#------------------------------------------------------------------------------ #$Date: 2009-11-16 02:43:51 +0100 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003391.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003391 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 631 _journal_page_last 633 _publ_section_title ; N-(1-Adamantyl)-[(pentafluoro-2-propenyl)thio]amino(fluoro)bis[2,4,6- tris(trifluoromethyl)phenyl]tin at 153K ; _chemical_formula_moiety '[Sn F (C9 H2 F9)2 {(C3 F5 S) (C10 H15) N}]' _chemical_formula_sum 'C31 H19 F24 N S Sn' _chemical_formula_weight 1012.22 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.168(2) _cell_length_b 13.323(2) _cell_length_c 19.470(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.72(1) _cell_angle_gamma 90.00 _cell_volume 3519.8(9) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 58 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_absorpt_coefficient_mu 0.939 _cell_measurement_temperature 153(2) _exptl_crystal_description blocks _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_colour yellow _chemical_compound_source ? _diffrn_measurement_device 'Stoe Siemens AED' _diffrn_measurement_method 'profile data from \w/2\q scans' _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.72637 _exptl_absorpt_correction_T_max 0.93230 _diffrn_reflns_number 5172 _reflns_number_total 4632 _reflns_number_observed 3627 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0623 _diffrn_reflns_theta_max 22.57 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0422 _refine_ls_wR_factor_obs 0.0895 _refine_ls_wR_factor_all 0.1022 _refine_ls_goodness_of_fit_obs 1.050 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_number_reflns 4631 _refine_ls_number_parameters 533 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^) + (0.0338P)^2^ + 15.3065P] where P = (F~o~^2^ +2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.004 _refine_diff_density_max 1.684 _refine_diff_density_min -.543 _refine_ls_extinction_method none loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv S1 1 0.33721(12) 0.31746(12) 0.04144(8) 0.0327(4) C1 1 0.4118(5) 0.3223(5) -0.0168(3) 0.038(2) C2 1 0.5197(6) 0.3378(6) 0.0114(4) 0.055(2) F1 1 0.5410(3) 0.4128(4) 0.0589(3) 0.0791(15) F2 1 0.5637(4) 0.3580(5) -0.0387(3) 0.102(2) F3 1 0.5649(3) 0.2585(4) 0.0469(3) 0.0713(14) C3 1 0.3662(6) 0.3241(6) -0.0865(4) 0.055(2) F4 1 0.2699(4) 0.3171(4) -0.1147(2) 0.0717(14) F5 1 0.4062(4) 0.3394(5) -0.1378(2) 0.093(2) Sn1 1 0.40978(3) 0.23338(3) 0.19549(2) 0.02346(14) F6 1 0.2985(2) 0.1933(2) 0.2282(2) 0.0304(8) C4 1 0.5065(4) 0.1360(4) 0.2760(3) 0.0231(13) C5 1 0.5691(4) 0.0624(4) 0.2628(3) 0.0260(14) C6 1 0.6139(4) -0.0093(5) 0.3142(3) 0.033(2) H6 1 0.6537(4) -0.0604(5) 0.3029(3) 0.039 C7 1 0.6002(5) -0.0057(5) 0.3811(3) 0.034(2) C8 1 0.5442(4) 0.0688(5) 0.3976(3) 0.033(2) H8 1 0.5367(4) 0.0724(5) 0.4445(3) 0.040 C9 1 0.4984(4) 0.1391(4) 0.3468(3) 0.0256(14) C10 1 0.6006(4) 0.0560(5) 0.1961(3) 0.033(2) F7 1 0.5983(3) -0.0368(3) 0.1715(2) 0.0507(11) F8 1 0.5484(2) 0.1132(3) 0.1425(2) 0.0352(9) F9 1 0.6947(3) 0.0877(3) 0.2092(2) 0.0464(10) C11 1 0.6499(5) -0.0809(6) 0.4383(4) 0.052(2) F10 0.843(8) 0.7038(6) -0.1470(5) 0.4155(3) 0.077(2) F11 0.843(8) 0.5835(5) -0.1369(6) 0.4562(4) 0.091(3) F12 0.843(8) 0.7041(8) -0.0405(5) 0.4949(4) 0.111(4) F10' 0.157(8) 0.6234(31) -0.0686(31) 0.4949(16) 0.077(2) F11' 0.157(8) 0.7446(16) -0.0555(31) 0.4560(23) 0.091(3) F12' 0.157(8) 0.6458(37) -0.1725(17) 0.4208(19) 0.111(4) C12 1 0.4431(4) 0.2184(5) 0.3743(3) 0.0318(15) F13 1 0.4302(3) 0.3025(2) 0.3356(2) 0.0373(9) F14 1 0.3556(3) 0.1898(3) 0.3792(2) 0.0387(9) F15 1 0.4942(3) 0.2456(3) 0.4415(2) 0.0414(9) C13 1 0.4293(4) 0.3947(4) 0.2120(3) 0.0229(13) C14 1 0.5246(4) 0.4357(4) 0.2317(3) 0.0257(14) C15 1 0.5414(4) 0.5355(5) 0.2507(3) 0.0311(15) H15 1 0.6068(4) 0.5609(5) 0.2648(3) 0.037 C16 1 0.4637(4) 0.5980(4) 0.2493(3) 0.0279(14) C17 1 0.3691(5) 0.5608(5) 0.2293(3) 0.034(2) H17 1 0.3153(5) 0.6038(5) 0.2285(3) 0.041 C18 1 0.3523(4) 0.4608(4) 0.2103(3) 0.0290(14) C19 1 0.6143(5) 0.3739(5) 0.2356(4) 0.037(2) F16 1 0.6794(3) 0.4243(3) 0.2115(3) 0.0625(13) F17 1 0.5930(2) 0.2914(3) 0.1946(2) 0.0381(9) F18 1 0.6587(3) 0.3430(4) 0.3007(2) 0.0717(15) C20 1 0.4797(6) 0.7069(5) 0.2695(4) 0.048(2) F19 1 0.5734(3) 0.7326(3) 0.2847(3) 0.0740(15) F20 1 0.4490(4) 0.7296(4) 0.3252(3) 0.085(2) F21 1 0.4325(4) 0.7669(3) 0.2169(3) 0.089(2) C21 1 0.2461(5) 0.4269(5) 0.1914(4) 0.041(2) F22 1 0.2263(2) 0.3512(3) 0.1459(2) 0.0374(9) F23 1 0.2225(3) 0.3960(4) 0.2493(2) 0.0721(15) F24 1 0.1854(3) 0.4989(3) 0.1640(4) 0.098(2) N1 1 0.3632(3) 0.2081(3) 0.0878(2) 0.0264(12) C22 1 0.2979(4) 0.1201(4) 0.0584(3) 0.0293(14) C23 1 0.3286(5) 0.0310(5) 0.1093(3) 0.037(2) H23A 1 0.3227(5) 0.0493(5) 0.1572(3) 0.044 H23B 1 0.3984(5) 0.0140(5) 0.1146(3) 0.044 C24 1 0.3076(5) 0.0914(5) -0.0150(3) 0.045(2) H24A 1 0.3770(5) 0.0742(5) -0.0108(3) 0.053 H24B 1 0.2885(5) 0.1490(5) -0.0482(3) 0.053 C25 1 0.1893(4) 0.1446(5) 0.0514(4) 0.037(2) H25A 1 0.1822(4) 0.1627(5) 0.0990(4) 0.045 H25B 1 0.1678(4) 0.2027(5) 0.0189(4) 0.045 C26 1 0.1250(5) 0.0537(5) 0.0217(4) 0.045(2) H26 1 0.0546(5) 0.0701(5) 0.0174(4) 0.054 C27 1 0.1569(5) -0.0353(5) 0.0714(4) 0.045(2) H27A 1 0.1474(5) -0.0196(5) 0.1187(4) 0.054 H27B 1 0.1155(5) -0.0941(5) 0.0513(4) 0.054 C28 1 0.2638(5) -0.0603(5) 0.0808(4) 0.041(2) H28 1 0.2845(5) -0.1182(5) 0.1146(4) 0.050 C29 1 0.2752(6) -0.0879(6) 0.0063(5) 0.065(2) H29A 1 0.3451(6) -0.1029(6) 0.0106(5) 0.078 H29B 1 0.2358(6) -0.1486(6) -0.0124(5) 0.078 C30 1 0.2400(6) -0.0004(6) -0.0456(4) 0.052(2) H30 1 0.2458(6) -0.0184(6) -0.0941(4) 0.062 C31 1 0.1345(5) 0.0263(6) -0.0508(4) 0.048(2) H31A 1 0.1131(5) 0.0835(6) -0.0841(4) 0.058 H31B 1 0.0912(5) -0.0316(6) -0.0702(4) 0.058 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 S1 0.0379(10) 0.0011(7) 0.0100(7) 0.0302(9) 0.0068(7) 0.0302(9) C1 0.045(4) -0.004(3) 0.018(3) 0.037(4) 0.009(3) 0.037(4) C2 0.051(5) 0.000(4) 0.027(4) 0.061(6) 0.018(5) 0.060(5) F1 0.064(3) -0.017(3) 0.002(3) 0.068(3) -0.003(3) 0.093(4) F2 0.066(3) -0.012(4) 0.041(3) 0.178(6) 0.046(4) 0.074(4) F3 0.052(3) 0.015(3) 0.025(2) 0.085(4) 0.027(3) 0.081(3) C3 0.064(6) -0.010(4) 0.025(4) 0.064(6) 0.008(4) 0.043(5) F4 0.075(3) -0.019(3) 0.000(2) 0.097(4) 0.010(2) 0.034(2) F5 0.112(4) -0.021(4) 0.040(3) 0.132(5) 0.012(3) 0.045(3) Sn1 0.0236(2) 0.0006(2) 0.0062(2) 0.0233(2) 0.0006(2) 0.0232(2) F6 0.027(2) -0.0019(15) 0.011(2) 0.034(2) -0.002(2) 0.032(2) C4 0.021(3) 0.000(2) 0.004(3) 0.018(3) 0.001(2) 0.028(3) C5 0.020(3) 0.000(3) 0.008(3) 0.029(4) 0.003(3) 0.029(3) C6 0.023(4) 0.003(3) 0.007(3) 0.035(4) 0.002(3) 0.039(4) C7 0.030(4) 0.000(3) 0.003(3) 0.029(4) 0.010(3) 0.040(4) C8 0.032(4) 0.002(3) 0.005(3) 0.039(4) 0.006(3) 0.027(4) C9 0.022(3) -0.003(3) 0.010(3) 0.025(3) 0.001(3) 0.032(4) C10 0.027(4) 0.010(3) 0.009(3) 0.035(4) 0.005(3) 0.037(4) F7 0.075(3) 0.013(2) 0.030(2) 0.036(2) -0.007(2) 0.048(2) F8 0.035(2) 0.010(2) 0.012(2) 0.040(2) 0.003(2) 0.032(2) F9 0.028(2) 0.010(2) 0.017(2) 0.069(3) 0.011(2) 0.046(2) C11 0.049(5) 0.014(4) 0.013(4) 0.053(5) 0.012(4) 0.052(5) F10 0.099(5) 0.048(4) 0.031(4) 0.065(4) 0.035(3) 0.072(4) F11 0.086(5) 0.016(4) 0.033(4) 0.091(6) 0.063(5) 0.099(6) F12 0.165(8) 0.010(5) -0.060(5) 0.054(4) 0.004(3) 0.056(4) F10' 0.099(5) 0.048(4) 0.031(4) 0.065(4) 0.035(3) 0.072(4) F11' 0.086(5) 0.016(4) 0.033(4) 0.091(6) 0.063(5) 0.099(6) F12' 0.165(8) 0.010(5) -0.060(5) 0.054(4) 0.004(3) 0.056(4) C12 0.032(4) -0.002(3) 0.008(3) 0.033(4) -0.004(3) 0.030(4) F13 0.059(2) 0.007(2) 0.022(2) 0.026(2) 0.001(2) 0.033(2) F14 0.040(2) -0.001(2) 0.022(2) 0.041(2) -0.002(2) 0.042(2) F15 0.054(2) 0.001(2) 0.006(2) 0.043(2) -0.005(2) 0.025(2) C13 0.033(4) 0.002(3) 0.011(3) 0.020(3) 0.001(2) 0.019(3) C14 0.028(4) 0.000(3) 0.007(3) 0.028(4) 0.003(3) 0.021(3) C15 0.028(4) -0.006(3) 0.006(3) 0.034(4) -0.001(3) 0.030(4) C16 0.035(4) -0.003(3) 0.011(3) 0.020(3) 0.000(3) 0.030(3) C17 0.039(4) 0.004(3) 0.015(3) 0.026(4) 0.001(3) 0.039(4) C18 0.029(4) 0.000(3) 0.012(3) 0.028(4) 0.003(3) 0.032(4) C19 0.027(4) -0.006(3) 0.008(3) 0.043(4) -0.005(3) 0.039(4) F16 0.035(2) -0.012(2) 0.042(3) 0.046(3) -0.016(2) 0.119(4) F17 0.034(2) -0.001(2) 0.020(2) 0.032(2) -0.013(2) 0.053(2) F18 0.065(3) 0.046(3) -0.013(2) 0.089(4) -0.009(2) 0.043(3) C20 0.054(5) -0.007(4) 0.028(4) 0.034(5) -0.009(4) 0.063(5) F19 0.052(3) -0.020(2) 0.042(3) 0.039(2) -0.032(3) 0.140(5) F20 0.110(4) -0.030(3) 0.073(4) 0.061(3) -0.048(3) 0.109(4) F21 0.108(4) 0.006(3) 0.016(4) 0.027(2) 0.005(3) 0.122(5) C21 0.036(4) 0.007(3) 0.015(4) 0.030(4) -0.004(4) 0.057(5) F22 0.027(2) -0.002(2) 0.009(2) 0.039(2) -0.008(2) 0.046(2) F23 0.062(3) -0.040(3) 0.044(3) 0.106(4) -0.038(3) 0.065(3) F24 0.031(2) 0.008(2) -0.006(3) 0.037(3) -0.006(3) 0.202(6) N1 0.030(3) -0.001(2) 0.007(2) 0.023(3) 0.004(2) 0.025(3) C22 0.033(4) -0.005(3) 0.006(3) 0.030(4) -0.001(3) 0.023(3) C23 0.041(4) 0.000(3) 0.001(3) 0.032(4) 0.000(3) 0.033(4) C24 0.055(5) -0.013(4) 0.018(3) 0.047(4) -0.012(3) 0.036(4) C25 0.036(4) -0.005(3) 0.006(3) 0.035(4) 0.003(3) 0.039(4) C26 0.036(4) -0.007(3) 0.007(3) 0.046(4) 0.016(4) 0.049(4) C27 0.046(4) -0.013(3) 0.007(4) 0.038(4) 0.006(3) 0.047(4) C28 0.051(5) -0.006(3) 0.009(3) 0.029(4) 0.000(3) 0.042(4) C29 0.070(6) -0.010(4) 0.035(5) 0.042(5) -0.037(5) 0.090(7) C30 0.079(6) -0.016(4) 0.031(4) 0.049(5) -0.013(4) 0.037(4) C31 0.056(5) -0.022(4) 0.008(4) 0.046(5) -0.005(3) 0.038(4)