calc R . . C17 C 0.4436(3) 0.0755(3) 0.3460(5) 0.090(2) Uani 1 1 d . . . H13A H 0.4407 0.0625 0.3976 0.135 Uiso 1 1 calc R . . H13B H 0.4777 0.0901 0.3374 0.135 Uiso 1 1 calc R . . H13C H 0.4372 0.0441 0.3120 0.135 Uiso 1 1 calc R . . C18 C 0.7393(2) 0.0892(2) 0.5859(4) 0.0676(18) Uani 1 1 d . . . H18A H 0.7130 0.0630 0.5696 0.101 Uiso 1 1 calc R . . H18B H 0.7444 0.0853 0.6398 0.101 Uiso 1 1 calc R . . H18C H 0.7709 0.0808 0.5598 0.101 Uiso 1 1 calc R . . C19 C 0.72288(18) 0.1501(2) 0.5681(3) 0.0442(12) Uani 1 1 d . . . C20 C 0.75372(19) 0.1984(2) 0.5853(3) 0.0446(13) Uani 1 1 d . . . C21 C 0.8021(2) 0.1990(2) 0.6179(4) 0.0707(19) Uani 1 1 d . . . H15 H 0.8183 0.1644 0.6290 0.085 Uiso 1 1 calc R . . C22 C 0.8271(3) 0.2500 0.6345(6) 0.078(3) Uani 1 2 d S . . H14 H 0.8598 0.2500 0.6561 0.094 Uiso 1 2 calc SR . . C23 C 0.6391(2) 0.1229(2) 0.5174(3) 0.0473(13) Uani 1 1 d . . . C24 C 0.6015(2) 0.1109(2) 0.5713(3) 0.0529(14) Uani 1 1 d . . . C25 C 0.5619(2) 0.0727(2) 0.5488(4) 0.0672(18) Uani 1 1 d . . . H23 H 0.5361 0.0627 0.5831 0.081 Uiso 1 1 calc R . . C26 C 0.5614(3) 0.0510(3) 0.4786(4) 0.074(2) Uani 1 1 d . . . H22 H 0.5353 0.0255 0.4656 0.089 Uiso 1 1 calc R . . C27 C 0.5973(3) 0.0645(3) 0.4254(4) 0.078(2) Uani 1 1 d . . . H21 H 0.5949 0.0494 0.3766 0.093 Uiso 1 1 calc R . . C28 C 0.6375(2) 0.1010(2) 0.4441(3) 0.0595(15) Uani 1 1 d . . . C29 C 0.6014(2) 0.1356(3) 0.6516(4) 0.0671(17) Uani 1 1 d . . . H25 H 0.6299 0.1631 0.6544 0.081 Uiso 1 1 calc R . . C30 C 0.6109(3) 0.0911(3) 0.7110(4) 0.094(2) Uani 1 1 d . . . H26A H 0.5816 0.0661 0.7144 0.141 Uiso 1 1 calc R . . H26B H 0.6164 0.1094 0.7593 0.141 Uiso 1 1 calc R . . H26C H 0.6409 0.0692 0.6977 0.141 Uiso 1 1 calc R . . C31 C 0.5517(3) 0.1694(3) 0.6662(5) 0.098(3) Uani 1 1 d . . . H27A H 0.5228 0.1437 0.6649 0.148 Uiso 1 1 calc R . . H27B H 0.5477 0.1982 0.6276 0.148 Uiso 1 1 calc R . . H27C H 0.5536 0.1874 0.7152 0.148 Uiso 1 1 calc R . . C32 C 0.6797(3) 0.1158(3) 0.3888(4) 0.094(2) Uani 1 1 d . . . H28 H 0.7015 0.1450 0.4127 0.113 Uiso 1 1 calc R . . C33 C 0.7141(5) 0.0614(4) 0.3743(7) 0.179(6) Uani 1 1 d . . . H29A H 0.7232 0.0444 0.4222 0.268 Uiso 1 1 calc R . . H29B H 0.7448 0.0725 0.3476 0.268 Uiso 1 1 calc R . . H29C H 0.6952 0.0341 0.3444 0.268 Uiso 1 1 calc R . . C34 C 0.6535(5) 0.1443(6) 0.3139(5) 0.168(4) Uani 1 1 d U . . H30A H 0.6241 0.1220 0.2988 0.252 Uiso 1 1 calc R . . H30B H 0.6781 0.1452 0.2732 0.252 Uiso 1 1 calc R . . H30C H 0.6426 0.1828 0.3254 0.252 Uiso 1 1 calc R . . C35 C 0.5263(3) 0.9955(4) 0.8642(4) 0.097(3) Uani 1 1 d . . . H35A H 0.5279 0.9877 0.8100 0.117 Uiso 1 1 calc R . . H35B H 0.5157 0.9609 0.8905 0.117 Uiso 1 1 calc R . . C36 C 0.5778(3) 1.0163(5) 0.8935(5) 0.125(4) Uani 1 1 d . . . H36A H 0.5971 0.9851 0.9163 0.150 Uiso 1 1 calc R . . H36B H 0.5981 1.0330 0.8528 0.150 Uiso 1 1 calc R . . C37 C 0.5648(3) 1.0587(5) 0.9492(6) 0.138(4) Uani 1 1 d . . . H37A H 0.5913 1.0880 0.9509 0.166 Uiso 1 1 calc R . . H37B H 0.5626 1.0410 0.9990 0.166 Uiso 1 1 calc R . . C38 C 0.5160(3) 1.0846(3) 0.9300(5) 0.096(3) Uani 1 1 d . . . H38A H 0.5211 1.1208 0.9038 0.116 Uiso 1 1 calc R . . H38B H 0.4955 1.0913 0.9753 0.116 Uiso 1 1 calc R . . N1 N 0.3655(2) 0.2500 0.5252(3) 0.0386(13) Uani 1 2 d S . . N2 N 0.33848(15) 0.16237(17) 0.4566(2) 0.0439(10) Uani 1 1 d . . . N3 N 0.67914(15) 0.16318(16) 0.5385(2) 0.0426(10) Uani 1 1 d . . . N4 N 0.7299(2) 0.2500 0.5691(3) 0.0390(13) Uani 1 2 d S . . O1 O 0.49081(15) 1.04280(18) 0.8800(2) 0.0658(11) Uani 1 1 d . . . Cl1 Cl 0.40537(7) 0.95437(7) 0.83558(11) 0.0782(5) Uani 1 1 d . . . Cl2 Cl 0.37971(6) 1.06964(7) 0.94709(8) 0.0678(4) Uani 1 1 d . . . Cl3 Cl 0.33413(5) 1.06917(7) 0.75790(8) 0.0630(4) Uani 1 1 d . . . Cl4 Cl 0.43632(6) 1.15532(6) 0.81801(8) 0.0572(4) Uani 1 1 d . . . Cl5 Cl 0.46045(5) 1.04141(6) 0.70460(8) 0.0540(3) Uani 1 1 d . . . As2 As 0.66411(3) 0.2500 0.52427(4) 0.0431(2) Uani 1 2 d S . . Sn1 Sn 0.414729(13) 1.055519(15) 0.82175(2) 0.04535(14) Uani 1 1 d U . . As1 As 0.33094(3) 0.2500 0.43236(5) 0.0485(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.084(4) 0.037(3) 0.062(4) 0.001(3) -0.014(3) 0.011(3) C2 0.054(3) 0.033(3) 0.056(3) 0.004(3) -0.002(3) -0.001(2) C3 0.041(3) 0.038(3) 0.047(3) -0.002(2) -0.005(2) 0.002(2) C4 0.057(3) 0.029(3) 0.051(3) 0.001(2) -0.008(3) 0.002(2) C5 0.065(5) 0.053(5) 0.045(5) 0.000 -0.014(4) 0.000 C6 0.068(4) 0.024(3) 0.060(3) -0.003(2) -0.024(3) -0.003(3) C7 0.060(4) 0.042(3) 0.079(4) 0.007(3) -0.027(3) -0.011(3) C8 0.075(4) 0.052(4) 0.082(5) 0.000(4) -0.025(4) -0.010(3) C9 0.119(6) 0.051(4) 0.066(4) 0.003(3) -0.048(4) -0.015(4) C10 0.108(6) 0.038(3) 0.058(4) -0.004(3) -0.016(4) 0.005(3) C11 0.074(4) 0.039(3) 0.046(3) 0.000(3) -0.014(3) 0.006(3) C12 0.057(4) 0.059(4) 0.097(5) 0.001(4) -0.008(4) -0.016(3) C13 0.087(5) 0.070(5) 0.139(7) -0.005(5) 0.001(5) 0.001(4) C14 0.110(7) 0.085(6) 0.135(7) 0.005(5) 0.017(6) -0.008(5) C15 0.080(4) 0.048(4) 0.066(4) -0.008(3) -0.010(3) 0.005(3) C16 0.134(8) 0.094(6) 0.106(6) 0.031(5) 0.001(5) -0.005(5) C17 0.089(5) 0.075(5) 0.107(6) -0.018(4) -0.006(5) 0.003(4) C18 0.061(4) 0.030(3) 0.113(5) -0.003(3) -0.011(3) -0.002(3) C19 0.030(3) 0.035(3) 0.067(3) 0.003(3) 0.004(3) -0.001(2) C20 0.046(3) 0.027(3) 0.061(3) 0.001(2) -0.001(3) 0.004(2) C21 0.057(4) 0.028(3) 0.127(6) -0.005(3) -0.021(4) 0.005(3) C22 0.060(5) 0.034(5) 0.141(9) 0.000 -0.029(6) 0.000 C23 0.047(3) 0.034(3) 0.061(4) 0.002(3) -0.002(3) -0.007(2) C24 0.049(3) 0.033(3) 0.076(4) 0.001(3) 0.002(3) 0.003(2) C25 0.049(3) 0.042(3) 0.110(6) 0.003(4) 0.008(4) -0.007(3) C26 0.087(5) 0.042(4) 0.093(5) -0.002(4) -0.045(4) -0.022(3) C27 0.108(6) 0.051(4) 0.074(5) -0.002(3) -0.023(4) -0.024(4) C28 0.078(4) 0.044(3) 0.056(4) -0.006(3) -0.005(3) -0.007(3) C29 0.070(4) 0.055(4) 0.077(4) -0.006(3) 0.029(3) -0.014(3) C30 0.129(6) 0.087(5) 0.066(4) 0.009(4) 0.010(4) -0.003(5) C31 0.094(5) 0.054(4) 0.146(7) -0.014(4) 0.061(5) 0.003(4) C32 0.152(7) 0.057(4) 0.074(5) -0.009(4) 0.019(5) -0.013(5) C33 0.259(14) 0.074(6) 0.204(12) -0.042(6) 0.169(11) -0.013(7) C34 0.206(8) 0.196(9) 0.102(6) 0.036(6) -0.010(6) -0.056(7) C35 0.082(5) 0.138(7) 0.072(5) 0.003(4) 0.007(4) 0.070(5) C36 0.079(6) 0.199(11) 0.098(6) 0.071(7) 0.002(5) 0.057(6) C37 0.073(5) 0.230(13) 0.112(7) -0.041(8) -0.045(5) 0.011(7) C38 0.083(5) 0.082(5) 0.124(7) 0.025(5) -0.053(5) -0.012(4) N1 0.051(3) 0.022(3) 0.043(3) 0.000 -0.005(3) 0.000 N2 0.037(2) 0.031(2) 0.063(3) 0.000(2) -0.014(2) 0.0022(18) N3 0.042(2) 0.028(2) 0.058(3) -0.0041(19) -0.003(2) -0.0013(18) N4 0.038(3) 0.028(3) 0.050(4) 0.000 -0.001(3) 0.000 O1 0.056(2) 0.072(3) 0.070(3) 0.006(2) -0.006(2) 0.011(2) Cl1 0.0877(12) 0.0405(9) 0.1062(14) 0.0102(8) 0.0173(10) -0.0071(8) Cl2 0.0704(10) 0.0763(11) 0.0566(9) 0.0112(8) 0.0089(7) 0.0166(8) Cl3 0.0458(8) 0.0816(11) 0.0616(9) -0.0001(8) -0.0022(7) -0.0001(7) Cl4 0.0746(9) 0.0384(7) 0.0587(9) 0.0029(6) -0.0033(7) 0.0035(7) Cl5 0.0524(8) 0.0516(8) 0.0579(8) -0.0065(7) 0.0056(7) -0.0020(6) As2 0.0441(4) 0.0325(4) 0.0525(5) 0.000 -0.0036(3) 0.000 Sn1 0.0445(2) 0.0402(2) 0.0514(3) 0.00395(17) 0.00227(16) 0.00224(16) As1 0.0544(5) 0.0355(4) 0.0556(5) 0.000 -0.0161(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.484(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N2 1.302(6) . ? C2 C3 1.424(7) . ? C3 C4 1.367(7) . ? C3 N1 1.395(5) . ? C4 C5 1.384(6) . ? C4 H4 0.9300 . ? C5 C4 1.384(6) 7_565 ? C5 H5 0.9300 . ? C6 C7 1.381(8) . ? C6 C11 1.387(8) . ? C6 N2 1.468(6) . ? C7 C8 1.406(8) . ? C7 C12 1.505(9) . ? C8 C9 1.349(10) . ? C8 H8 0.9300 . ? C9 C10 1.371(10) . ? C9 H11 0.9300 . ? C10 C11 1.427(8) . ? C10 H10 0.9300 . ? C11 C15 1.511(8) . ? C12 C13 1.505(9) . ? C12 C14 1.513(9) . ? C12 H32 0.9800 . ? C13 H34A 0.9600 . ? C13 H34B 0.9600 . ? C13 H34C 0.9600 . ? C14 H33A 0.9600 . ? C14 H33B 0.9600 . ? C14 H33C 0.9600 . ? C15 C17 1.502(9) . ? C15 C16 1.528(9) . ? C15 H12 0.9800 . ? C16 H31A 0.9600 . ? C16 H31B 0.9600 . ? C16 H31C 0.9600 . ? C17 H13A 0.9600 . ? C17 H13B 0.9600 . ? C17 H13C 0.9600 . ? C18 C19 1.514(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N3 1.285(6) . ? C19 C20 1.415(7) . ? C20 N4 1.382(5) . ? C20 C21 1.381(7) . ? C21 C22 1.384(7) . ? C21 H15 0.9300 . ? C22 C21 1.384(7) 7_565 ? C22 H14 0.9300 . ? C23 C28 1.387(7) . ? C23 C24 1.389(7) . ? C23 N3 1.448(6) . ? C24 C25 1.416(8) . ? C24 C29 1.525(8) . ? C25 C26 1.333(9) . ? C25 H23 0.9300 . ? C26 C27 1.357(10) . ? C26 H22 0.9300 . ? C27 C28 1.384(8) . ? C27 H21 0.9300 . ? C28 C32 1.505(9) . ? C29 C30 1.493(9) . ? C29 C31 1.532(9) . ? C29 H25 0.9800 . ? C30 H26A 0.9600 . ? C30 H26B 0.9600 . ? C30 H26C 0.9600 . ? C31 H27A 0.9600 . ? C31 H27B 0.9600 . ? C31 H27C 0.9600 . ? C32 C33 1.570(11) . ? C32 C34 1.626(12) . ? C32 H28 0.9800 . ? C33 H29A 0.9600 . ? C33 H29B 0.9600 . ? C33 H29C 0.9600 . ? C34 H30A 0.9600 . ? C34 H30B 0.9600 . ? C34 H30C 0.9600 . ? C35 O1 1.463(7) . ? C35 C36 1.513(12) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.432(12) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.442(11) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 O1 1.464(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? N1 C3 1.395(5) 7_565 ? N1 As1 1.862(5) . ? N2 As1 2.095(4) . ? N3 As2 2.076(4) . ? N4 C20 1.382(5) 7_565 ? N4 As2 1.879(5) . ? O1 Sn1 2.244(4) . ? Cl1 Sn1 2.3822(16) . ? Cl2 Sn1 2.4060(15) . ? Cl3 Sn1 2.3949(14) . ? Cl4 Sn1 2.3934(15) . ? Cl5 Sn1 2.3994(15) . ? As2 N3 2.076(4) 7_565 ? As1 N2 2.095(4) 7_565 ? 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 C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 C3 113.0(4) . . ? N2 C2 C1 124.4(5) . . ? C3 C2 C1 122.6(5) . . ? C4 C3 N1 120.8(4) . . ? C4 C3 C2 126.5(5) . . ? N1 C3 C2 112.7(4) . . ? C3 C4 C5 120.4(5) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C4 119.3(7) . 7_565 ? C4 C5 H5 120.3 . . ? C4 C5 H5 120.3 7_565 . ? C7 C6 C11 125.1(5) . . ? C7 C6 N2 117.0(5) . . ? C11 C6 N2 117.8(5) . . ? C6 C7 C8 116.2(6) . . ? C6 C7 C12 124.0(5) . . ? C8 C7 C12 119.9(6) . . ? C9 C8 C7 122.0(7) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C10 120.1(6) . . ? C8 C9 H11 120.0 . . ? C10 C9 H11 120.0 . . ? C9 C10 C11 121.9(6) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C6 C11 C10 114.6(6) . . ? C6 C11 C15 125.1(5) . . ? C10 C11 C15 120.2(6) . . ? C13 C12 C7 112.5(6) . . ? C13 C12 C14 109.9(6) . . ? C7 C12 C14 113.1(6) . . ? C13 C12 H32 107.0 . . ? C7 C12 H32 107.0 . . ? C14 C12 H32 107.0 . . ? C12 C13 H34A 109.5 . . ? C12 C13 H34B 109.5 . . ? H34A C13 H34B 109.5 . . ? C12 C13 H34C 109.5 . . ? H34A C13 H34C 109.5 . . ? H34B C13 H34C 109.5 . . ? C12 C14 H33A 109.5 . . ? C12 C14 H33B 109.5 . . ? H33A C14 H33B 109.5 . . ? C12 C14 H33C 109.5 . . ? H33A C14 H33C 109.5 . . ? H33B C14 H33C 109.5 . . ? C17 C15 C11 112.2(5) . . ? C17 C15 C16 109.1(6) . . ? C11 C15 C16 115.3(5) . . ? C17 C15 H12 106.6 . . ? C11 C15 H12 106.6 . . ? C16 C15 H12 106.6 . . ? C15 C16 H31A 109.5 . . ? C15 C16 H31B 109.5 . . ? H31A C16 H31B 109.5 . . ? C15 C16 H31C 109.5 . . ? H31A C16 H31C 109.5 . . ? H31B C16 H31C 109.5 . . ? C15 C17 H13A 109.5 . . ? C15 C17 H13B 109.5 . . ? H13A C17 H13B 109.5 . . ? C15 C17 H13C 109.5 . . ? H13A C17 H13C 109.5 . . ? H13B C17 H13C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 C20 113.4(4) . . ? N3 C19 C18 123.7(4) . . ? C20 C19 C18 122.8(4) . . ? N4 C20 C21 119.0(5) . . ? N4 C20 C19 113.2(4) . . ? C21 C20 C19 127.7(5) . . ? C20 C21 C22 121.4(5) . . ? C20 C21 H15 119.3 . . ? C22 C21 H15 119.3 . . ? C21 C22 C21 118.3(8) 7_565 . ? C21 C22 H14 120.9 7_565 . ? C21 C22 H14 120.9 . . ? C28 C23 C24 122.5(5) . . ? C28 C23 N3 119.9(5) . . ? C24 C23 N3 117.4(5) . . ? C23 C24 C25 116.5(5) . . ? C23 C24 C29 123.8(5) . . ? C25 C24 C29 119.7(5) . . ? C26 C25 C24 120.3(6) . . ? C26 C25 H23 119.9 . . ? C24 C25 H23 119.9 . . ? C25 C26 C27 122.9(6) . . ? C25 C26 H22 118.6 . . ? C27 C26 H22 118.6 . . ? C26 C27 C28 119.7(6) . . ? C26 C27 H21 120.1 . . ? C28 C27 H21 120.1 . . ? C27 C28 C23 118.0(6) . . ? C27 C28 C32 122.4(6) . . ? C23 C28 C32 119.5(5) . . ? C30 C29 C24 112.6(5) . . ? C30 C29 C31 112.3(6) . . ? C24 C29 C31 110.5(6) . . ? C30 C29 H25 107.0 . . ? C24 C29 H25 107.0 . . ? C31 C29 H25 107.0 . . ? C29 C30 H26A 109.5 . . ? C29 C30 H26B 109.5 . . ? H26A C30 H26B 109.5 . . ? C29 C30 H26C 109.5 . . ? H26A C30 H26C 109.5 . . ? H26B C30 H26C 109.5 . . ? C29 C31 H27A 109.5 . . ? C29 C31 H27B 109.5 . . ? H27A C31 H27B 109.5 . . ? C29 C31 H27C 109.5 . . ? H27A C31 H27C 109.5 . . ? H27B C31 H27C 109.5 . . ? C28 C32 C33 109.5(6) . . ? C28 C32 C34 108.2(7) . . ? C33 C32 C34 115.9(8) . . ? C28 C32 H28 107.7 . . ? C33 C32 H28 107.7 . . ? C34 C32 H28 107.7 . . ? C32 C33 H29A 109.5 . . ? C32 C33 H29B 109.5 . . ? H29A C33 H29B 109.5 . . ? C32 C33 H29C 109.5 . . ? H29A C33 H29C 109.5 . . ? H29B C33 H29C 109.5 . . ? C32 C34 H30A 109.5 . . ? C32 C34 H30B 109.5 . . ? H30A C34 H30B 109.5 . . ? C32 C34 H30C 109.5 . . ? H30A C34 H30C 109.5 . . ? H30B C34 H30C 109.5 . . ? O1 C35 C36 104.5(7) . . ? O1 C35 H35A 110.9 . . ? C36 C35 H35A 110.9 . . ? O1 C35 H35B 110.9 . . ? C36 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? C37 C36 C35 104.2(7) . . ? C37 C36 H36A 110.9 . . ? C35 C36 H36A 110.9 . . ? C37 C36 H36B 110.9 . . ? C35 C36 H36B 110.9 . . ? H36A C36 H36B 108.9 . . ? C36 C37 C38 109.6(7) . . ? C36 C37 H37A 109.8 . . ? C38 C37 H37A 109.8 . . ? C36 C37 H37B 109.8 . . ? C38 C37 H37B 109.8 . . ? H37A C37 H37B 108.2 . . ? C37 C38 O1 104.8(7) . . ? C37 C38 H38A 110.8 . . ? O1 C38 H38A 110.8 . . ? C37 C38 H38B 110.8 . . ? O1 C38 H38B 110.8 . . ? H38A C38 H38B 108.9 . . ? C3 N1 C3 118.1(5) 7_565 . ? C3 N1 As1 120.9(3) 7_565 . ? C3 N1 As1 120.9(3) . . ? C2 N2 C6 123.6(4) . . ? C2 N2 As1 116.2(3) . . ? C6 N2 As1 120.1(3) . . ? C19 N3 C23 125.7(4) . . ? C19 N3 As2 116.5(3) . . ? C23 N3 As2 117.8(3) . . ? C20 N4 C20 120.9(6) 7_565 . ? C20 N4 As2 119.6(3) 7_565 . ? C20 N4 As2 119.6(3) . . ? C35 O1 C38 109.5(5) . . ? C35 O1 Sn1 124.5(4) . . ? C38 O1 Sn1 125.3(4) . . ? N4 As2 N3 77.23(11) . 7_565 ? N4 As2 N3 77.23(11) . . ? N3 As2 N3 154.2(2) 7_565 . ? O1 Sn1 Cl1 84.97(12) . . ? O1 Sn1 Cl4 86.27(11) . . ? Cl1 Sn1 Cl4 171.24(6) . . ? O1 Sn1 Cl3 179.21(11) . . ? Cl1 Sn1 Cl3 95.18(6) . . ? Cl4 Sn1 Cl3 93.58(6) . . ? O1 Sn1 Cl5 86.48(11) . . ? Cl1 Sn1 Cl5 90.14(6) . . ? Cl4 Sn1 Cl5 89.65(5) . . ? Cl3 Sn1 Cl5 92.74(5) . . ? O1 Sn1 Cl2 86.12(11) . . ? Cl1 Sn1 Cl2 90.19(6) . . ? Cl4 Sn1 Cl2 88.89(5) . . ? Cl3 Sn1 Cl2 94.65(5) . . ? Cl5 Sn1 Cl2 172.54(5) . . ? N1 As1 N2 77.12(11) . 7_565 ? N1 As1 N2 77.12(11) . . ? N2 As1 N2 154.2(2) 7_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 C4 179.3(5) . . . . ? C1 C2 C3 C4 0.3(8) . . . . ? N2 C2 C3 N1 -0.8(7) . . . . ? C1 C2 C3 N1 -179.7(5) . . . . ? N1 C3 C4 C5 0.7(8) . . . . ? C2 C3 C4 C5 -179.4(6) . . . . ? C3 C4 C5 C4 -0.4(11) . . . 7_565 ? C11 C6 C7 C8 3.2(8) . . . . ? N2 C6 C7 C8 179.4(5) . . . . ? C11 C6 C7 C12 -177.9(5) . . . . ? N2 C6 C7 C12 -1.7(8) . . . . ? C6 C7 C8 C9 -1.4(9) . . . . ? C12 C7 C8 C9 179.7(6) . . . . ? C7 C8 C9 C10 -0.1(10) . . . . ? C8 C9 C10 C11 0.0(9) . . . . ? C7 C6 C11 C10 -3.2(8) . . . . ? N2 C6 C11 C10 -179.4(4) . . . . ? C7 C6 C11 C15 178.5(5) . . . . ? N2 C6 C11 C15 2.3(8) . . . . ? C9 C10 C11 C6 1.6(8) . . . . ? C9 C10 C11 C15 179.9(6) . . . . ? C6 C7 C12 C13 115.0(6) . . . . ? C8 C7 C12 C13 -66.2(7) . . . . ? C6 C7 C12 C14 -119.8(7) . . . . ? C8 C7 C12 C14 59.1(8) . . . . ? C6 C11 C15 C17 110.7(6) . . . . ? C10 C11 C15 C17 -67.4(7) . . . . ? C6 C11 C15 C16 -123.6(7) . . . . ? C10 C11 C15 C16 58.3(8) . . . . ? N3 C19 C20 N4 1.9(7) . . . . ? C18 C19 C20 N4 -175.7(5) . . . . ? N3 C19 C20 C21 179.3(6) . . . . ? C18 C19 C20 C21 1.7(9) . . . . ? N4 C20 C21 C22 0.0(11) . . . . ? C19 C20 C21 C22 -177.3(7) . . . . ? C20 C21 C22 C21 0.4(15) . . . 7_565 ? C28 C23 C24 C25 2.7(8) . . . . ? N3 C23 C24 C25 178.2(5) . . . . ? C28 C23 C24 C29 -178.2(5) . . . . ? N3 C23 C24 C29 -2.7(8) . . . . ? C23 C24 C25 C26 -1.2(8) . . . . ? C29 C24 C25 C26 179.7(6) . . . . ? C24 C25 C26 C27 -1.2(10) . . . . ? C25 C26 C27 C28 2.1(11) . . . . ? C26 C27 C28 C23 -0.6(10) . . . . ? C26 C27 C28 C32 177.4(6) . . . . ? C24 C23 C28 C27 -1.9(9) . . . . ? N3 C23 C28 C27 -177.3(5) . . . . ? C24 C23 C28 C32 -179.9(5) . . . . ? N3 C23 C28 C32 4.7(8) . . . . ? C23 C24 C29 C30 -111.9(6) . . . . ? C25 C24 C29 C30 67.1(7) . . . . ? C23 C24 C29 C31 121.6(6) . . . . ? C25 C24 C29 C31 -59.4(7) . . . . ? C27 C28 C32 C33 -69.0(10) . . . . ? C23 C28 C32 C33 108.9(8) . . . . ? C27 C28 C32 C34 58.1(9) . . . . ? C23 C28 C32 C34 -123.9(7) . . . . ? O1 C35 C36 C37 23.6(9) . . . . ? C35 C36 C37 C38 -28.3(11) . . . . ? C36 C37 C38 O1 21.3(11) . . . . ? C4 C3 N1 C3 -0.9(9) . . . 7_565 ? C2 C3 N1 C3 179.2(4) . . . 7_565 ? C4 C3 N1 As1 179.9(4) . . . . ? C2 C3 N1 As1 -0.1(6) . . . . ? C3 C2 N2 C6 179.7(5) . . . . ? C1 C2 N2 C6 -1.4(8) . . . . ? C3 C2 N2 As1 1.2(6) . . . . ? C1 C2 N2 As1 -179.8(4) . . . . ? C7 C6 N2 C2 91.6(6) . . . . ? C11 C6 N2 C2 -91.8(6) . . . . ? C7 C6 N2 As1 -89.9(5) . . . . ? C11 C6 N2 As1 86.6(5) . . . . ? C20 C19 N3 C23 -177.9(5) . . . . ? C18 C19 N3 C23 -0.3(9) . . . . ? C20 C19 N3 As2 -0.5(6) . . . . ? C18 C19 N3 As2 177.1(4) . . . . ? C28 C23 N3 C19 -92.0(7) . . . . ? C24 C23 N3 C19 92.3(6) . . . . ? C28 C23 N3 As2 90.7(5) . . . . ? C24 C23 N3 As2 -85.0(5) . . . . ? C21 C20 N4 C20 -0.3(10) . . . 7_565 ? C19 C20 N4 C20 177.4(4) . . . 7_565 ? C21 C20 N4 As2 179.7(5) . . . . ? C19 C20 N4 As2 -2.6(7) . . . . ? C36 C35 O1 C38 -11.3(7) . . . . ? C36 C35 O1 Sn1 159.9(4) . . . . ? C37 C38 O1 C35 -5.3(9) . . . . ? C37 C38 O1 Sn1 -176.4(6) . . . . ? C20 N4 As2 N3 -1.8(4) 7_565 . . 7_565 ? C20 N4 As2 N3 178.2(5) . . . 7_565 ? C20 N4 As2 N3 -178.2(5) 7_565 . . . ? C20 N4 As2 N3 1.8(4) . . . . ? C19 N3 As2 N4 -0.7(4) . . . . ? C23 N3 As2 N4 176.9(4) . . . . ? C19 N3 As2 N3 -8.7(8) . . . 7_565 ? C23 N3 As2 N3 168.8(4) . . . 7_565 ? C35 O1 Sn1 Cl1 41.8(5) . . . . ? C38 O1 Sn1 Cl1 -148.5(5) . . . . ? C35 O1 Sn1 Cl4 -138.5(5) . . . . ? C38 O1 Sn1 Cl4 31.2(5) . . . . ? C35 O1 Sn1 Cl5 -48.7(5) . . . . ? C38 O1 Sn1 Cl5 121.1(5) . . . . ? C35 O1 Sn1 Cl2 132.3(5) . . . . ? C38 O1 Sn1 Cl2 -57.9(5) . . . . ? C3 N1 As1 N2 -0.5(4) 7_565 . . 7_565 ? C3 N1 As1 N2 178.7(5) . . . 7_565 ? C3 N1 As1 N2 -178.7(5) 7_565 . . . ? C3 N1 As1 N2 0.5(4) . . . . ? C2 N2 As1 N1 -1.0(4) . . . . ? C6 N2 As1 N1 -179.5(4) . . . . ? C2 N2 As1 N2 -5.2(8) . . . 7_565 ? C6 N2 As1 N2 176.3(4) . . . 7_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.950 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.110 # Attachment '295979.cif' data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 295979' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 As N2, C4 H8 Cl5 O Sn' _chemical_formula_sum 'C24 H32 As Cl5 N2 O Sn ' _chemical_formula_weight 735.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p2(1)/c _symmetry_space_group_name_Hall -p2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.497(4) _cell_length_b 15.947(3) _cell_length_c 20.677(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.97(3) _cell_angle_gamma 90.00 _cell_volume 6096(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 2.374 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22842 _diffrn_reflns_av_R_equivalents 0.1109 _diffrn_reflns_av_sigmaI/netI 0.2595 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13842 _reflns_number_gt 5367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _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^)+(0.0571P)^2^+66.4005P] 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 13842 _refine_ls_number_parameters 625 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2446 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2287 _refine_ls_wR_factor_gt 0.1804 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4453(7) 0.7401(8) 0.8458(6) 0.036(3) Uani 1 1 d . . . H1 H 0.4748 0.7315 0.8108 0.043 Uiso 1 1 calc R . . C2 C 0.3836(7) 0.7882(8) 0.8431(7) 0.048(4) Uani 1 1 d . . . H2 H 0.3684 0.8169 0.8059 0.057 Uiso 1 1 calc R . . C3 C 0.5200(7) 0.6553(8) 0.9232(7) 0.045(4) Uani 1 1 d . . . C4 C 0.5809(7) 0.6919(8) 0.9539(8) 0.051(4) Uani 1 1 d . . . C5 C 0.6374(7) 0.6408(9) 0.9721(8) 0.054(4) Uani 1 1 d . . . H5 H 0.6777 0.6647 0.9929 0.065 Uiso 1 1 calc R . . C6 C 0.6376(8) 0.5545(8) 0.9609(7) 0.045(4) Uani 1 1 d . . . C7 C 0.5757(7) 0.5209(8) 0.9320(7) 0.045(4) Uani 1 1 d . . . H7 H 0.5737 0.4631 0.9261 0.054 Uiso 1 1 calc R . . C8 C 0.5159(7) 0.5687(9) 0.9109(7) 0.042(4) Uani 1 1 d . . . C9 C 0.5830(9) 0.7853(10) 0.9647(11) 0.097(7) Uani 1 1 d . . . H9A H 0.6324 0.8038 0.9677 0.145 Uiso 1 1 calc R . . H9B H 0.5596 0.7986 1.0041 0.145 Uiso 1 1 calc R . . H9C H 0.5584 0.8130 0.9291 0.145 Uiso 1 1 calc R . . C10 C 0.7002(7) 0.4997(8) 0.9811(8) 0.056(4) Uani 1 1 d . . . H10A H 0.7043 0.4975 1.0274 0.084 Uiso 1 1 calc R . . H10B H 0.7439 0.5224 0.9644 0.084 Uiso 1 1 calc R . . H10C H 0.6925 0.4442 0.9642 0.084 Uiso 1 1 calc R . . C11 C 0.4505(8) 0.5286(9) 0.8790(8) 0.066(5) Uani 1 1 d . . . H11A H 0.4618 0.4720 0.8672 0.098 Uiso 1 1 calc R . . H11B H 0.4364 0.5598 0.8409 0.098 Uiso 1 1 calc R . . H11C H 0.4115 0.5285 0.9084 0.098 Uiso 1 1 calc R . . C12 C 0.2810(7) 0.8389(7) 0.9009(6) 0.035(3) Uani 1 1 d . . . C13 C 0.2849(7) 0.9245(8) 0.9132(6) 0.037(3) Uani 1 1 d . . . C14 C 0.2213(7) 0.9681(8) 0.9155(6) 0.041(4) Uani 1 1 d . . . H14 H 0.2231 1.0259 0.9214 0.049 Uiso 1 1 calc R . . C15 C 0.1545(7) 0.9292(8) 0.9093(6) 0.040(4) Uani 1 1 d . . . C16 C 0.1530(6) 0.8431(8) 0.8958(6) 0.036(3) Uani 1 1 d . . . H16 H 0.1086 0.8169 0.8885 0.043 Uiso 1 1 calc R . . C17 C 0.2141(7) 0.7969(7) 0.8931(6) 0.032(3) Uani 1 1 d U . . C18 C 0.3565(7) 0.9709(8) 0.9233(7) 0.049(4) Uani 1 1 d . . . H18A H 0.3807 0.9737 0.8830 0.074 Uiso 1 1 calc R . . H18B H 0.3864 0.9415 0.9546 0.074 Uiso 1 1 calc R . . H18C H 0.3474 1.0266 0.9385 0.074 Uiso 1 1 calc R . . C19 C 0.0830(7) 0.9791(8) 0.9120(7) 0.050(4) Uani 1 1 d . . . H19A H 0.0508 0.9618 0.8771 0.075 Uiso 1 1 calc R . . H19B H 0.0930 1.0379 0.9080 0.075 Uiso 1 1 calc R . . H19C H 0.0609 0.9686 0.9525 0.075 Uiso 1 1 calc R . . C20 C 0.2116(6) 0.7033(7) 0.8793(7) 0.038(3) Uani 1 1 d . . . H20A H 0.1637 0.6879 0.8644 0.057 Uiso 1 1 calc R . . H20B H 0.2241 0.6729 0.9182 0.057 Uiso 1 1 calc R . . H20C H 0.2454 0.6899 0.8466 0.057 Uiso 1 1 calc R . . C21 C 0.7359(7) 0.7480(9) 0.3170(8) 0.049(4) Uani 1 1 d . . . H21 H 0.7064 0.7555 0.3521 0.059 Uiso 1 1 calc R . . C22 C 0.7964(7) 0.7006(8) 0.3207(7) 0.041(4) Uani 1 1 d . . . H22 H 0.8137 0.6743 0.3582 0.049 Uiso 1 1 calc R . . C23 C 0.6612(6) 0.8421(8) 0.2465(6) 0.037(3) Uani 1 1 d . . . C24 C 0.6010(7) 0.8117(9) 0.2112(7) 0.048(4) Uani 1 1 d . . . C25 C 0.5443(7) 0.8684(8) 0.1964(8) 0.052(4) Uani 1 1 d . . . H25 H 0.5040 0.8505 0.1719 0.062 Uiso 1 1 calc R . . C26 C 0.5481(7) 0.9494(8) 0.2180(7) 0.039(3) Uani 1 1 d . . . C27 C 0.6078(7) 0.9761(8) 0.2526(7) 0.040(4) Uani 1 1 d . . . H27 H 0.6100 1.0318 0.2659 0.049 Uiso 1 1 calc R . . C28 C 0.6656(7) 0.9235(8) 0.2689(8) 0.047(4) Uani 1 1 d . . . C29 C 0.5959(8) 0.7226(9) 0.1836(9) 0.074(6) Uani 1 1 d . . . H29A H 0.5921 0.6832 0.2184 0.111 Uiso 1 1 calc R . . H29B H 0.6384 0.7106 0.1599 0.111 Uiso 1 1 calc R . . H29C H 0.5539 0.7183 0.1552 0.111 Uiso 1 1 calc R . . C30 C 0.4876(7) 1.0119(8) 0.2019(8) 0.060(5) Uani 1 1 d . . . H30A H 0.4944 1.0354 0.1598 0.090 Uiso 1 1 calc R . . H30B H 0.4885 1.0559 0.2336 0.090 Uiso 1 1 calc R . . H30C H 0.4417 0.9837 0.2022 0.090 Uiso 1 1 calc R . . C31 C 0.7314(8) 0.9546(9) 0.3063(8) 0.066(5) Uani 1 1 d . . . H31A H 0.7332 0.9296 0.3485 0.099 Uiso 1 1 calc R . . H31B H 0.7290 1.0145 0.3103 0.099 Uiso 1 1 calc R . . H31C H 0.7741 0.9395 0.2838 0.099 Uiso 1 1 calc R . . C32 C 0.8951(7) 0.6440(9) 0.2561(6) 0.038(3) Uani 1 1 d . . . C33 C 0.9623(7) 0.6812(8) 0.2676(7) 0.040(4) Uani 1 1 d . . . C34 C 1.0219(7) 0.6297(8) 0.2591(6) 0.039(3) Uani 1 1 d . . . H34 H 1.0681 0.6523 0.2644 0.046 Uiso 1 1 calc R . . C35 C 1.0145(8) 0.5446(8) 0.2428(7) 0.046(4) Uani 1 1 d . . . C36 C 0.9475(9) 0.5114(9) 0.2322(8) 0.057(4) Uani 1 1 d . . . H36 H 0.9430 0.4554 0.2202 0.068 Uiso 1 1 calc R . . C37 C 0.8849(7) 0.5601(9) 0.2390(6) 0.042(4) Uani 1 1 d . . . C38 C 0.9715(7) 0.7708(8) 0.2841(6) 0.043(4) Uani 1 1 d . . . H38A H 1.0210 0.7867 0.2789 0.065 Uiso 1 1 calc R . . H38B H 0.9587 0.7798 0.3281 0.065 Uiso 1 1 calc R . . H38C H 0.9408 0.8040 0.2559 0.065 Uiso 1 1 calc R . . C39 C 1.0840(8) 0.4920(9) 0.2386(8) 0.060(5) Uani 1 1 d . . . H39A H 1.0901 0.4581 0.2767 0.089 Uiso 1 1 calc R . . H39B H 1.1248 0.5287 0.2352 0.089 Uiso 1 1 calc R . . H39C H 1.0804 0.4565 0.2011 0.089 Uiso 1 1 calc R . . C40 C 0.8126(8) 0.5208(9) 0.2262(8) 0.062(5) Uani 1 1 d . . . H40A H 0.7812 0.5344 0.2607 0.093 Uiso 1 1 calc R . . H40B H 0.8179 0.4610 0.2236 0.093 Uiso 1 1 calc R . . H40C H 0.7920 0.5416 0.1861 0.093 Uiso 1 1 calc R . . C41 C 0.2146(7) 0.9563(8) 1.0968(8) 0.051(4) Uani 1 1 d . . . H41A H 0.2339 0.9432 1.0550 0.062 Uiso 1 1 calc R . . H41B H 0.2463 0.9965 1.1187 0.062 Uiso 1 1 calc R . . C42 C 0.1382(7) 0.9907(8) 1.0892(7) 0.047(4) Uani 1 1 d . . . H42A H 0.1246 1.0224 1.1270 0.057 Uiso 1 1 calc R . . H42B H 0.1323 1.0256 1.0510 0.057 Uiso 1 1 calc R . . C43 C 0.0961(8) 0.9113(9) 1.0825(8) 0.064(5) Uani 1 1 d . . . H43A H 0.1002 0.8874 1.0397 0.077 Uiso 1 1 calc R . . H43B H 0.0455 0.9202 1.0910 0.077 Uiso 1 1 calc R . . C44 C 0.1329(6) 0.8551(9) 1.1347(8) 0.056(4) Uani 1 1 d . . . H44A H 0.1120 0.8641 1.1765 0.067 Uiso 1 1 calc R . . H44B H 0.1280 0.7963 1.1232 0.067 Uiso 1 1 calc R . . C45 C 1.0149(8) 0.6043(10) 0.0875(7) 0.056(4) Uani 1 1 d . . . H45A H 0.9876 0.5532 0.0939 0.067 Uiso 1 1 calc R . . H45B H 1.0087 0.6409 0.1244 0.067 Uiso 1 1 calc R . . C46 C 1.0939(8) 0.5846(10) 0.0797(8) 0.065(5) Uani 1 1 d . . . H46A H 1.1072 0.5325 0.1011 0.078 Uiso 1 1 calc R . . H46B H 1.1244 0.6294 0.0969 0.078 Uiso 1 1 calc R . . C47 C 1.0999(8) 0.5773(8) 0.0071(7) 0.051(4) Uani 1 1 d . . . H47A H 1.0859 0.5216 -0.0076 0.061 Uiso 1 1 calc R . . H47B H 1.1490 0.5883 -0.0055 0.061 Uiso 1 1 calc R . . C48 C 1.0485(7) 0.6426(9) -0.0210(8) 0.055(4) Uani 1 1 d . . . H48A H 1.0722 0.6965 -0.0249 0.066 Uiso 1 1 calc R . . H48B H 1.0289 0.6257 -0.0632 0.066 Uiso 1 1 calc R . . N1 N 0.4582(5) 0.7063(7) 0.9060(6) 0.041(3) Uani 1 1 d . . . N2 N 0.3467(5) 0.7909(6) 0.8977(5) 0.038(3) Uani 1 1 d . . . N3 N 0.7212(5) 0.7840(6) 0.2585(6) 0.036(3) Uani 1 1 d . . . N4 N 0.8299(5) 0.6959(6) 0.2614(5) 0.032(3) Uani 1 1 d . . . O1 O 0.2075(4) 0.8804(5) 1.1357(5) 0.040(2) Uani 1 1 d . . . O2 O 0.9906(5) 0.6458(5) 0.0278(4) 0.043(2) Uani 1 1 d . . . Cl1 Cl 0.22058(18) 0.7077(2) 1.21453(17) 0.0433(9) Uani 1 1 d . . . Cl2 Cl 0.33309(17) 0.87487(19) 1.23964(17) 0.0404(9) Uani 1 1 d . . . Cl3 Cl 0.37170(17) 0.8764(2) 1.08172(17) 0.0419(9) Uani 1 1 d . . . Cl4 Cl 0.24722(17) 0.7263(2) 1.05199(17) 0.0439(9) Uani 1 1 d . . . Cl5 Cl 0.39486(18) 0.6892(2) 1.16144(19) 0.0474(10) Uani 1 1 d . . . Cl6 Cl 0.83430(19) 0.6202(2) 0.08125(17) 0.0453(9) Uani 1 1 d . . . Cl7 Cl 0.93423(18) 0.7920(2) 0.11445(16) 0.0428(9) Uani 1 1 d . . . Cl8 Cl 0.95868(17) 0.81808(19) -0.04712(17) 0.0407(8) Uani 1 1 d . . . Cl9 Cl 0.86281(19) 0.6406(2) -0.07768(16) 0.0422(9) Uani 1 1 d . . . Cl10 Cl 0.78355(18) 0.8082(2) 0.00561(19) 0.0498(10) Uani 1 1 d . . . As1 As 0.38947(8) 0.73111(9) 0.96416(7) 0.0443(4) Uani 1 1 d . . . As2 As 0.78591(8) 0.75689(10) 0.19767(8) 0.0479(4) Uani 1 1 d . . . Sn1 Sn 0.29839(5) 0.78917(5) 1.14882(5) 0.0329(3) Uani 1 1 d . . . Sn2 Sn 0.89099(5) 0.72385(5) 0.01617(5) 0.0355(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(8) 0.048(8) 0.025(8) -0.007(7) 0.015(6) -0.011(7) C2 0.051(9) 0.041(8) 0.050(10) 0.003(7) -0.014(8) -0.015(7) C3 0.036(8) 0.045(9) 0.055(11) -0.010(7) 0.021(7) 0.006(7) C4 0.026(8) 0.041(9) 0.088(13) -0.024(8) 0.012(8) -0.014(7) C5 0.032(8) 0.060(10) 0.071(12) -0.019(9) 0.002(8) -0.008(8) C6 0.053(9) 0.042(9) 0.040(10) 0.000(7) 0.015(8) 0.012(7) C7 0.041(9) 0.035(8) 0.060(11) -0.007(7) 0.006(8) 0.005(7) C8 0.040(8) 0.050(9) 0.038(9) 0.000(7) 0.014(7) -0.001(7) C9 0.052(10) 0.057(11) 0.18(2) -0.036(13) -0.017(13) 0.004(9) C10 0.046(9) 0.033(8) 0.089(13) 0.005(8) 0.009(9) 0.001(7) C11 0.071(11) 0.047(9) 0.078(13) -0.008(9) -0.007(10) 0.004(8) C12 0.034(8) 0.031(7) 0.039(9) 0.005(6) 0.009(7) 0.004(6) C13 0.033(7) 0.044(8) 0.034(9) 0.005(7) -0.002(6) -0.001(7) C14 0.059(10) 0.030(7) 0.034(9) 0.005(6) 0.012(7) 0.002(7) C15 0.048(9) 0.042(8) 0.033(9) -0.004(7) 0.015(7) 0.009(7) C16 0.027(7) 0.043(8) 0.037(9) 0.000(7) 0.009(6) 0.009(6) C17 0.040(6) 0.037(6) 0.020(6) 0.004(5) -0.001(5) 0.009(5) C18 0.063(10) 0.036(8) 0.050(10) -0.003(7) 0.020(8) 0.002(7) C19 0.047(9) 0.040(8) 0.062(11) 0.003(8) 0.007(8) 0.006(7) C20 0.025(7) 0.035(7) 0.053(10) -0.009(7) 0.000(7) 0.004(6) C21 0.033(8) 0.055(9) 0.059(12) 0.001(8) 0.006(8) -0.009(7) C22 0.046(8) 0.036(8) 0.041(9) -0.009(7) 0.027(7) 0.003(7) C23 0.029(7) 0.044(8) 0.038(9) -0.005(7) 0.004(7) -0.010(6) C24 0.036(8) 0.046(9) 0.063(11) -0.009(8) -0.001(8) 0.009(7) C25 0.046(9) 0.037(9) 0.073(12) -0.009(8) 0.002(8) -0.008(7) C26 0.031(8) 0.048(9) 0.038(9) 0.000(7) 0.013(7) -0.009(7) C27 0.044(9) 0.036(8) 0.043(10) -0.010(7) 0.022(8) -0.006(7) C28 0.041(9) 0.039(8) 0.061(11) 0.001(8) 0.003(8) -0.001(7) C29 0.043(9) 0.048(10) 0.130(17) -0.032(10) -0.009(10) 0.001(8) C30 0.042(9) 0.038(8) 0.102(15) 0.005(9) 0.024(9) 0.000(7) C31 0.056(10) 0.052(10) 0.088(14) -0.012(9) -0.015(10) 0.005(8) C32 0.041(8) 0.056(9) 0.018(8) 0.001(7) 0.005(6) 0.024(7) C33 0.049(9) 0.026(7) 0.045(10) -0.010(6) 0.016(7) -0.011(7) C34 0.040(8) 0.037(8) 0.039(9) 0.003(7) 0.004(7) -0.002(6) C35 0.061(10) 0.027(8) 0.050(10) 0.010(7) 0.014(8) 0.007(7) C36 0.076(12) 0.029(8) 0.067(12) 0.005(8) 0.016(10) -0.009(8) C37 0.045(9) 0.049(9) 0.031(9) 0.008(7) 0.012(7) 0.007(7) C38 0.054(9) 0.049(9) 0.027(8) 0.014(7) 0.011(7) -0.005(7) C39 0.062(10) 0.048(9) 0.070(12) 0.014(8) 0.015(9) 0.022(8) C40 0.055(10) 0.065(11) 0.065(12) 0.012(9) 0.000(9) -0.020(8) C41 0.050(9) 0.031(8) 0.073(12) 0.009(8) -0.004(8) 0.000(7) C42 0.046(9) 0.044(9) 0.052(10) 0.003(7) -0.006(8) 0.010(7) C43 0.050(10) 0.067(11) 0.073(13) -0.005(10) -0.023(9) 0.001(8) C44 0.024(7) 0.058(10) 0.087(13) -0.001(9) 0.011(8) 0.013(7) C45 0.068(11) 0.071(11) 0.026(9) 0.003(8) -0.018(8) 0.028(9) C46 0.051(10) 0.065(11) 0.079(14) 0.032(10) -0.014(10) 0.007(8) C47 0.051(9) 0.037(8) 0.064(12) 0.002(8) -0.005(8) 0.016(7) C48 0.058(10) 0.050(9) 0.060(11) 0.004(8) 0.024(9) 0.002(8) N1 0.029(6) 0.047(7) 0.045(8) -0.005(6) 0.004(6) 0.005(5) N2 0.038(6) 0.031(6) 0.046(8) 0.001(5) 0.013(6) 0.001(5) N3 0.024(5) 0.034(6) 0.051(8) -0.006(6) 0.013(5) 0.002(5) N4 0.019(5) 0.046(7) 0.032(7) 0.005(5) 0.000(5) 0.001(5) O1 0.034(5) 0.022(5) 0.064(7) -0.006(4) 0.006(5) 0.000(4) O2 0.049(6) 0.046(5) 0.037(6) 0.004(5) 0.018(5) 0.012(5) Cl1 0.0453(19) 0.0401(19) 0.045(2) 0.0043(17) 0.0126(17) -0.0086(16) Cl2 0.0421(19) 0.0382(19) 0.041(2) -0.0025(16) 0.0056(17) -0.0012(15) Cl3 0.0430(19) 0.0414(19) 0.042(2) 0.0051(16) 0.0116(17) -0.0044(15) Cl4 0.0395(18) 0.052(2) 0.040(2) -0.0089(17) 0.0048(16) -0.0022(16) Cl5 0.045(2) 0.0369(19) 0.061(3) 0.0050(18) 0.0098(19) 0.0099(16) Cl6 0.052(2) 0.0433(19) 0.041(2) 0.0007(17) 0.0108(18) -0.0031(17) Cl7 0.054(2) 0.0409(19) 0.034(2) -0.0088(16) -0.0008(17) -0.0017(16) Cl8 0.047(2) 0.0342(18) 0.042(2) 0.0048(16) 0.0075(17) 0.0009(15) Cl9 0.060(2) 0.0372(19) 0.030(2) -0.0008(15) 0.0012(17) -0.0090(16) Cl10 0.0382(19) 0.046(2) 0.065(3) -0.0081(19) 0.0019(19) 0.0102(16) As1 0.0411(8) 0.0551(9) 0.0373(9) 0.0023(8) 0.0096(7) 0.0158(7) As2 0.0400(8) 0.0614(10) 0.0430(10) 0.0059(8) 0.0111(7) 0.0131(7) Sn1 0.0326(5) 0.0314(5) 0.0352(6) 0.0009(4) 0.0079(4) 0.0024(4) Sn2 0.0363(5) 0.0344(5) 0.0358(6) -0.0033(4) 0.0035(4) 0.0022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.372(16) . ? C1 C2 1.375(18) . ? C1 H1 0.9300 . ? C2 N2 1.339(16) . ? C2 H2 0.9300 . ? C3 C4 1.402(18) . ? C3 C8 1.406(18) . ? C3 N1 1.437(16) . ? C4 C5 1.368(19) . ? C4 C9 1.506(19) . ? C5 C6 1.396(18) . ? C5 H5 0.9300 . ? C6 C7 1.382(18) . ? C6 C10 1.498(18) . ? C7 C8 1.401(18) . ? C7 H7 0.9300 . ? C8 C11 1.500(19) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.391(17) . ? C12 C17 1.411(17) . ? C12 N2 1.439(15) . ? C13 C14 1.368(17) . ? C13 C18 1.525(17) . ? C14 C15 1.386(18) . ? C14 H14 0.9300 . ? C15 C16 1.401(17) . ? C15 C19 1.546(17) . ? C16 C17 1.351(16) . ? C16 H16 0.9300 . ? C17 C20 1.521(16) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.351(18) . ? C21 N3 1.357(17) . ? C21 H21 0.9300 . ? C22 N4 1.393(15) . ? C22 H22 0.9300 . ? C23 C28 1.380(18) . ? C23 C24 1.398(18) . ? C23 N3 1.461(16) . ? C24 C25 1.410(18) . ? C24 C29 1.532(18) . ? C25 C26 1.368(17) . ? C25 H25 0.9300 . ? C26 C27 1.365(17) . ? C26 C30 1.527(18) . ? C27 C28 1.391(18) . ? C27 H27 0.9300 . ? C28 C31 1.502(19) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.389(18) . ? C32 C37 1.396(18) . ? C32 N4 1.470(14) . ? C33 C34 1.391(17) . ? C33 C38 1.477(17) . ? C34 C35 1.404(17) . ? C34 H34 0.9300 . ? C35 C36 1.357(19) . ? C35 C39 1.540(17) . ? C36 C37 1.406(19) . ? C36 H36 0.9300 . ? C37 C40 1.493(18) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 O1 1.461(15) . ? C41 C42 1.520(17) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.490(18) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.543(19) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 O1 1.438(14) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 O2 1.458(15) . ? C45 C46 1.508(18) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.51(2) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.513(18) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 O2 1.497(14) . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? N1 As1 1.823(10) . ? N2 As1 1.831(11) . ? N3 As2 1.818(10) . ? N4 As2 1.809(10) . ? O1 Sn1 2.233(8) . ? O2 Sn2 2.230(8) . ? Cl1 Sn1 2.396(3) . ? Cl2 Sn1 2.392(4) . ? Cl3 Sn1 2.414(3) . ? Cl4 Sn1 2.404(4) . ? Cl5 Sn1 2.400(3) . ? Cl6 Sn2 2.396(3) . ? Cl7 Sn2 2.417(3) . ? Cl8 Sn2 2.377(3) . ? Cl9 Sn2 2.393(3) . ? Cl10 Sn2 2.404(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.9(12) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? N2 C2 C1 115.5(13) . . ? N2 C2 H2 122.2 . . ? C1 C2 H2 122.2 . . ? C4 C3 C8 122.0(13) . . ? C4 C3 N1 119.8(12) . . ? C8 C3 N1 118.2(13) . . ? C5 C4 C3 118.0(13) . . ? C5 C4 C9 122.3(13) . . ? C3 C4 C9 119.7(14) . . ? C4 C5 C6 123.3(14) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C7 C6 C5 116.5(13) . . ? C7 C6 C10 121.1(13) . . ? C5 C6 C10 122.4(14) . . ? C6 C7 C8 123.9(13) . . ? C6 C7 H7 118.0 . . ? C8 C7 H7 118.0 . . ? C3 C8 C7 116.1(13) . . ? C3 C8 C11 122.4(13) . . ? C7 C8 C11 121.4(13) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 121.7(11) . . ? C13 C12 N2 119.5(11) . . ? C17 C12 N2 118.8(10) . . ? C14 C13 C12 117.8(12) . . ? C14 C13 C18 119.5(12) . . ? C12 C13 C18 122.7(11) . . ? C13 C14 C15 122.3(12) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C14 C15 C16 117.9(12) . . ? C14 C15 C19 121.8(12) . . ? C16 C15 C19 120.1(12) . . ? C17 C16 C15 122.2(12) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C12 117.9(12) . . ? C16 C17 C20 121.5(12) . . ? C12 C17 C20 120.5(10) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N3 115.2(13) . . ? C22 C21 H21 122.4 . . ? N3 C21 H21 122.4 . . ? C21 C22 N4 112.0(13) . . ? C21 C22 H22 124.0 . . ? N4 C22 H22 124.0 . . ? C28 C23 C24 122.6(13) . . ? C28 C23 N3 120.3(12) . . ? C24 C23 N3 117.1(11) . . ? C25 C24 C23 117.7(13) . . ? C25 C24 C29 118.5(13) . . ? C23 C24 C29 123.7(12) . . ? C26 C25 C24 120.3(14) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 119.9(13) . . ? C25 C26 C30 121.1(13) . . ? C27 C26 C30 119.0(12) . . ? C26 C27 C28 122.7(13) . . ? C26 C27 H27 118.7 . . ? C28 C27 H27 118.7 . . ? C27 C28 C23 116.8(13) . . ? C27 C28 C31 121.8(13) . . ? C23 C28 C31 121.3(13) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5 . . ? C26 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 124.4(12) . . ? C33 C32 N4 118.6(12) . . ? C37 C32 N4 117.0(12) . . ? C32 C33 C34 115.8(11) . . ? C32 C33 C38 123.2(12) . . ? C34 C33 C38 121.0(12) . . ? C33 C34 C35 122.0(12) . . ? C33 C34 H34 119.0 . . ? C35 C34 H34 119.0 . . ? C36 C35 C34 119.8(13) . . ? C36 C35 C39 122.5(13) . . ? C34 C35 C39 117.7(13) . . ? C35 C36 C37 121.3(13) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C32 C37 C36 116.7(13) . . ? C32 C37 C40 124.1(13) . . ? C36 C37 C40 119.2(13) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O1 C41 C42 104.8(10) . . ? O1 C41 H41A 110.8 . . ? C42 C41 H41A 110.8 . . ? O1 C41 H41B 110.8 . . ? C42 C41 H41B 110.8 . . ? H41A C41 H41B 108.9 . . ? C43 C42 C41 100.6(11) . . ? C43 C42 H42A 111.7 . . ? C41 C42 H42A 111.7 . . ? C43 C42 H42B 111.7 . . ? C41 C42 H42B 111.7 . . ? H42A C42 H42B 109.4 . . ? C42 C43 C44 102.3(11) . . ? C42 C43 H43A 111.3 . . ? C44 C43 H43A 111.3 . . ? C42 C43 H43B 111.3 . . ? C44 C43 H43B 111.3 . . ? H43A C43 H43B 109.2 . . ? O1 C44 C43 104.3(11) . . ? O1 C44 H44A 110.9 . . ? C43 C44 H44A 110.9 . . ? O1 C44 H44B 110.9 . . ? C43 C44 H44B 110.9 . . ? H44A C44 H44B 108.9 . . ? O2 C45 C46 106.0(12) . . ? O2 C45 H45A 110.5 . . ? C46 C45 H45A 110.5 . . ? O2 C45 H45B 110.5 . . ? C46 C45 H45B 110.5 . . ? H45A C45 H45B 108.7 . . ? C45 C46 C47 103.1(12) . . ? C45 C46 H46A 111.1 . . ? C47 C46 H46A 111.1 . . ? C45 C46 H46B 111.1 . . ? C47 C46 H46B 111.1 . . ? H46A C46 H46B 109.1 . . ? C46 C47 C48 105.1(12) . . ? C46 C47 H47A 110.7 . . ? C48 C47 H47A 110.7 . . ? C46 C47 H47B 110.7 . . ? C48 C47 H47B 110.7 . . ? H47A C47 H47B 108.8 . . ? O2 C48 C47 102.6(11) . . ? O2 C48 H48A 111.2 . . ? C47 C48 H48A 111.2 . . ? O2 C48 H48B 111.2 . . ? C47 C48 H48B 111.2 . . ? H48A C48 H48B 109.2 . . ? C1 N1 C3 124.0(11) . . ? C1 N1 As1 114.2(8) . . ? C3 N1 As1 121.8(9) . . ? C2 N2 C12 120.7(11) . . ? C2 N2 As1 113.4(9) . . ? C12 N2 As1 125.9(9) . . ? C21 N3 C23 123.1(11) . . ? C21 N3 As2 113.6(9) . . ? C23 N3 As2 123.2(9) . . ? C22 N4 C32 119.2(10) . . ? C22 N4 As2 114.1(8) . . ? C32 N4 As2 126.7(8) . . ? C44 O1 C41 109.2(10) . . ? C44 O1 Sn1 122.4(7) . . ? C41 O1 Sn1 121.7(7) . . ? C45 O2 C48 110.4(10) . . ? C45 O2 Sn2 125.0(7) . . ? C48 O2 Sn2 123.6(8) . . ? N1 As1 N2 84.9(5) . . ? N4 As2 N3 85.0(5) . . ? O1 Sn1 Cl2 84.5(2) . . ? O1 Sn1 Cl5 178.9(2) . . ? Cl2 Sn1 Cl5 96.65(13) . . ? O1 Sn1 Cl1 87.6(2) . . ? Cl2 Sn1 Cl1 90.85(12) . . ? Cl5 Sn1 Cl1 92.13(12) . . ? O1 Sn1 Cl4 84.1(2) . . ? Cl2 Sn1 Cl4 168.33(12) . . ? Cl5 Sn1 Cl4 94.78(13) . . ? Cl1 Sn1 Cl4 91.09(12) . . ? O1 Sn1 Cl3 89.4(2) . . ? Cl2 Sn1 Cl3 88.93(12) . . ? Cl5 Sn1 Cl3 90.85(12) . . ? Cl1 Sn1 Cl3 177.02(12) . . ? Cl4 Sn1 Cl3 88.54(12) . . ? O2 Sn2 Cl8 87.9(2) . . ? O2 Sn2 Cl9 86.2(3) . . ? Cl8 Sn2 Cl9 90.48(12) . . ? O2 Sn2 Cl6 86.0(2) . . ? Cl8 Sn2 Cl6 173.90(12) . . ? Cl9 Sn2 Cl6 89.17(12) . . ? O2 Sn2 Cl10 179.0(2) . . ? Cl8 Sn2 Cl10 92.61(12) . . ? Cl9 Sn2 Cl10 94.61(13) . . ? Cl6 Sn2 Cl10 93.48(13) . . ? O2 Sn2 Cl7 85.0(3) . . ? Cl8 Sn2 Cl7 90.75(12) . . ? Cl9 Sn2 Cl7 171.04(12) . . ? Cl6 Sn2 Cl7 88.67(12) . . ? Cl10 Sn2 Cl7 94.20(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 -2.3(17) . . . . ? C8 C3 C4 C5 0(2) . . . . ? N1 C3 C4 C5 177.2(13) . . . . ? C8 C3 C4 C9 178.8(15) . . . . ? N1 C3 C4 C9 -4(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C9 C4 C5 C6 -178.0(16) . . . . ? C4 C5 C6 C7 -2(2) . . . . ? C4 C5 C6 C10 179.9(14) . . . . ? C5 C6 C7 C8 3(2) . . . . ? C10 C6 C7 C8 -178.8(13) . . . . ? C4 C3 C8 C7 1(2) . . . . ? N1 C3 C8 C7 -176.3(12) . . . . ? C4 C3 C8 C11 179.1(14) . . . . ? N1 C3 C8 C11 2(2) . . . . ? C6 C7 C8 C3 -3(2) . . . . ? C6 C7 C8 C11 179.1(14) . . . . ? C17 C12 C13 C14 -2(2) . . . . ? N2 C12 C13 C14 179.6(12) . . . . ? C17 C12 C13 C18 178.6(12) . . . . ? N2 C12 C13 C18 0(2) . . . . ? C12 C13 C14 C15 3(2) . . . . ? C18 C13 C14 C15 -177.4(13) . . . . ? C13 C14 C15 C16 -4(2) . . . . ? C13 C14 C15 C19 179.9(13) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C19 C15 C16 C17 -179.8(12) . . . . ? C15 C16 C17 C12 -3.4(19) . . . . ? C15 C16 C17 C20 179.1(12) . . . . ? C13 C12 C17 C16 2.2(19) . . . . ? N2 C12 C17 C16 -179.6(11) . . . . ? C13 C12 C17 C20 179.7(12) . . . . ? N2 C12 C17 C20 -2.0(18) . . . . ? N3 C21 C22 N4 -2.6(17) . . . . ? C28 C23 C24 C25 2(2) . . . . ? N3 C23 C24 C25 -176.9(12) . . . . ? C28 C23 C24 C29 177.7(14) . . . . ? N3 C23 C24 C29 -1(2) . . . . ? C23 C24 C25 C26 -2(2) . . . . ? C29 C24 C25 C26 -177.4(14) . . . . ? C24 C25 C26 C27 1(2) . . . . ? C24 C25 C26 C30 179.4(13) . . . . ? C25 C26 C27 C28 -2(2) . . . . ? C30 C26 C27 C28 -179.6(13) . . . . ? C26 C27 C28 C23 2(2) . . . . ? C26 C27 C28 C31 179.0(13) . . . . ? C24 C23 C28 C27 -2(2) . . . . ? N3 C23 C28 C27 176.8(11) . . . . ? C24 C23 C28 C31 -179.4(14) . . . . ? N3 C23 C28 C31 0(2) . . . . ? C37 C32 C33 C34 2(2) . . . . ? N4 C32 C33 C34 -177.4(11) . . . . ? C37 C32 C33 C38 178.4(12) . . . . ? N4 C32 C33 C38 -1(2) . . . . ? C32 C33 C34 C35 -3(2) . . . . ? C38 C33 C34 C35 -179.3(13) . . . . ? C33 C34 C35 C36 3(2) . . . . ? C33 C34 C35 C39 -176.4(13) . . . . ? C34 C35 C36 C37 -2(2) . . . . ? C39 C35 C36 C37 177.4(13) . . . . ? C33 C32 C37 C36 -1(2) . . . . ? N4 C32 C37 C36 178.3(12) . . . . ? C33 C32 C37 C40 -179.6(13) . . . . ? N4 C32 C37 C40 0(2) . . . . ? C35 C36 C37 C32 1(2) . . . . ? C35 C36 C37 C40 179.5(14) . . . . ? O1 C41 C42 C43 -37.3(15) . . . . ? C41 C42 C43 C44 42.5(15) . . . . ? C42 C43 C44 O1 -33.3(15) . . . . ? O2 C45 C46 C47 -26.8(15) . . . . ? C45 C46 C47 C48 36.2(15) . . . . ? C46 C47 C48 O2 -31.1(14) . . . . ? C2 C1 N1 C3 -178.2(11) . . . . ? C2 C1 N1 As1 2.0(14) . . . . ? C4 C3 N1 C1 96.6(17) . . . . ? C8 C3 N1 C1 -86.1(16) . . . . ? C4 C3 N1 As1 -83.6(15) . . . . ? C8 C3 N1 As1 93.7(14) . . . . ? C1 C2 N2 C12 -179.7(11) . . . . ? C1 C2 N2 As1 1.5(15) . . . . ? C13 C12 N2 C2 -83.1(16) . . . . ? C17 C12 N2 C2 98.6(14) . . . . ? C13 C12 N2 As1 95.5(13) . . . . ? C17 C12 N2 As1 -82.8(14) . . . . ? C22 C21 N3 C23 -175.4(11) . . . . ? C22 C21 N3 As2 1.7(15) . . . . ? C28 C23 N3 C21 75.1(17) . . . . ? C24 C23 N3 C21 -105.7(15) . . . . ? C28 C23 N3 As2 -101.7(14) . . . . ? C24 C23 N3 As2 77.4(14) . . . . ? C21 C22 N4 C32 -177.7(11) . . . . ? C21 C22 N4 As2 2.3(14) . . . . ? C33 C32 N4 C22 -91.0(15) . . . . ? C37 C32 N4 C22 89.5(14) . . . . ? C33 C32 N4 As2 88.9(14) . . . . ? C37 C32 N4 As2 -90.6(13) . . . . ? C43 C44 O1 C41 9.8(14) . . . . ? C43 C44 O1 Sn1 -141.9(9) . . . . ? C42 C41 O1 C44 17.0(15) . . . . ? C42 C41 O1 Sn1 169.0(8) . . . . ? C46 C45 O2 C48 7.7(15) . . . . ? C46 C45 O2 Sn2 -161.5(9) . . . . ? C47 C48 O2 C45 14.5(14) . . . . ? C47 C48 O2 Sn2 -176.1(8) . . . . ? C1 N1 As1 N2 -1.0(9) . . . . ? C3 N1 As1 N2 179.2(10) . . . . ? C2 N2 As1 N1 -0.3(9) . . . . ? C12 N2 As1 N1 -179.0(10) . . . . ? C22 N4 As2 N3 -1.2(9) . . . . ? C32 N4 As2 N3 178.9(11) . . . . ? C21 N3 As2 N4 -0.3(9) . . . . ? C23 N3 As2 N4 176.9(10) . . . . ? C44 O1 Sn1 Cl2 -122.9(10) . . . . ? C41 O1 Sn1 Cl2 88.8(9) . . . . ? C44 O1 Sn1 Cl1 -31.8(10) . . . . ? C41 O1 Sn1 Cl1 179.9(9) . . . . ? C44 O1 Sn1 Cl4 59.5(10) . . . . ? C41 O1 Sn1 Cl4 -88.7(9) . . . . ? C44 O1 Sn1 Cl3 148.1(10) . . . . ? C41 O1 Sn1 Cl3 -0.1(9) . . . . ? C45 O2 Sn2 Cl8 139.4(10) . . . . ? C48 O2 Sn2 Cl8 -28.5(9) . . . . ? C45 O2 Sn2 Cl9 -130.0(10) . . . . ? C48 O2 Sn2 Cl9 62.1(9) . . . . ? C45 O2 Sn2 Cl6 -40.5(10) . . . . ? C48 O2 Sn2 Cl6 151.6(9) . . . . ? C45 O2 Sn2 Cl7 48.5(10) . . . . ? C48 O2 Sn2 Cl7 -119.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.808 _refine_diff_density_min -1.467 _refine_diff_density_rms 0.170