data_{Sn{OSiPh3}2}2 _audit_creation_date 2013-04-23T14:27:53-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C72 H60 O4 Si4 Sn2' _chemical_formula_sum 'C72 H60 O4 Si4 Sn2' _chemical_formula_weight 1338.94 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1634(5) _cell_length_b 14.7460(6) _cell_length_c 22.1742(10) _cell_angle_alpha 83.641(2) _cell_angle_beta 89.206(2) _cell_angle_gamma 70.997(2) _cell_volume 3429.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7968 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.86 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.943 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.190 0.337 0.208 217 33 ' ' 2 -0.190 0.663 0.792 217 33 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_unetI/netI 0.0708 _diffrn_reflns_number 34505 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 15524 _reflns_number_gt 11114 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^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_number_reflns 15524 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0947 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.793 _refine_diff_density_min -0.66 _refine_diff_density_rms 0.102 _iucr_refine_instructions_details ; .res file for SHELXL : sqz.res ................................................................. TITL import in P -1 CELL 0.71073 11.1634 14.7460 22.1742 83.641 89.206 70.997 ZERR 2.00 0.0005 0.0006 0.0010 0.002 0.002 0.002 LATT 1 SFAC C H O SI SN UNIT 144 120 8 8 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.042900 FVAR 2.90813 MOLE 1 SN1 5 0.418775 0.128197 0.668238 11.00000 0.02319 0.02369 = 0.02160 -0.00274 0.00097 -0.00736 O1 3 0.239155 0.184008 0.637643 11.00000 0.02619 0.03487 = 0.02940 -0.00274 -0.00567 -0.01204 SI1 4 0.126812 0.196351 0.589169 11.00000 0.02364 0.02377 = 0.02224 -0.00095 -0.00194 -0.00941 C1 1 0.036126 0.113239 0.617195 11.00000 0.02297 0.02556 = 0.03072 0.00380 -0.00429 -0.00625 C2 1 0.025582 0.039170 0.585427 11.00000 0.03505 0.03193 = 0.03629 0.00277 -0.00766 -0.01550 AFIX 43 H2 2 0.062024 0.031419 0.546577 11.00000 -1.20000 AFIX 0 C3 1 -0.037688 -0.023567 0.609932 11.00000 0.04878 0.04104 = 0.05518 0.00523 -0.01062 -0.02884 AFIX 43 H3 2 -0.043940 -0.073612 0.587899 11.00000 -1.20000 AFIX 0 C4 1 -0.090428 -0.012581 0.665654 11.00000 0.04275 0.04624 = 0.06464 0.01859 -0.00464 -0.02441 AFIX 43 H4 2 -0.133513 -0.055320 0.682048 11.00000 -1.20000 AFIX 0 C5 1 -0.082467 0.059372 0.698705 11.00000 0.03692 0.04992 = 0.04289 0.00951 0.00594 -0.01706 AFIX 43 H5 2 -0.119474 0.066425 0.737474 11.00000 -1.20000 AFIX 0 C6 1 -0.018833 0.121537 0.673896 11.00000 0.03103 0.03566 = 0.03536 -0.00013 -0.00273 -0.00860 AFIX 43 H6 2 -0.012863 0.171102 0.696455 11.00000 -1.20000 AFIX 0 C7 1 0.192004 0.165764 0.512750 11.00000 0.02762 0.02552 = 0.02449 -0.00092 -0.00069 -0.01563 C8 1 0.147229 0.227792 0.459568 11.00000 0.03537 0.02724 = 0.02972 0.00107 -0.00490 -0.01322 AFIX 43 H8 2 0.077997 0.285542 0.461428 11.00000 -1.20000 AFIX 0 C9 1 0.202301 0.206377 0.404045 11.00000 0.05352 0.04046 = 0.02314 0.00218 -0.00179 -0.02722 AFIX 43 H9 2 0.170172 0.249649 0.368560 11.00000 -1.20000 AFIX 0 C10 1 0.303111 0.123031 0.399766 11.00000 0.05092 0.04690 = 0.03029 -0.01380 0.00812 -0.03015 AFIX 43 H10 2 0.341460 0.109233 0.361856 11.00000 -1.20000 AFIX 0 C11 1 0.347272 0.059882 0.451862 11.00000 0.03897 0.03693 = 0.03960 -0.01508 0.01052 -0.01774 AFIX 43 H11 2 0.415022 0.001351 0.449667 11.00000 -1.20000 AFIX 0 C12 1 0.292519 0.082187 0.507163 11.00000 0.03099 0.03101 = 0.03277 -0.00216 -0.00093 -0.01330 AFIX 43 H12 2 0.325048 0.038639 0.542491 11.00000 -1.20000 AFIX 0 C13 1 0.020527 0.324382 0.581673 11.00000 0.02946 0.02479 = 0.02268 -0.00020 0.00027 -0.01181 C14 1 0.062810 0.397773 0.599125 11.00000 0.03428 0.03182 = 0.02786 -0.00196 -0.00510 -0.01171 AFIX 43 H14 2 0.145276 0.381549 0.616701 11.00000 -1.20000 AFIX 0 C15 1 -0.014156 0.493566 0.591054 11.00000 0.04936 0.03141 = 0.04072 -0.00530 -0.00203 -0.01900 AFIX 43 H15 2 0.017176 0.542029 0.602474 11.00000 -1.20000 AFIX 0 C16 1 -0.133744 0.519480 0.567078 11.00000 0.04303 0.02316 = 0.03921 -0.00201 -0.00006 -0.00614 AFIX 43 H16 2 -0.186053 0.585232 0.562453 11.00000 -1.20000 AFIX 0 C17 1 -0.178112 0.448751 0.549527 11.00000 0.02793 0.03214 = 0.04435 -0.00060 -0.00533 -0.00164 AFIX 43 H17 2 -0.261264 0.466040 0.532562 11.00000 -1.20000 AFIX 0 C18 1 -0.102251 0.353415 0.556547 11.00000 0.02731 0.02745 = 0.03318 -0.00227 0.00080 -0.01081 AFIX 43 H18 2 -0.134211 0.305996 0.543965 11.00000 -1.20000 AFIX 0 SI2 4 0.363205 0.026582 0.804638 11.00000 0.02402 0.02237 = 0.02176 0.00195 -0.00182 -0.00905 O2 3 0.341429 0.127954 0.758999 11.00000 0.03021 0.02142 = 0.02133 0.00008 0.00177 -0.00970 C21 1 0.387704 -0.071193 0.754028 11.00000 0.02647 0.02205 = 0.01916 0.00241 -0.00306 -0.00672 C22 1 0.293071 -0.069178 0.712809 11.00000 0.02612 0.02752 = 0.03196 0.00049 -0.00724 -0.00325 AFIX 43 H22 2 0.214087 -0.018527 0.711085 11.00000 -1.20000 AFIX 0 C23 1 0.313841 -0.141263 0.674046 11.00000 0.03902 0.04134 = 0.02720 -0.00256 -0.01029 -0.01105 AFIX 43 H23 2 0.249064 -0.138490 0.645872 11.00000 -1.20000 AFIX 0 C24 1 0.427450 -0.216543 0.676185 11.00000 0.04807 0.03101 = 0.02639 -0.00668 -0.00018 -0.01345 AFIX 43 H24 2 0.440279 -0.265604 0.650061 11.00000 -1.20000 AFIX 0 C25 1 0.521393 -0.219600 0.716431 11.00000 0.03126 0.02570 = 0.03943 -0.00184 0.00320 -0.00543 AFIX 43 H25 2 0.599910 -0.270730 0.718071 11.00000 -1.20000 AFIX 0 C26 1 0.501546 -0.147518 0.754984 11.00000 0.02844 0.02983 = 0.02801 0.00245 -0.00507 -0.01051 AFIX 43 H26 2 0.567394 -0.150569 0.782610 11.00000 -1.20000 AFIX 0 C27 1 0.221636 0.037643 0.852709 11.00000 0.02278 0.02819 = 0.02281 0.00178 -0.00042 -0.00638 C28 1 0.160744 -0.031830 0.857869 11.00000 0.03056 0.03769 = 0.04234 -0.00449 0.00457 -0.01512 AFIX 43 H28 2 0.191363 -0.086735 0.836285 11.00000 -1.20000 AFIX 0 C29 1 0.056014 -0.021483 0.894189 11.00000 0.03248 0.04681 = 0.05606 -0.00131 0.00355 -0.01788 AFIX 43 H29 2 0.015664 -0.069396 0.897206 11.00000 -1.20000 AFIX 0 C30 1 0.009979 0.057235 0.925837 11.00000 0.02871 0.06008 = 0.03742 0.00419 0.00718 -0.00826 AFIX 43 H30 2 -0.062071 0.063680 0.950414 11.00000 -1.20000 AFIX 0 C31 1 0.068702 0.127436 0.921935 11.00000 0.04574 0.04339 = 0.02984 -0.00503 0.01076 -0.00762 AFIX 43 H31 2 0.036416 0.182595 0.943173 11.00000 -1.20000 AFIX 0 C32 1 0.175510 0.115949 0.886497 11.00000 0.04265 0.03334 = 0.03062 -0.00205 0.00567 -0.01454 AFIX 43 H32 2 0.218001 0.162420 0.885262 11.00000 -1.20000 AFIX 0 C33 1 0.508458 0.000500 0.853913 11.00000 0.02721 0.02362 = 0.02594 -0.00091 -0.00275 -0.00966 C34 1 0.517608 -0.048018 0.912353 11.00000 0.03001 0.03505 = 0.02542 0.00119 -0.00293 -0.01025 AFIX 43 H34 2 0.447297 -0.065017 0.928137 11.00000 -1.20000 AFIX 0 C35 1 0.627709 -0.071983 0.947957 11.00000 0.04155 0.03935 = 0.02786 0.00284 -0.00627 -0.00877 AFIX 43 H35 2 0.632020 -0.104657 0.987683 11.00000 -1.20000 AFIX 0 C36 1 0.730187 -0.048062 0.925259 11.00000 0.03483 0.04935 = 0.03658 -0.00200 -0.01095 -0.01431 AFIX 43 H36 2 0.805552 -0.064356 0.949315 11.00000 -1.20000 AFIX 0 C37 1 0.723465 0.000190 0.866839 11.00000 0.03109 0.05402 = 0.04470 0.00354 -0.00242 -0.02208 AFIX 43 H37 2 0.794098 0.016821 0.851139 11.00000 -1.20000 AFIX 0 C38 1 0.614288 0.023472 0.832209 11.00000 0.03701 0.04553 = 0.02497 0.00625 -0.00845 -0.02090 AFIX 43 H38 2 0.610693 0.056024 0.792490 11.00000 -1.20000 AFIX 0 SN2 5 0.237990 0.279955 0.759093 11.00000 0.02151 0.02453 = 0.02266 -0.00158 0.00033 -0.00665 O51 3 0.341335 0.291384 0.830540 11.00000 0.02847 0.03394 = 0.02992 -0.01027 0.00119 -0.01045 SI11 4 0.318695 0.359893 0.884861 11.00000 0.02671 0.02855 = 0.02396 -0.00479 -0.00087 -0.00985 C51 1 0.169260 0.362763 0.925546 11.00000 0.02665 0.02914 = 0.02979 -0.00800 0.00252 -0.00831 C52 1 0.051598 0.396789 0.894682 11.00000 0.03204 0.04938 = 0.02562 -0.00390 -0.00018 -0.01071 AFIX 43 H52 2 0.048159 0.418281 0.852543 11.00000 -1.20000 AFIX 0 C53 1 -0.060325 0.399905 0.924170 11.00000 0.02708 0.05741 = 0.04460 -0.01483 -0.00352 -0.00826 AFIX 43 H53 2 -0.138200 0.421601 0.901674 11.00000 -1.20000 AFIX 0 C54 1 -0.059571 0.371998 0.985394 11.00000 0.03164 0.06025 = 0.03843 -0.01100 0.00882 -0.01236 AFIX 43 H54 2 -0.136382 0.375746 1.005573 11.00000 -1.20000 AFIX 0 C55 1 0.054071 0.338632 1.016852 11.00000 0.04399 0.07382 = 0.03140 -0.00536 0.00714 -0.01746 AFIX 43 H55 2 0.055842 0.318919 1.059189 11.00000 -1.20000 AFIX 0 C56 1 0.167300 0.333246 0.987456 11.00000 0.03015 0.06190 = 0.02713 -0.00046 -0.00194 -0.01441 AFIX 43 H56 2 0.244887 0.308883 1.010180 11.00000 -1.20000 AFIX 0 C57 1 0.458049 0.312571 0.939388 11.00000 0.02871 0.03132 = 0.02400 -0.00061 -0.00026 -0.01507 C58 1 0.539237 0.218103 0.943831 11.00000 0.03181 0.03966 = 0.03315 -0.00403 0.00236 -0.01442 AFIX 43 H58 2 0.524262 0.174912 0.918421 11.00000 -1.20000 AFIX 0 C59 1 0.642594 0.184671 0.984711 11.00000 0.03225 0.03471 = 0.04052 0.00683 0.00040 -0.00440 AFIX 43 H59 2 0.696713 0.119556 0.986700 11.00000 -1.20000 AFIX 0 C60 1 0.666119 0.245722 1.022017 11.00000 0.04188 0.04459 = 0.04720 0.00477 -0.01724 -0.01762 AFIX 43 H60 2 0.736064 0.223049 1.049944 11.00000 -1.20000 AFIX 0 C61 1 0.587932 0.339364 1.018558 11.00000 0.06341 0.05108 = 0.06246 -0.00752 -0.02786 -0.02592 AFIX 43 H61 2 0.603996 0.381983 1.044084 11.00000 -1.20000 AFIX 0 C62 1 0.484594 0.372896 0.977788 11.00000 0.04842 0.03155 = 0.05870 -0.00539 -0.02200 -0.00818 AFIX 43 H62 2 0.431188 0.438177 0.976143 11.00000 -1.20000 AFIX 0 C63 1 0.307324 0.486471 0.855546 11.00000 0.03345 0.02750 = 0.02196 -0.00230 -0.00185 -0.00681 C64 1 0.206913 0.567608 0.864724 11.00000 0.04344 0.03724 = 0.03621 -0.00577 0.00093 -0.01247 AFIX 43 H64 2 0.136317 0.559731 0.886408 11.00000 -1.20000 AFIX 0 C65 1 0.204884 0.661172 0.843344 11.00000 0.05132 0.03345 = 0.04764 -0.00814 -0.00446 -0.00346 AFIX 43 H65 2 0.134752 0.715402 0.851232 11.00000 -1.20000 AFIX 0 C66 1 0.304577 0.673865 0.811041 11.00000 0.06500 0.03134 = 0.04679 0.00362 -0.00506 -0.01746 AFIX 43 H66 2 0.303221 0.737017 0.795837 11.00000 -1.20000 AFIX 0 C67 1 0.406779 0.595224 0.800566 11.00000 0.06055 0.04104 = 0.06808 0.00637 0.01644 -0.01917 AFIX 43 H67 2 0.475484 0.604033 0.777665 11.00000 -1.20000 AFIX 0 C68 1 0.409693 0.502432 0.823550 11.00000 0.04714 0.03409 = 0.06152 -0.00060 0.01485 -0.00991 AFIX 43 H68 2 0.482351 0.448925 0.817456 11.00000 -1.20000 AFIX 0 O71 3 0.392064 0.272000 0.696369 11.00000 0.02521 0.02499 = 0.02053 -0.00110 0.00190 -0.01151 SI12 4 0.478425 0.335379 0.664220 11.00000 0.02624 0.02987 = 0.02021 -0.00062 -0.00055 -0.01438 C71 1 0.616898 0.321895 0.715299 11.00000 0.02896 0.03527 = 0.02374 -0.00493 0.00037 -0.01418 C72 1 0.634614 0.269821 0.772759 11.00000 0.03155 0.03543 = 0.03274 -0.00272 -0.00085 -0.01122 AFIX 43 H72 2 0.573635 0.241133 0.787711 11.00000 -1.20000 AFIX 0 C73 1 0.740514 0.259546 0.808279 11.00000 0.03342 0.05584 = 0.02952 -0.00157 -0.00844 -0.01170 AFIX 43 H73 2 0.750864 0.224307 0.847477 11.00000 -1.20000 AFIX 0 C74 1 0.830935 0.299757 0.787487 11.00000 0.03129 0.07868 = 0.03854 -0.02414 -0.00411 -0.01871 AFIX 43 H74 2 0.903771 0.291554 0.811902 11.00000 -1.20000 AFIX 0 C75 1 0.814761 0.351799 0.731140 11.00000 0.04108 0.08209 = 0.04585 -0.01849 0.00515 -0.04135 AFIX 43 H75 2 0.877246 0.379049 0.716357 11.00000 -1.20000 AFIX 0 C76 1 0.707104 0.364930 0.695433 11.00000 0.04903 0.06552 = 0.02995 -0.00217 -0.00030 -0.03831 AFIX 43 H76 2 0.695078 0.403450 0.657307 11.00000 -1.20000 AFIX 0 C77 1 0.380795 0.463965 0.642503 11.00000 0.03262 0.02879 = 0.03251 -0.00189 -0.00588 -0.01751 C78 1 0.283096 0.516229 0.676388 11.00000 0.04387 0.03229 = 0.06361 -0.00139 0.00784 -0.01239 AFIX 43 H78 2 0.262070 0.485650 0.713073 11.00000 -1.20000 AFIX 0 C79 1 0.215189 0.611648 0.658416 11.00000 0.04302 0.04037 = 0.10557 -0.02564 0.01465 -0.00922 AFIX 43 H79 2 0.149329 0.645965 0.683038 11.00000 -1.20000 AFIX 0 C80 1 0.242266 0.657476 0.605003 11.00000 0.06431 0.02686 = 0.08777 0.00254 -0.03189 -0.01752 AFIX 43 H80 2 0.193770 0.722541 0.591888 11.00000 -1.20000 AFIX 0 C81 1 0.339382 0.608187 0.571383 11.00000 0.09125 0.03224 = 0.04474 0.00719 -0.01963 -0.02606 AFIX 43 H81 2 0.360273 0.639680 0.535023 11.00000 -1.20000 AFIX 0 C82 1 0.407972 0.513078 0.589359 11.00000 0.06474 0.03471 = 0.03592 -0.00185 0.00185 -0.02414 AFIX 43 H82 2 0.475376 0.480115 0.565016 11.00000 -1.20000 AFIX 0 C83 1 0.533751 0.279418 0.592368 11.00000 0.03077 0.02839 = 0.01948 0.00110 0.00216 -0.01682 C84 1 0.657439 0.219379 0.584075 11.00000 0.03075 0.03392 = 0.02616 0.00630 -0.00399 -0.01362 AFIX 43 H84 2 0.720646 0.211521 0.614278 11.00000 -1.20000 AFIX 0 C85 1 0.690276 0.171146 0.533138 11.00000 0.03565 0.03264 = 0.03700 0.00146 0.00219 -0.00827 AFIX 43 H85 2 0.775261 0.131582 0.528307 11.00000 -1.20000 AFIX 0 C86 1 0.598868 0.180802 0.489336 11.00000 0.05243 0.02619 = 0.02946 -0.00369 0.00148 -0.01400 AFIX 43 H86 2 0.620737 0.146435 0.454816 11.00000 -1.20000 AFIX 0 C87 1 0.475410 0.240324 0.495424 11.00000 0.03677 0.03537 = 0.02680 -0.00043 -0.00610 -0.01660 AFIX 43 H87 2 0.413102 0.247575 0.464882 11.00000 -1.20000 AFIX 0 C88 1 0.443269 0.289283 0.546370 11.00000 0.02675 0.03136 = 0.02772 -0.00299 -0.00074 -0.01232 AFIX 43 H88 2 0.358626 0.330215 0.550268 11.00000 -1.20000 HKLF 4 REM import in P -1 REM R1 = 0.0422 for 11114 Fo > 4sig(Fo) and 0.0645 for all 15524 data REM 739 parameters refined using 0 restraints END WGHT 0.0429 0.0000 REM Highest difference peak 0.79, deepest hole -0.66, 1-sigma level 0.10 Q1 1 0.1013 0.3140 0.8124 11.00000 0.05 0.79 Q2 1 0.4016 0.0210 0.4220 11.00000 0.05 0.76 Q3 1 0.2273 0.2699 0.7130 11.00000 0.05 0.55 Q4 1 -0.0849 0.4652 0.9042 11.00000 0.05 0.54 Q5 1 0.1619 0.2802 0.8507 11.00000 0.05 0.48 Q6 1 0.5042 0.2230 0.7886 11.00000 0.05 0.46 Q7 1 0.3178 0.0510 0.4918 11.00000 0.05 0.43 Q8 1 0.4215 0.4098 0.6520 11.00000 0.05 0.42 Q9 1 0.0354 0.4402 0.5803 11.00000 0.05 0.42 Q10 1 -0.1436 0.4872 1.0217 11.00000 0.05 0.41 Q11 1 0.2985 0.3826 0.6221 11.00000 0.05 0.41 Q12 1 0.9431 0.3508 0.6813 11.00000 0.05 0.40 Q13 1 0.1930 0.1628 0.5607 11.00000 0.05 0.40 Q14 1 0.4635 0.0393 0.8386 11.00000 0.05 0.39 Q15 1 0.1837 0.2128 0.5292 11.00000 0.05 0.39 Q16 1 0.2072 0.4025 0.9838 11.00000 0.05 0.39 Q17 1 0.6539 0.1810 0.5719 11.00000 0.05 0.38 Q18 1 0.6223 0.3639 0.9870 11.00000 0.05 0.38 Q19 1 -0.0852 -0.0463 0.6704 11.00000 0.05 0.38 Q20 1 0.7793 -0.2596 0.8389 11.00000 0.05 0.38 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 0.41877(2) 0.128197(17) 0.668238(10) 0.02289(7) Uani 1 1 d . . . O1 O 0.2392(2) 0.18401(17) 0.63764(10) 0.0296(6) Uani 1 1 d . . . Si1 Si 0.12681(9) 0.19635(7) 0.58917(4) 0.0229(2) Uani 1 1 d . . . C1 C 0.0361(3) 0.1132(2) 0.61719(15) 0.0273(8) Uani 1 1 d . . . C2 C 0.0256(4) 0.0392(3) 0.58543(17) 0.0337(9) Uani 1 1 d . . . H2 H 0.062 0.0314 0.5466 0.04 Uiso 1 1 calc R . . C3 C -0.0377(4) -0.0236(3) 0.6099(2) 0.0456(11) Uani 1 1 d . . . H3 H -0.0439 -0.0736 0.5879 0.055 Uiso 1 1 calc R . . C4 C -0.0904(4) -0.0126(3) 0.6657(2) 0.0507(12) Uani 1 1 d . . . H4 H -0.1335 -0.0553 0.682 0.061 Uiso 1 1 calc R . . C5 C -0.0825(4) 0.0594(3) 0.69871(19) 0.0437(11) Uani 1 1 d . . . H5 H -0.1195 0.0664 0.7375 0.052 Uiso 1 1 calc R . . C6 C -0.0188(4) 0.1215(3) 0.67390(17) 0.0348(9) Uani 1 1 d . . . H6 H -0.0129 0.1711 0.6965 0.042 Uiso 1 1 calc R . . C7 C 0.1920(3) 0.1658(2) 0.51275(14) 0.0243(8) Uani 1 1 d . . . C8 C 0.1472(4) 0.2278(3) 0.45957(15) 0.0303(8) Uani 1 1 d . . . H8 H 0.078 0.2855 0.4614 0.036 Uiso 1 1 calc R . . C9 C 0.2023(4) 0.2064(3) 0.40404(16) 0.0366(10) Uani 1 1 d . . . H9 H 0.1702 0.2496 0.3686 0.044 Uiso 1 1 calc R . . C10 C 0.3031(4) 0.1230(3) 0.39977(17) 0.0386(10) Uani 1 1 d . . . H10 H 0.3415 0.1092 0.3619 0.046 Uiso 1 1 calc R . . C11 C 0.3473(4) 0.0599(3) 0.45186(17) 0.0364(9) Uani 1 1 d . . . H11 H 0.415 0.0014 0.4497 0.044 Uiso 1 1 calc R . . C12 C 0.2925(4) 0.0822(3) 0.50716(16) 0.0309(8) Uani 1 1 d . . . H12 H 0.325 0.0386 0.5425 0.037 Uiso 1 1 calc R . . C13 C 0.0205(3) 0.3244(2) 0.58167(14) 0.0251(8) Uani 1 1 d . . . C14 C 0.0628(4) 0.3978(3) 0.59913(15) 0.0311(8) Uani 1 1 d . . . H14 H 0.1453 0.3815 0.6167 0.037 Uiso 1 1 calc R . . C15 C -0.0142(4) 0.4936(3) 0.59105(17) 0.0389(10) Uani 1 1 d . . . H15 H 0.0172 0.542 0.6025 0.047 Uiso 1 1 calc R . . C16 C -0.1337(4) 0.5195(3) 0.56708(16) 0.0364(9) Uani 1 1 d . . . H16 H -0.1861 0.5852 0.5625 0.044 Uiso 1 1 calc R . . C17 C -0.1781(4) 0.4488(3) 0.54953(17) 0.0370(9) Uani 1 1 d . . . H17 H -0.2613 0.466 0.5326 0.044 Uiso 1 1 calc R . . C18 C -0.1023(3) 0.3534(3) 0.55655(15) 0.0289(8) Uani 1 1 d . . . H18 H -0.1342 0.306 0.544 0.035 Uiso 1 1 calc R . . Si2 Si 0.36320(9) 0.02658(7) 0.80464(4) 0.0227(2) Uani 1 1 d . . . O2 O 0.3414(2) 0.12795(16) 0.75900(9) 0.0242(5) Uani 1 1 d . . . C21 C 0.3877(3) -0.0712(2) 0.75403(14) 0.0232(7) Uani 1 1 d . . . C22 C 0.2931(3) -0.0692(3) 0.71281(15) 0.0301(8) Uani 1 1 d . . . H22 H 0.2141 -0.0185 0.7111 0.036 Uiso 1 1 calc R . . C23 C 0.3138(4) -0.1413(3) 0.67405(16) 0.0363(9) Uani 1 1 d . . . H23 H 0.2491 -0.1385 0.6459 0.044 Uiso 1 1 calc R . . C24 C 0.4274(4) -0.2165(3) 0.67618(16) 0.0347(9) Uani 1 1 d . . . H24 H 0.4403 -0.2656 0.6501 0.042 Uiso 1 1 calc R . . C25 C 0.5214(4) -0.2196(3) 0.71643(16) 0.0332(9) Uani 1 1 d . . . H25 H 0.5999 -0.2707 0.7181 0.04 Uiso 1 1 calc R . . C26 C 0.5015(3) -0.1475(3) 0.75498(15) 0.0289(8) Uani 1 1 d . . . H26 H 0.5674 -0.1506 0.7826 0.035 Uiso 1 1 calc R . . C27 C 0.2216(3) 0.0376(2) 0.85271(15) 0.0254(8) Uani 1 1 d . . . C28 C 0.1607(4) -0.0318(3) 0.85787(17) 0.0359(9) Uani 1 1 d . . . H28 H 0.1914 -0.0867 0.8363 0.043 Uiso 1 1 calc R . . C29 C 0.0560(4) -0.0215(3) 0.89419(19) 0.0443(11) Uani 1 1 d . . . H29 H 0.0157 -0.0694 0.8972 0.053 Uiso 1 1 calc R . . C30 C 0.0100(4) 0.0572(3) 0.92584(18) 0.0444(11) Uani 1 1 d . . . H30 H -0.0621 0.0637 0.9504 0.053 Uiso 1 1 calc R . . C31 C 0.0687(4) 0.1274(3) 0.92193(17) 0.0414(10) Uani 1 1 d . . . H31 H 0.0364 0.1826 0.9432 0.05 Uiso 1 1 calc R . . C32 C 0.1755(4) 0.1159(3) 0.88650(16) 0.0352(9) Uani 1 1 d . . . H32 H 0.218 0.1624 0.8853 0.042 Uiso 1 1 calc R . . C33 C 0.5085(3) 0.0005(2) 0.85391(15) 0.0254(8) Uani 1 1 d . . . C34 C 0.5176(4) -0.0480(3) 0.91235(15) 0.0306(8) Uani 1 1 d . . . H34 H 0.4473 -0.065 0.9281 0.037 Uiso 1 1 calc R . . C35 C 0.6277(4) -0.0720(3) 0.94796(16) 0.0378(10) Uani 1 1 d . . . H35 H 0.632 -0.1047 0.9877 0.045 Uiso 1 1 calc R . . C36 C 0.7302(4) -0.0481(3) 0.92526(17) 0.0402(10) Uani 1 1 d . . . H36 H 0.8056 -0.0644 0.9493 0.048 Uiso 1 1 calc R . . C37 C 0.7235(4) 0.0002(3) 0.86684(18) 0.0419(10) Uani 1 1 d . . . H37 H 0.7941 0.0168 0.8511 0.05 Uiso 1 1 calc R . . C38 C 0.6143(4) 0.0235(3) 0.83221(16) 0.0347(9) Uani 1 1 d . . . H38 H 0.6107 0.056 0.7925 0.042 Uiso 1 1 calc R . . Sn2 Sn 0.23799(2) 0.279955(17) 0.759093(10) 0.02319(7) Uani 1 1 d . . . O51 O 0.3413(2) 0.29138(18) 0.83054(10) 0.0302(6) Uani 1 1 d . . . Si11 Si 0.31870(9) 0.35989(7) 0.88486(4) 0.0260(2) Uani 1 1 d . . . C51 C 0.1693(3) 0.3628(3) 0.92555(16) 0.0284(8) Uani 1 1 d . . . C52 C 0.0516(4) 0.3968(3) 0.89468(16) 0.0363(9) Uani 1 1 d . . . H52 H 0.0482 0.4183 0.8525 0.044 Uiso 1 1 calc R . . C53 C -0.0603(4) 0.3999(3) 0.92417(18) 0.0436(10) Uani 1 1 d . . . H53 H -0.1382 0.4216 0.9017 0.052 Uiso 1 1 calc R . . C54 C -0.0596(4) 0.3720(3) 0.98539(18) 0.0437(10) Uani 1 1 d . . . H54 H -0.1364 0.3757 1.0056 0.052 Uiso 1 1 calc R . . C55 C 0.0541(4) 0.3386(3) 1.01685(19) 0.0503(12) Uani 1 1 d . . . H55 H 0.0558 0.3189 1.0592 0.06 Uiso 1 1 calc R . . C56 C 0.1673(4) 0.3332(3) 0.98746(16) 0.0402(10) Uani 1 1 d . . . H56 H 0.2449 0.3089 1.0102 0.048 Uiso 1 1 calc R . . C57 C 0.4580(3) 0.3126(3) 0.93939(15) 0.0269(8) Uani 1 1 d . . . C58 C 0.5392(4) 0.2181(3) 0.94383(16) 0.0342(9) Uani 1 1 d . . . H58 H 0.5243 0.1749 0.9184 0.041 Uiso 1 1 calc R . . C59 C 0.6426(4) 0.1847(3) 0.98471(17) 0.0383(9) Uani 1 1 d . . . H59 H 0.6967 0.1196 0.9867 0.046 Uiso 1 1 calc R . . C60 C 0.6661(4) 0.2457(3) 1.02202(18) 0.0443(11) Uani 1 1 d . . . H60 H 0.7361 0.223 1.0499 0.053 Uiso 1 1 calc R . . C61 C 0.5879(5) 0.3394(3) 1.0186(2) 0.0568(13) Uani 1 1 d . . . H61 H 0.604 0.382 1.0441 0.068 Uiso 1 1 calc R . . C62 C 0.4846(4) 0.3729(3) 0.97779(19) 0.0472(11) Uani 1 1 d . . . H62 H 0.4312 0.4382 0.9761 0.057 Uiso 1 1 calc R . . C63 C 0.3073(4) 0.4865(3) 0.85555(15) 0.0284(8) Uani 1 1 d . . . C64 C 0.2069(4) 0.5676(3) 0.86472(17) 0.0390(10) Uani 1 1 d . . . H64 H 0.1363 0.5597 0.8864 0.047 Uiso 1 1 calc R . . C65 C 0.2049(4) 0.6612(3) 0.84334(18) 0.0463(11) Uani 1 1 d . . . H65 H 0.1348 0.7154 0.8512 0.056 Uiso 1 1 calc R . . C66 C 0.3046(5) 0.6739(3) 0.81104(19) 0.0479(11) Uani 1 1 d . . . H66 H 0.3032 0.737 0.7958 0.057 Uiso 1 1 calc R . . C67 C 0.4068(5) 0.5952(3) 0.8006(2) 0.0571(13) Uani 1 1 d . . . H67 H 0.4755 0.604 0.7777 0.068 Uiso 1 1 calc R . . C68 C 0.4097(4) 0.5024(3) 0.82355(19) 0.0489(11) Uani 1 1 d . . . H68 H 0.4824 0.4489 0.8175 0.059 Uiso 1 1 calc R . . O71 O 0.3921(2) 0.27200(16) 0.69637(9) 0.0229(5) Uani 1 1 d . . . Si12 Si 0.47842(9) 0.33538(7) 0.66422(4) 0.0243(2) Uani 1 1 d . . . C71 C 0.6169(3) 0.3219(3) 0.71530(15) 0.0283(8) Uani 1 1 d . . . C72 C 0.6346(4) 0.2698(3) 0.77276(16) 0.0332(9) Uani 1 1 d . . . H72 H 0.5736 0.2411 0.7877 0.04 Uiso 1 1 calc R . . C73 C 0.7405(4) 0.2595(3) 0.80828(17) 0.0405(10) Uani 1 1 d . . . H73 H 0.7509 0.2243 0.8475 0.049 Uiso 1 1 calc R . . C74 C 0.8309(4) 0.2998(3) 0.78749(18) 0.0479(12) Uani 1 1 d . . . H74 H 0.9038 0.2916 0.8119 0.057 Uiso 1 1 calc R . . C75 C 0.8148(4) 0.3518(4) 0.73114(19) 0.0503(12) Uani 1 1 d . . . H75 H 0.8772 0.379 0.7164 0.06 Uiso 1 1 calc R . . C76 C 0.7071(4) 0.3649(3) 0.69543(17) 0.0436(11) Uani 1 1 d . . . H76 H 0.6951 0.4034 0.6573 0.052 Uiso 1 1 calc R . . C77 C 0.3808(4) 0.4640(3) 0.64250(16) 0.0295(8) Uani 1 1 d . . . C78 C 0.2831(4) 0.5162(3) 0.6764(2) 0.0470(11) Uani 1 1 d . . . H78 H 0.2621 0.4856 0.7131 0.056 Uiso 1 1 calc R . . C79 C 0.2152(5) 0.6116(3) 0.6584(3) 0.0628(14) Uani 1 1 d . . . H79 H 0.1493 0.646 0.683 0.075 Uiso 1 1 calc R . . C80 C 0.2423(5) 0.6575(3) 0.6050(2) 0.0594(15) Uani 1 1 d . . . H80 H 0.1938 0.7225 0.5919 0.071 Uiso 1 1 calc R . . C81 C 0.3394(5) 0.6082(3) 0.5714(2) 0.0553(14) Uani 1 1 d . . . H81 H 0.3603 0.6397 0.535 0.066 Uiso 1 1 calc R . . C82 C 0.4080(4) 0.5131(3) 0.58936(17) 0.0434(11) Uani 1 1 d . . . H82 H 0.4754 0.4801 0.565 0.052 Uiso 1 1 calc R . . C83 C 0.5338(3) 0.2794(3) 0.59237(14) 0.0248(8) Uani 1 1 d . . . C84 C 0.6574(4) 0.2194(3) 0.58408(16) 0.0302(8) Uani 1 1 d . . . H84 H 0.7206 0.2115 0.6143 0.036 Uiso 1 1 calc R . . C85 C 0.6903(4) 0.1711(3) 0.53314(16) 0.0362(9) Uani 1 1 d . . . H85 H 0.7753 0.1316 0.5283 0.043 Uiso 1 1 calc R . . C86 C 0.5989(4) 0.1808(3) 0.48934(16) 0.0357(9) Uani 1 1 d . . . H86 H 0.6207 0.1464 0.4548 0.043 Uiso 1 1 calc R . . C87 C 0.4754(4) 0.2403(3) 0.49542(16) 0.0320(9) Uani 1 1 d . . . H87 H 0.4131 0.2476 0.4649 0.038 Uiso 1 1 calc R . . C88 C 0.4433(3) 0.2893(3) 0.54637(15) 0.0279(8) Uani 1 1 d . . . H88 H 0.3586 0.3302 0.5503 0.034 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 0.02319(13) 0.02369(13) 0.02160(13) -0.00274(9) 0.00097(10) -0.00736(11) O1 0.0262(14) 0.0349(15) 0.0294(13) -0.0027(11) -0.0057(11) -0.0120(12) Si1 0.0236(5) 0.0238(5) 0.0222(5) -0.0010(4) -0.0019(4) -0.0094(4) C1 0.0230(19) 0.026(2) 0.0307(19) 0.0038(15) -0.0043(16) -0.0062(16) C2 0.035(2) 0.032(2) 0.036(2) 0.0028(17) -0.0077(18) -0.0155(19) C3 0.049(3) 0.041(3) 0.055(3) 0.005(2) -0.011(2) -0.029(2) C4 0.043(3) 0.046(3) 0.065(3) 0.019(2) -0.005(2) -0.024(2) C5 0.037(2) 0.050(3) 0.043(2) 0.010(2) 0.006(2) -0.017(2) C6 0.031(2) 0.036(2) 0.035(2) -0.0001(17) -0.0027(18) -0.0086(19) C7 0.0276(19) 0.0255(19) 0.0245(18) -0.0009(14) -0.0007(15) -0.0156(17) C8 0.035(2) 0.027(2) 0.030(2) 0.0011(15) -0.0049(17) -0.0132(18) C9 0.054(3) 0.040(2) 0.0231(19) 0.0022(17) -0.0018(18) -0.027(2) C10 0.051(3) 0.047(3) 0.030(2) -0.0138(19) 0.0081(19) -0.030(2) C11 0.039(2) 0.037(2) 0.040(2) -0.0151(18) 0.0105(19) -0.018(2) C12 0.031(2) 0.031(2) 0.033(2) -0.0022(16) -0.0009(17) -0.0133(18) C13 0.029(2) 0.0248(19) 0.0227(17) -0.0002(14) 0.0003(15) -0.0118(16) C14 0.034(2) 0.032(2) 0.0279(19) -0.0020(16) -0.0051(16) -0.0117(18) C15 0.049(3) 0.031(2) 0.041(2) -0.0053(18) -0.002(2) -0.019(2) C16 0.043(2) 0.023(2) 0.039(2) -0.0020(16) -0.0001(19) -0.0061(19) C17 0.028(2) 0.032(2) 0.044(2) -0.0006(18) -0.0053(18) -0.0016(18) C18 0.027(2) 0.027(2) 0.033(2) -0.0023(15) 0.0008(16) -0.0108(17) Si2 0.0240(5) 0.0224(5) 0.0218(5) 0.0020(4) -0.0018(4) -0.0091(4) O2 0.0302(13) 0.0214(13) 0.0213(12) 0.0001(9) 0.0018(10) -0.0097(11) C21 0.0265(19) 0.0220(18) 0.0192(17) 0.0024(14) -0.0031(15) -0.0067(16) C22 0.026(2) 0.028(2) 0.032(2) 0.0005(16) -0.0072(16) -0.0033(17) C23 0.039(2) 0.041(2) 0.027(2) -0.0026(17) -0.0103(18) -0.011(2) C24 0.048(3) 0.031(2) 0.026(2) -0.0067(16) -0.0002(18) -0.013(2) C25 0.031(2) 0.026(2) 0.039(2) -0.0018(16) 0.0032(18) -0.0054(17) C26 0.028(2) 0.030(2) 0.0280(19) 0.0024(15) -0.0051(16) -0.0105(17) C27 0.0228(18) 0.028(2) 0.0228(18) 0.0018(14) -0.0004(15) -0.0064(16) C28 0.031(2) 0.038(2) 0.042(2) -0.0045(18) 0.0046(18) -0.0151(19) C29 0.032(2) 0.047(3) 0.056(3) -0.001(2) 0.004(2) -0.018(2) C30 0.029(2) 0.060(3) 0.037(2) 0.004(2) 0.0072(19) -0.008(2) C31 0.046(3) 0.043(3) 0.030(2) -0.0050(18) 0.0108(19) -0.008(2) C32 0.043(2) 0.033(2) 0.031(2) -0.0021(16) 0.0057(18) -0.015(2) C33 0.0272(19) 0.0236(19) 0.0259(18) -0.0009(14) -0.0027(15) -0.0097(16) C34 0.030(2) 0.035(2) 0.0254(19) 0.0012(16) -0.0029(16) -0.0102(18) C35 0.042(2) 0.039(2) 0.028(2) 0.0028(17) -0.0063(18) -0.009(2) C36 0.035(2) 0.049(3) 0.037(2) -0.0020(19) -0.0109(19) -0.014(2) C37 0.031(2) 0.054(3) 0.045(2) 0.004(2) -0.0024(19) -0.022(2) C38 0.037(2) 0.046(2) 0.0250(19) 0.0063(17) -0.0085(17) -0.021(2) Sn2 0.02151(13) 0.02453(14) 0.02266(13) -0.00158(9) 0.00033(10) -0.00665(11) O51 0.0285(14) 0.0339(15) 0.0299(13) -0.0103(11) 0.0012(11) -0.0104(12) Si11 0.0267(5) 0.0286(6) 0.0240(5) -0.0048(4) -0.0009(4) -0.0098(5) C51 0.027(2) 0.029(2) 0.0298(19) -0.0080(15) 0.0025(16) -0.0083(17) C52 0.032(2) 0.049(3) 0.026(2) -0.0039(17) -0.0002(17) -0.011(2) C53 0.027(2) 0.057(3) 0.045(3) -0.015(2) -0.0035(19) -0.008(2) C54 0.032(2) 0.060(3) 0.038(2) -0.011(2) 0.0088(19) -0.012(2) C55 0.044(3) 0.074(3) 0.031(2) -0.005(2) 0.007(2) -0.017(3) C56 0.030(2) 0.062(3) 0.027(2) -0.0005(19) -0.0019(17) -0.014(2) C57 0.029(2) 0.031(2) 0.0240(18) -0.0006(15) -0.0003(15) -0.0151(17) C58 0.032(2) 0.040(2) 0.033(2) -0.0040(17) 0.0024(17) -0.0144(19) C59 0.032(2) 0.035(2) 0.041(2) 0.0068(18) 0.0004(18) -0.0044(19) C60 0.042(3) 0.045(3) 0.047(3) 0.005(2) -0.017(2) -0.018(2) C61 0.063(3) 0.051(3) 0.062(3) -0.008(2) -0.028(3) -0.026(3) C62 0.048(3) 0.032(2) 0.059(3) -0.005(2) -0.022(2) -0.008(2) C63 0.033(2) 0.028(2) 0.0220(18) -0.0023(15) -0.0019(16) -0.0068(17) C64 0.043(3) 0.037(2) 0.036(2) -0.0058(18) 0.0009(19) -0.012(2) C65 0.051(3) 0.033(2) 0.048(3) -0.0081(19) -0.004(2) -0.003(2) C66 0.065(3) 0.031(2) 0.047(3) 0.0036(19) -0.005(2) -0.017(2) C67 0.061(3) 0.041(3) 0.068(3) 0.006(2) 0.016(3) -0.019(3) C68 0.047(3) 0.034(2) 0.062(3) -0.001(2) 0.015(2) -0.010(2) O71 0.0252(13) 0.0250(13) 0.0205(12) -0.0011(9) 0.0019(10) -0.0115(11) Si12 0.0262(5) 0.0299(6) 0.0202(5) -0.0006(4) -0.0006(4) -0.0144(5) C71 0.029(2) 0.035(2) 0.0237(18) -0.0049(15) 0.0004(15) -0.0142(18) C72 0.032(2) 0.035(2) 0.033(2) -0.0027(17) -0.0009(17) -0.0112(19) C73 0.033(2) 0.056(3) 0.030(2) -0.0016(19) -0.0084(18) -0.012(2) C74 0.031(2) 0.079(4) 0.039(2) -0.024(2) -0.0041(19) -0.019(2) C75 0.041(3) 0.082(4) 0.046(3) -0.018(2) 0.005(2) -0.041(3) C76 0.049(3) 0.066(3) 0.030(2) -0.0022(19) -0.0003(19) -0.038(3) C77 0.033(2) 0.029(2) 0.033(2) -0.0019(16) -0.0059(17) -0.0175(18) C78 0.044(3) 0.032(2) 0.064(3) -0.001(2) 0.008(2) -0.012(2) C79 0.043(3) 0.040(3) 0.106(4) -0.026(3) 0.015(3) -0.009(2) C80 0.064(3) 0.027(2) 0.088(4) 0.003(3) -0.032(3) -0.018(3) C81 0.091(4) 0.032(3) 0.045(3) 0.007(2) -0.020(3) -0.026(3) C82 0.065(3) 0.035(2) 0.036(2) -0.0018(18) 0.002(2) -0.024(2) C83 0.031(2) 0.028(2) 0.0195(17) 0.0011(14) 0.0022(15) -0.0168(17) C84 0.031(2) 0.034(2) 0.0262(19) 0.0063(16) -0.0040(16) -0.0136(18) C85 0.036(2) 0.033(2) 0.037(2) 0.0015(17) 0.0022(18) -0.0083(19) C86 0.052(3) 0.026(2) 0.029(2) -0.0037(16) 0.0015(19) -0.014(2) C87 0.037(2) 0.035(2) 0.0268(19) -0.0004(16) -0.0061(17) -0.0166(19) C88 0.027(2) 0.031(2) 0.0277(19) -0.0030(15) -0.0007(16) -0.0123(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 1.999(2) . ? Sn1 O2 2.179(2) . ? Sn1 O71 2.202(2) . ? O1 Si1 1.615(2) . ? Si1 C13 1.865(4) . ? Si1 C7 1.878(4) . ? Si1 C1 1.880(3) . ? C1 C6 1.391(5) . ? C1 C2 1.400(5) . ? C2 C3 1.398(5) . ? C2 H2 0.95 . ? C3 C4 1.364(6) . ? C3 H3 0.95 . ? C4 C5 1.381(6) . ? C4 H4 0.95 . ? C5 C6 1.396(5) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.387(5) . ? C7 C8 1.399(4) . ? C8 C9 1.390(5) . ? C8 H8 0.95 . ? C9 C10 1.381(6) . ? C9 H9 0.95 . ? C10 C11 1.387(5) . ? C10 H10 0.95 . ? C11 C12 1.387(5) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.399(5) . ? C13 C14 1.405(4) . ? C14 C15 1.387(5) . ? C14 H14 0.95 . ? C15 C16 1.361(5) . ? C15 H15 0.95 . ? C16 C17 1.384(5) . ? C16 H16 0.95 . ? C17 C18 1.378(5) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? Si2 O2 1.659(2) . ? Si2 C27 1.867(4) . ? Si2 C21 1.872(3) . ? Si2 C33 1.876(3) . ? O2 Sn2 2.162(2) . ? C21 C26 1.395(5) . ? C21 C22 1.397(4) . ? C22 C23 1.400(5) . ? C22 H22 0.95 . ? C23 C24 1.384(5) . ? C23 H23 0.95 . ? C24 C25 1.373(5) . ? C24 H24 0.95 . ? C25 C26 1.397(5) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C28 1.396(4) . ? C27 C32 1.398(5) . ? C28 C29 1.387(5) . ? C28 H28 0.95 . ? C29 C30 1.373(6) . ? C29 H29 0.95 . ? C30 C31 1.389(5) . ? C30 H30 0.95 . ? C31 C32 1.393(5) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? C33 C38 1.397(5) . ? C33 C34 1.397(4) . ? C34 C35 1.393(5) . ? C34 H34 0.95 . ? C35 C36 1.376(5) . ? C35 H35 0.95 . ? C36 C37 1.398(5) . ? C36 H36 0.95 . ? C37 C38 1.374(5) . ? C37 H37 0.95 . ? C38 H38 0.95 . ? Sn2 O51 2.026(2) . ? Sn2 O71 2.178(2) . ? O51 Si11 1.622(2) . ? Si11 C63 1.871(4) . ? Si11 C51 1.876(4) . ? Si11 C57 1.878(3) . ? C51 C56 1.396(5) . ? C51 C52 1.402(5) . ? C52 C53 1.392(5) . ? C52 H52 0.95 . ? C53 C54 1.374(5) . ? C53 H53 0.95 . ? C54 C55 1.371(6) . ? C54 H54 0.95 . ? C55 C56 1.397(5) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 C58 1.386(5) . ? C57 C62 1.397(5) . ? C58 C59 1.398(5) . ? C58 H58 0.95 . ? C59 C60 1.374(5) . ? C59 H59 0.95 . ? C60 C61 1.367(6) . ? C60 H60 0.95 . ? C61 C62 1.397(5) . ? C61 H61 0.95 . ? C62 H62 0.95 . ? C63 C64 1.380(5) . ? C63 C68 1.407(5) . ? C64 C65 1.401(5) . ? C64 H64 0.95 . ? C65 C66 1.368(6) . ? C65 H65 0.95 . ? C66 C67 1.375(6) . ? C66 H66 0.95 . ? C67 C68 1.396(5) . ? C67 H67 0.95 . ? C68 H68 0.95 . ? O71 Si12 1.653(2) . ? Si12 C77 1.866(4) . ? Si12 C71 1.874(3) . ? Si12 C83 1.880(4) . ? C71 C72 1.394(5) . ? C71 C76 1.397(5) . ? C72 C73 1.387(5) . ? C72 H72 0.95 . ? C73 C74 1.378(5) . ? C73 H73 0.95 . ? C74 C75 1.373(6) . ? C74 H74 0.95 . ? C75 C76 1.396(5) . ? C75 H75 0.95 . ? C76 H76 0.95 . ? C77 C78 1.381(6) . ? C77 C82 1.396(5) . ? C78 C79 1.379(6) . ? C78 H78 0.95 . ? C79 C80 1.377(7) . ? C79 H79 0.95 . ? C80 C81 1.358(7) . ? C80 H80 0.95 . ? C81 C82 1.377(6) . ? C81 H81 0.95 . ? C82 H82 0.95 . ? C83 C84 1.399(5) . ? C83 C88 1.408(4) . ? C84 C85 1.383(5) . ? C84 H84 0.95 . ? C85 C86 1.381(5) . ? C85 H85 0.95 . ? C86 C87 1.386(5) . ? C86 H86 0.95 . ? C87 C88 1.388(5) . ? C87 H87 0.95 . ? C88 H88 0.95 . ? 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 O1 Sn1 O2 86.45(9) . . ? O1 Sn1 O71 85.59(9) . . ? O2 Sn1 O71 73.46(8) . . ? Si1 O1 Sn1 152.71(16) . . ? O1 Si1 C13 108.62(14) . . ? O1 Si1 C7 111.11(14) . . ? C13 Si1 C7 108.86(15) . . ? O1 Si1 C1 108.87(14) . . ? C13 Si1 C1 110.37(16) . . ? C7 Si1 C1 109.01(15) . . ? C6 C1 C2 117.2(3) . . ? C6 C1 Si1 119.1(3) . . ? C2 C1 Si1 123.6(3) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.4(4) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.5(4) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C1 C6 C5 122.1(4) . . ? C1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C12 C7 C8 116.9(3) . . ? C12 C7 Si1 120.9(3) . . ? C8 C7 Si1 122.2(3) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C10 C11 C12 120.0(4) . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C7 C12 C11 122.4(4) . . ? C7 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C18 C13 C14 116.5(3) . . ? C18 C13 Si1 122.6(2) . . ? C14 C13 Si1 120.9(3) . . ? C15 C14 C13 120.9(3) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 121.3(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 119.1(4) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 121.9(3) . . ? C17 C18 H18 119 . . ? C13 C18 H18 119 . . ? O2 Si2 C27 109.94(14) . . ? O2 Si2 C21 106.13(13) . . ? C27 Si2 C21 111.29(15) . . ? O2 Si2 C33 109.86(13) . . ? C27 Si2 C33 110.08(15) . . ? C21 Si2 C33 109.48(16) . . ? Si2 O2 Sn2 137.75(13) . . ? Si2 O2 Sn1 121.95(13) . . ? Sn2 O2 Sn1 100.17(8) . . ? C26 C21 C22 117.4(3) . . ? C26 C21 Si2 121.5(2) . . ? C22 C21 Si2 121.0(3) . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.0(4) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C21 C26 C25 121.8(3) . . ? C21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C28 C27 C32 117.8(3) . . ? C28 C27 Si2 122.2(3) . . ? C32 C27 Si2 120.0(3) . . ? C29 C28 C27 120.7(4) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C28 120.8(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 120.0(4) . . ? C29 C30 H30 120 . . ? C31 C30 H30 120 . . ? C30 C31 C32 119.2(4) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C27 121.5(3) . . ? C31 C32 H32 119.2 . . ? C27 C32 H32 119.2 . . ? C38 C33 C34 117.5(3) . . ? C38 C33 Si2 121.2(2) . . ? C34 C33 Si2 121.1(3) . . ? C35 C34 C33 121.4(3) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C36 C35 C34 119.6(3) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 120.0(3) . . ? C35 C36 H36 120 . . ? C37 C36 H36 120 . . ? C38 C37 C36 119.7(3) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 121.7(3) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? O51 Sn2 O2 92.56(9) . . ? O51 Sn2 O71 92.85(9) . . ? O2 Sn2 O71 74.28(8) . . ? Si11 O51 Sn2 136.06(15) . . ? O51 Si11 C63 111.57(14) . . ? O51 Si11 C51 110.68(14) . . ? C63 Si11 C51 108.51(17) . . ? O51 Si11 C57 108.99(15) . . ? C63 Si11 C57 107.00(15) . . ? C51 Si11 C57 110.02(15) . . ? C56 C51 C52 116.1(3) . . ? C56 C51 Si11 122.9(3) . . ? C52 C51 Si11 120.9(3) . . ? C53 C52 C51 121.7(3) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? C54 C53 C52 120.8(4) . . ? C54 C53 H53 119.6 . . ? C52 C53 H53 119.6 . . ? C55 C54 C53 118.8(4) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 120.9(4) . . ? C54 C55 H55 119.6 . . ? C56 C55 H55 119.6 . . ? C51 C56 C55 121.6(4) . . ? C51 C56 H56 119.2 . . ? C55 C56 H56 119.2 . . ? C58 C57 C62 116.7(3) . . ? C58 C57 Si11 122.9(3) . . ? C62 C57 Si11 120.5(3) . . ? C57 C58 C59 121.8(3) . . ? C57 C58 H58 119.1 . . ? C59 C58 H58 119.1 . . ? C60 C59 C58 120.2(4) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C61 C60 C59 119.4(4) . . ? C61 C60 H60 120.3 . . ? C59 C60 H60 120.3 . . ? C60 C61 C62 120.5(4) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? C57 C62 C61 121.5(4) . . ? C57 C62 H62 119.3 . . ? C61 C62 H62 119.3 . . ? C64 C63 C68 116.3(4) . . ? C64 C63 Si11 124.9(3) . . ? C68 C63 Si11 118.8(3) . . ? C63 C64 C65 122.6(4) . . ? C63 C64 H64 118.7 . . ? C65 C64 H64 118.7 . . ? C66 C65 C64 119.5(4) . . ? C66 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C65 C66 C67 120.0(4) . . ? C65 C66 H66 120 . . ? C67 C66 H66 120 . . ? C66 C67 C68 120.1(4) . . ? C66 C67 H67 120 . . ? C68 C67 H67 120 . . ? C67 C68 C63 121.4(4) . . ? C67 C68 H68 119.3 . . ? C63 C68 H68 119.3 . . ? Si12 O71 Sn2 142.51(14) . . ? Si12 O71 Sn1 118.43(12) . . ? Sn2 O71 Sn1 98.93(8) . . ? O71 Si12 C77 111.56(14) . . ? O71 Si12 C71 109.58(13) . . ? C77 Si12 C71 112.91(15) . . ? O71 Si12 C83 104.20(13) . . ? C77 Si12 C83 107.71(16) . . ? C71 Si12 C83 110.51(16) . . ? C72 C71 C76 118.1(3) . . ? C72 C71 Si12 122.6(3) . . ? C76 C71 Si12 119.3(3) . . ? C73 C72 C71 120.6(3) . . ? C73 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C74 C73 C72 120.9(4) . . ? C74 C73 H73 119.5 . . ? C72 C73 H73 119.5 . . ? C75 C74 C73 119.4(4) . . ? C75 C74 H74 120.3 . . ? C73 C74 H74 120.3 . . ? C74 C75 C76 120.5(4) . . ? C74 C75 H75 119.8 . . ? C76 C75 H75 119.8 . . ? C75 C76 C71 120.6(4) . . ? C75 C76 H76 119.7 . . ? C71 C76 H76 119.7 . . ? C78 C77 C82 116.4(4) . . ? C78 C77 Si12 124.4(3) . . ? C82 C77 Si12 119.2(3) . . ? C79 C78 C77 121.8(4) . . ? C79 C78 H78 119.1 . . ? C77 C78 H78 119.1 . . ? C80 C79 C78 120.4(5) . . ? C80 C79 H79 119.8 . . ? C78 C79 H79 119.8 . . ? C81 C80 C79 118.9(5) . . ? C81 C80 H80 120.5 . . ? C79 C80 H80 120.5 . . ? C80 C81 C82 120.8(4) . . ? C80 C81 H81 119.6 . . ? C82 C81 H81 119.6 . . ? C81 C82 C77 121.6(5) . . ? C81 C82 H82 119.2 . . ? C77 C82 H82 119.2 . . ? C84 C83 C88 117.2(3) . . ? C84 C83 Si12 123.9(3) . . ? C88 C83 Si12 118.5(3) . . ? C85 C84 C83 121.8(3) . . ? C85 C84 H84 119.1 . . ? C83 C84 H84 119.1 . . ? C86 C85 C84 119.6(4) . . ? C86 C85 H85 120.2 . . ? C84 C85 H85 120.2 . . ? C85 C86 C87 120.4(4) . . ? C85 C86 H86 119.8 . . ? C87 C86 H86 119.8 . . ? C86 C87 C88 119.7(3) . . ? C86 C87 H87 120.2 . . ? C88 C87 H87 120.2 . . ? C87 C88 C83 121.2(4) . . ? C87 C88 H88 119.4 . . ? C83 C88 H88 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sn1 O1 Si1 -144.2(3) . . . . ? O71 Sn1 O1 Si1 142.1(3) . . . . ? Sn1 O1 Si1 C13 -143.1(3) . . . . ? Sn1 O1 Si1 C7 -23.4(4) . . . . ? Sn1 O1 Si1 C1 96.7(3) . . . . ? O1 Si1 C1 C6 57.4(3) . . . . ? C13 Si1 C1 C6 -61.8(3) . . . . ? C7 Si1 C1 C6 178.7(3) . . . . ? O1 Si1 C1 C2 -119.3(3) . . . . ? C13 Si1 C1 C2 121.6(3) . . . . ? C7 Si1 C1 C2 2.1(3) . . . . ? C6 C1 C2 C3 0.0(5) . . . . ? Si1 C1 C2 C3 176.7(3) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 -0.2(7) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C2 C1 C6 C5 -0.2(5) . . . . ? Si1 C1 C6 C5 -177.0(3) . . . . ? C4 C5 C6 C1 0.1(6) . . . . ? O1 Si1 C7 C12 47.4(3) . . . . ? C13 Si1 C7 C12 167.0(2) . . . . ? C1 Si1 C7 C12 -72.5(3) . . . . ? O1 Si1 C7 C8 -128.9(3) . . . . ? C13 Si1 C7 C8 -9.3(3) . . . . ? C1 Si1 C7 C8 111.1(3) . . . . ? C12 C7 C8 C9 -0.5(5) . . . . ? Si1 C7 C8 C9 175.9(2) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 1.1(5) . . . . ? C9 C10 C11 C12 -1.7(5) . . . . ? C8 C7 C12 C11 0.0(5) . . . . ? Si1 C7 C12 C11 -176.6(2) . . . . ? C10 C11 C12 C7 1.2(5) . . . . ? O1 Si1 C13 C18 -162.4(3) . . . . ? C7 Si1 C13 C18 76.5(3) . . . . ? C1 Si1 C13 C18 -43.1(3) . . . . ? O1 Si1 C13 C14 20.2(3) . . . . ? C7 Si1 C13 C14 -100.9(3) . . . . ? C1 Si1 C13 C14 139.5(3) . . . . ? C18 C13 C14 C15 -0.5(5) . . . . ? Si1 C13 C14 C15 177.1(3) . . . . ? C13 C14 C15 C16 1.2(6) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 C18 0.3(6) . . . . ? C16 C17 C18 C13 0.4(6) . . . . ? C14 C13 C18 C17 -0.3(5) . . . . ? Si1 C13 C18 C17 -177.9(3) . . . . ? C27 Si2 O2 Sn2 28.4(2) . . . . ? C21 Si2 O2 Sn2 148.83(18) . . . . ? C33 Si2 O2 Sn2 -92.9(2) . . . . ? C27 Si2 O2 Sn1 -146.66(14) . . . . ? C21 Si2 O2 Sn1 -26.20(18) . . . . ? C33 Si2 O2 Sn1 92.06(17) . . . . ? O1 Sn1 O2 Si2 117.51(14) . . . . ? O71 Sn1 O2 Si2 -156.04(15) . . . . ? O1 Sn1 O2 Sn2 -59.09(9) . . . . ? O71 Sn1 O2 Sn2 27.36(8) . . . . ? O2 Si2 C21 C26 116.9(3) . . . . ? C27 Si2 C21 C26 -123.5(3) . . . . ? C33 Si2 C21 C26 -1.6(3) . . . . ? O2 Si2 C21 C22 -61.7(3) . . . . ? C27 Si2 C21 C22 57.9(3) . . . . ? C33 Si2 C21 C22 179.8(3) . . . . ? C26 C21 C22 C23 -0.4(5) . . . . ? Si2 C21 C22 C23 178.2(3) . . . . ? C21 C22 C23 C24 0.9(6) . . . . ? C22 C23 C24 C25 -0.8(6) . . . . ? C23 C24 C25 C26 0.4(5) . . . . ? C22 C21 C26 C25 0.0(5) . . . . ? Si2 C21 C26 C25 -178.6(3) . . . . ? C24 C25 C26 C21 0.0(5) . . . . ? O2 Si2 C27 C28 129.3(3) . . . . ? C21 Si2 C27 C28 12.0(3) . . . . ? C33 Si2 C27 C28 -109.5(3) . . . . ? O2 Si2 C27 C32 -52.6(3) . . . . ? C21 Si2 C27 C32 -169.9(3) . . . . ? C33 Si2 C27 C32 68.5(3) . . . . ? C32 C27 C28 C29 1.7(5) . . . . ? Si2 C27 C28 C29 179.8(3) . . . . ? C27 C28 C29 C30 0.0(6) . . . . ? C28 C29 C30 C31 -0.3(6) . . . . ? C29 C30 C31 C32 -1.1(6) . . . . ? C30 C31 C32 C27 2.8(6) . . . . ? C28 C27 C32 C31 -3.1(6) . . . . ? Si2 C27 C32 C31 178.8(3) . . . . ? O2 Si2 C33 C38 -34.8(3) . . . . ? C27 Si2 C33 C38 -156.0(3) . . . . ? C21 Si2 C33 C38 81.4(3) . . . . ? O2 Si2 C33 C34 149.2(3) . . . . ? C27 Si2 C33 C34 28.0(4) . . . . ? C21 Si2 C33 C34 -94.6(3) . . . . ? C38 C33 C34 C35 0.5(6) . . . . ? Si2 C33 C34 C35 176.6(3) . . . . ? C33 C34 C35 C36 -0.4(6) . . . . ? C34 C35 C36 C37 0.1(6) . . . . ? C35 C36 C37 C38 -0.1(7) . . . . ? C36 C37 C38 C33 0.3(7) . . . . ? C34 C33 C38 C37 -0.5(6) . . . . ? Si2 C33 C38 C37 -176.6(3) . . . . ? Si2 O2 Sn2 O51 64.48(18) . . . . ? Sn1 O2 Sn2 O51 -119.81(9) . . . . ? Si2 O2 Sn2 O71 156.73(19) . . . . ? Sn1 O2 Sn2 O71 -27.57(8) . . . . ? O2 Sn2 O51 Si11 -152.80(19) . . . . ? O71 Sn2 O51 Si11 132.82(19) . . . . ? Sn2 O51 Si11 C63 -69.2(2) . . . . ? Sn2 O51 Si11 C51 51.7(2) . . . . ? Sn2 O51 Si11 C57 172.86(18) . . . . ? O51 Si11 C51 C56 120.6(3) . . . . ? C63 Si11 C51 C56 -116.7(3) . . . . ? C57 Si11 C51 C56 0.1(4) . . . . ? O51 Si11 C51 C52 -60.4(3) . . . . ? C63 Si11 C51 C52 62.3(3) . . . . ? C57 Si11 C51 C52 179.0(3) . . . . ? C56 C51 C52 C53 -0.6(6) . . . . ? Si11 C51 C52 C53 -179.7(3) . . . . ? C51 C52 C53 C54 1.8(6) . . . . ? C52 C53 C54 C55 -1.6(7) . . . . ? C53 C54 C55 C56 0.2(7) . . . . ? C52 C51 C56 C55 -0.8(6) . . . . ? Si11 C51 C56 C55 178.3(3) . . . . ? C54 C55 C56 C51 1.0(7) . . . . ? O51 Si11 C57 C58 -21.4(3) . . . . ? C63 Si11 C57 C58 -142.2(3) . . . . ? C51 Si11 C57 C58 100.1(3) . . . . ? O51 Si11 C57 C62 158.3(3) . . . . ? C63 Si11 C57 C62 37.6(4) . . . . ? C51 Si11 C57 C62 -80.1(3) . . . . ? C62 C57 C58 C59 0.0(5) . . . . ? Si11 C57 C58 C59 179.8(3) . . . . ? C57 C58 C59 C60 0.1(6) . . . . ? C58 C59 C60 C61 -0.3(6) . . . . ? C59 C60 C61 C62 0.3(7) . . . . ? C58 C57 C62 C61 0.0(6) . . . . ? Si11 C57 C62 C61 -179.8(3) . . . . ? C60 C61 C62 C57 -0.2(7) . . . . ? O51 Si11 C63 C64 124.3(3) . . . . ? C51 Si11 C63 C64 2.1(3) . . . . ? C57 Si11 C63 C64 -116.5(3) . . . . ? O51 Si11 C63 C68 -58.2(3) . . . . ? C51 Si11 C63 C68 179.6(3) . . . . ? C57 Si11 C63 C68 60.9(3) . . . . ? C68 C63 C64 C65 0.5(5) . . . . ? Si11 C63 C64 C65 178.0(3) . . . . ? C63 C64 C65 C66 1.2(6) . . . . ? C64 C65 C66 C67 -1.0(6) . . . . ? C65 C66 C67 C68 -0.8(7) . . . . ? C66 C67 C68 C63 2.6(7) . . . . ? C64 C63 C68 C67 -2.3(6) . . . . ? Si11 C63 C68 C67 180.0(3) . . . . ? O51 Sn2 O71 Si12 -65.7(2) . . . . ? O2 Sn2 O71 Si12 -157.6(2) . . . . ? O51 Sn2 O71 Sn1 119.00(9) . . . . ? O2 Sn2 O71 Sn1 27.14(8) . . . . ? O1 Sn1 O71 Si12 -116.17(14) . . . . ? O2 Sn1 O71 Si12 156.24(15) . . . . ? O1 Sn1 O71 Sn2 60.57(9) . . . . ? O2 Sn1 O71 Sn2 -27.03(8) . . . . ? Sn2 O71 Si12 C77 -39.1(2) . . . . ? Sn1 O71 Si12 C77 135.57(15) . . . . ? Sn2 O71 Si12 C71 86.7(2) . . . . ? Sn1 O71 Si12 C71 -98.63(16) . . . . ? Sn2 O71 Si12 C83 -155.1(2) . . . . ? Sn1 O71 Si12 C83 19.64(18) . . . . ? O71 Si12 C71 C72 -3.4(4) . . . . ? C77 Si12 C71 C72 121.6(3) . . . . ? C83 Si12 C71 C72 -117.7(3) . . . . ? O71 Si12 C71 C76 176.2(3) . . . . ? C77 Si12 C71 C76 -58.8(4) . . . . ? C83 Si12 C71 C76 61.9(4) . . . . ? C76 C71 C72 C73 -1.5(6) . . . . ? Si12 C71 C72 C73 178.2(3) . . . . ? C71 C72 C73 C74 -0.5(7) . . . . ? C72 C73 C74 C75 0.9(7) . . . . ? C73 C74 C75 C76 0.7(7) . . . . ? C74 C75 C76 C71 -2.8(7) . . . . ? C72 C71 C76 C75 3.1(6) . . . . ? Si12 C71 C76 C75 -176.5(3) . . . . ? O71 Si12 C77 C78 37.4(3) . . . . ? C71 Si12 C77 C78 -86.6(3) . . . . ? C83 Si12 C77 C78 151.1(3) . . . . ? O71 Si12 C77 C82 -144.1(3) . . . . ? C71 Si12 C77 C82 92.0(3) . . . . ? C83 Si12 C77 C82 -30.3(3) . . . . ? C82 C77 C78 C79 0.6(6) . . . . ? Si12 C77 C78 C79 179.1(3) . . . . ? C77 C78 C79 C80 1.0(6) . . . . ? C78 C79 C80 C81 -2.1(7) . . . . ? C79 C80 C81 C82 1.7(6) . . . . ? C80 C81 C82 C77 -0.1(6) . . . . ? C78 C77 C82 C81 -1.0(5) . . . . ? Si12 C77 C82 C81 -179.6(3) . . . . ? O71 Si12 C83 C84 -105.4(3) . . . . ? C77 Si12 C83 C84 136.0(3) . . . . ? C71 Si12 C83 C84 12.2(3) . . . . ? O71 Si12 C83 C88 67.3(3) . . . . ? C77 Si12 C83 C88 -51.3(3) . . . . ? C71 Si12 C83 C88 -175.1(2) . . . . ? C88 C83 C84 C85 -0.3(5) . . . . ? Si12 C83 C84 C85 172.6(3) . . . . ? C83 C84 C85 C86 -1.0(5) . . . . ? C84 C85 C86 C87 1.6(5) . . . . ? C85 C86 C87 C88 -1.0(5) . . . . ? C86 C87 C88 C83 -0.3(5) . . . . ? C84 C83 C88 C87 0.9(5) . . . . ? Si12 C83 C88 C87 -172.3(3) . . . . ? #===END data_{Sn{OSiPh3}{OiPr}}2 _audit_creation_date 2013-03-12T11:27:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H44 O4 Si2 Sn2' _chemical_formula_sum 'C42 H44 O4 Si2 Sn2' _chemical_formula_weight 906.33 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7036(2) _cell_length_b 9.22800(10) _cell_length_c 13.5312(3) _cell_angle_alpha 83.7984(7) _cell_angle_beta 87.4022(8) _cell_angle_gamma 66.1500(6) _cell_volume 988.16(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9101 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 27.47 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.754 _exptl_absorpt_correction_T_max 0.884 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_number 16296 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 4471 _reflns_number_gt 4152 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+0.0305P] 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_number_reflns 4471 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0732 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.615 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.208 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 8.7036 9.2280 13.5312 83.7984 87.4022 66.1500 ZERR 1 0.0002 0.0001 0.0003 0.0007 0.0008 0.0006 LATT 1 SFAC C H O SI SN UNIT 42 44 4 2 2 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.041700 0.030500 FVAR 0.74606 SN1 5 0.600353 0.126862 0.498037 11.00000 0.02169 0.02656 = 0.01996 -0.00312 0.00023 -0.00420 O1 3 0.685063 0.088981 0.360486 11.00000 0.02800 0.02719 = 0.02346 0.00132 0.00694 -0.01008 SI1 4 0.736890 0.138039 0.250053 11.00000 0.01652 0.01664 = 0.01937 -0.00089 0.00228 -0.00695 C1 1 0.565395 0.170654 0.160499 11.00000 0.01484 0.01923 = 0.02342 -0.00382 0.00272 -0.00531 C2 1 0.476817 0.072107 0.170710 11.00000 0.02484 0.02192 = 0.03265 0.00049 0.00114 -0.01064 AFIX 43 H2 2 0.503938 -0.010016 0.223989 11.00000 -1.20000 AFIX 0 C3 1 0.350270 0.091750 0.104715 11.00000 0.02513 0.03007 = 0.04315 -0.00690 -0.00025 -0.01729 AFIX 43 H3 2 0.292551 0.023135 0.112732 11.00000 -1.20000 AFIX 0 C4 1 0.309039 0.211740 0.027399 11.00000 0.02367 0.03548 = 0.03334 -0.00807 -0.00288 -0.01264 AFIX 43 H4 2 0.221398 0.226780 -0.017152 11.00000 -1.20000 AFIX 0 C5 1 0.394662 0.309587 0.014750 11.00000 0.02880 0.03093 = 0.03024 0.00271 -0.00586 -0.01333 AFIX 43 H5 2 0.367897 0.390436 -0.039283 11.00000 -1.20000 AFIX 0 C6 1 0.520096 0.289594 0.081216 11.00000 0.02342 0.02514 = 0.03033 -0.00129 -0.00016 -0.01315 AFIX 43 H6 2 0.576836 0.359019 0.072456 11.00000 -1.20000 AFIX 0 C7 1 0.935857 -0.027648 0.213444 11.00000 0.01862 0.01498 = 0.02490 0.00032 0.00248 -0.00915 C8 1 0.960716 -0.080784 0.118571 11.00000 0.02333 0.02196 = 0.02094 -0.00033 -0.00107 -0.01027 AFIX 43 H8 2 0.875974 -0.029022 0.069587 11.00000 -1.20000 AFIX 0 C9 1 1.107139 -0.208024 0.094396 11.00000 0.03008 0.02626 = 0.02522 -0.01025 0.00718 -0.01150 AFIX 43 H9 2 1.120757 -0.242743 0.029742 11.00000 -1.20000 AFIX 0 C10 1 1.232550 -0.283703 0.164500 11.00000 0.02202 0.02202 = 0.03612 -0.00512 0.00540 -0.00447 AFIX 43 H10 2 1.332266 -0.370611 0.148275 11.00000 -1.20000 AFIX 0 C11 1 1.211886 -0.232032 0.258478 11.00000 0.02207 0.02322 = 0.03330 0.00135 -0.00551 -0.00308 AFIX 43 H11 2 1.298032 -0.283064 0.306721 11.00000 -1.20000 AFIX 0 C12 1 1.065346 -0.105637 0.282378 11.00000 0.02505 0.02269 = 0.02230 -0.00298 -0.00080 -0.00786 AFIX 43 H12 2 1.052948 -0.071468 0.347136 11.00000 -1.20000 AFIX 0 C13 1 0.778471 0.323527 0.243200 11.00000 0.01700 0.01887 = 0.01825 0.00111 -0.00278 -0.00722 C14 1 0.916059 0.334192 0.190308 11.00000 0.02224 0.02288 = 0.02552 -0.00509 0.00266 -0.01066 AFIX 43 H14 2 0.989757 0.245958 0.157420 11.00000 -1.20000 AFIX 0 C15 1 0.947120 0.471269 0.184900 11.00000 0.02963 0.03288 = 0.03034 -0.00252 0.00343 -0.02000 AFIX 43 H15 2 1.040892 0.475869 0.148097 11.00000 -1.20000 AFIX 0 C16 1 0.842820 0.600561 0.232560 11.00000 0.03555 0.02019 = 0.03357 0.00074 -0.00533 -0.01460 AFIX 43 H16 2 0.864601 0.693897 0.229100 11.00000 -1.20000 AFIX 0 C17 1 0.706254 0.592887 0.285414 11.00000 0.03290 0.01812 = 0.04046 -0.00637 0.00170 -0.00525 AFIX 43 H17 2 0.634132 0.681403 0.318642 11.00000 -1.20000 AFIX 0 C18 1 0.673516 0.457168 0.290399 11.00000 0.02134 0.01931 = 0.03358 -0.00138 0.00247 -0.00542 AFIX 43 H18 2 0.578256 0.454606 0.326439 11.00000 -1.20000 AFIX 0 O2 3 0.367465 0.113940 0.467454 11.00000 0.01648 0.02977 = 0.03202 0.01376 0.00015 -0.00276 C21 1 0.226734 0.230994 0.410281 11.00000 0.02098 0.03148 = 0.02660 0.00777 -0.00269 -0.00039 AFIX 13 H21 2 0.223819 0.189549 0.345403 11.00000 -1.20000 AFIX 0 C22 1 0.250216 0.383964 0.389241 11.00000 0.02821 0.03497 = 0.07183 0.02304 -0.00967 -0.00446 AFIX 137 H22A 2 0.256135 0.425137 0.452113 11.00000 -1.50000 H22B 2 0.155180 0.462159 0.350058 11.00000 -1.50000 H22C 2 0.354651 0.364389 0.351827 11.00000 -1.50000 AFIX 0 C23 1 0.066569 0.251478 0.465319 11.00000 0.01754 0.04727 = 0.04588 0.00811 -0.00114 -0.00162 AFIX 137 H23A 2 0.052141 0.150927 0.471273 11.00000 -1.50000 H23B 2 -0.028600 0.334647 0.428799 11.00000 -1.50000 H23C 2 0.071684 0.282224 0.531789 11.00000 -1.50000 HKLF 4 REM import in P -1 REM R1 = 0.0233 for 4152 Fo > 4sig(Fo) and 0.0274 for all 4471 data REM 228 parameters refined using 0 restraints END WGHT 0.0382 0.0000 REM Highest difference peak 0.62, deepest hole -0.51, 1-sigma level 0.21 Q1 1 0.8531 0.3149 0.2323 11.00000 0.05 0.62 Q2 1 0.7191 0.3958 0.2535 11.00000 0.05 0.59 Q3 1 0.7448 0.3854 0.2738 11.00000 0.05 0.58 Q4 1 0.3561 0.3552 0.0156 11.00000 0.05 0.57 Q5 1 0.4982 0.1531 0.1732 11.00000 0.05 0.57 Q6 1 0.8217 0.3364 0.2098 11.00000 0.05 0.55 Q7 1 0.4850 0.2683 0.0367 11.00000 0.05 0.52 Q8 1 0.5735 0.1804 0.1124 11.00000 0.05 0.50 Q9 1 0.4393 0.3054 0.0533 11.00000 0.05 0.49 Q10 1 0.2405 0.3017 0.3980 11.00000 0.05 0.48 Q11 1 0.8003 0.2806 0.2777 11.00000 0.05 0.47 Q12 1 0.6067 0.4843 0.2822 11.00000 0.05 0.47 Q13 1 0.2181 0.3354 0.4213 11.00000 0.05 0.46 Q14 1 1.3385 -0.3035 0.4047 11.00000 0.05 0.46 Q15 1 1.3575 -0.2532 0.2843 11.00000 0.05 0.45 Q16 1 0.4349 -0.2073 0.1046 11.00000 0.05 0.45 Q17 1 1.3605 -0.2632 0.3327 11.00000 0.05 0.44 Q18 1 0.5000 0.5000 0.5000 10.50000 0.05 0.44 Q19 1 0.8530 0.7737 0.2649 11.00000 0.05 0.44 Q20 1 0.4330 0.3337 -0.0646 11.00000 0.05 0.44 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 0.600353(18) 0.126862(16) 0.498037(11) 0.02446(7) Uani 1 1 d . . . O1 O 0.6851(2) 0.08898(18) 0.36049(12) 0.0271(4) Uani 1 1 d . . . Si1 Si 0.73689(7) 0.13804(6) 0.25005(4) 0.01756(13) Uani 1 1 d . . . C1 C 0.5654(3) 0.1707(2) 0.16050(17) 0.0196(4) Uani 1 1 d . . . C2 C 0.4768(3) 0.0721(3) 0.17071(18) 0.0264(5) Uani 1 1 d . . . H2 H 0.5039 -0.01 0.224 0.032 Uiso 1 1 calc R . . C3 C 0.3503(3) 0.0918(3) 0.1047(2) 0.0305(5) Uani 1 1 d . . . H3 H 0.2926 0.0231 0.1127 0.037 Uiso 1 1 calc R . . C4 C 0.3090(3) 0.2117(3) 0.02740(19) 0.0301(5) Uani 1 1 d . . . H4 H 0.2214 0.2268 -0.0172 0.036 Uiso 1 1 calc R . . C5 C 0.3947(3) 0.3096(3) 0.01475(19) 0.0298(5) Uani 1 1 d . . . H5 H 0.3679 0.3904 -0.0393 0.036 Uiso 1 1 calc R . . C6 C 0.5201(3) 0.2896(3) 0.08122(18) 0.0253(5) Uani 1 1 d . . . H6 H 0.5768 0.359 0.0725 0.03 Uiso 1 1 calc R . . C7 C 0.9359(3) -0.0276(2) 0.21344(16) 0.0190(4) Uani 1 1 d . . . C8 C 0.9607(3) -0.0808(2) 0.11857(17) 0.0218(4) Uani 1 1 d . . . H8 H 0.876 -0.029 0.0696 0.026 Uiso 1 1 calc R . . C9 C 1.1071(3) -0.2080(3) 0.09440(18) 0.0268(5) Uani 1 1 d . . . H9 H 1.1208 -0.2427 0.0297 0.032 Uiso 1 1 calc R . . C10 C 1.2326(3) -0.2837(3) 0.16450(19) 0.0281(5) Uani 1 1 d . . . H10 H 1.3323 -0.3706 0.1483 0.034 Uiso 1 1 calc R . . C11 C 1.2119(3) -0.2320(3) 0.25848(19) 0.0283(5) Uani 1 1 d . . . H11 H 1.298 -0.2831 0.3067 0.034 Uiso 1 1 calc R . . C12 C 1.0653(3) -0.1056(2) 0.28238(17) 0.0238(5) Uani 1 1 d . . . H12 H 1.0529 -0.0715 0.3471 0.029 Uiso 1 1 calc R . . C13 C 0.7785(3) 0.3235(2) 0.24320(16) 0.0182(4) Uani 1 1 d . . . C14 C 0.9161(3) 0.3342(3) 0.19031(17) 0.0229(5) Uani 1 1 d . . . H14 H 0.9898 0.246 0.1574 0.027 Uiso 1 1 calc R . . C15 C 0.9471(3) 0.4713(3) 0.18490(19) 0.0287(5) Uani 1 1 d . . . H15 H 1.0409 0.4759 0.1481 0.034 Uiso 1 1 calc R . . C16 C 0.8428(3) 0.6006(3) 0.23256(19) 0.0288(5) Uani 1 1 d . . . H16 H 0.8646 0.6939 0.2291 0.035 Uiso 1 1 calc R . . C17 C 0.7063(3) 0.5929(3) 0.2854(2) 0.0319(6) Uani 1 1 d . . . H17 H 0.6341 0.6814 0.3186 0.038 Uiso 1 1 calc R . . C18 C 0.6735(3) 0.4572(2) 0.29040(18) 0.0258(5) Uani 1 1 d . . . H18 H 0.5783 0.4546 0.3264 0.031 Uiso 1 1 calc R . . O2 O 0.36746(19) 0.11394(19) 0.46745(13) 0.0296(4) Uani 1 1 d . . . C21 C 0.2267(3) 0.2310(3) 0.41028(19) 0.0304(5) Uani 1 1 d . . . H21 H 0.2238 0.1895 0.3454 0.036 Uiso 1 1 calc R . . C22 C 0.2502(3) 0.3840(3) 0.3892(3) 0.0496(8) Uani 1 1 d . . . H22A H 0.2561 0.4251 0.4521 0.074 Uiso 1 1 calc R . . H22B H 0.1552 0.4622 0.3501 0.074 Uiso 1 1 calc R . . H22C H 0.3547 0.3644 0.3518 0.074 Uiso 1 1 calc R . . C23 C 0.0666(3) 0.2515(3) 0.4653(2) 0.0416(7) Uani 1 1 d . . . H23A H 0.0521 0.1509 0.4713 0.062 Uiso 1 1 calc R . . H23B H -0.0286 0.3346 0.4288 0.062 Uiso 1 1 calc R . . H23C H 0.0717 0.2822 0.5318 0.062 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 0.02169(11) 0.02656(10) 0.01996(11) -0.00312(7) 0.00023(7) -0.00420(7) O1 0.0280(9) 0.0272(8) 0.0235(9) 0.0013(6) 0.0069(7) -0.0101(7) Si1 0.0165(3) 0.0166(3) 0.0194(3) -0.0009(2) 0.0023(2) -0.0070(2) C1 0.0148(10) 0.0192(9) 0.0234(12) -0.0038(8) 0.0027(9) -0.0053(8) C2 0.0248(12) 0.0219(10) 0.0326(14) 0.0005(9) 0.0011(10) -0.0106(9) C3 0.0251(13) 0.0301(12) 0.0431(16) -0.0069(11) -0.0002(11) -0.0173(10) C4 0.0237(12) 0.0355(12) 0.0333(14) -0.0081(11) -0.0029(10) -0.0126(10) C5 0.0288(13) 0.0309(12) 0.0302(14) 0.0027(10) -0.0059(10) -0.0133(10) C6 0.0234(12) 0.0251(11) 0.0303(13) -0.0013(9) -0.0002(10) -0.0131(9) C7 0.0186(11) 0.0150(9) 0.0249(12) 0.0003(8) 0.0025(9) -0.0092(8) C8 0.0233(11) 0.0220(10) 0.0209(11) -0.0003(8) -0.0011(9) -0.0103(9) C9 0.0301(13) 0.0263(11) 0.0252(13) -0.0103(9) 0.0072(10) -0.0115(10) C10 0.0220(12) 0.0220(10) 0.0361(14) -0.0051(10) 0.0054(10) -0.0045(9) C11 0.0221(12) 0.0232(11) 0.0333(14) 0.0013(10) -0.0055(10) -0.0031(9) C12 0.0250(12) 0.0227(10) 0.0223(12) -0.0030(9) -0.0008(9) -0.0079(9) C13 0.0170(10) 0.0189(9) 0.0182(11) 0.0011(8) -0.0028(8) -0.0072(8) C14 0.0222(11) 0.0229(10) 0.0255(12) -0.0051(9) 0.0027(9) -0.0107(9) C15 0.0296(13) 0.0329(12) 0.0303(14) -0.0025(10) 0.0034(10) -0.0200(10) C16 0.0356(14) 0.0202(10) 0.0336(14) 0.0007(9) -0.0053(11) -0.0146(10) C17 0.0329(13) 0.0181(10) 0.0405(15) -0.0064(10) 0.0017(11) -0.0052(9) C18 0.0213(11) 0.0193(10) 0.0336(14) -0.0014(9) 0.0025(10) -0.0054(9) O2 0.0165(8) 0.0298(8) 0.0320(10) 0.0138(7) 0.0002(7) -0.0028(6) C21 0.0210(12) 0.0315(12) 0.0266(13) 0.0078(10) -0.0027(10) -0.0004(10) C22 0.0282(15) 0.0350(14) 0.072(2) 0.0230(14) -0.0097(14) -0.0045(12) C23 0.0175(12) 0.0473(15) 0.0459(17) 0.0081(13) -0.0011(11) -0.0016(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 1.9844(16) . ? Sn1 O2 2.1257(16) 2_656 ? Sn1 O2 2.1392(17) . ? O1 Si1 1.6122(16) . ? Si1 C1 1.873(2) . ? Si1 C7 1.878(2) . ? Si1 C13 1.880(2) . ? C1 C6 1.395(3) . ? C1 C2 1.404(3) . ? C2 C3 1.391(3) . ? C2 H2 0.95 . ? C3 C4 1.383(4) . ? C3 H3 0.95 . ? C4 C5 1.378(3) . ? C4 H4 0.95 . ? C5 C6 1.387(3) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.397(3) . ? C7 C8 1.400(3) . ? C8 C9 1.395(3) . ? C8 H8 0.95 . ? C9 C10 1.383(4) . ? C9 H9 0.95 . ? C10 C11 1.385(3) . ? C10 H10 0.95 . ? C11 C12 1.390(3) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.399(3) . ? C13 C18 1.403(3) . ? C14 C15 1.390(3) . ? C14 H14 0.95 . ? C15 C16 1.379(3) . ? C15 H15 0.95 . ? C16 C17 1.382(4) . ? C16 H16 0.95 . ? C17 C18 1.387(3) . ? C17 H17 0.95 . ? C18 H18 0.95 . ? O2 C21 1.449(3) . ? O2 Sn1 2.1257(16) 2_656 ? C21 C22 1.502(4) . ? C21 C23 1.502(3) . ? C21 H21 1 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? 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 O1 Sn1 O2 92.27(6) . 2_656 ? O1 Sn1 O2 93.17(7) . . ? O2 Sn1 O2 72.64(7) 2_656 . ? Si1 O1 Sn1 155.20(10) . . ? O1 Si1 C1 109.82(9) . . ? O1 Si1 C7 108.54(9) . . ? C1 Si1 C7 109.75(10) . . ? O1 Si1 C13 112.26(9) . . ? C1 Si1 C13 108.93(9) . . ? C7 Si1 C13 107.50(9) . . ? C6 C1 C2 116.8(2) . . ? C6 C1 Si1 123.03(16) . . ? C2 C1 Si1 120.16(17) . . ? C3 C2 C1 121.6(2) . . ? C3 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 119.8(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C1 122.0(2) . . ? C5 C6 H6 119 . . ? C1 C6 H6 119 . . ? C12 C7 C8 117.16(19) . . ? C12 C7 Si1 120.24(16) . . ? C8 C7 Si1 122.58(16) . . ? C9 C8 C7 121.5(2) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 120.0(2) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 119.6(2) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 121.6(2) . . ? C11 C12 H12 119.2 . . ? C7 C12 H12 119.2 . . ? C14 C13 C18 117.05(19) . . ? C14 C13 Si1 121.17(16) . . ? C18 C13 Si1 121.78(16) . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 120.5(2) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.3(2) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C18 120.6(2) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 121.2(2) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? C21 O2 Sn1 122.98(14) . 2_656 ? C21 O2 Sn1 127.87(13) . . ? Sn1 O2 Sn1 107.36(7) 2_656 . ? O2 C21 C22 109.9(2) . . ? O2 C21 C23 109.1(2) . . ? C22 C21 C23 112.9(2) . . ? O2 C21 H21 108.3 . . ? C22 C21 H21 108.3 . . ? C23 C21 H21 108.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Sn1 O1 Si1 -179.5(2) 2_656 . . . ? O2 Sn1 O1 Si1 107.8(2) . . . . ? Sn1 O1 Si1 C1 -100.9(2) . . . . ? Sn1 O1 Si1 C7 139.1(2) . . . . ? Sn1 O1 Si1 C13 20.5(3) . . . . ? O1 Si1 C1 C6 142.65(18) . . . . ? C7 Si1 C1 C6 -98.11(19) . . . . ? C13 Si1 C1 C6 19.3(2) . . . . ? O1 Si1 C1 C2 -38.0(2) . . . . ? C7 Si1 C1 C2 81.20(19) . . . . ? C13 Si1 C1 C2 -161.36(17) . . . . ? C6 C1 C2 C3 0.2(3) . . . . ? Si1 C1 C2 C3 -179.14(18) . . . . ? C1 C2 C3 C4 -0.5(4) . . . . ? C2 C3 C4 C5 1.1(4) . . . . ? C3 C4 C5 C6 -1.4(4) . . . . ? C4 C5 C6 C1 1.2(4) . . . . ? C2 C1 C6 C5 -0.5(3) . . . . ? Si1 C1 C6 C5 178.79(18) . . . . ? O1 Si1 C7 C12 -41.01(18) . . . . ? C1 Si1 C7 C12 -161.03(16) . . . . ? C13 Si1 C7 C12 80.63(18) . . . . ? O1 Si1 C7 C8 137.67(16) . . . . ? C1 Si1 C7 C8 17.65(18) . . . . ? C13 Si1 C7 C8 -100.69(17) . . . . ? C12 C7 C8 C9 1.1(3) . . . . ? Si1 C7 C8 C9 -177.57(16) . . . . ? C7 C8 C9 C10 -0.7(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 C7 0.0(3) . . . . ? C8 C7 C12 C11 -0.8(3) . . . . ? Si1 C7 C12 C11 177.92(16) . . . . ? O1 Si1 C13 C14 136.80(18) . . . . ? C1 Si1 C13 C14 -101.35(19) . . . . ? C7 Si1 C13 C14 17.5(2) . . . . ? O1 Si1 C13 C18 -43.3(2) . . . . ? C1 Si1 C13 C18 78.5(2) . . . . ? C7 Si1 C13 C18 -162.62(18) . . . . ? C18 C13 C14 C15 0.0(3) . . . . ? Si1 C13 C14 C15 179.89(19) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C17 -0.4(4) . . . . ? C15 C16 C17 C18 -0.2(4) . . . . ? C16 C17 C18 C13 0.7(4) . . . . ? C14 C13 C18 C17 -0.6(3) . . . . ? Si1 C13 C18 C17 179.51(19) . . . . ? O1 Sn1 O2 C21 -73.56(19) . . . . ? O2 Sn1 O2 C21 -164.9(2) 2_656 . . . ? O1 Sn1 O2 Sn1 91.38(8) . . . 2_656 ? O2 Sn1 O2 Sn1 0 2_656 . . 2_656 ? Sn1 O2 C21 C22 -173.77(18) 2_656 . . . ? Sn1 O2 C21 C22 -11.0(3) . . . . ? Sn1 O2 C21 C23 62.0(3) 2_656 . . . ? Sn1 O2 C21 C23 -135.23(19) . . . . ? #===END data_{Sn{OSiPh3}{Cl}}2 _audit_creation_date 2013-05-25T08:03:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H30 Cl2 O2 Si2 Sn2' _chemical_formula_sum 'C36 H30 Cl2 O2 Si2 Sn2' _chemical_formula_weight 859.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8651(2) _cell_length_b 12.6482(3) _cell_length_c 14.6314(3) _cell_angle_alpha 94.7490(10) _cell_angle_beta 104.7980(10) _cell_angle_gamma 105.6150(10) _cell_volume 1677.28(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9790 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.5 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.749 _exptl_absorpt_correction_T_max 0.839 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_unetI/netI 0.0199 _diffrn_reflns_number 27575 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7648 _reflns_number_gt 7347 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+1.4284P] 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_number_reflns 7648 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0204 _refine_ls_R_factor_gt 0.0193 _refine_ls_wR_factor_ref 0.047 _refine_ls_wR_factor_gt 0.0462 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.645 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.062 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 9.8651 12.6482 14.6314 94.749 104.798 105.615 ZERR 2.00 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H O SI CL SN UNIT 72 60 4 4 4 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.016400 1.428400 FVAR 0.37748 SN1 6 0.636644 0.522339 0.198039 11.00000 0.01878 0.01710 = 0.02414 0.00493 0.01120 0.00565 SN2 6 0.465648 0.409448 0.361382 11.00000 0.02205 0.01466 = 0.02061 0.00302 0.00970 0.00518 CL1 5 0.388640 0.443768 0.086682 11.00000 0.02755 0.03083 = 0.02469 0.00375 0.00279 0.00824 CL2 5 0.674551 0.475117 0.509161 11.00000 0.02950 0.02720 = 0.02184 0.00417 0.00764 0.01444 SI1 4 0.522696 0.692644 0.327504 11.00000 0.01492 0.01293 = 0.01585 0.00126 0.00368 0.00385 O1 3 0.539071 0.565764 0.309303 11.00000 0.01944 0.01426 = 0.01820 0.00214 0.00627 0.00604 C2 1 0.632478 0.777520 0.255827 11.00000 0.01875 0.01328 = 0.01805 0.00316 0.00595 0.00602 C3 1 0.770885 0.854424 0.298006 11.00000 0.02083 0.02548 = 0.01957 0.00150 0.00462 0.00343 AFIX 43 H3 2 0.810772 0.867442 0.365720 11.00000 -1.20000 AFIX 0 C4 1 0.851544 0.912351 0.242932 11.00000 0.01932 0.03033 = 0.03173 0.00622 0.00782 0.00055 AFIX 43 H4 2 0.944595 0.965513 0.273390 11.00000 -1.20000 AFIX 0 C5 1 0.797718 0.893314 0.144740 11.00000 0.02735 0.03336 = 0.03119 0.01487 0.01508 0.00863 AFIX 43 H5 2 0.854174 0.932113 0.107385 11.00000 -1.20000 AFIX 0 C6 1 0.660599 0.817205 0.100369 11.00000 0.03283 0.03522 = 0.01949 0.00993 0.00663 0.00854 AFIX 43 H6 2 0.622941 0.803464 0.032501 11.00000 -1.20000 AFIX 0 C7 1 0.578444 0.761069 0.155711 11.00000 0.02435 0.02311 = 0.02093 0.00486 0.00216 0.00325 AFIX 43 H7 2 0.483607 0.710463 0.124927 11.00000 -1.20000 AFIX 0 C8 1 0.328579 0.692474 0.280426 11.00000 0.01728 0.01929 = 0.01575 0.00240 0.00534 0.00610 C9 1 0.299831 0.793427 0.265593 11.00000 0.02268 0.01767 = 0.02888 0.00484 0.00835 0.00469 AFIX 43 H9 2 0.379492 0.860208 0.280982 11.00000 -1.20000 AFIX 0 C10 1 0.157547 0.797779 0.228932 11.00000 0.02751 0.02424 = 0.02978 0.00968 0.00996 0.01361 AFIX 43 H10 2 0.140561 0.867062 0.219463 11.00000 -1.20000 AFIX 0 C11 1 0.040214 0.701206 0.206119 11.00000 0.02004 0.03187 = 0.02334 0.00504 0.00574 0.01153 AFIX 43 H11 2 -0.057359 0.704141 0.181361 11.00000 -1.20000 AFIX 0 C12 1 0.065590 0.600407 0.219510 11.00000 0.01808 0.02404 = 0.02909 0.00021 0.00466 0.00259 AFIX 43 H12 2 -0.014710 0.533994 0.203586 11.00000 -1.20000 AFIX 0 C13 1 0.208352 0.596031 0.256227 11.00000 0.02077 0.01787 = 0.02513 0.00268 0.00447 0.00537 AFIX 43 H13 2 0.224427 0.526329 0.265007 11.00000 -1.20000 AFIX 0 C14 1 0.607922 0.758615 0.456085 11.00000 0.01796 0.01435 = 0.01690 0.00279 0.00544 0.00171 C15 1 0.752097 0.759851 0.501261 11.00000 0.01997 0.02037 = 0.01924 0.00416 0.00676 0.00559 AFIX 43 H15 2 0.798052 0.717892 0.469305 11.00000 -1.20000 AFIX 0 C16 1 0.829294 0.821199 0.591869 11.00000 0.02089 0.02981 = 0.01960 0.00680 0.00363 0.00183 AFIX 43 H16 2 0.927813 0.822621 0.620645 11.00000 -1.20000 AFIX 0 C17 1 0.761485 0.880176 0.639809 11.00000 0.02838 0.02530 = 0.01716 -0.00128 0.00639 -0.00520 AFIX 43 H17 2 0.813653 0.922237 0.701692 11.00000 -1.20000 AFIX 0 C18 1 0.618258 0.878028 0.597929 11.00000 0.02995 0.02283 = 0.02661 -0.00264 0.01625 0.00092 AFIX 43 H18 2 0.571705 0.917431 0.631741 11.00000 -1.20000 AFIX 0 C19 1 0.541671 0.818555 0.506556 11.00000 0.01861 0.01959 = 0.02391 0.00205 0.00824 0.00378 AFIX 43 H19 2 0.443658 0.818536 0.478096 11.00000 -1.20000 AFIX 0 SI2 4 0.652671 0.265044 0.240247 11.00000 0.01705 0.01536 = 0.01609 0.00238 0.00564 0.00692 O21 3 0.607129 0.377969 0.268133 11.00000 0.02042 0.01630 = 0.01802 0.00253 0.00708 0.00808 C22 1 0.483726 0.150514 0.169809 11.00000 0.02288 0.01751 = 0.01445 0.00349 0.00706 0.00501 C23 1 0.342510 0.161069 0.153641 11.00000 0.02260 0.02338 = 0.01879 0.00304 0.00743 0.00526 AFIX 43 H23 2 0.330868 0.228821 0.178495 11.00000 -1.20000 AFIX 0 C24 1 0.218339 0.074379 0.101850 11.00000 0.02342 0.03376 = 0.02202 0.00575 0.00471 0.00177 AFIX 43 H24 2 0.123279 0.083246 0.091789 11.00000 -1.20000 AFIX 0 C25 1 0.233859 -0.024676 0.065104 11.00000 0.03539 0.02310 = 0.02212 0.00443 0.00117 -0.00623 AFIX 43 H25 2 0.149399 -0.084271 0.030420 11.00000 -1.20000 AFIX 0 C26 1 0.372109 -0.036652 0.078945 11.00000 0.04866 0.01736 = 0.02835 -0.00078 0.00646 0.00742 AFIX 43 H26 2 0.382823 -0.104356 0.053150 11.00000 -1.20000 AFIX 0 C27 1 0.495742 0.049752 0.130400 11.00000 0.03317 0.02213 = 0.02441 0.00150 0.00689 0.01143 AFIX 43 H27 2 0.590368 0.040438 0.139088 11.00000 -1.20000 AFIX 0 C28 1 0.746866 0.224877 0.354356 11.00000 0.02065 0.02548 = 0.01905 0.00599 0.00888 0.01278 C29 1 0.720454 0.115288 0.371290 11.00000 0.02558 0.02871 = 0.02666 0.00967 0.01086 0.01129 AFIX 43 H29 2 0.656356 0.056589 0.321612 11.00000 -1.20000 AFIX 0 C30 1 0.786050 0.090235 0.459410 11.00000 0.03330 0.04264 = 0.03504 0.02183 0.01659 0.02141 AFIX 43 H30 2 0.767102 0.015040 0.469445 11.00000 -1.20000 AFIX 0 C31 1 0.878801 0.174925 0.532299 11.00000 0.03515 0.06570 = 0.02179 0.01749 0.01255 0.03335 AFIX 43 H31 2 0.921746 0.158158 0.593081 11.00000 -1.20000 AFIX 0 C32 1 0.909039 0.283542 0.516940 11.00000 0.03102 0.05453 = 0.02179 -0.00492 0.00042 0.02376 AFIX 43 H32 2 0.973908 0.341577 0.566934 11.00000 -1.20000 AFIX 0 C33 1 0.844940 0.308763 0.428403 11.00000 0.02579 0.03042 = 0.02591 0.00070 0.00474 0.01526 AFIX 43 H33 2 0.868101 0.383913 0.418139 11.00000 -1.20000 AFIX 0 C34 1 0.781027 0.297100 0.164015 11.00000 0.01844 0.01597 = 0.01909 0.00023 0.00637 0.00491 C35 1 0.924469 0.289521 0.194052 11.00000 0.02457 0.02746 = 0.02621 0.00733 0.00859 0.01261 AFIX 43 H35 2 0.957759 0.268184 0.254530 11.00000 -1.20000 AFIX 0 C36 1 1.018871 0.312473 0.137463 11.00000 0.02129 0.03250 = 0.03545 0.00289 0.01099 0.01129 AFIX 43 H36 2 1.115300 0.306207 0.159163 11.00000 -1.20000 AFIX 0 C37 1 0.972710 0.344511 0.049372 11.00000 0.02459 0.03227 = 0.02639 -0.00135 0.01462 0.00281 AFIX 43 H37 2 1.037613 0.360700 0.010847 11.00000 -1.20000 AFIX 0 C38 1 0.831457 0.352917 0.017492 11.00000 0.02713 0.03331 = 0.01773 0.00052 0.00689 0.00373 AFIX 43 H38 2 0.799460 0.375132 -0.042766 11.00000 -1.20000 AFIX 0 C39 1 0.736835 0.328611 0.074307 11.00000 0.01812 0.02602 = 0.01822 -0.00055 0.00387 0.00576 AFIX 43 H39 2 0.639874 0.333548 0.051594 11.00000 -1.20000 HKLF 4 REM import in P -1 REM R1 = 0.0193 for 7347 Fo > 4sig(Fo) and 0.0204 for all 7648 data REM 397 parameters refined using 0 restraints END WGHT 0.0155 1.4567 REM Highest difference peak 0.64, deepest hole -0.34, 1-sigma level 0.06 Q1 1 0.5628 0.4426 0.3855 11.00000 0.05 0.64 Q2 1 0.5737 0.7182 0.3982 11.00000 0.05 0.56 Q3 1 0.4166 0.6930 0.3033 11.00000 0.05 0.45 Q4 1 0.5819 0.7379 0.2893 11.00000 0.05 0.43 Q5 1 0.7255 0.2906 0.1983 11.00000 0.05 0.38 Q6 1 0.6880 0.8322 0.2734 11.00000 0.05 0.37 Q7 1 0.7046 0.5411 0.2442 11.00000 0.05 0.36 Q8 1 0.5596 0.2014 0.1925 11.00000 0.05 0.36 Q9 1 0.7107 0.2404 0.3044 11.00000 0.05 0.35 Q10 1 0.7750 0.7886 0.5514 11.00000 0.05 0.35 Q11 1 0.3037 0.7418 0.2816 11.00000 0.05 0.35 Q12 1 0.6490 0.5759 0.1687 11.00000 0.05 0.35 Q13 1 0.1385 0.6044 0.2367 11.00000 0.05 0.34 Q14 1 0.5763 0.7882 0.4902 11.00000 0.05 0.34 Q15 1 0.2708 0.6573 0.2854 11.00000 0.05 0.33 Q16 1 0.9065 0.3619 0.0420 11.00000 0.05 0.33 Q17 1 0.2867 0.1180 0.1144 11.00000 0.05 0.33 Q18 1 0.8593 0.1365 0.4850 11.00000 0.05 0.32 Q19 1 0.7402 0.8424 0.1263 11.00000 0.05 0.32 Q20 1 0.9802 0.3179 0.0892 11.00000 0.05 0.32 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 0.636644(13) 0.522339(10) 0.198039(9) 0.01890(4) Uani 1 1 d . . . Sn2 Sn 0.465648(13) 0.409448(9) 0.361382(9) 0.01848(4) Uani 1 1 d . . . Cl1 Cl 0.38864(5) 0.44377(4) 0.08668(3) 0.02878(10) Uani 1 1 d . . . Cl2 Cl 0.67455(5) 0.47512(4) 0.50916(3) 0.02492(9) Uani 1 1 d . . . Si1 Si 0.52270(5) 0.69264(4) 0.32750(3) 0.01485(9) Uani 1 1 d . . . O1 O 0.53907(13) 0.56576(10) 0.30930(9) 0.0170(2) Uani 1 1 d . . . C2 C 0.63248(19) 0.77752(13) 0.25583(12) 0.0163(3) Uani 1 1 d . . . C3 C 0.7709(2) 0.85442(16) 0.29801(14) 0.0231(4) Uani 1 1 d . . . H3 H 0.8108 0.8674 0.3657 0.028 Uiso 1 1 calc R . . C4 C 0.8515(2) 0.91235(17) 0.24293(15) 0.0284(4) Uani 1 1 d . . . H4 H 0.9446 0.9655 0.2734 0.034 Uiso 1 1 calc R . . C5 C 0.7977(2) 0.89331(17) 0.14474(15) 0.0289(4) Uani 1 1 d . . . H5 H 0.8542 0.9321 0.1074 0.035 Uiso 1 1 calc R . . C6 C 0.6606(2) 0.81721(18) 0.10037(15) 0.0294(4) Uani 1 1 d . . . H6 H 0.6229 0.8035 0.0325 0.035 Uiso 1 1 calc R . . C7 C 0.5784(2) 0.76107(16) 0.15571(14) 0.0244(4) Uani 1 1 d . . . H7 H 0.4836 0.7105 0.1249 0.029 Uiso 1 1 calc R . . C8 C 0.32858(19) 0.69247(14) 0.28043(12) 0.0172(3) Uani 1 1 d . . . C9 C 0.2998(2) 0.79343(15) 0.26559(14) 0.0231(4) Uani 1 1 d . . . H9 H 0.3795 0.8602 0.281 0.028 Uiso 1 1 calc R . . C10 C 0.1575(2) 0.79778(16) 0.22893(14) 0.0253(4) Uani 1 1 d . . . H10 H 0.1406 0.8671 0.2195 0.03 Uiso 1 1 calc R . . C11 C 0.0402(2) 0.70121(17) 0.20612(14) 0.0244(4) Uani 1 1 d . . . H11 H -0.0574 0.7041 0.1814 0.029 Uiso 1 1 calc R . . C12 C 0.0656(2) 0.60041(16) 0.21951(14) 0.0252(4) Uani 1 1 d . . . H12 H -0.0147 0.534 0.2036 0.03 Uiso 1 1 calc R . . C13 C 0.2084(2) 0.59603(15) 0.25623(14) 0.0218(4) Uani 1 1 d . . . H13 H 0.2244 0.5263 0.265 0.026 Uiso 1 1 calc R . . C14 C 0.60792(19) 0.75861(14) 0.45609(12) 0.0170(3) Uani 1 1 d . . . C15 C 0.75210(19) 0.75985(15) 0.50126(13) 0.0197(3) Uani 1 1 d . . . H15 H 0.7981 0.7179 0.4693 0.024 Uiso 1 1 calc R . . C16 C 0.8293(2) 0.82120(16) 0.59187(13) 0.0249(4) Uani 1 1 d . . . H16 H 0.9278 0.8226 0.6206 0.03 Uiso 1 1 calc R . . C17 C 0.7615(2) 0.88018(16) 0.63981(14) 0.0267(4) Uani 1 1 d . . . H17 H 0.8137 0.9222 0.7017 0.032 Uiso 1 1 calc R . . C18 C 0.6183(2) 0.87803(16) 0.59793(14) 0.0267(4) Uani 1 1 d . . . H18 H 0.5717 0.9174 0.6317 0.032 Uiso 1 1 calc R . . C19 C 0.5417(2) 0.81855(15) 0.50656(13) 0.0208(4) Uani 1 1 d . . . H19 H 0.4437 0.8185 0.4781 0.025 Uiso 1 1 calc R . . Si2 Si 0.65267(5) 0.26504(4) 0.24025(3) 0.01560(9) Uani 1 1 d . . . O21 O 0.60713(13) 0.37797(10) 0.26813(9) 0.0174(2) Uani 1 1 d . . . C22 C 0.4837(2) 0.15051(14) 0.16981(12) 0.0181(3) Uani 1 1 d . . . C23 C 0.3425(2) 0.16107(16) 0.15364(13) 0.0217(4) Uani 1 1 d . . . H23 H 0.3309 0.2288 0.1785 0.026 Uiso 1 1 calc R . . C24 C 0.2183(2) 0.07438(17) 0.10185(14) 0.0281(4) Uani 1 1 d . . . H24 H 0.1233 0.0832 0.0918 0.034 Uiso 1 1 calc R . . C25 C 0.2339(2) -0.02468(17) 0.06510(14) 0.0313(5) Uani 1 1 d . . . H25 H 0.1494 -0.0843 0.0304 0.038 Uiso 1 1 calc R . . C26 C 0.3721(3) -0.03665(16) 0.07895(15) 0.0332(5) Uani 1 1 d . . . H26 H 0.3828 -0.1044 0.0531 0.04 Uiso 1 1 calc R . . C27 C 0.4957(2) 0.04975(16) 0.13040(14) 0.0263(4) Uani 1 1 d . . . H27 H 0.5904 0.0404 0.1391 0.032 Uiso 1 1 calc R . . C28 C 0.7469(2) 0.22488(15) 0.35436(13) 0.0198(4) Uani 1 1 d . . . C29 C 0.7205(2) 0.11529(17) 0.37129(14) 0.0254(4) Uani 1 1 d . . . H29 H 0.6564 0.0566 0.3216 0.03 Uiso 1 1 calc R . . C30 C 0.7860(2) 0.0902(2) 0.45941(16) 0.0327(5) Uani 1 1 d . . . H30 H 0.7671 0.015 0.4694 0.039 Uiso 1 1 calc R . . C31 C 0.8788(2) 0.1749(2) 0.53230(15) 0.0357(5) Uani 1 1 d . . . H31 H 0.9217 0.1582 0.5931 0.043 Uiso 1 1 calc R . . C32 C 0.9090(2) 0.2835(2) 0.51694(15) 0.0356(5) Uani 1 1 d . . . H32 H 0.9739 0.3416 0.5669 0.043 Uiso 1 1 calc R . . C33 C 0.8449(2) 0.30876(17) 0.42840(14) 0.0267(4) Uani 1 1 d . . . H33 H 0.8681 0.3839 0.4181 0.032 Uiso 1 1 calc R . . C34 C 0.78103(19) 0.29710(14) 0.16401(13) 0.0179(3) Uani 1 1 d . . . C35 C 0.9245(2) 0.28952(16) 0.19405(14) 0.0247(4) Uani 1 1 d . . . H35 H 0.9578 0.2682 0.2545 0.03 Uiso 1 1 calc R . . C36 C 1.0189(2) 0.31247(17) 0.13746(15) 0.0287(4) Uani 1 1 d . . . H36 H 1.1153 0.3062 0.1592 0.034 Uiso 1 1 calc R . . C37 C 0.9727(2) 0.34451(17) 0.04937(14) 0.0279(4) Uani 1 1 d . . . H37 H 1.0376 0.3607 0.0108 0.033 Uiso 1 1 calc R . . C38 C 0.8315(2) 0.35292(17) 0.01749(14) 0.0273(4) Uani 1 1 d . . . H38 H 0.7995 0.3751 -0.0428 0.033 Uiso 1 1 calc R . . C39 C 0.7368(2) 0.32861(15) 0.07431(13) 0.0215(4) Uani 1 1 d . . . H39 H 0.6399 0.3335 0.0516 0.026 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 0.01878(6) 0.01710(6) 0.02414(7) 0.00493(5) 0.01120(5) 0.00565(5) Sn2 0.02205(7) 0.01466(6) 0.02061(7) 0.00302(4) 0.00970(5) 0.00518(5) Cl1 0.0276(2) 0.0308(2) 0.0247(2) 0.00375(19) 0.00279(19) 0.00824(19) Cl2 0.0295(2) 0.0272(2) 0.0218(2) 0.00417(17) 0.00764(18) 0.01444(18) Si1 0.0149(2) 0.0129(2) 0.0158(2) 0.00126(17) 0.00368(17) 0.00385(17) O1 0.0194(6) 0.0143(6) 0.0182(6) 0.0021(5) 0.0063(5) 0.0060(5) C2 0.0188(8) 0.0133(7) 0.0180(8) 0.0032(6) 0.0060(7) 0.0060(6) C3 0.0208(9) 0.0255(9) 0.0196(9) 0.0015(7) 0.0046(7) 0.0034(7) C4 0.0193(9) 0.0303(10) 0.0317(11) 0.0062(8) 0.0078(8) 0.0005(8) C5 0.0273(10) 0.0334(11) 0.0312(11) 0.0149(9) 0.0151(9) 0.0086(8) C6 0.0328(11) 0.0352(11) 0.0195(10) 0.0099(8) 0.0066(8) 0.0085(9) C7 0.0244(9) 0.0231(9) 0.0209(9) 0.0049(7) 0.0022(7) 0.0032(7) C8 0.0173(8) 0.0193(8) 0.0158(8) 0.0024(6) 0.0053(7) 0.0061(7) C9 0.0227(9) 0.0177(8) 0.0289(10) 0.0048(7) 0.0083(8) 0.0047(7) C10 0.0275(10) 0.0242(9) 0.0298(10) 0.0097(8) 0.0100(8) 0.0136(8) C11 0.0200(9) 0.0319(10) 0.0233(10) 0.0050(8) 0.0057(7) 0.0115(8) C12 0.0181(9) 0.0240(9) 0.0291(10) 0.0002(8) 0.0047(8) 0.0026(7) C13 0.0208(9) 0.0179(8) 0.0251(10) 0.0027(7) 0.0045(7) 0.0054(7) C14 0.0180(8) 0.0143(8) 0.0169(8) 0.0028(6) 0.0054(7) 0.0017(6) C15 0.0200(9) 0.0204(8) 0.0192(9) 0.0042(7) 0.0068(7) 0.0056(7) C16 0.0209(9) 0.0298(10) 0.0196(9) 0.0068(8) 0.0036(7) 0.0018(8) C17 0.0284(10) 0.0253(9) 0.0172(9) -0.0013(7) 0.0064(8) -0.0052(8) C18 0.0300(10) 0.0228(9) 0.0266(10) -0.0026(8) 0.0162(8) 0.0009(8) C19 0.0186(8) 0.0196(8) 0.0239(9) 0.0021(7) 0.0082(7) 0.0038(7) Si2 0.0171(2) 0.0154(2) 0.0161(2) 0.00238(17) 0.00564(18) 0.00692(18) O21 0.0204(6) 0.0163(6) 0.0180(6) 0.0025(5) 0.0071(5) 0.0081(5) C22 0.0229(9) 0.0175(8) 0.0145(8) 0.0035(6) 0.0071(7) 0.0050(7) C23 0.0226(9) 0.0234(9) 0.0188(9) 0.0030(7) 0.0074(7) 0.0053(7) C24 0.0234(10) 0.0338(11) 0.0220(10) 0.0057(8) 0.0047(8) 0.0018(8) C25 0.0354(11) 0.0231(10) 0.0221(10) 0.0044(8) 0.0012(8) -0.0062(8) C26 0.0487(13) 0.0174(9) 0.0283(11) -0.0008(8) 0.0065(9) 0.0074(9) C27 0.0332(11) 0.0221(9) 0.0244(10) 0.0015(7) 0.0069(8) 0.0114(8) C28 0.0206(9) 0.0255(9) 0.0191(9) 0.0060(7) 0.0089(7) 0.0128(7) C29 0.0256(10) 0.0287(10) 0.0267(10) 0.0097(8) 0.0109(8) 0.0113(8) C30 0.0333(11) 0.0426(12) 0.0350(12) 0.0218(10) 0.0166(9) 0.0214(10) C31 0.0351(12) 0.0657(16) 0.0218(10) 0.0175(10) 0.0126(9) 0.0334(11) C32 0.0310(11) 0.0545(14) 0.0218(10) -0.0049(9) 0.0004(8) 0.0238(10) C33 0.0258(10) 0.0304(10) 0.0259(10) 0.0007(8) 0.0047(8) 0.0153(8) C34 0.0184(8) 0.0160(8) 0.0191(9) 0.0002(6) 0.0064(7) 0.0049(6) C35 0.0246(9) 0.0275(10) 0.0262(10) 0.0073(8) 0.0086(8) 0.0126(8) C36 0.0213(9) 0.0325(11) 0.0354(11) 0.0029(9) 0.0110(8) 0.0113(8) C37 0.0246(10) 0.0323(10) 0.0264(10) -0.0014(8) 0.0146(8) 0.0028(8) C38 0.0271(10) 0.0333(11) 0.0177(9) 0.0005(8) 0.0069(8) 0.0037(8) C39 0.0181(8) 0.0260(9) 0.0182(9) -0.0006(7) 0.0039(7) 0.0058(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O21 2.1558(12) . ? Sn1 O1 2.1944(12) . ? Sn1 Cl1 2.4525(5) . ? Sn2 O1 2.1851(12) . ? Sn2 O21 2.2694(12) . ? Sn2 Cl2 2.4733(5) . ? Si1 O1 1.6623(12) . ? Si1 C8 1.8615(18) . ? Si1 C14 1.8700(18) . ? Si1 C2 1.8884(18) . ? C2 C3 1.395(2) . ? C2 C7 1.401(2) . ? C3 C4 1.390(3) . ? C3 H3 0.95 . ? C4 C5 1.374(3) . ? C4 H4 0.95 . ? C5 C6 1.387(3) . ? C5 H5 0.95 . ? C6 C7 1.392(3) . ? C6 H6 0.95 . ? C7 H7 0.95 . ? C8 C13 1.398(2) . ? C8 C9 1.403(2) . ? C9 C10 1.387(3) . ? C9 H9 0.95 . ? C10 C11 1.385(3) . ? C10 H10 0.95 . ? C11 C12 1.384(3) . ? C11 H11 0.95 . ? C12 C13 1.391(3) . ? C12 H12 0.95 . ? C13 H13 0.95 . ? C14 C15 1.402(2) . ? C14 C19 1.403(2) . ? C15 C16 1.391(3) . ? C15 H15 0.95 . ? C16 C17 1.385(3) . ? C16 H16 0.95 . ? C17 C18 1.381(3) . ? C17 H17 0.95 . ? C18 C19 1.391(3) . ? C18 H18 0.95 . ? C19 H19 0.95 . ? Si2 O21 1.6586(12) . ? Si2 C28 1.8738(18) . ? Si2 C22 1.8746(18) . ? Si2 C34 1.8793(18) . ? C22 C23 1.397(3) . ? C22 C27 1.402(2) . ? C23 C24 1.394(3) . ? C23 H23 0.95 . ? C24 C25 1.384(3) . ? C24 H24 0.95 . ? C25 C26 1.378(3) . ? C25 H25 0.95 . ? C26 C27 1.388(3) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C29 1.395(3) . ? C28 C33 1.399(3) . ? C29 C30 1.390(3) . ? C29 H29 0.95 . ? C30 C31 1.381(3) . ? C30 H30 0.95 . ? C31 C32 1.375(3) . ? C31 H31 0.95 . ? C32 C33 1.392(3) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 C39 1.400(3) . ? C34 C35 1.403(3) . ? C35 C36 1.388(3) . ? C35 H35 0.95 . ? C36 C37 1.385(3) . ? C36 H36 0.95 . ? C37 C38 1.388(3) . ? C37 H37 0.95 . ? C38 C39 1.393(3) . ? C38 H38 0.95 . ? C39 H39 0.95 . ? 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 O21 Sn1 O1 76.68(4) . . ? O21 Sn1 Cl1 90.72(3) . . ? O1 Sn1 Cl1 89.09(3) . . ? O1 Sn2 O21 74.56(4) . . ? O1 Sn2 Cl2 90.76(3) . . ? O21 Sn2 Cl2 93.91(3) . . ? O1 Si1 C8 111.68(7) . . ? O1 Si1 C14 111.31(7) . . ? C8 Si1 C14 113.02(8) . . ? O1 Si1 C2 105.64(7) . . ? C8 Si1 C2 107.57(8) . . ? C14 Si1 C2 107.18(8) . . ? Si1 O1 Sn2 135.78(7) . . ? Si1 O1 Sn1 119.83(6) . . ? Sn2 O1 Sn1 104.08(5) . . ? C3 C2 C7 117.23(16) . . ? C3 C2 Si1 122.67(13) . . ? C7 C2 Si1 120.04(13) . . ? C4 C3 C2 121.30(18) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 120.49(18) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.74(18) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 119.72(19) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 121.48(18) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? C13 C8 C9 117.50(16) . . ? C13 C8 Si1 123.51(13) . . ? C9 C8 Si1 118.97(13) . . ? C10 C9 C8 121.37(17) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 120.04(18) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C12 C11 C10 119.76(18) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.19(18) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 121.13(17) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? C15 C14 C19 117.80(16) . . ? C15 C14 Si1 118.62(13) . . ? C19 C14 Si1 123.14(14) . . ? C16 C15 C14 121.42(17) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.52(18) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 120.20(18) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.45(18) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 120.57(17) . . ? C18 C19 H19 119.7 . . ? C14 C19 H19 119.7 . . ? O21 Si2 C28 108.11(7) . . ? O21 Si2 C22 109.72(7) . . ? C28 Si2 C22 111.49(8) . . ? O21 Si2 C34 109.19(7) . . ? C28 Si2 C34 109.89(8) . . ? C22 Si2 C34 108.42(8) . . ? Si2 O21 Sn1 125.56(7) . . ? Si2 O21 Sn2 130.90(7) . . ? Sn1 O21 Sn2 102.55(5) . . ? C23 C22 C27 117.28(17) . . ? C23 C22 Si2 122.44(13) . . ? C27 C22 Si2 120.28(14) . . ? C24 C23 C22 121.44(18) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 119.83(19) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 119.85(18) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.29(19) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C22 121.29(19) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C29 C28 C33 117.64(17) . . ? C29 C28 Si2 123.46(15) . . ? C33 C28 Si2 118.85(14) . . ? C30 C29 C28 121.3(2) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 C29 119.8(2) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 120.03(19) . . ? C32 C31 H31 120 . . ? C30 C31 H31 120 . . ? C31 C32 C33 120.2(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.9(2) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? C39 C34 C35 117.17(16) . . ? C39 C34 Si2 121.29(13) . . ? C35 C34 Si2 121.53(14) . . ? C36 C35 C34 121.51(18) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C37 C36 C35 120.09(18) . . ? C37 C36 H36 120 . . ? C35 C36 H36 120 . . ? C36 C37 C38 119.88(18) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C37 C38 C39 119.67(19) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C34 121.67(17) . . ? C38 C39 H39 119.2 . . ? C34 C39 H39 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 Si1 O1 Sn2 -66.38(12) . . . . ? C14 Si1 O1 Sn2 60.97(12) . . . . ? C2 Si1 O1 Sn2 176.96(9) . . . . ? C8 Si1 O1 Sn1 106.07(8) . . . . ? C14 Si1 O1 Sn1 -126.59(8) . . . . ? C2 Si1 O1 Sn1 -10.59(9) . . . . ? O21 Sn2 O1 Si1 -175.74(11) . . . . ? Cl2 Sn2 O1 Si1 -81.89(10) . . . . ? O21 Sn2 O1 Sn1 11.01(4) . . . . ? Cl2 Sn2 O1 Sn1 104.86(4) . . . . ? O21 Sn1 O1 Si1 173.94(8) . . . . ? Cl1 Sn1 O1 Si1 -95.10(7) . . . . ? O21 Sn1 O1 Sn2 -11.49(5) . . . . ? Cl1 Sn1 O1 Sn2 79.47(4) . . . . ? O1 Si1 C2 C3 -103.81(15) . . . . ? C8 Si1 C2 C3 136.78(15) . . . . ? C14 Si1 C2 C3 14.97(17) . . . . ? O1 Si1 C2 C7 73.36(15) . . . . ? C8 Si1 C2 C7 -46.04(16) . . . . ? C14 Si1 C2 C7 -167.86(14) . . . . ? C7 C2 C3 C4 0.1(3) . . . . ? Si1 C2 C3 C4 177.35(15) . . . . ? C2 C3 C4 C5 -1.4(3) . . . . ? C3 C4 C5 C6 1.2(3) . . . . ? C4 C5 C6 C7 0.2(3) . . . . ? C5 C6 C7 C2 -1.6(3) . . . . ? C3 C2 C7 C6 1.4(3) . . . . ? Si1 C2 C7 C6 -175.95(16) . . . . ? O1 Si1 C8 C13 15.58(18) . . . . ? C14 Si1 C8 C13 -110.84(16) . . . . ? C2 Si1 C8 C13 131.05(15) . . . . ? O1 Si1 C8 C9 -162.63(14) . . . . ? C14 Si1 C8 C9 70.96(16) . . . . ? C2 Si1 C8 C9 -47.15(16) . . . . ? C13 C8 C9 C10 0.4(3) . . . . ? Si1 C8 C9 C10 178.74(15) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C9 C10 C11 C12 -0.4(3) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? C11 C12 C13 C8 0.1(3) . . . . ? C9 C8 C13 C12 -0.5(3) . . . . ? Si1 C8 C13 C12 -178.71(15) . . . . ? O1 Si1 C14 C15 50.77(15) . . . . ? C8 Si1 C14 C15 177.38(13) . . . . ? C2 Si1 C14 C15 -64.28(15) . . . . ? O1 Si1 C14 C19 -137.03(14) . . . . ? C8 Si1 C14 C19 -10.42(17) . . . . ? C2 Si1 C14 C19 107.92(15) . . . . ? C19 C14 C15 C16 -2.0(3) . . . . ? Si1 C14 C15 C16 170.58(14) . . . . ? C14 C15 C16 C17 1.7(3) . . . . ? C15 C16 C17 C18 0.0(3) . . . . ? C16 C17 C18 C19 -1.3(3) . . . . ? C17 C18 C19 C14 0.9(3) . . . . ? C15 C14 C19 C18 0.8(3) . . . . ? Si1 C14 C19 C18 -171.51(14) . . . . ? C28 Si2 O21 Sn1 135.62(9) . . . . ? C22 Si2 O21 Sn1 -102.60(9) . . . . ? C34 Si2 O21 Sn1 16.10(11) . . . . ? C28 Si2 O21 Sn2 -57.81(11) . . . . ? C22 Si2 O21 Sn2 63.97(11) . . . . ? C34 Si2 O21 Sn2 -177.34(8) . . . . ? O1 Sn1 O21 Si2 -179.38(9) . . . . ? Cl1 Sn1 O21 Si2 91.73(8) . . . . ? O1 Sn1 O21 Sn2 10.98(4) . . . . ? Cl1 Sn1 O21 Sn2 -77.91(4) . . . . ? O1 Sn2 O21 Si2 -179.97(10) . . . . ? Cl2 Sn2 O21 Si2 90.32(9) . . . . ? O1 Sn2 O21 Sn1 -11.14(5) . . . . ? Cl2 Sn2 O21 Sn1 -100.85(4) . . . . ? O21 Si2 C22 C23 -5.46(17) . . . . ? C28 Si2 C22 C23 114.27(15) . . . . ? C34 Si2 C22 C23 -124.63(15) . . . . ? O21 Si2 C22 C27 174.11(14) . . . . ? C28 Si2 C22 C27 -66.15(16) . . . . ? C34 Si2 C22 C27 54.95(17) . . . . ? C27 C22 C23 C24 1.1(3) . . . . ? Si2 C22 C23 C24 -179.35(14) . . . . ? C22 C23 C24 C25 -0.1(3) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? C24 C25 C26 C27 0.7(3) . . . . ? C25 C26 C27 C22 0.3(3) . . . . ? C23 C22 C27 C26 -1.2(3) . . . . ? Si2 C22 C27 C26 179.25(16) . . . . ? O21 Si2 C28 C29 137.81(15) . . . . ? C22 Si2 C28 C29 17.13(18) . . . . ? C34 Si2 C28 C29 -103.11(16) . . . . ? O21 Si2 C28 C33 -39.68(16) . . . . ? C22 Si2 C28 C33 -160.36(14) . . . . ? C34 Si2 C28 C33 79.41(16) . . . . ? C33 C28 C29 C30 1.7(3) . . . . ? Si2 C28 C29 C30 -175.84(15) . . . . ? C28 C29 C30 C31 0.3(3) . . . . ? C29 C30 C31 C32 -1.6(3) . . . . ? C30 C31 C32 C33 0.8(3) . . . . ? C31 C32 C33 C28 1.3(3) . . . . ? C29 C28 C33 C32 -2.5(3) . . . . ? Si2 C28 C33 C32 175.17(15) . . . . ? O21 Si2 C34 C39 -62.05(16) . . . . ? C28 Si2 C34 C39 179.53(14) . . . . ? C22 Si2 C34 C39 57.45(16) . . . . ? O21 Si2 C34 C35 118.55(15) . . . . ? C28 Si2 C34 C35 0.13(17) . . . . ? C22 Si2 C34 C35 -121.95(15) . . . . ? C39 C34 C35 C36 0.1(3) . . . . ? Si2 C34 C35 C36 179.56(15) . . . . ? C34 C35 C36 C37 0.5(3) . . . . ? C35 C36 C37 C38 -0.4(3) . . . . ? C36 C37 C38 C39 -0.2(3) . . . . ? C37 C38 C39 C34 0.9(3) . . . . ? C35 C34 C39 C38 -0.8(3) . . . . ? Si2 C34 C39 C38 179.76(15) . . . . ? #===END data_{Sn(OiPr}{Cl}}2 _audit_creation_date 2013-04-23T16:00:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C6 H14 Cl2 O2 Sn2' _chemical_formula_sum 'C6 H14 Cl2 O2 Sn2' _chemical_formula_weight 426.45 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 6.6503(3) _cell_length_b 10.2650(4) _cell_length_c 9.0775(3) _cell_angle_alpha 90 _cell_angle_beta 104.8330(10) _cell_angle_gamma 90 _cell_volume 599.03(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3277 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.48 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.580 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.461 _exptl_absorpt_correction_T_max 0.760 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_number 5006 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 1368 _reflns_number_gt 1310 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.5435P] 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_number_reflns 1368 _refine_ls_number_parameters 57 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.852 _refine_diff_density_min -1.474 _refine_diff_density_rms 0.177 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 21/a CELL 0.71073 6.6503 10.2650 9.0775 90.000 104.833 90.000 ZERR 2.00 0.0003 0.0004 0.0003 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H O SN CL UNIT 12 28 4 4 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.041000 0.543500 FVAR 0.59355 SN1 4 0.804090 0.101536 0.530161 11.00000 0.02057 0.01826 = 0.01798 -0.00033 0.00698 0.00273 CL 5 0.666475 -0.077489 0.668773 11.00000 0.01966 0.03292 = 0.02466 0.00718 0.00953 0.00116 O1 3 0.881435 -0.028388 0.372061 11.00000 0.01579 0.02525 = 0.01511 -0.00092 0.00540 0.00153 C2 1 0.763189 -0.042575 0.214809 11.00000 0.01750 0.02068 = 0.01821 -0.00160 0.00532 -0.00296 AFIX 13 H2 2 0.618582 -0.070063 0.213794 11.00000 -1.20000 AFIX 0 C3 1 0.860107 -0.147992 0.137541 11.00000 0.02633 0.02913 = 0.02241 -0.00691 0.00361 0.00212 AFIX 137 H3A 2 1.000329 -0.121184 0.134264 11.00000 -1.50000 H3B 2 0.774359 -0.161314 0.033478 11.00000 -1.50000 H3C 2 0.868126 -0.229453 0.195056 11.00000 -1.50000 AFIX 0 C4 1 0.751655 0.086006 0.132679 11.00000 0.02735 0.02924 = 0.02085 0.00531 0.00343 -0.00062 AFIX 137 H4A 2 0.680666 0.150127 0.181575 11.00000 -1.50000 H4B 2 0.674147 0.074847 0.026039 11.00000 -1.50000 H4C 2 0.892657 0.116596 0.137054 11.00000 -1.50000 HKLF 4 REM import in P 21/a REM R1 = 0.0282 for 1310 Fo > 4sig(Fo) and 0.0295 for all 1368 data REM 57 parameters refined using 0 restraints END WGHT 0.0411 0.5357 REM Highest difference peak 0.85, deepest hole -1.47, 1-sigma level 0.18 Q1 1 0.8752 0.1018 0.3577 11.00000 0.05 0.85 Q2 1 0.8725 0.0323 0.4248 11.00000 0.05 0.83 Q3 1 0.7534 0.1012 0.6881 11.00000 0.05 0.74 Q4 1 0.8560 0.1483 0.6071 11.00000 0.05 0.69 Q5 1 0.7764 0.1593 0.6150 11.00000 0.05 0.65 Q6 1 0.6577 0.0138 0.6634 11.00000 0.05 0.65 Q7 1 0.8421 -0.3174 0.3396 11.00000 0.05 0.63 Q8 1 0.7465 0.0367 0.6344 11.00000 0.05 0.62 Q9 1 0.9123 0.1760 0.4224 11.00000 0.05 0.57 Q10 1 0.7701 0.1451 0.4479 11.00000 0.05 0.52 Q11 1 1.0963 0.0229 0.3533 11.00000 0.05 0.52 Q12 1 0.7485 0.0042 0.1615 11.00000 0.05 0.50 Q13 1 0.7279 0.1144 0.4450 11.00000 0.05 0.48 Q14 1 0.6458 0.0168 0.4822 11.00000 0.05 0.47 Q15 1 0.8196 -0.4023 0.2435 11.00000 0.05 0.45 Q16 1 0.7273 0.2386 0.4233 11.00000 0.05 0.45 Q17 1 1.0440 -0.0984 0.2780 11.00000 0.05 0.44 Q18 1 1.0201 -0.0345 0.1582 11.00000 0.05 0.43 Q19 1 0.5152 0.0214 0.6389 11.00000 0.05 0.42 Q20 1 0.8089 0.0165 0.3004 11.00000 0.05 0.42 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.80409(3) 0.10154(2) 0.53016(2) 0.01856(12) Uani 1 1 d . . . Cl Cl 0.66647(13) -0.07749(9) 0.66877(11) 0.0250(2) Uani 1 1 d . . . O1 O 0.8814(3) -0.0284(2) 0.3721(3) 0.0185(5) Uani 1 1 d . . . C2 C 0.7632(5) -0.0426(3) 0.2148(4) 0.0187(6) Uani 1 1 d . . . H2 H 0.6186 -0.0701 0.2138 0.022 Uiso 1 1 calc R . . C3 C 0.8601(5) -0.1480(4) 0.1375(4) 0.0264(7) Uani 1 1 d . . . H3A H 1.0003 -0.1212 0.1343 0.04 Uiso 1 1 calc R . . H3B H 0.7744 -0.1613 0.0335 0.04 Uiso 1 1 calc R . . H3C H 0.8681 -0.2295 0.1951 0.04 Uiso 1 1 calc R . . C4 C 0.7517(6) 0.0860(3) 0.1327(5) 0.0263(8) Uani 1 1 d . . . H4A H 0.6807 0.1501 0.1816 0.039 Uiso 1 1 calc R . . H4B H 0.6741 0.0748 0.026 0.039 Uiso 1 1 calc R . . H4C H 0.8927 0.1166 0.1371 0.039 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 0.02057(16) 0.01826(18) 0.01798(18) -0.00033(8) 0.00698(11) 0.00273(7) Cl 0.0197(4) 0.0329(5) 0.0247(5) 0.0072(4) 0.0095(3) 0.0012(3) O1 0.0158(10) 0.0252(12) 0.0151(11) -0.0009(10) 0.0054(8) 0.0015(9) C2 0.0175(14) 0.0207(17) 0.0182(16) -0.0016(13) 0.0053(12) -0.0030(11) C3 0.0263(17) 0.029(2) 0.0224(18) -0.0069(16) 0.0036(14) 0.0021(15) C4 0.0273(19) 0.029(2) 0.0208(18) 0.0053(14) 0.0034(15) -0.0006(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O1 2.117(2) . ? Sn1 O1 2.185(2) 3_756 ? Sn1 Cl 2.5273(9) . ? O1 C2 1.450(4) . ? C2 C4 1.508(5) . ? C2 C3 1.520(5) . ? C2 H2 1 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? 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 O1 Sn1 O1 71.67(10) . 3_756 ? O1 Sn1 Cl 93.51(7) . . ? O1 Sn1 Cl 88.79(6) 3_756 . ? C2 O1 Sn1 124.48(18) . . ? C2 O1 Sn1 125.93(18) . 3_756 ? Sn1 O1 Sn1 108.33(10) . 3_756 ? O1 C2 C4 110.2(3) . . ? O1 C2 C3 109.8(3) . . ? C4 C2 C3 111.6(3) . . ? O1 C2 H2 108.4 . . ? C4 C2 H2 108.4 . . ? C3 C2 H2 108.4 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Sn1 O1 C2 -167.8(3) 3_756 . . . ? Cl Sn1 O1 C2 104.7(2) . . . . ? O1 Sn1 O1 Sn1 0 3_756 . . 3_756 ? Cl Sn1 O1 Sn1 -87.55(9) . . . 3_756 ? Sn1 O1 C2 C4 58.7(3) . . . . ? Sn1 O1 C2 C4 -106.9(3) 3_756 . . . ? Sn1 O1 C2 C3 -177.9(2) . . . . ? Sn1 O1 C2 C3 16.4(4) 3_756 . . . ? #===END