# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_email JIANFANGMA@YAHOO.COM.CN _publ_section_title ; Monoorganooxotin Cage, Diorganotin Ladders, Diorganotin Double Chain and Triorganotin Single Chain Formed with Phosphonate and Arsonate Ligands ; loop_ _publ_author_name 'Jian-Fang Ma.' 'Min-Zhong Su.' 'Yun-Peng Xie.' 'Jin Yang.' # Attachment 'crystals.cif' data_compound-1 _database_code_depnum_ccdc_archive 'CCDC 737801' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H96 O21 P4 Sn6' _chemical_formula_weight 1929.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.437(7) _cell_length_b 12.829(6) _cell_length_c 14.246(6) _cell_angle_alpha 63.359(14) _cell_angle_beta 82.908(19) _cell_angle_gamma 70.228(19) _cell_volume 1910.8(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used Total _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.379 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.190 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 954 _exptl_absorpt_coefficient_mu 2.076 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.565 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18475 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8514 _reflns_number_gt 7219 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0715P)^2^+1.3231P] 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 8514 _refine_ls_number_parameters 387 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.108 _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 0.6673(5) 0.0548(5) 0.0971(4) 0.0567(12) Uani 1 1 d . . . H1A H 0.6336 0.0147 0.0707 0.068 Uiso 1 1 calc R . . H1B H 0.7378 0.0609 0.0607 0.068 Uiso 1 1 calc R . . C2 C 0.6962(6) -0.0261(5) 0.2139(5) 0.0767(18) Uani 1 1 d D . . H2A H 0.7334 0.0111 0.2405 0.092 Uiso 1 1 calc R . . H2B H 0.6261 -0.0311 0.2513 0.092 Uiso 1 1 calc R . . C3 C 0.7741(9) -0.1548(6) 0.2344(7) 0.120(3) Uani 1 1 d D . . H3A H 0.7333 -0.1937 0.2132 0.144 Uiso 1 1 calc R . . H3B H 0.8398 -0.1481 0.1904 0.144 Uiso 1 1 calc R . . C4 C 0.8148(13) -0.2344(11) 0.3431(10) 0.192(7) Uani 1 1 d . . . H4A H 0.8632 -0.3135 0.3489 0.288 Uiso 1 1 calc R . . H4B H 0.7507 -0.2440 0.3874 0.288 Uiso 1 1 calc R . . H4C H 0.8574 -0.1983 0.3645 0.288 Uiso 1 1 calc R . . C5 C 0.3409(6) 0.4816(5) -0.2949(4) 0.0636(15) Uani 1 1 d . . . H5A H 0.4117 0.4645 -0.3306 0.076 Uiso 1 1 calc R . . H5B H 0.3064 0.4196 -0.2837 0.076 Uiso 1 1 calc R . . C6 C 0.2618(7) 0.6052(6) -0.3675(5) 0.0804(19) Uani 1 1 d D . . H6A H 0.2904 0.6694 -0.3733 0.097 Uiso 1 1 calc R . . H6B H 0.1867 0.6185 -0.3378 0.097 Uiso 1 1 calc R . . C7 C 0.2518(10) 0.6141(8) -0.4767(6) 0.129(4) Uani 1 1 d D . . H7A H 0.3283 0.5906 -0.5016 0.155 Uiso 1 1 calc R . . H7B H 0.2165 0.5545 -0.4704 0.155 Uiso 1 1 calc R . . C8 C 0.1881(13) 0.7319(11) -0.5547(8) 0.171(6) Uani 1 1 d D . . H8A H 0.1864 0.7273 -0.6198 0.257 Uiso 1 1 calc R . . H8B H 0.2238 0.7915 -0.5643 0.257 Uiso 1 1 calc R . . H8C H 0.1115 0.7560 -0.5321 0.257 Uiso 1 1 calc R . . C9 C 0.1381(6) 0.2993(7) 0.1754(6) 0.088(2) Uani 1 1 d D . . H9A H 0.0766 0.3712 0.1734 0.105 Uiso 1 1 calc R . . H9B H 0.1104 0.2646 0.1390 0.105 Uiso 1 1 calc R . . C10 C 0.1659(11) 0.2041(12) 0.2909(8) 0.155(5) Uani 1 1 d D . . H10A H 0.2074 0.1260 0.2892 0.186 Uiso 1 1 calc R . . H10B H 0.2201 0.2255 0.3167 0.186 Uiso 1 1 calc R . . C11 C 0.0839(15) 0.1796(16) 0.3712(12) 0.208(7) Uani 1 1 d D . . H11A H 0.0248 0.1645 0.3453 0.250 Uiso 1 1 calc R . . H11B H 0.0481 0.2533 0.3816 0.250 Uiso 1 1 calc R . . C12 C 0.1258(15) 0.077(2) 0.4733(11) 0.251(11) Uani 1 1 d . . . H12A H 0.0635 0.0704 0.5204 0.376 Uiso 1 1 calc R . . H12B H 0.1831 0.0911 0.5014 0.376 Uiso 1 1 calc R . . H12C H 0.1584 0.0022 0.4654 0.376 Uiso 1 1 calc R . . C13 C 0.1413(6) 0.4142(8) -0.1051(6) 0.086(2) Uani 1 1 d . . . H13A H 0.1489 0.4177 -0.1742 0.129 Uiso 1 1 calc R . . H13B H 0.0975 0.4939 -0.1095 0.129 Uiso 1 1 calc R . . H13C H 0.1030 0.3558 -0.0620 0.129 Uiso 1 1 calc R . . C14 C 0.3730(6) 0.0944(5) 0.0993(6) 0.0719(17) Uani 1 1 d . . . H14A H 0.4385 0.0220 0.1157 0.108 Uiso 1 1 calc R . . H14B H 0.3507 0.1293 0.0265 0.108 Uiso 1 1 calc R . . H14C H 0.3110 0.0728 0.1423 0.108 Uiso 1 1 calc R . . C15 C 0.5926(6) 0.2508(6) -0.1682(5) 0.079(2) Uani 1 1 d . . . H15A H 0.5553 0.2815 -0.2348 0.119 Uiso 1 1 calc R . . H15B H 0.6246 0.1628 -0.1392 0.119 Uiso 1 1 calc R . . H15C H 0.6525 0.2858 -0.1776 0.119 Uiso 1 1 calc R . . C16 C 0.8881(4) 0.2141(4) 0.0925(4) 0.0451(10) Uani 1 1 d . . . C17 C 0.9606(5) 0.1808(6) 0.0236(5) 0.0683(15) Uani 1 1 d . . . H17 H 0.9494 0.2315 -0.0482 0.082 Uiso 1 1 calc R . . C18 C 1.0509(6) 0.0719(7) 0.0598(7) 0.091(2) Uani 1 1 d . . . H18 H 1.1006 0.0522 0.0115 0.110 Uiso 1 1 calc R . . C19 C 1.0690(6) -0.0054(7) 0.1610(7) 0.094(2) Uani 1 1 d . . . H19 H 1.1284 -0.0797 0.1836 0.113 Uiso 1 1 calc R . . C20 C 0.9974(7) 0.0276(7) 0.2310(6) 0.100(3) Uani 1 1 d . . . H20 H 1.0099 -0.0240 0.3025 0.120 Uiso 1 1 calc R . . C21 C 0.9079(5) 0.1350(6) 0.1979(5) 0.0739(18) Uani 1 1 d . . . H21 H 0.8599 0.1549 0.2470 0.089 Uiso 1 1 calc R . . C22 C 0.4942(4) 0.2656(5) 0.3795(4) 0.0508(11) Uani 1 1 d . . . C23 C 0.5502(8) 0.1448(7) 0.4357(5) 0.098(3) Uani 1 1 d . . . H23 H 0.5809 0.0947 0.4016 0.117 Uiso 1 1 calc R . . C24 C 0.5623(9) 0.0945(9) 0.5455(6) 0.123(4) Uani 1 1 d . . . H24 H 0.5965 0.0102 0.5839 0.147 Uiso 1 1 calc R . . C25 C 0.5257(9) 0.1653(10) 0.5949(5) 0.109(3) Uani 1 1 d . . . H25 H 0.5393 0.1316 0.6670 0.130 Uiso 1 1 calc R . . C26 C 0.4703(9) 0.2829(10) 0.5430(6) 0.113(3) Uani 1 1 d . . . H26 H 0.4422 0.3310 0.5793 0.135 Uiso 1 1 calc R . . C27 C 0.4528(7) 0.3369(6) 0.4345(5) 0.081(2) Uani 1 1 d . . . H27 H 0.4136 0.4204 0.3987 0.097 Uiso 1 1 calc R . . O1 O 0.5129(3) 0.2835(3) -0.0994(3) 0.0456(7) Uani 1 1 d . . . O2 O 0.2516(3) 0.3772(3) -0.0600(3) 0.0515(8) Uani 1 1 d . . . O3 O 0.4005(3) 0.1815(3) 0.1191(3) 0.0495(8) Uani 1 1 d . . . O4 O 0.4193(2) 0.3986(3) 0.0109(2) 0.0354(6) Uani 1 1 d . . . O5 O 0.5550(3) 0.2454(3) 0.2014(2) 0.0435(7) Uani 1 1 d . . . O6 O 0.3474(3) 0.3527(3) 0.2201(2) 0.0489(7) Uani 1 1 d . . . O7 O 0.4901(3) 0.4594(3) 0.1958(2) 0.0454(7) Uani 1 1 d . . . O8 O 0.7281(3) 0.3776(3) 0.1435(2) 0.0447(7) Uani 1 1 d . . . O9 O 0.8047(3) 0.4530(3) -0.0407(3) 0.0470(7) Uani 1 1 d . . . O10 O 0.6753(3) 0.3253(3) 0.0055(2) 0.0430(7) Uani 1 1 d . . . P1 P 0.76566(9) 0.35082(10) 0.04793(9) 0.0388(2) Uani 1 1 d . . . P2 P 0.47166(10) 0.33533(10) 0.23989(8) 0.0404(2) Uani 1 1 d . . . Sn1 Sn 0.55292(2) 0.23656(2) 0.05961(2) 0.03830(9) Uani 1 1 d . . . Sn2 Sn 0.38235(3) 0.45975(3) -0.14498(2) 0.04019(10) Uani 1 1 d . . . Sn3 Sn 0.27752(3) 0.35665(3) 0.09255(2) 0.04289(10) Uani 1 1 d . . . O11 O 0.2030(11) 0.6064(12) 0.2410(10) 0.107(3) Uiso 0.50 1 d PD . . C28 C 0.1301(16) 0.5465(18) 0.2974(14) 0.110(5) Uiso 0.50 1 d PD . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.058(3) 0.039(3) 0.069(3) -0.029(2) 0.001(2) -0.003(2) C2 0.079(4) 0.042(3) 0.081(4) -0.015(3) -0.008(3) 0.001(3) C3 0.140(8) 0.049(4) 0.101(6) -0.001(4) -0.004(5) 0.012(4) C4 0.190(14) 0.110(9) 0.164(11) -0.017(8) -0.062(10) 0.046(9) C5 0.078(4) 0.063(3) 0.057(3) -0.034(3) -0.014(3) -0.014(3) C6 0.094(5) 0.077(4) 0.061(3) -0.025(3) -0.030(3) -0.013(4) C7 0.194(11) 0.092(6) 0.081(5) -0.033(4) -0.074(6) 0.001(6) C8 0.231(15) 0.143(10) 0.087(6) -0.013(7) -0.050(8) -0.030(10) C9 0.055(4) 0.072(4) 0.125(6) -0.030(4) 0.033(4) -0.035(3) C10 0.201(12) 0.231(14) 0.128(8) -0.102(9) 0.091(8) -0.177(12) C11 0.217(18) 0.219(18) 0.156(13) -0.060(13) 0.060(12) -0.081(15) C12 0.194(17) 0.33(3) 0.104(9) -0.032(13) 0.024(10) -0.023(17) C13 0.056(4) 0.116(6) 0.093(5) -0.046(4) -0.018(3) -0.026(4) C14 0.081(4) 0.049(3) 0.099(5) -0.037(3) -0.006(3) -0.026(3) C15 0.091(5) 0.074(4) 0.059(3) -0.042(3) 0.001(3) 0.010(3) C16 0.030(2) 0.043(2) 0.061(3) -0.027(2) -0.0044(18) -0.0024(18) C17 0.061(3) 0.058(3) 0.071(3) -0.027(3) 0.007(3) -0.004(3) C18 0.058(4) 0.084(5) 0.112(6) -0.055(4) 0.010(4) 0.015(3) C19 0.061(4) 0.068(4) 0.109(6) -0.030(4) -0.009(4) 0.024(3) C20 0.085(5) 0.072(4) 0.077(4) -0.006(4) -0.006(4) 0.018(4) C21 0.059(4) 0.066(4) 0.061(3) -0.018(3) -0.003(3) 0.009(3) C22 0.056(3) 0.053(3) 0.038(2) -0.017(2) 0.0051(19) -0.016(2) C23 0.136(7) 0.061(4) 0.053(3) -0.015(3) -0.012(4) 0.011(4) C24 0.153(9) 0.088(6) 0.064(4) -0.003(4) -0.018(5) 0.002(6) C25 0.141(8) 0.125(7) 0.041(3) -0.029(4) -0.006(4) -0.027(6) C26 0.150(8) 0.144(9) 0.054(4) -0.062(5) 0.012(5) -0.037(7) C27 0.120(6) 0.071(4) 0.050(3) -0.033(3) 0.013(3) -0.022(4) O1 0.0537(19) 0.0402(16) 0.0469(16) -0.0283(14) -0.0054(14) -0.0038(14) O2 0.0442(18) 0.053(2) 0.065(2) -0.0280(17) -0.0080(15) -0.0174(15) O3 0.0520(19) 0.0389(17) 0.061(2) -0.0250(15) -0.0008(15) -0.0132(15) O4 0.0377(15) 0.0335(14) 0.0363(14) -0.0191(11) -0.0008(11) -0.0067(12) O5 0.0488(18) 0.0379(16) 0.0416(15) -0.0201(13) -0.0026(13) -0.0059(13) O6 0.0501(19) 0.0521(19) 0.0441(16) -0.0238(15) 0.0051(14) -0.0128(15) O7 0.0495(19) 0.0399(17) 0.0456(16) -0.0221(14) 0.0037(13) -0.0090(14) O8 0.0454(17) 0.0394(16) 0.0471(16) -0.0222(13) -0.0081(13) -0.0027(13) O9 0.0418(17) 0.0384(16) 0.0543(18) -0.0201(14) 0.0042(14) -0.0060(13) O10 0.0368(16) 0.0502(18) 0.0466(16) -0.0272(14) 0.0021(13) -0.0109(13) P1 0.0321(5) 0.0365(5) 0.0461(6) -0.0216(5) -0.0032(4) -0.0020(4) P2 0.0464(6) 0.0373(6) 0.0351(5) -0.0176(4) 0.0018(4) -0.0080(5) Sn1 0.04071(17) 0.03130(15) 0.04259(16) -0.02064(12) -0.00216(12) -0.00356(12) Sn2 0.04466(18) 0.03813(17) 0.04049(16) -0.02274(13) -0.00580(12) -0.00605(12) Sn3 0.03882(17) 0.03923(17) 0.05071(18) -0.02057(14) 0.00246(13) -0.01150(13) _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 1.523(8) . ? C1 Sn1 2.139(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.518(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.457(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.509(8) . ? C5 Sn2 2.131(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.526(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.430(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.539(11) . ? C9 Sn3 2.126(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.434(13) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.457(18) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O2 1.423(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 O3 1.418(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 O1 1.402(6) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.362(7) . ? C16 C21 1.379(7) . ? C16 P1 1.798(4) . ? C17 C18 1.383(9) . ? C17 H17 0.9300 . ? C18 C19 1.327(11) . ? C18 H18 0.9300 . ? C19 C20 1.367(11) . ? C19 H19 0.9300 . ? C20 C21 1.367(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.350(8) . ? C22 C27 1.392(8) . ? C22 P2 1.791(5) . ? C23 C24 1.404(10) . ? C23 H23 0.9300 . ? C24 C25 1.321(13) . ? C24 H24 0.9300 . ? C25 C26 1.312(12) . ? C25 H25 0.9300 . ? C26 C27 1.392(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? O1 Sn1 2.144(3) . ? O1 Sn2 2.152(3) . ? O2 Sn3 2.120(4) . ? O2 Sn2 2.181(4) . ? O3 Sn3 2.142(3) . ? O3 Sn1 2.187(4) . ? O4 Sn2 2.050(3) . ? O4 Sn1 2.054(3) . ? O4 Sn3 2.081(3) . ? O5 P2 1.525(3) . ? O5 Sn1 2.076(3) . ? O6 P2 1.529(4) . ? O6 Sn3 2.082(3) . ? O7 P2 1.515(3) . ? O7 Sn2 2.067(3) 2_665 ? O8 P1 1.531(3) . ? O8 Sn2 2.082(3) 2_665 ? O9 P1 1.531(4) . ? O9 Sn3 2.105(3) 2_665 ? O10 P1 1.526(3) . ? O10 Sn1 2.075(3) . ? Sn2 O7 2.067(3) 2_665 ? Sn2 O8 2.082(3) 2_665 ? Sn3 O9 2.105(3) 2_665 ? O11 C28 1.340(15) . ? 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 Sn1 114.8(4) . . ? C2 C1 H1A 108.6 . . ? Sn1 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? Sn1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C3 C2 C1 111.6(6) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? C4 C3 C2 115.1(9) . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Sn2 117.1(4) . . ? C6 C5 H5A 108.0 . . ? Sn2 C5 H5A 108.0 . . ? C6 C5 H5B 108.0 . . ? Sn2 C5 H5B 108.0 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 111.8(6) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? C8 C7 C6 116.2(8) . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Sn3 114.9(5) . . ? C10 C9 H9A 108.5 . . ? Sn3 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? Sn3 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C9 125.5(12) . . ? C11 C10 H10A 106.0 . . ? C9 C10 H10A 106.0 . . ? C11 C10 H10B 106.0 . . ? C9 C10 H10B 106.0 . . ? H10A C10 H10B 106.3 . . ? C10 C11 C12 117.2(15) . . ? C10 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? C10 C11 H11B 108.0 . . ? C12 C11 H11B 108.0 . . ? H11A C11 H11B 107.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 H13A 109.5 . . ? O2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 117.5(5) . . ? C17 C16 P1 121.6(4) . . ? C21 C16 P1 120.8(4) . . ? C16 C17 C18 120.3(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 122.3(7) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C20 117.8(6) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C21 C20 C19 121.3(7) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C16 120.7(6) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C23 C22 C27 117.3(5) . . ? C23 C22 P2 122.9(5) . . ? C27 C22 P2 119.8(4) . . ? C22 C23 C24 120.4(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.8(8) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 120.4(7) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.0(8) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.9(7) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C15 O1 Sn1 124.2(3) . . ? C15 O1 Sn2 124.0(3) . . ? Sn1 O1 Sn2 101.87(12) . . ? C13 O2 Sn3 123.0(4) . . ? C13 O2 Sn2 122.5(4) . . ? Sn3 O2 Sn2 100.66(13) . . ? C14 O3 Sn3 121.5(3) . . ? C14 O3 Sn1 123.1(4) . . ? Sn3 O3 Sn1 100.06(14) . . ? Sn2 O4 Sn1 108.72(13) . . ? Sn2 O4 Sn3 106.55(13) . . ? Sn1 O4 Sn3 106.72(13) . . ? P2 O5 Sn1 129.12(18) . . ? P2 O6 Sn3 128.12(19) . . ? P2 O7 Sn2 141.5(2) . 2_665 ? P1 O8 Sn2 127.55(18) . 2_665 ? P1 O9 Sn3 125.77(19) . 2_665 ? P1 O10 Sn1 139.8(2) . . ? O10 P1 O9 109.89(19) . . ? O10 P1 O8 113.66(18) . . ? O9 P1 O8 112.17(19) . . ? O10 P1 C16 107.9(2) . . ? O9 P1 C16 107.0(2) . . ? O8 P1 C16 105.8(2) . . ? O7 P2 O5 114.21(19) . . ? O7 P2 O6 109.95(19) . . ? O5 P2 O6 111.73(19) . . ? O7 P2 C22 107.6(2) . . ? O5 P2 C22 106.3(2) . . ? O6 P2 C22 106.6(2) . . ? O4 Sn1 O10 93.24(13) . . ? O4 Sn1 O5 87.64(11) . . ? O10 Sn1 O5 89.36(12) . . ? O4 Sn1 C1 167.00(17) . . ? O10 Sn1 C1 96.60(19) . . ? O5 Sn1 C1 100.91(17) . . ? O4 Sn1 O1 74.59(11) . . ? O10 Sn1 O1 89.34(13) . . ? O5 Sn1 O1 162.08(12) . . ? C1 Sn1 O1 96.99(17) . . ? O4 Sn1 O3 75.11(13) . . ? O10 Sn1 O3 167.00(12) . . ? O5 Sn1 O3 84.50(13) . . ? C1 Sn1 O3 95.81(19) . . ? O1 Sn1 O3 92.99(13) . . ? O4 Sn2 O7 93.63(12) . 2_665 ? O4 Sn2 O8 87.83(11) . 2_665 ? O7 Sn2 O8 89.12(13) 2_665 2_665 ? O4 Sn2 C5 166.63(18) . . ? O7 Sn2 C5 96.1(2) 2_665 . ? O8 Sn2 C5 101.43(18) 2_665 . ? O4 Sn2 O1 74.48(11) . . ? O7 Sn2 O1 88.26(13) 2_665 . ? O8 Sn2 O1 161.91(12) 2_665 . ? C5 Sn2 O1 96.65(18) . . ? O4 Sn2 O2 74.68(12) . . ? O7 Sn2 O2 167.51(12) 2_665 . ? O8 Sn2 O2 86.10(14) 2_665 . ? C5 Sn2 O2 96.1(2) . . ? O1 Sn2 O2 92.71(14) . . ? O4 Sn3 O6 86.61(12) . . ? O4 Sn3 O9 87.70(12) . 2_665 ? O6 Sn3 O9 89.00(13) . 2_665 ? O4 Sn3 O2 75.41(12) . . ? O6 Sn3 O2 161.99(14) . . ? O9 Sn3 O2 89.22(13) 2_665 . ? O4 Sn3 C9 175.2(2) . . ? O6 Sn3 C9 95.2(3) . . ? O9 Sn3 C9 96.8(2) 2_665 . ? O2 Sn3 C9 102.8(3) . . ? O4 Sn3 O3 75.55(13) . . ? O6 Sn3 O3 90.16(13) . . ? O9 Sn3 O3 163.25(13) 2_665 . ? O2 Sn3 O3 86.43(14) . . ? C9 Sn3 O3 100.0(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.027 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.123 #===END data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 737802' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H69 O9 P3 Sn3' _chemical_formula_weight 1166.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.794(3) _cell_length_b 21.870(5) _cell_length_c 17.051(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.379(8) _cell_angle_gamma 90.00 _cell_volume 5204.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used total _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.47 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.289 _exptl_crystal_size_mid 0.139 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.566 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47860 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11628 _reflns_number_gt 7901 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2\s(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^)+(0.0841P)^2^+3.0748P] 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 11628 _refine_ls_number_parameters 453 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1605 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9677(7) 0.9383(4) 0.2639(5) 0.087(3) Uani 1 1 d D . . H1A H 0.9109 0.9213 0.2721 0.104 Uiso 1 1 calc R . . H1B H 0.9476 0.9553 0.2082 0.104 Uiso 1 1 calc R . . C2 C 1.0323(13) 0.8869(8) 0.2651(11) 0.264(13) Uani 1 1 d D . . H2A H 1.0679 0.8776 0.3228 0.317 Uiso 1 1 calc R . . H2B H 0.9930 0.8515 0.2420 0.317 Uiso 1 1 calc R . . C3 C 1.0971(13) 0.8940(12) 0.2238(18) 0.317(17) Uani 1 1 d D . . H3A H 1.1329 0.9304 0.2480 0.381 Uiso 1 1 calc R . . H3B H 1.0583 0.9055 0.1677 0.381 Uiso 1 1 calc R . . C4 C 1.1673(12) 0.8535(9) 0.2125(15) 0.256(11) Uani 1 1 d D . . H4A H 1.1998 0.8731 0.1791 0.383 Uiso 1 1 calc R . . H4B H 1.1366 0.8170 0.1853 0.383 Uiso 1 1 calc R . . H4C H 1.2129 0.8433 0.2657 0.383 Uiso 1 1 calc R . . C5 C 1.1323(5) 1.0711(4) 0.3691(6) 0.085(3) Uani 1 1 d D . . H5A H 1.1167 1.0973 0.3206 0.103 Uiso 1 1 calc R . . H5B H 1.1315 1.0972 0.4149 0.103 Uiso 1 1 calc R . . C6 C 1.2308(13) 1.0544(12) 0.3866(19) 0.365(17) Uiso 1 1 d D . . H6A H 1.2326 1.0248 0.3447 0.438 Uiso 1 1 calc R . . H6B H 1.2508 1.0331 0.4394 0.438 Uiso 1 1 calc R . . C7 C 1.3096(13) 1.1037(10) 0.3911(17) 0.290(14) Uani 1 1 d D . . H7A H 1.3038 1.1370 0.4267 0.348 Uiso 1 1 calc R . . H7B H 1.3724 1.0855 0.4159 0.348 Uiso 1 1 calc R . . C8 C 1.302(2) 1.1284(16) 0.309(2) 0.41(2) Uiso 1 1 d D . . H8A H 1.3637 1.1423 0.3095 0.622 Uiso 1 1 calc R . . H8B H 1.2576 1.1619 0.2958 0.622 Uiso 1 1 calc R . . H8C H 1.2794 1.0969 0.2677 0.622 Uiso 1 1 calc R . . C9 C 0.6602(5) 0.9249(3) 0.1071(5) 0.0631(18) Uani 1 1 d D . . H9A H 0.6650 0.9388 0.1623 0.076 Uiso 1 1 calc R . . H9B H 0.5955 0.9096 0.0815 0.076 Uiso 1 1 calc R . . C10 C 0.7261(6) 0.8723(4) 0.1172(6) 0.086(3) Uani 1 1 d D . . H10A H 0.7914 0.8874 0.1345 0.103 Uiso 1 1 calc R . . H10B H 0.7132 0.8525 0.0637 0.103 Uiso 1 1 calc R . . C11 C 0.7183(9) 0.8254(5) 0.1791(10) 0.149(6) Uani 1 1 d D . . H11A H 0.7171 0.8469 0.2285 0.179 Uiso 1 1 calc R . . H11B H 0.6570 0.8049 0.1559 0.179 Uiso 1 1 calc R . . C12 C 0.7929(11) 0.7786(7) 0.2048(11) 0.202(8) Uani 1 1 d D . . H12A H 0.7809 0.7524 0.2454 0.302 Uiso 1 1 calc R . . H12B H 0.8543 0.7979 0.2286 0.302 Uiso 1 1 calc R . . H12C H 0.7925 0.7549 0.1574 0.302 Uiso 1 1 calc R . . C13 C 0.7495(5) 1.0390(4) -0.0381(5) 0.071(2) Uani 1 1 d D . . C14 C 0.7752(15) 0.9904(8) -0.0916(12) 0.104(7) Uani 0.50 1 d PD . . C14' C 0.8479(13) 1.0111(10) -0.0218(17) 0.130(9) Uani 0.50 1 d PD . . C15 C 0.8405(13) 0.9440(7) -0.0394(14) 0.215(10) Uani 1 1 d D . . C16 C 0.8941(16) 0.9041(11) -0.0717(15) 0.300(13) Uiso 1 1 d D . . H16A H 0.9301 0.8765 -0.0289 0.451 Uiso 1 1 calc R . . H16B H 0.9372 0.9274 -0.0914 0.451 Uiso 1 1 calc R . . H16C H 0.8514 0.8811 -0.1170 0.451 Uiso 1 1 calc R . . C17 C 0.6908(5) 0.9781(3) 0.3433(5) 0.0623(18) Uani 1 1 d D . . H17A H 0.7274 0.9596 0.3116 0.075 Uiso 1 1 calc R . . H17B H 0.7270 0.9725 0.4017 0.075 Uiso 1 1 calc R . . C18 C 0.5983(6) 0.9445(4) 0.3243(7) 0.099(3) Uani 1 1 d D . . H18A H 0.6121 0.9018 0.3383 0.119 Uiso 1 1 calc R . . H18B H 0.5647 0.9468 0.2649 0.119 Uiso 1 1 calc R . . C19 C 0.5316(9) 0.9679(6) 0.3694(10) 0.145(5) Uani 1 1 d D . . H19A H 0.5684 0.9698 0.4282 0.175 Uiso 1 1 calc R . . H19B H 0.5139 1.0095 0.3510 0.175 Uiso 1 1 calc R . . C20 C 0.4403(11) 0.9334(7) 0.3608(15) 0.258(12) Uani 1 1 d D . . H20A H 0.4057 0.9541 0.3916 0.388 Uiso 1 1 calc R . . H20B H 0.4557 0.8927 0.3820 0.388 Uiso 1 1 calc R . . H20C H 0.4014 0.9316 0.3032 0.388 Uiso 1 1 calc R . . C21 C 0.5997(5) 1.1442(3) 0.3462(5) 0.0643(19) Uani 1 1 d D . . H21A H 0.5324 1.1372 0.3158 0.077 Uiso 1 1 calc R . . H21B H 0.6078 1.1420 0.4050 0.077 Uiso 1 1 calc R . . C22 C 0.6246(6) 1.2070(4) 0.3274(6) 0.084(2) Uani 1 1 d D . . H22A H 0.6132 1.2107 0.2682 0.101 Uiso 1 1 calc R . . H22B H 0.6922 1.2144 0.3563 0.101 Uiso 1 1 calc R . . C23 C 0.5654(8) 1.2550(4) 0.3538(8) 0.117(4) Uani 1 1 d D . . H23A H 0.4980 1.2480 0.3237 0.140 Uiso 1 1 calc R . . H23B H 0.5753 1.2501 0.4126 0.140 Uiso 1 1 calc R . . C24 C 0.5904(11) 1.3187(5) 0.3383(11) 0.187(7) Uani 1 1 d D . . H24A H 0.5516 1.3469 0.3564 0.281 Uiso 1 1 calc R . . H24B H 0.5789 1.3243 0.2799 0.281 Uiso 1 1 calc R . . H24C H 0.6568 1.3262 0.3685 0.281 Uiso 1 1 calc R . . C31 C 0.8288(5) 1.1570(3) 0.1473(5) 0.0632(18) Uani 1 1 d . . . C32 C 0.7540(6) 1.1978(5) 0.1256(7) 0.108(4) Uani 1 1 d . . . H32 H 0.6996 1.1892 0.1393 0.130 Uiso 1 1 calc R . . C33 C 0.7578(8) 1.2516(5) 0.0835(8) 0.130(5) Uani 1 1 d . . . H33 H 0.7090 1.2804 0.0734 0.156 Uiso 1 1 calc R . . C34 C 0.8336(9) 1.2615(6) 0.0575(8) 0.130(4) Uani 1 1 d . . . H34 H 0.8338 1.2947 0.0235 0.156 Uiso 1 1 calc R . . C35 C 0.9070(9) 1.2238(6) 0.0805(10) 0.163(7) Uani 1 1 d . . . H35 H 0.9607 1.2326 0.0657 0.195 Uiso 1 1 calc R . . C36 C 0.9067(8) 1.1724(5) 0.1251(9) 0.133(5) Uani 1 1 d . . . H36 H 0.9603 1.1472 0.1409 0.159 Uiso 1 1 calc R . . C37 C 0.4717(4) 1.1434(3) 0.0990(4) 0.0551(16) Uani 1 1 d . . . C38 C 0.4059(5) 1.1581(4) 0.1363(5) 0.076(2) Uani 1 1 d . . . H38 H 0.3875 1.1284 0.1670 0.091 Uiso 1 1 calc R . . C39 C 0.3658(6) 1.2158(5) 0.1298(7) 0.102(3) Uani 1 1 d . . . H39 H 0.3208 1.2246 0.1554 0.123 Uiso 1 1 calc R . . C40 C 0.3927(8) 1.2591(5) 0.0857(8) 0.120(4) Uani 1 1 d . . . H40 H 0.3664 1.2981 0.0817 0.144 Uiso 1 1 calc R . . C41 C 0.4566(7) 1.2469(4) 0.0477(8) 0.112(4) Uani 1 1 d . . . H41 H 0.4745 1.2773 0.0176 0.134 Uiso 1 1 calc R . . C42 C 0.4964(5) 1.1884(4) 0.0530(6) 0.080(2) Uani 1 1 d . . . H42 H 0.5396 1.1798 0.0255 0.096 Uiso 1 1 calc R . . O4 O 0.9278(3) 1.0772(2) 0.2618(3) 0.0580(11) Uani 1 1 d . . . O5 O 0.7859(3) 1.0357(2) 0.1491(3) 0.0597(12) Uani 1 1 d . . . O6 O 0.7608(3) 1.1077(2) 0.2557(3) 0.0564(11) Uani 1 1 d . . . O7 O 0.5887(3) 1.0695(2) 0.0562(3) 0.0566(11) Uani 1 1 d . . . O8 O 0.5718(3) 1.0553(2) 0.1989(3) 0.0619(12) Uani 1 1 d . . . P2 P 0.82582(10) 1.08925(8) 0.20557(10) 0.0475(4) Uani 1 1 d . . . P3 P 0.52055(10) 1.06771(8) 0.10809(10) 0.0489(4) Uani 1 1 d . . . Sn1 Sn 1.01354(3) 1.01213(2) 0.34780(3) 0.04658(13) Uani 1 1 d . . . Sn2 Sn 0.67448(3) 1.002838(19) 0.03869(3) 0.04542(13) Uani 1 1 d . . . Sn3 Sn 0.67963(3) 1.073237(19) 0.31781(3) 0.04445(13) Uani 1 1 d . . . P1 P 0.89855(10) 1.07257(7) 0.46676(10) 0.0438(3) Uiso 1 1 d . . . O1 O 0.9208(3) 1.02361(19) 0.4111(3) 0.0470(9) Uiso 1 1 d . . . O3 O 0.7983(3) 1.0967(2) 0.4268(3) 0.0534(10) Uiso 1 1 d . . . O2 O 0.9128(3) 1.0486(2) 0.5524(3) 0.0573(11) Uiso 1 1 d . . . C25 C 0.9815(4) 1.1346(3) 0.4752(4) 0.0553(15) Uiso 1 1 d . . . C26 C 0.9605(5) 1.1801(4) 0.4153(5) 0.072(2) Uiso 1 1 d . . . H26 H 0.9022 1.1799 0.3721 0.086 Uiso 1 1 calc R . . C30 C 1.0681(5) 1.1366(4) 0.5394(5) 0.074(2) Uiso 1 1 d . . . H30 H 1.0829 1.1062 0.5797 0.089 Uiso 1 1 calc R . . C28 C 1.1109(7) 1.2271(5) 0.4863(6) 0.097(3) Uiso 1 1 d . . . H28 H 1.1534 1.2594 0.4910 0.116 Uiso 1 1 calc R . . C29 C 1.1338(7) 1.1836(4) 0.5447(6) 0.092(3) Uiso 1 1 d . . . H29 H 1.1921 1.1846 0.5878 0.110 Uiso 1 1 calc R . . C27 C 1.0279(6) 1.2263(5) 0.4202(6) 0.095(3) Uiso 1 1 d . . . H27 H 1.0161 1.2560 0.3790 0.114 Uiso 1 1 calc R . . O9 O 0.4394(3) 1.0229(2) 0.0738(3) 0.0598(11) Uiso 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 0.114(7) 0.077(6) 0.057(5) -0.025(4) 0.012(4) 0.013(5) C2 0.28(2) 0.26(2) 0.199(19) -0.135(18) 0.019(17) 0.13(2) C3 0.181(19) 0.44(4) 0.40(4) 0.12(3) 0.20(2) 0.13(2) C4 0.169(15) 0.26(2) 0.37(3) -0.03(2) 0.132(18) 0.053(16) C5 0.040(4) 0.096(6) 0.117(7) -0.023(5) 0.021(4) -0.009(4) C7 0.162(16) 0.22(2) 0.45(4) 0.03(3) 0.04(2) -0.090(16) C9 0.060(4) 0.068(5) 0.056(4) 0.002(3) 0.013(3) -0.002(3) C10 0.070(5) 0.069(5) 0.114(7) 0.024(5) 0.024(5) 0.002(4) C11 0.127(9) 0.079(7) 0.251(17) 0.059(9) 0.075(10) 0.031(7) C12 0.212(16) 0.163(16) 0.226(19) 0.085(14) 0.066(15) -0.005(13) C13 0.064(4) 0.090(6) 0.069(5) 0.005(4) 0.036(4) -0.009(4) C14 0.112(16) 0.114(17) 0.111(18) -0.002(13) 0.071(15) -0.016(13) C14' 0.122(19) 0.17(3) 0.12(2) 0.001(18) 0.069(17) -0.016(17) C15 0.26(2) 0.123(12) 0.37(3) 0.061(15) 0.25(2) 0.076(13) C17 0.066(4) 0.051(4) 0.064(5) 0.005(3) 0.012(3) -0.003(3) C18 0.101(7) 0.060(5) 0.143(9) 0.002(6) 0.048(6) -0.013(5) C19 0.136(10) 0.118(10) 0.218(16) 0.010(10) 0.106(11) -0.015(8) C20 0.185(16) 0.161(15) 0.50(4) 0.038(19) 0.21(2) -0.040(12) C21 0.053(4) 0.072(5) 0.060(4) -0.010(4) 0.008(3) 0.017(3) C22 0.084(5) 0.077(6) 0.093(7) -0.007(5) 0.031(5) 0.016(4) C23 0.137(9) 0.082(7) 0.134(10) -0.022(7) 0.049(7) 0.021(6) C24 0.200(15) 0.072(8) 0.30(2) -0.010(11) 0.097(15) 0.026(9) C31 0.066(4) 0.064(4) 0.061(5) 0.008(4) 0.022(3) -0.009(3) C32 0.077(6) 0.097(7) 0.144(9) 0.069(7) 0.027(6) 0.009(5) C33 0.103(8) 0.094(8) 0.180(12) 0.067(8) 0.030(8) 0.011(6) C34 0.132(9) 0.111(9) 0.147(11) 0.062(8) 0.047(8) -0.025(8) C35 0.137(10) 0.145(12) 0.256(18) 0.105(12) 0.131(12) 0.031(9) C36 0.111(8) 0.109(8) 0.215(14) 0.081(9) 0.104(9) 0.027(6) C37 0.047(3) 0.067(4) 0.046(4) -0.009(3) 0.009(3) 0.005(3) C38 0.062(4) 0.110(7) 0.060(5) 0.008(4) 0.025(4) 0.023(4) C39 0.077(6) 0.114(8) 0.120(9) -0.015(7) 0.036(6) 0.039(6) C40 0.116(8) 0.074(7) 0.165(12) -0.004(7) 0.041(8) 0.034(6) C41 0.095(7) 0.061(6) 0.185(12) 0.004(6) 0.055(7) 0.012(5) C42 0.071(5) 0.068(5) 0.100(7) 0.000(5) 0.029(4) 0.009(4) O4 0.042(2) 0.073(3) 0.050(3) 0.006(2) 0.0035(18) -0.006(2) O5 0.046(2) 0.062(3) 0.059(3) -0.006(2) 0.000(2) -0.001(2) O6 0.054(2) 0.062(3) 0.056(3) 0.008(2) 0.021(2) -0.003(2) O7 0.053(2) 0.056(3) 0.060(3) 0.002(2) 0.018(2) 0.0113(19) O8 0.050(2) 0.091(4) 0.037(2) -0.003(2) 0.0034(18) 0.001(2) P2 0.0398(8) 0.0568(10) 0.0415(9) 0.0041(7) 0.0076(6) -0.0046(6) P3 0.0367(8) 0.0587(10) 0.0453(9) -0.0039(7) 0.0056(6) 0.0023(6) Sn1 0.0357(2) 0.0616(3) 0.0403(2) -0.00694(18) 0.00981(16) 0.00067(17) Sn2 0.0379(2) 0.0507(3) 0.0446(3) 0.00015(18) 0.00955(17) 0.00074(16) Sn3 0.0379(2) 0.0510(3) 0.0412(2) 0.00026(17) 0.00893(16) 0.00286(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.471(13) . ? C1 Sn1 2.115(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.375(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.425(15) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.434(17) . ? C5 Sn1 2.112(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.572(17) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.469(18) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.482(9) . ? C9 Sn2 2.114(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.502(11) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.462(13) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14' 1.517(17) . ? C13 C14 1.530(16) . ? C13 Sn2 2.130(7) . ? C14 C14' 1.39(3) . ? C14 C15 1.477(17) . ? C14' C15 1.496(17) . ? C15 C16 1.408(16) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.492(9) . ? C17 Sn3 2.120(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.527(12) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.511(13) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.484(10) . ? C21 Sn3 2.104(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.528(10) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.490(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C31 C36 1.369(11) . ? C31 C32 1.372(11) . ? C31 P2 1.793(7) . ? C32 C33 1.389(12) . ? C32 H32 0.9300 . ? C33 C34 1.354(15) . ? C33 H33 0.9300 . ? C34 C35 1.315(15) . ? C34 H34 0.9300 . ? C35 C36 1.359(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.366(9) . ? C37 C42 1.382(11) . ? C37 P3 1.792(7) . ? C38 C39 1.383(12) . ? C38 H38 0.9300 . ? C39 C40 1.349(15) . ? C39 H39 0.9300 . ? C40 C41 1.339(15) . ? C40 H40 0.9300 . ? C41 C42 1.398(12) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? O4 P2 1.519(4) . ? O4 Sn1 2.133(4) . ? O5 P2 1.506(5) . ? O5 Sn2 2.173(4) . ? O6 P2 1.538(4) . ? O6 Sn3 1.994(4) . ? O7 P3 1.547(5) . ? O7 Sn2 2.019(4) . ? O8 P3 1.505(4) . ? O8 Sn3 2.159(4) . ? P3 O9 1.510(5) . ? Sn1 O1 2.023(4) . ? Sn1 O2 2.148(5) 3_776 ? Sn2 O9 2.165(5) 3_675 ? Sn3 O3 2.152(4) . ? P1 O2 1.500(5) . ? P1 O3 1.507(4) . ? P1 O1 1.538(4) . ? P1 C25 1.803(7) . ? O2 Sn1 2.148(5) 3_776 ? C25 C30 1.383(10) . ? C25 C26 1.384(10) . ? C26 C27 1.403(11) . ? C26 H26 0.9300 . ? C30 C29 1.395(11) . ? C30 H30 0.9300 . ? C28 C29 1.337(12) . ? C28 C27 1.364(12) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C27 H27 0.9300 . ? O9 Sn2 2.165(5) 3_675 ? 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 Sn1 120.8(9) . . ? C2 C1 H1A 107.1 . . ? Sn1 C1 H1A 107.1 . . ? C2 C1 H1B 107.1 . . ? Sn1 C1 H1B 107.1 . . ? H1A C1 H1B 106.8 . . ? C3 C2 C1 117.9(18) . . ? C3 C2 H2A 107.8 . . ? C1 C2 H2A 107.8 . . ? C3 C2 H2B 107.8 . . ? C1 C2 H2B 107.8 . . ? H2A C2 H2B 107.2 . . ? C2 C3 C4 132(2) . . ? C2 C3 H3A 104.4 . . ? C4 C3 H3A 104.4 . . ? C2 C3 H3B 104.4 . . ? C4 C3 H3B 104.4 . . ? H3A C3 H3B 105.6 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Sn1 127.6(12) . . ? C6 C5 H5A 105.4 . . ? Sn1 C5 H5A 105.4 . . ? C6 C5 H5B 105.4 . . ? Sn1 C5 H5B 105.4 . . ? H5A C5 H5B 106.0 . . ? C5 C6 C7 121.4(19) . . ? C5 C6 H6A 107.0 . . ? C7 C6 H6A 107.0 . . ? C5 C6 H6B 107.0 . . ? C7 C6 H6B 107.0 . . ? H6A C6 H6B 106.7 . . ? C8 C7 C6 112.5(17) . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 Sn2 120.6(5) . . ? C10 C9 H9A 107.2 . . ? Sn2 C9 H9A 107.2 . . ? C10 C9 H9B 107.2 . . ? Sn2 C9 H9B 107.2 . . ? H9A C9 H9B 106.8 . . ? C9 C10 C11 114.3(8) . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C10 117.5(11) . . ? C12 C11 H11A 107.9 . . ? C10 C11 H11A 107.9 . . ? C12 C11 H11B 107.9 . . ? C10 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14' C13 C14 54.3(12) . . ? C14' C13 Sn2 113.7(10) . . ? C14 C13 Sn2 113.1(8) . . ? C14' C14 C15 62.8(11) . . ? C14' C14 C13 62.4(10) . . ? C15 C14 C13 111.1(14) . . ? C14 C14' C15 61.5(11) . . ? C14 C14' C13 63.3(11) . . ? C15 C14' C13 110.8(14) . . ? C16 C15 C14 122.0(19) . . ? C16 C15 C14' 132.3(17) . . ? C14 C15 C14' 55.7(13) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 Sn3 115.8(5) . . ? C18 C17 H17A 108.3 . . ? Sn3 C17 H17A 108.3 . . ? C18 C17 H17B 108.3 . . ? Sn3 C17 H17B 108.3 . . ? H17A C17 H17B 107.4 . . ? C17 C18 C19 115.2(8) . . ? C17 C18 H18A 108.5 . . ? C19 C18 H18A 108.5 . . ? C17 C18 H18B 108.5 . . ? C19 C18 H18B 108.5 . . ? H18A C18 H18B 107.5 . . ? C20 C19 C18 119.4(12) . . ? C20 C19 H19A 107.5 . . ? C18 C19 H19A 107.5 . . ? C20 C19 H19B 107.5 . . ? C18 C19 H19B 107.5 . . ? H19A C19 H19B 107.0 . . ? 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 . . ? C22 C21 Sn3 115.7(5) . . ? C22 C21 H21A 108.4 . . ? Sn3 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? Sn3 C21 H21B 108.4 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 111.3(7) . . ? C21 C22 H22A 109.4 . . ? C23 C22 H22A 109.4 . . ? C21 C22 H22B 109.4 . . ? C23 C22 H22B 109.4 . . ? H22A C22 H22B 108.0 . . ? C24 C23 C22 112.9(10) . . ? C24 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C36 C31 C32 116.3(8) . . ? C36 C31 P2 122.3(7) . . ? C32 C31 P2 121.4(6) . . ? C31 C32 C33 121.6(9) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 119.0(11) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C33 119.6(10) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 122.0(10) . . ? C34 C35 H35 119.0 . . ? C36 C35 H35 119.0 . . ? C35 C36 C31 121.2(10) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C38 C37 C42 117.3(7) . . ? C38 C37 P3 120.5(6) . . ? C42 C37 P3 122.2(5) . . ? C37 C38 C39 122.0(9) . . ? C37 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C40 C39 C38 119.2(9) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C41 C40 C39 121.1(10) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.0(11) . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C37 C42 C41 120.3(9) . . ? C37 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? P2 O4 Sn1 142.2(3) . . ? P2 O5 Sn2 146.6(3) . . ? P2 O6 Sn3 142.5(3) . . ? P3 O7 Sn2 128.9(3) . . ? P3 O8 Sn3 153.7(3) . . ? O5 P2 O4 111.4(3) . . ? O5 P2 O6 112.0(3) . . ? O4 P2 O6 111.6(3) . . ? O5 P2 C31 111.4(3) . . ? O4 P2 C31 107.0(3) . . ? O6 P2 C31 103.0(3) . . ? O8 P3 O9 110.2(3) . . ? O8 P3 O7 113.0(3) . . ? O9 P3 O7 112.4(3) . . ? O8 P3 C37 107.8(3) . . ? O9 P3 C37 108.7(3) . . ? O7 P3 C37 104.4(3) . . ? O1 Sn1 C5 120.4(3) . . ? O1 Sn1 C1 109.5(3) . . ? C5 Sn1 C1 130.1(4) . . ? O1 Sn1 O4 86.01(17) . . ? C5 Sn1 O4 89.0(3) . . ? C1 Sn1 O4 93.4(3) . . ? O1 Sn1 O2 84.85(16) . 3_776 ? C5 Sn1 O2 93.8(3) . 3_776 ? C1 Sn1 O2 91.6(3) . 3_776 ? O4 Sn1 O2 170.61(18) . 3_776 ? O7 Sn2 C9 108.5(2) . . ? O7 Sn2 C13 107.7(3) . . ? C9 Sn2 C13 143.7(3) . . ? O7 Sn2 O9 88.63(18) . 3_675 ? C9 Sn2 O9 95.1(2) . 3_675 ? C13 Sn2 O9 87.8(2) . 3_675 ? O7 Sn2 O5 88.07(17) . . ? C9 Sn2 O5 88.5(2) . . ? C13 Sn2 O5 90.6(3) . . ? O9 Sn2 O5 175.73(17) 3_675 . ? O6 Sn3 C21 109.1(2) . . ? O6 Sn3 C17 117.4(2) . . ? C21 Sn3 C17 133.5(3) . . ? O6 Sn3 O3 84.59(17) . . ? C21 Sn3 O3 89.2(2) . . ? C17 Sn3 O3 94.1(2) . . ? O6 Sn3 O8 87.56(18) . . ? C21 Sn3 O8 93.1(2) . . ? C17 Sn3 O8 89.9(2) . . ? O3 Sn3 O8 172.14(17) . . ? O2 P1 O3 111.2(3) . . ? O2 P1 O1 111.6(3) . . ? O3 P1 O1 110.1(2) . . ? O2 P1 C25 108.3(3) . . ? O3 P1 C25 108.3(3) . . ? O1 P1 C25 107.1(3) . . ? P1 O1 Sn1 137.6(2) . . ? P1 O3 Sn3 134.9(3) . . ? P1 O2 Sn1 149.1(3) . 3_776 ? C30 C25 C26 118.9(7) . . ? C30 C25 P1 121.0(6) . . ? C26 C25 P1 120.1(5) . . ? C25 C26 C27 119.5(8) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C25 C30 C29 121.1(8) . . ? C25 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C29 C28 C27 122.8(10) . . ? C29 C28 H28 118.6 . . ? C27 C28 H28 118.6 . . ? C28 C29 C30 118.5(9) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C28 C27 C26 119.0(10) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? P3 O9 Sn2 142.8(3) . 3_675 ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.312 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.123 #===END data_compound-3 _database_code_depnum_ccdc_archive 'CCDC 737803' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H22 As N O6 Sn' _chemical_formula_weight 493.94 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' 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 c2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3171(10) _cell_length_b 16.9883(11) _cell_length_c 12.3270(15) _cell_angle_alpha 90.000(2) _cell_angle_beta 122.929(2) _cell_angle_gamma 90.000(2) _cell_volume 3746.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used total _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.163 _exptl_crystal_size_mid 0.133 _exptl_crystal_size_min 0.111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 3.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.708 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9411 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3329 _reflns_number_gt 2486 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL-PLUS (Sheldrick, 1990)' _computing_publication_material SHELXL-97 _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^ > 2\s(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^)+(0.0765P)^2^+23.2170P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3329 _refine_ls_number_parameters 182 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.202 _refine_ls_shift/su_mean 0.014 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 0.3193(6) 0.3748(6) 0.3932(9) 0.079(3) Uani 1 1 d . . . H1A H 0.2665 0.3881 0.3434 0.095 Uiso 1 1 calc R . . H1B H 0.3348 0.3712 0.3326 0.095 Uiso 1 1 calc R . . C2 C 0.3263(6) 0.2934(6) 0.4483(10) 0.083(3) Uani 1 1 d . . . H2A H 0.3786 0.2782 0.4975 0.099 Uiso 1 1 calc R . . H2B H 0.3095 0.2949 0.5072 0.099 Uiso 1 1 calc R . . C3 C 0.2817(8) 0.2320(7) 0.3455(12) 0.110(4) Uani 1 1 d . . . H3A H 0.2289 0.2435 0.3039 0.132 Uiso 1 1 calc R . . H3B H 0.2939 0.2353 0.2803 0.132 Uiso 1 1 calc R . . C4 C 0.2963(9) 0.1492(8) 0.3980(14) 0.133(5) Uani 1 1 d . . . H4A H 0.2666 0.1130 0.3286 0.199 Uiso 1 1 calc R . . H4B H 0.2833 0.1451 0.4611 0.199 Uiso 1 1 calc R . . H4C H 0.3483 0.1369 0.4376 0.199 Uiso 1 1 calc R . . C5 C 0.4665(5) 0.3296(4) 0.9266(8) 0.058(2) Uani 1 1 d . . . C6 C 0.5027(5) 0.3265(5) 1.0606(8) 0.066(2) Uani 1 1 d . . . H6 H 0.5118 0.3729 1.1069 0.079 Uiso 1 1 calc R . . C7 C 0.5251(6) 0.2561(5) 1.1249(9) 0.076(3) Uani 1 1 d . . . H7 H 0.5508 0.2555 1.2146 0.091 Uiso 1 1 calc R . . C8 C 0.5103(6) 0.1868(6) 1.0592(10) 0.082(3) Uani 1 1 d . . . C9 C 0.4729(7) 0.1900(5) 0.9255(10) 0.088(3) Uani 1 1 d . . . C10 C 0.4521(6) 0.2609(5) 0.8603(8) 0.069(3) Uani 1 1 d . . . H10 H 0.4282 0.2618 0.7708 0.083 Uiso 1 1 calc R . . C11 C 0.3436(6) 0.5758(6) 0.5668(12) 0.089(3) Uani 1 1 d D . . H11A H 0.3472 0.5640 0.6470 0.107 Uiso 1 1 calc R . . H11B H 0.3824 0.6142 0.5884 0.107 Uiso 1 1 calc R . . C12 C 0.2713(13) 0.6191(16) 0.485(3) 0.306(16) Uiso 1 1 d D . . H12A H 0.2679 0.6629 0.5325 0.367 Uiso 1 1 calc R . . H12B H 0.2659 0.6388 0.4068 0.367 Uiso 1 1 calc R . . C13 C 0.2131(12) 0.557(2) 0.455(4) 0.36(2) Uiso 1 1 d D . . H13A H 0.2354 0.5112 0.5096 0.434 Uiso 1 1 calc R . . H13B H 0.1864 0.5416 0.3654 0.434 Uiso 1 1 calc R . . C14 C 0.162(2) 0.600(2) 0.486(4) 0.37(2) Uiso 1 1 d D . . H14A H 0.1254 0.5638 0.4784 0.548 Uiso 1 1 calc R . . H14B H 0.1381 0.6426 0.4269 0.548 Uiso 1 1 calc R . . H14C H 0.1913 0.6197 0.5729 0.548 Uiso 1 1 calc R . . N1 N 0.4515(8) 0.1201(9) 0.8466(16) 0.145(5) Uiso 1 1 d . . . O1 O 0.4001(3) 0.4037(3) 0.6822(5) 0.0606(15) Uani 1 1 d . . . O2 O 0.5110(3) 0.4874(3) 0.8920(5) 0.0522(13) Uani 1 1 d . . . O3 O 0.3738(3) 0.4728(3) 0.8554(5) 0.0616(15) Uani 1 1 d . . . O4 O 0.5345(6) 0.1205(4) 1.1317(8) 0.102(3) Uani 1 1 d D . . O5 O 0.4749(6) 0.0545(7) 0.9066(12) 0.146(4) Uiso 1 1 d . . . O6 O 0.4175(7) 0.1238(8) 0.7286(15) 0.177(5) Uiso 1 1 d . . . As1 As 0.43610(5) 0.42724(4) 0.83598(7) 0.0497(3) Uani 1 1 d . . . Sn1 Sn 0.37754(3) 0.47199(3) 0.51816(5) 0.0536(2) Uani 1 1 d . . . H8A H 0.493(4) 0.098(6) 1.067(8) 0.10(4) Uiso 1 1 d 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 0.112(8) 0.070(6) 0.051(5) -0.013(5) 0.041(5) -0.021(6) C2 0.104(8) 0.085(7) 0.073(7) -0.026(5) 0.056(6) -0.029(6) C3 0.142(11) 0.088(8) 0.087(8) -0.022(7) 0.055(8) -0.047(8) C4 0.188(15) 0.097(10) 0.125(12) -0.047(9) 0.093(11) -0.057(10) C5 0.086(6) 0.043(4) 0.049(5) 0.005(4) 0.039(4) 0.000(4) C6 0.097(7) 0.052(5) 0.055(5) 0.005(4) 0.045(5) 0.006(5) C7 0.115(8) 0.061(6) 0.053(5) 0.006(4) 0.046(6) 0.000(5) C8 0.114(8) 0.057(6) 0.073(7) 0.015(5) 0.051(6) -0.004(5) C9 0.140(10) 0.044(5) 0.061(6) -0.013(4) 0.042(6) -0.012(5) C10 0.111(8) 0.047(5) 0.046(5) 0.001(4) 0.040(5) -0.002(5) C11 0.113(9) 0.072(7) 0.097(8) 0.012(6) 0.068(7) 0.023(6) O1 0.100(4) 0.048(3) 0.038(3) -0.008(2) 0.039(3) -0.016(3) O2 0.073(3) 0.044(3) 0.040(3) -0.002(2) 0.030(3) -0.004(2) O3 0.076(4) 0.064(4) 0.036(3) -0.009(2) 0.025(3) 0.003(3) O4 0.153(8) 0.057(4) 0.080(5) 0.025(4) 0.054(6) 0.010(5) As1 0.0760(6) 0.0399(4) 0.0325(4) -0.0031(3) 0.0290(4) -0.0051(4) Sn1 0.0734(4) 0.0493(3) 0.0365(3) -0.0014(2) 0.0288(3) -0.0016(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.511(14) . ? C1 Sn1 2.136(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.513(14) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.507(18) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.360(11) . ? C5 C6 1.393(11) . ? C5 As1 1.906(8) . ? C6 C7 1.370(12) . ? C6 H6 0.9300 . ? C7 C8 1.364(13) . ? C7 H7 0.9300 . ? C8 O4 1.354(11) . ? C8 C9 1.388(14) . ? C9 C10 1.381(12) . ? C9 N1 1.443(16) . ? C10 H10 0.9300 . ? C11 C12 1.498(17) . ? C11 Sn1 2.113(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.510(18) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.510(19) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N1 O6 1.224(17) . ? N1 O5 1.279(16) . ? O1 As1 1.662(5) . ? O1 Sn1 2.146(5) . ? O2 As1 1.695(5) . ? O2 Sn1 2.020(6) 2_656 ? O3 As1 1.662(6) . ? O3 Sn1 2.177(5) 6_566 ? O4 H8A 0.89(2) . ? Sn1 O2 2.020(6) 2_656 ? Sn1 O3 2.177(5) 6_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 Sn1 120.4(6) . . ? C2 C1 H1A 107.2 . . ? Sn1 C1 H1A 107.2 . . ? C2 C1 H1B 107.2 . . ? Sn1 C1 H1B 107.2 . . ? H1A C1 H1B 106.9 . . ? C3 C2 C1 113.0(9) . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2B 109.0 . . ? C1 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 113.3(10) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 118.6(8) . . ? C10 C5 As1 120.0(6) . . ? C6 C5 As1 121.3(6) . . ? C7 C6 C5 120.9(8) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 120.9(9) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? O4 C8 C7 116.3(9) . . ? O4 C8 C9 125.6(10) . . ? C7 C8 C9 118.1(9) . . ? C10 C9 C8 121.3(9) . . ? C10 C9 N1 116.3(10) . . ? C8 C9 N1 122.4(11) . . ? C5 C10 C9 120.2(8) . . ? C5 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 Sn1 127.3(15) . . ? C12 C11 H11A 105.4 . . ? Sn1 C11 H11A 105.5 . . ? C12 C11 H11B 105.6 . . ? Sn1 C11 H11B 105.4 . . ? H11A C11 H11B 106.1 . . ? C13 C12 C11 103.4(16) . . ? C13 C12 H12A 111.1 . . ? C11 C12 H12A 111.1 . . ? C13 C12 H12B 111.1 . . ? C11 C12 H12B 111.1 . . ? H12A C12 H12B 109.1 . . ? C12 C13 C14 102(3) . . ? C12 C13 H13A 111.2 . . ? C14 C13 H13A 111.4 . . ? C12 C13 H13B 111.3 . . ? C14 C13 H13B 111.5 . . ? H13A C13 H13B 109.1 . . ? C13 C14 H14A 109.0 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.8 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O6 N1 O5 121.7(16) . . ? O6 N1 C9 121.6(15) . . ? O5 N1 C9 116.5(14) . . ? As1 O1 Sn1 132.3(3) . . ? As1 O2 Sn1 135.4(3) . 2_656 ? As1 O3 Sn1 134.5(3) . 6_566 ? C8 O4 H8A 86(8) . . ? O3 As1 O1 111.5(3) . . ? O3 As1 O2 108.0(3) . . ? O1 As1 O2 111.0(3) . . ? O3 As1 C5 111.4(3) . . ? O1 As1 C5 105.0(3) . . ? O2 As1 C5 109.9(3) . . ? O2 Sn1 C11 102.6(4) 2_656 . ? O2 Sn1 C1 123.0(3) 2_656 . ? C11 Sn1 C1 134.1(5) . . ? O2 Sn1 O1 87.7(2) 2_656 . ? C11 Sn1 O1 96.9(3) . . ? C1 Sn1 O1 90.4(3) . . ? O2 Sn1 O3 83.8(2) 2_656 6_565 ? C11 Sn1 O3 93.2(3) . 6_565 ? C1 Sn1 O3 87.3(3) . 6_565 ? O1 Sn1 O3 168.0(2) . 6_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.266 _refine_diff_density_min -0.978 _refine_diff_density_rms 0.129 #===END data_compound-4 _database_code_depnum_ccdc_archive 'CCDC 737804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 As N O8 S Sn' _chemical_formula_weight 649.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' As As 0.0500 2.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6540 1.4250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.393(6) _cell_length_b 10.437(5) _cell_length_c 14.206(6) _cell_angle_alpha 91.074(14) _cell_angle_beta 92.744(19) _cell_angle_gamma 107.485(18) _cell_volume 1326.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used Total _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.215 _exptl_crystal_size_mid 0.210 _exptl_crystal_size_min 0.186 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.644 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _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 13180 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6007 _reflns_number_gt 4175 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2\s(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^)+(0.0355P)^2^+0.6873P] 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 6007 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 C1 C 0.4257(6) 0.3262(5) 1.1296(3) 0.0451(12) Uani 1 1 d . . . H1A H 0.4447 0.4222 1.1240 0.054 Uiso 1 1 calc R . . H1B H 0.3186 0.2864 1.1327 0.054 Uiso 1 1 calc R . . C2 C 0.4985(7) 0.3032(6) 1.2205(4) 0.0628(16) Uani 1 1 d . . . H2A H 0.6061 0.3381 1.2168 0.075 Uiso 1 1 calc R . . H2B H 0.4737 0.2072 1.2292 0.075 Uiso 1 1 calc R . . C3 C 0.4530(9) 0.3682(8) 1.3055(4) 0.086(2) Uani 1 1 d . . . H3A H 0.4740 0.4636 1.2957 0.104 Uiso 1 1 calc R . . H3B H 0.3460 0.3305 1.3108 0.104 Uiso 1 1 calc R . . C4 C 0.5307(11) 0.3497(10) 1.3956(5) 0.141(4) Uani 1 1 d . . . H4A H 0.4969 0.3929 1.4465 0.211 Uiso 1 1 calc R . . H4B H 0.6366 0.3889 1.3917 0.211 Uiso 1 1 calc R . . H4C H 0.5087 0.2555 1.4067 0.211 Uiso 1 1 calc R . . C5 C 0.5662(6) 0.2629(5) 0.8660(3) 0.0469(13) Uani 1 1 d . . . H5A H 0.5673 0.3498 0.8425 0.056 Uiso 1 1 calc R . . H5B H 0.6685 0.2597 0.8689 0.056 Uiso 1 1 calc R . . C6 C 0.4777(7) 0.1580(6) 0.7972(4) 0.0646(17) Uani 1 1 d . . . H6A H 0.3742 0.1576 0.7966 0.077 Uiso 1 1 calc R . . H6B H 0.4814 0.0713 0.8186 0.077 Uiso 1 1 calc R . . C7 C 0.5273(9) 0.1737(7) 0.6992(4) 0.085(2) Uani 1 1 d . . . H7A H 0.5285 0.2625 0.6795 0.102 Uiso 1 1 calc R . . H7B H 0.6293 0.1701 0.6998 0.102 Uiso 1 1 calc R . . C8 C 0.4375(11) 0.0746(9) 0.6277(5) 0.142(4) Uani 1 1 d . . . H8A H 0.4801 0.0938 0.5675 0.213 Uiso 1 1 calc R . . H8B H 0.3369 0.0794 0.6239 0.213 Uiso 1 1 calc R . . H8C H 0.4371 -0.0140 0.6450 0.213 Uiso 1 1 calc R . . C9 C 0.8915(5) 0.5854(5) 1.1725(3) 0.0405(11) Uani 1 1 d . . . C10 C 1.0938(8) 0.5563(7) 1.2679(5) 0.081(2) Uani 1 1 d . . . H10 H 1.1771 0.5257 1.2736 0.097 Uiso 1 1 calc R . . C11 C 1.0161(7) 0.5434(6) 1.1805(4) 0.0676(17) Uani 1 1 d . . . H11 H 1.0484 0.5069 1.1284 0.081 Uiso 1 1 calc R . . C12 C 1.0521(8) 0.6119(8) 1.3453(5) 0.086(2) Uani 1 1 d . . . C13 C 0.9274(9) 0.6503(8) 1.3355(5) 0.095(3) Uani 1 1 d . . . H13 H 0.8941 0.6850 1.3880 0.114 Uiso 1 1 calc R . . C14 C 0.8475(7) 0.6399(7) 1.2498(4) 0.0746(19) Uani 1 1 d . . . H14 H 0.7639 0.6700 1.2449 0.089 Uiso 1 1 calc R . . C15 C 1.1433(9) 0.6310(10) 1.4395(5) 0.133(4) Uani 1 1 d . . . H15A H 1.2279 0.5986 1.4329 0.200 Uiso 1 1 calc R . . H15B H 1.0819 0.5817 1.4868 0.200 Uiso 1 1 calc R . . H15C H 1.1774 0.7248 1.4578 0.200 Uiso 1 1 calc R . . C16 C 0.8787(6) 0.0901(5) 1.1555(4) 0.0488(13) Uani 1 1 d . . . C17 C 0.8802(8) 0.1802(7) 1.2255(5) 0.086(2) Uani 1 1 d . . . H17 H 0.8245 0.2398 1.2185 0.103 Uiso 1 1 calc R . . C18 C 0.9668(10) 0.1822(9) 1.3084(6) 0.107(3) Uani 1 1 d . . . H18 H 0.9692 0.2431 1.3575 0.128 Uiso 1 1 calc R . . C19 C 1.0458(8) 0.0962(8) 1.3165(5) 0.082(2) Uani 1 1 d . . . C20 C 1.0506(9) 0.0095(8) 1.2456(6) 0.095(2) Uani 1 1 d . . . H20 H 1.1110 -0.0463 1.2521 0.113 Uiso 1 1 calc R . . C21 C 0.9643(8) 0.0054(7) 1.1634(5) 0.079(2) Uani 1 1 d . . . H21 H 0.9645 -0.0543 1.1140 0.095 Uiso 1 1 calc R . . As1 As 0.75264(5) 0.07563(4) 1.04432(4) 0.03873(15) Uani 1 1 d . . . N1 N 1.1330(9) 0.0974(11) 1.4071(6) 0.129(3) Uani 1 1 d . . . O1 O 0.7369(4) 0.4273(3) 1.0369(3) 0.0537(10) Uani 1 1 d . . . O2 O 0.6749(4) 0.6292(3) 1.0745(2) 0.0537(9) Uani 1 1 d . . . O3 O 0.9020(4) 0.6406(4) 0.9968(2) 0.0588(10) Uani 1 1 d . . . O4 O 0.6999(4) -0.0825(3) 1.0045(3) 0.0489(9) Uani 1 1 d . . . O5 O 0.6126(4) 0.1349(3) 1.0697(2) 0.0415(8) Uani 1 1 d . . . O6 O 0.8528(4) 0.1612(3) 0.9559(2) 0.0528(9) Uani 1 1 d . . . H6 H 0.8832 0.2416 0.9706 0.079 Uiso 1 1 calc R . . O7 O 1.2012(11) 0.0128(10) 1.4107(6) 0.194(4) Uani 1 1 d . . . O8 O 1.1384(9) 0.1815(12) 1.4661(5) 0.199(5) Uani 1 1 d . . . S1 S 0.79393(14) 0.57058(11) 1.06181(8) 0.0389(3) Uani 1 1 d . . . Sn1 Sn 0.49182(4) 0.25053(3) 1.00568(2) 0.03455(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.037(3) 0.053(3) -0.007(2) 0.000(2) 0.012(2) C2 0.075(4) 0.078(4) 0.045(3) -0.003(3) -0.004(3) 0.038(3) C3 0.096(6) 0.121(6) 0.053(4) -0.013(4) -0.007(4) 0.053(5) C4 0.175(10) 0.215(11) 0.056(5) -0.018(6) -0.017(6) 0.098(9) C5 0.044(3) 0.058(3) 0.041(3) 0.001(3) 0.003(2) 0.018(3) C6 0.075(4) 0.061(4) 0.049(3) -0.012(3) -0.001(3) 0.008(3) C7 0.104(6) 0.092(5) 0.047(4) -0.012(4) 0.008(4) 0.013(4) C8 0.192(11) 0.141(8) 0.057(5) -0.034(5) -0.011(6) 0.001(7) C9 0.033(3) 0.041(3) 0.044(3) 0.000(2) -0.006(2) 0.006(2) C10 0.064(5) 0.098(5) 0.081(5) 0.014(4) -0.015(4) 0.027(4) C11 0.054(4) 0.088(5) 0.062(4) -0.007(3) -0.009(3) 0.027(3) C12 0.061(5) 0.118(6) 0.056(4) 0.018(4) -0.014(4) -0.006(4) C13 0.085(6) 0.140(7) 0.051(4) -0.020(4) 0.000(4) 0.023(5) C14 0.068(5) 0.109(5) 0.052(4) -0.019(4) -0.007(3) 0.038(4) C15 0.096(7) 0.200(10) 0.063(5) 0.036(6) -0.033(4) -0.013(6) C16 0.036(3) 0.043(3) 0.067(4) -0.005(3) -0.006(3) 0.014(2) C17 0.085(5) 0.096(5) 0.087(5) -0.044(4) -0.036(4) 0.054(4) C18 0.113(7) 0.133(7) 0.087(6) -0.046(5) -0.027(5) 0.063(6) C19 0.068(5) 0.108(6) 0.070(4) -0.012(4) -0.022(4) 0.030(4) C20 0.089(6) 0.107(6) 0.108(6) -0.001(5) -0.027(5) 0.064(5) C21 0.080(5) 0.084(5) 0.084(5) -0.011(4) -0.020(4) 0.046(4) As1 0.0293(3) 0.0278(2) 0.0571(3) -0.0032(2) -0.0023(2) 0.0067(2) N1 0.097(6) 0.195(10) 0.097(6) -0.004(6) -0.035(5) 0.054(6) O1 0.042(2) 0.0420(19) 0.067(2) -0.0130(18) -0.0020(18) -0.0008(16) O2 0.053(2) 0.057(2) 0.058(2) 0.0078(19) -0.0035(18) 0.0272(19) O3 0.047(2) 0.058(2) 0.056(2) -0.0023(19) 0.0007(18) -0.0058(18) O4 0.0347(19) 0.0299(16) 0.078(2) -0.0078(17) -0.0035(17) 0.0051(14) O5 0.040(2) 0.0362(17) 0.055(2) 0.0065(16) 0.0060(16) 0.0201(15) O6 0.044(2) 0.0404(19) 0.069(2) 0.0014(18) 0.0080(18) 0.0035(16) O7 0.209(10) 0.234(9) 0.153(7) -0.009(6) -0.102(6) 0.105(8) O8 0.152(7) 0.376(14) 0.086(5) -0.085(7) -0.056(5) 0.120(8) S1 0.0351(7) 0.0344(6) 0.0427(7) -0.0035(6) -0.0026(5) 0.0044(5) Sn1 0.0341(2) 0.02792(16) 0.0414(2) -0.00326(14) -0.00140(14) 0.00981(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.489(7) . ? C1 Sn1 2.111(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.515(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.487(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.477(7) . ? C5 Sn1 2.128(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.487(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.471(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C14 1.365(8) . ? C9 C11 1.368(8) . ? C9 S1 1.761(5) . ? C10 C12 1.361(10) . ? C10 C11 1.394(8) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.350(11) . ? C12 C15 1.530(9) . ? C13 C14 1.384(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.352(8) . ? C16 C21 1.365(8) . ? C16 As1 1.903(5) . ? C17 C18 1.395(9) . ? C17 H17 0.9300 . ? C18 C19 1.328(10) . ? C18 H18 0.9300 . ? C19 C20 1.352(10) . ? C19 N1 1.490(10) . ? C20 C21 1.383(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? As1 O4 1.654(3) . ? As1 O5 1.664(3) . ? As1 O6 1.706(3) . ? N1 O8 1.189(11) . ? N1 O7 1.238(11) . ? O1 S1 1.459(3) . ? O1 Sn1 2.494(3) . ? O2 S1 1.443(4) . ? O2 Sn1 2.528(3) 2_667 ? O3 S1 1.445(3) . ? O4 Sn1 2.099(3) 2_657 ? O5 Sn1 2.082(3) . ? O6 H6 0.8200 . ? Sn1 O4 2.099(3) 2_657 ? Sn1 O2 2.528(3) 2_667 ? 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 Sn1 116.9(4) . . ? C2 C1 H1A 108.1 . . ? Sn1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? Sn1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C1 C2 C3 113.8(5) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C4 C3 C2 113.6(6) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 Sn1 116.3(4) . . ? C6 C5 H5A 108.2 . . ? Sn1 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? Sn1 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 115.1(5) . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C6 116.7(6) . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C11 119.3(5) . . ? C14 C9 S1 121.7(4) . . ? C11 C9 S1 119.0(4) . . ? C12 C10 C11 122.4(7) . . ? C12 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C9 C11 C10 118.9(6) . . ? C9 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C13 C12 C10 117.3(6) . . ? C13 C12 C15 121.2(8) . . ? C10 C12 C15 121.5(8) . . ? C12 C13 C14 122.1(7) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C9 C14 C13 120.0(7) . . ? C9 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 121.2(6) . . ? C17 C16 As1 120.5(4) . . ? C21 C16 As1 118.3(5) . . ? C16 C17 C18 118.9(7) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C19 C18 C17 119.4(7) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 122.4(7) . . ? C18 C19 N1 118.2(9) . . ? C20 C19 N1 119.4(8) . . ? C19 C20 C21 118.8(7) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C16 C21 C20 119.2(7) . . ? C16 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? O4 As1 O5 114.51(17) . . ? O4 As1 O6 103.60(17) . . ? O5 As1 O6 111.64(16) . . ? O4 As1 C16 108.5(2) . . ? O5 As1 C16 108.3(2) . . ? O6 As1 C16 110.1(2) . . ? O8 N1 O7 126.1(9) . . ? O8 N1 C19 118.9(10) . . ? O7 N1 C19 114.8(10) . . ? S1 O1 Sn1 138.9(2) . . ? S1 O2 Sn1 144.9(2) . 2_667 ? As1 O4 Sn1 139.5(2) . 2_657 ? As1 O5 Sn1 137.69(18) . . ? As1 O6 H6 109.5 . . ? O2 S1 O3 113.9(2) . . ? O2 S1 O1 112.0(2) . . ? O3 S1 O1 111.2(2) . . ? O2 S1 C9 106.1(2) . . ? O3 S1 C9 106.3(2) . . ? O1 S1 C9 106.7(2) . . ? O5 Sn1 O4 89.98(13) . 2_657 ? O5 Sn1 C1 97.74(16) . . ? O4 Sn1 C1 92.76(17) 2_657 . ? O5 Sn1 C5 102.10(17) . . ? O4 Sn1 C5 102.82(17) 2_657 . ? C1 Sn1 C5 154.6(2) . . ? O5 Sn1 O1 80.60(13) . . ? O4 Sn1 O1 170.26(12) 2_657 . ? C1 Sn1 O1 86.10(16) . . ? C5 Sn1 O1 81.76(16) . . ? O5 Sn1 O2 174.62(11) . 2_667 ? O4 Sn1 O2 84.67(13) 2_657 2_667 ? C1 Sn1 O2 83.13(16) . 2_667 ? C5 Sn1 O2 78.60(17) . 2_667 ? O1 Sn1 O2 104.77(13) . 2_667 ? 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 Sn1 C1 C2 C3 176.2(5) . . . . ? C1 C2 C3 C4 -177.6(7) . . . . ? Sn1 C5 C6 C7 176.7(5) . . . . ? C5 C6 C7 C8 -177.3(7) . . . . ? C14 C9 C11 C10 0.7(9) . . . . ? S1 C9 C11 C10 179.5(5) . . . . ? C12 C10 C11 C9 -1.5(10) . . . . ? C11 C10 C12 C13 2.5(11) . . . . ? C11 C10 C12 C15 -177.1(7) . . . . ? C10 C12 C13 C14 -2.8(12) . . . . ? C15 C12 C13 C14 176.8(7) . . . . ? C11 C9 C14 C13 -1.0(10) . . . . ? S1 C9 C14 C13 -179.7(5) . . . . ? C12 C13 C14 C9 2.1(12) . . . . ? C21 C16 C17 C18 -2.5(11) . . . . ? As1 C16 C17 C18 176.0(6) . . . . ? C16 C17 C18 C19 0.2(13) . . . . ? C17 C18 C19 C20 2.8(14) . . . . ? C17 C18 C19 N1 -177.9(8) . . . . ? C18 C19 C20 C21 -3.4(13) . . . . ? N1 C19 C20 C21 177.3(7) . . . . ? C17 C16 C21 C20 1.9(10) . . . . ? As1 C16 C21 C20 -176.6(6) . . . . ? C19 C20 C21 C16 1.0(12) . . . . ? C17 C16 As1 O4 -147.9(5) . . . . ? C21 C16 As1 O4 30.6(5) . . . . ? C17 C16 As1 O5 -23.1(6) . . . . ? C21 C16 As1 O5 155.4(5) . . . . ? C17 C16 As1 O6 99.3(5) . . . . ? C21 C16 As1 O6 -82.2(5) . . . . ? C18 C19 N1 O8 -5.7(14) . . . . ? C20 C19 N1 O8 173.6(10) . . . . ? C18 C19 N1 O7 178.4(10) . . . . ? C20 C19 N1 O7 -2.2(14) . . . . ? O5 As1 O4 Sn1 -13.2(4) . . . 2_657 ? O6 As1 O4 Sn1 -135.0(3) . . . 2_657 ? C16 As1 O4 Sn1 107.9(3) . . . 2_657 ? O4 As1 O5 Sn1 -98.4(3) . . . . ? O6 As1 O5 Sn1 18.9(3) . . . . ? C16 As1 O5 Sn1 140.4(3) . . . . ? Sn1 O2 S1 O3 34.8(5) 2_667 . . . ? Sn1 O2 S1 O1 -92.5(4) 2_667 . . . ? Sn1 O2 S1 C9 151.4(4) 2_667 . . . ? Sn1 O1 S1 O2 1.7(4) . . . . ? Sn1 O1 S1 O3 -127.0(3) . . . . ? Sn1 O1 S1 C9 117.5(3) . . . . ? C14 C9 S1 O2 1.9(5) . . . . ? C11 C9 S1 O2 -176.9(4) . . . . ? C14 C9 S1 O3 123.5(5) . . . . ? C11 C9 S1 O3 -55.3(5) . . . . ? C14 C9 S1 O1 -117.7(5) . . . . ? C11 C9 S1 O1 63.5(5) . . . . ? As1 O5 Sn1 O4 112.7(3) . . . 2_657 ? As1 O5 Sn1 C1 -154.5(3) . . . . ? As1 O5 Sn1 C5 9.6(3) . . . . ? As1 O5 Sn1 O1 -69.8(3) . . . . ? As1 O5 Sn1 O2 106.6(12) . . . 2_667 ? C2 C1 Sn1 O5 10.8(4) . . . . ? C2 C1 Sn1 O4 101.2(4) . . . 2_657 ? C2 C1 Sn1 C5 -130.5(5) . . . . ? C2 C1 Sn1 O1 -69.1(4) . . . . ? C2 C1 Sn1 O2 -174.5(4) . . . 2_667 ? C6 C5 Sn1 O5 91.4(4) . . . . ? C6 C5 Sn1 O4 -1.3(5) . . . 2_657 ? C6 C5 Sn1 C1 -127.9(5) . . . . ? C6 C5 Sn1 O1 169.9(4) . . . . ? C6 C5 Sn1 O2 -83.1(4) . . . 2_667 ? S1 O1 Sn1 O5 -145.6(3) . . . . ? S1 O1 Sn1 O4 -130.6(7) . . . 2_657 ? S1 O1 Sn1 C1 -47.1(3) . . . . ? S1 O1 Sn1 C5 110.6(4) . . . . ? S1 O1 Sn1 O2 34.8(3) . . . 2_667 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C11 H11 O3 0.93 2.48 3.393(8) 166.7 2_767 O6 H6 O3 0.82 2.05 2.641(5) 128.8 2_767 C21 H21 O6 0.93 2.54 3.288(8) 137.8 2_757 C13 H13 O8 0.93 2.56 3.471(11) 167.0 2_768 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.988 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.116 #===END data_compound-5 _database_code_depnum_ccdc_archive 'CCDC 737805' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H70 As2 N2 O11 Sn4' _chemical_formula_weight 1908.02 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.806(3) _cell_length_b 14.635(4) _cell_length_c 23.623(7) _cell_angle_alpha 80.774(11) _cell_angle_beta 88.419(10) _cell_angle_gamma 65.454(10) _cell_volume 3971.4(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used total _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 28.62 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.178 _exptl_crystal_size_mid 0.177 _exptl_crystal_size_min 0.084 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 2.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.696 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ; Higashi,T (1995) Program for absorption correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _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 38230 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 28.62 _reflns_number_total 17825 _reflns_number_gt 11214 _reflns_threshold_expression >2\s(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0619P)^2^+14.3942P] 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 17825 _refine_ls_number_parameters 740 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _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 0.5669(6) 0.2586(5) 0.9356(2) 0.059(2) Uani 1 1 d G . . C2 C 0.6484(6) 0.2246(5) 0.9807(3) 0.091(3) Uani 1 1 d G . . H2 H 0.7167 0.1672 0.9798 0.109 Uiso 1 1 calc R . . C3 C 0.6280(9) 0.2764(8) 1.0271(3) 0.118(5) Uani 1 1 d G . . H3 H 0.6825 0.2537 1.0573 0.142 Uiso 1 1 calc R . . C4 C 0.5260(10) 0.3623(8) 1.0285(4) 0.151(7) Uani 1 1 d G . . H4 H 0.5123 0.3970 1.0595 0.181 Uiso 1 1 calc R . . C5 C 0.4444(8) 0.3963(8) 0.9834(5) 0.250(15) Uani 1 1 d G . . H5 H 0.3762 0.4537 0.9843 0.300 Uiso 1 1 calc R . . C6 C 0.4649(6) 0.3444(7) 0.9370(4) 0.171(8) Uani 1 1 d G . . H6 H 0.4103 0.3672 0.9068 0.205 Uiso 1 1 calc R . . C7 C 0.7352(5) 0.1380(5) 0.8202(3) 0.064(2) Uani 1 1 d G . . C8 C 0.7685(7) 0.0483(5) 0.7978(3) 0.093(3) Uani 1 1 d G . . H8 H 0.7266 0.0091 0.8051 0.112 Uiso 1 1 calc R . . C9 C 0.8645(8) 0.0170(6) 0.7646(4) 0.131(5) Uani 1 1 d G . . H9 H 0.8868 -0.0430 0.7496 0.157 Uiso 1 1 calc R . . C10 C 0.9272(7) 0.0755(8) 0.7537(4) 0.152(7) Uani 1 1 d G . . H10 H 0.9915 0.0546 0.7315 0.183 Uiso 1 1 calc R . . C11 C 0.8939(7) 0.1653(7) 0.7761(5) 0.172(9) Uani 1 1 d G . . H11 H 0.9359 0.2044 0.7689 0.207 Uiso 1 1 calc R . . C12 C 0.7979(7) 0.1965(5) 0.8094(4) 0.096(4) Uani 1 1 d G . . H12 H 0.7757 0.2566 0.8244 0.115 Uiso 1 1 calc R . . C13 C 0.5108(7) 0.0737(5) 0.8703(3) 0.066(2) Uani 1 1 d G . . C14 C 0.4772(8) 0.0360(7) 0.9220(2) 0.131(6) Uani 1 1 d G . . H14 H 0.4858 0.0582 0.9556 0.158 Uiso 1 1 calc R . . C15 C 0.4308(9) -0.0350(7) 0.9236(3) 0.141(6) Uiso 1 1 d G . . H15 H 0.4084 -0.0602 0.9581 0.170 Uiso 1 1 calc R . . C16 C 0.4179(8) -0.0682(6) 0.8734(4) 0.133(6) Uani 1 1 d G . . H16 H 0.3869 -0.1157 0.8744 0.160 Uiso 1 1 calc R . . C17 C 0.4515(8) -0.0305(6) 0.8217(3) 0.097(4) Uani 1 1 d G . . H17 H 0.4429 -0.0528 0.7881 0.117 Uiso 1 1 calc R . . C18 C 0.4979(7) 0.0404(6) 0.8202(2) 0.083(3) Uani 1 1 d G . . H18 H 0.5203 0.0656 0.7856 0.100 Uiso 1 1 calc R . . C19 C 0.7673(4) 0.4480(4) 0.81698(16) 0.0422(16) Uani 1 1 d G . . C20 C 0.7205(3) 0.4432(4) 0.8706(2) 0.061(2) Uani 1 1 d G . . H20 H 0.6413 0.4741 0.8739 0.073 Uiso 1 1 calc R . . C21 C 0.7921(5) 0.3924(5) 0.91925(15) 0.075(3) Uani 1 1 d G . . H21 H 0.7608 0.3892 0.9551 0.090 Uiso 1 1 calc R . . C22 C 0.9104(5) 0.3464(5) 0.9143(2) 0.083(3) Uani 1 1 d G . . H22 H 0.9583 0.3124 0.9469 0.100 Uiso 1 1 calc R . . C23 C 0.9572(3) 0.3511(5) 0.8607(3) 0.077(3) Uani 1 1 d G . . H23 H 1.0364 0.3203 0.8574 0.092 Uiso 1 1 calc R . . C24 C 0.8857(4) 0.4020(4) 0.81204(19) 0.057(2) Uani 1 1 d G . . H24 H 0.9170 0.4051 0.7762 0.068 Uiso 1 1 calc R . . C25 C 0.6748(5) 0.4808(5) 0.66233(19) 0.054(2) Uani 1 1 d G . . C26 C 0.5824(5) 0.5320(5) 0.6228(2) 0.077(3) Uani 1 1 d G . . H26 H 0.5163 0.5844 0.6326 0.093 Uiso 1 1 calc R . . C27 C 0.5889(7) 0.5050(6) 0.5686(2) 0.098(4) Uani 1 1 d G . . H27 H 0.5271 0.5393 0.5422 0.117 Uiso 1 1 calc R . . C28 C 0.6877(8) 0.4267(7) 0.5539(2) 0.110(5) Uani 1 1 d G . . H28 H 0.6920 0.4086 0.5177 0.132 Uiso 1 1 calc R . . C29 C 0.7800(6) 0.3755(6) 0.5935(3) 0.106(4) Uani 1 1 d G . . H29 H 0.8461 0.3231 0.5836 0.127 Uiso 1 1 calc R . . C30 C 0.7736(4) 0.4025(5) 0.6477(3) 0.091(3) Uani 1 1 d G . . H30 H 0.8353 0.3682 0.6741 0.109 Uiso 1 1 calc R . . C31 C 0.5174(4) 0.6483(4) 0.7546(2) 0.0467(17) Uani 1 1 d G . . C32 C 0.4410(4) 0.6452(4) 0.7970(2) 0.054(2) Uani 1 1 d G . . H32 H 0.4563 0.5852 0.8224 0.065 Uiso 1 1 calc R . . C33 C 0.3416(4) 0.7318(5) 0.8014(3) 0.072(3) Uani 1 1 d G . . H33 H 0.2905 0.7298 0.8298 0.086 Uiso 1 1 calc R . . C34 C 0.3187(4) 0.8216(4) 0.7634(3) 0.086(3) Uani 1 1 d G . . H34 H 0.2523 0.8795 0.7664 0.103 Uiso 1 1 calc R . . C35 C 0.3952(6) 0.8246(4) 0.7210(3) 0.085(3) Uani 1 1 d G . . H35 H 0.3799 0.8846 0.6956 0.101 Uiso 1 1 calc R . . C36 C 0.4945(5) 0.7380(5) 0.7166(2) 0.067(2) Uani 1 1 d G . . H36 H 0.5457 0.7400 0.6882 0.080 Uiso 1 1 calc R . . C37 C 0.6095(4) 0.9357(4) 0.6234(3) 0.062(2) Uani 1 1 d G . . C38 C 0.5349(6) 0.9312(5) 0.5834(3) 0.087(3) Uani 1 1 d G . . H38 H 0.5626 0.8845 0.5582 0.105 Uiso 1 1 calc R . . C39 C 0.4189(6) 0.9965(6) 0.5811(3) 0.112(4) Uani 1 1 d G . . H39 H 0.3690 0.9935 0.5543 0.134 Uiso 1 1 calc R . . C40 C 0.3775(4) 1.0664(5) 0.6187(3) 0.089(3) Uani 1 1 d G . . H40 H 0.2998 1.1101 0.6171 0.107 Uiso 1 1 calc R . . C41 C 0.4521(6) 1.0709(4) 0.6587(3) 0.087(3) Uani 1 1 d G . . H41 H 0.4243 1.1176 0.6839 0.104 Uiso 1 1 calc R . . C42 C 0.5681(5) 1.0056(5) 0.6611(2) 0.073(3) Uani 1 1 d G . . H42 H 0.6180 1.0086 0.6878 0.088 Uiso 1 1 calc R . . C43 C 0.8188(5) 0.7498(4) 0.5626(2) 0.057(2) Uani 1 1 d G . . C44 C 0.8199(5) 0.6531(5) 0.5722(2) 0.071(3) Uani 1 1 d G . . H44 H 0.8015 0.6276 0.6078 0.085 Uiso 1 1 calc R . . C45 C 0.8486(6) 0.5947(4) 0.5285(3) 0.082(3) Uani 1 1 d G . . H45 H 0.8494 0.5301 0.5349 0.098 Uiso 1 1 calc R . . C46 C 0.8761(6) 0.6329(6) 0.4753(3) 0.089(3) Uani 1 1 d G . . H46 H 0.8953 0.5938 0.4460 0.106 Uiso 1 1 calc R . . C47 C 0.8749(6) 0.7296(6) 0.46570(19) 0.092(4) Uani 1 1 d G . . H47 H 0.8933 0.7551 0.4301 0.110 Uiso 1 1 calc R . . C48 C 0.8463(6) 0.7880(4) 0.5094(2) 0.080(3) Uani 1 1 d G . . H48 H 0.8455 0.8527 0.5030 0.097 Uiso 1 1 calc R . . C49 C 0.8936(5) 0.9259(4) 0.6156(3) 0.059(2) Uani 1 1 d G . . C50 C 0.9967(5) 0.8828(4) 0.6478(2) 0.065(2) Uani 1 1 d G . . H50 H 1.0151 0.8229 0.6738 0.078 Uiso 1 1 calc R . . C51 C 1.0725(5) 0.9291(6) 0.6411(3) 0.087(3) Uani 1 1 d G . . H51 H 1.1416 0.9003 0.6627 0.104 Uiso 1 1 calc R . . C52 C 1.0452(6) 1.0186(6) 0.6022(4) 0.103(4) Uani 1 1 d G . . H52 H 1.0959 1.0496 0.5977 0.123 Uiso 1 1 calc R . . C53 C 0.9420(7) 1.0617(5) 0.5700(3) 0.114(5) Uani 1 1 d G . . H53 H 0.9237 1.1215 0.5440 0.137 Uiso 1 1 calc R . . C54 C 0.8662(5) 1.0153(5) 0.5767(3) 0.091(4) Uani 1 1 d G . . H54 H 0.7971 1.0442 0.5551 0.110 Uiso 1 1 calc R . . C55 C 0.1834(4) 0.6176(4) 0.66480(18) 0.0489(18) Uani 1 1 d G . . C56 C 0.2654(4) 0.6572(4) 0.66202(19) 0.057(2) Uani 1 1 d G . . H56 H 0.3096 0.6485 0.6947 0.068 Uiso 1 1 calc R . . C57 C 0.2811(5) 0.7098(5) 0.6105(2) 0.073(3) Uani 1 1 d G . . H57 H 0.3360 0.7363 0.6086 0.088 Uiso 1 1 calc R . . C58 C 0.2150(5) 0.7227(5) 0.56168(19) 0.079(3) Uani 1 1 d G . . H58 H 0.2255 0.7579 0.5272 0.094 Uiso 1 1 calc R . . C59 C 0.1330(5) 0.6831(5) 0.56446(18) 0.084(3) Uani 1 1 d G . . H59 H 0.0887 0.6918 0.5318 0.101 Uiso 1 1 calc R . . C60 C 0.1172(4) 0.6305(5) 0.6160(2) 0.069(3) Uani 1 1 d G . . H60 H 0.0624 0.6040 0.6179 0.082 Uiso 1 1 calc R . . C61 C 0.1381(5) 0.6043(4) 0.81773(18) 0.0511(19) Uani 1 1 d G . . C62 C 0.1860(5) 0.5477(4) 0.8710(2) 0.076(3) Uani 1 1 d G . . H62 H 0.2293 0.4778 0.8746 0.091 Uiso 1 1 calc R . . C63 C 0.1693(6) 0.5956(5) 0.91887(18) 0.099(4) Uani 1 1 d G . . H63 H 0.2014 0.5577 0.9545 0.119 Uiso 1 1 calc R . . C64 C 0.1046(6) 0.7001(5) 0.9135(2) 0.089(3) Uani 1 1 d G . . H64 H 0.0934 0.7321 0.9455 0.107 Uiso 1 1 calc R . . C65 C 0.0567(5) 0.7567(4) 0.8602(3) 0.074(3) Uani 1 1 d G . . H65 H 0.0134 0.8266 0.8566 0.089 Uiso 1 1 calc R . . C66 C 0.0734(5) 0.7088(4) 0.8123(2) 0.057(2) Uani 1 1 d G . . H66 H 0.0414 0.7467 0.7767 0.068 Uiso 1 1 calc R . . C67 C 0.1546(5) 0.3913(5) 0.7400(3) 0.059(2) Uani 1 1 d G . . C68 C 0.0908(6) 0.3809(6) 0.6968(3) 0.093(4) Uani 1 1 d G . . H68 H 0.0466 0.4373 0.6701 0.111 Uiso 1 1 calc R . . C69 C 0.0933(7) 0.2860(8) 0.6935(4) 0.120(6) Uani 1 1 d G . . H69 H 0.0506 0.2790 0.6646 0.144 Uiso 1 1 calc R . . C70 C 0.1594(8) 0.2017(6) 0.7334(5) 0.152(8) Uani 1 1 d G . . H70 H 0.1611 0.1382 0.7311 0.183 Uiso 1 1 calc R . . C71 C 0.2232(7) 0.2122(5) 0.7766(5) 0.152(8) Uani 1 1 d G . . H71 H 0.2674 0.1557 0.8033 0.183 Uiso 1 1 calc R . . C72 C 0.2207(6) 0.3070(6) 0.7799(3) 0.108(4) Uani 1 1 d G . . H72 H 0.2634 0.3140 0.8088 0.129 Uiso 1 1 calc R . . C73 C 0.4824(4) 0.3432(4) 0.68650(16) 0.0411(16) Uani 1 1 d G . . C74 C 0.5885(3) 0.2698(4) 0.67514(18) 0.056(2) Uani 1 1 d G . . H74 H 0.6495 0.2456 0.7021 0.067 Uiso 1 1 calc R . . C75 C 0.6035(3) 0.2326(4) 0.6235(2) 0.063(2) Uani 1 1 d G . . H75 H 0.6745 0.1835 0.6159 0.076 Uiso 1 1 calc R . . C76 C 0.5124(4) 0.2688(4) 0.58330(17) 0.0507(18) Uani 1 1 d G . . C77 C 0.4062(4) 0.3421(4) 0.59467(18) 0.064(2) Uani 1 1 d G . . H77 H 0.3453 0.3663 0.5678 0.076 Uiso 1 1 calc R . . C78 C 0.3912(3) 0.3793(4) 0.6463(2) 0.060(2) Uani 1 1 d G . . H78 H 0.3202 0.4284 0.6539 0.072 Uiso 1 1 calc R . . C79 C 0.8184(5) 0.6758(4) 0.81614(17) 0.0490(18) Uani 1 1 d G . . C80 C 0.7282(6) 0.7637(5) 0.8281(2) 0.114(5) Uani 1 1 d G . . H80 H 0.6815 0.8119 0.7983 0.137 Uiso 1 1 calc R . . C81 C 0.7079(7) 0.7795(6) 0.8846(3) 0.162(8) Uani 1 1 d G . . H81 H 0.6476 0.8383 0.8926 0.194 Uiso 1 1 calc R . . C82 C 0.7778(7) 0.7073(6) 0.9291(2) 0.122(5) Uani 1 1 d GD . . C83 C 0.8679(6) 0.6194(5) 0.91717(19) 0.072(3) Uani 1 1 d G . . H83 H 0.9146 0.5712 0.9470 0.087 Uiso 1 1 calc R . . C84 C 0.8882(4) 0.6037(4) 0.8607(2) 0.060(2) Uani 1 1 d G . . H84 H 0.9485 0.5448 0.8527 0.072 Uiso 1 1 calc R . . O1 O 0.3394(4) 0.4737(4) 0.7625(2) 0.0511(13) Uani 1 1 d . . . O2 O 0.4719(4) 0.2845(4) 0.8072(2) 0.0558(14) Uani 1 1 d . . . O1W O 0.7339(18) 0.0117(15) 0.9442(7) 0.277(9) Uani 1 1 d . . . O3 O 0.5694(4) 0.4206(4) 0.7752(2) 0.0449(11) Uani 1 1 d . . . O4 O 0.8178(7) 0.7762(5) 0.7050(3) 0.091(2) Uani 1 1 d . . . O5 O 0.9761(4) 0.5915(6) 0.7293(3) 0.085(2) Uani 1 1 d . . . O6 O 0.7579(4) 0.6151(5) 0.7134(2) 0.0577(15) Uani 1 1 d . . . O7 O 0.4464(8) 0.2578(8) 0.4971(4) 0.137(4) Uani 1 1 d . . . O8 O 0.6131(7) 0.1692(7) 0.5216(3) 0.103(3) Uani 1 1 d . . . O9 O 0.676(2) 0.802(2) 0.9940(10) 0.319(11) Uiso 1 1 d . . . O10 O 0.8190(12) 0.6524(11) 1.0243(6) 0.174(5) Uiso 1 1 d . . . As1 As 0.46478(5) 0.38662(5) 0.75921(3) 0.03640(16) Uani 1 1 d . . . As2 As 0.84491(5) 0.65913(6) 0.73853(3) 0.03729(17) Uani 1 1 d . . . Sn1 Sn 0.65805(4) 0.52281(4) 0.74468(2) 0.04206(13) Uani 1 1 d . . . Sn2 Sn 0.15918(4) 0.53471(4) 0.74394(2) 0.04703(14) Uani 1 1 d . . . Sn3 Sn 0.78010(5) 0.84709(4) 0.62394(2) 0.05619(16) Uani 1 1 d . . . Sn4 Sn 0.58533(5) 0.18193(4) 0.86521(2) 0.05287(15) Uani 1 1 d . . . N1 N 0.5232(8) 0.2310(7) 0.5303(3) 0.070(2) Uani 1 1 d . . . N2 N 0.774(2) 0.7277(18) 0.9903(7) 0.199(7) Uiso 1 1 d 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 0.071(6) 0.065(5) 0.048(4) -0.010(4) -0.001(4) -0.033(5) C2 0.098(9) 0.105(9) 0.079(7) -0.011(6) -0.020(6) -0.052(7) C3 0.184(16) 0.159(14) 0.054(6) -0.022(7) -0.023(8) -0.110(13) C4 0.183(18) 0.197(19) 0.106(11) -0.095(12) 0.029(12) -0.089(15) C5 0.141(16) 0.28(3) 0.21(2) -0.18(2) -0.072(14) 0.087(16) C6 0.109(11) 0.183(16) 0.151(13) -0.121(12) -0.028(10) 0.042(11) C7 0.053(5) 0.058(5) 0.068(5) -0.012(4) 0.009(4) -0.010(4) C8 0.081(8) 0.086(8) 0.114(9) -0.038(7) 0.010(7) -0.028(6) C9 0.101(10) 0.137(13) 0.134(12) -0.074(10) 0.042(9) -0.014(9) C10 0.096(11) 0.175(17) 0.197(18) -0.075(14) 0.076(11) -0.056(12) C11 0.138(14) 0.153(15) 0.27(2) -0.115(16) 0.131(15) -0.086(13) C12 0.070(7) 0.084(8) 0.137(10) -0.041(7) 0.033(7) -0.030(6) C13 0.089(7) 0.060(5) 0.056(5) -0.012(4) 0.010(5) -0.040(5) C14 0.226(17) 0.151(13) 0.097(9) -0.050(9) 0.064(10) -0.149(13) C16 0.203(17) 0.119(11) 0.135(12) -0.029(10) 0.029(11) -0.121(12) C17 0.124(10) 0.087(8) 0.096(9) -0.028(7) -0.006(7) -0.052(8) C18 0.114(9) 0.083(7) 0.069(6) -0.026(5) -0.001(6) -0.052(7) C19 0.040(4) 0.051(4) 0.040(4) -0.014(3) 0.004(3) -0.020(3) C20 0.063(5) 0.091(7) 0.038(4) -0.017(4) 0.003(3) -0.040(5) C21 0.087(7) 0.104(8) 0.039(4) -0.004(5) -0.003(4) -0.047(6) C22 0.075(7) 0.099(8) 0.072(6) 0.017(6) -0.029(5) -0.041(6) C23 0.035(4) 0.092(7) 0.083(7) 0.012(6) -0.007(4) -0.015(5) C24 0.039(4) 0.071(6) 0.058(5) -0.011(4) 0.008(3) -0.021(4) C25 0.063(5) 0.077(6) 0.045(4) -0.024(4) 0.020(4) -0.046(5) C26 0.087(7) 0.093(7) 0.045(5) -0.011(5) -0.017(5) -0.031(6) C27 0.131(11) 0.124(10) 0.040(5) -0.014(6) -0.011(6) -0.055(9) C28 0.173(14) 0.140(12) 0.078(8) -0.061(8) 0.050(9) -0.111(12) C29 0.091(9) 0.141(12) 0.091(8) -0.066(8) 0.035(7) -0.040(8) C30 0.064(6) 0.111(9) 0.103(8) -0.061(7) 0.019(6) -0.029(6) C31 0.031(4) 0.056(5) 0.057(4) -0.019(4) -0.001(3) -0.018(3) C32 0.044(4) 0.069(5) 0.052(4) -0.024(4) 0.006(3) -0.021(4) C33 0.047(5) 0.098(8) 0.083(6) -0.058(6) 0.017(4) -0.028(5) C34 0.067(7) 0.062(6) 0.125(10) -0.040(6) -0.009(6) -0.015(5) C35 0.078(7) 0.047(5) 0.123(9) -0.017(6) -0.011(6) -0.018(5) C36 0.072(6) 0.074(6) 0.069(6) -0.018(5) 0.003(5) -0.043(5) C37 0.071(6) 0.055(5) 0.052(5) -0.008(4) 0.012(4) -0.021(4) C38 0.080(7) 0.097(8) 0.072(6) -0.033(6) -0.001(5) -0.017(6) C39 0.090(9) 0.146(12) 0.084(8) -0.015(8) -0.017(7) -0.034(9) C40 0.056(6) 0.096(8) 0.088(8) -0.022(6) -0.004(5) -0.001(6) C41 0.086(8) 0.064(6) 0.093(8) -0.015(6) 0.026(6) -0.016(6) C42 0.064(6) 0.066(6) 0.083(7) -0.018(5) 0.011(5) -0.018(5) C43 0.051(5) 0.064(5) 0.045(4) -0.012(4) 0.001(3) -0.011(4) C44 0.078(7) 0.083(7) 0.061(5) -0.018(5) 0.010(5) -0.041(6) C45 0.071(7) 0.086(7) 0.092(8) -0.038(6) 0.002(5) -0.028(6) C46 0.068(7) 0.113(10) 0.076(7) -0.049(7) 0.002(5) -0.018(6) C47 0.107(9) 0.104(9) 0.045(5) -0.021(6) 0.017(5) -0.022(7) C48 0.098(8) 0.077(7) 0.050(5) -0.010(5) 0.020(5) -0.021(6) C49 0.061(5) 0.046(5) 0.061(5) -0.011(4) 0.015(4) -0.015(4) C50 0.067(6) 0.055(5) 0.061(5) -0.005(4) -0.007(4) -0.014(4) C51 0.075(7) 0.080(7) 0.101(8) -0.022(6) -0.003(6) -0.026(6) C52 0.097(9) 0.088(9) 0.128(11) -0.019(8) 0.012(8) -0.044(8) C53 0.128(11) 0.093(9) 0.122(11) 0.031(8) -0.020(9) -0.061(9) C54 0.067(6) 0.058(6) 0.120(9) 0.026(6) -0.008(6) -0.011(5) C55 0.039(4) 0.054(5) 0.051(4) -0.020(4) 0.007(3) -0.012(3) C56 0.042(4) 0.068(5) 0.054(5) -0.014(4) 0.000(3) -0.016(4) C57 0.059(6) 0.082(7) 0.072(6) -0.009(5) 0.007(5) -0.025(5) C58 0.062(6) 0.091(7) 0.051(5) -0.003(5) 0.015(4) -0.004(5) C59 0.056(6) 0.124(9) 0.046(5) -0.015(5) -0.012(4) -0.012(6) C60 0.039(4) 0.101(7) 0.059(5) -0.024(5) -0.008(4) -0.018(5) C61 0.038(4) 0.075(6) 0.040(4) -0.021(4) 0.004(3) -0.019(4) C62 0.068(6) 0.081(7) 0.054(5) -0.021(5) -0.012(4) -0.002(5) C63 0.092(8) 0.111(9) 0.061(6) -0.027(6) -0.017(5) -0.004(7) C64 0.087(8) 0.125(10) 0.060(6) -0.050(6) 0.006(5) -0.038(7) C65 0.063(6) 0.080(7) 0.087(7) -0.048(6) 0.020(5) -0.025(5) C66 0.049(5) 0.062(5) 0.062(5) -0.013(4) -0.001(4) -0.023(4) C67 0.041(4) 0.067(6) 0.074(6) -0.028(5) 0.023(4) -0.023(4) C68 0.091(8) 0.130(10) 0.107(8) -0.082(8) 0.059(7) -0.076(8) C69 0.103(10) 0.173(15) 0.150(13) -0.113(12) 0.080(9) -0.097(11) C70 0.115(13) 0.114(12) 0.28(2) -0.107(14) 0.107(14) -0.076(11) C71 0.079(9) 0.088(9) 0.31(2) -0.039(12) 0.062(12) -0.054(8) C72 0.078(8) 0.095(9) 0.173(13) -0.027(9) 0.029(8) -0.058(7) C73 0.037(4) 0.050(4) 0.039(4) -0.010(3) 0.000(3) -0.020(3) C74 0.035(4) 0.074(6) 0.053(4) -0.023(4) -0.001(3) -0.013(4) C75 0.046(5) 0.075(6) 0.058(5) -0.022(4) -0.002(4) -0.011(4) C76 0.060(5) 0.056(5) 0.046(4) -0.022(4) 0.007(3) -0.030(4) C77 0.040(4) 0.084(6) 0.055(5) -0.023(4) -0.010(4) -0.009(4) C78 0.041(4) 0.078(6) 0.054(5) -0.028(4) -0.001(3) -0.011(4) C79 0.045(4) 0.061(5) 0.043(4) -0.015(4) 0.006(3) -0.022(4) C80 0.092(8) 0.112(9) 0.062(6) -0.035(6) 0.000(5) 0.040(7) C81 0.158(14) 0.167(14) 0.057(7) -0.044(8) 0.011(8) 0.041(11) C82 0.173(14) 0.144(12) 0.041(5) -0.046(7) 0.015(7) -0.049(11) C83 0.084(7) 0.093(7) 0.045(5) -0.010(5) 0.001(4) -0.043(6) C84 0.055(5) 0.075(6) 0.049(4) -0.003(4) -0.005(4) -0.027(4) O1 0.030(2) 0.056(3) 0.065(3) -0.019(3) -0.001(2) -0.012(2) O2 0.052(3) 0.060(3) 0.055(3) 0.007(3) -0.005(2) -0.028(3) O1W 0.32(2) 0.31(2) 0.162(13) -0.061(14) 0.010(13) -0.077(19) O3 0.030(2) 0.055(3) 0.052(3) -0.013(2) 0.001(2) -0.018(2) O4 0.161(7) 0.052(4) 0.051(4) -0.001(3) 0.000(4) -0.038(4) O5 0.026(3) 0.145(6) 0.080(4) -0.061(4) 0.003(3) -0.017(3) O6 0.048(3) 0.101(5) 0.045(3) -0.013(3) 0.006(2) -0.051(3) O7 0.110(7) 0.159(9) 0.091(6) -0.075(6) -0.039(5) 0.015(6) O8 0.090(6) 0.128(7) 0.075(5) -0.056(5) 0.007(4) -0.015(5) As1 0.0279(3) 0.0444(4) 0.0377(3) -0.0103(3) 0.0016(3) -0.0146(3) As2 0.0276(3) 0.0474(4) 0.0363(3) -0.0079(3) 0.0030(3) -0.0148(3) Sn1 0.0325(2) 0.0628(3) 0.0364(2) -0.0159(2) 0.00348(18) -0.0226(2) Sn2 0.0293(2) 0.0655(4) 0.0471(3) -0.0228(2) 0.00503(19) -0.0159(2) Sn3 0.0621(4) 0.0529(3) 0.0474(3) -0.0086(3) 0.0091(2) -0.0182(3) Sn4 0.0595(3) 0.0516(3) 0.0480(3) -0.0106(2) 0.0049(2) -0.0229(3) N1 0.069(5) 0.079(6) 0.054(4) -0.028(4) 0.004(4) -0.016(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.3900 . ? C1 C6 1.3900 . ? C1 Sn4 2.107(5) . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 H3 0.9300 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 Sn4 2.076(5) . ? C8 C9 1.3900 . ? C8 H8 0.9300 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 Sn4 2.151(5) . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C19 Sn1 2.082(3) . ? C20 C21 1.3900 . ? C20 H20 0.9300 . ? C21 C22 1.3900 . ? C21 H21 0.9300 . ? C22 C23 1.3900 . ? C22 H22 0.9300 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 Sn1 2.112(4) . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 H27 0.9300 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 Sn1 2.009(4) . ? C32 C33 1.3900 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 H33 0.9300 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C37 Sn3 2.024(5) . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 C40 1.3900 . ? C39 H39 0.9300 . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 C42 1.3900 . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C43 Sn3 2.099(4) . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C49 Sn3 2.187(5) . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 C52 1.3900 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 H52 0.9300 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C55 Sn2 2.148(4) . ? C56 C57 1.3900 . ? C56 H56 0.9300 . ? C57 C58 1.3900 . ? C57 H57 0.9300 . ? C58 C59 1.3900 . ? C58 H58 0.9300 . ? C59 C60 1.3900 . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C61 Sn2 2.113(4) . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 C65 1.3900 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? C67 C68 1.3900 . ? C67 C72 1.3900 . ? C67 Sn2 2.140(5) . ? C68 C69 1.3900 . ? C68 H68 0.9300 . ? C69 C70 1.3900 . ? C69 H69 0.9300 . ? C70 C71 1.3900 . ? C70 H70 0.9300 . ? C71 C72 1.3900 . ? C71 H71 0.9300 . ? C72 H72 0.9300 . ? C73 C74 1.3900 . ? C73 C78 1.3900 . ? C73 As1 1.901(3) . ? C74 C75 1.3900 . ? C74 H74 0.9300 . ? C75 C76 1.3900 . ? C75 H75 0.9300 . ? C76 C77 1.3900 . ? C76 N1 1.429(8) . ? C77 C78 1.3900 . ? C77 H77 0.9300 . ? C78 H78 0.9300 . ? C79 C80 1.3900 . ? C79 C84 1.3900 . ? C79 As2 1.891(4) . ? C80 C81 1.3900 . ? C80 H80 0.9300 . ? C81 C82 1.3900 . ? C81 H81 0.9300 . ? C82 C83 1.3900 . ? C82 N2 1.516(14) . ? C83 C84 1.3900 . ? C83 H83 0.9300 . ? C84 H84 0.9300 . ? O1 As1 1.591(5) . ? O1 Sn2 2.130(5) . ? O2 As1 1.696(5) . ? O2 Sn4 1.969(5) . ? O3 As1 1.681(5) . ? O3 Sn1 2.251(5) . ? O4 As2 1.664(6) . ? O4 Sn3 1.993(6) . ? O5 As2 1.587(5) . ? O5 Sn2 2.154(5) 1_655 ? O6 As2 1.663(5) . ? O6 Sn1 2.251(5) . ? O7 N1 1.166(10) . ? O8 N1 1.169(10) . ? O9 N2 1.29(3) . ? O10 N2 1.19(2) . ? Sn2 O5 2.154(5) 1_455 ? 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 C6 120.0 . . ? C2 C1 Sn4 123.2(4) . . ? C6 C1 Sn4 116.8(4) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 Sn4 116.8(4) . . ? C12 C7 Sn4 123.1(4) . . ? C7 C8 C9 120.0 . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 120.0 . . ? C14 C13 Sn4 121.9(4) . . ? C18 C13 Sn4 118.1(4) . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.0 . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 120.0 . . ? C20 C19 Sn1 119.2(3) . . ? C24 C19 Sn1 120.8(2) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 120.0 . . ? C26 C25 Sn1 118.2(3) . . ? C30 C25 Sn1 121.8(3) . . ? C27 C26 C25 120.0 . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 120.0 . . ? C32 C31 Sn1 121.0(3) . . ? C36 C31 Sn1 118.9(3) . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C38 C37 C42 120.0 . . ? C38 C37 Sn3 120.3(4) . . ? C42 C37 Sn3 119.6(4) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 Sn3 125.0(3) . . ? C48 C43 Sn3 115.0(3) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 Sn3 119.1(3) . . ? C54 C49 Sn3 120.8(3) . . ? C49 C50 C51 120.0 . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C52 C51 C50 120.0 . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? C56 C55 C60 120.0 . . ? C56 C55 Sn2 120.5(3) . . ? C60 C55 Sn2 119.5(3) . . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 120.0 . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C60 C59 C58 120.0 . . ? C60 C59 H59 120.0 . . ? C58 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 Sn2 121.4(3) . . ? C66 C61 Sn2 118.6(3) . . ? C63 C62 C61 120.0 . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C64 C63 C62 120.0 . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.0 . . ? C63 C64 H64 120.0 . . ? C65 C64 H64 120.0 . . ? C66 C65 C64 120.0 . . ? C66 C65 H65 120.0 . . ? C64 C65 H65 120.0 . . ? C65 C66 C61 120.0 . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C68 C67 C72 120.0 . . ? C68 C67 Sn2 120.9(4) . . ? C72 C67 Sn2 119.0(4) . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C71 C70 C69 120.0 . . ? C71 C70 H70 120.0 . . ? C69 C70 H70 120.0 . . ? C70 C71 C72 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C67 120.0 . . ? C71 C72 H72 120.0 . . ? C67 C72 H72 120.0 . . ? C74 C73 C78 120.0 . . ? C74 C73 As1 118.2(3) . . ? C78 C73 As1 121.8(3) . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C77 C76 C75 120.0 . . ? C77 C76 N1 118.1(5) . . ? C75 C76 N1 121.9(5) . . ? C78 C77 C76 120.0 . . ? C78 C77 H77 120.0 . . ? C76 C77 H77 120.0 . . ? C77 C78 C73 120.0 . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? C80 C79 C84 120.0 . . ? C80 C79 As2 118.5(3) . . ? C84 C79 As2 121.5(3) . . ? C81 C80 C79 120.0 . . ? C81 C80 H80 120.0 . . ? C79 C80 H80 120.0 . . ? C80 C81 C82 120.0 . . ? C80 C81 H81 120.0 . . ? C82 C81 H81 120.0 . . ? C83 C82 C81 120.0 . . ? C83 C82 N2 116.6(10) . . ? C81 C82 N2 122.5(10) . . ? C84 C83 C82 120.0 . . ? C84 C83 H83 120.0 . . ? C82 C83 H83 120.0 . . ? C83 C84 C79 120.0 . . ? C83 C84 H84 120.0 . . ? C79 C84 H84 120.0 . . ? As1 O1 Sn2 149.7(3) . . ? As1 O2 Sn4 136.4(3) . . ? As1 O3 Sn1 144.4(3) . . ? As2 O4 Sn3 134.9(4) . . ? As2 O5 Sn2 155.9(4) . 1_655 ? As2 O6 Sn1 140.1(3) . . ? O1 As1 O3 112.9(3) . . ? O1 As1 O2 106.2(3) . . ? O3 As1 O2 109.7(2) . . ? O1 As1 C73 110.2(2) . . ? O3 As1 C73 112.2(2) . . ? O2 As1 C73 105.1(3) . . ? O5 As2 O6 112.3(3) . . ? O5 As2 O4 106.2(4) . . ? O6 As2 O4 111.1(3) . . ? O5 As2 C79 111.8(3) . . ? O6 As2 C79 111.5(3) . . ? O4 As2 C79 103.5(3) . . ? C31 Sn1 C19 116.4(2) . . ? C31 Sn1 C25 115.7(2) . . ? C19 Sn1 C25 127.8(2) . . ? C31 Sn1 O6 92.0(2) . . ? C19 Sn1 O6 92.65(19) . . ? C25 Sn1 O6 86.9(2) . . ? C31 Sn1 O3 92.12(19) . . ? C19 Sn1 O3 85.53(19) . . ? C25 Sn1 O3 91.3(2) . . ? O6 Sn1 O3 175.9(2) . . ? C61 Sn2 O1 87.0(2) . . ? C61 Sn2 C67 126.3(2) . . ? O1 Sn2 C67 95.5(2) . . ? C61 Sn2 C55 116.8(2) . . ? O1 Sn2 C55 88.78(19) . . ? C67 Sn2 C55 116.8(2) . . ? C61 Sn2 O5 91.8(2) . 1_455 ? O1 Sn2 O5 176.9(2) . 1_455 ? C67 Sn2 O5 83.0(3) . 1_455 ? C55 Sn2 O5 94.3(2) . 1_455 ? O4 Sn3 C37 103.4(3) . . ? O4 Sn3 C43 114.6(2) . . ? C37 Sn3 C43 111.6(3) . . ? O4 Sn3 C49 100.7(3) . . ? C37 Sn3 C49 116.4(2) . . ? C43 Sn3 C49 109.6(2) . . ? O2 Sn4 C7 102.1(3) . . ? O2 Sn4 C1 103.7(3) . . ? C7 Sn4 C1 121.0(3) . . ? O2 Sn4 C13 95.3(3) . . ? C7 Sn4 C13 111.8(3) . . ? C1 Sn4 C13 117.4(3) . . ? O7 N1 O8 120.3(9) . . ? O7 N1 C76 122.7(8) . . ? O8 N1 C76 117.0(8) . . ? O10 N2 O9 127(2) . . ? O10 N2 C82 113.1(18) . . ? O9 N2 C82 106.1(19) . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.173 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.129 #===END