# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hidekazu Arii' _publ_contact_author_address ; ; _publ_contact_author_email kunio.mochida@gakushuin.ac.jp loop_ _publ_author_name H.Arii K.Mochida T.Kawashima # Attachment '- CIF.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 878354' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H19 Cl N2 O2 Sn' _chemical_formula_weight 473.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6310(13) _cell_length_b 6.7457(8) _cell_length_c 11.9584(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.5870(10) _cell_angle_gamma 90.00 _cell_volume 932.05(18) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 3348 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.687 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 1.531 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8029 _exptl_absorpt_correction_T_max 0.9004 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 5240 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.54 _reflns_number_total 3602 _reflns_number_gt 3412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(17) _refine_ls_number_reflns 3602 _refine_ls_number_parameters 236 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.030 _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 Sn1 Sn 0.260850(14) 0.14876(4) 0.776066(13) 0.01933(5) Uani 1 1 d . . . Cl1 Cl 0.29285(7) -0.16166(10) 0.67309(7) 0.02595(17) Uani 1 1 d . . . O1 O 0.42362(18) 0.4022(3) 0.50563(17) 0.0232(5) Uani 1 1 d . . . O2 O 0.02301(18) 0.3173(3) 0.48657(17) 0.0216(5) Uani 1 1 d . . . N1 N 0.3596(2) 0.3155(3) 0.6692(2) 0.0183(5) Uani 1 1 d . . . N2 N 0.1203(2) 0.2408(4) 0.6542(2) 0.0176(5) Uani 1 1 d . . . C1 C 0.2268(3) 0.3146(4) 0.4938(2) 0.0190(6) Uani 1 1 d . . . C2 C 0.2179(3) 0.3374(5) 0.3676(2) 0.0233(7) Uani 1 1 d . . . H2A H 0.1402 0.2987 0.3343 0.035 Uiso 1 1 calc R . . H2B H 0.2755 0.2523 0.3377 0.035 Uiso 1 1 calc R . . H2C H 0.2322 0.4759 0.3487 0.035 Uiso 1 1 calc R . . C3 C 0.3327(3) 0.3390(4) 0.5591(3) 0.0196(6) Uani 1 1 d . . . C4 C 0.4772(3) 0.3957(4) 0.7015(3) 0.0223(7) Uani 1 1 d . . . H4 H 0.4706 0.5353 0.7282 0.027 Uiso 1 1 calc R . . C5 C 0.5263(3) 0.3974(5) 0.5878(3) 0.0256(7) Uani 1 1 d . . . H5A H 0.5752 0.5159 0.5806 0.031 Uiso 1 1 calc R . . H5B H 0.5729 0.2770 0.5784 0.031 Uiso 1 1 calc R . . C6 C 0.5434(3) 0.2747(5) 0.7941(3) 0.0206(7) Uani 1 1 d . . . C7 C 0.5727(3) 0.3561(5) 0.9004(3) 0.0261(7) Uani 1 1 d . . . H7 H 0.5528 0.4896 0.9146 0.031 Uiso 1 1 calc R . . C8 C 0.6309(4) 0.2428(7) 0.9856(3) 0.0306(9) Uani 1 1 d . . . H8 H 0.6496 0.2986 1.0584 0.037 Uiso 1 1 calc R . . C9 C 0.6619(3) 0.0502(7) 0.9658(3) 0.0319(10) Uani 1 1 d . . . H9 H 0.7048 -0.0245 1.0236 0.038 Uiso 1 1 calc R . . C10 C 0.6306(3) -0.0341(5) 0.8617(3) 0.0278(7) Uani 1 1 d . . . H10 H 0.6497 -0.1684 0.8486 0.033 Uiso 1 1 calc R . . C11 C 0.5715(3) 0.0763(5) 0.7767(3) 0.0213(8) Uani 1 1 d . . . H11 H 0.5496 0.0169 0.7054 0.026 Uiso 1 1 calc R . . C12 C 0.1271(3) 0.2878(4) 0.5477(2) 0.0182(6) Uani 1 1 d . . . C13 C -0.0007(3) 0.2528(4) 0.6789(2) 0.0186(6) Uani 1 1 d . . . H13 H -0.0250 0.1214 0.7069 0.022 Uiso 1 1 calc R . . C14 C -0.0664(3) 0.2932(4) 0.5607(2) 0.0200(6) Uani 1 1 d . . . H14A H -0.1176 0.1805 0.5360 0.024 Uiso 1 1 calc R . . H14B H -0.1139 0.4148 0.5615 0.024 Uiso 1 1 calc R . . C15 C -0.0198(2) 0.4127(4) 0.7650(2) 0.0185(6) Uani 1 1 d . . . C16 C -0.1152(3) 0.4014(5) 0.8262(3) 0.0228(7) Uani 1 1 d . . . H16 H -0.1671 0.2926 0.8152 0.027 Uiso 1 1 calc R . . C17 C -0.1340(3) 0.5479(5) 0.9026(3) 0.0242(7) Uani 1 1 d . . . H17 H -0.1994 0.5396 0.9433 0.029 Uiso 1 1 calc R . . C18 C -0.0590(3) 0.7065(4) 0.9207(2) 0.0246(7) Uani 1 1 d . . . H18 H -0.0725 0.8069 0.9734 0.030 Uiso 1 1 calc R . . C19 C 0.0358(3) 0.7174(5) 0.8612(3) 0.0261(7) Uani 1 1 d . . . H19 H 0.0885 0.8247 0.8742 0.031 Uiso 1 1 calc R . . C20 C 0.0548(3) 0.5729(4) 0.7825(3) 0.0222(7) Uani 1 1 d . . . H20 H 0.1191 0.5839 0.7406 0.027 Uiso 1 1 calc R . . 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 Sn1 0.01854(9) 0.02271(9) 0.01607(9) 0.00232(12) -0.00092(6) 0.00166(11) Cl1 0.0235(4) 0.0175(3) 0.0362(4) 0.0011(3) 0.0004(3) 0.0011(3) O1 0.0180(11) 0.0259(11) 0.0252(12) 0.0078(9) 0.0012(9) -0.0012(9) O2 0.0179(11) 0.0258(11) 0.0198(11) 0.0019(9) -0.0037(8) -0.0021(8) N1 0.0159(13) 0.0172(12) 0.0204(13) 0.0009(10) -0.0036(10) 0.0001(9) N2 0.0162(13) 0.0197(12) 0.0169(13) -0.0001(10) 0.0020(10) 0.0019(10) C1 0.0217(16) 0.0157(14) 0.0190(15) 0.0014(12) 0.0000(12) 0.0003(11) C2 0.0172(16) 0.0284(16) 0.0234(16) 0.0016(13) -0.0009(12) 0.0021(13) C3 0.0201(16) 0.0122(13) 0.0264(16) 0.0020(12) 0.0021(12) 0.0031(11) C4 0.0194(16) 0.0145(14) 0.0316(18) -0.0013(12) -0.0028(13) -0.0014(11) C5 0.0201(16) 0.0266(17) 0.0288(17) 0.0085(13) -0.0023(13) -0.0058(13) C6 0.0107(16) 0.0225(17) 0.0282(19) -0.0008(14) 0.0004(13) -0.0014(12) C7 0.0231(18) 0.0277(17) 0.0274(18) -0.0060(14) 0.0028(14) -0.0068(14) C8 0.029(2) 0.049(2) 0.0141(18) -0.0028(16) 0.0019(15) -0.0104(18) C9 0.024(2) 0.045(2) 0.027(2) 0.0161(18) 0.0001(16) 0.0003(17) C10 0.0267(19) 0.0271(17) 0.0295(19) 0.0047(14) 0.0034(14) 0.0031(14) C11 0.0201(18) 0.0247(16) 0.0185(16) -0.0015(12) 0.0000(13) 0.0022(12) C12 0.0195(16) 0.0129(13) 0.0207(15) -0.0037(11) -0.0041(12) -0.0002(11) C13 0.0179(15) 0.0157(14) 0.0213(16) 0.0030(11) -0.0009(12) -0.0003(11) C14 0.0186(16) 0.0207(14) 0.0203(16) -0.0021(12) 0.0006(12) -0.0008(12) C15 0.0155(15) 0.0219(15) 0.0174(15) 0.0022(11) -0.0015(11) -0.0008(11) C16 0.0168(15) 0.0268(16) 0.0238(16) 0.0025(13) -0.0017(12) -0.0030(12) C17 0.0200(17) 0.0354(18) 0.0176(16) 0.0025(13) 0.0039(12) 0.0029(13) C18 0.0248(18) 0.0307(19) 0.0175(15) -0.0049(11) -0.0012(13) 0.0060(12) C19 0.0240(18) 0.0249(15) 0.0286(18) -0.0032(12) -0.0004(14) -0.0043(12) C20 0.0195(16) 0.0250(14) 0.0225(16) 0.0008(12) 0.0044(13) -0.0019(12) _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 Sn1 N1 2.134(3) . ? Sn1 N2 2.153(2) . ? Sn1 Cl1 2.4789(8) . ? O1 C3 1.366(4) . ? O1 C5 1.457(4) . ? O2 C12 1.355(3) . ? O2 C14 1.450(4) . ? N1 C3 1.328(4) . ? N1 C4 1.480(4) . ? N2 C12 1.323(4) . ? N2 C13 1.473(4) . ? C1 C3 1.390(4) . ? C1 C12 1.402(4) . ? C1 C2 1.509(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C6 1.514(5) . ? C4 C5 1.535(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.390(5) . ? C6 C11 1.399(5) . ? C7 C8 1.387(5) . ? C7 H7 0.9500 . ? C8 C9 1.376(5) . ? C8 H8 0.9500 . ? C9 C10 1.379(5) . ? C9 H9 0.9500 . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C15 1.525(4) . ? C13 C14 1.553(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.386(4) . ? C15 C16 1.400(4) . ? C16 C17 1.380(4) . ? C16 H16 0.9500 . ? C17 C18 1.382(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(5) . ? C18 H18 0.9500 . ? C19 C20 1.390(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N2 82.05(9) . . ? N1 Sn1 Cl1 91.48(7) . . ? N2 Sn1 Cl1 93.02(7) . . ? C3 O1 C5 107.3(2) . . ? C12 O2 C14 108.2(2) . . ? C3 N1 C4 108.7(2) . . ? C3 N1 Sn1 125.1(2) . . ? C4 N1 Sn1 125.53(18) . . ? C12 N2 C13 110.1(2) . . ? C12 N2 Sn1 126.6(2) . . ? C13 N2 Sn1 123.25(18) . . ? C3 C1 C12 118.9(3) . . ? C3 C1 C2 120.3(3) . . ? C12 C1 C2 120.5(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 113.2(3) . . ? N1 C3 C1 129.5(3) . . ? O1 C3 C1 117.2(3) . . ? N1 C4 C6 111.8(3) . . ? N1 C4 C5 101.4(2) . . ? C6 C4 C5 116.3(3) . . ? N1 C4 H4 109.0 . . ? C6 C4 H4 109.0 . . ? C5 C4 H4 109.0 . . ? O1 C5 C4 103.7(2) . . ? O1 C5 H5A 111.0 . . ? C4 C5 H5A 111.0 . . ? O1 C5 H5B 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C11 118.5(4) . . ? C7 C6 C4 120.4(3) . . ? C11 C6 C4 121.0(3) . . ? C8 C7 C6 120.1(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 119.9(4) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.0(3) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C6 120.8(4) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? N2 C12 O2 114.0(3) . . ? N2 C12 C1 128.1(3) . . ? O2 C12 C1 117.9(3) . . ? N2 C13 C15 113.0(2) . . ? N2 C13 C14 102.0(2) . . ? C15 C13 C14 113.3(2) . . ? N2 C13 H13 109.4 . . ? C15 C13 H13 109.4 . . ? C14 C13 H13 109.4 . . ? O2 C14 C13 105.3(2) . . ? O2 C14 H14A 110.7 . . ? C13 C14 H14A 110.7 . . ? O2 C14 H14B 110.7 . . ? C13 C14 H14B 110.7 . . ? H14A C14 H14B 108.8 . . ? C20 C15 C16 118.9(3) . . ? C20 C15 C13 121.1(3) . . ? C16 C15 C13 120.0(3) . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 119.2(3) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 120.7(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C15 C20 C19 120.2(3) . . ? C15 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.569 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.068 #===END data_compound2 _database_code_depnum_ccdc_archive 'CCDC 878355' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H27 F6 N2 O3 Sb Sn' _chemical_formula_weight 745.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.1820(14) _cell_length_b 15.1820(14) _cell_length_c 23.151(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5336.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 _exptl_absorpt_coefficient_mu 2.019 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6882 _exptl_absorpt_correction_T_max 0.7516 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 59287 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6137 _reflns_number_gt 6071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0200P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 6137 _refine_ls_number_parameters 337 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1344 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.079 _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 Sn1 Sn 0.66738(5) 0.24199(4) 0.09527(3) 0.04208(18) Uani 1 1 d . . . O1 O 0.7340(5) 0.5059(4) 0.1508(3) 0.0417(16) Uani 1 1 d . . . O2 O 0.4492(5) 0.3883(4) 0.1682(3) 0.0411(16) Uani 1 1 d . . . O3 O 0.6059(5) 0.2999(5) 0.0122(3) 0.0487(17) Uani 1 1 d U . . N1 N 0.7186(5) 0.3667(5) 0.1185(3) 0.0334(16) Uani 1 1 d . . . H1 H 0.7073 0.3877 0.0815 0.040 Uiso 1 1 calc R . . N2 N 0.5529(6) 0.2928(5) 0.1369(4) 0.0364(18) Uani 1 1 d . . . C1 C 0.5924(7) 0.4477(6) 0.1595(4) 0.037(2) Uani 1 1 d . . . C2 C 0.5593(7) 0.5352(6) 0.1815(4) 0.041(2) Uani 1 1 d . . . H2A H 0.5941 0.5532 0.2151 0.061 Uiso 1 1 calc R . . H2B H 0.4973 0.5298 0.1925 0.061 Uiso 1 1 calc R . . H2C H 0.5652 0.5796 0.1510 0.061 Uiso 1 1 calc R . . C3 C 0.6779(7) 0.4373(5) 0.1414(4) 0.036(2) Uani 1 1 d . . . C4 C 0.8149(6) 0.3865(5) 0.1112(5) 0.038(2) Uani 1 1 d . . . H4 H 0.8478 0.3606 0.1445 0.046 Uiso 1 1 calc R . . C5 C 0.8134(7) 0.4863(6) 0.1181(5) 0.044(3) Uani 1 1 d . . . H5A H 0.8663 0.5068 0.1392 0.052 Uiso 1 1 calc R . . H5B H 0.8117 0.5155 0.0799 0.052 Uiso 1 1 calc R . . C6 C 0.8541(6) 0.3502(6) 0.0551(5) 0.045(2) Uani 1 1 d U . . C7 C 0.9178(7) 0.2861(6) 0.0576(6) 0.051(2) Uani 1 1 d U . . H7 H 0.9378 0.2638 0.0936 0.061 Uiso 1 1 calc R . . C8 C 0.9524(8) 0.2547(7) 0.0056(7) 0.061(3) Uani 1 1 d U . . H8 H 0.9985 0.2124 0.0056 0.073 Uiso 1 1 calc R . . C9 C 0.9185(8) 0.2861(7) -0.0459(7) 0.062(3) Uani 1 1 d U . . H9 H 0.9429 0.2650 -0.0811 0.075 Uiso 1 1 calc R . . C10 C 0.8540(7) 0.3440(8) -0.0485(6) 0.057(2) Uani 1 1 d U . . H10 H 0.8321 0.3632 -0.0848 0.068 Uiso 1 1 calc R . . C11 C 0.8179(6) 0.3769(7) 0.0029(5) 0.046(2) Uani 1 1 d U . . H11 H 0.7696 0.4167 0.0021 0.055 Uiso 1 1 calc R . . C12 C 0.5354(7) 0.3757(5) 0.1544(4) 0.0352(19) Uani 1 1 d . . . C13 C 0.4706(7) 0.2427(7) 0.1360(4) 0.040(2) Uani 1 1 d . . . H13 H 0.4505 0.2362 0.0951 0.047 Uiso 1 1 calc R . . C14 C 0.4056(7) 0.3033(6) 0.1683(5) 0.049(3) Uani 1 1 d . . . H14A H 0.3483 0.3064 0.1480 0.058 Uiso 1 1 calc R . . H14B H 0.3956 0.2823 0.2083 0.058 Uiso 1 1 calc R . . C15 C 0.4774(6) 0.1524(5) 0.1632(4) 0.0297(17) Uani 1 1 d . . . C16 C 0.4415(6) 0.0789(6) 0.1366(4) 0.036(2) Uani 1 1 d . . . H16 H 0.4158 0.0835 0.0994 0.043 Uiso 1 1 calc R . . C17 C 0.4437(6) -0.0022(6) 0.1654(6) 0.048(3) Uani 1 1 d . . . H17 H 0.4181 -0.0526 0.1478 0.058 Uiso 1 1 calc R . . C18 C 0.4817(6) -0.0098(6) 0.2180(5) 0.041(2) Uani 1 1 d . . . H18 H 0.4815 -0.0650 0.2373 0.049 Uiso 1 1 calc R . . C19 C 0.5207(7) 0.0620(6) 0.2438(4) 0.042(2) Uani 1 1 d . . . H19 H 0.5491 0.0556 0.2801 0.050 Uiso 1 1 calc R . . C20 C 0.5185(6) 0.1437(6) 0.2168(4) 0.0341(19) Uani 1 1 d . . . H20 H 0.5449 0.1934 0.2348 0.041 Uiso 1 1 calc R . . C21 C 0.6186(9) 0.2573(11) -0.0431(5) 0.071(3) Uani 1 1 d U . . H21A H 0.6813 0.2601 -0.0548 0.085 Uiso 1 1 calc R . . H21B H 0.6006 0.1947 -0.0411 0.085 Uiso 1 1 calc R . . C22 C 0.5672(11) 0.3021(11) -0.0811(6) 0.085(3) Uani 1 1 d U . . H22A H 0.5085 0.2742 -0.0838 0.102 Uiso 1 1 calc R . . H22B H 0.5945 0.3015 -0.1199 0.102 Uiso 1 1 calc R . . C23 C 0.5584(10) 0.3972(10) -0.0593(5) 0.071(3) Uani 1 1 d U . . H23A H 0.6095 0.4336 -0.0709 0.086 Uiso 1 1 calc R . . H23B H 0.5035 0.4251 -0.0734 0.086 Uiso 1 1 calc R . . C24 C 0.5559(8) 0.3829(8) 0.0057(5) 0.051(2) Uani 1 1 d U . . H24A H 0.5848 0.4319 0.0265 0.061 Uiso 1 1 calc R . . H24B H 0.4947 0.3765 0.0198 0.061 Uiso 1 1 calc R . . F1 F 0.5953(5) 0.7463(6) 0.0379(4) 0.078(2) Uani 1 1 d . . . F2 F 0.6411(6) 0.5771(6) 0.0476(3) 0.084(3) Uani 1 1 d . . . F3 F 0.7614(5) 0.7019(5) 0.0486(5) 0.102(3) Uani 1 1 d . . . F4 F 0.3327(6) 0.3327(6) 0.0000 0.177(10) Uani 1 2 d S . . F5 F 0.3232(9) 0.1703(7) 0.0302(8) 0.207(9) Uani 1 1 d . . . F6 F 0.2114(16) 0.2806(13) 0.0695(6) 0.261(11) Uani 1 1 d . . . F7 F 0.1597(5) 0.1597(5) 0.0000 0.113(5) Uani 1 2 d S . . Sb1 Sb 0.66980(4) 0.66980(4) 0.0000 0.02907(17) Uani 1 2 d S . . Sb2 Sb 0.24808(5) 0.24808(5) 0.0000 0.0404(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0424(4) 0.0163(3) 0.0675(4) -0.0021(3) 0.0211(3) -0.0045(3) O1 0.054(4) 0.027(3) 0.045(4) -0.006(3) -0.018(3) -0.001(3) O2 0.053(4) 0.023(3) 0.047(4) 0.003(3) 0.016(3) 0.013(3) O3 0.037(3) 0.063(4) 0.047(4) -0.025(3) 0.006(3) -0.001(3) N1 0.036(4) 0.028(4) 0.036(4) 0.003(3) 0.002(3) -0.003(3) N2 0.044(5) 0.020(3) 0.045(5) 0.001(3) 0.011(4) 0.001(3) C1 0.059(6) 0.031(4) 0.022(4) 0.003(3) 0.003(4) 0.006(4) C2 0.062(7) 0.029(5) 0.031(4) -0.001(4) 0.010(4) 0.001(4) C3 0.064(6) 0.019(4) 0.025(4) 0.007(3) 0.002(4) 0.003(4) C4 0.031(5) 0.018(4) 0.066(6) 0.015(4) -0.023(4) -0.004(3) C5 0.043(6) 0.029(4) 0.059(6) 0.010(4) -0.030(5) -0.014(4) C6 0.032(4) 0.031(4) 0.071(5) -0.003(4) 0.001(4) -0.015(3) C7 0.035(4) 0.028(4) 0.090(6) 0.002(4) 0.008(5) -0.008(4) C8 0.050(5) 0.027(4) 0.106(7) -0.001(5) 0.027(5) -0.010(4) C9 0.056(5) 0.038(5) 0.093(6) -0.013(5) 0.031(5) -0.029(4) C10 0.033(4) 0.058(5) 0.080(6) 0.001(5) 0.000(4) -0.025(4) C11 0.027(4) 0.042(4) 0.068(5) 0.000(4) -0.001(4) -0.011(3) C12 0.055(6) 0.015(4) 0.036(4) 0.003(3) 0.014(4) 0.006(3) C13 0.045(5) 0.031(5) 0.042(5) 0.004(4) 0.017(4) 0.000(4) C14 0.048(6) 0.032(5) 0.066(7) 0.005(5) 0.032(5) 0.006(4) C15 0.035(4) 0.020(4) 0.034(4) -0.005(3) 0.002(3) -0.004(3) C16 0.028(4) 0.039(5) 0.040(5) -0.013(4) -0.013(4) 0.012(4) C17 0.034(5) 0.023(4) 0.088(9) -0.011(5) -0.007(5) -0.001(4) C18 0.038(5) 0.024(4) 0.060(6) 0.008(4) 0.003(5) 0.006(4) C19 0.058(6) 0.038(5) 0.030(5) 0.006(4) 0.003(4) 0.007(4) C20 0.039(5) 0.029(4) 0.034(4) -0.001(4) -0.006(4) -0.006(4) C21 0.062(6) 0.092(7) 0.058(5) -0.037(5) -0.001(5) 0.015(5) C22 0.083(7) 0.113(8) 0.060(6) -0.031(6) -0.005(5) 0.011(6) C23 0.083(6) 0.087(7) 0.044(5) -0.009(5) 0.002(5) -0.015(6) C24 0.050(5) 0.062(5) 0.041(5) -0.017(4) 0.000(4) -0.007(4) F1 0.050(4) 0.080(5) 0.102(6) -0.036(5) 0.001(4) 0.017(4) F2 0.087(6) 0.092(6) 0.073(5) 0.058(5) -0.004(4) -0.016(5) F3 0.061(5) 0.082(6) 0.163(9) -0.045(6) -0.065(6) 0.006(4) F4 0.061(5) 0.061(5) 0.41(3) 0.049(11) -0.049(11) -0.027(7) F5 0.157(11) 0.071(6) 0.39(2) 0.060(11) -0.179(14) 0.007(8) F6 0.42(3) 0.26(2) 0.098(9) -0.088(11) 0.099(14) -0.033(19) F7 0.049(4) 0.049(4) 0.240(17) -0.004(7) 0.004(7) 0.000(5) Sb1 0.0281(2) 0.0281(2) 0.0310(3) 0.0038(2) -0.0038(2) -0.0035(3) Sb2 0.0417(3) 0.0417(3) 0.0379(4) 0.0072(3) -0.0072(3) 0.0038(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 N1 2.116(8) . ? Sn1 N2 2.131(8) . ? Sn1 O3 2.312(8) . ? O1 C3 1.363(11) . ? O1 C5 1.454(13) . ? O2 C12 1.360(12) . ? O2 C14 1.450(11) . ? O3 C21 1.446(12) . ? O3 C24 1.478(14) . ? N1 C3 1.346(11) . ? N1 C4 1.504(12) . ? N1 H1 0.9300 . ? N2 C12 1.348(10) . ? N2 C13 1.464(12) . ? C1 C3 1.373(15) . ? C1 C12 1.400(14) . ? C1 C2 1.509(12) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C5 1.524(12) . ? C4 C6 1.532(15) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.373(15) . ? C6 C11 1.386(16) . ? C7 C8 1.397(18) . ? C7 H7 0.9500 . ? C8 C9 1.38(2) . ? C8 H8 0.9500 . ? C9 C10 1.317(18) . ? C9 H9 0.9500 . ? C10 C11 1.403(16) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C15 1.513(12) . ? C13 C14 1.543(13) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.386(12) . ? C15 C20 1.396(12) . ? C16 C17 1.401(14) . ? C16 H16 0.9500 . ? C17 C18 1.352(15) . ? C17 H17 0.9500 . ? C18 C19 1.376(14) . ? C18 H18 0.9500 . ? C19 C20 1.389(13) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.36(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.54(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.521(16) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? F1 Sb1 1.844(7) . ? F2 Sb1 1.841(6) . ? F3 Sb1 1.854(7) . ? F4 Sb2 1.818(12) . ? F5 Sb2 1.784(9) . ? F6 Sb2 1.772(11) . ? F7 Sb2 1.898(11) . ? Sb1 F2 1.841(6) 7 ? Sb1 F1 1.844(7) 7 ? Sb1 F3 1.854(7) 7 ? Sb2 F6 1.772(11) 7 ? Sb2 F5 1.784(9) 7 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N2 82.0(3) . . ? N1 Sn1 O3 91.1(3) . . ? N2 Sn1 O3 84.8(3) . . ? C3 O1 C5 106.2(7) . . ? C12 O2 C14 108.3(7) . . ? C21 O3 C24 111.1(9) . . ? C21 O3 Sn1 120.8(7) . . ? C24 O3 Sn1 128.0(6) . . ? C3 N1 C4 109.3(8) . . ? C3 N1 Sn1 130.1(7) . . ? C4 N1 Sn1 120.5(5) . . ? C3 N1 H1 90.3 . . ? C4 N1 H1 90.3 . . ? Sn1 N1 H1 90.3 . . ? C12 N2 C13 108.7(8) . . ? C12 N2 Sn1 129.4(7) . . ? C13 N2 Sn1 120.1(6) . . ? C3 C1 C12 118.0(8) . . ? C3 C1 C2 121.2(9) . . ? C12 C1 C2 120.7(9) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 112.6(9) . . ? N1 C3 C1 130.2(9) . . ? O1 C3 C1 117.0(8) . . ? N1 C4 C5 99.9(7) . . ? N1 C4 C6 113.7(7) . . ? C5 C4 C6 117.0(8) . . ? N1 C4 H4 108.6 . . ? C5 C4 H4 108.6 . . ? C6 C4 H4 108.6 . . ? O1 C5 C4 105.7(8) . . ? O1 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? O1 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C7 C6 C11 121.6(11) . . ? C7 C6 C4 119.5(11) . . ? C11 C6 C4 118.6(9) . . ? C6 C7 C8 118.0(13) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C9 C8 C7 119.0(11) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C10 C9 C8 123.1(13) . . ? C10 C9 H9 118.5 . . ? C8 C9 H9 118.5 . . ? C9 C10 C11 119.3(13) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C6 C11 C10 118.7(10) . . ? C6 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? N2 C12 O2 113.1(8) . . ? N2 C12 C1 129.2(9) . . ? O2 C12 C1 117.7(7) . . ? N2 C13 C15 114.0(8) . . ? N2 C13 C14 103.3(8) . . ? C15 C13 C14 112.5(7) . . ? N2 C13 H13 108.9 . . ? C15 C13 H13 108.9 . . ? C14 C13 H13 108.9 . . ? O2 C14 C13 103.7(7) . . ? O2 C14 H14A 111.0 . . ? C13 C14 H14A 111.0 . . ? O2 C14 H14B 111.0 . . ? C13 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? C16 C15 C20 119.6(8) . . ? C16 C15 C13 121.2(8) . . ? C20 C15 C13 119.1(8) . . ? C15 C16 C17 119.2(9) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.8(9) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.5(9) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 120.1(9) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 119.6(8) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? C22 C21 O3 105.8(11) . . ? C22 C21 H21A 110.6 . . ? O3 C21 H21A 110.6 . . ? C22 C21 H21B 110.6 . . ? O3 C21 H21B 110.6 . . ? H21A C21 H21B 108.7 . . ? C21 C22 C23 108.0(13) . . ? C21 C22 H22A 110.1 . . ? C23 C22 H22A 110.1 . . ? C21 C22 H22B 110.1 . . ? C23 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? C24 C23 C22 101.1(12) . . ? C24 C23 H23A 111.5 . . ? C22 C23 H23A 111.5 . . ? C24 C23 H23B 111.5 . . ? C22 C23 H23B 111.5 . . ? H23A C23 H23B 109.4 . . ? O3 C24 C23 102.1(9) . . ? O3 C24 H24A 111.3 . . ? C23 C24 H24A 111.3 . . ? O3 C24 H24B 111.3 . . ? C23 C24 H24B 111.3 . . ? H24A C24 H24B 109.2 . . ? F2 Sb1 F2 89.8(5) 7 . ? F2 Sb1 F1 92.9(4) 7 7 ? F2 Sb1 F1 88.0(4) . 7 ? F2 Sb1 F1 88.0(4) 7 . ? F2 Sb1 F1 92.9(4) . . ? F1 Sb1 F1 178.7(6) 7 . ? F2 Sb1 F3 90.8(4) 7 7 ? F2 Sb1 F3 178.2(4) . 7 ? F1 Sb1 F3 90.3(4) 7 7 ? F1 Sb1 F3 88.7(4) . 7 ? F2 Sb1 F3 178.2(4) 7 . ? F2 Sb1 F3 90.8(4) . . ? F1 Sb1 F3 88.7(4) 7 . ? F1 Sb1 F3 90.3(4) . . ? F3 Sb1 F3 88.6(7) 7 . ? F6 Sb2 F6 177.1(14) 7 . ? F6 Sb2 F5 91.7(10) 7 7 ? F6 Sb2 F5 88.3(10) . 7 ? F6 Sb2 F5 88.3(10) 7 . ? F6 Sb2 F5 91.7(10) . . ? F5 Sb2 F5 178.2(8) 7 . ? F6 Sb2 F4 91.5(7) 7 . ? F6 Sb2 F4 91.5(7) . . ? F5 Sb2 F4 90.9(4) 7 . ? F5 Sb2 F4 90.9(4) . . ? F6 Sb2 F7 88.5(7) 7 . ? F6 Sb2 F7 88.5(7) . . ? F5 Sb2 F7 89.1(4) 7 . ? F5 Sb2 F7 89.1(4) . . ? F4 Sb2 F7 180.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.163 _refine_diff_density_min -1.400 _refine_diff_density_rms 0.149 #===END data_compound3 _database_code_depnum_ccdc_archive 'CCDC 878356' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 F6 N4 O12 S2 Sn2' _chemical_formula_weight 1318.47 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.106(4) _cell_length_b 15.498(4) _cell_length_c 22.757(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5328(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9940 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8522 _exptl_absorpt_correction_T_max 0.8978 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 55967 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.51 _reflns_number_total 12089 _reflns_number_gt 11019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0753P)^2^+42.6920P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 12089 _refine_ls_number_parameters 687 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1746 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Sn1 Sn 0.56565(3) 0.74407(3) 0.75254(2) 0.02235(12) Uani 1 1 d . . . Sn2 Sn 0.49527(4) 0.83810(4) 0.45366(2) 0.02527(13) Uani 1 1 d . . . S1 S 0.44208(14) 0.72898(13) 0.61280(9) 0.0245(4) Uani 1 1 d . . . S2 S 0.48133(17) 0.69875(19) 0.14787(13) 0.0443(6) Uani 1 1 d . . . O1 O 0.4995(5) 1.0113(3) 0.7208(2) 0.0288(12) Uani 1 1 d . . . O2 O 0.7864(4) 0.8988(4) 0.6921(3) 0.0289(13) Uani 1 1 d . . . O3 O 0.6353(4) 0.7873(4) 0.8438(2) 0.0278(12) Uani 1 1 d . . . O4 O 0.5247(4) 0.7404(4) 0.6436(3) 0.0330(13) Uani 1 1 d . . . O5 O 0.4471(4) 0.7508(5) 0.5508(2) 0.0353(13) Uani 1 1 d . . . O6 O 0.3636(4) 0.7596(5) 0.6422(3) 0.0376(14) Uani 1 1 d . . . O7 O 0.7573(4) 0.7706(4) 0.5178(3) 0.0289(13) Uani 1 1 d . . . O8 O 0.6412(4) 1.0507(4) 0.5304(3) 0.0297(13) Uani 1 1 d . . . O9 O 0.5665(5) 0.8945(4) 0.3699(3) 0.0338(14) Uani 1 1 d . . . O10 O 0.4072(6) 0.6572(7) 0.1195(5) 0.070(3) Uani 1 1 d . . . O11 O 0.4623(10) 0.7385(12) 0.2025(5) 0.118(5) Uani 1 1 d . . . O12 O 0.5583(7) 0.6517(7) 0.1465(7) 0.096(4) Uani 1 1 d . . . F1 F 0.4222(5) 0.5819(4) 0.6678(3) 0.0479(15) Uani 1 1 d . . . F2 F 0.4970(5) 0.5729(4) 0.5868(3) 0.0483(14) Uani 1 1 d . . . F3 F 0.3554(4) 0.5891(4) 0.5845(3) 0.0448(15) Uani 1 1 d . . . F4 F 0.5689(5) 0.8403(5) 0.1203(4) 0.068(2) Uani 1 1 d . . . F5 F 0.4342(7) 0.8410(7) 0.0938(8) 0.148(6) Uani 1 1 d . . . F6 F 0.5249(10) 0.7682(8) 0.0492(4) 0.134(5) Uani 1 1 d . . . N1 N 0.5163(4) 0.8722(4) 0.7444(3) 0.0240(13) Uani 1 1 d . . . N2 N 0.6838(4) 0.8026(4) 0.7194(3) 0.0212(13) Uani 1 1 d . . . N3 N 0.6202(5) 0.7871(5) 0.4801(4) 0.0299(16) Uani 1 1 d . . . N4 N 0.5462(5) 0.9512(5) 0.4960(3) 0.0270(15) Uani 1 1 d . . . C1 C 0.6423(6) 0.9544(5) 0.7045(3) 0.0249(16) Uani 1 1 d . . . C2 C 0.6710(7) 1.0428(5) 0.6843(4) 0.0316(19) Uani 1 1 d . . . H2A H 0.7354 1.0435 0.6790 0.047 Uiso 1 1 calc R . . H2B H 0.6543 1.0858 0.7139 0.047 Uiso 1 1 calc R . . H2C H 0.6420 1.0566 0.6469 0.047 Uiso 1 1 calc R . . C3 C 0.5540(6) 0.9423(5) 0.7239(3) 0.0245(16) Uani 1 1 d . . . C4 C 0.4208(5) 0.8901(4) 0.7527(4) 0.0238(15) Uani 1 1 d . . . H4 H 0.3872 0.8695 0.7175 0.029 Uiso 1 1 calc R . . C5 C 0.4207(6) 0.9902(5) 0.7539(5) 0.0303(17) Uani 1 1 d . . . H5A H 0.3670 1.0138 0.7348 0.036 Uiso 1 1 calc R . . H5B H 0.4244 1.0124 0.7946 0.036 Uiso 1 1 calc R . . C6 C 0.3833(6) 0.8479(6) 0.8077(4) 0.0310(18) Uani 1 1 d . . . C7 C 0.3102(7) 0.7938(6) 0.8032(6) 0.044(3) Uani 1 1 d . . . H7 H 0.2840 0.7837 0.7659 0.053 Uiso 1 1 calc R . . C8 C 0.2748(8) 0.7540(7) 0.8536(8) 0.067(4) Uani 1 1 d . . . H8 H 0.2232 0.7191 0.8508 0.080 Uiso 1 1 calc R . . C9 C 0.3154(9) 0.7661(9) 0.9068(6) 0.062(4) Uani 1 1 d . . . H9 H 0.2932 0.7371 0.9405 0.075 Uiso 1 1 calc R . . C10 C 0.3886(8) 0.8201(8) 0.9123(5) 0.053(3) Uani 1 1 d . . . H10 H 0.4151 0.8286 0.9497 0.063 Uiso 1 1 calc R . . C11 C 0.4228(7) 0.8612(7) 0.8636(4) 0.037(2) Uani 1 1 d . . . H11 H 0.4725 0.8983 0.8674 0.044 Uiso 1 1 calc R . . C12 C 0.7005(6) 0.8841(6) 0.7055(3) 0.0243(16) Uani 1 1 d . . . C13 C 0.7694(5) 0.7558(5) 0.7233(3) 0.0237(15) Uani 1 1 d . . . H13 H 0.7896 0.7548 0.7652 0.028 Uiso 1 1 calc R . . C14 C 0.8292(6) 0.8164(6) 0.6878(4) 0.033(2) Uani 1 1 d . . . H14A H 0.8895 0.8186 0.7048 0.040 Uiso 1 1 calc R . . H14B H 0.8333 0.7975 0.6463 0.040 Uiso 1 1 calc R . . C15 C 0.7655(5) 0.6642(6) 0.7001(4) 0.0245(15) Uani 1 1 d . . . C16 C 0.8081(6) 0.5979(6) 0.7286(5) 0.039(2) Uani 1 1 d . . . H16 H 0.8358 0.6089 0.7654 0.046 Uiso 1 1 calc R . . C17 C 0.8115(7) 0.5158(6) 0.7053(6) 0.046(3) Uani 1 1 d . . . H17 H 0.8422 0.4712 0.7255 0.055 Uiso 1 1 calc R . . C18 C 0.7701(6) 0.4987(6) 0.6522(5) 0.033(2) Uani 1 1 d . . . H18 H 0.7727 0.4424 0.6357 0.040 Uiso 1 1 calc R . . C19 C 0.7251(6) 0.5631(6) 0.6232(4) 0.0311(19) Uani 1 1 d . . . H19 H 0.6947 0.5508 0.5877 0.037 Uiso 1 1 calc R . . C20 C 0.7242(6) 0.6463(6) 0.6460(4) 0.0319(19) Uani 1 1 d . . . H20 H 0.6955 0.6913 0.6250 0.038 Uiso 1 1 calc R . . C21 C 0.6315(7) 0.7349(6) 0.8970(4) 0.0341(19) Uani 1 1 d . . . H21A H 0.6507 0.6750 0.8888 0.041 Uiso 1 1 calc R . . H21B H 0.5707 0.7336 0.9130 0.041 Uiso 1 1 calc R . . C22 C 0.6944(8) 0.7784(7) 0.9397(5) 0.043(2) Uani 1 1 d . . . H22A H 0.6754 0.7693 0.9809 0.051 Uiso 1 1 calc R . . H22B H 0.7556 0.7568 0.9348 0.051 Uiso 1 1 calc R . . C23 C 0.6871(7) 0.8719(6) 0.9223(4) 0.037(2) Uani 1 1 d . . . H23A H 0.7395 0.9050 0.9352 0.044 Uiso 1 1 calc R . . H23B H 0.6331 0.8986 0.9389 0.044 Uiso 1 1 calc R . . C24 C 0.6821(6) 0.8672(6) 0.8558(4) 0.0280(17) Uani 1 1 d . . . H24A H 0.6494 0.9173 0.8398 0.034 Uiso 1 1 calc R . . H24B H 0.7422 0.8661 0.8384 0.034 Uiso 1 1 calc R . . C25 C 0.4283(7) 0.6121(6) 0.6119(4) 0.0298(17) Uani 1 1 d . . . C26 C 0.6983(6) 0.9120(5) 0.5225(4) 0.0249(16) Uani 1 1 d . . . C27 C 0.7870(5) 0.9454(7) 0.5457(4) 0.0321(18) Uani 1 1 d . . . H27A H 0.8013 1.0003 0.5264 0.048 Uiso 1 1 calc R . . H27B H 0.8335 0.9031 0.5372 0.048 Uiso 1 1 calc R . . H27C H 0.7830 0.9543 0.5882 0.048 Uiso 1 1 calc R . . C28 C 0.6891(5) 0.8248(6) 0.5069(4) 0.0254(16) Uani 1 1 d . . . C29 C 0.6376(6) 0.6937(5) 0.4794(4) 0.0267(17) Uani 1 1 d . . . H29 H 0.6093 0.6660 0.5144 0.032 Uiso 1 1 calc R . . C30 C 0.7378(6) 0.6909(6) 0.4857(4) 0.0317(19) Uani 1 1 d . . . H30A H 0.7569 0.6395 0.5082 0.038 Uiso 1 1 calc R . . H30B H 0.7671 0.6905 0.4468 0.038 Uiso 1 1 calc R . . C31 C 0.6021(5) 0.6524(5) 0.4231(4) 0.0259(16) Uani 1 1 d . . . C32 C 0.5366(6) 0.5916(6) 0.4256(5) 0.034(2) Uani 1 1 d . . . H32 H 0.5130 0.5742 0.4624 0.041 Uiso 1 1 calc R . . C33 C 0.5037(7) 0.5542(6) 0.3721(5) 0.044(2) Uani 1 1 d . . . H33 H 0.4596 0.5105 0.3736 0.053 Uiso 1 1 calc R . . C34 C 0.5345(7) 0.5803(6) 0.3204(5) 0.041(2) Uani 1 1 d . . . H34 H 0.5119 0.5556 0.2853 0.049 Uiso 1 1 calc R . . C35 C 0.5995(7) 0.6436(7) 0.3173(4) 0.039(2) Uani 1 1 d . . . H35 H 0.6209 0.6625 0.2802 0.047 Uiso 1 1 calc R . . C36 C 0.6330(7) 0.6791(6) 0.3690(5) 0.037(2) Uani 1 1 d . . . H36 H 0.6776 0.7221 0.3670 0.045 Uiso 1 1 calc R . . C37 C 0.6285(6) 0.9669(5) 0.5162(3) 0.0244(16) Uani 1 1 d . . . C38 C 0.4953(6) 1.0332(6) 0.4950(4) 0.0316(17) Uani 1 1 d . . . H38 H 0.4867 1.0519 0.4533 0.038 Uiso 1 1 calc R . . C39 C 0.5575(7) 1.0965(6) 0.5258(5) 0.040(2) Uani 1 1 d . . . H39A H 0.5645 1.1499 0.5024 0.048 Uiso 1 1 calc R . . H39B H 0.5347 1.1118 0.5652 0.048 Uiso 1 1 calc R . . C40 C 0.4057(5) 1.0251(5) 0.5247(4) 0.0256(16) Uani 1 1 d . . . C41 C 0.3318(6) 1.0650(6) 0.5003(4) 0.0318(19) Uani 1 1 d . . . H41 H 0.3369 1.0943 0.4638 0.038 Uiso 1 1 calc R . . C42 C 0.2504(6) 1.0625(6) 0.5289(5) 0.033(2) Uani 1 1 d . . . H42 H 0.2001 1.0896 0.5119 0.040 Uiso 1 1 calc R . . C43 C 0.2430(6) 1.0203(6) 0.5822(5) 0.0331(19) Uani 1 1 d . . . H43 H 0.1878 1.0194 0.6022 0.040 Uiso 1 1 calc R . . C44 C 0.3157(6) 0.9794(6) 0.6068(5) 0.034(2) Uani 1 1 d . . . H44 H 0.3102 0.9494 0.6430 0.041 Uiso 1 1 calc R . . C45 C 0.3969(6) 0.9828(6) 0.5778(4) 0.0319(19) Uani 1 1 d . . . H45 H 0.4471 0.9555 0.5948 0.038 Uiso 1 1 calc R . . C46 C 0.5355(7) 0.8812(8) 0.3104(4) 0.045(3) Uani 1 1 d . . . H46A H 0.4878 0.9227 0.3008 0.053 Uiso 1 1 calc R . . H46B H 0.5124 0.8219 0.3055 0.053 Uiso 1 1 calc R . . C47 C 0.6143(10) 0.8955(10) 0.2715(5) 0.061(3) Uani 1 1 d . . . H47A H 0.6465 0.8408 0.2646 0.073 Uiso 1 1 calc R . . H47B H 0.5962 0.9202 0.2332 0.073 Uiso 1 1 calc R . . C48 C 0.6702(11) 0.9579(12) 0.3052(5) 0.077(5) Uani 1 1 d . . . H48A H 0.7338 0.9476 0.2972 0.093 Uiso 1 1 calc R . . H48B H 0.6556 1.0179 0.2940 0.093 Uiso 1 1 calc R . . C49 C 0.6504(8) 0.9430(8) 0.3679(4) 0.043(3) Uani 1 1 d . . . H49A H 0.6985 0.9095 0.3866 0.052 Uiso 1 1 calc R . . H49B H 0.6443 0.9987 0.3888 0.052 Uiso 1 1 calc R . . C50 C 0.5018(11) 0.7916(8) 0.1015(6) 0.059(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0243(2) 0.0167(2) 0.0260(2) 0.0004(2) 0.0019(2) -0.00083(19) Sn2 0.0210(2) 0.0272(3) 0.0276(3) -0.0032(2) -0.0003(2) 0.0005(2) S1 0.0253(9) 0.0255(9) 0.0226(9) -0.0001(7) -0.0018(8) -0.0001(8) S2 0.0386(14) 0.0496(14) 0.0447(14) 0.0077(11) 0.0049(11) 0.0018(11) O1 0.041(3) 0.021(3) 0.025(3) 0.000(2) -0.005(3) 0.007(3) O2 0.030(3) 0.027(3) 0.030(3) 0.000(2) 0.006(3) -0.008(3) O3 0.040(3) 0.029(3) 0.014(3) 0.005(2) -0.001(2) -0.002(3) O4 0.033(3) 0.039(3) 0.027(3) -0.003(3) -0.008(2) -0.006(3) O5 0.039(3) 0.046(3) 0.020(3) 0.005(3) -0.001(2) 0.003(3) O6 0.036(3) 0.036(3) 0.041(4) -0.003(3) 0.000(3) 0.010(3) O7 0.023(3) 0.036(3) 0.028(3) 0.003(3) -0.001(2) 0.005(2) O8 0.035(3) 0.027(3) 0.027(3) -0.002(2) -0.002(2) -0.004(3) O9 0.040(3) 0.044(3) 0.017(3) -0.001(2) -0.002(3) -0.011(3) O10 0.051(5) 0.066(6) 0.093(7) 0.005(6) -0.002(5) -0.017(5) O11 0.132(11) 0.174(14) 0.048(6) -0.012(8) 0.033(6) -0.029(11) O12 0.060(6) 0.048(5) 0.178(13) 0.015(7) -0.001(8) 0.018(5) F1 0.066(4) 0.041(3) 0.036(3) 0.014(2) -0.001(3) -0.007(3) F2 0.047(3) 0.033(3) 0.064(4) -0.005(3) 0.010(4) 0.006(3) F3 0.045(3) 0.044(3) 0.045(3) -0.005(3) -0.010(3) -0.015(3) F4 0.054(4) 0.044(4) 0.105(6) -0.006(4) -0.017(4) -0.014(4) F5 0.084(7) 0.070(6) 0.290(19) 0.054(9) -0.092(10) 0.003(6) F6 0.215(14) 0.134(9) 0.052(5) 0.015(6) 0.004(7) -0.103(10) N1 0.024(3) 0.022(3) 0.026(3) -0.001(3) 0.000(3) 0.000(2) N2 0.025(3) 0.019(3) 0.020(3) 0.000(2) 0.004(3) 0.002(3) N3 0.022(3) 0.027(4) 0.040(4) 0.003(3) 0.004(3) 0.005(3) N4 0.023(3) 0.025(3) 0.033(4) -0.002(3) -0.004(3) 0.005(3) C1 0.040(5) 0.020(4) 0.015(4) 0.000(3) 0.002(3) -0.005(3) C2 0.049(5) 0.021(4) 0.025(4) 0.003(3) 0.004(4) -0.002(4) C3 0.036(4) 0.022(4) 0.016(3) -0.004(3) -0.004(3) 0.001(3) C4 0.024(3) 0.018(3) 0.030(4) -0.007(3) -0.005(3) -0.004(3) C5 0.032(4) 0.023(3) 0.036(5) -0.002(4) -0.001(4) 0.003(3) C6 0.026(4) 0.025(4) 0.042(5) -0.001(4) 0.005(4) 0.012(4) C7 0.038(5) 0.022(4) 0.074(8) -0.003(5) 0.009(5) 0.007(4) C8 0.048(6) 0.021(5) 0.131(14) 0.012(7) 0.046(8) 0.000(5) C9 0.068(8) 0.057(8) 0.062(8) 0.018(6) 0.041(7) 0.033(7) C10 0.060(7) 0.067(8) 0.031(5) 0.013(5) 0.020(5) 0.036(6) C11 0.043(5) 0.045(5) 0.023(4) 0.002(4) 0.008(4) 0.019(4) C12 0.029(4) 0.030(4) 0.014(3) -0.004(3) 0.005(3) -0.010(3) C13 0.022(3) 0.025(4) 0.024(4) -0.004(3) 0.003(3) -0.002(3) C14 0.032(4) 0.032(5) 0.036(5) 0.004(4) 0.008(4) 0.000(4) C15 0.022(3) 0.026(4) 0.026(4) 0.002(3) 0.005(3) 0.000(3) C16 0.026(4) 0.028(4) 0.062(7) 0.007(4) -0.003(4) 0.005(4) C17 0.038(5) 0.023(4) 0.076(8) 0.006(5) -0.008(5) 0.009(4) C18 0.033(5) 0.024(4) 0.043(6) -0.001(4) 0.013(4) -0.003(3) C19 0.043(5) 0.028(4) 0.022(4) 0.002(3) 0.005(4) 0.000(4) C20 0.039(5) 0.021(4) 0.035(5) 0.004(3) 0.006(4) 0.010(4) C21 0.043(5) 0.026(4) 0.034(5) 0.009(4) 0.005(4) -0.002(4) C22 0.051(6) 0.038(5) 0.040(6) 0.006(4) -0.004(5) -0.007(5) C23 0.049(6) 0.038(5) 0.023(4) 0.001(4) -0.002(4) -0.008(4) C24 0.034(4) 0.028(4) 0.022(4) 0.000(3) -0.008(3) -0.005(3) C25 0.037(4) 0.029(4) 0.023(4) -0.001(3) -0.003(4) -0.001(4) C26 0.025(4) 0.029(4) 0.020(4) -0.001(3) 0.001(3) -0.005(3) C27 0.026(4) 0.049(5) 0.021(4) 0.002(4) -0.001(3) -0.006(4) C28 0.021(3) 0.031(4) 0.024(4) 0.002(3) 0.008(3) 0.000(3) C29 0.025(4) 0.026(4) 0.029(4) 0.003(3) 0.000(3) -0.004(3) C30 0.028(4) 0.030(4) 0.037(5) 0.003(4) -0.001(4) 0.002(4) C31 0.023(3) 0.021(4) 0.034(4) -0.001(3) 0.002(3) 0.014(3) C32 0.023(4) 0.036(5) 0.043(5) -0.001(4) 0.005(4) 0.004(4) C33 0.023(4) 0.031(5) 0.077(7) -0.014(5) 0.001(5) -0.001(4) C34 0.030(4) 0.031(5) 0.061(7) -0.016(4) -0.004(4) 0.004(4) C35 0.041(5) 0.049(6) 0.027(5) -0.003(4) 0.005(4) 0.014(5) C36 0.037(5) 0.026(4) 0.048(6) -0.008(4) 0.004(4) 0.003(4) C37 0.033(4) 0.032(4) 0.008(3) 0.000(3) 0.007(3) -0.008(4) C38 0.031(4) 0.030(4) 0.034(4) -0.005(3) -0.005(4) 0.004(4) C39 0.037(5) 0.027(4) 0.056(6) -0.006(4) -0.004(5) -0.002(4) C40 0.026(4) 0.020(4) 0.031(4) -0.007(3) -0.004(3) 0.000(3) C41 0.035(5) 0.025(4) 0.036(5) -0.001(4) -0.012(4) 0.001(4) C42 0.026(4) 0.024(4) 0.049(6) -0.004(4) -0.010(4) 0.002(3) C43 0.031(4) 0.028(4) 0.041(5) -0.009(4) 0.005(4) -0.006(4) C44 0.037(5) 0.029(4) 0.037(5) -0.007(4) 0.005(4) -0.004(4) C45 0.029(4) 0.026(4) 0.041(5) -0.003(4) -0.006(4) 0.004(4) C46 0.042(5) 0.060(7) 0.031(5) 0.005(5) -0.016(4) -0.011(5) C47 0.072(8) 0.082(9) 0.028(5) -0.004(6) 0.012(5) -0.023(7) C48 0.086(10) 0.117(13) 0.028(6) -0.010(7) 0.010(6) -0.060(10) C49 0.052(6) 0.059(7) 0.020(4) -0.006(4) -0.001(4) -0.025(6) C50 0.070(8) 0.048(6) 0.059(7) 0.012(5) -0.019(7) -0.006(7) _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 Sn1 N1 2.129(6) . ? Sn1 N2 2.139(7) . ? Sn1 O3 2.422(6) . ? Sn1 O4 2.557(6) . ? Sn2 N3 2.132(7) . ? Sn2 N4 2.144(7) . ? Sn2 O9 2.356(6) . ? Sn2 O5 2.692(6) . ? S1 O6 1.441(7) . ? S1 O4 1.442(6) . ? S1 O5 1.453(6) . ? S1 C25 1.823(9) . ? S2 O12 1.373(10) . ? S2 O11 1.418(12) . ? S2 O10 1.444(10) . ? S2 C50 1.812(12) . ? O1 C3 1.352(10) . ? O1 C5 1.446(11) . ? O2 C12 1.353(10) . ? O2 C14 1.435(11) . ? O3 C24 1.453(10) . ? O3 C21 1.458(10) . ? O7 C28 1.353(10) . ? O7 C30 1.466(11) . ? O8 C37 1.352(10) . ? O8 C39 1.452(12) . ? O9 C46 1.447(11) . ? O9 C49 1.475(12) . ? F1 C25 1.360(10) . ? F2 C25 1.331(11) . ? F3 C25 1.315(11) . ? F4 C50 1.333(15) . ? F5 C50 1.288(17) . ? F6 C50 1.292(17) . ? N1 C3 1.313(11) . ? N1 C4 1.481(10) . ? N2 C12 1.326(10) . ? N2 C13 1.485(10) . ? N3 C28 1.341(11) . ? N3 C29 1.472(11) . ? N4 C37 1.348(11) . ? N4 C38 1.485(11) . ? C1 C12 1.401(12) . ? C1 C3 1.417(12) . ? C1 C2 1.509(11) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C6 1.522(13) . ? C4 C5 1.552(10) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.390(14) . ? C6 C11 1.419(14) . ? C7 C8 1.408(18) . ? C7 H7 0.9500 . ? C8 C9 1.37(2) . ? C8 H8 0.9500 . ? C9 C10 1.39(2) . ? C9 H9 0.9500 . ? C10 C11 1.379(14) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C15 1.516(12) . ? C13 C14 1.534(12) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.376(12) . ? C15 C20 1.407(13) . ? C16 C17 1.381(15) . ? C16 H16 0.9500 . ? C17 C18 1.386(17) . ? C17 H17 0.9500 . ? C18 C19 1.376(13) . ? C18 H18 0.9500 . ? C19 C20 1.390(12) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.516(14) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.507(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.515(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 C37 1.362(12) . ? C26 C28 1.404(12) . ? C26 C27 1.530(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.521(12) . ? C29 C31 1.530(12) . ? C29 H29 1.0000 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.368(13) . ? C31 C36 1.379(14) . ? C32 C33 1.438(15) . ? C32 H32 0.9500 . ? C33 C34 1.327(17) . ? C33 H33 0.9500 . ? C34 C35 1.389(15) . ? C34 H34 0.9500 . ? C35 C36 1.395(14) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C38 C40 1.518(13) . ? C38 C39 1.528(13) . ? C38 H38 1.0000 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C45 1.383(13) . ? C40 C41 1.392(12) . ? C41 C42 1.392(14) . ? C41 H41 0.9500 . ? C42 C43 1.383(14) . ? C42 H42 0.9500 . ? C43 C44 1.385(14) . ? C43 H43 0.9500 . ? C44 C45 1.394(13) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.499(16) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.495(18) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.475(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn1 N2 82.3(2) . . ? N1 Sn1 O3 88.2(2) . . ? N2 Sn1 O3 79.8(2) . . ? N1 Sn1 O4 81.4(2) . . ? N2 Sn1 O4 82.5(2) . . ? O3 Sn1 O4 160.5(2) . . ? N3 Sn2 N4 81.9(3) . . ? N3 Sn2 O9 87.8(3) . . ? N4 Sn2 O9 84.1(3) . . ? N3 Sn2 O5 79.7(2) . . ? N4 Sn2 O5 98.0(2) . . ? O9 Sn2 O5 166.9(2) . . ? O6 S1 O4 116.5(4) . . ? O6 S1 O5 114.6(4) . . ? O4 S1 O5 113.4(4) . . ? O6 S1 C25 103.8(4) . . ? O4 S1 C25 103.1(4) . . ? O5 S1 C25 103.1(4) . . ? O12 S2 O11 115.0(9) . . ? O12 S2 O10 114.1(7) . . ? O11 S2 O10 115.5(7) . . ? O12 S2 C50 105.3(8) . . ? O11 S2 C50 101.6(8) . . ? O10 S2 C50 103.1(6) . . ? C3 O1 C5 107.2(6) . . ? C12 O2 C14 107.3(7) . . ? C24 O3 C21 109.7(6) . . ? C24 O3 Sn1 127.5(5) . . ? C21 O3 Sn1 122.7(5) . . ? S1 O4 Sn1 133.1(4) . . ? S1 O5 Sn2 158.2(4) . . ? C28 O7 C30 106.2(6) . . ? C37 O8 C39 109.2(7) . . ? C46 O9 C49 108.7(7) . . ? C46 O9 Sn2 123.8(6) . . ? C49 O9 Sn2 127.4(5) . . ? C3 N1 C4 108.2(6) . . ? C3 N1 Sn1 130.6(6) . . ? C4 N1 Sn1 120.4(5) . . ? C12 N2 C13 108.3(7) . . ? C12 N2 Sn1 130.3(6) . . ? C13 N2 Sn1 119.9(5) . . ? C28 N3 C29 107.1(7) . . ? C28 N3 Sn2 130.8(6) . . ? C29 N3 Sn2 121.3(6) . . ? C37 N4 C38 109.2(7) . . ? C37 N4 Sn2 129.2(6) . . ? C38 N4 Sn2 120.5(5) . . ? C12 C1 C3 118.9(7) . . ? C12 C1 C2 122.0(8) . . ? C3 C1 C2 119.1(8) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 114.2(8) . . ? N1 C3 C1 129.0(8) . . ? O1 C3 C1 116.8(7) . . ? N1 C4 C6 112.7(7) . . ? N1 C4 C5 101.1(6) . . ? C6 C4 C5 114.5(7) . . ? N1 C4 H4 109.4 . . ? C6 C4 H4 109.4 . . ? C5 C4 H4 109.4 . . ? O1 C5 C4 102.4(6) . . ? O1 C5 H5A 111.3 . . ? C4 C5 H5A 111.3 . . ? O1 C5 H5B 111.3 . . ? C4 C5 H5B 111.3 . . ? H5A C5 H5B 109.2 . . ? C7 C6 C11 119.1(10) . . ? C7 C6 C4 119.6(9) . . ? C11 C6 C4 121.3(8) . . ? C6 C7 C8 120.5(13) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 119.3(12) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 121.2(11) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 120.2(12) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C6 119.8(11) . . ? C10 C11 H11 120.1 . . ? C6 C11 H11 120.1 . . ? N2 C12 O2 113.4(8) . . ? N2 C12 C1 128.7(8) . . ? O2 C12 C1 117.9(7) . . ? N2 C13 C15 113.8(6) . . ? N2 C13 C14 100.5(7) . . ? C15 C13 C14 114.3(7) . . ? N2 C13 H13 109.3 . . ? C15 C13 H13 109.3 . . ? C14 C13 H13 109.3 . . ? O2 C14 C13 104.1(7) . . ? O2 C14 H14A 110.9 . . ? C13 C14 H14A 110.9 . . ? O2 C14 H14B 110.9 . . ? C13 C14 H14B 110.9 . . ? H14A C14 H14B 109.0 . . ? C16 C15 C20 118.2(9) . . ? C16 C15 C13 121.1(8) . . ? C20 C15 C13 120.5(7) . . ? C15 C16 C17 121.6(11) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C18 119.7(10) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.1(9) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.0(9) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C15 120.3(8) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? O3 C21 C22 105.1(7) . . ? O3 C21 H21A 110.7 . . ? C22 C21 H21A 110.7 . . ? O3 C21 H21B 110.7 . . ? C22 C21 H21B 110.7 . . ? H21A C21 H21B 108.8 . . ? C23 C22 C21 102.3(8) . . ? C23 C22 H22A 111.3 . . ? C21 C22 H22A 111.3 . . ? C23 C22 H22B 111.3 . . ? C21 C22 H22B 111.3 . . ? H22A C22 H22B 109.2 . . ? C22 C23 C24 102.7(8) . . ? C22 C23 H23A 111.2 . . ? C24 C23 H23A 111.2 . . ? C22 C23 H23B 111.2 . . ? C24 C23 H23B 111.2 . . ? H23A C23 H23B 109.1 . . ? O3 C24 C23 104.7(7) . . ? O3 C24 H24A 110.8 . . ? C23 C24 H24A 110.8 . . ? O3 C24 H24B 110.8 . . ? C23 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? F3 C25 F2 109.0(7) . . ? F3 C25 F1 107.1(8) . . ? F2 C25 F1 107.3(8) . . ? F3 C25 S1 111.7(6) . . ? F2 C25 S1 111.7(7) . . ? F1 C25 S1 109.9(6) . . ? C37 C26 C28 119.9(8) . . ? C37 C26 C27 120.1(8) . . ? C28 C26 C27 120.0(8) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 O7 113.8(8) . . ? N3 C28 C26 127.7(8) . . ? O7 C28 C26 118.4(7) . . ? N3 C29 C30 101.8(7) . . ? N3 C29 C31 110.9(7) . . ? C30 C29 C31 114.5(7) . . ? N3 C29 H29 109.8 . . ? C30 C29 H29 109.8 . . ? C31 C29 H29 109.8 . . ? O7 C30 C29 102.9(7) . . ? O7 C30 H30A 111.2 . . ? C29 C30 H30A 111.2 . . ? O7 C30 H30B 111.2 . . ? C29 C30 H30B 111.2 . . ? H30A C30 H30B 109.1 . . ? C32 C31 C36 119.2(9) . . ? C32 C31 C29 120.4(8) . . ? C36 C31 C29 120.3(8) . . ? C31 C32 C33 119.5(9) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C34 C33 C32 120.4(9) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.6(10) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 119.4(10) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 120.8(9) . . ? C31 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? N4 C37 O8 112.6(8) . . ? N4 C37 C26 129.6(8) . . ? O8 C37 C26 117.8(7) . . ? N4 C38 C40 112.6(7) . . ? N4 C38 C39 102.9(7) . . ? C40 C38 C39 113.4(7) . . ? N4 C38 H38 109.2 . . ? C40 C38 H38 109.2 . . ? C39 C38 H38 109.2 . . ? O8 C39 C38 104.8(7) . . ? O8 C39 H39A 110.8 . . ? C38 C39 H39A 110.8 . . ? O8 C39 H39B 110.8 . . ? C38 C39 H39B 110.8 . . ? H39A C39 H39B 108.9 . . ? C45 C40 C41 118.8(9) . . ? C45 C40 C38 120.9(8) . . ? C41 C40 C38 120.1(8) . . ? C40 C41 C42 120.7(9) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C43 C42 C41 119.6(8) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 C44 120.5(9) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C45 119.3(9) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C40 C45 C44 121.1(9) . . ? C40 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? O9 C46 C47 106.0(8) . . ? O9 C46 H46A 110.5 . . ? C47 C46 H46A 110.5 . . ? O9 C46 H46B 110.5 . . ? C47 C46 H46B 110.5 . . ? H46A C46 H46B 108.7 . . ? C48 C47 C46 104.0(10) . . ? C48 C47 H47A 111.0 . . ? C46 C47 H47A 111.0 . . ? C48 C47 H47B 111.0 . . ? C46 C47 H47B 111.0 . . ? H47A C47 H47B 109.0 . . ? C49 C48 C47 106.3(10) . . ? C49 C48 H48A 110.5 . . ? C47 C48 H48A 110.5 . . ? C49 C48 H48B 110.5 . . ? C47 C48 H48B 110.5 . . ? H48A C48 H48B 108.7 . . ? O9 C49 C48 106.5(8) . . ? O9 C49 H49A 110.4 . . ? C48 C49 H49A 110.4 . . ? O9 C49 H49B 110.4 . . ? C48 C49 H49B 110.4 . . ? H49A C49 H49B 108.6 . . ? F5 C50 F6 104.8(13) . . ? F5 C50 F4 108.1(10) . . ? F6 C50 F4 104.5(13) . . ? F5 C50 S2 114.5(12) . . ? F6 C50 S2 111.1(9) . . ? F4 C50 S2 113.1(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.372 _refine_diff_density_min -1.536 _refine_diff_density_rms 0.184 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 878357' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H29 F6 N2 O3 Sb Sn' _chemical_formula_weight 759.94 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.2143(9) _cell_length_b 15.2143(9) _cell_length_c 23.8249(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5514.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9946 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.956 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8284 _exptl_absorpt_correction_T_max 0.8592 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 31181 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.55 _reflns_number_total 6331 _reflns_number_gt 5935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0286P)^2^+11.7048P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 6331 _refine_ls_number_parameters 357 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C25 C 0.9049(9) 0.1849(10) -0.1291(5) 0.091(4) Uani 0.65 1 d P A 1 H25A H 0.9490 0.1565 -0.1531 0.137 Uiso 0.65 1 calc PR A 1 H25B H 0.8884 0.2416 -0.1454 0.137 Uiso 0.65 1 calc PR A 1 H25C H 0.8529 0.1472 -0.1264 0.137 Uiso 0.65 1 calc PR A 1 C26 C 0.8605(15) 0.0878(10) -0.0886(7) 0.070(6) Uani 0.35 1 d P A 2 H26A H 0.8311 0.0336 -0.0767 0.106 Uiso 0.35 1 calc PR A 2 H26B H 0.8809 0.0814 -0.1274 0.106 Uiso 0.35 1 calc PR A 2 H26C H 0.8191 0.1370 -0.0863 0.106 Uiso 0.35 1 calc PR A 2 Sn1 Sn 0.82724(2) 0.259993(17) 0.099957(13) 0.03239(8) Uani 1 1 d . . . O1 O 0.7568(2) -0.00329(19) 0.14992(15) 0.0424(8) Uani 1 1 d . . . O2 O 1.0429(3) 0.1100(2) 0.1683(2) 0.0692(14) Uani 1 1 d . . . O3 O 0.8893(3) 0.2042(2) 0.01857(15) 0.0498(9) Uani 1 1 d . A . C1 C 0.8993(4) 0.0542(3) 0.1606(2) 0.0469(13) Uani 1 1 d . . . N1 N 0.7744(2) 0.1342(2) 0.11927(14) 0.0295(7) Uani 1 1 d . . . N2 N 0.9414(3) 0.2068(2) 0.13921(19) 0.0396(9) Uani 1 1 d . . . C2 C 0.9307(4) -0.0342(3) 0.1815(3) 0.0668(19) Uani 1 1 d . . . H2A H 0.9239 -0.0780 0.1516 0.100 Uiso 1 1 calc R . . H2B H 0.8957 -0.0519 0.2141 0.100 Uiso 1 1 calc R . . H2C H 0.9927 -0.0302 0.1922 0.100 Uiso 1 1 calc R . . C3 C 0.8129(3) 0.0652(3) 0.14278(19) 0.0374(10) Uani 1 1 d . . . C4 C 0.6786(3) 0.1160(3) 0.11267(19) 0.0356(9) Uani 1 1 d . . . H4 H 0.6455 0.1414 0.1451 0.043 Uiso 1 1 calc R . . C5 C 0.6790(4) 0.0155(3) 0.1168(2) 0.0407(11) Uani 1 1 d . . . H5A H 0.6253 -0.0063 0.1357 0.049 Uiso 1 1 calc R . . H5B H 0.6831 -0.0117 0.0791 0.049 Uiso 1 1 calc R . . C6 C 0.6425(4) 0.1527(3) 0.0580(2) 0.0499(11) Uani 1 1 d U . . C7 C 0.5759(5) 0.2145(4) 0.0607(3) 0.0665(14) Uani 1 1 d U . . H7 H 0.5531 0.2341 0.0957 0.080 Uiso 1 1 calc R . . C8 C 0.5428(5) 0.2479(4) 0.0087(4) 0.0814(16) Uani 1 1 d U . . H8 H 0.4964 0.2896 0.0082 0.098 Uiso 1 1 calc R . . C9 C 0.5793(6) 0.2184(5) -0.0402(4) 0.0863(17) Uani 1 1 d U . . H9 H 0.5573 0.2420 -0.0744 0.104 Uiso 1 1 calc R . . C10 C 0.6449(5) 0.1578(5) -0.0436(3) 0.0817(16) Uani 1 1 d U . . H10 H 0.6674 0.1384 -0.0786 0.098 Uiso 1 1 calc R . . C11 C 0.6770(4) 0.1259(4) 0.0068(2) 0.0631(13) Uani 1 1 d U . . H11 H 0.7238 0.0847 0.0064 0.076 Uiso 1 1 calc R . . C12 C 0.9566(4) 0.1242(3) 0.1560(3) 0.0491(13) Uani 1 1 d . . . C13 C 1.0254(3) 0.2552(3) 0.1373(2) 0.0426(12) Uani 1 1 d . . . H13 H 1.0448 0.2607 0.0973 0.051 Uiso 1 1 calc R . . C14 C 1.0884(4) 0.1945(3) 0.1682(3) 0.066(2) Uani 1 1 d . . . H14A H 1.1454 0.1902 0.1483 0.079 Uiso 1 1 calc R . . H14B H 1.0990 0.2154 0.2070 0.079 Uiso 1 1 calc R . . C15 C 1.0204(3) 0.3458(3) 0.16311(19) 0.0345(10) Uani 1 1 d . . . C16 C 1.0556(3) 0.4179(3) 0.1359(2) 0.0383(10) Uani 1 1 d . . . H16 H 1.0791 0.4120 0.0991 0.046 Uiso 1 1 calc R . . C17 C 1.0566(3) 0.5000(3) 0.1630(2) 0.0441(12) Uani 1 1 d . . . H17 H 1.0817 0.5493 0.1445 0.053 Uiso 1 1 calc R . . C18 C 1.0218(3) 0.5099(3) 0.2155(2) 0.0420(11) Uani 1 1 d . . . H18 H 1.0238 0.5654 0.2337 0.050 Uiso 1 1 calc R . . C19 C 0.9839(4) 0.4387(3) 0.2418(2) 0.0472(12) Uani 1 1 d . . . H19 H 0.9585 0.4461 0.2779 0.057 Uiso 1 1 calc R . . C20 C 0.9820(4) 0.3562(3) 0.2164(2) 0.0431(11) Uani 1 1 d . . . H20 H 0.9553 0.3077 0.2348 0.052 Uiso 1 1 calc R . . C21 C 0.8847(5) 0.2521(5) -0.0332(3) 0.077(2) Uani 1 1 d . A . H21A H 0.9080 0.3124 -0.0286 0.093 Uiso 1 1 calc R . . H21B H 0.8234 0.2555 -0.0471 0.093 Uiso 1 1 calc R . . C22 C 0.9418(7) 0.1988(10) -0.0730(3) 0.127(5) Uani 1 1 d . . . H22 H 1.0033 0.2218 -0.0747 0.153 Uiso 1 1 calc R A 1 C23 C 0.9386(6) 0.1055(7) -0.0505(4) 0.103(3) Uani 1 1 d . A . H23 H 0.9915 0.0707 -0.0619 0.124 Uiso 1 1 calc R B 2 C24 C 0.9369(4) 0.1216(4) 0.0103(3) 0.0663(18) Uani 1 1 d . . . H24A H 0.9066 0.0729 0.0299 0.080 Uiso 1 1 calc R A . H24B H 0.9974 0.1264 0.0252 0.080 Uiso 1 1 calc R . . F1 F 0.7019(3) 0.2346(3) 0.2949(2) 0.0954(15) Uani 1 1 d . . . F2 F 0.7464(3) 0.4029(3) 0.2888(2) 0.0998(15) Uani 1 1 d . . . F3 F 0.5770(3) 0.3568(3) 0.2952(2) 0.1021(16) Uani 1 1 d . . . F4 F 0.3257(3) 0.3257(3) 0.0000 0.104(2) Uani 1 2 d S . . F5 F 0.1584(4) 0.3171(4) 0.0263(3) 0.133(2) Uani 1 1 d . . . F6 F 0.2709(5) 0.2046(4) 0.0719(3) 0.144(2) Uani 1 1 d . . . F7 F 0.1524(3) 0.1524(3) 0.0000 0.166(5) Uani 1 2 d S . . Sb1 Sb 0.671307(18) 0.328693(18) 0.2500 0.02914(9) Uani 1 2 d S . . Sb2 Sb 0.23834(3) 0.23834(3) 0.0000 0.0766(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C25 0.085(8) 0.106(10) 0.082(8) 0.016(7) -0.005(7) -0.007(8) C26 0.121(17) 0.033(8) 0.058(10) 0.025(7) -0.015(10) -0.015(9) Sn1 0.03152(14) 0.01792(12) 0.04773(16) 0.00016(11) -0.00329(14) 0.00018(11) O1 0.054(2) 0.0264(15) 0.0469(19) 0.0043(14) -0.0014(18) -0.0084(15) O2 0.055(2) 0.0281(18) 0.124(4) -0.005(2) -0.043(3) 0.0069(16) O3 0.055(2) 0.0393(19) 0.055(2) 0.0056(16) 0.0145(18) 0.0011(16) C1 0.056(3) 0.027(2) 0.058(3) 0.005(2) -0.022(3) 0.000(2) N1 0.0324(19) 0.0226(16) 0.0336(18) -0.0045(14) -0.0012(15) -0.0026(13) N2 0.038(2) 0.0258(17) 0.056(3) -0.0021(17) -0.0131(19) 0.0009(15) C2 0.080(4) 0.027(3) 0.094(5) 0.011(3) -0.040(4) -0.003(3) C3 0.056(3) 0.0219(18) 0.034(2) 0.0002(17) -0.008(2) -0.0037(19) C4 0.038(2) 0.0250(19) 0.044(2) -0.0044(17) 0.009(2) -0.0046(18) C5 0.048(3) 0.030(2) 0.043(2) -0.0006(18) 0.009(2) -0.014(2) C6 0.049(2) 0.040(2) 0.060(2) 0.011(2) -0.018(2) -0.0244(19) C7 0.068(3) 0.033(2) 0.098(3) 0.007(2) -0.037(3) -0.014(2) C8 0.085(3) 0.041(3) 0.118(4) 0.017(3) -0.047(3) -0.019(3) C9 0.092(4) 0.069(3) 0.098(4) 0.029(3) -0.044(3) -0.046(3) C10 0.080(3) 0.088(3) 0.077(3) 0.022(3) -0.026(3) -0.046(3) C11 0.060(3) 0.075(3) 0.054(2) 0.015(2) -0.019(2) -0.034(2) C12 0.054(3) 0.028(2) 0.065(3) -0.002(2) -0.024(3) 0.006(2) C13 0.033(2) 0.029(2) 0.067(3) -0.008(2) -0.011(2) 0.0036(19) C14 0.044(3) 0.035(3) 0.119(6) -0.005(3) -0.038(3) 0.004(2) C15 0.031(2) 0.028(2) 0.044(3) -0.0022(18) -0.0100(18) 0.0016(17) C16 0.030(2) 0.037(2) 0.048(3) 0.005(2) -0.0010(19) 0.0019(18) C17 0.039(3) 0.025(2) 0.069(3) 0.012(2) -0.007(2) -0.0002(18) C18 0.041(3) 0.030(2) 0.055(3) -0.003(2) -0.009(2) 0.0045(19) C19 0.058(3) 0.041(3) 0.043(3) -0.002(2) -0.005(2) 0.001(2) C20 0.050(3) 0.033(2) 0.047(3) 0.004(2) -0.004(2) -0.008(2) C21 0.081(5) 0.095(6) 0.056(4) 0.018(4) 0.018(3) 0.008(4) C22 0.103(7) 0.230(15) 0.050(4) -0.023(6) 0.008(4) 0.044(8) C23 0.085(6) 0.108(7) 0.116(7) -0.052(6) -0.007(5) 0.034(5) C24 0.060(4) 0.050(3) 0.089(5) -0.014(3) 0.022(3) 0.004(3) F1 0.091(3) 0.075(3) 0.120(3) 0.061(3) -0.016(3) 0.009(2) F2 0.083(3) 0.084(3) 0.132(4) -0.035(3) -0.051(3) -0.005(2) F3 0.079(3) 0.109(4) 0.118(4) -0.019(3) 0.060(3) 0.010(2) F4 0.067(2) 0.067(2) 0.178(7) -0.012(3) 0.012(3) -0.019(3) F5 0.106(4) 0.085(3) 0.208(6) 0.011(4) 0.071(4) 0.036(3) F6 0.173(7) 0.120(5) 0.139(5) 0.015(4) -0.031(5) -0.004(4) F7 0.070(3) 0.070(3) 0.358(15) 0.041(5) -0.041(5) -0.026(3) Sb1 0.03022(12) 0.03022(12) 0.02696(17) 0.00201(11) 0.00201(11) 0.00254(16) Sb2 0.04387(19) 0.04387(19) 0.1421(6) -0.0083(3) 0.0083(3) 0.0071(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C25 C22 1.466(14) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C23 1.52(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Sn1 N1 2.126(3) . ? Sn1 N2 2.133(4) . ? Sn1 O3 2.318(4) . ? O1 C3 1.358(5) . ? O1 C5 1.451(6) . ? O2 C12 1.363(6) . ? O2 C14 1.461(6) . ? O3 C21 1.435(7) . ? O3 C24 1.462(7) . ? C1 C12 1.381(7) . ? C1 C3 1.391(7) . ? C1 C2 1.512(7) . ? N1 C3 1.327(6) . ? N1 C4 1.492(6) . ? N2 C12 1.338(6) . ? N2 C13 1.476(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C6 1.519(7) . ? C4 C5 1.533(6) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.385(9) . ? C6 C11 1.389(9) . ? C7 C8 1.430(9) . ? C7 H7 0.9500 . ? C8 C9 1.367(12) . ? C8 H8 0.9500 . ? C9 C10 1.361(12) . ? C9 H9 0.9500 . ? C10 C11 1.384(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C15 1.512(6) . ? C13 C14 1.522(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.382(6) . ? C15 C20 1.406(7) . ? C16 C17 1.406(7) . ? C16 H16 0.9500 . ? C17 C18 1.367(8) . ? C17 H17 0.9500 . ? C18 C19 1.377(7) . ? C18 H18 0.9500 . ? C19 C20 1.394(7) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.521(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.518(16) . ? C22 H22 1.0000 . ? C23 C24 1.469(11) . ? C23 H23 1.0000 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? F1 Sb1 1.846(3) . ? F2 Sb1 1.854(4) . ? F3 Sb1 1.844(4) . ? F4 Sb2 1.879(6) . ? F5 Sb2 1.818(5) . ? F6 Sb2 1.856(6) . ? F7 Sb2 1.848(6) . ? Sb1 F3 1.844(4) 8_665 ? Sb1 F1 1.846(3) 8_665 ? Sb1 F2 1.854(4) 8_665 ? Sb2 F5 1.818(5) 7 ? Sb2 F6 1.856(6) 7 ? 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 C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N1 Sn1 N2 82.62(14) . . ? N1 Sn1 O3 90.31(13) . . ? N2 Sn1 O3 84.02(15) . . ? C3 O1 C5 107.1(3) . . ? C12 O2 C14 108.4(4) . . ? C21 O3 C24 110.2(5) . . ? C21 O3 Sn1 120.9(4) . . ? C24 O3 Sn1 128.9(4) . . ? C12 C1 C3 118.7(4) . . ? C12 C1 C2 120.9(5) . . ? C3 C1 C2 120.3(4) . . ? C3 N1 C4 109.2(4) . . ? C3 N1 Sn1 129.6(3) . . ? C4 N1 Sn1 120.9(3) . . ? C12 N2 C13 109.2(4) . . ? C12 N2 Sn1 128.9(3) . . ? C13 N2 Sn1 120.1(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 112.5(4) . . ? N1 C3 C1 129.8(4) . . ? O1 C3 C1 117.7(4) . . ? N1 C4 C6 112.0(4) . . ? N1 C4 C5 100.1(4) . . ? C6 C4 C5 115.0(4) . . ? N1 C4 H4 109.8 . . ? C6 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? O1 C5 C4 103.5(4) . . ? O1 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? O1 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C11 121.1(6) . . ? C7 C6 C4 118.3(6) . . ? C11 C6 C4 120.6(5) . . ? C6 C7 C8 117.3(8) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? C9 C8 C7 118.7(7) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C10 C9 C8 124.7(8) . . ? C10 C9 H9 117.6 . . ? C8 C9 H9 117.6 . . ? C9 C10 C11 116.5(8) . . ? C9 C10 H10 121.8 . . ? C11 C10 H10 121.8 . . ? C10 C11 C6 121.7(7) . . ? C10 C11 H11 119.1 . . ? C6 C11 H11 119.1 . . ? N2 C12 O2 112.3(5) . . ? N2 C12 C1 129.7(5) . . ? O2 C12 C1 117.9(4) . . ? N2 C13 C15 113.5(4) . . ? N2 C13 C14 103.1(4) . . ? C15 C13 C14 112.8(4) . . ? N2 C13 H13 109.1 . . ? C15 C13 H13 109.1 . . ? C14 C13 H13 109.1 . . ? O2 C14 C13 103.7(4) . . ? O2 C14 H14A 111.0 . . ? C13 C14 H14A 111.0 . . ? O2 C14 H14B 111.0 . . ? C13 C14 H14B 111.0 . . ? H14A C14 H14B 109.0 . . ? C16 C15 C20 119.7(4) . . ? C16 C15 C13 120.8(4) . . ? C20 C15 C13 119.4(4) . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.9(5) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 119.5(5) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 121.3(5) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C19 C20 C15 118.9(5) . . ? C19 C20 H20 120.5 . . ? C15 C20 H20 120.5 . . ? O3 C21 C22 103.7(7) . . ? O3 C21 H21A 111.0 . . ? C22 C21 H21A 111.0 . . ? O3 C21 H21B 111.0 . . ? C22 C21 H21B 111.0 . . ? H21A C21 H21B 109.0 . . ? C25 C22 C23 100.1(11) . . ? C25 C22 C21 115.2(9) . . ? C23 C22 C21 105.1(8) . . ? C25 C22 H22 111.8 . . ? C23 C22 H22 111.8 . . ? C21 C22 H22 111.8 . . ? C24 C23 C22 101.1(7) . . ? C24 C23 C26 127.2(11) . . ? C22 C23 C26 88.8(9) . . ? C24 C23 H23 111.8 . . ? C22 C23 H23 111.8 . . ? C26 C23 H23 111.8 . . ? O3 C24 C23 106.6(6) . . ? O3 C24 H24A 110.4 . . ? C23 C24 H24A 110.4 . . ? O3 C24 H24B 110.4 . . ? C23 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? F3 Sb1 F3 88.9(3) . 8_665 ? F3 Sb1 F1 178.8(2) . 8_665 ? F3 Sb1 F1 92.1(2) 8_665 8_665 ? F3 Sb1 F1 92.1(2) . . ? F3 Sb1 F1 178.8(2) 8_665 . ? F1 Sb1 F1 86.8(3) 8_665 . ? F3 Sb1 F2 92.7(2) . . ? F3 Sb1 F2 87.7(2) 8_665 . ? F1 Sb1 F2 87.9(2) 8_665 . ? F1 Sb1 F2 91.6(2) . . ? F3 Sb1 F2 87.7(2) . 8_665 ? F3 Sb1 F2 92.7(2) 8_665 8_665 ? F1 Sb1 F2 91.6(2) 8_665 8_665 ? F1 Sb1 F2 87.9(2) . 8_665 ? F2 Sb1 F2 179.4(3) . 8_665 ? F5 Sb2 F5 179.2(4) . 7 ? F5 Sb2 F7 89.60(19) . . ? F5 Sb2 F7 89.60(19) 7 . ? F5 Sb2 F6 92.5(3) . . ? F5 Sb2 F6 87.5(3) 7 . ? F7 Sb2 F6 89.6(2) . . ? F5 Sb2 F6 87.5(3) . 7 ? F5 Sb2 F6 92.5(3) 7 7 ? F7 Sb2 F6 89.6(2) . 7 ? F6 Sb2 F6 179.2(4) . 7 ? F5 Sb2 F4 90.40(19) . . ? F5 Sb2 F4 90.40(19) 7 . ? F7 Sb2 F4 180.00(19) . . ? F6 Sb2 F4 90.4(2) . . ? F6 Sb2 F4 90.4(2) 7 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.378 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.080 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 878358' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H29 F3 N2 O6 S Sn' _chemical_formula_weight 673.26 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.2892(13) _cell_length_b 15.2892(13) _cell_length_c 23.565(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5508.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.41 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7991 _exptl_absorpt_correction_T_max 0.8149 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 61765 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6314 _reflns_number_gt 5993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0253P)^2^+6.4663P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(2) _refine_ls_number_reflns 6314 _refine_ls_number_parameters 490 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C6B C 0.6267(17) 0.1569(17) 0.0637(13) 0.043(3) Uani 0.30 1 d PU A 2 C7B C 0.5542(11) 0.2072(9) 0.0794(7) 0.044(2) Uani 0.30 1 d PU A 2 H7B H 0.5376 0.2146 0.1179 0.052 Uiso 0.30 1 calc PR A 2 C8B C 0.5067(11) 0.2466(10) 0.0340(6) 0.051(2) Uani 0.30 1 d PU A 2 H8B H 0.4547 0.2789 0.0411 0.061 Uiso 0.30 1 calc PR A 2 C9B C 0.5388(13) 0.2364(12) -0.0217(9) 0.052(2) Uani 0.30 1 d PU A 2 H9B H 0.5095 0.2667 -0.0513 0.062 Uiso 0.30 1 calc PR A 2 C10B C 0.6121(14) 0.1838(12) -0.0364(8) 0.049(2) Uani 0.30 1 d PU A 2 H10B H 0.6301 0.1736 -0.0744 0.059 Uiso 0.30 1 calc PR A 2 C11B C 0.6552(12) 0.1485(9) 0.0107(8) 0.046(2) Uani 0.30 1 d PU A 2 H11B H 0.7078 0.1167 0.0045 0.055 Uiso 0.30 1 calc PR A 2 C25B C 0.8523(19) 0.0843(18) -0.0895(10) 0.120(9) Uani 0.30 1 d P B 2 H25D H 0.8132 0.1350 -0.0875 0.180 Uiso 0.30 1 calc PR B 2 H25E H 0.8213 0.0322 -0.0760 0.180 Uiso 0.30 1 calc PR B 2 H25F H 0.8709 0.0753 -0.1288 0.180 Uiso 0.30 1 calc PR B 2 C6A C 0.6484(6) 0.1420(6) 0.0558(5) 0.050(2) Uani 0.70 1 d P A 1 C7A C 0.5845(6) 0.2075(5) 0.0543(3) 0.0626(19) Uani 0.70 1 d P A 1 H7A H 0.5623 0.2289 0.0893 0.075 Uiso 0.70 1 calc PR A 1 C8A C 0.5518(8) 0.2429(6) 0.0044(5) 0.083(3) Uani 0.70 1 d P A 1 H8A H 0.5075 0.2864 0.0048 0.100 Uiso 0.70 1 calc PR A 1 C9A C 0.5857(8) 0.2128(6) -0.0449(5) 0.074(3) Uani 0.70 1 d P A 1 H9A H 0.5644 0.2369 -0.0794 0.089 Uiso 0.70 1 calc PR A 1 C10A C 0.6508(6) 0.1476(7) -0.0480(3) 0.073(2) Uani 0.70 1 d P A 1 H10A H 0.6732 0.1278 -0.0833 0.088 Uiso 0.70 1 calc PR A 1 C11A C 0.6806(5) 0.1137(6) 0.0031(3) 0.0559(16) Uani 0.70 1 d P A 1 H11A H 0.7244 0.0697 0.0024 0.067 Uiso 0.70 1 calc PR A 1 C25A C 0.9012(6) 0.1866(7) -0.1328(4) 0.096(3) Uani 0.70 1 d P C 1 H25A H 0.9396 0.1500 -0.1561 0.143 Uiso 0.70 1 calc PR C 1 H25B H 0.8988 0.2457 -0.1488 0.143 Uiso 0.70 1 calc PR C 1 H25C H 0.8423 0.1614 -0.1323 0.143 Uiso 0.70 1 calc PR C 1 S2 S 0.82220(15) 0.76559(15) 0.48425(10) 0.0600(5) Uani 0.50 1 d P D 3 O6 O 0.8656(11) 0.7032(9) 0.5183(7) 0.116(5) Uani 0.50 1 d P D 3 O7 O 0.7990(12) 0.7247(9) 0.4294(7) 0.092(6) Uani 0.50 1 d P D 3 O8 O 0.8588(8) 0.8447(8) 0.5146(5) 0.090(3) Uani 0.50 1 d P D 3 F3 F 0.6923(7) 0.6753(7) 0.4831(3) 0.119(3) Uani 0.50 1 d P E 4 F4 F 0.8321(9) 0.6674(7) 0.5070(7) 0.122(5) Uani 0.50 1 d P E 4 F5 F 0.8075(12) 0.7314(15) 0.4291(8) 0.194(10) Uani 0.50 1 d P E 4 C27 C 0.7723(8) 0.7134(8) 0.4829(7) 0.090(4) Uani 0.50 1 d P E 4 Sn1 Sn 0.823282(17) 0.255125(14) 0.104200(12) 0.04677(8) Uani 1 1 d . . . S1 S 0.73552(11) 0.30119(10) 0.25334(7) 0.0369(4) Uani 0.50 1 d P . . F1 F 0.7356(5) 0.4208(4) 0.2842(3) 0.0692(16) Uani 0.50 1 d P . . F2A F 0.6164(6) 0.4099(6) 0.2204(4) 0.094(3) Uani 0.50 1 d P . . F2B F 0.6503(9) 0.4014(9) 0.1989(5) 0.148(6) Uani 0.50 1 d P . . O1 O 0.7573(2) -0.01155(14) 0.14743(10) 0.0495(6) Uani 1 1 d . . . O2 O 1.0406(2) 0.10249(19) 0.16761(18) 0.0796(11) Uani 1 1 d . . . O3 O 0.8861(2) 0.2020(2) 0.01896(13) 0.0668(8) Uani 1 1 d . C . O4B O 0.7750(5) 0.2568(6) 0.2154(3) 0.068(2) Uani 0.50 1 d P . . O4A O 0.7618(5) 0.2947(4) 0.1942(3) 0.0547(16) Uani 0.50 1 d P . . O5 O 0.7734(5) 0.3769(5) 0.2768(3) 0.0651(18) Uani 0.50 1 d P . . N1 N 0.77290(19) 0.12699(17) 0.11777(11) 0.0385(6) Uani 1 1 d . A . N2 N 0.9390(2) 0.19967(18) 0.13994(15) 0.0461(7) Uani 1 1 d . . . C1 C 0.8981(3) 0.0478(2) 0.15925(19) 0.0579(11) Uani 1 1 d . . . C2 C 0.9299(4) -0.0403(3) 0.1804(3) 0.0833(18) Uani 1 1 d . . . H2A H 0.9162 -0.0854 0.1522 0.125 Uiso 1 1 calc R . . H2B H 0.9007 -0.0545 0.2163 0.125 Uiso 1 1 calc R . . H2C H 0.9932 -0.0381 0.1864 0.125 Uiso 1 1 calc R . . C3 C 0.8123(3) 0.0582(2) 0.14125(15) 0.0430(8) Uani 1 1 d . . . C4 C 0.6785(3) 0.1082(2) 0.11147(14) 0.0440(8) Uani 1 1 d . . . H4 H 0.6440 0.1341 0.1434 0.053 Uiso 1 1 calc R A 1 C5 C 0.6792(3) 0.0080(2) 0.11472(16) 0.0493(9) Uani 1 1 d . A . H5A H 0.6261 -0.0141 0.1341 0.059 Uiso 1 1 calc R . . H5B H 0.6826 -0.0182 0.0764 0.059 Uiso 1 1 calc R . . C12 C 0.9551(3) 0.1180(2) 0.1554(2) 0.0563(10) Uani 1 1 d . . . C13 C 1.0235(2) 0.2480(3) 0.13621(19) 0.0532(9) Uani 1 1 d . . . H13 H 1.0414 0.2529 0.0955 0.064 Uiso 1 1 calc R . . C14 C 1.0857(3) 0.1851(3) 0.1671(3) 0.0859(18) Uani 1 1 d . . . H14A H 1.1421 0.1802 0.1467 0.103 Uiso 1 1 calc R . . H14B H 1.0973 0.2055 0.2063 0.103 Uiso 1 1 calc R . . C15 C 1.0196(2) 0.3380(2) 0.16200(16) 0.0423(8) Uani 1 1 d . . . C16 C 1.0549(2) 0.4092(2) 0.13417(17) 0.0459(9) Uani 1 1 d . . . H16 H 1.0776 0.4022 0.0969 0.055 Uiso 1 1 calc R . . C17 C 1.0579(3) 0.4906(2) 0.15961(18) 0.0523(9) Uani 1 1 d . . . H17 H 1.0833 0.5387 0.1401 0.063 Uiso 1 1 calc R . . C18 C 1.0236(3) 0.5020(3) 0.21374(19) 0.0516(10) Uani 1 1 d . . . H18 H 1.0259 0.5577 0.2316 0.062 Uiso 1 1 calc R . . C19 C 0.9865(3) 0.4324(3) 0.24111(16) 0.0504(9) Uani 1 1 d . . . H19 H 0.9617 0.4404 0.2777 0.060 Uiso 1 1 calc R . . C20 C 0.9845(3) 0.3504(2) 0.21634(17) 0.0499(9) Uani 1 1 d . . . H20 H 0.9593 0.3025 0.2362 0.060 Uiso 1 1 calc R . . C21 C 0.8795(4) 0.2483(5) -0.0336(2) 0.0931(18) Uani 1 1 d . C . H21A H 0.9039 0.3081 -0.0303 0.112 Uiso 1 1 calc R . . H21B H 0.8180 0.2520 -0.0465 0.112 Uiso 1 1 calc R . . C22 C 0.9355(5) 0.1907(7) -0.0744(2) 0.120(3) Uani 1 1 d . . . H22 H 0.9970 0.2129 -0.0751 0.144 Uiso 1 1 calc R C 1 C23 C 0.9342(6) 0.1010(5) -0.0514(4) 0.114(3) Uani 1 1 d . B . H23 H 0.9861 0.0657 -0.0633 0.137 Uiso 1 1 calc R F 2 C24 C 0.9333(4) 0.1198(4) 0.0100(3) 0.0856(18) Uani 1 1 d . . . H24A H 0.9040 0.0717 0.0307 0.103 Uiso 1 1 calc R C . H24B H 0.9940 0.1250 0.0244 0.103 Uiso 1 1 calc R . . C26 C 0.6695(6) 0.3761(5) 0.2618(4) 0.0514(18) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C6B 0.055(6) 0.026(5) 0.048(6) 0.001(4) -0.009(5) -0.005(4) C7B 0.057(6) 0.024(4) 0.050(5) -0.001(4) -0.010(4) -0.002(4) C8B 0.065(5) 0.031(4) 0.058(5) 0.002(4) -0.010(4) 0.000(4) C9B 0.064(6) 0.033(4) 0.057(6) 0.004(4) -0.013(5) 0.001(4) C10B 0.059(6) 0.034(5) 0.055(5) 0.007(4) -0.007(5) -0.004(4) C11B 0.056(6) 0.032(4) 0.049(5) 0.004(4) -0.006(4) -0.004(4) C25B 0.16(3) 0.12(2) 0.080(14) 0.023(14) -0.004(16) 0.013(18) C6A 0.051(5) 0.038(5) 0.060(6) 0.009(4) -0.015(4) -0.017(3) C7A 0.085(6) 0.031(3) 0.071(5) -0.006(3) -0.020(4) -0.002(4) C8A 0.117(8) 0.039(4) 0.093(7) 0.006(5) -0.039(6) -0.006(4) C9A 0.084(7) 0.047(5) 0.090(6) 0.017(4) -0.026(5) -0.024(5) C10A 0.070(5) 0.106(7) 0.044(3) 0.008(4) -0.007(3) -0.028(5) C11A 0.048(4) 0.082(5) 0.038(3) 0.007(3) -0.006(3) -0.012(3) C25A 0.082(6) 0.115(8) 0.089(6) 0.014(5) -0.013(5) -0.002(5) S2 0.0482(11) 0.0597(13) 0.0721(13) -0.0036(10) -0.0052(10) 0.0053(11) O6 0.132(13) 0.105(11) 0.112(8) 0.004(8) -0.045(8) 0.047(9) O7 0.120(12) 0.083(7) 0.073(9) -0.015(6) 0.039(8) -0.038(8) O8 0.084(6) 0.080(6) 0.107(11) 0.017(6) -0.016(6) -0.024(5) F3 0.126(7) 0.132(7) 0.098(7) -0.035(6) 0.017(5) -0.054(6) F4 0.117(9) 0.070(6) 0.180(13) 0.000(6) 0.014(9) 0.049(6) F5 0.106(10) 0.38(3) 0.099(11) -0.087(12) -0.009(8) 0.074(12) C27 0.080(8) 0.063(6) 0.129(11) -0.004(7) 0.024(7) 0.000(6) Sn1 0.04855(15) 0.02340(10) 0.06836(15) -0.00140(11) -0.00740(12) 0.00054(10) S1 0.0353(8) 0.0388(8) 0.0367(7) -0.0013(7) -0.0013(8) 0.0017(6) F1 0.083(4) 0.048(3) 0.077(4) -0.015(3) -0.008(3) -0.002(3) F2A 0.099(7) 0.075(4) 0.107(7) 0.029(5) 0.001(5) 0.046(5) F2B 0.163(11) 0.134(9) 0.146(10) 0.106(8) 0.058(7) 0.084(8) O1 0.0696(17) 0.0329(11) 0.0461(12) 0.0081(11) 0.0005(15) -0.0081(12) O2 0.064(2) 0.0357(15) 0.140(3) -0.0079(18) -0.037(2) 0.0100(14) O3 0.079(2) 0.0631(19) 0.0584(18) 0.0201(15) 0.0176(16) -0.0027(16) O4B 0.056(4) 0.079(5) 0.071(5) 0.001(4) 0.021(3) 0.025(4) O4A 0.062(4) 0.053(4) 0.049(4) -0.008(3) 0.021(3) 0.009(3) O5 0.061(4) 0.053(4) 0.081(5) -0.008(4) -0.014(3) -0.013(3) N1 0.0519(18) 0.0290(13) 0.0346(14) -0.0015(10) -0.0014(12) -0.0002(11) N2 0.0491(17) 0.0292(14) 0.0599(19) -0.0021(14) -0.0069(15) 0.0014(11) C1 0.077(3) 0.0301(17) 0.067(3) 0.0044(17) -0.019(2) 0.0042(18) C2 0.099(4) 0.033(2) 0.118(5) 0.008(2) -0.036(3) 0.002(2) C3 0.063(2) 0.0293(14) 0.0367(16) -0.0020(13) -0.0029(17) -0.0003(15) C4 0.055(2) 0.0386(16) 0.0381(17) 0.0035(14) 0.0067(17) -0.0068(15) C5 0.058(2) 0.0433(18) 0.046(2) 0.0054(15) 0.0064(18) -0.0102(18) C12 0.064(3) 0.0317(17) 0.073(3) -0.0047(18) -0.018(2) 0.0056(16) C13 0.0440(19) 0.0399(18) 0.076(3) -0.009(2) -0.0028(18) 0.0026(17) C14 0.060(3) 0.039(2) 0.158(6) -0.007(3) -0.037(3) 0.009(2) C15 0.0379(17) 0.0359(17) 0.053(2) 0.0006(15) -0.0095(15) 0.0011(14) C16 0.0393(19) 0.046(2) 0.053(2) 0.0078(16) -0.0015(16) 0.0036(15) C17 0.047(2) 0.0368(18) 0.073(3) 0.0157(18) 0.0014(19) -0.0011(15) C18 0.054(2) 0.0327(17) 0.068(3) -0.0024(18) -0.0073(19) 0.0003(16) C19 0.062(2) 0.047(2) 0.0421(19) 0.0007(16) 0.0003(17) -0.0026(17) C20 0.062(2) 0.0370(19) 0.051(2) 0.0123(16) -0.0037(18) -0.0067(17) C21 0.105(4) 0.105(4) 0.070(3) 0.027(4) 0.007(3) -0.026(4) C22 0.116(6) 0.192(9) 0.053(3) -0.006(4) 0.013(3) -0.016(6) C23 0.121(6) 0.099(5) 0.121(6) -0.014(5) 0.022(5) 0.021(5) C24 0.096(4) 0.075(4) 0.086(4) -0.013(3) 0.039(3) -0.002(3) C26 0.050(4) 0.041(4) 0.063(5) 0.002(3) 0.005(4) 0.008(3) _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 C6B C11B 1.33(3) . ? C6B C7B 1.40(3) . ? C6B C4 1.56(3) . ? C7B C8B 1.43(2) . ? C7B H7B 0.9500 . ? C8B C9B 1.41(3) . ? C8B H8B 0.9500 . ? C9B C10B 1.42(3) . ? C9B H9B 0.9500 . ? C10B C11B 1.40(3) . ? C10B H10B 0.9500 . ? C11B H11B 0.9500 . ? C25B C23 1.56(3) . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C6A C7A 1.400(11) . ? C6A C11A 1.404(12) . ? C6A C4 1.483(13) . ? C7A C8A 1.387(12) . ? C7A H7A 0.9500 . ? C8A C9A 1.352(15) . ? C8A H8A 0.9500 . ? C9A C10A 1.411(13) . ? C9A H9A 0.9500 . ? C10A C11A 1.387(10) . ? C10A H10A 0.9500 . ? C11A H11A 0.9500 . ? C25A C22 1.474(10) . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? S2 O6 1.413(14) . ? S2 S2 1.431(5) 7_556 ? S2 O8 1.466(11) 7_556 ? S2 O7 1.479(17) . ? S2 O8 1.512(11) . ? O8 O8 0.753(16) 7_556 ? O8 S2 1.466(11) 7_556 ? F3 F3 0.876(13) 7_556 ? F3 C27 1.355(14) . ? F3 C27 1.716(14) 7_556 ? F4 C27 1.287(17) . ? F5 C27 1.40(2) . ? C27 C27 1.51(2) 7_556 ? C27 F3 1.716(14) 7_556 ? Sn1 N1 2.129(3) . ? Sn1 N2 2.135(3) . ? Sn1 O3 2.370(3) . ? Sn1 O4A 2.398(6) . ? S1 S1 0.809(3) 8_665 ? S1 O4B 1.274(7) . ? S1 O4B 1.383(7) 8_665 ? S1 O5 1.407(6) . ? S1 O4A 1.453(6) . ? S1 C26 1.540(8) . ? S1 O4A 1.633(6) 8_665 ? S1 C26 1.801(7) 8_665 ? S1 O5 2.181(6) 8_665 ? F1 C26 1.328(10) . ? F2A C26 1.290(12) 8_665 ? F2A C26 1.371(13) . ? F2A F2A 1.506(19) 8_665 ? F2B C26 1.481(13) 8_665 ? F2B C26 1.560(14) . ? O1 C3 1.365(4) . ? O1 C5 1.453(5) . ? O2 C12 1.359(5) . ? O2 C14 1.439(6) . ? O3 C21 1.429(6) . ? O3 C24 1.465(6) . ? O4B S1 1.383(7) 8_665 ? O4B O4B 1.768(15) 8_665 ? O4A S1 1.633(6) 8_665 ? O5 S1 2.181(6) 8_665 ? N1 C3 1.332(4) . ? N1 C4 1.478(5) . ? N2 C12 1.324(5) . ? N2 C13 1.491(5) . ? C1 C12 1.385(6) . ? C1 C3 1.388(6) . ? C1 C2 1.517(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C5 1.534(5) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C13 C15 1.504(5) . ? C13 C14 1.537(6) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.382(5) . ? C15 C20 1.402(6) . ? C16 C17 1.382(6) . ? C16 H16 0.9500 . ? C17 C18 1.390(6) . ? C17 H17 0.9500 . ? C18 C19 1.368(5) . ? C18 H18 0.9500 . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.560(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.474(11) . ? C22 H22 1.0000 . ? C23 C24 1.476(9) . ? C23 H23 1.0000 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 C26 1.134(17) 8_665 ? C26 F2A 1.290(12) 8_665 ? C26 F2B 1.481(13) 8_665 ? C26 S1 1.801(7) 8_665 ? 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 C11B C6B C7B 124(2) . . ? C11B C6B C4 117.6(17) . . ? C7B C6B C4 118(2) . . ? C6B C7B C8B 116.1(19) . . ? C6B C7B H7B 122.0 . . ? C8B C7B H7B 122.0 . . ? C9B C8B C7B 118.2(15) . . ? C9B C8B H8B 120.9 . . ? C7B C8B H8B 120.9 . . ? C8B C9B C10B 124.3(16) . . ? C8B C9B H9B 117.9 . . ? C10B C9B H9B 117.9 . . ? C11B C10B C9B 113.4(17) . . ? C11B C10B H10B 123.3 . . ? C9B C10B H10B 123.3 . . ? C6B C11B C10B 123.6(19) . . ? C6B C11B H11B 118.2 . . ? C10B C11B H11B 118.2 . . ? C23 C25B H25D 109.5 . . ? C23 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C23 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C7A C6A C11A 116.2(10) . . ? C7A C6A C4 119.3(8) . . ? C11A C6A C4 124.5(7) . . ? C8A C7A C6A 123.5(9) . . ? C8A C7A H7A 118.2 . . ? C6A C7A H7A 118.2 . . ? C9A C8A C7A 117.2(10) . . ? C9A C8A H8A 121.4 . . ? C7A C8A H8A 121.4 . . ? C8A C9A C10A 123.7(10) . . ? C8A C9A H9A 118.1 . . ? C10A C9A H9A 118.1 . . ? C11A C10A C9A 116.8(9) . . ? C11A C10A H10A 121.6 . . ? C9A C10A H10A 121.6 . . ? C10A C11A C6A 122.6(9) . . ? C10A C11A H11A 118.7 . . ? C6A C11A H11A 118.7 . . ? C22 C25A H25A 109.5 . . ? C22 C25A H25B 109.5 . . ? C22 C25A H25C 109.5 . . ? O6 S2 S2 113.5(8) . 7_556 ? O6 S2 O8 122.4(7) . 7_556 ? S2 S2 O8 62.9(6) 7_556 7_556 ? O6 S2 O7 108.9(9) . . ? S2 S2 O7 124.3(8) 7_556 . ? O8 S2 O7 118.9(6) 7_556 . ? O6 S2 O8 95.6(7) . . ? S2 S2 O8 59.7(6) 7_556 . ? O8 S2 O8 29.3(6) 7_556 . ? O7 S2 O8 147.2(6) . . ? O8 O8 S2 78.8(13) 7_556 7_556 ? O8 O8 S2 72.0(13) 7_556 . ? S2 O8 S2 57.4(3) 7_556 . ? F3 F3 C27 98.3(9) 7_556 . ? F3 F3 C27 51.4(7) 7_556 7_556 ? C27 F3 C27 57.4(9) . 7_556 ? F4 C27 F3 113.9(13) . . ? F4 C27 F5 103.5(14) . . ? F3 C27 F5 115.7(14) . . ? F4 C27 C27 120.9(18) . 7_556 ? F3 C27 C27 73.4(6) . 7_556 ? F5 C27 C27 126.5(16) . 7_556 ? F4 C27 F3 107.7(12) . 7_556 ? F3 C27 F3 30.3(5) . 7_556 ? F5 C27 F3 142.2(14) . 7_556 ? C27 C27 F3 49.2(6) 7_556 7_556 ? N1 Sn1 N2 82.82(11) . . ? N1 Sn1 O3 87.63(11) . . ? N2 Sn1 O3 82.08(13) . . ? N1 Sn1 O4A 87.56(18) . . ? N2 Sn1 O4A 94.4(2) . . ? O3 Sn1 O4A 174.34(18) . . ? S1 S1 O4B 79.8(4) 8_665 . ? S1 S1 O4B 65.1(4) 8_665 8_665 ? O4B S1 O4B 83.3(7) . 8_665 ? S1 S1 O5 158.8(4) 8_665 . ? O4B S1 O5 121.3(5) . . ? O4B S1 O5 116.7(5) 8_665 . ? S1 S1 O4A 87.6(4) 8_665 . ? O4B S1 O4A 32.9(3) . . ? O4B S1 O4A 115.4(5) 8_665 . ? O5 S1 O4A 108.6(4) . . ? S1 S1 C26 95.0(3) 8_665 . ? O4B S1 C26 143.0(5) . . ? O4B S1 C26 127.8(5) 8_665 . ? O5 S1 C26 66.8(4) . . ? O4A S1 C26 110.9(4) . . ? S1 S1 O4A 62.7(3) 8_665 8_665 ? O4B S1 O4A 110.5(6) . 8_665 ? O4B S1 O4A 28.9(3) 8_665 8_665 ? O5 S1 O4A 107.7(4) . 8_665 ? O4A S1 O4A 139.7(4) . 8_665 ? C26 S1 O4A 98.9(4) . 8_665 ? S1 S1 C26 58.4(3) 8_665 8_665 ? O4B S1 C26 116.3(5) . 8_665 ? O4B S1 C26 113.3(5) 8_665 8_665 ? O5 S1 C26 105.2(4) . 8_665 ? O4A S1 C26 95.1(4) . 8_665 ? C26 S1 C26 38.7(6) . 8_665 ? O4A S1 C26 91.6(4) 8_665 8_665 ? S1 S1 O5 13.5(2) 8_665 8_665 ? O4B S1 O5 82.3(4) . 8_665 ? O4B S1 O5 78.5(4) 8_665 8_665 ? O5 S1 O5 151.8(5) . 8_665 ? O4A S1 O5 82.6(4) . 8_665 ? C26 S1 O5 85.1(4) . 8_665 ? O4A S1 O5 73.4(3) 8_665 8_665 ? C26 S1 O5 47.0(3) 8_665 8_665 ? C26 F2A C26 50.3(7) 8_665 . ? C26 F2A F2A 58.1(6) 8_665 8_665 ? C26 F2A F2A 53.0(6) . 8_665 ? C26 F2B C26 43.7(6) 8_665 . ? C3 O1 C5 106.8(3) . . ? C12 O2 C14 107.9(3) . . ? C21 O3 C24 109.6(4) . . ? C21 O3 Sn1 122.4(4) . . ? C24 O3 Sn1 128.0(3) . . ? S1 O4B S1 35.2(2) . 8_665 ? S1 O4B O4B 51.0(4) . 8_665 ? S1 O4B O4B 45.7(4) 8_665 8_665 ? S1 O4A S1 29.68(16) . 8_665 ? S1 O4A Sn1 166.8(4) . . ? S1 O4A Sn1 146.0(4) 8_665 . ? S1 O5 S1 7.72(14) . 8_665 ? C3 N1 C4 109.2(3) . . ? C3 N1 Sn1 128.7(2) . . ? C4 N1 Sn1 121.1(2) . . ? C12 N2 C13 108.8(3) . . ? C12 N2 Sn1 129.6(3) . . ? C13 N2 Sn1 119.8(2) . . ? C12 C1 C3 119.1(3) . . ? C12 C1 C2 120.5(4) . . ? C3 C1 C2 120.3(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 112.5(3) . . ? N1 C3 C1 130.1(3) . . ? O1 C3 C1 117.4(3) . . ? N1 C4 C6A 108.9(4) . . ? N1 C4 C5 100.6(3) . . ? C6A C4 C5 113.2(5) . . ? N1 C4 C6B 118.3(11) . . ? C6A C4 C6B 16.4(10) . . ? C5 C4 C6B 120.9(10) . . ? N1 C4 H4 111.2 . . ? C6A C4 H4 111.2 . . ? C5 C4 H4 111.2 . . ? C6B C4 H4 94.8 . . ? O1 C5 C4 103.7(3) . . ? O1 C5 H5A 111.0 . . ? C4 C5 H5A 111.0 . . ? O1 C5 H5B 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? N2 C12 O2 113.7(4) . . ? N2 C12 C1 129.1(4) . . ? O2 C12 C1 117.2(3) . . ? N2 C13 C15 113.3(3) . . ? N2 C13 C14 101.4(3) . . ? C15 C13 C14 113.9(4) . . ? N2 C13 H13 109.3 . . ? C15 C13 H13 109.3 . . ? C14 C13 H13 109.3 . . ? O2 C14 C13 104.8(4) . . ? O2 C14 H14A 110.8 . . ? C13 C14 H14A 110.8 . . ? O2 C14 H14B 110.8 . . ? C13 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? C16 C15 C20 118.4(3) . . ? C16 C15 C13 120.9(4) . . ? C20 C15 C13 120.6(3) . . ? C15 C16 C17 121.1(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.9(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.4(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 121.0(4) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 120.0(4) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? O3 C21 C22 102.5(6) . . ? O3 C21 H21A 111.3 . . ? C22 C21 H21A 111.3 . . ? O3 C21 H21B 111.3 . . ? C22 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C25A C22 C23 107.4(8) . . ? C25A C22 C21 113.9(7) . . ? C23 C22 C21 106.9(6) . . ? C25A C22 H22 109.5 . . ? C23 C22 H22 109.5 . . ? C21 C22 H22 109.5 . . ? C22 C23 C24 100.3(6) . . ? C22 C23 C25B 87.2(11) . . ? C24 C23 C25B 126.0(11) . . ? C22 C23 H23 112.8 . . ? C24 C23 H23 112.8 . . ? C25B C23 H23 112.8 . . ? O3 C24 C23 108.2(6) . . ? O3 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O3 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C26 C26 F2A 68.6(8) 8_665 8_665 ? C26 C26 F1 168.5(8) 8_665 . ? F2A C26 F1 122.8(9) 8_665 . ? C26 C26 F2A 61.1(7) 8_665 . ? F2A C26 F2A 68.9(9) 8_665 . ? F1 C26 F2A 122.7(8) . . ? C26 C26 F2B 71.9(10) 8_665 8_665 ? F2A C26 F2B 29.8(5) 8_665 8_665 ? F1 C26 F2B 116.7(10) . 8_665 ? F2A C26 F2B 96.5(9) . 8_665 ? C26 C26 S1 83.2(3) 8_665 . ? F2A C26 S1 136.5(7) 8_665 . ? F1 C26 S1 86.3(5) . . ? F2A C26 S1 125.2(7) . . ? F2B C26 S1 111.0(6) 8_665 . ? C26 C26 F2B 64.5(10) 8_665 . ? F2A C26 F2B 96.3(9) 8_665 . ? F1 C26 F2B 113.2(9) . . ? F2A C26 F2B 28.2(4) . . ? F2B C26 F2B 121.5(8) 8_665 . ? S1 C26 F2B 100.6(6) . . ? C26 C26 S1 58.1(3) 8_665 8_665 ? F2A C26 S1 112.5(7) 8_665 8_665 ? F1 C26 S1 112.1(6) . 8_665 ? F2A C26 S1 111.3(7) . 8_665 ? F2B C26 S1 92.7(6) 8_665 8_665 ? S1 C26 S1 26.60(16) . 8_665 ? F2B C26 S1 95.3(6) . 8_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.557 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.059 #===END data_compound7 _database_code_depnum_ccdc_archive 'CCDC 886108' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H29 F6 Ge N2 O3 Sb' _chemical_formula_weight 713.84 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P4(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 15.0665(12) _cell_length_b 15.0665(12) _cell_length_c 23.9834(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5444.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9853 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 2.168 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6710 _exptl_absorpt_correction_T_max 0.6710 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 30618 _diffrn_reflns_av_R_equivalents 0.0305 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6253 _reflns_number_gt 5822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.014(17) _refine_ls_number_reflns 6253 _refine_ls_number_parameters 358 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.102 _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 C25 C 0.4043(8) 0.6951(9) -0.1260(4) 0.075(3) Uani 0.65 1 d PD A 1 H25A H 0.4437 0.6575 -0.1483 0.113 Uiso 0.65 1 calc PR A 1 H25B H 0.3998 0.7539 -0.1433 0.113 Uiso 0.65 1 calc PR A 1 H25C H 0.3453 0.6680 -0.1240 0.113 Uiso 0.65 1 calc PR A 1 C26 C 0.3769(17) 0.5809(12) -0.0913(8) 0.083(8) Uani 0.35 1 d PD A 2 H26A H 0.3630 0.5178 -0.0864 0.124 Uiso 0.35 1 calc PR A 2 H26B H 0.4032 0.5901 -0.1283 0.124 Uiso 0.35 1 calc PR A 2 H26C H 0.3224 0.6159 -0.0881 0.124 Uiso 0.35 1 calc PR A 2 Ge1 Ge 0.33636(3) 0.74817(3) 0.10087(2) 0.03123(11) Uani 1 1 d . . . O1 O 0.2592(3) 0.4987(2) 0.15066(16) 0.0496(10) Uani 1 1 d . . . O2 O 0.5493(3) 0.6139(3) 0.1663(3) 0.089(2) Uani 1 1 d . . . O3 O 0.3909(3) 0.7038(3) 0.02296(17) 0.0469(10) Uani 1 1 d . A . N1 N 0.2823(3) 0.6353(3) 0.11726(16) 0.0296(8) Uani 1 1 d . . . N2 N 0.4429(3) 0.7063(3) 0.1364(2) 0.0401(11) Uani 1 1 d . . . C1 C 0.4051(5) 0.5535(4) 0.1604(3) 0.059(2) Uani 1 1 d . . . C2 C 0.4353(6) 0.4637(4) 0.1829(4) 0.096(4) Uani 1 1 d . . . H2A H 0.4984 0.4667 0.1926 0.144 Uiso 1 1 calc R . . H2B H 0.4264 0.4181 0.1543 0.144 Uiso 1 1 calc R . . H2C H 0.4006 0.4486 0.2161 0.144 Uiso 1 1 calc R . . C3 C 0.3185(4) 0.5652(3) 0.1430(2) 0.0401(12) Uani 1 1 d . . . C4 C 0.1855(3) 0.6197(3) 0.1105(2) 0.0343(11) Uani 1 1 d . . . H4 H 0.1526 0.6489 0.1418 0.041 Uiso 1 1 calc R . . C5 C 0.1819(4) 0.5181(3) 0.1178(2) 0.0389(12) Uani 1 1 d . . . H5A H 0.1270 0.4998 0.1374 0.047 Uiso 1 1 calc R . . H5B H 0.1845 0.4877 0.0812 0.047 Uiso 1 1 calc R . . C6 C 0.1509(3) 0.6540(3) 0.0555(2) 0.0413(11) Uani 1 1 d U . . C7 C 0.0853(5) 0.7178(4) 0.0544(3) 0.0580(14) Uani 1 1 d U . . H7 H 0.0626 0.7421 0.0880 0.070 Uiso 1 1 calc R . . C8 C 0.0524(5) 0.7467(4) 0.0018(4) 0.0705(15) Uani 1 1 d U . . H8 H 0.0068 0.7902 -0.0001 0.085 Uiso 1 1 calc R . . C9 C 0.0866(5) 0.7115(5) -0.0459(4) 0.0717(16) Uani 1 1 d U . . H9 H 0.0645 0.7317 -0.0808 0.086 Uiso 1 1 calc R . . C10 C 0.1516(5) 0.6481(5) -0.0455(3) 0.0647(15) Uani 1 1 d U . . H10 H 0.1739 0.6243 -0.0794 0.078 Uiso 1 1 calc R . . C11 C 0.1838(4) 0.6197(4) 0.0050(3) 0.0494(12) Uani 1 1 d U . . H11 H 0.2293 0.5760 0.0059 0.059 Uiso 1 1 calc R . . C12 C 0.4616(5) 0.6246(4) 0.1545(3) 0.0566(18) Uani 1 1 d . . . C13 C 0.5254(3) 0.7593(4) 0.1344(3) 0.0465(14) Uani 1 1 d . . . H13 H 0.5432 0.7680 0.0946 0.056 Uiso 1 1 calc R . . C14 C 0.5927(5) 0.6989(4) 0.1628(4) 0.074(3) Uani 1 1 d . . . H14A H 0.6478 0.6946 0.1405 0.089 Uiso 1 1 calc R . . H14B H 0.6077 0.7213 0.2004 0.089 Uiso 1 1 calc R . . C15 C 0.5174(3) 0.8493(3) 0.1625(2) 0.0352(11) Uani 1 1 d . . . C16 C 0.5537(3) 0.9240(3) 0.1376(3) 0.0395(12) Uani 1 1 d . . . H16 H 0.5779 0.9206 0.1011 0.047 Uiso 1 1 calc R . . C17 C 0.5543(4) 1.0043(3) 0.1667(3) 0.0424(13) Uani 1 1 d . . . H17 H 0.5809 1.0551 0.1502 0.051 Uiso 1 1 calc R . . C18 C 0.5171(4) 1.0112(3) 0.2190(2) 0.0398(12) Uani 1 1 d . . . H18 H 0.5185 1.0660 0.2385 0.048 Uiso 1 1 calc R . . C19 C 0.4779(4) 0.9375(4) 0.2426(2) 0.0416(12) Uani 1 1 d . . . H19 H 0.4503 0.9424 0.2781 0.050 Uiso 1 1 calc R . . C20 C 0.4781(4) 0.8561(4) 0.2151(2) 0.0415(12) Uani 1 1 d . . . H20 H 0.4517 0.8056 0.2320 0.050 Uiso 1 1 calc R . . C21 C 0.3816(5) 0.7551(5) -0.0274(3) 0.0648(19) Uani 1 1 d . A . H21A H 0.4029 0.8167 -0.0220 0.078 Uiso 1 1 calc R . . H21B H 0.3190 0.7566 -0.0400 0.078 Uiso 1 1 calc R . . C22 C 0.4408(7) 0.7042(9) -0.0692(3) 0.104(4) Uani 1 1 d D . . H22 H 0.5026 0.7284 -0.0699 0.125 Uiso 1 1 calc R A 1 C23 C 0.4392(7) 0.6086(8) -0.0489(5) 0.111(4) Uani 1 1 d D A . H23 H 0.4979 0.5820 -0.0590 0.134 Uiso 1 1 calc R B 2 C24 C 0.4402(5) 0.6223(5) 0.0116(3) 0.068(2) Uani 1 1 d . . . H24A H 0.4119 0.5714 0.0307 0.082 Uiso 1 1 calc R A . H24B H 0.5020 0.6278 0.0251 0.082 Uiso 1 1 calc R . . F1 F 0.4042(3) 0.2536(3) 0.03987(18) 0.0730(12) Uani 1 1 d . . . F2 F 0.3577(4) 0.4243(3) 0.0451(2) 0.0937(17) Uani 1 1 d . . . F3 F 0.2353(3) 0.2985(3) 0.0462(2) 0.0933(16) Uani 1 1 d . . . F4 F 0.8333(3) 0.8333(3) 0.0000 0.097(2) Uani 1 2 d S . . F5 F 0.6666(4) 0.8220(4) 0.0324(3) 0.131(2) Uani 1 1 d . . . F6 F 0.7850(4) 0.7046(4) 0.0688(3) 0.128(2) Uani 1 1 d . . . F7 F 0.6580(3) 0.6580(3) 0.0000 0.173(5) Uani 1 2 d S . . Sb1 Sb 0.32894(2) 0.32894(2) 0.0000 0.02873(10) Uani 1 2 d S . . Sb2 Sb 0.74536(3) 0.74536(3) 0.0000 0.0824(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C25 0.073(8) 0.083(9) 0.070(7) 0.007(6) 0.017(6) -0.007(7) C26 0.16(2) 0.039(10) 0.051(11) 0.024(9) -0.034(13) -0.023(12) Ge1 0.0282(2) 0.0193(2) 0.0462(3) -0.0014(2) -0.0043(2) 0.0008(2) O1 0.071(3) 0.0357(19) 0.042(2) 0.0099(17) -0.018(2) -0.020(2) O2 0.065(3) 0.031(2) 0.170(6) 0.004(3) -0.072(4) 0.003(2) O3 0.048(2) 0.038(2) 0.054(2) 0.0069(17) 0.0132(18) 0.0043(17) N1 0.033(2) 0.0240(19) 0.032(2) -0.0029(15) -0.0043(16) -0.0033(15) N2 0.037(2) 0.026(2) 0.057(3) -0.002(2) -0.017(2) 0.0013(17) C1 0.068(4) 0.030(3) 0.080(5) 0.011(3) -0.046(4) -0.006(3) C2 0.110(7) 0.038(4) 0.141(8) 0.038(4) -0.086(6) -0.015(4) C3 0.060(3) 0.026(2) 0.034(3) 0.0054(19) -0.015(3) -0.006(2) C4 0.033(3) 0.032(2) 0.037(3) -0.011(2) 0.007(2) -0.007(2) C5 0.044(3) 0.036(3) 0.037(3) -0.001(2) 0.002(2) -0.013(2) C6 0.036(2) 0.034(2) 0.055(2) 0.001(2) -0.012(2) -0.0152(18) C7 0.055(3) 0.032(2) 0.087(3) -0.001(2) -0.024(3) -0.010(2) C8 0.068(3) 0.037(3) 0.106(4) 0.011(3) -0.034(3) -0.012(2) C9 0.072(3) 0.058(3) 0.085(3) 0.022(3) -0.032(3) -0.031(3) C10 0.060(3) 0.070(3) 0.064(3) 0.015(3) -0.019(3) -0.030(3) C11 0.041(2) 0.059(3) 0.048(2) 0.004(2) -0.013(2) -0.022(2) C12 0.059(4) 0.034(3) 0.077(5) 0.004(3) -0.039(4) 0.000(3) C13 0.029(3) 0.034(3) 0.076(4) -0.012(3) -0.011(3) 0.001(2) C14 0.050(4) 0.027(3) 0.144(7) -0.011(4) -0.045(4) 0.006(3) C15 0.028(2) 0.025(2) 0.052(3) 0.001(2) -0.013(2) 0.0034(18) C16 0.030(2) 0.035(3) 0.054(3) 0.008(2) -0.001(2) 0.007(2) C17 0.039(3) 0.025(2) 0.064(4) 0.012(2) -0.001(3) 0.002(2) C18 0.041(3) 0.027(2) 0.052(3) -0.004(2) -0.009(2) 0.005(2) C19 0.045(3) 0.041(3) 0.038(3) -0.001(2) -0.006(2) 0.001(2) C20 0.043(3) 0.032(3) 0.050(3) 0.012(2) -0.007(2) -0.005(2) C21 0.064(4) 0.072(5) 0.058(4) 0.013(4) 0.000(3) -0.016(4) C22 0.095(7) 0.176(12) 0.040(4) -0.016(5) 0.012(4) 0.015(7) C23 0.097(8) 0.114(9) 0.123(9) -0.061(8) -0.011(6) 0.029(7) C24 0.056(4) 0.048(4) 0.100(6) -0.027(4) 0.025(4) 0.000(3) F1 0.059(2) 0.068(3) 0.092(3) 0.038(2) -0.012(2) 0.010(2) F2 0.114(4) 0.066(3) 0.102(4) -0.042(3) -0.048(3) 0.000(3) F3 0.059(3) 0.113(4) 0.109(4) 0.039(3) 0.043(3) 0.009(2) F4 0.063(2) 0.063(2) 0.165(6) -0.017(3) 0.017(3) -0.015(3) F5 0.098(4) 0.086(4) 0.209(6) 0.026(4) 0.080(4) 0.043(3) F6 0.127(5) 0.078(4) 0.178(6) 0.020(4) -0.019(5) 0.016(3) F7 0.070(3) 0.070(3) 0.380(16) 0.037(6) -0.037(6) -0.023(4) Sb1 0.02843(13) 0.02843(13) 0.02933(19) -0.00152(13) 0.00152(13) 0.00023(18) Sb2 0.03901(19) 0.03901(19) 0.1691(8) -0.0087(3) 0.0087(3) 0.0056(3) _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 C25 C22 1.474(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C23 1.446(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Ge1 N2 1.925(4) . ? Ge1 N1 1.926(4) . ? Ge1 O3 2.148(4) . ? O1 C3 1.355(6) . ? O1 C5 1.438(7) . ? O2 C12 1.360(7) . ? O2 C14 1.439(7) . ? O3 C21 1.441(7) . ? O3 C24 1.461(7) . ? N1 C3 1.340(6) . ? N1 C4 1.487(6) . ? N2 C12 1.334(7) . ? N2 C13 1.478(7) . ? C1 C12 1.377(9) . ? C1 C3 1.380(8) . ? C1 C2 1.526(8) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C6 1.511(7) . ? C4 C5 1.541(7) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.379(9) . ? C6 C11 1.407(9) . ? C7 C8 1.424(10) . ? C7 H7 0.9500 . ? C8 C9 1.362(12) . ? C8 H8 0.9500 . ? C9 C10 1.367(11) . ? C9 H9 0.9500 . ? C10 C11 1.374(8) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C15 1.519(7) . ? C13 C14 1.523(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.387(7) . ? C15 C20 1.398(8) . ? C16 C17 1.396(8) . ? C16 H16 0.9500 . ? C17 C18 1.377(8) . ? C17 H17 0.9500 . ? C18 C19 1.380(8) . ? C18 H18 0.9500 . ? C19 C20 1.392(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.547(11) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.521(15) . ? C22 H22 1.0000 . ? C23 C24 1.465(13) . ? C23 H23 1.0000 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? F1 Sb1 1.867(4) . ? F2 Sb1 1.851(4) . ? F3 Sb1 1.851(4) . ? F4 Sb2 1.873(6) . ? F5 Sb2 1.829(5) . ? F6 Sb2 1.859(7) . ? F7 Sb2 1.862(7) . ? Sb1 F2 1.851(4) 7 ? Sb1 F3 1.851(4) 7 ? Sb1 F1 1.867(3) 7 ? Sb2 F5 1.829(5) 7 ? Sb2 F6 1.860(7) 7 ? 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 C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 Ge1 N1 88.42(18) . . ? N2 Ge1 O3 87.95(19) . . ? N1 Ge1 O3 93.72(16) . . ? C3 O1 C5 108.1(4) . . ? C12 O2 C14 108.9(5) . . ? C21 O3 C24 110.1(5) . . ? C21 O3 Ge1 121.7(4) . . ? C24 O3 Ge1 128.2(4) . . ? C3 N1 C4 109.0(4) . . ? C3 N1 Ge1 128.2(4) . . ? C4 N1 Ge1 122.2(3) . . ? C12 N2 C13 109.4(5) . . ? C12 N2 Ge1 128.5(4) . . ? C13 N2 Ge1 120.6(4) . . ? C12 C1 C3 117.0(5) . . ? C12 C1 C2 122.8(6) . . ? C3 C1 C2 120.2(5) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 112.1(5) . . ? N1 C3 C1 128.6(5) . . ? O1 C3 C1 119.2(5) . . ? N1 C4 C6 112.3(4) . . ? N1 C4 C5 100.3(4) . . ? C6 C4 C5 115.2(4) . . ? N1 C4 H4 109.6 . . ? C6 C4 H4 109.6 . . ? C5 C4 H4 109.6 . . ? O1 C5 C4 103.6(4) . . ? O1 C5 H5A 111.0 . . ? C4 C5 H5A 111.0 . . ? O1 C5 H5B 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C11 119.5(6) . . ? C7 C6 C4 120.1(6) . . ? C11 C6 C4 120.3(5) . . ? C6 C7 C8 118.6(7) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 119.6(7) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C8 C9 C10 122.4(7) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C11 118.5(8) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C6 121.3(6) . . ? C10 C11 H11 119.4 . . ? C6 C11 H11 119.4 . . ? N2 C12 O2 112.4(6) . . ? N2 C12 C1 128.4(6) . . ? O2 C12 C1 119.2(5) . . ? N2 C13 C15 113.7(5) . . ? N2 C13 C14 102.8(5) . . ? C15 C13 C14 112.9(5) . . ? N2 C13 H13 109.1 . . ? C15 C13 H13 109.1 . . ? C14 C13 H13 109.1 . . ? O2 C14 C13 104.8(5) . . ? O2 C14 H14A 110.8 . . ? C13 C14 H14A 110.8 . . ? O2 C14 H14B 110.8 . . ? C13 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? C16 C15 C20 119.8(5) . . ? C16 C15 C13 120.1(5) . . ? C20 C15 C13 120.0(5) . . ? C15 C16 C17 119.4(5) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.2(5) . . ? C17 C18 H18 120.4 . . ? C19 C18 H18 120.4 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C15 119.5(5) . . ? C19 C20 H20 120.2 . . ? C15 C20 H20 120.2 . . ? O3 C21 C22 102.8(7) . . ? O3 C21 H21A 111.2 . . ? C22 C21 H21A 111.2 . . ? O3 C21 H21B 111.2 . . ? C22 C21 H21B 111.2 . . ? H21A C21 H21B 109.1 . . ? C25 C22 C23 101.7(10) . . ? C25 C22 C21 115.4(9) . . ? C23 C22 C21 104.7(8) . . ? C25 C22 H22 111.5 . . ? C23 C22 H22 111.5 . . ? C21 C22 H22 111.5 . . ? C26 C23 C24 138.1(14) . . ? C26 C23 C22 93.3(11) . . ? C24 C23 C22 100.6(7) . . ? C26 C23 H23 106.7 . . ? C24 C23 H23 106.7 . . ? C22 C23 H23 106.7 . . ? O3 C24 C23 107.4(7) . . ? O3 C24 H24A 110.2 . . ? C23 C24 H24A 110.2 . . ? O3 C24 H24B 110.2 . . ? C23 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? F2 Sb1 F2 88.8(4) . 7 ? F2 Sb1 F3 91.2(3) . . ? F2 Sb1 F3 178.6(2) 7 . ? F2 Sb1 F3 178.6(2) . 7 ? F2 Sb1 F3 91.2(3) 7 7 ? F3 Sb1 F3 88.9(4) . 7 ? F2 Sb1 F1 88.3(2) . 7 ? F2 Sb1 F1 91.7(2) 7 7 ? F3 Sb1 F1 89.7(2) . 7 ? F3 Sb1 F1 90.3(2) 7 7 ? F2 Sb1 F1 91.7(2) . . ? F2 Sb1 F1 88.3(2) 7 . ? F3 Sb1 F1 90.3(2) . . ? F3 Sb1 F1 89.7(2) 7 . ? F1 Sb1 F1 180.0(3) 7 . ? F5 Sb2 F5 178.6(4) . 7 ? F5 Sb2 F6 92.3(3) . . ? F5 Sb2 F6 87.7(3) 7 . ? F5 Sb2 F6 87.7(3) . 7 ? F5 Sb2 F6 92.3(3) 7 7 ? F6 Sb2 F6 179.3(4) . 7 ? F5 Sb2 F7 89.3(2) . . ? F5 Sb2 F7 89.3(2) 7 . ? F6 Sb2 F7 89.6(2) . . ? F6 Sb2 F7 89.6(2) 7 . ? F5 Sb2 F4 90.7(2) . . ? F5 Sb2 F4 90.7(2) 7 . ? F6 Sb2 F4 90.4(2) . . ? F6 Sb2 F4 90.4(2) 7 . ? F7 Sb2 F4 180.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.144 _refine_diff_density_min -2.101 _refine_diff_density_rms 0.093 #===END data_compound8 _database_code_depnum_ccdc_archive 'CCDC 886109' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H58 F6 Ge2 N4 O12 S2' _chemical_formula_weight 1254.32 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P2(1)2(1)2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.9107(12) _cell_length_b 15.3498(12) _cell_length_c 23.7808(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5442.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.06 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7858 _exptl_absorpt_correction_T_max 0.8327 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker TXS fine-focus rotating anode' _diffrn_radiation_monochromator 'Bruker Helios multilayer confocal mirror' _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 29445 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12250 _reflns_number_gt 10093 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[?^2^(Fo^2^)+(0.0200P)^2^+70.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.025(12) _refine_ls_number_reflns 12250 _refine_ls_number_parameters 783 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1666 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.068 _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 C31A C 0.3827(8) 0.8379(8) 0.8083(4) 0.038(3) Uani 0.60 1 d PGU A 1 C32A C 0.3081(7) 0.7848(8) 0.8010(4) 0.055(3) Uani 0.60 1 d PGU A 1 H32A H 0.2861 0.7732 0.7643 0.066 Uiso 0.60 1 calc PR A 1 C33A C 0.2657(6) 0.7486(6) 0.8475(4) 0.059(3) Uani 0.60 1 d PGU A 1 H33A H 0.2147 0.7123 0.8426 0.071 Uiso 0.60 1 calc PR A 1 C34A C 0.2978(7) 0.7656(6) 0.9013(4) 0.061(4) Uani 0.60 1 d PGU A 1 H34A H 0.2688 0.7408 0.9331 0.073 Uiso 0.60 1 calc PR A 1 C35A C 0.3724(8) 0.8187(8) 0.9085(4) 0.065(4) Uani 0.60 1 d PGU A 1 H35A H 0.3944 0.8303 0.9453 0.078 Uiso 0.60 1 calc PR A 1 C36A C 0.4148(8) 0.8549(8) 0.8620(5) 0.049(4) Uani 0.60 1 d PGU A 1 H36A H 0.4658 0.8912 0.8670 0.058 Uiso 0.60 1 calc PR A 1 C46A C 0.6873(14) 0.8707(9) 0.8575(8) 0.063(5) Uani 0.60 1 d P B 1 H46A H 0.7486 0.8664 0.8418 0.075 Uiso 0.60 1 calc PR B 1 H46B H 0.6563 0.9200 0.8390 0.075 Uiso 0.60 1 calc PR B 1 C47A C 0.6921(13) 0.8863(12) 0.9179(7) 0.095(5) Uani 0.60 1 d P B 1 H47A H 0.7486 0.9160 0.9285 0.114 Uiso 0.60 1 calc PR B 1 H47B H 0.6405 0.9210 0.9314 0.114 Uiso 0.60 1 calc PR B 1 C48A C 0.6893(9) 0.8003(11) 0.9385(5) 0.066(3) Uani 0.60 1 d P B 1 H48A H 0.7514 0.7764 0.9420 0.079 Uiso 0.60 1 calc PR B 1 C49A C 0.6337(10) 0.7436(11) 0.8981(6) 0.067(3) Uani 0.60 1 d P B 1 H49A H 0.6599 0.6845 0.8954 0.081 Uiso 0.60 1 calc PR B 1 H49B H 0.5713 0.7383 0.9120 0.081 Uiso 0.60 1 calc PR B 1 C50A C 0.6409(16) 0.7959(13) 0.9952(10) 0.121(7) Uani 0.60 1 d P B 1 H50A H 0.6402 0.8539 1.0125 0.181 Uiso 0.60 1 calc PR B 1 H50B H 0.6724 0.7551 1.0201 0.181 Uiso 0.60 1 calc PR B 1 H50C H 0.5792 0.7759 0.9895 0.181 Uiso 0.60 1 calc PR B 1 C31B C 0.3914(15) 0.8394(14) 0.8210(7) 0.053(5) Uani 0.40 1 d PGU A 2 C32B C 0.3234(13) 0.7775(12) 0.8237(5) 0.066(6) Uani 0.40 1 d PGU A 2 H32B H 0.2988 0.7542 0.7900 0.080 Uiso 0.40 1 calc PR A 2 C33B C 0.2914(11) 0.7497(9) 0.8756(6) 0.060(5) Uani 0.40 1 d PGU A 2 H33B H 0.2449 0.7074 0.8774 0.072 Uiso 0.40 1 calc PR A 2 C34B C 0.3273(12) 0.7838(10) 0.9248(5) 0.066(5) Uani 0.40 1 d PGU A 2 H34B H 0.3054 0.7648 0.9603 0.079 Uiso 0.40 1 calc PR A 2 C35B C 0.3953(12) 0.8456(13) 0.9222(7) 0.066(5) Uani 0.40 1 d PGU A 2 H35B H 0.4199 0.8689 0.9558 0.079 Uiso 0.40 1 calc PR A 2 C36B C 0.4273(14) 0.8734(14) 0.8703(9) 0.061(5) Uani 0.40 1 d PGU A 2 H36B H 0.4738 0.9157 0.8685 0.073 Uiso 0.40 1 calc PR A 2 C46B C 0.672(2) 0.849(2) 0.8688(13) 0.061(4) Uani 0.40 1 d PU B 2 H46C H 0.6519 0.9034 0.8511 0.074 Uiso 0.40 1 calc PR B 2 H46D H 0.7383 0.8444 0.8647 0.074 Uiso 0.40 1 calc PR B 2 C47B C 0.646(2) 0.8463(16) 0.9319(8) 0.076(4) Uani 0.40 1 d PU B 2 H47C H 0.5860 0.8759 0.9333 0.091 Uiso 0.40 1 calc PR B 2 C48B C 0.6252(18) 0.7543(14) 0.9407(8) 0.075(4) Uani 0.40 1 d PU B 2 H48B H 0.5750 0.7490 0.9677 0.090 Uiso 0.40 1 calc PR B 2 H48C H 0.6782 0.7250 0.9572 0.090 Uiso 0.40 1 calc PR B 2 C49B C 0.5997(17) 0.7085(14) 0.8852(8) 0.065(3) Uani 0.40 1 d PU B 2 H49C H 0.5343 0.6987 0.8817 0.078 Uiso 0.40 1 calc PR B 2 H49D H 0.6324 0.6531 0.8796 0.078 Uiso 0.40 1 calc PR B 2 C50B C 0.7014(14) 0.8969(12) 0.9687(7) 0.067(5) Uani 0.40 1 d P B 2 H50D H 0.6755 0.8970 1.0066 0.100 Uiso 0.40 1 calc PR B 2 H50E H 0.7052 0.9568 0.9547 0.100 Uiso 0.40 1 calc PR B 2 H50F H 0.7616 0.8714 0.9700 0.100 Uiso 0.40 1 calc PR B 2 Ge1 Ge 0.01147(3) 0.66366(4) 0.52752(2) 0.03769(14) Uani 1 1 d . . . Ge2 Ge 0.57511(4) 0.74910(4) 0.76107(3) 0.04405(16) Uani 1 1 d . B . S1 S 0.54696(10) 0.22984(10) 0.87688(6) 0.0462(3) Uani 1 1 d . . . S2 S 0.01114(15) 0.31440(13) 0.63928(11) 0.0764(6) Uani 1 1 d . . . F1 F 0.4949(3) 0.0759(2) 0.90894(17) 0.0707(11) Uani 1 1 d . . . F2 F 0.5785(6) 0.0800(4) 0.8354(4) 0.168(4) Uani 1 1 d . . . F3 F 0.6354(4) 0.1013(6) 0.9142(6) 0.224(7) Uani 1 1 d . . . F4 F 0.0906(5) 0.1648(5) 0.6415(3) 0.130(2) Uani 1 1 d . . . F5 F 0.0593(5) 0.2093(4) 0.5585(2) 0.113(2) Uani 1 1 d . . . F6 F -0.0529(5) 0.1605(4) 0.6150(3) 0.118(2) Uani 1 1 d D . . O1 O 0.2643(2) 0.7350(3) 0.47587(15) 0.0487(10) Uani 1 1 d . . . O2 O 0.1443(3) 0.4528(4) 0.4609(3) 0.086(2) Uani 1 1 d . . . O3 O 0.0608(3) 0.6115(3) 0.60703(17) 0.0561(11) Uani 1 1 d . . . O4 O 0.5015(4) 1.0011(3) 0.72587(16) 0.0609(13) Uani 1 1 d . B . O5 O 0.7942(4) 0.8891(3) 0.7079(3) 0.0792(18) Uani 1 1 d . B . O6 O 0.6345(4) 0.7835(4) 0.84580(18) 0.0629(12) Uani 1 1 d U . . O7 O 0.5334(7) 0.2555(4) 0.9326(3) 0.145(4) Uani 1 1 d . . . O8 O 0.4723(4) 0.2352(6) 0.8425(4) 0.150(4) Uani 1 1 d . . . O9 O 0.6294(3) 0.2611(4) 0.85426(19) 0.0637(13) Uani 1 1 d . . . O10 O 0.0939(5) 0.3526(5) 0.6278(4) 0.136(4) Uani 1 1 d . . . O11 O -0.0245(6) 0.2996(4) 0.6936(3) 0.110(3) Uani 1 1 d . . . O12 O -0.0599(6) 0.3456(5) 0.6026(4) 0.126(3) Uani 1 1 d . . . N1 N 0.1273(3) 0.7131(3) 0.51084(16) 0.0326(9) Uani 1 1 d . . . N2 N 0.0527(3) 0.5570(3) 0.4926(2) 0.0441(11) Uani 1 1 d . . . N3 N 0.5225(3) 0.8635(3) 0.75378(17) 0.0392(10) Uani 1 1 d . . . N4 N 0.6857(3) 0.7949(3) 0.73161(18) 0.0368(9) Uani 1 1 d . . . C1 C 0.2068(4) 0.5946(5) 0.4660(3) 0.0585(18) Uani 1 1 d . . . C2 C 0.2936(5) 0.5637(7) 0.4394(4) 0.095(3) Uani 1 1 d . . . H2A H 0.3084 0.6013 0.4074 0.143 Uiso 1 1 calc R . . H2B H 0.2864 0.5036 0.4263 0.143 Uiso 1 1 calc R . . H2C H 0.3420 0.5664 0.4672 0.143 Uiso 1 1 calc R . . C3 C 0.1964(4) 0.6793(4) 0.4841(2) 0.0419(13) Uani 1 1 d . . . C4 C 0.1427(4) 0.8092(4) 0.5176(2) 0.0365(11) Uani 1 1 d . . . H4 H 0.1125 0.8415 0.4864 0.044 Uiso 1 1 calc R . . C5 C 0.2457(4) 0.8122(4) 0.5094(2) 0.0414(12) Uani 1 1 d . . . H5A H 0.2641 0.8658 0.4893 0.050 Uiso 1 1 calc R . . H5B H 0.2773 0.8096 0.5460 0.050 Uiso 1 1 calc R . . C6 C 0.1098(3) 0.8424(4) 0.5731(2) 0.0404(11) Uani 1 1 d . . . C7 C 0.0406(4) 0.9011(4) 0.5748(3) 0.0511(14) Uani 1 1 d . . . H7 H 0.0138 0.9196 0.5406 0.061 Uiso 1 1 calc R . . C8 C 0.0084(4) 0.9343(5) 0.6258(3) 0.0652(19) Uani 1 1 d . . . H8 H -0.0380 0.9767 0.6264 0.078 Uiso 1 1 calc R . . C9 C 0.0464(5) 0.9035(5) 0.6759(3) 0.0594(17) Uani 1 1 d . . . H9 H 0.0244 0.9238 0.7111 0.071 Uiso 1 1 calc R . . C10 C 0.1147(5) 0.8447(4) 0.6746(3) 0.0554(15) Uani 1 1 d . . . H10 H 0.1403 0.8250 0.7089 0.066 Uiso 1 1 calc R . . C11 C 0.1470(4) 0.8135(4) 0.6251(2) 0.0462(13) Uani 1 1 d . . . H11 H 0.1946 0.7723 0.6251 0.055 Uiso 1 1 calc R . . C12 C 0.1344(4) 0.5382(5) 0.4727(3) 0.0600(17) Uani 1 1 d . . . C13 C -0.0014(4) 0.4764(4) 0.4975(3) 0.0536(15) Uani 1 1 d . . . H13 H -0.0107 0.4615 0.5380 0.064 Uiso 1 1 calc R . . C14 C 0.0606(5) 0.4110(5) 0.4706(5) 0.088(3) Uani 1 1 d . . . H14A H 0.0689 0.3602 0.4957 0.106 Uiso 1 1 calc R . . H14B H 0.0350 0.3902 0.4346 0.106 Uiso 1 1 calc R . . C15 C -0.0915(3) 0.4841(4) 0.4678(2) 0.0399(11) Uani 1 1 d . . . C16 C -0.1676(4) 0.4479(4) 0.4923(2) 0.0411(12) Uani 1 1 d . . . H16 H -0.1641 0.4230 0.5288 0.049 Uiso 1 1 calc R . . C17 C -0.2481(4) 0.4483(4) 0.4637(3) 0.0502(14) Uani 1 1 d . . . H17 H -0.2994 0.4222 0.4804 0.060 Uiso 1 1 calc R . . C18 C -0.2552(4) 0.4859(4) 0.4112(3) 0.0468(13) Uani 1 1 d . . . H18 H -0.3107 0.4854 0.3917 0.056 Uiso 1 1 calc R . . C19 C -0.1811(4) 0.5238(4) 0.3878(3) 0.0509(14) Uani 1 1 d . . . H19 H -0.1858 0.5507 0.3519 0.061 Uiso 1 1 calc R . . C20 C -0.0989(4) 0.5237(4) 0.4157(3) 0.0472(13) Uani 1 1 d . . . H20 H -0.0481 0.5507 0.3991 0.057 Uiso 1 1 calc R . . C21 C 0.0103(6) 0.6200(5) 0.6580(3) 0.069(2) Uani 1 1 d . . . H21A H -0.0519 0.5989 0.6531 0.083 Uiso 1 1 calc R . . H21B H 0.0090 0.6812 0.6712 0.083 Uiso 1 1 calc R . . C22 C 0.0642(9) 0.5605(6) 0.6997(3) 0.091(3) Uani 1 1 d . . . H22 H 0.0407 0.4995 0.6985 0.109 Uiso 1 1 calc R . . C23 C 0.1595(7) 0.5635(7) 0.6776(4) 0.092(3) Uani 1 1 d . . . H23A H 0.1909 0.6170 0.6901 0.111 Uiso 1 1 calc R . . H23B H 0.1942 0.5119 0.6898 0.111 Uiso 1 1 calc R . . C24 C 0.1450(6) 0.5635(6) 0.6160(3) 0.074(2) Uani 1 1 d . . . H24A H 0.1953 0.5927 0.5965 0.088 Uiso 1 1 calc R . . H24B H 0.1398 0.5032 0.6016 0.088 Uiso 1 1 calc R . . C25 C 0.0619(7) 0.5946(7) 0.7582(4) 0.089(3) Uani 1 1 d . . . H25A H 0.0963 0.5557 0.7828 0.134 Uiso 1 1 calc R . . H25B H -0.0003 0.5974 0.7712 0.134 Uiso 1 1 calc R . . H25C H 0.0884 0.6530 0.7591 0.134 Uiso 1 1 calc R . . C26 C 0.6483(5) 0.9471(4) 0.7138(3) 0.0598(18) Uani 1 1 d . . . C27 C 0.6813(8) 1.0373(5) 0.6949(4) 0.095(3) Uani 1 1 d . B . H27A H 0.7348 1.0307 0.6714 0.142 Uiso 1 1 calc R . . H27B H 0.6961 1.0725 0.7280 0.142 Uiso 1 1 calc R . . H27C H 0.6340 1.0664 0.6732 0.142 Uiso 1 1 calc R . . C28 C 0.5606(4) 0.9344(3) 0.7310(2) 0.0435(13) Uani 1 1 d . B . C29 C 0.4256(4) 0.8779(4) 0.7600(2) 0.0457(13) Uani 1 1 d . A . H29 H 0.3957 0.8548 0.7255 0.055 Uiso 1 1 calc R C 1 C30 C 0.4232(5) 0.9771(4) 0.7569(2) 0.0521(15) Uani 1 1 d . . . H30A H 0.3683 0.9971 0.7374 0.062 Uiso 1 1 calc R B . H30B H 0.4245 1.0028 0.7950 0.062 Uiso 1 1 calc R . . C37 C 0.7052(5) 0.8764(4) 0.7170(3) 0.0565(18) Uani 1 1 d . B . C38 C 0.7700(3) 0.7446(4) 0.7370(3) 0.0443(12) Uani 1 1 d . B . H38 H 0.7858 0.7380 0.7776 0.053 Uiso 1 1 calc R . . C39 C 0.8377(5) 0.8049(4) 0.7082(4) 0.070(2) Uani 1 1 d . . . H39A H 0.8947 0.8071 0.7295 0.084 Uiso 1 1 calc R B . H39B H 0.8504 0.7851 0.6694 0.084 Uiso 1 1 calc R . . C40 C 0.7665(3) 0.6548(3) 0.7089(2) 0.0356(10) Uani 1 1 d . . . C41 C 0.8037(4) 0.5841(4) 0.7353(2) 0.0411(11) Uani 1 1 d . B . H41 H 0.8258 0.5901 0.7726 0.049 Uiso 1 1 calc R . . C42 C 0.8097(4) 0.5037(4) 0.7084(3) 0.0446(13) Uani 1 1 d . . . H42 H 0.8377 0.4559 0.7268 0.054 Uiso 1 1 calc R B . C43 C 0.7746(4) 0.4933(4) 0.6546(2) 0.0413(12) Uani 1 1 d . B . H43 H 0.7785 0.4387 0.6359 0.050 Uiso 1 1 calc R . . C44 C 0.7337(4) 0.5642(4) 0.6285(2) 0.0446(13) Uani 1 1 d . . . H44 H 0.7082 0.5575 0.5922 0.054 Uiso 1 1 calc R B . C45 C 0.7298(4) 0.6440(4) 0.6550(2) 0.0412(12) Uani 1 1 d . B . H45 H 0.7021 0.6919 0.6366 0.049 Uiso 1 1 calc R . . C51 C 0.5678(6) 0.1163(5) 0.8882(4) 0.0683(19) Uani 1 1 d . . . C52 C 0.0368(8) 0.2164(9) 0.6112(4) 0.182(10) Uani 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 C31A 0.034(5) 0.032(5) 0.049(6) 0.012(5) 0.004(5) 0.013(4) C32A 0.057(7) 0.036(5) 0.071(8) -0.003(6) 0.021(6) 0.008(5) C33A 0.057(6) 0.034(5) 0.087(8) -0.003(6) 0.025(6) 0.003(5) C34A 0.086(9) 0.030(6) 0.068(9) 0.010(6) 0.028(7) 0.003(6) C35A 0.072(9) 0.077(9) 0.046(7) 0.011(6) 0.022(6) 0.023(7) C36A 0.044(6) 0.059(7) 0.043(8) 0.009(6) 0.008(5) 0.018(5) C46A 0.082(12) 0.039(8) 0.067(11) -0.008(6) -0.044(9) 0.004(7) C47A 0.096(12) 0.107(13) 0.082(10) -0.031(9) 0.008(9) -0.039(11) C48A 0.056(7) 0.092(11) 0.050(6) -0.017(6) -0.006(5) -0.006(7) C49A 0.071(8) 0.072(9) 0.059(8) -0.004(7) -0.015(6) 0.007(7) C50A 0.119(16) 0.089(12) 0.155(18) 0.013(12) 0.050(14) 0.001(12) C31B 0.059(10) 0.068(10) 0.033(8) -0.024(8) -0.008(7) 0.044(9) C32B 0.096(13) 0.039(9) 0.063(10) -0.015(9) -0.007(10) 0.026(9) C33B 0.092(12) 0.028(7) 0.060(11) -0.009(9) 0.001(9) 0.012(9) C34B 0.079(12) 0.054(10) 0.065(11) -0.005(9) -0.011(9) 0.034(9) C35B 0.059(10) 0.091(13) 0.048(9) -0.003(9) -0.008(7) 0.047(9) C36B 0.065(11) 0.086(12) 0.031(8) -0.021(8) -0.008(8) 0.032(9) C46B 0.074(8) 0.063(8) 0.047(7) 0.030(7) -0.001(6) 0.018(7) C47B 0.099(9) 0.069(8) 0.059(7) 0.018(7) -0.003(7) 0.002(8) C48B 0.110(9) 0.063(7) 0.053(7) 0.019(6) -0.003(7) -0.007(8) C49B 0.093(8) 0.055(7) 0.046(6) 0.016(6) -0.008(6) 0.000(7) C50B 0.093(14) 0.063(11) 0.044(8) 0.008(8) -0.022(9) 0.004(10) Ge1 0.0213(2) 0.0449(3) 0.0468(3) -0.0060(2) -0.0016(2) 0.0001(2) Ge2 0.0323(3) 0.0248(2) 0.0751(4) -0.0058(3) 0.0096(2) 0.0010(2) S1 0.0428(7) 0.0464(9) 0.0494(7) 0.0048(6) 0.0065(6) 0.0050(6) S2 0.0581(11) 0.0535(10) 0.1175(17) -0.0097(10) 0.0053(11) 0.0055(9) F1 0.076(3) 0.051(2) 0.085(3) 0.0072(19) 0.016(2) -0.013(2) F2 0.211(9) 0.086(4) 0.206(8) -0.074(5) 0.133(7) -0.026(5) F3 0.053(3) 0.158(7) 0.460(18) 0.190(10) -0.048(6) 0.012(4) F4 0.131(6) 0.102(4) 0.156(6) 0.003(4) -0.017(4) 0.069(5) F5 0.113(5) 0.125(5) 0.102(4) -0.027(3) 0.014(3) 0.024(4) F6 0.115(5) 0.090(4) 0.150(5) 0.011(4) -0.027(4) -0.048(4) O1 0.0353(19) 0.076(3) 0.0353(17) -0.0026(19) 0.0055(15) -0.0105(19) O2 0.045(3) 0.060(3) 0.154(6) -0.050(4) 0.012(3) -0.002(2) O3 0.044(2) 0.081(3) 0.043(2) 0.014(2) 0.0111(18) -0.002(2) O4 0.082(3) 0.052(2) 0.049(2) 0.0197(18) 0.018(2) 0.030(3) O5 0.064(3) 0.035(2) 0.138(5) 0.006(3) 0.052(3) -0.005(2) O6 0.071(3) 0.069(3) 0.049(2) 0.021(2) -0.005(2) 0.013(3) O7 0.239(11) 0.075(4) 0.122(5) -0.038(4) 0.130(6) -0.044(5) O8 0.068(4) 0.209(9) 0.172(7) 0.154(7) -0.065(4) -0.056(5) O9 0.051(3) 0.079(3) 0.062(3) 0.003(2) -0.002(2) -0.025(3) O10 0.072(4) 0.093(5) 0.243(10) -0.055(6) 0.042(6) -0.035(4) O11 0.161(8) 0.076(4) 0.093(4) -0.017(3) 0.025(5) 0.017(5) O12 0.103(5) 0.113(6) 0.164(7) 0.049(5) 0.003(5) 0.059(5) N1 0.029(2) 0.041(2) 0.0276(18) -0.0024(16) 0.0013(15) -0.0020(18) N2 0.025(2) 0.050(3) 0.057(3) -0.014(2) -0.0038(19) 0.0005(19) N3 0.041(2) 0.036(2) 0.040(2) -0.0026(17) 0.0019(18) 0.0157(19) N4 0.041(2) 0.025(2) 0.045(2) 0.0005(17) 0.0084(19) 0.0015(17) C1 0.035(3) 0.079(5) 0.061(4) -0.032(4) 0.010(3) -0.004(3) C2 0.046(4) 0.108(7) 0.132(8) -0.064(6) 0.036(5) -0.006(4) C3 0.032(2) 0.061(4) 0.033(2) -0.003(2) 0.0049(19) -0.006(2) C4 0.034(3) 0.043(3) 0.033(2) 0.007(2) -0.0032(19) -0.005(2) C5 0.033(3) 0.052(3) 0.040(3) 0.010(2) -0.001(2) -0.004(2) C6 0.034(2) 0.041(3) 0.047(3) 0.002(2) -0.002(2) -0.013(2) C7 0.028(3) 0.068(4) 0.057(3) -0.003(3) -0.004(2) 0.000(3) C8 0.027(3) 0.078(5) 0.091(5) -0.029(4) 0.000(3) -0.003(3) C9 0.045(3) 0.069(5) 0.064(4) -0.017(3) 0.014(3) -0.022(3) C10 0.068(4) 0.051(4) 0.047(3) -0.008(3) 0.000(3) -0.013(3) C11 0.053(3) 0.045(3) 0.040(3) -0.001(2) -0.004(2) -0.008(3) C12 0.035(3) 0.072(4) 0.073(4) -0.029(4) 0.002(3) 0.004(3) C13 0.036(3) 0.040(3) 0.085(4) -0.010(3) -0.009(3) 0.000(3) C14 0.040(4) 0.057(4) 0.168(9) -0.036(5) -0.014(5) 0.004(3) C15 0.030(2) 0.038(3) 0.052(3) -0.012(2) 0.008(2) -0.001(2) C16 0.039(3) 0.032(3) 0.051(3) -0.002(2) 0.009(2) 0.001(2) C17 0.035(3) 0.045(3) 0.071(4) -0.007(3) 0.007(3) -0.007(2) C18 0.032(3) 0.040(3) 0.069(4) -0.002(3) -0.008(3) 0.009(2) C19 0.043(3) 0.057(4) 0.053(3) -0.004(3) -0.003(3) 0.003(3) C20 0.032(3) 0.051(3) 0.058(3) -0.001(3) 0.005(2) -0.002(2) C21 0.078(5) 0.082(5) 0.048(3) 0.003(3) 0.014(3) -0.030(4) C22 0.163(10) 0.066(5) 0.043(4) 0.003(3) -0.007(5) 0.010(6) C23 0.096(7) 0.084(6) 0.097(6) -0.013(5) -0.029(6) 0.029(6) C24 0.069(5) 0.073(5) 0.079(5) 0.027(4) -0.015(4) 0.017(4) C25 0.073(6) 0.112(7) 0.082(5) -0.008(5) 0.002(5) -0.007(5) C26 0.080(5) 0.034(3) 0.066(4) 0.014(3) 0.027(3) 0.012(3) C27 0.120(8) 0.038(4) 0.126(7) 0.033(4) 0.059(6) 0.010(4) C28 0.061(4) 0.033(3) 0.036(3) 0.004(2) 0.011(2) 0.014(2) C29 0.043(3) 0.056(3) 0.038(3) -0.010(2) -0.005(2) 0.016(3) C30 0.060(4) 0.052(3) 0.044(3) 0.001(2) 0.004(3) 0.030(3) C37 0.065(4) 0.030(3) 0.074(4) 0.002(3) 0.036(3) -0.001(3) C38 0.029(2) 0.035(3) 0.069(3) -0.001(3) 0.007(2) 0.001(2) C39 0.053(4) 0.025(3) 0.131(7) 0.004(3) 0.036(4) -0.002(3) C40 0.024(2) 0.034(3) 0.049(3) 0.000(2) 0.0109(19) -0.004(2) C41 0.034(3) 0.041(3) 0.048(3) 0.003(2) -0.006(2) -0.008(2) C42 0.045(3) 0.026(3) 0.063(3) 0.016(2) -0.007(3) 0.003(2) C43 0.043(3) 0.029(3) 0.052(3) 0.003(2) 0.008(2) -0.002(2) C44 0.053(3) 0.049(3) 0.032(2) 0.007(2) 0.000(2) 0.000(3) C45 0.042(3) 0.039(3) 0.042(3) 0.012(2) 0.007(2) 0.008(2) C51 0.062(5) 0.045(4) 0.098(5) 0.001(4) 0.012(4) 0.006(3) C52 0.215(15) 0.271(19) 0.060(5) 0.032(8) 0.026(7) 0.219(16) _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 C31A C32A 1.3900 . ? C31A C36A 1.3900 . ? C31A C29 1.450(9) . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.3900 . ? C33A H33A 0.9500 . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A H36A 0.9500 . ? C46A C47A 1.46(2) . ? C46A O6 1.577(16) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47A C48A 1.41(2) . ? C47A H47A 0.9900 . ? C47A H47B 0.9900 . ? C48A C50A 1.53(2) . ? C48A C49A 1.538(19) . ? C48A H48A 1.0000 . ? C49A O6 1.386(15) . ? C49A H49A 0.9900 . ? C49A H49B 0.9900 . ? C50A H50A 0.9800 . ? C50A H50B 0.9800 . ? C50A H50C 0.9800 . ? C31B C32B 1.3900 . ? C31B C36B 1.3900 . ? C31B C29 1.649(14) . ? C32B C33B 1.3900 . ? C32B H32B 0.9500 . ? C33B C34B 1.3900 . ? C33B H33B 0.9500 . ? C34B C35B 1.3900 . ? C34B H34B 0.9500 . ? C35B C36B 1.3900 . ? C35B H35B 0.9500 . ? C36B H36B 0.9500 . ? C46B O6 1.27(4) . ? C46B C47B 1.55(4) . ? C46B H46C 0.9900 . ? C46B H46D 0.9900 . ? C47B C50B 1.44(3) . ? C47B C48B 1.46(3) . ? C47B H47C 1.0000 . ? C48B C49B 1.54(3) . ? C48B H48B 0.9900 . ? C48B H48C 0.9900 . ? C49B O6 1.574(19) . ? C49B H49C 0.9900 . ? C49B H49D 0.9900 . ? C50B H50D 0.9800 . ? C50B H50E 0.9800 . ? C50B H50F 0.9800 . ? Ge1 N1 1.928(4) . ? Ge1 N2 1.937(5) . ? Ge1 O3 2.181(4) . ? Ge2 N4 1.924(4) . ? Ge2 N3 1.931(4) . ? Ge2 O6 2.264(5) . ? S1 O8 1.383(5) . ? S1 O7 1.397(6) . ? S1 O9 1.425(5) . ? S1 C51 1.791(7) . ? S2 O10 1.394(7) . ? S2 O11 1.415(7) . ? S2 O12 1.454(8) . ? S2 C52 1.689(12) . ? F1 C51 1.345(9) . ? F2 C51 1.382(11) . ? F3 C51 1.206(11) . ? F4 C52 1.339(10) . ? F5 C52 1.304(10) . ? F6 C52 1.590(15) . ? O1 C3 1.339(7) . ? O1 C5 1.455(7) . ? O2 C12 1.348(8) . ? O2 C14 1.422(9) . ? O3 C21 1.433(8) . ? O3 C24 1.471(9) . ? O4 C28 1.356(7) . ? O4 C30 1.430(8) . ? O5 C37 1.359(9) . ? O5 C39 1.446(8) . ? N1 C3 1.318(7) . ? N1 C4 1.502(7) . ? N2 C12 1.337(7) . ? N2 C13 1.481(8) . ? N3 C28 1.342(7) . ? N3 C29 1.468(7) . ? N4 C37 1.331(7) . ? N4 C38 1.480(7) . ? C1 C3 1.379(9) . ? C1 C12 1.393(9) . ? C1 C2 1.517(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C4 C6 1.497(7) . ? C4 C5 1.549(7) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.371(8) . ? C6 C11 1.426(8) . ? C7 C8 1.399(9) . ? C7 H7 0.9500 . ? C8 C9 1.403(11) . ? C8 H8 0.9500 . ? C9 C10 1.361(10) . ? C9 H9 0.9500 . ? C10 C11 1.359(9) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C13 C14 1.506(9) . ? C13 C15 1.523(8) . ? C13 H13 1.0000 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.384(9) . ? C15 C16 1.390(8) . ? C16 C17 1.381(8) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 H17 0.9500 . ? C18 C19 1.367(9) . ? C18 H18 0.9500 . ? C19 C20 1.394(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.568(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C25 1.486(11) . ? C22 C23 1.515(16) . ? C22 H22 1.0000 . ? C23 C24 1.482(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C37 1.380(9) . ? C26 C28 1.385(10) . ? C26 C27 1.537(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.525(9) . ? C29 H29 1.0000 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C38 C40 1.532(8) . ? C38 C39 1.532(8) . ? C38 H38 1.0000 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.371(8) . ? C40 C45 1.405(8) . ? C41 C42 1.394(8) . ? C41 H41 0.9500 . ? C42 C43 1.393(8) . ? C42 H42 0.9500 . ? C43 C44 1.393(8) . ? C43 H43 0.9500 . ? C44 C45 1.378(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? 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 C32A C31A C36A 120.0 . . ? C32A C31A C29 120.2(7) . . ? C36A C31A C29 119.8(8) . . ? C33A C32A C31A 120.0 . . ? C33A C32A H32A 120.0 . . ? C31A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A H33A 120.0 . . ? C32A C33A H33A 120.0 . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C36A C35A C34A 120.0 . . ? C36A C35A H35A 120.0 . . ? C34A C35A H35A 120.0 . . ? C35A C36A C31A 120.0 . . ? C35A C36A H36A 120.0 . . ? C31A C36A H36A 120.0 . . ? C47A C46A O6 109.8(13) . . ? C47A C46A H46A 109.7 . . ? O6 C46A H46A 109.7 . . ? C47A C46A H46B 109.7 . . ? O6 C46A H46B 109.7 . . ? H46A C46A H46B 108.2 . . ? C48A C47A C46A 100.7(12) . . ? C48A C47A H47A 111.6 . . ? C46A C47A H47A 111.6 . . ? C48A C47A H47B 111.6 . . ? C46A C47A H47B 111.6 . . ? H47A C47A H47B 109.4 . . ? C47A C48A C50A 111.1(14) . . ? C47A C48A C49A 109.2(12) . . ? C50A C48A C49A 105.8(14) . . ? C47A C48A H48A 110.2 . . ? C50A C48A H48A 110.2 . . ? C49A C48A H48A 110.2 . . ? O6 C49A C48A 107.8(12) . . ? O6 C49A H49A 110.1 . . ? C48A C49A H49A 110.1 . . ? O6 C49A H49B 110.1 . . ? C48A C49A H49B 110.1 . . ? H49A C49A H49B 108.5 . . ? C32B C31B C36B 120.0 . . ? C32B C31B C29 120.7(13) . . ? C36B C31B C29 119.2(13) . . ? C31B C32B C33B 120.0 . . ? C31B C32B H32B 120.0 . . ? C33B C32B H32B 120.0 . . ? C34B C33B C32B 120.0 . . ? C34B C33B H33B 120.0 . . ? C32B C33B H33B 120.0 . . ? C33B C34B C35B 120.0 . . ? C33B C34B H34B 120.0 . . ? C35B C34B H34B 120.0 . . ? C34B C35B C36B 120.0 . . ? C34B C35B H35B 120.0 . . ? C36B C35B H35B 120.0 . . ? C35B C36B C31B 120.0 . . ? C35B C36B H36B 120.0 . . ? C31B C36B H36B 120.0 . . ? O6 C46B C47B 106(2) . . ? O6 C46B H46C 110.4 . . ? C47B C46B H46C 110.4 . . ? O6 C46B H46D 110.4 . . ? C47B C46B H46D 110.4 . . ? H46C C46B H46D 108.6 . . ? C50B C47B C48B 123.9(19) . . ? C50B C47B C46B 115(2) . . ? C48B C47B C46B 102(2) . . ? C50B C47B H47C 104.5 . . ? C48B C47B H47C 104.5 . . ? C46B C47B H47C 104.5 . . ? C47B C48B C49B 111.8(16) . . ? C47B C48B H48B 109.3 . . ? C49B C48B H48B 109.3 . . ? C47B C48B H48C 109.3 . . ? C49B C48B H48C 109.3 . . ? H48B C48B H48C 107.9 . . ? C48B C49B O6 95.4(14) . . ? C48B C49B H49C 112.7 . . ? O6 C49B H49C 112.7 . . ? C48B C49B H49D 112.7 . . ? O6 C49B H49D 112.7 . . ? H49C C49B H49D 110.2 . . ? C47B C50B H50D 109.5 . . ? C47B C50B H50E 109.5 . . ? H50D C50B H50E 109.5 . . ? C47B C50B H50F 109.5 . . ? H50D C50B H50F 109.5 . . ? H50E C50B H50F 109.5 . . ? N1 Ge1 N2 87.69(19) . . ? N1 Ge1 O3 91.17(17) . . ? N2 Ge1 O3 87.4(2) . . ? N4 Ge2 N3 89.06(19) . . ? N4 Ge2 O6 84.47(19) . . ? N3 Ge2 O6 91.53(18) . . ? O8 S1 O7 115.3(7) . . ? O8 S1 O9 116.8(3) . . ? O7 S1 O9 112.8(4) . . ? O8 S1 C51 106.6(5) . . ? O7 S1 C51 99.0(4) . . ? O9 S1 C51 103.6(4) . . ? O10 S2 O11 125.4(6) . . ? O10 S2 O12 112.9(6) . . ? O11 S2 O12 109.1(5) . . ? O10 S2 C52 95.6(6) . . ? O11 S2 C52 107.6(5) . . ? O12 S2 C52 102.8(5) . . ? C3 O1 C5 107.2(4) . . ? C12 O2 C14 108.0(5) . . ? C21 O3 C24 111.8(5) . . ? C21 O3 Ge1 121.5(4) . . ? C24 O3 Ge1 126.7(4) . . ? C28 O4 C30 106.8(4) . . ? C37 O5 C39 108.0(5) . . ? C46B O6 C49A 88.0(13) . . ? C46B O6 C49B 117.8(14) . . ? C49A O6 C49B 30.6(8) . . ? C46B O6 C46A 15.3(16) . . ? C49A O6 C46A 102.7(10) . . ? C49B O6 C46A 132.9(11) . . ? C46B O6 Ge2 137.8(11) . . ? C49A O6 Ge2 133.8(8) . . ? C49B O6 Ge2 103.3(9) . . ? C46A O6 Ge2 123.4(7) . . ? C3 N1 C4 108.6(4) . . ? C3 N1 Ge1 130.2(4) . . ? C4 N1 Ge1 120.1(3) . . ? C12 N2 C13 110.1(5) . . ? C12 N2 Ge1 128.5(4) . . ? C13 N2 Ge1 120.0(4) . . ? C28 N3 C29 109.6(4) . . ? C28 N3 Ge2 127.0(4) . . ? C29 N3 Ge2 121.9(4) . . ? C37 N4 C38 109.1(5) . . ? C37 N4 Ge2 128.7(4) . . ? C38 N4 Ge2 120.3(3) . . ? C3 C1 C12 117.7(5) . . ? C3 C1 C2 121.3(6) . . ? C12 C1 C2 121.0(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 O1 114.2(5) . . ? N1 C3 C1 127.5(5) . . ? O1 C3 C1 118.2(5) . . ? C6 C4 N1 112.3(4) . . ? C6 C4 C5 115.2(4) . . ? N1 C4 C5 99.6(4) . . ? C6 C4 H4 109.8 . . ? N1 C4 H4 109.8 . . ? C5 C4 H4 109.8 . . ? O1 C5 C4 103.5(4) . . ? O1 C5 H5A 111.1 . . ? C4 C5 H5A 111.1 . . ? O1 C5 H5B 111.1 . . ? C4 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? C7 C6 C11 118.1(5) . . ? C7 C6 C4 119.8(5) . . ? C11 C6 C4 122.1(5) . . ? C6 C7 C8 121.6(6) . . ? C6 C7 H7 119.2 . . ? C8 C7 H7 119.2 . . ? C7 C8 C9 118.4(6) . . ? C7 C8 H8 120.8 . . ? C9 C8 H8 120.8 . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 121.2(7) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C6 120.3(6) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? N2 C12 O2 112.5(6) . . ? N2 C12 C1 127.7(6) . . ? O2 C12 C1 119.7(6) . . ? N2 C13 C14 100.9(5) . . ? N2 C13 C15 112.3(5) . . ? C14 C13 C15 113.3(6) . . ? N2 C13 H13 110.0 . . ? C14 C13 H13 110.0 . . ? C15 C13 H13 110.0 . . ? O2 C14 C13 107.8(6) . . ? O2 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O2 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.5 . . ? C20 C15 C16 119.0(5) . . ? C20 C15 C13 121.3(5) . . ? C16 C15 C13 119.7(5) . . ? C17 C16 C15 120.1(5) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.9(5) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C19 C18 C17 119.1(6) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 121.0(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C15 C20 C19 119.8(6) . . ? C15 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? O3 C21 C22 102.2(7) . . ? O3 C21 H21A 111.3 . . ? C22 C21 H21A 111.3 . . ? O3 C21 H21B 111.3 . . ? C22 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C25 C22 C23 109.5(9) . . ? C25 C22 C21 112.0(8) . . ? C23 C22 C21 104.2(7) . . ? C25 C22 H22 110.3 . . ? C23 C22 H22 110.3 . . ? C21 C22 H22 110.3 . . ? C24 C23 C22 101.8(7) . . ? C24 C23 H23A 111.4 . . ? C22 C23 H23A 111.4 . . ? C24 C23 H23B 111.4 . . ? C22 C23 H23B 111.4 . . ? H23A C23 H23B 109.3 . . ? O3 C24 C23 105.5(7) . . ? O3 C24 H24A 110.6 . . ? C23 C24 H24A 110.6 . . ? O3 C24 H24B 110.6 . . ? C23 C24 H24B 110.6 . . ? H24A C24 H24B 108.8 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C37 C26 C28 117.0(6) . . ? C37 C26 C27 121.9(7) . . ? C28 C26 C27 121.1(6) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 O4 112.0(5) . . ? N3 C28 C26 129.4(5) . . ? O4 C28 C26 118.7(5) . . ? C31A C29 N3 116.8(7) . . ? C31A C29 C30 116.8(7) . . ? N3 C29 C30 99.8(5) . . ? C31A C29 C31B 9.8(11) . . ? N3 C29 C31B 109.8(9) . . ? C30 C29 C31B 113.2(9) . . ? C31A C29 H29 107.6 . . ? N3 C29 H29 107.6 . . ? C30 C29 H29 107.6 . . ? C31B C29 H29 117.2 . . ? O4 C30 C29 105.3(5) . . ? O4 C30 H30A 110.7 . . ? C29 C30 H30A 110.7 . . ? O4 C30 H30B 110.7 . . ? C29 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? N4 C37 O5 112.9(6) . . ? N4 C37 C26 128.3(6) . . ? O5 C37 C26 118.7(6) . . ? N4 C38 C40 113.7(4) . . ? N4 C38 C39 101.9(5) . . ? C40 C38 C39 111.8(5) . . ? N4 C38 H38 109.7 . . ? C40 C38 H38 109.7 . . ? C39 C38 H38 109.7 . . ? O5 C39 C38 104.3(5) . . ? O5 C39 H39A 110.9 . . ? C38 C39 H39A 110.9 . . ? O5 C39 H39B 110.9 . . ? C38 C39 H39B 110.9 . . ? H39A C39 H39B 108.9 . . ? C41 C40 C45 118.8(5) . . ? C41 C40 C38 119.9(5) . . ? C45 C40 C38 121.2(5) . . ? C40 C41 C42 121.2(5) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C43 C42 C41 119.9(5) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 119.0(5) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C45 C44 C43 120.7(5) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C40 120.4(5) . . ? C44 C45 H45 119.8 . . ? C40 C45 H45 119.8 . . ? F3 C51 F1 113.5(8) . . ? F3 C51 F2 107.0(10) . . ? F1 C51 F2 103.9(7) . . ? F3 C51 S1 114.1(7) . . ? F1 C51 S1 111.3(5) . . ? F2 C51 S1 106.1(6) . . ? F5 C52 F4 108.3(7) . . ? F5 C52 F6 103.0(10) . . ? F4 C52 F6 98.9(10) . . ? F5 C52 S2 120.9(9) . . ? F4 C52 S2 116.8(9) . . ? F6 C52 S2 105.5(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.083 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.091