# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef 'kob14lu.cif' _publ_contact_author ; Reinhold Tacke Institut f\"ur Anorganische Chemie Julius-Maximilians-Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Germany ; _publ_contact_author_phone '049 931 3185251' _publ_contact_author_fax '049 931 3184609' _publ_contact_author_email r.tacke@uni-wuerzburg.de _publ_section_title ; Syntheses and Structural Characterisation of Neutral Pentacoordinate Silicon(IV)Complexes with a Tridentate Dianionic N,N,S Chelate Ligand ; loop_ _publ_author_name _publ_author_address C.Kobelt ; Institut f\"ur Anorganische Chemie Julius-Maximilians-Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Germany ; C.Burschka ; Institut f\"ur Anorganische Chemie Julius-Maximilians-Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Germany ; R.Tacke ; Institut f\"ur Anorganische Chemie Julius-Maximilians-Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Germany ; _publ_contact_author_name 'Reinhold Tacke' data_kob03e_compound_1_x_0.5_C7H8 _database_code_depnum_ccdc_archive 'CCDC 832632' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H15 Cl N2 S Si), C7 H8' _chemical_formula_sum 'C21.50 H19 Cl N2 S Si' _chemical_formula_weight 400.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.132(3) _cell_length_b 12.5246(17) _cell_length_c 17.107(2) _cell_angle_alpha 90.00 _cell_angle_beta 120.487(13) _cell_angle_gamma 90.00 _cell_volume 3901.6(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 6.65 _cell_measurement_theta_max 26.7 _exptl_crystal_description oktahedron _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .5 _exptl_crystal_size_min .4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7832 _exptl_absorpt_correction_T_max 0.8423 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24326 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 29.11 _reflns_number_total 5193 _reflns_number_gt 4263 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob03b in C2/c CELL 0.71073 21.1316 12.5246 17.1069 90.000 120.487 90.000 ZERR 8.0 0.0028 0.0017 0.0022 0.000 0.013 0.000 REM CELL 0.71073 21.2194 12.4938 17.0829 90.000 120.576 90.000 REm ZERR 8.00 0.0042 0.0025 0.0034 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N Si S Cl UNIT 172 152 16 8 8 8 L.S. 8 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.049500 2.869100 FVAR 0.34745 MOLE 1 C1 1 0.160110 0.547162 0.102569 11.00000 0.02407 0.02385 = 0.02524 0.00142 0.01545 0.00145 C2 1 0.091923 0.562872 0.023932 11.00000 0.02829 0.04136 = 0.03105 -0.00579 0.01193 0.00769 AFIX 43 H2 2 0.079836 0.523091 -0.029141 11.00000 -1.20000 AFIX 0 C3 1 0.041426 0.635898 0.022142 11.00000 0.02761 0.04731 = 0.04091 -0.00085 0.01258 0.01176 AFIX 43 H3 2 -0.004579 0.645531 -0.031907 11.00000 -1.20000 AFIX 0 C4 1 0.058187 0.694578 0.099124 11.00000 0.03618 0.02901 = 0.05013 0.00240 0.02858 0.00798 AFIX 43 H4 2 0.023445 0.743476 0.098198 11.00000 -1.20000 AFIX 0 C5 1 0.125807 0.681491 0.177290 11.00000 0.04294 0.02330 = 0.03606 -0.00096 0.02773 0.00088 AFIX 43 H5 2 0.137795 0.722364 0.229810 11.00000 -1.20000 AFIX 0 C6 1 0.176394 0.608377 0.179089 11.00000 0.03105 0.02261 = 0.02621 0.00112 0.01645 0.00059 AFIX 43 H6 2 0.222610 0.599998 0.233075 11.00000 -1.20000 AFIX 0 C7 1 0.304405 0.621193 0.080247 11.00000 0.02830 0.02877 = 0.03318 0.00285 0.01447 -0.00008 AFIX 43 H7 2 0.317879 0.641725 0.140191 11.00000 -1.20000 AFIX 0 C8 1 0.327542 0.682691 0.032144 11.00000 0.03474 0.02957 = 0.04671 0.00809 0.02198 -0.00067 AFIX 43 H8 2 0.357493 0.743770 0.059145 11.00000 -1.20000 AFIX 0 C9 1 0.306242 0.653626 -0.056293 11.00000 0.04228 0.03694 = 0.04940 0.01473 0.03138 0.00441 AFIX 43 H9 2 0.321638 0.694713 -0.090352 11.00000 -1.20000 AFIX 0 C10 1 0.262457 0.564443 -0.094423 11.00000 0.04075 0.03645 = 0.03468 0.00923 0.02517 0.00595 AFIX 43 H10 2 0.246306 0.544616 -0.155315 11.00000 -1.20000 AFIX 0 C11 1 0.242490 0.504158 -0.041545 11.00000 0.02596 0.02893 = 0.02514 0.00575 0.01521 0.00668 C12 1 0.197258 0.404800 -0.072616 11.00000 0.02870 0.03045 = 0.02211 0.00150 0.01549 0.00346 AFIX 23 H12A 2 0.148494 0.420262 -0.126121 11.00000 -1.20000 H12B 2 0.221816 0.350199 -0.089902 11.00000 -1.20000 AFIX 0 C13 1 0.149284 0.270649 -0.012915 11.00000 0.02410 0.02322 = 0.02934 0.00025 0.01601 0.00496 C14 1 0.115787 0.213486 -0.094551 11.00000 0.03172 0.03089 = 0.03370 -0.00595 0.01951 0.00107 AFIX 43 H14 2 0.118720 0.239256 -0.144849 11.00000 -1.20000 AFIX 0 C15 1 0.078092 0.118796 -0.102420 11.00000 0.03337 0.03063 = 0.04685 -0.01195 0.02091 -0.00051 AFIX 43 H15 2 0.055720 0.080606 -0.158094 11.00000 -1.20000 AFIX 0 C16 1 0.072922 0.079964 -0.030298 11.00000 0.03370 0.02383 = 0.05600 -0.00210 0.02422 0.00009 AFIX 43 H16 2 0.046812 0.015765 -0.036553 11.00000 -1.20000 AFIX 0 C17 1 0.106369 0.135683 0.052187 11.00000 0.03095 0.02740 = 0.04306 0.00508 0.02127 0.00307 AFIX 43 H17 2 0.103282 0.108946 0.102117 11.00000 -1.20000 AFIX 0 C18 1 0.144105 0.230194 0.060934 11.00000 0.02445 0.02459 = 0.03125 0.00277 0.01586 0.00500 C19 1 0.500000 0.640048 0.250000 10.50000 0.03987 0.03821 = 0.08612 0.00000 0.01762 0.00000 AFIX 137 H19A 2 0.507028 0.613966 0.307895 10.50000 -1.50000 H19B 2 0.540003 0.613966 0.241846 10.50000 -1.50000 H19C 2 0.452968 0.613966 0.200259 10.50000 -1.50000 AFIX 0 C20 1 0.500000 0.761327 0.250000 10.50000 0.02694 0.03591 = 0.03467 0.00000 0.00983 0.00000 C21 1 0.544565 0.818269 0.227152 11.00000 0.03312 0.05256 = 0.03968 -0.00464 0.02035 -0.00237 AFIX 43 H21 2 0.575728 0.780687 0.211662 11.00000 -1.20000 AFIX 0 C22 1 0.544570 0.928849 0.226453 11.00000 0.04191 0.05382 = 0.04238 0.00710 0.01731 -0.01199 AFIX 43 H22 2 0.575083 0.966327 0.209856 11.00000 -1.20000 AFIX 0 C23 1 0.500000 0.984963 0.250000 10.50000 0.05072 0.03258 = 0.04491 0.00000 0.00412 0.00000 AFIX 43 H23 2 0.500001 1.060814 0.250002 10.50000 -1.20000 AFIX 0 CL 6 0.325265 0.454974 0.227238 11.00000 0.02536 0.03300 = 0.02307 0.00256 0.00892 0.00210 N1 3 0.263059 0.532542 0.043904 11.00000 0.02281 0.02619 = 0.02534 0.00409 0.01384 0.00282 N2 3 0.188991 0.365842 0.001967 11.00000 0.02627 0.02463 = 0.02349 0.00080 0.01542 0.00176 S 5 0.191849 0.303101 0.162371 11.00000 0.03524 0.03070 = 0.02555 0.00437 0.01702 -0.00101 SI 4 0.222356 0.440081 0.102964 11.00000 0.02185 0.02304 = 0.02027 0.00126 0.01159 0.00293 HKLF 4 REM kob03b in C2/c REM R1 = 0.0366 for 4263 Fo > 4sig(Fo) and 0.0463 for all 5193 data REM 242 parameters refined using 0 restraints END WGHT 0.0495 2.8691 REM Highest difference peak 0.417, deepest hole -0.306, 1-sigma level 0.054 Q1 1 0.2579 0.4968 0.0791 11.00000 0.05 0.42 Q2 1 0.2287 0.3656 0.1478 11.00000 0.05 0.36 Q3 1 0.1849 0.5146 0.1010 11.00000 0.05 0.34 Q4 1 0.2806 0.4619 0.1551 11.00000 0.05 0.34 Q5 1 0.2762 0.4095 0.1700 11.00000 0.05 0.34 Q6 1 0.1957 0.3781 0.1286 11.00000 0.05 0.33 Q7 1 0.0444 0.6433 0.0698 11.00000 0.05 0.28 Q8 1 0.1421 0.2528 0.0273 11.00000 0.05 0.27 Q9 1 0.1505 0.6442 0.1829 11.00000 0.05 0.26 Q10 1 0.1789 0.4070 0.0273 11.00000 0.05 0.24 Q11 1 0.2238 0.4459 -0.0552 11.00000 0.05 0.23 Q12 1 0.2700 0.6162 -0.0826 11.00000 0.05 0.23 Q13 1 0.2062 0.3383 0.1149 11.00000 0.05 0.23 Q14 1 0.1488 0.2602 0.1022 11.00000 0.05 0.23 Q15 1 0.1545 0.2448 0.1800 11.00000 0.05 0.22 Q16 1 0.0714 0.5944 0.0356 11.00000 0.05 0.22 Q17 1 0.5211 0.7927 0.2408 11.00000 0.05 0.22 Q18 1 0.3221 0.6451 0.0613 11.00000 0.05 0.22 Q19 1 0.0871 0.1044 0.0110 11.00000 0.05 0.21 Q20 1 0.1301 0.5276 0.0780 11.00000 0.05 0.21 ; _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^)+(0.0495P)^2^+2.8691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5193 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0975 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.16011(8) 0.54716(11) 0.10257(9) 0.0230(3) Uani 1 1 d . . . C2 C 0.09192(9) 0.56287(14) 0.02393(11) 0.0350(3) Uani 1 1 d . . . H2 H 0.0798 0.5231 -0.0291 0.042 Uiso 1 1 calc R . . C3 C 0.04143(9) 0.63590(15) 0.02214(12) 0.0408(4) Uani 1 1 d . . . H3 H -0.0046 0.6455 -0.0319 0.049 Uiso 1 1 calc R . . C4 C 0.05819(10) 0.69458(13) 0.09912(12) 0.0354(3) Uani 1 1 d . . . H4 H 0.0234 0.7435 0.0982 0.042 Uiso 1 1 calc R . . C5 C 0.12581(9) 0.68149(12) 0.17729(11) 0.0306(3) Uani 1 1 d . . . H5 H 0.1378 0.7224 0.2298 0.037 Uiso 1 1 calc R . . C6 C 0.17639(8) 0.60838(11) 0.17909(9) 0.0258(3) Uani 1 1 d . . . H6 H 0.2226 0.6000 0.2331 0.031 Uiso 1 1 calc R . . C7 C 0.30441(8) 0.62119(12) 0.08025(11) 0.0306(3) Uani 1 1 d . . . H7 H 0.3179 0.6417 0.1402 0.037 Uiso 1 1 calc R . . C8 C 0.32754(9) 0.68269(13) 0.03214(12) 0.0364(4) Uani 1 1 d . . . H8 H 0.3575 0.7438 0.0591 0.044 Uiso 1 1 calc R . . C9 C 0.30624(10) 0.65363(14) -0.05629(13) 0.0392(4) Uani 1 1 d . . . H9 H 0.3216 0.6947 -0.0904 0.047 Uiso 1 1 calc R . . C10 C 0.26246(10) 0.56444(13) -0.09442(11) 0.0345(3) Uani 1 1 d . . . H10 H 0.2463 0.5446 -0.1553 0.041 Uiso 1 1 calc R . . C11 C 0.24249(8) 0.50416(12) -0.04155(9) 0.0256(3) Uani 1 1 d . . . C12 C 0.19726(8) 0.40480(12) -0.07262(9) 0.0259(3) Uani 1 1 d . . . H12A H 0.1485 0.4203 -0.1261 0.031 Uiso 1 1 calc R . . H12B H 0.2218 0.3502 -0.0899 0.031 Uiso 1 1 calc R . . C13 C 0.14928(8) 0.27065(11) -0.01291(10) 0.0244(3) Uani 1 1 d . . . C14 C 0.11579(9) 0.21349(13) -0.09455(11) 0.0308(3) Uani 1 1 d . . . H14 H 0.1187 0.2393 -0.1448 0.037 Uiso 1 1 calc R . . C15 C 0.07809(9) 0.11880(13) -0.10242(12) 0.0367(4) Uani 1 1 d . . . H15 H 0.0557 0.0806 -0.1581 0.044 Uiso 1 1 calc R . . C16 C 0.07292(9) 0.07996(13) -0.03030(13) 0.0372(4) Uani 1 1 d . . . H16 H 0.0468 0.0158 -0.0366 0.045 Uiso 1 1 calc R . . C17 C 0.10637(9) 0.13568(13) 0.05219(12) 0.0327(3) Uani 1 1 d . . . H17 H 0.1033 0.1089 0.1021 0.039 Uiso 1 1 calc R . . C18 C 0.14411(8) 0.23019(11) 0.06093(10) 0.0260(3) Uani 1 1 d . . . C19 C 0.5000 0.6400(2) 0.2500 0.0613(9) Uani 1 2 d S . . H19A H 0.5070 0.6140 0.3079 0.092 Uiso 0.50 1 calc PR . . H19B H 0.5400 0.6140 0.2418 0.092 Uiso 0.50 1 calc PR . . H19C H 0.4530 0.6140 0.2003 0.092 Uiso 0.50 1 calc PR . . C20 C 0.5000 0.7613(2) 0.2500 0.0351(5) Uani 1 2 d S . . C21 C 0.54456(10) 0.81827(16) 0.22715(12) 0.0409(4) Uani 1 1 d . . . H21 H 0.5757 0.7807 0.2117 0.049 Uiso 1 1 calc R . . C22 C 0.54457(11) 0.92885(17) 0.22645(13) 0.0479(5) Uani 1 1 d . . . H22 H 0.5751 0.9663 0.2099 0.057 Uiso 1 1 calc R . . C23 C 0.5000 0.9850(2) 0.2500 0.0519(7) Uani 1 2 d S . . H23 H 0.5000 1.0608 0.2500 0.062 Uiso 1 2 calc SR . . Cl Cl 0.325265(19) 0.45497(3) 0.22724(2) 0.02867(9) Uani 1 1 d . . . N1 N 0.26306(6) 0.53254(10) 0.04390(8) 0.0240(2) Uani 1 1 d . . . N2 N 0.18899(7) 0.36584(10) 0.00197(8) 0.0235(2) Uani 1 1 d . . . S S 0.19185(2) 0.30310(3) 0.16237(2) 0.02977(10) Uani 1 1 d . . . Si Si 0.22236(2) 0.44008(3) 0.10296(2) 0.02131(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0241(6) 0.0239(6) 0.0252(6) 0.0014(5) 0.0155(5) 0.0014(5) C2 0.0283(7) 0.0414(9) 0.0310(7) -0.0058(6) 0.0119(6) 0.0077(7) C3 0.0276(8) 0.0473(10) 0.0409(9) -0.0008(7) 0.0126(7) 0.0118(7) C4 0.0362(8) 0.0290(8) 0.0501(9) 0.0024(7) 0.0286(8) 0.0080(6) C5 0.0429(9) 0.0233(7) 0.0361(7) -0.0010(5) 0.0277(7) 0.0009(6) C6 0.0311(7) 0.0226(6) 0.0262(6) 0.0011(5) 0.0164(6) 0.0006(5) C7 0.0283(7) 0.0288(7) 0.0332(7) 0.0029(6) 0.0145(6) -0.0001(6) C8 0.0347(8) 0.0296(8) 0.0467(9) 0.0081(7) 0.0220(7) -0.0007(6) C9 0.0423(9) 0.0369(9) 0.0494(9) 0.0147(7) 0.0314(8) 0.0044(7) C10 0.0407(9) 0.0364(8) 0.0347(8) 0.0092(6) 0.0252(7) 0.0060(7) C11 0.0260(7) 0.0289(7) 0.0251(6) 0.0058(5) 0.0152(5) 0.0067(6) C12 0.0287(7) 0.0305(7) 0.0221(6) 0.0015(5) 0.0155(5) 0.0035(6) C13 0.0241(6) 0.0232(6) 0.0293(6) 0.0002(5) 0.0160(5) 0.0050(5) C14 0.0317(8) 0.0309(7) 0.0337(7) -0.0059(6) 0.0195(6) 0.0011(6) C15 0.0334(8) 0.0306(8) 0.0468(9) -0.0119(7) 0.0209(7) -0.0005(6) C16 0.0337(8) 0.0238(7) 0.0560(10) -0.0021(7) 0.0242(8) 0.0001(6) C17 0.0310(7) 0.0274(7) 0.0431(8) 0.0051(6) 0.0213(7) 0.0031(6) C18 0.0244(7) 0.0246(7) 0.0312(7) 0.0028(5) 0.0159(6) 0.0050(5) C19 0.0399(15) 0.0382(15) 0.086(2) 0.000 0.0176(15) 0.000 C20 0.0269(10) 0.0359(12) 0.0347(11) 0.000 0.0098(9) 0.000 C21 0.0331(8) 0.0526(11) 0.0397(9) -0.0046(7) 0.0204(7) -0.0024(8) C22 0.0419(10) 0.0538(11) 0.0424(9) 0.0071(8) 0.0173(8) -0.0120(9) C23 0.0507(16) 0.0326(13) 0.0449(14) 0.000 0.0041(12) 0.000 Cl 0.02536(17) 0.03300(19) 0.02307(16) 0.00256(12) 0.00892(13) 0.00210(13) N1 0.0228(5) 0.0262(6) 0.0253(5) 0.0041(4) 0.0138(5) 0.0028(5) N2 0.0263(6) 0.0246(6) 0.0235(5) 0.0008(4) 0.0154(5) 0.0018(5) S 0.0352(2) 0.03070(19) 0.02555(17) 0.00437(13) 0.01702(15) -0.00101(15) Si 0.02185(18) 0.02304(18) 0.02027(17) 0.00126(13) 0.01159(14) 0.00293(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.399(2) . ? C1 C6 1.4010(19) . ? C1 Si 1.8761(14) . ? C2 C3 1.394(2) . ? C3 C4 1.388(2) . ? C4 C5 1.385(2) . ? C5 C6 1.396(2) . ? C7 N1 1.353(2) . ? C7 C8 1.385(2) . ? C8 C9 1.390(3) . ? C9 C10 1.384(3) . ? C10 C11 1.398(2) . ? C11 N1 1.3444(17) . ? C11 C12 1.493(2) . ? C12 N2 1.4569(17) . ? C13 C14 1.400(2) . ? C13 N2 1.4048(19) . ? C13 C18 1.4160(19) . ? C14 C15 1.397(2) . ? C15 C16 1.381(3) . ? C16 C17 1.402(2) . ? C17 C18 1.392(2) . ? C18 S 1.7568(15) . ? C19 C20 1.519(4) . ? C20 C21 1.386(2) 2_655 ? C20 C21 1.386(2) . ? C21 C22 1.385(3) . ? C22 C23 1.389(3) . ? C23 C22 1.389(3) 2_655 ? Cl Si 2.1430(7) . ? N1 Si 1.9958(12) . ? N2 Si 1.7637(12) . ? S Si 2.2487(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.80(13) . . ? C2 C1 Si 118.82(11) . . ? C6 C1 Si 123.26(11) . . ? C3 C2 C1 121.12(15) . . ? C4 C3 C2 120.17(16) . . ? C5 C4 C3 119.67(14) . . ? C4 C5 C6 120.16(14) . . ? C5 C6 C1 121.07(14) . . ? N1 C7 C8 121.58(15) . . ? C7 C8 C9 118.95(16) . . ? C10 C9 C8 119.60(15) . . ? C9 C10 C11 118.68(15) . . ? N1 C11 C10 121.57(14) . . ? N1 C11 C12 113.76(12) . . ? C10 C11 C12 124.66(13) . . ? N2 C12 C11 107.87(11) . . ? C14 C13 N2 124.60(13) . . ? C14 C13 C18 118.56(14) . . ? N2 C13 C18 116.83(12) . . ? C15 C14 C13 120.35(15) . . ? C16 C15 C14 120.84(15) . . ? C15 C16 C17 119.73(15) . . ? C18 C17 C16 120.01(15) . . ? C17 C18 C13 120.51(14) . . ? C17 C18 S 123.96(12) . . ? C13 C18 S 115.45(11) . . ? C21 C20 C21 118.1(2) 2_655 . ? C21 C20 C19 120.96(12) 2_655 . ? C21 C20 C19 120.96(12) . . ? C22 C21 C20 121.33(18) . . ? C21 C22 C23 120.04(19) . . ? C22 C23 C22 119.2(3) 2_655 . ? C11 N1 C7 119.58(13) . . ? C11 N1 Si 114.35(10) . . ? C7 N1 Si 125.95(10) . . ? C13 N2 C12 116.84(11) . . ? C13 N2 Si 122.01(9) . . ? C12 N2 Si 121.02(10) . . ? C18 S Si 95.90(5) . . ? N2 Si C1 116.25(6) . . ? N2 Si N1 82.57(5) . . ? C1 Si N1 93.72(6) . . ? N2 Si Cl 135.87(5) . . ? C1 Si Cl 107.34(5) . . ? N1 Si Cl 88.32(4) . . ? N2 Si S 88.67(4) . . ? C1 Si S 100.71(5) . . ? N1 Si S 165.34(4) . . ? Cl Si S 89.85(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 C6 C1 C2 C3 -0.9(2) . . . . ? Si C1 C2 C3 175.26(14) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C3 C4 C5 C6 -1.0(2) . . . . ? C4 C5 C6 C1 0.0(2) . . . . ? C2 C1 C6 C5 0.9(2) . . . . ? Si C1 C6 C5 -175.06(11) . . . . ? N1 C7 C8 C9 1.5(2) . . . . ? C7 C8 C9 C10 0.1(3) . . . . ? C8 C9 C10 C11 -1.7(2) . . . . ? C9 C10 C11 N1 1.9(2) . . . . ? C9 C10 C11 C12 -178.38(15) . . . . ? N1 C11 C12 N2 -0.54(17) . . . . ? C10 C11 C12 N2 179.72(14) . . . . ? N2 C13 C14 C15 179.30(14) . . . . ? C18 C13 C14 C15 0.1(2) . . . . ? C13 C14 C15 C16 0.2(2) . . . . ? C14 C15 C16 C17 -0.5(2) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C16 C17 C18 C13 -0.2(2) . . . . ? C16 C17 C18 S -176.73(12) . . . . ? C14 C13 C18 C17 -0.1(2) . . . . ? N2 C13 C18 C17 -179.35(13) . . . . ? C14 C13 C18 S 176.71(11) . . . . ? N2 C13 C18 S -2.54(17) . . . . ? C21 C20 C21 C22 -0.40(13) 2_655 . . . ? C19 C20 C21 C22 179.61(13) . . . . ? C20 C21 C22 C23 0.8(3) . . . . ? C21 C22 C23 C22 -0.39(13) . . . 2_655 ? C10 C11 N1 C7 -0.3(2) . . . . ? C12 C11 N1 C7 179.90(13) . . . . ? C10 C11 N1 Si 175.99(12) . . . . ? C12 C11 N1 Si -3.77(15) . . . . ? C8 C7 N1 C11 -1.4(2) . . . . ? C8 C7 N1 Si -177.23(12) . . . . ? C14 C13 N2 C12 -2.0(2) . . . . ? C18 C13 N2 C12 177.20(12) . . . . ? C14 C13 N2 Si 173.94(11) . . . . ? C18 C13 N2 Si -6.86(17) . . . . ? C11 C12 N2 C13 -178.51(12) . . . . ? C11 C12 N2 Si 5.50(16) . . . . ? C17 C18 S Si -175.59(12) . . . . ? C13 C18 S Si 7.73(11) . . . . ? C13 N2 Si C1 -91.39(12) . . . . ? C12 N2 Si C1 84.39(12) . . . . ? C13 N2 Si N1 178.12(11) . . . . ? C12 N2 Si N1 -6.10(11) . . . . ? C13 N2 Si Cl 98.31(11) . . . . ? C12 N2 Si Cl -85.91(12) . . . . ? C13 N2 Si S 9.90(11) . . . . ? C12 N2 Si S -174.32(10) . . . . ? C2 C1 Si N2 -0.21(14) . . . . ? C6 C1 Si N2 175.73(11) . . . . ? C2 C1 Si N1 83.34(13) . . . . ? C6 C1 Si N1 -100.72(12) . . . . ? C2 C1 Si Cl 172.73(11) . . . . ? C6 C1 Si Cl -11.33(13) . . . . ? C2 C1 Si S -94.04(12) . . . . ? C6 C1 Si S 81.90(12) . . . . ? C11 N1 Si N2 5.46(10) . . . . ? C7 N1 Si N2 -178.48(13) . . . . ? C11 N1 Si C1 -110.55(10) . . . . ? C7 N1 Si C1 65.51(13) . . . . ? C11 N1 Si Cl 142.18(10) . . . . ? C7 N1 Si Cl -41.76(12) . . . . ? C11 N1 Si S 59.2(2) . . . . ? C7 N1 Si S -124.72(16) . . . . ? C18 S Si N2 -8.68(6) . . . . ? C18 S Si C1 107.79(7) . . . . ? C18 S Si N1 -61.82(17) . . . . ? C18 S Si Cl -144.58(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.417 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.054 # ***************************** compound 2 x 0.5 C7H8 ************** data_kob05l_2 _database_code_depnum_ccdc_archive 'CCDC 832633' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H15 Br N2 S Si), C7 H8' _chemical_formula_sum 'C21.50 H19 Br N2 S Si' _chemical_formula_weight 445.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.133(4) _cell_length_b 12.662(3) _cell_length_c 17.279(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.25(3) _cell_angle_gamma 90.00 _cell_volume 3952.5(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3213 _cell_measurement_theta_min 8.25 _cell_measurement_theta_max 27.75 _exptl_crystal_description long_prism _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 2.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3656 _exptl_absorpt_correction_T_max 0.3993 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26240 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 29.11 _reflns_number_total 4998 _reflns_number_gt 3768 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob05h in C2/c CELL 0.71073 21.1329 12.6615 17.2794 90.000 121.255 90.000 ZERR 8.00 0.0042 0.0025 0.0035 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N Si S Br UNIT 172 152 16 8 8 8 L.S. 12 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.049400 FVAR 0.38093 BR 6 0.163848 0.954879 0.263575 11.00000 0.02278 0.03240 = 0.02204 -0.00143 0.00964 -0.00211 C1 1 0.338993 1.046558 0.399014 11.00000 0.01886 0.02641 = 0.02158 -0.00156 0.01270 -0.00301 C2 1 0.322947 1.105440 0.322843 11.00000 0.02687 0.02308 = 0.02424 -0.00292 0.01473 -0.00365 AFIX 43 H2 2 0.276393 1.096517 0.268586 11.00000 0.03020 AFIX 0 C3 1 0.373842 1.177447 0.324420 11.00000 0.03922 0.02372 = 0.03400 0.00024 0.02731 -0.00111 AFIX 43 H3 2 0.361686 1.216943 0.271723 11.00000 0.03796 AFIX 0 C4 1 0.441895 1.190948 0.402923 11.00000 0.03348 0.03143 = 0.04527 -0.00240 0.02624 -0.00842 AFIX 43 H4 2 0.477031 1.238713 0.404048 11.00000 0.04542 AFIX 0 C5 1 0.458451 1.134763 0.479468 11.00000 0.02579 0.05411 = 0.04077 0.00105 0.01092 -0.01644 AFIX 43 H5 2 0.504796 1.144955 0.533758 11.00000 0.05732 AFIX 0 C6 1 0.407447 1.062667 0.477874 11.00000 0.02731 0.04773 = 0.02837 0.00609 0.01122 -0.01063 AFIX 43 H6 2 0.419645 1.024334 0.531123 11.00000 0.05387 AFIX 0 C7 1 0.195810 1.119882 0.422247 11.00000 0.02671 0.03154 = 0.03005 -0.00289 0.01496 -0.00082 AFIX 43 H7 2 0.182264 1.141175 0.362871 11.00000 0.03019 AFIX 0 C8 1 0.173350 1.180312 0.470413 11.00000 0.03186 0.02978 = 0.04430 -0.00759 0.02179 0.00084 AFIX 43 H8 2 0.143875 1.241571 0.444087 11.00000 0.03157 AFIX 0 C9 1 0.194644 1.149907 0.558163 11.00000 0.03919 0.03785 = 0.04738 -0.01510 0.03119 -0.00510 AFIX 43 H9 2 0.179676 1.190109 0.592369 11.00000 0.03854 AFIX 0 C10 1 0.237643 1.060910 0.594815 11.00000 0.03855 0.03773 = 0.03038 -0.00947 0.02408 -0.00627 AFIX 43 H10 2 0.253701 1.040038 0.655073 11.00000 0.04493 AFIX 0 C11 1 0.257321 1.001746 0.542162 11.00000 0.02230 0.02999 = 0.02210 -0.00514 0.01450 -0.00746 C12 1 0.302748 0.903132 0.573068 11.00000 0.02532 0.03108 = 0.02150 -0.00276 0.01577 -0.00498 AFIX 23 H12A 2 0.351836 0.917828 0.627297 11.00000 0.02817 H12B 2 0.277738 0.848676 0.588925 11.00000 0.02379 AFIX 0 C13 1 0.351412 0.771727 0.513624 11.00000 0.01909 0.02373 = 0.02776 0.00042 0.01401 -0.00472 C14 1 0.385737 0.714649 0.594894 11.00000 0.03081 0.02987 = 0.03156 0.00389 0.02034 -0.00198 AFIX 43 H14 2 0.382830 0.739376 0.644868 11.00000 0.04426 AFIX 0 C15 1 0.424132 0.621786 0.602860 11.00000 0.03122 0.03093 = 0.04446 0.01267 0.02111 0.00087 AFIX 43 H15 2 0.447233 0.583779 0.658307 11.00000 0.03994 AFIX 0 C16 1 0.428947 0.584301 0.530582 11.00000 0.03230 0.02484 = 0.05133 0.00204 0.02441 -0.00023 AFIX 43 H16 2 0.455602 0.521307 0.536753 11.00000 0.02813 AFIX 0 C17 1 0.394486 0.639509 0.448850 11.00000 0.02833 0.02806 = 0.03993 -0.00717 0.02059 -0.00434 AFIX 43 H17 2 0.397109 0.613469 0.399027 11.00000 0.03652 AFIX 0 C18 1 0.356105 0.733016 0.440006 11.00000 0.01969 0.02576 = 0.02641 -0.00250 0.01242 -0.00612 C19 1 0.000000 1.142609 0.250000 10.50000 0.03401 0.04046 = 0.08993 0.00000 0.01622 0.00000 AFIX 137 H19A 2 0.001582 1.116809 0.304449 10.50000 -1.50000 H19B 2 0.043480 1.116809 0.249436 10.50000 -1.50000 H19C 2 -0.045061 1.116809 0.196115 10.50000 -1.50000 AFIX 0 C20 1 0.000000 1.262339 0.250000 10.50000 0.02395 0.03904 = 0.03688 0.00000 0.01086 0.00000 C21 1 0.045056 1.318925 0.228700 11.00000 0.03064 0.05661 = 0.03966 -0.00554 0.01995 -0.00528 AFIX 43 H21 2 0.076721 1.281803 0.214346 11.00000 -1.20000 AFIX 0 C22 1 0.045060 1.427808 0.227829 11.00000 0.04172 0.05945 = 0.04235 0.00462 0.01642 -0.01726 AFIX 43 H22 2 0.075871 1.464887 0.212070 11.00000 -1.20000 AFIX 0 C23 1 0.000000 1.483042 0.250000 10.50000 0.05012 0.03342 = 0.04615 0.00000 0.00052 0.00000 AFIX 43 H23 2 0.000001 1.558073 0.250000 10.50000 -1.20000 AFIX 0 N1 3 0.236780 1.030793 0.457771 11.00000 0.01915 0.02614 = 0.02448 -0.00503 0.01290 -0.00426 N2 3 0.311301 0.866005 0.499191 11.00000 0.02430 0.02463 = 0.02113 -0.00156 0.01572 -0.00267 S 5 0.307131 0.805217 0.339269 11.00000 0.03061 0.03283 = 0.02347 -0.00359 0.01540 0.00220 SI 4 0.277040 0.939907 0.398854 11.00000 0.01837 0.02352 = 0.01834 -0.00133 0.01085 -0.00339 HKLF 4 REM kob05h in C2/c REM R1 = 0.0317 for 3768 Fo > 4sig(Fo) and 0.0495 for all 4998 data REM 257 parameters refined using 0 restraints END WGHT 0.0494 0.0000 REM Highest difference peak 0.462, deepest hole -0.570, 1-sigma level 0.079 Q1 1 0.3028 1.0072 0.4014 11.00000 0.05 0.46 Q2 1 0.1737 1.0270 0.2614 11.00000 0.05 0.45 Q3 1 0.2836 0.9567 0.5651 11.00000 0.05 0.36 Q4 1 0.2471 0.9973 0.4415 11.00000 0.05 0.36 Q5 1 0.1688 0.8775 0.2627 11.00000 0.05 0.36 Q6 1 0.3284 0.8195 0.3764 11.00000 0.05 0.34 Q7 1 0.3156 0.9193 0.4877 11.00000 0.05 0.33 Q8 1 0.2198 0.9648 0.3330 11.00000 0.05 0.33 Q9 1 0.3046 0.8461 0.3181 11.00000 0.05 0.33 Q10 1 0.3348 0.8598 0.3491 11.00000 0.05 0.31 Q11 1 0.2180 1.0656 0.4299 11.00000 0.05 0.30 Q12 1 0.3568 0.7641 0.4787 11.00000 0.05 0.30 Q13 1 0.4278 1.0869 0.4641 11.00000 0.05 0.30 Q14 1 0.1828 0.9459 0.2085 11.00000 0.05 0.29 Q15 1 0.2743 0.9033 0.4505 11.00000 0.05 0.29 Q16 1 0.2529 1.0216 0.4986 11.00000 0.05 0.29 Q17 1 0.1578 0.9577 0.3270 11.00000 0.05 0.29 Q18 1 0.3439 1.1428 0.3244 11.00000 0.05 0.29 Q19 1 0.2206 0.9605 0.4692 11.00000 0.05 0.29 Q20 1 0.2244 1.0955 0.4566 11.00000 0.05 0.28 ; _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^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4998 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0795 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br Br 0.163848(11) 0.954879(17) 0.263575(15) 0.02668(7) Uani 1 1 d . . . C1 C 0.33899(10) 1.04656(16) 0.39901(15) 0.0212(4) Uani 1 1 d . . . C2 C 0.32295(11) 1.10544(16) 0.32284(16) 0.0240(4) Uani 1 1 d . . . H2 H 0.2764 1.0965 0.2686 0.030(7) Uiso 1 1 calc R . . C3 C 0.37384(13) 1.17745(17) 0.32442(18) 0.0284(5) Uani 1 1 d . . . H3 H 0.3617 1.2169 0.2717 0.038(7) Uiso 1 1 calc R . . C4 C 0.44190(13) 1.19095(19) 0.40292(19) 0.0340(5) Uani 1 1 d . . . H4 H 0.4770 1.2387 0.4040 0.045(8) Uiso 1 1 calc R . . C5 C 0.45845(13) 1.1348(2) 0.4795(2) 0.0432(7) Uani 1 1 d . . . H5 H 0.5048 1.1450 0.5338 0.057(9) Uiso 1 1 calc R . . C6 C 0.40745(13) 1.0627(2) 0.47787(18) 0.0360(6) Uani 1 1 d . . . H6 H 0.4196 1.0243 0.5311 0.054(9) Uiso 1 1 calc R . . C7 C 0.19581(12) 1.11988(18) 0.42225(18) 0.0293(5) Uani 1 1 d . . . H7 H 0.1823 1.1412 0.3629 0.030(7) Uiso 1 1 calc R . . C8 C 0.17335(13) 1.18031(19) 0.47041(19) 0.0343(6) Uani 1 1 d . . . H8 H 0.1439 1.2416 0.4441 0.032(7) Uiso 1 1 calc R . . C9 C 0.19464(14) 1.1499(2) 0.5582(2) 0.0373(6) Uani 1 1 d . . . H9 H 0.1797 1.1901 0.5924 0.039(7) Uiso 1 1 calc R . . C10 C 0.23764(14) 1.06091(19) 0.59481(19) 0.0326(5) Uani 1 1 d . . . H10 H 0.2537 1.0400 0.6551 0.045(8) Uiso 1 1 calc R . . C11 C 0.25732(11) 1.00175(17) 0.54216(15) 0.0234(4) Uani 1 1 d . . . C12 C 0.30275(11) 0.90313(17) 0.57307(15) 0.0242(4) Uani 1 1 d . . . H12A H 0.3518 0.9178 0.6273 0.028(6) Uiso 1 1 calc R . . H12B H 0.2777 0.8487 0.5889 0.024(6) Uiso 1 1 calc R . . C13 C 0.35141(11) 0.77173(16) 0.51362(16) 0.0227(4) Uani 1 1 d . . . C14 C 0.38574(12) 0.71465(18) 0.59489(17) 0.0288(5) Uani 1 1 d . . . H14 H 0.3828 0.7394 0.6449 0.044(8) Uiso 1 1 calc R . . C15 C 0.42413(13) 0.62179(18) 0.60286(19) 0.0348(6) Uani 1 1 d . . . H15 H 0.4472 0.5838 0.6583 0.040(8) Uiso 1 1 calc R . . C16 C 0.42895(13) 0.58430(18) 0.5306(2) 0.0349(6) Uani 1 1 d . . . H16 H 0.4556 0.5213 0.5368 0.028(6) Uiso 1 1 calc R . . C17 C 0.39449(12) 0.63951(18) 0.44885(18) 0.0307(5) Uani 1 1 d . . . H17 H 0.3971 0.6135 0.3990 0.037(7) Uiso 1 1 calc R . . C18 C 0.35611(11) 0.73302(16) 0.44001(16) 0.0237(4) Uani 1 1 d . . . C19 C 0.0000 1.1426(3) 0.2500 0.0623(14) Uani 1 2 d S . . H19A H 0.0016 1.1168 0.3044 0.094 Uiso 0.50 1 calc PR . . H19B H 0.0435 1.1168 0.2494 0.094 Uiso 0.50 1 calc PR . . H19C H -0.0451 1.1168 0.1961 0.094 Uiso 0.50 1 calc PR . . C20 C 0.0000 1.2623(3) 0.2500 0.0356(8) Uani 1 2 d S . . C21 C 0.04506(14) 1.3189(2) 0.2287(2) 0.0415(6) Uani 1 1 d . . . H21 H 0.0767 1.2818 0.2143 0.050 Uiso 1 1 calc R . . C22 C 0.04506(16) 1.4278(3) 0.2278(2) 0.0504(8) Uani 1 1 d . . . H22 H 0.0759 1.4649 0.2121 0.060 Uiso 1 1 calc R . . C23 C 0.0000 1.4830(3) 0.2500 0.0548(12) Uani 1 2 d S . . H23 H 0.0000 1.5581 0.2500 0.066 Uiso 1 2 calc SR . . N1 N 0.23678(9) 1.03079(13) 0.45777(13) 0.0225(4) Uani 1 1 d . . . N2 N 0.31130(9) 0.86601(13) 0.49919(12) 0.0215(4) Uani 1 1 d . . . S S 0.30713(3) 0.80522(4) 0.33927(4) 0.02833(13) Uani 1 1 d . . . Si Si 0.27704(3) 0.93991(4) 0.39885(4) 0.01945(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br 0.02278(10) 0.03240(12) 0.02204(13) -0.00143(9) 0.00964(8) -0.00211(8) C1 0.0189(8) 0.0264(9) 0.0216(12) -0.0016(8) 0.0127(8) -0.0030(7) C2 0.0269(10) 0.0231(10) 0.0242(13) -0.0029(8) 0.0147(9) -0.0037(8) C3 0.0392(12) 0.0237(10) 0.0340(15) 0.0002(9) 0.0273(11) -0.0011(9) C4 0.0335(11) 0.0314(12) 0.0453(17) -0.0024(10) 0.0262(12) -0.0084(9) C5 0.0258(11) 0.0541(16) 0.0408(17) 0.0010(12) 0.0109(11) -0.0164(11) C6 0.0273(10) 0.0477(14) 0.0284(15) 0.0061(10) 0.0112(10) -0.0106(10) C7 0.0267(10) 0.0315(11) 0.0301(14) -0.0029(9) 0.0150(10) -0.0008(8) C8 0.0319(11) 0.0298(11) 0.0443(17) -0.0076(10) 0.0218(11) 0.0008(9) C9 0.0392(12) 0.0379(13) 0.0474(18) -0.0151(11) 0.0312(13) -0.0051(10) C10 0.0385(12) 0.0377(13) 0.0304(15) -0.0095(10) 0.0241(11) -0.0063(9) C11 0.0223(9) 0.0300(10) 0.0221(13) -0.0051(8) 0.0145(9) -0.0075(8) C12 0.0253(9) 0.0311(11) 0.0215(13) -0.0028(9) 0.0158(9) -0.0050(8) C13 0.0191(8) 0.0237(10) 0.0278(13) 0.0004(8) 0.0140(9) -0.0047(7) C14 0.0308(10) 0.0299(11) 0.0316(14) 0.0039(9) 0.0203(10) -0.0020(9) C15 0.0312(11) 0.0309(12) 0.0445(17) 0.0127(10) 0.0211(11) 0.0009(9) C16 0.0323(11) 0.0248(10) 0.0513(18) 0.0020(10) 0.0244(12) -0.0002(9) C17 0.0283(10) 0.0281(11) 0.0399(16) -0.0072(10) 0.0206(10) -0.0043(8) C18 0.0197(9) 0.0258(10) 0.0264(13) -0.0025(8) 0.0124(9) -0.0061(7) C19 0.0340(19) 0.040(2) 0.090(4) 0.000 0.016(2) 0.000 C20 0.0239(14) 0.0390(18) 0.037(2) 0.000 0.0109(14) 0.000 C21 0.0306(12) 0.0566(17) 0.0397(17) -0.0055(12) 0.0200(12) -0.0053(11) C22 0.0417(14) 0.0594(19) 0.0423(19) 0.0046(13) 0.0164(13) -0.0173(13) C23 0.050(2) 0.0334(19) 0.046(3) 0.000 0.0005(19) 0.000 N1 0.0191(7) 0.0261(9) 0.0245(11) -0.0050(7) 0.0129(7) -0.0043(6) N2 0.0243(8) 0.0246(8) 0.0211(10) -0.0016(7) 0.0157(7) -0.0027(6) S 0.0306(3) 0.0328(3) 0.0235(3) -0.0036(2) 0.0154(2) 0.0022(2) Si 0.0184(2) 0.0235(3) 0.0183(3) -0.0013(2) 0.0108(2) -0.00339(19) _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 Br Si 2.3280(13) . ? C1 C2 1.393(3) . ? C1 C6 1.395(3) . ? C1 Si 1.880(2) . ? C2 C3 1.399(3) . ? C3 C4 1.383(4) . ? C4 C5 1.378(4) . ? C5 C6 1.402(3) . ? C7 N1 1.359(3) . ? C7 C8 1.383(3) . ? C8 C9 1.393(4) . ? C9 C10 1.378(4) . ? C10 C11 1.398(3) . ? C11 N1 1.339(3) . ? C11 C12 1.495(3) . ? C12 N2 1.457(3) . ? C13 C14 1.401(3) . ? C13 N2 1.409(3) . ? C13 C18 1.414(3) . ? C14 C15 1.394(3) . ? C15 C16 1.388(4) . ? C16 C17 1.395(4) . ? C17 C18 1.398(3) . ? C18 S 1.751(2) . ? C19 C20 1.516(5) . ? C20 C21 1.385(3) . ? C20 C21 1.385(3) 2 ? C21 C22 1.379(4) . ? C22 C23 1.386(4) . ? C23 C22 1.386(4) 2 ? N1 Si 1.9958(18) . ? N2 Si 1.7616(19) . ? S Si 2.2477(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.74(19) . . ? C2 C1 Si 123.72(16) . . ? C6 C1 Si 118.36(17) . . ? C1 C2 C3 121.5(2) . . ? C4 C3 C2 119.8(2) . . ? C5 C4 C3 119.6(2) . . ? C4 C5 C6 120.5(2) . . ? C1 C6 C5 120.8(2) . . ? N1 C7 C8 121.6(2) . . ? C7 C8 C9 118.9(2) . . ? C10 C9 C8 119.3(2) . . ? C9 C10 C11 119.1(2) . . ? N1 C11 C10 121.6(2) . . ? N1 C11 C12 113.81(18) . . ? C10 C11 C12 124.6(2) . . ? N2 C12 C11 107.77(18) . . ? C14 C13 N2 124.4(2) . . ? C14 C13 C18 118.8(2) . . ? N2 C13 C18 116.80(19) . . ? C15 C14 C13 120.4(2) . . ? C16 C15 C14 120.7(2) . . ? C15 C16 C17 119.7(2) . . ? C16 C17 C18 120.2(2) . . ? C17 C18 C13 120.2(2) . . ? C17 C18 S 124.11(19) . . ? C13 C18 S 115.60(16) . . ? C21 C20 C21 117.7(4) . 2 ? C21 C20 C19 121.14(18) . . ? C21 C20 C19 121.14(18) 2 . ? C22 C21 C20 121.6(3) . . ? C21 C22 C23 119.8(3) . . ? C22 C23 C22 119.4(4) 2 . ? C11 N1 C7 119.36(19) . . ? C11 N1 Si 114.46(14) . . ? C7 N1 Si 126.04(16) . . ? C13 N2 C12 117.06(18) . . ? C13 N2 Si 121.76(14) . . ? C12 N2 Si 121.10(14) . . ? C18 S Si 95.88(8) . . ? N2 Si C1 116.73(9) . . ? N2 Si N1 82.56(8) . . ? C1 Si N1 93.78(8) . . ? N2 Si S 88.76(6) . . ? C1 Si S 100.56(7) . . ? N1 Si S 165.45(6) . . ? N2 Si Br 135.64(6) . . ? C1 Si Br 107.16(7) . . ? N1 Si Br 88.70(6) . . ? S Si Br 89.39(3) . . ? 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 C6 C1 C2 C3 0.8(3) . . . . ? Si C1 C2 C3 -174.25(16) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C6 1.2(4) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? Si C1 C6 C5 174.5(2) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? N1 C7 C8 C9 1.3(3) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 -1.6(3) . . . . ? C9 C10 C11 N1 1.5(3) . . . . ? C9 C10 C11 C12 -179.2(2) . . . . ? N1 C11 C12 N2 -0.3(2) . . . . ? C10 C11 C12 N2 -179.63(19) . . . . ? N2 C13 C14 C15 179.80(19) . . . . ? C18 C13 C14 C15 0.4(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 -0.6(3) . . . . ? C15 C16 C17 C18 0.9(3) . . . . ? C16 C17 C18 C13 -0.6(3) . . . . ? C16 C17 C18 S -176.78(17) . . . . ? C14 C13 C18 C17 -0.1(3) . . . . ? N2 C13 C18 C17 -179.53(17) . . . . ? C14 C13 C18 S 176.45(15) . . . . ? N2 C13 C18 S -3.0(2) . . . . ? C21 C20 C21 C22 -0.5(2) 2 . . . ? C19 C20 C21 C22 179.5(2) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C21 C22 C23 C22 -0.5(2) . . . 2 ? C10 C11 N1 C7 0.0(3) . . . . ? C12 C11 N1 C7 -179.39(18) . . . . ? C10 C11 N1 Si 175.99(16) . . . . ? C12 C11 N1 Si -3.4(2) . . . . ? C8 C7 N1 C11 -1.4(3) . . . . ? C8 C7 N1 Si -176.90(16) . . . . ? C14 C13 N2 C12 -2.8(3) . . . . ? C18 C13 N2 C12 176.66(16) . . . . ? C14 C13 N2 Si 173.96(15) . . . . ? C18 C13 N2 Si -6.6(2) . . . . ? C11 C12 N2 C13 -178.67(16) . . . . ? C11 C12 N2 Si 4.6(2) . . . . ? C17 C18 S Si -175.48(17) . . . . ? C13 C18 S Si 8.16(15) . . . . ? C13 N2 Si C1 -91.27(17) . . . . ? C12 N2 Si C1 85.31(16) . . . . ? C13 N2 Si N1 178.23(16) . . . . ? C12 N2 Si N1 -5.19(15) . . . . ? C13 N2 Si S 9.94(15) . . . . ? C12 N2 Si S -173.48(14) . . . . ? C13 N2 Si Br 97.79(15) . . . . ? C12 N2 Si Br -85.62(16) . . . . ? C2 C1 Si N2 174.08(16) . . . . ? C6 C1 Si N2 -1.0(2) . . . . ? C2 C1 Si N1 -102.35(18) . . . . ? C6 C1 Si N1 82.58(19) . . . . ? C2 C1 Si S 80.11(18) . . . . ? C6 C1 Si S -94.96(18) . . . . ? C2 C1 Si Br -12.54(19) . . . . ? C6 C1 Si Br 172.38(17) . . . . ? C11 N1 Si N2 4.75(14) . . . . ? C7 N1 Si N2 -179.56(17) . . . . ? C11 N1 Si C1 -111.73(15) . . . . ? C7 N1 Si C1 63.95(18) . . . . ? C11 N1 Si S 58.6(3) . . . . ? C7 N1 Si S -125.7(2) . . . . ? C11 N1 Si Br 141.16(13) . . . . ? C7 N1 Si Br -43.16(16) . . . . ? C18 S Si N2 -8.94(8) . . . . ? C18 S Si C1 108.03(10) . . . . ? C18 S Si N1 -62.2(3) . . . . ? C18 S Si Br -144.62(7) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.462 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.079 ##***************************** compound 3 x 0.5 C7H8 ***************** data_kob06d_3 _database_code_depnum_ccdc_archive 'CCDC 832634' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H15 N3 O S Si), C7 H8' _chemical_formula_sum 'C22.50 H19 N3 O S Si' _chemical_formula_weight 407.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.439(4) _cell_length_b 12.6603(18) _cell_length_c 16.963(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.544(15) _cell_angle_gamma 90.00 _cell_volume 4044.5(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 7.75 _cell_measurement_theta_max 24.8 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.238 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method 'omega scan ' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31456 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 29.14 _reflns_number_total 5407 _reflns_number_gt 4022 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob06b in C2/c CELL 0.71073 21.4387 12.6603 16.9629 90.000 118.544 90.000 ZERR 8.00 0.0035 0.0018 0.0024 0.000 0.015 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O Si S UNIT 180 152 24 8 8 8 L.S. 12 TEMP -100 ACTA HTAB 2.5 CONF BOND FMAP 2 PLAN 20 WGHT 0.063200 2.471300 FVAR 0.39209 MOLE 1 C1 1 0.157637 1.048977 0.101319 11.00000 0.02979 0.03375 = 0.03106 0.00098 0.01716 0.00128 C2 1 0.172408 1.111247 0.176682 11.00000 0.04252 0.03277 = 0.03135 0.00209 0.02028 0.00136 AFIX 43 H2 2 0.217056 1.104512 0.229221 11.00000 -1.20000 AFIX 0 C3 1 0.122702 1.182739 0.175715 11.00000 0.05838 0.03294 = 0.04407 0.00181 0.03468 0.00333 AFIX 43 H3 2 0.133613 1.223881 0.227547 11.00000 -1.20000 AFIX 0 C4 1 0.057558 1.194224 0.099783 11.00000 0.04630 0.03852 = 0.06168 0.00469 0.03603 0.00812 AFIX 43 H4 2 0.023603 1.242813 0.099284 11.00000 -1.20000 AFIX 0 C5 1 0.042274 1.134082 0.024330 11.00000 0.03268 0.05269 = 0.05377 0.00031 0.01606 0.00911 AFIX 43 H5 2 -0.002273 1.141829 -0.028205 11.00000 -1.20000 AFIX 0 C6 1 0.091946 1.062300 0.025163 11.00000 0.03195 0.04870 = 0.03838 -0.00566 0.01274 0.00582 AFIX 43 H6 2 0.080806 1.021813 -0.027067 11.00000 -1.20000 AFIX 0 C7 1 0.149251 0.736732 0.064992 11.00000 0.03187 0.03562 = 0.04167 0.00614 0.01998 0.00831 C8 1 0.112505 0.643046 0.057386 11.00000 0.04124 0.03801 = 0.05866 0.00880 0.02732 0.00587 AFIX 43 H8 2 0.109257 0.616632 0.107720 11.00000 -1.20000 AFIX 0 C9 1 0.080529 0.587951 -0.023591 11.00000 0.03986 0.03719 = 0.07343 -0.00157 0.02756 0.00097 AFIX 43 H9 2 0.055597 0.524131 -0.028575 11.00000 -1.20000 AFIX 0 C10 1 0.085408 0.627026 -0.096733 11.00000 0.03636 0.04726 = 0.06178 -0.01659 0.02229 0.00034 AFIX 43 H10 2 0.063763 0.589428 -0.151895 11.00000 -1.20000 AFIX 0 C11 1 0.121461 0.720312 -0.090582 11.00000 0.03789 0.04824 = 0.04310 -0.00717 0.02221 0.00363 AFIX 43 H11 2 0.124095 0.745972 -0.141538 11.00000 -1.20000 AFIX 0 C12 1 0.153970 0.776902 -0.009959 11.00000 0.02811 0.03744 = 0.03599 -0.00027 0.01772 0.00635 C13 1 0.199452 0.911399 -0.072434 11.00000 0.03881 0.04748 = 0.03008 0.00552 0.02203 0.00866 AFIX 23 H13A 2 0.152328 0.927073 -0.123961 11.00000 -1.20000 H13B 2 0.223207 0.857822 -0.091429 11.00000 -1.20000 AFIX 0 C14 1 0.243131 1.009360 -0.042428 11.00000 0.03674 0.04505 = 0.03940 0.01265 0.02551 0.01283 C15 1 0.265196 1.068541 -0.094436 11.00000 0.06082 0.04957 = 0.05854 0.01790 0.04326 0.01328 AFIX 43 H15 2 0.250893 1.049155 -0.154794 11.00000 -1.20000 AFIX 0 C16 1 0.307911 1.155181 -0.056659 11.00000 0.06366 0.05372 = 0.08274 0.02664 0.05321 0.01165 AFIX 43 H16 2 0.324019 1.195669 -0.090561 11.00000 -1.20000 AFIX 0 C17 1 0.327371 1.183197 0.031108 11.00000 0.04707 0.04343 = 0.08118 0.01565 0.03608 0.00199 AFIX 43 H17 2 0.357290 1.242404 0.058147 11.00000 -1.20000 AFIX 0 C18 1 0.302585 1.123691 0.078652 11.00000 0.03683 0.04274 = 0.05498 0.00808 0.02101 0.00003 AFIX 43 H18 2 0.314617 1.143906 0.138172 11.00000 -1.20000 AFIX 0 C19 1 0.359250 0.952944 0.258340 11.00000 0.03226 0.03247 = 0.03828 0.00035 0.01185 0.00170 C20 1 0.500000 0.148555 0.250000 10.50000 0.06626 0.05787 = 0.11820 0.00000 0.01505 0.00000 AFIX 137 H20A 2 0.507869 0.122752 0.308516 10.50000 -1.50000 H20B 2 0.538003 0.122752 0.238502 10.50000 -1.50000 H20C 2 0.454128 0.122752 0.202981 10.50000 -1.50000 AFIX 0 C21 1 0.500000 0.268084 0.250000 10.50000 0.03864 0.05243 = 0.05097 0.00000 0.01352 0.00000 C22 1 0.543777 0.324093 0.226624 11.00000 0.04460 0.08066 = 0.05567 -0.00961 0.02879 -0.00226 AFIX 43 H22 2 0.574657 0.286761 0.210851 11.00000 -1.20000 AFIX 0 C23 1 0.543915 0.432275 0.225543 11.00000 0.05931 0.07954 = 0.05385 0.00644 0.02566 -0.01888 AFIX 43 H23 2 0.573994 0.469044 0.208097 11.00000 -1.20000 AFIX 0 C24 1 0.500000 0.488256 0.250000 10.50000 0.07404 0.04795 = 0.05765 0.00000 0.00951 0.00000 AFIX 43 H24 2 0.499999 0.563293 0.249999 10.50000 -1.20000 AFIX 0 N1 3 0.261655 1.037467 0.042452 11.00000 0.02913 0.03972 = 0.03909 0.00779 0.01909 0.00506 N2 3 0.191387 0.871753 0.002991 11.00000 0.03315 0.03864 = 0.02924 0.00340 0.01932 0.00433 N3 3 0.301003 0.966336 0.203327 11.00000 0.03529 0.05370 = 0.03607 0.00349 0.01296 0.00313 O 4 0.417828 0.942434 0.315095 11.00000 0.03962 0.06936 = 0.07651 -0.00245 -0.00550 0.00727 S 6 0.194585 0.808470 0.164961 11.00000 0.04932 0.04156 = 0.03306 0.00803 0.02244 0.00305 SI 5 0.220986 0.946130 0.102608 11.00000 0.02784 0.03519 = 0.02746 0.00339 0.01405 0.00450 HKLF 4 REM kob06b in C2/c REM R1 = 0.0452 for 4022 Fo > 4sig(Fo) and 0.0625 for all 5407 data REM 260 parameters refined using 0 restraints END WGHT 0.0632 2.4715 REM Highest difference peak 0.373, deepest hole -0.541, 1-sigma level 0.053 Q1 1 0.2010 0.8778 0.1328 11.00000 0.05 0.37 Q2 1 0.1828 1.0195 0.1038 11.00000 0.05 0.37 Q3 1 0.2495 0.7866 0.2281 11.00000 0.05 0.28 Q4 1 0.4147 1.0032 0.2885 11.00000 0.05 0.28 Q5 1 0.2428 1.0166 0.0659 11.00000 0.05 0.25 Q6 1 0.2518 0.7991 0.1691 11.00000 0.05 0.24 Q7 1 0.1637 0.9440 0.0255 11.00000 0.05 0.24 Q8 1 0.3949 0.9355 0.3401 11.00000 0.05 0.23 Q9 1 0.2413 0.8821 0.0627 11.00000 0.05 0.23 Q10 1 0.2082 0.7217 0.1386 11.00000 0.05 0.22 Q11 1 0.1388 0.8327 0.1613 11.00000 0.05 0.22 Q12 1 0.2692 0.8998 0.1650 11.00000 0.05 0.21 Q13 1 0.1687 1.0626 0.1432 11.00000 0.05 0.21 Q14 1 0.1453 1.1399 0.1820 11.00000 0.05 0.20 Q15 1 0.1528 0.8751 0.1402 11.00000 0.05 0.19 Q16 1 0.2505 0.8222 0.0412 11.00000 0.05 0.19 Q17 1 0.1370 0.8854 -0.0091 11.00000 0.05 0.19 Q18 1 0.1456 0.6862 0.0728 11.00000 0.05 0.18 Q19 1 0.2011 0.9861 -0.0719 11.00000 0.05 0.18 Q20 1 0.2840 0.9537 0.1552 11.00000 0.05 0.18 ; _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^)+(0.0632P)^2^+2.4713P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5407 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1170 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15764(8) 1.04898(13) 0.10132(11) 0.0305(3) Uani 1 1 d . . . C2 C 0.17241(9) 1.11125(13) 0.17668(11) 0.0345(3) Uani 1 1 d . . . H2 H 0.2171 1.1045 0.2292 0.041 Uiso 1 1 calc R . . C3 C 0.12270(11) 1.18274(14) 0.17572(13) 0.0409(4) Uani 1 1 d . . . H3 H 0.1336 1.2239 0.2275 0.049 Uiso 1 1 calc R . . C4 C 0.05756(11) 1.19422(15) 0.09978(15) 0.0446(4) Uani 1 1 d . . . H4 H 0.0236 1.2428 0.0993 0.054 Uiso 1 1 calc R . . C5 C 0.04227(10) 1.13408(17) 0.02433(15) 0.0483(5) Uani 1 1 d . . . H5 H -0.0023 1.1418 -0.0282 0.058 Uiso 1 1 calc R . . C6 C 0.09195(9) 1.06230(16) 0.02516(13) 0.0414(4) Uani 1 1 d . . . H6 H 0.0808 1.0218 -0.0271 0.050 Uiso 1 1 calc R . . C7 C 0.14925(9) 0.73673(14) 0.06499(12) 0.0354(3) Uani 1 1 d . . . C8 C 0.11251(10) 0.64305(15) 0.05739(15) 0.0445(4) Uani 1 1 d . . . H8 H 0.1093 0.6166 0.1077 0.053 Uiso 1 1 calc R . . C9 C 0.08053(10) 0.58795(16) -0.02359(16) 0.0500(5) Uani 1 1 d . . . H9 H 0.0556 0.5241 -0.0286 0.060 Uiso 1 1 calc R . . C10 C 0.08541(10) 0.62703(17) -0.09673(16) 0.0489(5) Uani 1 1 d . . . H10 H 0.0638 0.5894 -0.1519 0.059 Uiso 1 1 calc R . . C11 C 0.12146(10) 0.72031(16) -0.09058(13) 0.0419(4) Uani 1 1 d . . . H11 H 0.1241 0.7460 -0.1415 0.050 Uiso 1 1 calc R . . C12 C 0.15397(8) 0.77690(14) -0.00996(11) 0.0329(3) Uani 1 1 d . . . C13 C 0.19945(9) 0.91140(15) -0.07243(11) 0.0365(4) Uani 1 1 d . . . H13A H 0.1523 0.9271 -0.1240 0.044 Uiso 1 1 calc R . . H13B H 0.2232 0.8578 -0.0914 0.044 Uiso 1 1 calc R . . C14 C 0.24313(9) 1.00936(15) -0.04243(12) 0.0374(4) Uani 1 1 d . . . C15 C 0.26520(12) 1.06854(17) -0.09444(16) 0.0502(5) Uani 1 1 d . . . H15 H 0.2509 1.0492 -0.1548 0.060 Uiso 1 1 calc R . . C16 C 0.30791(13) 1.15518(19) -0.05666(18) 0.0592(6) Uani 1 1 d . . . H16 H 0.3240 1.1957 -0.0906 0.071 Uiso 1 1 calc R . . C17 C 0.32737(12) 1.18320(17) 0.03111(18) 0.0550(6) Uani 1 1 d . . . H17 H 0.3573 1.2424 0.0581 0.066 Uiso 1 1 calc R . . C18 C 0.30259(10) 1.12369(16) 0.07865(15) 0.0452(4) Uani 1 1 d . . . H18 H 0.3146 1.1439 0.1382 0.054 Uiso 1 1 calc R . . C19 C 0.35925(9) 0.95294(13) 0.25834(12) 0.0364(4) Uani 1 1 d . . . C20 C 0.5000 0.1486(3) 0.2500 0.0928(15) Uani 1 2 d S . . H20A H 0.5079 0.1228 0.3085 0.139 Uiso 0.50 1 calc PR . . H20B H 0.5380 0.1228 0.2385 0.139 Uiso 0.50 1 calc PR . . H20C H 0.4541 0.1228 0.2030 0.139 Uiso 0.50 1 calc PR . . C21 C 0.5000 0.2681(3) 0.2500 0.0506(7) Uani 1 2 d S . . C22 C 0.54378(12) 0.3241(2) 0.22662(16) 0.0583(6) Uani 1 1 d . . . H22 H 0.5747 0.2868 0.2109 0.070 Uiso 1 1 calc R . . C23 C 0.54392(14) 0.4323(2) 0.22554(17) 0.0648(7) Uani 1 1 d . . . H23 H 0.5740 0.4690 0.2081 0.078 Uiso 1 1 calc R . . C24 C 0.5000 0.4883(3) 0.2500 0.0689(10) Uani 1 2 d S . . H24 H 0.5000 0.5633 0.2500 0.083 Uiso 1 2 calc SR . . N1 N 0.26166(7) 1.03747(12) 0.04245(10) 0.0348(3) Uani 1 1 d . . . N2 N 0.19139(7) 0.87175(11) 0.00299(9) 0.0319(3) Uani 1 1 d . . . N3 N 0.30100(8) 0.96634(14) 0.20333(10) 0.0434(4) Uani 1 1 d . . . O O 0.41783(8) 0.94243(15) 0.31509(13) 0.0756(6) Uani 1 1 d . . . S S 0.19458(3) 0.80847(4) 0.16496(3) 0.04017(13) Uani 1 1 d . . . Si Si 0.22099(2) 0.94613(4) 0.10261(3) 0.02981(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0298(7) 0.0338(8) 0.0311(8) 0.0010(6) 0.0172(6) 0.0013(6) C2 0.0425(9) 0.0328(8) 0.0314(8) 0.0021(6) 0.0203(7) 0.0014(7) C3 0.0584(11) 0.0329(8) 0.0441(10) 0.0018(7) 0.0347(9) 0.0033(8) C4 0.0463(10) 0.0385(9) 0.0617(12) 0.0047(8) 0.0360(10) 0.0081(8) C5 0.0327(9) 0.0527(11) 0.0538(11) 0.0003(9) 0.0161(8) 0.0091(8) C6 0.0320(8) 0.0487(10) 0.0384(9) -0.0057(8) 0.0127(7) 0.0058(7) C7 0.0319(8) 0.0356(8) 0.0417(9) 0.0061(7) 0.0200(7) 0.0083(6) C8 0.0412(9) 0.0380(9) 0.0587(12) 0.0088(8) 0.0273(9) 0.0059(7) C9 0.0399(9) 0.0372(10) 0.0734(14) -0.0016(9) 0.0276(10) 0.0010(8) C10 0.0364(9) 0.0473(11) 0.0618(13) -0.0166(9) 0.0223(9) 0.0003(8) C11 0.0379(9) 0.0482(10) 0.0431(10) -0.0072(8) 0.0222(8) 0.0036(7) C12 0.0281(7) 0.0374(8) 0.0360(8) -0.0003(6) 0.0177(6) 0.0063(6) C13 0.0388(8) 0.0475(9) 0.0301(8) 0.0055(7) 0.0220(7) 0.0087(7) C14 0.0367(8) 0.0450(9) 0.0394(9) 0.0126(7) 0.0255(7) 0.0128(7) C15 0.0608(12) 0.0496(11) 0.0585(12) 0.0179(9) 0.0433(11) 0.0133(9) C16 0.0637(13) 0.0537(12) 0.0827(17) 0.0266(12) 0.0532(13) 0.0116(10) C17 0.0471(11) 0.0434(11) 0.0812(16) 0.0156(10) 0.0361(11) 0.0020(9) C18 0.0368(9) 0.0427(10) 0.0550(11) 0.0081(8) 0.0210(8) 0.0000(7) C19 0.0323(8) 0.0325(8) 0.0383(9) 0.0004(7) 0.0118(7) 0.0017(6) C20 0.066(2) 0.058(2) 0.118(4) 0.000 0.015(2) 0.000 C21 0.0386(13) 0.0524(16) 0.0510(16) 0.000 0.0135(12) 0.000 C22 0.0446(11) 0.0807(17) 0.0557(13) -0.0096(11) 0.0288(10) -0.0023(11) C23 0.0593(14) 0.0795(17) 0.0538(13) 0.0064(12) 0.0257(11) -0.0189(12) C24 0.074(2) 0.0480(18) 0.058(2) 0.000 0.0095(17) 0.000 N1 0.0291(6) 0.0397(7) 0.0391(7) 0.0078(6) 0.0191(6) 0.0051(5) N2 0.0331(6) 0.0386(7) 0.0292(6) 0.0034(5) 0.0193(5) 0.0043(5) N3 0.0353(8) 0.0537(10) 0.0361(8) 0.0035(7) 0.0130(6) 0.0031(7) O 0.0396(8) 0.0694(11) 0.0765(12) -0.0024(9) -0.0055(8) 0.0073(7) S 0.0493(3) 0.0416(2) 0.0331(2) 0.00803(17) 0.02244(19) 0.00305(19) Si 0.0278(2) 0.0352(2) 0.0275(2) 0.00339(17) 0.01405(17) 0.00450(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.394(2) . ? C1 C2 1.403(2) . ? C1 Si 1.8740(16) . ? C2 C3 1.392(2) . ? C3 C4 1.383(3) . ? C4 C5 1.387(3) . ? C5 C6 1.395(3) . ? C7 C8 1.395(3) . ? C7 C12 1.417(2) . ? C7 S 1.7521(19) . ? C8 C9 1.394(3) . ? C9 C10 1.385(3) . ? C10 C11 1.388(3) . ? C11 C12 1.399(2) . ? C12 N2 1.402(2) . ? C13 N2 1.460(2) . ? C13 C14 1.490(3) . ? C14 N1 1.346(2) . ? C14 C15 1.401(2) . ? C15 C16 1.375(3) . ? C16 C17 1.387(4) . ? C17 C18 1.382(3) . ? C18 N1 1.350(2) . ? C19 N3 1.160(2) . ? C19 O 1.169(2) . ? C20 C21 1.513(5) . ? C21 C22 1.377(3) . ? C21 C22 1.377(3) 2_655 ? C22 C23 1.370(4) . ? C23 C24 1.391(3) . ? C24 C23 1.391(3) 2_655 ? N1 Si 1.9972(15) . ? N2 Si 1.7664(15) . ? N3 Si 1.7681(17) . ? S Si 2.2469(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.69(15) . . ? C6 C1 Si 120.04(13) . . ? C2 C1 Si 122.20(12) . . ? C3 C2 C1 121.08(17) . . ? C4 C3 C2 120.40(17) . . ? C3 C4 C5 119.34(17) . . ? C4 C5 C6 120.37(18) . . ? C1 C6 C5 121.11(18) . . ? C8 C7 C12 120.09(18) . . ? C8 C7 S 123.90(15) . . ? C12 C7 S 115.97(13) . . ? C9 C8 C7 120.43(19) . . ? C10 C9 C8 119.46(19) . . ? C9 C10 C11 120.95(19) . . ? C10 C11 C12 120.57(19) . . ? C11 C12 N2 124.90(16) . . ? C11 C12 C7 118.51(17) . . ? N2 C12 C7 116.59(15) . . ? N2 C13 C14 107.77(14) . . ? N1 C14 C15 121.10(19) . . ? N1 C14 C13 113.69(14) . . ? C15 C14 C13 125.21(18) . . ? C16 C15 C14 118.9(2) . . ? C15 C16 C17 119.74(19) . . ? C18 C17 C16 119.0(2) . . ? N1 C18 C17 121.5(2) . . ? N3 C19 O 177.8(2) . . ? C22 C21 C22 118.0(3) . 2_655 ? C22 C21 C20 120.99(16) . . ? C22 C21 C20 120.99(16) 2_655 . ? C23 C22 C21 121.7(2) . . ? C22 C23 C24 120.0(2) . . ? C23 C24 C23 118.7(3) . 2_655 ? C14 N1 C18 119.72(16) . . ? C14 N1 Si 114.57(12) . . ? C18 N1 Si 125.67(14) . . ? C12 N2 C13 117.12(14) . . ? C12 N2 Si 121.58(11) . . ? C13 N2 Si 121.09(12) . . ? C19 N3 Si 158.55(16) . . ? C7 S Si 95.42(6) . . ? N2 Si N3 137.79(7) . . ? N2 Si C1 115.61(7) . . ? N3 Si C1 105.89(8) . . ? N2 Si N1 82.23(7) . . ? N3 Si N1 87.20(7) . . ? C1 Si N1 94.74(7) . . ? N2 Si S 88.89(5) . . ? N3 Si S 90.21(6) . . ? C1 Si S 101.55(5) . . ? N1 Si S 163.59(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 C6 C1 C2 C3 0.9(2) . . . . ? Si C1 C2 C3 -176.15(13) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 C6 0.4(3) . . . . ? C2 C1 C6 C5 -0.8(3) . . . . ? Si C1 C6 C5 176.30(16) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? C12 C7 C8 C9 0.4(3) . . . . ? S C7 C8 C9 -176.98(14) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C9 C10 C11 C12 0.2(3) . . . . ? C10 C11 C12 N2 -179.86(16) . . . . ? C10 C11 C12 C7 0.1(2) . . . . ? C8 C7 C12 C11 -0.3(2) . . . . ? S C7 C12 C11 177.20(12) . . . . ? C8 C7 C12 N2 179.58(14) . . . . ? S C7 C12 N2 -2.88(19) . . . . ? N2 C13 C14 N1 -1.86(19) . . . . ? N2 C13 C14 C15 177.17(16) . . . . ? N1 C14 C15 C16 1.6(3) . . . . ? C13 C14 C15 C16 -177.37(18) . . . . ? C14 C15 C16 C17 -1.0(3) . . . . ? C15 C16 C17 C18 -0.7(3) . . . . ? C16 C17 C18 N1 1.9(3) . . . . ? C22 C21 C22 C23 -0.59(18) 2_655 . . . ? C20 C21 C22 C23 179.41(18) . . . . ? C21 C22 C23 C24 1.2(4) . . . . ? C22 C23 C24 C23 -0.57(17) . . . 2_655 ? C15 C14 N1 C18 -0.4(2) . . . . ? C13 C14 N1 C18 178.62(15) . . . . ? C15 C14 N1 Si 177.36(14) . . . . ? C13 C14 N1 Si -3.57(18) . . . . ? C17 C18 N1 C14 -1.3(3) . . . . ? C17 C18 N1 Si -178.87(14) . . . . ? C11 C12 N2 C13 -2.9(2) . . . . ? C7 C12 N2 C13 177.23(14) . . . . ? C11 C12 N2 Si 171.87(13) . . . . ? C7 C12 N2 Si -8.04(19) . . . . ? C14 C13 N2 C12 -177.61(13) . . . . ? C14 C13 N2 Si 7.64(18) . . . . ? O C19 N3 Si 172(100) . . . . ? C8 C7 S Si -173.61(14) . . . . ? C12 C7 S Si 8.96(12) . . . . ? C12 N2 Si N3 100.65(15) . . . . ? C13 N2 Si N3 -84.83(16) . . . . ? C12 N2 Si C1 -90.73(13) . . . . ? C13 N2 Si C1 83.79(13) . . . . ? C12 N2 Si N1 177.72(13) . . . . ? C13 N2 Si N1 -7.77(12) . . . . ? C12 N2 Si S 11.56(12) . . . . ? C13 N2 Si S -173.93(12) . . . . ? C19 N3 Si N2 -11.1(5) . . . . ? C19 N3 Si C1 179.6(4) . . . . ? C19 N3 Si N1 -86.3(4) . . . . ? C19 N3 Si S 77.5(4) . . . . ? C6 C1 Si N2 0.33(17) . . . . ? C2 C1 Si N2 177.31(12) . . . . ? C6 C1 Si N3 172.40(14) . . . . ? C2 C1 Si N3 -10.62(16) . . . . ? C6 C1 Si N1 83.97(15) . . . . ? C2 C1 Si N1 -99.04(14) . . . . ? C6 C1 Si S -94.04(14) . . . . ? C2 C1 Si S 82.95(14) . . . . ? C14 N1 Si N2 6.23(12) . . . . ? C18 N1 Si N2 -176.11(15) . . . . ? C14 N1 Si N3 145.27(13) . . . . ? C18 N1 Si N3 -37.07(15) . . . . ? C14 N1 Si C1 -109.01(12) . . . . ? C18 N1 Si C1 68.65(15) . . . . ? C14 N1 Si S 64.1(2) . . . . ? C18 N1 Si S -118.26(19) . . . . ? C7 S Si N2 -10.09(7) . . . . ? C7 S Si N3 -147.89(8) . . . . ? C7 S Si C1 105.84(8) . . . . ? C7 S Si N1 -67.13(19) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.373 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.053 ##***************************** compound 4 ************************************ data_kob01l_4 _database_code_depnum_ccdc_archive 'CCDC 832635' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H15 N3 S2 Si' _chemical_formula_sum 'C19 H15 N3 S2 Si' _chemical_formula_weight 377.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.1469(13) _cell_length_b 22.193(3) _cell_length_c 29.661(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7337.6(17) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.15 _cell_measurement_theta_max 24.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3136 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7906 _exptl_absorpt_correction_T_max 0.8184 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60861 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.99 _reflns_number_total 8810 _reflns_number_gt 5938 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. Twinned structure ? It was considered that the relatively high R-factor, the high difference electron density 1.34 and the K-Value 2.7 for small reflections might be due to twinning. Furthermore Xprep found a monoclinic cell based on the original triclinic cell with beta 90.13 degrees. So a refinement was carried out in the space group P21/c (TWIN 1 0 0 0 -1 0 0 0 -1, BASF 0.5) which led to somewhat better results but with almost twice the number of parameters. The highly elongated ellipsoids C8 C9 C10 C11 still remained. So finally the orthorhombic space group Pbca still was given preference. TITL kob01c in Pbca CELL 0.71073 11.1469 22.1932 29.6608 90.000 90.000 90.000 ZERR 16. 0.0013 0.0026 0.0047 0.000 0.000 0.000 REM CELL 0.71073 11.1501 22.2657 29.5444 90.000 90.000 90.000 REM ZERR 16.00 0.0022 0.0045 0.0059 0.000 0.000 0.000 LATT 1 SYMM 0.5-X, -Y, 0.5+Z SYMM -X, 0.5+Y, 0.5-Z SYMM 0.5+X, 0.5-Y, -Z SFAC C H N Si S UNIT 304 240 48 16 32 L.S. 8 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.095600 2.350000 FVAR 0.35299 MOLE 2 C1 1 1.078715 0.116960 0.156875 11.00000 0.03620 0.05557 = 0.03681 -0.00431 0.00058 0.00070 C2 1 1.181321 0.136484 0.134284 11.00000 0.04479 0.08817 = 0.04086 -0.00607 0.00520 -0.01010 AFIX 43 H2 2 1.188334 0.177310 0.125024 11.00000 -1.20000 AFIX 0 C3 1 1.275549 0.094876 0.125169 11.00000 0.03569 0.14795 = 0.04474 -0.02798 0.00391 -0.00575 AFIX 43 H3 2 1.345455 0.107797 0.109607 11.00000 -1.20000 AFIX 0 C4 1 1.264888 0.035058 0.139167 11.00000 0.05589 0.09187 = 0.06545 -0.03753 -0.01656 0.02321 AFIX 43 H4 2 1.328164 0.007520 0.133181 11.00000 -1.20000 AFIX 0 C5 1 1.168482 0.016292 0.160524 11.00000 0.06229 0.06005 = 0.08667 -0.01771 -0.01963 0.01193 AFIX 43 H5 2 1.162692 -0.024567 0.169823 11.00000 -1.20000 AFIX 0 C6 1 1.074962 0.055981 0.169561 11.00000 0.04860 0.05224 = 0.07004 -0.00628 0.00037 0.00652 AFIX 43 H6 2 1.006019 0.041330 0.184870 11.00000 -1.20000 AFIX 0 C7 1 0.738176 0.095204 0.139786 11.00000 0.03879 0.06571 = 0.09335 -0.02375 -0.00688 0.01311 C8 1 0.654966 0.058346 0.118183 11.00000 0.04150 0.07731 = 0.15790 -0.04652 -0.01696 0.01043 AFIX 43 H8 2 0.644184 0.061060 0.086477 11.00000 -1.20000 AFIX 0 C9 1 0.588907 0.018258 0.142818 11.00000 0.05160 0.07040 = 0.25062 -0.04826 -0.02606 0.01289 AFIX 43 H9 2 0.533554 -0.007458 0.127890 11.00000 -1.20000 AFIX 0 C10 1 0.601557 0.014448 0.189986 11.00000 0.03858 0.05265 = 0.25956 0.01833 0.01876 0.00159 AFIX 43 H10 2 0.553468 -0.012990 0.206652 11.00000 -1.20000 AFIX 0 C11 1 0.685506 0.051298 0.212547 11.00000 0.04179 0.05049 = 0.15990 0.01937 0.01812 0.00854 AFIX 43 H11 2 0.694542 0.048972 0.244348 11.00000 -1.20000 AFIX 0 C12 1 0.754616 0.091004 0.187381 11.00000 0.03250 0.04345 = 0.09592 0.00074 0.00963 0.00619 C13 1 0.860754 0.126971 0.254660 11.00000 0.05144 0.06356 = 0.05056 0.01880 0.01777 0.01376 AFIX 23 H13A 2 0.882235 0.085691 0.264400 11.00000 -1.20000 H13B 2 0.786211 0.139082 0.270380 11.00000 -1.20000 AFIX 0 C14 1 0.959430 0.169533 0.265702 11.00000 0.05529 0.05209 = 0.04168 0.00565 0.00649 0.02118 C15 1 0.998357 0.183698 0.309005 11.00000 0.07912 0.08495 = 0.04661 -0.00139 -0.00167 0.03455 AFIX 43 H15 2 0.958951 0.166912 0.334476 11.00000 -1.20000 AFIX 0 C16 1 1.092789 0.221566 0.314760 11.00000 0.09160 0.07233 = 0.05914 -0.01319 -0.02088 0.03523 AFIX 43 H16 2 1.119661 0.231766 0.344181 11.00000 -1.20000 AFIX 0 C17 1 1.148599 0.244786 0.277604 11.00000 0.07781 0.04275 = 0.08949 -0.01626 -0.02916 0.01402 AFIX 43 H17 2 1.216061 0.270512 0.281146 11.00000 -1.20000 AFIX 0 C18 1 1.106991 0.230895 0.234550 11.00000 0.06049 0.03811 = 0.06928 0.00125 -0.00938 0.00216 AFIX 43 H18 2 1.145016 0.247886 0.208860 11.00000 -1.20000 AFIX 0 C19 1 0.957856 0.284128 0.130499 11.00000 0.07751 0.05640 = 0.04755 0.00635 -0.00651 -0.00011 MOLE 1 C21 1 0.411813 0.285521 0.067505 11.00000 0.05082 0.04209 = 0.04047 0.00473 0.00421 -0.00110 C22 1 0.519438 0.254408 0.061403 11.00000 0.05848 0.05552 = 0.05754 -0.00193 0.00761 0.01011 AFIX 43 H22 2 0.592401 0.271619 0.071802 11.00000 -1.20000 AFIX 0 C23 1 0.520968 0.198294 0.040190 11.00000 0.08695 0.06131 = 0.07599 -0.00116 0.02201 0.01735 AFIX 43 H23 2 0.594407 0.177012 0.036940 11.00000 -1.20000 AFIX 0 C24 1 0.415574 0.173658 0.023895 11.00000 0.11718 0.05315 = 0.08364 -0.01816 0.01580 -0.00172 AFIX 43 H24 2 0.416969 0.135571 0.009285 11.00000 -1.20000 AFIX 0 C25 1 0.307425 0.204372 0.028787 11.00000 0.09497 0.06023 = 0.09519 -0.01599 -0.00686 -0.01615 AFIX 43 H25 2 0.235258 0.187707 0.017177 11.00000 -1.20000 AFIX 0 C26 1 0.306065 0.259492 0.050755 11.00000 0.06072 0.04954 = 0.08059 -0.00868 -0.00277 -0.00983 AFIX 43 H26 2 0.232028 0.280077 0.054552 11.00000 -1.20000 AFIX 0 C27 1 0.434309 0.361432 0.196105 11.00000 0.04015 0.04558 = 0.03607 0.00330 0.00263 0.01076 C28 1 0.433629 0.356617 0.243219 11.00000 0.05103 0.05769 = 0.03621 0.00691 0.00557 0.01390 AFIX 43 H28 2 0.367477 0.338222 0.257995 11.00000 -1.20000 AFIX 0 C29 1 0.528782 0.378507 0.268355 11.00000 0.06267 0.06125 = 0.03565 0.00139 0.00009 0.02195 AFIX 43 H29 2 0.528390 0.374395 0.300236 11.00000 -1.20000 AFIX 0 C30 1 0.624210 0.406288 0.247208 11.00000 0.05425 0.05974 = 0.04216 -0.00547 -0.01170 0.01377 AFIX 43 H30 2 0.688883 0.421688 0.264597 11.00000 -1.20000 AFIX 0 C31 1 0.625921 0.411817 0.200269 11.00000 0.04386 0.05509 = 0.04258 -0.00093 -0.00342 0.00371 AFIX 43 H31 2 0.691793 0.431028 0.185902 11.00000 -1.20000 AFIX 0 C32 1 0.531515 0.389306 0.174374 11.00000 0.03891 0.04510 = 0.03494 0.00112 -0.00198 0.00701 C33 1 0.622755 0.426598 0.105346 11.00000 0.04137 0.06043 = 0.04211 0.00165 0.00204 -0.01637 AFIX 23 H33A 2 0.701141 0.407424 0.111704 11.00000 -1.20000 H33B 2 0.624749 0.468435 0.116903 11.00000 -1.20000 AFIX 0 C34 1 0.598649 0.426524 0.055805 11.00000 0.04319 0.04305 = 0.04085 -0.00073 0.00707 -0.00794 C35 1 0.673441 0.452670 0.023497 11.00000 0.05750 0.05241 = 0.04798 -0.00298 0.01579 -0.01617 AFIX 43 H35 2 0.745455 0.472458 0.032108 11.00000 -1.20000 AFIX 0 C36 1 0.640158 0.449061 -0.021318 11.00000 0.07434 0.04801 = 0.04264 -0.00167 0.02204 -0.00948 AFIX 43 H36 2 0.689505 0.466434 -0.043966 11.00000 -1.20000 AFIX 0 C37 1 0.534983 0.420138 -0.033102 11.00000 0.07153 0.04796 = 0.03609 -0.00214 0.00742 -0.00373 AFIX 43 H37 2 0.510790 0.417817 -0.063764 11.00000 -1.20000 AFIX 0 C38 1 0.465618 0.394662 0.000422 11.00000 0.05545 0.04761 = 0.03331 0.00007 0.00126 -0.00527 AFIX 43 H38 2 0.394022 0.373999 -0.007505 11.00000 -1.20000 AFIX 0 C39 1 0.197929 0.422744 0.057349 11.00000 0.04279 0.04184 = 0.04218 0.00118 -0.00032 -0.00520 MOLE 2 N2 3 0.842890 0.128574 0.206136 11.00000 0.04022 0.04807 = 0.05234 0.00647 0.00710 0.00496 N1 3 1.012332 0.193174 0.229232 11.00000 0.04994 0.03717 = 0.04683 0.00263 0.00148 0.00923 N3 3 0.972834 0.238973 0.150739 11.00000 0.08622 0.05474 = 0.05917 0.01773 -0.00606 0.00172 MOLE 1 N22 3 0.526425 0.392879 0.126972 11.00000 0.03663 0.04818 = 0.03508 0.00253 0.00338 -0.00632 N21 3 0.497525 0.398527 0.044302 11.00000 0.04339 0.04112 = 0.03468 0.00167 0.00276 -0.00448 N23 3 0.279434 0.399075 0.074933 11.00000 0.04260 0.04900 = 0.04368 0.00471 -0.00178 0.00128 MOLE 2 S1 5 0.824334 0.149744 0.112022 11.00000 0.04639 0.09794 = 0.05002 -0.00844 -0.00401 0.01049 S2 5 0.943880 0.345016 0.103835 11.00000 0.12819 0.06595 = 0.08330 0.03318 -0.02214 -0.00216 MOLE 1 S21 5 0.318314 0.335136 0.161035 11.00000 0.03960 0.06338 = 0.04033 0.00510 0.00591 -0.00723 S22 5 0.088544 0.456103 0.033319 11.00000 0.04654 0.06376 = 0.07278 0.02301 -0.01658 -0.00248 MOLE 2 SI1 4 0.946438 0.164840 0.170948 11.00000 0.04032 0.04490 = 0.03920 0.00498 0.00404 0.00421 MOLE 1 SI21 4 0.408193 0.361010 0.096135 11.00000 0.03405 0.04029 = 0.03405 0.00178 0.00055 -0.00149 HKLF 4 REM kob01c in Pbca REM R1 = 0.0571 for 5938 Fo > 4sig(Fo) and 0.0837 for all 8810 data REM 451 parameters refined using 0 restraints END WGHT 0.0956 2.3503 REM Highest difference peak 1.343, deepest hole -0.844, 1-sigma level 0.064 Q1 1 0.8167 0.1094 0.1164 11.00000 0.05 1.34 Q2 1 0.8569 0.3378 0.1149 11.00000 0.05 0.67 Q3 1 0.6034 0.0096 0.2209 11.00000 0.05 0.42 Q4 1 1.2858 0.1394 0.1176 11.00000 0.05 0.39 Q5 1 0.4086 0.3171 0.0706 11.00000 0.05 0.35 Q6 1 0.6140 0.0145 0.1786 11.00000 0.05 0.34 Q7 1 0.3961 0.3316 0.1325 11.00000 0.05 0.33 Q8 1 0.4572 0.1652 0.0550 11.00000 0.05 0.32 Q9 1 1.1209 0.0736 0.1513 11.00000 0.05 0.31 Q10 1 0.9075 0.3208 0.0805 11.00000 0.05 0.30 Q11 1 0.5758 -0.0059 0.1741 11.00000 0.05 0.30 Q12 1 0.6375 0.0355 0.1428 11.00000 0.05 0.28 Q13 1 1.1947 0.0474 0.1486 11.00000 0.05 0.28 Q14 1 0.8965 0.1354 0.1796 11.00000 0.05 0.28 Q15 1 0.8651 0.2811 0.1564 11.00000 0.05 0.27 Q16 1 0.7377 0.0669 0.1561 11.00000 0.05 0.27 Q17 1 0.3244 0.3588 0.1249 11.00000 0.05 0.27 Q18 1 0.9886 0.2404 0.0924 11.00000 0.05 0.25 Q19 1 0.3439 0.3746 0.1312 11.00000 0.05 0.25 Q20 1 0.9749 0.2978 0.0758 11.00000 0.05 0.25 ; _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^)+(0.0956P)^2^+2.3500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8810 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0787(2) 0.11696(13) 0.15688(9) 0.0429(6) Uani 1 1 d . . . C2 C 1.1813(3) 0.13648(18) 0.13428(10) 0.0579(8) Uani 1 1 d . . . H2 H 1.1883 0.1773 0.1250 0.070 Uiso 1 1 calc R . . C3 C 1.2755(3) 0.0949(2) 0.12517(11) 0.0761(13) Uani 1 1 d . . . H3 H 1.3455 0.1078 0.1096 0.091 Uiso 1 1 calc R . . C4 C 1.2649(3) 0.0351(2) 0.13917(13) 0.0711(11) Uani 1 1 d . . . H4 H 1.3282 0.0075 0.1332 0.085 Uiso 1 1 calc R . . C5 C 1.1685(3) 0.01629(18) 0.16052(14) 0.0697(10) Uani 1 1 d . . . H5 H 1.1627 -0.0246 0.1698 0.084 Uiso 1 1 calc R . . C6 C 1.0750(3) 0.05598(15) 0.16956(12) 0.0570(7) Uani 1 1 d . . . H6 H 1.0060 0.0413 0.1849 0.068 Uiso 1 1 calc R . . C7 C 0.7382(3) 0.09520(17) 0.13979(14) 0.0659(9) Uani 1 1 d . . . C8 C 0.6550(3) 0.0583(2) 0.1182(2) 0.0922(16) Uani 1 1 d . . . H8 H 0.6442 0.0611 0.0865 0.111 Uiso 1 1 calc R . . C9 C 0.5889(4) 0.0183(3) 0.1428(3) 0.124(3) Uani 1 1 d . . . H9 H 0.5336 -0.0075 0.1279 0.149 Uiso 1 1 calc R . . C10 C 0.6016(4) 0.0144(2) 0.1900(3) 0.117(2) Uani 1 1 d . . . H10 H 0.5535 -0.0130 0.2067 0.140 Uiso 1 1 calc R . . C11 C 0.6855(3) 0.05130(16) 0.2125(2) 0.0841(14) Uani 1 1 d . . . H11 H 0.6945 0.0490 0.2443 0.101 Uiso 1 1 calc R . . C12 C 0.7546(3) 0.09100(14) 0.18738(13) 0.0573(8) Uani 1 1 d . . . C13 C 0.8608(3) 0.12697(15) 0.25466(10) 0.0552(8) Uani 1 1 d . . . H13A H 0.8822 0.0857 0.2644 0.066 Uiso 1 1 calc R . . H13B H 0.7862 0.1391 0.2704 0.066 Uiso 1 1 calc R . . C14 C 0.9594(3) 0.16953(14) 0.26570(9) 0.0497(7) Uani 1 1 d . . . C15 C 0.9984(4) 0.1837(2) 0.30901(11) 0.0702(10) Uani 1 1 d . . . H15 H 0.9590 0.1669 0.3345 0.084 Uiso 1 1 calc R . . C16 C 1.0928(4) 0.22157(19) 0.31476(13) 0.0744(11) Uani 1 1 d . . . H16 H 1.1197 0.2318 0.3442 0.089 Uiso 1 1 calc R . . C17 C 1.1486(4) 0.24479(15) 0.27760(14) 0.0700(10) Uani 1 1 d . . . H17 H 1.2161 0.2705 0.2811 0.084 Uiso 1 1 calc R . . C18 C 1.1070(3) 0.23089(13) 0.23455(12) 0.0560(7) Uani 1 1 d . . . H18 H 1.1450 0.2479 0.2089 0.067 Uiso 1 1 calc R . . C19 C 0.9579(3) 0.28413(16) 0.13050(11) 0.0605(8) Uani 1 1 d . . . C21 C 0.4118(3) 0.28552(12) 0.06751(9) 0.0445(6) Uani 1 1 d . . . C22 C 0.5194(3) 0.25441(15) 0.06140(11) 0.0572(7) Uani 1 1 d . . . H22 H 0.5924 0.2716 0.0718 0.069 Uiso 1 1 calc R . . C23 C 0.5210(4) 0.19829(18) 0.04019(14) 0.0748(11) Uani 1 1 d . . . H23 H 0.5944 0.1770 0.0369 0.090 Uiso 1 1 calc R . . C24 C 0.4156(5) 0.17366(18) 0.02390(15) 0.0847(13) Uani 1 1 d . . . H24 H 0.4170 0.1356 0.0093 0.102 Uiso 1 1 calc R . . C25 C 0.3074(5) 0.20437(19) 0.02879(16) 0.0835(12) Uani 1 1 d . . . H25 H 0.2353 0.1877 0.0172 0.100 Uiso 1 1 calc R . . C26 C 0.3061(3) 0.25949(15) 0.05075(13) 0.0636(8) Uani 1 1 d . . . H26 H 0.2320 0.2801 0.0546 0.076 Uiso 1 1 calc R . . C27 C 0.4343(2) 0.36143(12) 0.19610(9) 0.0406(5) Uani 1 1 d . . . C28 C 0.4336(3) 0.35662(14) 0.24322(9) 0.0483(6) Uani 1 1 d . . . H28 H 0.3675 0.3382 0.2580 0.058 Uiso 1 1 calc R . . C29 C 0.5288(3) 0.37851(15) 0.26836(9) 0.0532(7) Uani 1 1 d . . . H29 H 0.5284 0.3744 0.3002 0.064 Uiso 1 1 calc R . . C30 C 0.6242(3) 0.40629(14) 0.24721(10) 0.0520(7) Uani 1 1 d . . . H30 H 0.6889 0.4217 0.2646 0.062 Uiso 1 1 calc R . . C31 C 0.6259(3) 0.41182(14) 0.20027(9) 0.0472(6) Uani 1 1 d . . . H31 H 0.6918 0.4310 0.1859 0.057 Uiso 1 1 calc R . . C32 C 0.5315(2) 0.38931(12) 0.17437(8) 0.0397(5) Uani 1 1 d . . . C33 C 0.6228(3) 0.42660(14) 0.10535(9) 0.0480(6) Uani 1 1 d . . . H33A H 0.7011 0.4074 0.1117 0.058 Uiso 1 1 calc R . . H33B H 0.6247 0.4684 0.1169 0.058 Uiso 1 1 calc R . . C34 C 0.5986(2) 0.42652(12) 0.05580(9) 0.0424(6) Uani 1 1 d . . . C35 C 0.6734(3) 0.45267(14) 0.02350(10) 0.0526(7) Uani 1 1 d . . . H35 H 0.7455 0.4725 0.0321 0.063 Uiso 1 1 calc R . . C36 C 0.6402(3) 0.44906(14) -0.02132(10) 0.0550(8) Uani 1 1 d . . . H36 H 0.6895 0.4664 -0.0440 0.066 Uiso 1 1 calc R . . C37 C 0.5350(3) 0.42014(14) -0.03310(9) 0.0519(7) Uani 1 1 d . . . H37 H 0.5108 0.4178 -0.0638 0.062 Uiso 1 1 calc R . . C38 C 0.4656(3) 0.39466(13) 0.00042(9) 0.0455(6) Uani 1 1 d . . . H38 H 0.3940 0.3740 -0.0075 0.055 Uiso 1 1 calc R . . C39 C 0.1979(2) 0.42274(12) 0.05735(9) 0.0423(6) Uani 1 1 d . . . N2 N 0.8429(2) 0.12857(11) 0.20614(8) 0.0469(5) Uani 1 1 d . . . N1 N 1.0123(2) 0.19317(10) 0.22923(8) 0.0446(5) Uani 1 1 d . . . N3 N 0.9728(3) 0.23897(13) 0.15074(10) 0.0667(8) Uani 1 1 d . . . N22 N 0.52642(19) 0.39288(10) 0.12697(7) 0.0400(5) Uani 1 1 d . . . N21 N 0.4975(2) 0.39853(10) 0.04430(7) 0.0397(5) Uani 1 1 d . . . N23 N 0.2794(2) 0.39908(11) 0.07493(8) 0.0451(5) Uani 1 1 d . . . S1 S 0.82433(7) 0.14974(5) 0.11202(3) 0.0648(2) Uani 1 1 d . . . S2 S 0.94388(14) 0.34502(5) 0.10383(4) 0.0925(4) Uani 1 1 d . . . S21 S 0.31831(6) 0.33514(4) 0.16104(2) 0.04777(18) Uani 1 1 d . . . S22 S 0.08854(7) 0.45610(4) 0.03332(3) 0.0610(2) Uani 1 1 d . . . Si1 Si 0.94644(7) 0.16484(3) 0.17095(2) 0.04147(18) Uani 1 1 d . . . Si21 Si 0.40819(6) 0.36101(3) 0.09613(2) 0.03613(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0362(12) 0.0556(15) 0.0368(12) -0.0043(11) 0.0006(10) 0.0007(11) C2 0.0448(15) 0.088(2) 0.0409(14) -0.0061(14) 0.0052(12) -0.0101(16) C3 0.0357(15) 0.148(4) 0.0447(16) -0.028(2) 0.0039(12) -0.006(2) C4 0.056(2) 0.092(3) 0.065(2) -0.038(2) -0.0166(16) 0.023(2) C5 0.062(2) 0.060(2) 0.087(3) -0.0177(18) -0.0196(19) 0.0119(17) C6 0.0486(16) 0.0522(17) 0.070(2) -0.0063(15) 0.0004(14) 0.0065(14) C7 0.0388(15) 0.066(2) 0.093(3) -0.0238(18) -0.0069(15) 0.0131(14) C8 0.0415(18) 0.077(3) 0.158(5) -0.047(3) -0.017(2) 0.0104(19) C9 0.052(2) 0.070(3) 0.251(9) -0.048(4) -0.026(4) 0.013(2) C10 0.039(2) 0.053(2) 0.260(8) 0.018(4) 0.019(3) 0.0016(17) C11 0.0418(17) 0.0505(19) 0.160(4) 0.019(2) 0.018(2) 0.0085(15) C12 0.0325(13) 0.0434(15) 0.096(2) 0.0007(15) 0.0096(14) 0.0062(12) C13 0.0514(16) 0.0636(18) 0.0506(16) 0.0188(14) 0.0178(13) 0.0138(14) C14 0.0553(16) 0.0521(16) 0.0417(14) 0.0056(12) 0.0065(12) 0.0212(14) C15 0.079(2) 0.085(3) 0.0466(17) -0.0014(17) -0.0017(16) 0.035(2) C16 0.092(3) 0.072(2) 0.059(2) -0.0132(18) -0.021(2) 0.035(2) C17 0.078(2) 0.0428(16) 0.089(3) -0.0163(17) -0.029(2) 0.0140(16) C18 0.0605(18) 0.0381(14) 0.069(2) 0.0013(13) -0.0094(15) 0.0022(13) C19 0.078(2) 0.0564(18) 0.0476(16) 0.0063(14) -0.0065(15) -0.0001(16) C21 0.0508(15) 0.0421(13) 0.0405(13) 0.0047(11) 0.0042(11) -0.0011(12) C22 0.0585(18) 0.0555(17) 0.0575(17) -0.0019(14) 0.0076(14) 0.0101(15) C23 0.087(3) 0.061(2) 0.076(2) -0.0012(18) 0.022(2) 0.017(2) C24 0.117(4) 0.053(2) 0.084(3) -0.0182(19) 0.016(3) -0.002(2) C25 0.095(3) 0.060(2) 0.095(3) -0.016(2) -0.007(2) -0.016(2) C26 0.0607(19) 0.0495(17) 0.081(2) -0.0087(16) -0.0028(17) -0.0098(15) C27 0.0402(13) 0.0456(14) 0.0361(12) 0.0033(10) 0.0026(10) 0.0108(11) C28 0.0510(15) 0.0577(16) 0.0362(13) 0.0069(11) 0.0056(11) 0.0139(13) C29 0.0627(18) 0.0613(18) 0.0357(13) 0.0014(12) 0.0001(12) 0.0219(15) C30 0.0543(16) 0.0597(17) 0.0422(14) -0.0055(13) -0.0117(12) 0.0138(14) C31 0.0439(14) 0.0551(16) 0.0426(14) -0.0009(12) -0.0034(11) 0.0037(12) C32 0.0389(13) 0.0451(14) 0.0349(12) 0.0011(10) -0.0020(10) 0.0070(11) C33 0.0414(14) 0.0604(17) 0.0421(14) 0.0016(12) 0.0020(11) -0.0164(13) C34 0.0432(14) 0.0431(13) 0.0408(13) -0.0007(10) 0.0071(11) -0.0079(11) C35 0.0575(17) 0.0524(16) 0.0480(15) -0.0030(12) 0.0158(13) -0.0162(14) C36 0.074(2) 0.0480(15) 0.0426(14) -0.0017(12) 0.0220(14) -0.0095(15) C37 0.072(2) 0.0480(15) 0.0361(13) -0.0021(11) 0.0074(13) -0.0037(14) C38 0.0555(16) 0.0476(15) 0.0333(12) 0.0001(10) 0.0013(11) -0.0053(12) C39 0.0428(14) 0.0418(13) 0.0422(13) 0.0012(10) -0.0003(11) -0.0052(11) N2 0.0402(12) 0.0481(13) 0.0523(13) 0.0065(10) 0.0071(10) 0.0050(10) N1 0.0499(13) 0.0372(11) 0.0468(12) 0.0026(9) 0.0015(10) 0.0092(10) N3 0.086(2) 0.0547(16) 0.0592(16) 0.0177(13) -0.0061(15) 0.0017(15) N22 0.0366(11) 0.0482(12) 0.0351(10) 0.0025(9) 0.0034(8) -0.0063(9) N21 0.0434(11) 0.0411(11) 0.0347(10) 0.0017(8) 0.0028(9) -0.0045(9) N23 0.0426(12) 0.0490(13) 0.0437(11) 0.0047(10) -0.0018(10) 0.0013(10) S1 0.0464(4) 0.0979(7) 0.0500(4) -0.0084(4) -0.0040(3) 0.0105(4) S2 0.1282(10) 0.0659(6) 0.0833(7) 0.0332(5) -0.0221(7) -0.0022(6) S21 0.0396(3) 0.0634(4) 0.0403(3) 0.0051(3) 0.0059(3) -0.0072(3) S22 0.0465(4) 0.0638(5) 0.0728(5) 0.0230(4) -0.0166(4) -0.0025(4) Si1 0.0403(4) 0.0449(4) 0.0392(4) 0.0050(3) 0.0040(3) 0.0042(3) Si21 0.0340(3) 0.0403(4) 0.0341(3) 0.0018(3) 0.0006(2) -0.0015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.395(4) . ? C1 C6 1.405(4) . ? C1 Si1 1.865(3) . ? C2 C3 1.424(5) . ? C3 C4 1.396(6) . ? C4 C5 1.315(6) . ? C5 C6 1.391(5) . ? C7 C8 1.393(5) . ? C7 C12 1.427(5) . ? C7 S1 1.751(4) . ? C8 C9 1.367(9) . ? C9 C10 1.409(10) . ? C10 C11 1.411(8) . ? C11 C12 1.388(5) . ? C12 N2 1.405(4) . ? C13 N2 1.453(4) . ? C13 C14 1.486(5) . ? C14 N1 1.339(4) . ? C14 C15 1.392(5) . ? C15 C16 1.358(6) . ? C16 C17 1.366(6) . ? C17 C18 1.393(5) . ? C18 N1 1.356(4) . ? C19 N3 1.180(4) . ? C19 S2 1.573(3) . ? C21 C22 1.396(4) . ? C21 C26 1.404(4) . ? C21 Si21 1.879(3) . ? C22 C23 1.395(5) . ? C23 C24 1.383(7) . ? C24 C25 1.392(7) . ? C25 C26 1.386(5) . ? C27 C28 1.402(4) . ? C27 C32 1.404(4) . ? C27 S21 1.759(3) . ? C28 C29 1.385(5) . ? C29 C30 1.380(5) . ? C30 C31 1.398(4) . ? C31 C32 1.395(4) . ? C32 N22 1.409(3) . ? C33 N22 1.458(3) . ? C33 C34 1.494(4) . ? C34 N21 1.332(3) . ? C34 C35 1.396(4) . ? C35 C36 1.382(4) . ? C36 C37 1.382(5) . ? C37 C38 1.381(4) . ? C38 N21 1.352(3) . ? C39 N23 1.172(4) . ? C39 S22 1.595(3) . ? N2 Si1 1.752(2) . ? N1 Si1 1.981(3) . ? N3 Si1 1.776(3) . ? N22 Si21 1.753(2) . ? N21 Si21 2.012(2) . ? N23 Si21 1.780(2) . ? S1 Si1 2.2404(11) . ? S21 Si21 2.2448(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 116.9(3) . . ? C2 C1 Si1 125.4(3) . . ? C6 C1 Si1 117.7(2) . . ? C1 C2 C3 119.6(4) . . ? C4 C3 C2 119.8(3) . . ? C5 C4 C3 120.9(3) . . ? C4 C5 C6 120.3(4) . . ? C5 C6 C1 122.4(3) . . ? C8 C7 C12 120.2(4) . . ? C8 C7 S1 123.7(4) . . ? C12 C7 S1 116.1(2) . . ? C9 C8 C7 119.7(6) . . ? C8 C9 C10 121.1(5) . . ? C9 C10 C11 120.2(5) . . ? C12 C11 C10 118.7(6) . . ? C11 C12 N2 123.5(4) . . ? C11 C12 C7 120.2(4) . . ? N2 C12 C7 116.3(3) . . ? N2 C13 C14 107.7(2) . . ? N1 C14 C15 121.3(3) . . ? N1 C14 C13 113.4(3) . . ? C15 C14 C13 125.3(3) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C17 119.0(3) . . ? C16 C17 C18 120.3(4) . . ? N1 C18 C17 120.1(3) . . ? N3 C19 S2 177.5(4) . . ? C22 C21 C26 118.2(3) . . ? C22 C21 Si21 121.2(2) . . ? C26 C21 Si21 120.6(2) . . ? C23 C22 C21 120.7(3) . . ? C24 C23 C22 120.0(4) . . ? C23 C24 C25 120.4(4) . . ? C26 C25 C24 119.4(4) . . ? C25 C26 C21 121.4(4) . . ? C28 C27 C32 119.7(3) . . ? C28 C27 S21 124.1(2) . . ? C32 C27 S21 116.22(19) . . ? C29 C28 C27 120.4(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C31 120.2(3) . . ? C32 C31 C30 120.4(3) . . ? C31 C32 C27 119.1(2) . . ? C31 C32 N22 124.0(2) . . ? C27 C32 N22 116.8(2) . . ? N22 C33 C34 107.4(2) . . ? N21 C34 C35 121.6(3) . . ? N21 C34 C33 113.9(2) . . ? C35 C34 C33 124.6(3) . . ? C36 C35 C34 118.4(3) . . ? C37 C36 C35 119.9(3) . . ? C38 C37 C36 118.9(3) . . ? N21 C38 C37 121.3(3) . . ? N23 C39 S22 178.9(3) . . ? C12 N2 C13 118.3(3) . . ? C12 N2 Si1 119.9(2) . . ? C13 N2 Si1 120.7(2) . . ? C14 N1 C18 119.4(3) . . ? C14 N1 Si1 114.7(2) . . ? C18 N1 Si1 125.9(2) . . ? C19 N3 Si1 159.3(3) . . ? C32 N22 C33 116.0(2) . . ? C32 N22 Si21 121.87(17) . . ? C33 N22 Si21 122.10(18) . . ? C34 N21 C38 119.9(2) . . ? C34 N21 Si21 114.60(17) . . ? C38 N21 Si21 125.39(19) . . ? C39 N23 Si21 174.2(2) . . ? C7 S1 Si1 94.00(13) . . ? C27 S21 Si21 95.40(9) . . ? N2 Si1 N3 137.39(14) . . ? N2 Si1 C1 113.11(12) . . ? N3 Si1 C1 108.75(15) . . ? N2 Si1 N1 82.54(11) . . ? N3 Si1 N1 86.50(12) . . ? C1 Si1 N1 94.76(11) . . ? N2 Si1 S1 89.76(9) . . ? N3 Si1 S1 88.62(11) . . ? C1 Si1 S1 102.74(9) . . ? N1 Si1 S1 162.48(8) . . ? N22 Si21 N23 126.79(12) . . ? N22 Si21 C21 125.41(12) . . ? N23 Si21 C21 106.31(12) . . ? N22 Si21 N21 81.93(10) . . ? N23 Si21 N21 86.14(10) . . ? C21 Si21 N21 90.75(11) . . ? N22 Si21 S21 89.50(8) . . ? N23 Si21 S21 93.70(8) . . ? C21 Si21 S21 99.73(9) . . ? N21 Si21 S21 169.10(7) . . ? 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 C6 C1 C2 C3 0.1(4) . . . . ? Si1 C1 C2 C3 -179.2(2) . . . . ? C1 C2 C3 C4 -0.4(5) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 C6 0.0(5) . . . . ? C4 C5 C6 C1 -0.4(5) . . . . ? C2 C1 C6 C5 0.3(5) . . . . ? Si1 C1 C6 C5 179.7(3) . . . . ? C12 C7 C8 C9 0.2(5) . . . . ? S1 C7 C8 C9 -177.9(3) . . . . ? C7 C8 C9 C10 1.4(7) . . . . ? C8 C9 C10 C11 -1.6(7) . . . . ? C9 C10 C11 C12 0.0(6) . . . . ? C10 C11 C12 N2 -178.3(3) . . . . ? C10 C11 C12 C7 1.6(5) . . . . ? C8 C7 C12 C11 -1.7(5) . . . . ? S1 C7 C12 C11 176.6(2) . . . . ? C8 C7 C12 N2 178.2(3) . . . . ? S1 C7 C12 N2 -3.6(4) . . . . ? N2 C13 C14 N1 -5.9(3) . . . . ? N2 C13 C14 C15 175.7(3) . . . . ? N1 C14 C15 C16 -0.9(5) . . . . ? C13 C14 C15 C16 177.4(3) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 C18 1.6(5) . . . . ? C16 C17 C18 N1 -1.4(5) . . . . ? C26 C21 C22 C23 -1.5(5) . . . . ? Si21 C21 C22 C23 179.8(3) . . . . ? C21 C22 C23 C24 1.7(6) . . . . ? C22 C23 C24 C25 -0.4(7) . . . . ? C23 C24 C25 C26 -1.0(7) . . . . ? C24 C25 C26 C21 1.1(6) . . . . ? C22 C21 C26 C25 0.1(5) . . . . ? Si21 C21 C26 C25 178.8(3) . . . . ? C32 C27 C28 C29 -0.8(4) . . . . ? S21 C27 C28 C29 180.0(2) . . . . ? C27 C28 C29 C30 1.2(4) . . . . ? C28 C29 C30 C31 -0.8(4) . . . . ? C29 C30 C31 C32 -0.1(4) . . . . ? C30 C31 C32 C27 0.5(4) . . . . ? C30 C31 C32 N22 -179.8(3) . . . . ? C28 C27 C32 C31 -0.1(4) . . . . ? S21 C27 C32 C31 179.3(2) . . . . ? C28 C27 C32 N22 -179.8(2) . . . . ? S21 C27 C32 N22 -0.5(3) . . . . ? N22 C33 C34 N21 1.9(4) . . . . ? N22 C33 C34 C35 -177.8(3) . . . . ? N21 C34 C35 C36 0.1(5) . . . . ? C33 C34 C35 C36 179.8(3) . . . . ? C34 C35 C36 C37 0.1(5) . . . . ? C35 C36 C37 C38 -0.8(5) . . . . ? C36 C37 C38 N21 1.3(5) . . . . ? C11 C12 N2 C13 -1.7(4) . . . . ? C7 C12 N2 C13 178.5(3) . . . . ? C11 C12 N2 Si1 166.3(2) . . . . ? C7 C12 N2 Si1 -13.5(3) . . . . ? C14 C13 N2 C12 179.0(2) . . . . ? C14 C13 N2 Si1 11.1(3) . . . . ? C15 C14 N1 C18 1.1(4) . . . . ? C13 C14 N1 C18 -177.4(2) . . . . ? C15 C14 N1 Si1 178.0(2) . . . . ? C13 C14 N1 Si1 -0.5(3) . . . . ? C17 C18 N1 C14 0.0(4) . . . . ? C17 C18 N1 Si1 -176.5(2) . . . . ? S2 C19 N3 Si1 -162(7) . . . . ? C31 C32 N22 C33 -4.9(4) . . . . ? C27 C32 N22 C33 174.8(2) . . . . ? C31 C32 N22 Si21 177.4(2) . . . . ? C27 C32 N22 Si21 -2.9(3) . . . . ? C34 C33 N22 C32 -178.3(2) . . . . ? C34 C33 N22 Si21 -0.6(3) . . . . ? C35 C34 N21 C38 0.4(4) . . . . ? C33 C34 N21 C38 -179.3(3) . . . . ? C35 C34 N21 Si21 177.3(2) . . . . ? C33 C34 N21 Si21 -2.4(3) . . . . ? C37 C38 N21 C34 -1.1(4) . . . . ? C37 C38 N21 Si21 -177.6(2) . . . . ? S22 C39 N23 Si21 -87(15) . . . . ? C8 C7 S1 Si1 -168.3(3) . . . . ? C12 C7 S1 Si1 13.5(2) . . . . ? C28 C27 S21 Si21 -178.2(2) . . . . ? C32 C27 S21 Si21 2.5(2) . . . . ? C12 N2 Si1 N3 106.4(3) . . . . ? C13 N2 Si1 N3 -85.9(3) . . . . ? C12 N2 Si1 C1 -85.1(2) . . . . ? C13 N2 Si1 C1 82.6(2) . . . . ? C12 N2 Si1 N1 -177.1(2) . . . . ? C13 N2 Si1 N1 -9.4(2) . . . . ? C12 N2 Si1 S1 18.7(2) . . . . ? C13 N2 Si1 S1 -173.6(2) . . . . ? C19 N3 Si1 N2 -68.4(9) . . . . ? C19 N3 Si1 C1 122.7(9) . . . . ? C19 N3 Si1 N1 -143.4(9) . . . . ? C19 N3 Si1 S1 19.7(9) . . . . ? C2 C1 Si1 N2 -171.7(2) . . . . ? C6 C1 Si1 N2 9.0(3) . . . . ? C2 C1 Si1 N3 0.1(3) . . . . ? C6 C1 Si1 N3 -179.2(2) . . . . ? C2 C1 Si1 N1 -87.8(3) . . . . ? C6 C1 Si1 N1 92.9(2) . . . . ? C2 C1 Si1 S1 93.0(2) . . . . ? C6 C1 Si1 S1 -86.3(2) . . . . ? C14 N1 Si1 N2 5.3(2) . . . . ? C18 N1 Si1 N2 -178.0(2) . . . . ? C14 N1 Si1 N3 144.0(2) . . . . ? C18 N1 Si1 N3 -39.3(3) . . . . ? C14 N1 Si1 C1 -107.4(2) . . . . ? C18 N1 Si1 C1 69.3(2) . . . . ? C14 N1 Si1 S1 69.9(4) . . . . ? C18 N1 Si1 S1 -113.4(3) . . . . ? C7 S1 Si1 N2 -16.01(13) . . . . ? C7 S1 Si1 N3 -153.43(16) . . . . ? C7 S1 Si1 C1 97.66(14) . . . . ? C7 S1 Si1 N1 -79.6(3) . . . . ? C32 N22 Si21 N23 98.1(2) . . . . ? C33 N22 Si21 N23 -79.5(3) . . . . ? C32 N22 Si21 C21 -97.8(2) . . . . ? C33 N22 Si21 C21 84.6(3) . . . . ? C32 N22 Si21 N21 177.1(2) . . . . ? C33 N22 Si21 N21 -0.5(2) . . . . ? C32 N22 Si21 S21 3.8(2) . . . . ? C33 N22 Si21 S21 -173.8(2) . . . . ? C39 N23 Si21 N22 118(2) . . . . ? C39 N23 Si21 C21 -48(2) . . . . ? C39 N23 Si21 N21 42(2) . . . . ? C39 N23 Si21 S21 -149(2) . . . . ? C22 C21 Si21 N22 -13.1(3) . . . . ? C26 C21 Si21 N22 168.3(2) . . . . ? C22 C21 Si21 N23 153.8(2) . . . . ? C26 C21 Si21 N23 -24.8(3) . . . . ? C22 C21 Si21 N21 67.6(2) . . . . ? C26 C21 Si21 N21 -111.0(3) . . . . ? C22 C21 Si21 S21 -109.4(2) . . . . ? C26 C21 Si21 S21 72.0(3) . . . . ? C34 N21 Si21 N22 1.7(2) . . . . ? C38 N21 Si21 N22 178.4(2) . . . . ? C34 N21 Si21 N23 129.7(2) . . . . ? C38 N21 Si21 N23 -53.6(2) . . . . ? C34 N21 Si21 C21 -124.0(2) . . . . ? C38 N21 Si21 C21 52.7(2) . . . . ? C34 N21 Si21 S21 40.2(5) . . . . ? C38 N21 Si21 S21 -143.1(3) . . . . ? C27 S21 Si21 N22 -3.11(12) . . . . ? C27 S21 Si21 N23 -129.95(12) . . . . ? C27 S21 Si21 C21 122.79(13) . . . . ? C27 S21 Si21 N21 -41.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.343 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.064 ##***************************** compound 5 x 0.5 C7H8 ********** data_kob02i_5 _database_code_depnum_ccdc_archive 'CCDC 832636' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C18 H15 N5 S Si), C7 H8' _chemical_formula_sum 'C21.50 H19 N5 S Si' _chemical_formula_weight 407.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 12.0354(17) _cell_length_b 13.1538(18) _cell_length_c 12.9714(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.259(17) _cell_angle_gamma 90.00 _cell_volume 2044.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 6.65 _cell_measurement_theta_max 24.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.235 _exptl_absorpt_correction_type multi_scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8216 _exptl_absorpt_correction_T_max 0.8626 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega-scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23950 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 29.15 _reflns_number_total 5456 _reflns_number_gt 3763 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDs _computing_cell_refinement Stoe-IPDs _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob02b in P2(1)/n CELL 0.71073 12.0354 13.1538 12.9714 90.000 95.259 90.000 ZERR 4.0 0.0017 0.0018 0.0018 0.000 0.017 0.000 REM CELL 0.71073 12.0532 13.1145 12.9905 90.000 94.857 90.000 REm ZERR 2.0 0.0023 0.0031 0.0029 0.000 0.025 0.000 REM CELL 0.71073 12.0571 13.1133 12.9868 90.000 94.793 90.000 REM ZERR 4.00 0.0024 0.0026 0.0026 0.000 0.030 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N Si S UNIT 86 76 20 4 4 L.S. 20 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.069800 0.461200 FVAR 0.88189 C1 1 0.403109 0.919574 0.680686 11.00000 0.03290 0.03217 = 0.03268 0.00387 0.00088 -0.00371 C2 1 0.426089 0.971239 0.773849 11.00000 0.06519 0.03642 = 0.03960 -0.00092 -0.00946 -0.00403 AFIX 43 H2 2 0.381894 1.028224 0.788991 11.00000 -1.20000 AFIX 0 C3 1 0.513370 0.940265 0.845317 11.00000 0.09129 0.05269 = 0.05008 0.00182 -0.03000 -0.00904 AFIX 43 H3 2 0.527347 0.975537 0.909097 11.00000 -1.20000 AFIX 0 C4 1 0.579487 0.858512 0.823632 11.00000 0.06204 0.05495 = 0.07840 0.01947 -0.03267 -0.00625 AFIX 43 H4 2 0.638214 0.837266 0.872848 11.00000 -1.20000 AFIX 0 C5 1 0.560533 0.808074 0.731371 11.00000 0.04013 0.05643 = 0.06938 0.01750 -0.00472 0.00620 AFIX 43 H5 2 0.607194 0.753023 0.715621 11.00000 -1.20000 AFIX 0 C6 1 0.473107 0.837719 0.661274 11.00000 0.03538 0.04697 = 0.04404 0.00722 0.00341 0.00588 AFIX 43 H6 2 0.459961 0.801553 0.597937 11.00000 -1.20000 AFIX 0 C7 1 0.411192 1.143239 0.590264 11.00000 0.03971 0.04157 = 0.04133 0.00401 0.00456 -0.00676 AFIX 43 H7 2 0.470981 1.103481 0.569141 11.00000 -1.20000 AFIX 0 C8 1 0.427336 1.245288 0.610413 11.00000 0.05643 0.04672 = 0.04551 0.00444 0.00247 -0.01653 AFIX 43 H8 2 0.497972 1.275688 0.604003 11.00000 -1.20000 AFIX 0 C9 1 0.339210 1.303278 0.640208 11.00000 0.07406 0.03580 = 0.04318 -0.00265 0.00135 -0.00868 AFIX 43 H9 2 0.349242 1.373623 0.654823 11.00000 -1.20000 AFIX 0 C10 1 0.237139 1.257950 0.648393 11.00000 0.06170 0.03634 = 0.04168 -0.00603 0.00806 0.00447 AFIX 43 H10 2 0.175682 1.296725 0.667526 11.00000 -1.20000 AFIX 0 C11 1 0.225686 1.154544 0.628171 11.00000 0.04143 0.03422 = 0.02759 -0.00142 0.00388 0.00438 C12 1 0.121641 1.094073 0.635372 11.00000 0.03684 0.03763 = 0.03966 -0.00272 0.00855 0.00663 AFIX 23 H12A 2 0.094894 1.102146 0.704841 11.00000 -1.20000 H12B 2 0.062346 1.117905 0.583006 11.00000 -1.20000 AFIX 0 C13 1 0.059743 0.917381 0.619259 11.00000 0.02919 0.04448 = 0.03163 0.00419 -0.00063 -0.00293 C14 1 -0.047106 0.942707 0.645630 11.00000 0.03235 0.05827 = 0.04884 0.00739 0.00615 0.00022 AFIX 43 H14 2 -0.064122 1.011058 0.661859 11.00000 -1.20000 AFIX 0 C15 1 -0.128673 0.867290 0.648042 11.00000 0.03358 0.08107 = 0.05872 0.01604 0.00612 -0.00774 AFIX 43 H15 2 -0.200695 0.884716 0.666886 11.00000 -1.20000 AFIX 0 C16 1 -0.105828 0.767589 0.623328 11.00000 0.04619 0.07165 = 0.05314 0.02069 -0.00329 -0.02289 AFIX 43 H16 2 -0.161923 0.716978 0.625168 11.00000 -1.20000 AFIX 0 C17 1 -0.000448 0.741699 0.595776 11.00000 0.04967 0.04981 = 0.04576 0.00999 -0.00828 -0.01535 AFIX 43 H17 2 0.015224 0.673398 0.578214 11.00000 -1.20000 AFIX 0 C18 1 0.082243 0.815778 0.593878 11.00000 0.03731 0.04210 = 0.03388 0.00295 -0.00547 -0.00616 N2 3 0.147740 0.987568 0.617005 11.00000 0.03042 0.03313 = 0.03508 -0.00215 0.00305 0.00117 N1 3 0.310961 1.098796 0.600209 11.00000 0.03453 0.03318 = 0.02952 0.00134 0.00348 0.00078 N3 3 0.333872 0.962409 0.459355 11.00000 0.03710 0.04694 = 0.03724 -0.00320 0.00644 0.00220 N4 3 0.299341 0.917856 0.384366 11.00000 0.03812 0.06458 = 0.04123 -0.00683 0.00567 0.00882 N5 3 0.270082 0.878278 0.307500 11.00000 0.07317 0.11410 = 0.04383 -0.03149 0.00096 -0.00011 S 5 0.217915 0.789539 0.562795 11.00000 0.04111 0.03561 = 0.06016 -0.01315 0.00165 -0.00213 SI 4 0.281024 0.951513 0.584708 11.00000 0.02797 0.03208 = 0.02953 -0.00321 0.00246 0.00184 PART -1 DELU C19 > C25 ISOR .005 C19 > C25 C19 1 0.682014 1.490028 0.563823 10.50000 0.10638 0.11917 = 0.11040 0.02047 -0.01455 -0.00405 AFIX 137 H19A 2 0.715537 1.557547 0.558889 10.50000 -1.20000 H19B 2 0.722164 1.441213 0.523863 10.50000 -1.20000 H19C 2 0.686804 1.468754 0.636501 10.50000 -1.20000 AFIX 66 C20 1 0.509734 1.555271 0.586646 10.50000 0.12149 0.06864 = 0.08530 -0.00456 0.02645 0.01385 AFIX 43 H20 2 0.547005 1.586375 0.646236 10.50000 -1.20000 AFIX 65 C21 1 0.396190 1.571294 0.562386 10.50000 0.10760 0.07376 = 0.11166 0.02488 0.01249 0.01217 AFIX 43 H21 2 0.355858 1.613348 0.605394 10.50000 -1.20000 AFIX 65 C22 1 0.341657 1.525784 0.475198 10.50000 0.09411 0.09126 = 0.10900 0.04178 0.00575 0.01046 AFIX 43 H22 2 0.264054 1.536735 0.458618 10.50000 -1.20000 AFIX 65 C23 1 0.400669 1.464252 0.412270 10.50000 0.11429 0.10545 = 0.07951 0.02290 -0.02253 -0.03238 AFIX 43 H23 2 0.363398 1.433148 0.352681 10.50000 -1.20000 AFIX 65 C24 1 0.514213 1.448229 0.436529 10.50000 0.09035 0.03849 = 0.05272 -0.00294 0.00672 -0.01050 AFIX 43 H24 2 0.554545 1.406174 0.393521 10.50000 -1.20000 AFIX 65 C25 1 0.568747 1.493737 0.523717 10.50000 0.06860 0.04347 = 0.05438 0.00390 -0.00272 0.00280 PART 0 HKLF 4 REM kob02b in P2(1)/n REM R1 = 0.0476 for 3763 Fo > 4sig(Fo) and 0.0711 for all 5456 data REM 278 parameters refined using 57 restraints END WGHT 0.0698 0.4613 REM Highest difference peak 0.556, deepest hole -0.356, 1-sigma level 0.052 Q1 1 0.3534 1.5516 0.5063 11.00000 0.05 0.56 Q2 1 0.3560 1.4831 0.4216 11.00000 0.05 0.47 Q3 1 0.5479 1.4357 0.4404 11.00000 0.05 0.44 Q4 1 0.5724 1.5843 0.6203 11.00000 0.05 0.36 Q5 1 0.3620 0.9401 0.6414 11.00000 0.05 0.34 Q6 1 0.3621 0.9816 0.7976 11.00000 0.05 0.30 Q7 1 0.4410 0.9478 0.8608 11.00000 0.05 0.28 Q8 1 0.2185 0.8801 0.5396 11.00000 0.05 0.25 Q9 1 0.2823 0.8548 0.5985 11.00000 0.05 0.24 Q10 1 0.2912 0.9812 0.4910 11.00000 0.05 0.23 Q11 1 0.1723 0.9509 0.5560 11.00000 0.05 0.22 Q12 1 0.1997 0.8782 0.5919 11.00000 0.05 0.22 Q13 1 0.5330 0.8914 0.8583 11.00000 0.05 0.22 Q14 1 0.3170 0.8928 0.6587 11.00000 0.05 0.22 Q15 1 0.0010 0.9284 0.6228 11.00000 0.05 0.21 Q16 1 0.2969 1.0479 0.5854 11.00000 0.05 0.20 Q17 1 0.3547 0.9975 0.4615 11.00000 0.05 0.20 Q18 1 0.5411 1.4970 0.5178 11.00000 0.05 0.19 Q19 1 0.2773 1.5013 0.4759 11.00000 0.05 0.19 Q20 1 0.1923 0.9814 0.6222 11.00000 0.05 0.18 ; _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^)+(0.0698P)^2^+0.4612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5456 _refine_ls_number_parameters 278 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0711 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.40311(14) 0.91957(14) 0.68069(14) 0.0327(4) Uani 1 1 d . . . C2 C 0.4261(2) 0.97124(17) 0.77385(17) 0.0479(5) Uani 1 1 d . . . H2 H 0.3819 1.0282 0.7890 0.058 Uiso 1 1 calc R . . C3 C 0.5134(3) 0.9403(2) 0.8453(2) 0.0669(8) Uani 1 1 d . . . H3 H 0.5273 0.9755 0.9091 0.080 Uiso 1 1 calc R . . C4 C 0.5795(2) 0.8585(2) 0.8236(2) 0.0675(8) Uani 1 1 d . . . H4 H 0.6382 0.8373 0.8728 0.081 Uiso 1 1 calc R . . C5 C 0.56053(18) 0.8081(2) 0.7314(2) 0.0559(6) Uani 1 1 d . . . H5 H 0.6072 0.7530 0.7156 0.067 Uiso 1 1 calc R . . C6 C 0.47311(16) 0.83772(17) 0.66127(16) 0.0421(5) Uani 1 1 d . . . H6 H 0.4600 0.8016 0.5979 0.051 Uiso 1 1 calc R . . C7 C 0.41119(16) 1.14324(16) 0.59026(16) 0.0408(4) Uani 1 1 d . . . H7 H 0.4710 1.1035 0.5691 0.049 Uiso 1 1 calc R . . C8 C 0.4273(2) 1.24529(18) 0.61041(17) 0.0497(5) Uani 1 1 d . . . H8 H 0.4980 1.2757 0.6040 0.060 Uiso 1 1 calc R . . C9 C 0.3392(2) 1.30328(17) 0.64021(17) 0.0513(5) Uani 1 1 d . . . H9 H 0.3492 1.3736 0.6548 0.062 Uiso 1 1 calc R . . C10 C 0.2371(2) 1.25795(16) 0.64839(17) 0.0464(5) Uani 1 1 d . . . H10 H 0.1757 1.2967 0.6675 0.056 Uiso 1 1 calc R . . C11 C 0.22569(15) 1.15454(15) 0.62817(13) 0.0344(4) Uani 1 1 d . . . C12 C 0.12164(15) 1.09407(15) 0.63537(15) 0.0377(4) Uani 1 1 d . . . H12A H 0.0949 1.1021 0.7048 0.045 Uiso 1 1 calc R . . H12B H 0.0623 1.1179 0.5830 0.045 Uiso 1 1 calc R . . C13 C 0.05974(14) 0.91738(16) 0.61926(14) 0.0353(4) Uani 1 1 d . . . C14 C -0.04711(16) 0.94271(19) 0.64563(17) 0.0463(5) Uani 1 1 d . . . H14 H -0.0641 1.0111 0.6619 0.056 Uiso 1 1 calc R . . C15 C -0.12867(18) 0.8673(2) 0.6480(2) 0.0577(6) Uani 1 1 d . . . H15 H -0.2007 0.8847 0.6669 0.069 Uiso 1 1 calc R . . C16 C -0.10583(19) 0.7676(2) 0.62333(19) 0.0575(6) Uani 1 1 d . . . H16 H -0.1619 0.7170 0.6252 0.069 Uiso 1 1 calc R . . C17 C -0.00045(19) 0.74170(19) 0.59578(17) 0.0492(5) Uani 1 1 d . . . H17 H 0.0152 0.6734 0.5782 0.059 Uiso 1 1 calc R . . C18 C 0.08224(16) 0.81578(16) 0.59388(15) 0.0383(4) Uani 1 1 d . . . N2 N 0.14774(12) 0.98757(12) 0.61701(12) 0.0329(3) Uani 1 1 d . . . N1 N 0.31096(12) 1.09880(12) 0.60021(11) 0.0324(3) Uani 1 1 d . . . N3 N 0.33387(13) 0.96241(14) 0.45936(13) 0.0402(4) Uani 1 1 d . . . N4 N 0.29934(14) 0.91786(16) 0.38437(14) 0.0478(4) Uani 1 1 d . . . N5 N 0.2701(2) 0.8783(2) 0.30750(17) 0.0773(8) Uani 1 1 d . . . S S 0.21792(4) 0.78954(4) 0.56280(5) 0.04581(16) Uani 1 1 d . . . Si Si 0.28102(4) 0.95151(4) 0.58471(4) 0.02987(13) Uani 1 1 d . . . C19 C 0.6820(8) 1.4900(9) 0.5638(9) 0.113(3) Uani 0.50 1 d PU A -1 H19A H 0.7155 1.5575 0.5589 0.136 Uiso 0.50 1 calc PR A -1 H19B H 0.7222 1.4412 0.5239 0.136 Uiso 0.50 1 calc PR A -1 H19C H 0.6868 1.4688 0.6365 0.136 Uiso 0.50 1 calc PR A -1 C20 C 0.5097(4) 1.5553(3) 0.5866(3) 0.091(2) Uani 0.50 1 d PGU A -1 H20 H 0.5470 1.5864 0.6462 0.109 Uiso 0.50 1 calc PR A -1 C21 C 0.3962(4) 1.5713(4) 0.5624(5) 0.098(2) Uani 0.50 1 d PGU A -1 H21 H 0.3559 1.6133 0.6054 0.117 Uiso 0.50 1 calc PR A -1 C22 C 0.3417(3) 1.5258(5) 0.4752(5) 0.098(2) Uani 0.50 1 d PGU A -1 H22 H 0.2641 1.5367 0.4586 0.118 Uiso 0.50 1 calc PR A -1 C23 C 0.4007(4) 1.4643(4) 0.4123(4) 0.102(2) Uani 0.50 1 d PGU A -1 H23 H 0.3634 1.4331 0.3527 0.122 Uiso 0.50 1 calc PR A -1 C24 C 0.5142(4) 1.4482(3) 0.4365(3) 0.0605(15) Uani 0.50 1 d PGU A -1 H24 H 0.5545 1.4062 0.3935 0.073 Uiso 0.50 1 calc PR A -1 C25 C 0.5687(3) 1.4937(3) 0.5237(3) 0.0560(11) Uani 0.50 1 d PGU A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0329(8) 0.0322(9) 0.0327(8) 0.0039(7) 0.0009(7) -0.0037(7) C2 0.0652(14) 0.0364(11) 0.0396(10) -0.0009(9) -0.0095(9) -0.0040(10) C3 0.091(2) 0.0527(15) 0.0501(14) 0.0018(12) -0.0300(13) -0.0090(14) C4 0.0620(14) 0.0550(15) 0.0784(18) 0.0195(14) -0.0327(13) -0.0062(12) C5 0.0401(10) 0.0564(14) 0.0694(16) 0.0175(12) -0.0047(10) 0.0062(10) C6 0.0354(9) 0.0470(12) 0.0440(11) 0.0072(9) 0.0034(8) 0.0059(8) C7 0.0397(9) 0.0416(11) 0.0413(10) 0.0040(8) 0.0046(8) -0.0068(8) C8 0.0564(12) 0.0467(12) 0.0455(11) 0.0044(10) 0.0025(9) -0.0165(10) C9 0.0741(15) 0.0358(11) 0.0432(11) -0.0026(9) 0.0014(10) -0.0087(10) C10 0.0617(13) 0.0363(11) 0.0417(11) -0.0060(9) 0.0081(9) 0.0045(9) C11 0.0414(9) 0.0342(9) 0.0276(8) -0.0014(7) 0.0039(7) 0.0044(7) C12 0.0368(9) 0.0376(10) 0.0397(10) -0.0027(8) 0.0085(7) 0.0066(8) C13 0.0292(8) 0.0445(11) 0.0316(9) 0.0042(8) -0.0006(7) -0.0029(7) C14 0.0324(9) 0.0583(14) 0.0488(11) 0.0074(10) 0.0061(8) 0.0002(9) C15 0.0336(10) 0.0811(19) 0.0587(14) 0.0160(13) 0.0061(9) -0.0077(11) C16 0.0462(12) 0.0716(17) 0.0531(13) 0.0207(12) -0.0033(10) -0.0229(11) C17 0.0497(11) 0.0498(13) 0.0458(11) 0.0100(10) -0.0083(9) -0.0153(10) C18 0.0373(9) 0.0421(11) 0.0339(9) 0.0029(8) -0.0055(7) -0.0062(8) N2 0.0304(7) 0.0331(8) 0.0351(8) -0.0021(6) 0.0031(6) 0.0012(6) N1 0.0345(7) 0.0332(8) 0.0295(7) 0.0013(6) 0.0035(6) 0.0008(6) N3 0.0371(8) 0.0469(10) 0.0372(8) -0.0032(7) 0.0064(7) 0.0022(7) N4 0.0381(8) 0.0646(12) 0.0412(9) -0.0068(9) 0.0057(7) 0.0088(8) N5 0.0732(14) 0.114(2) 0.0438(11) -0.0315(13) 0.0010(10) -0.0001(14) S 0.0411(3) 0.0356(3) 0.0602(3) -0.0131(2) 0.0017(2) -0.0021(2) Si 0.0280(2) 0.0321(3) 0.0295(2) -0.00321(19) 0.00246(17) 0.00184(18) C19 0.106(4) 0.119(5) 0.110(5) 0.020(4) -0.015(4) -0.004(4) C20 0.121(4) 0.069(4) 0.085(4) -0.005(3) 0.026(3) 0.014(4) C21 0.108(4) 0.074(3) 0.112(4) 0.025(3) 0.012(3) 0.012(3) C22 0.094(4) 0.091(4) 0.109(4) 0.042(3) 0.006(3) 0.010(3) C23 0.114(4) 0.105(4) 0.080(3) 0.023(3) -0.023(3) -0.032(4) C24 0.090(3) 0.038(3) 0.053(3) -0.003(2) 0.007(3) -0.011(2) C25 0.069(3) 0.043(2) 0.054(2) 0.004(2) -0.003(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(3) . ? C1 C6 1.404(3) . ? C1 Si 1.8842(19) . ? C2 C3 1.397(3) . ? C3 C4 1.382(4) . ? C4 C5 1.369(4) . ? C5 C6 1.382(3) . ? C7 N1 1.357(2) . ? C7 C8 1.378(3) . ? C8 C9 1.390(3) . ? C9 C10 1.378(3) . ? C10 C11 1.390(3) . ? C11 N1 1.338(2) . ? C11 C12 1.494(3) . ? C12 N2 1.460(2) . ? C13 C14 1.401(3) . ? C13 N2 1.407(2) . ? C13 C18 1.409(3) . ? C14 C15 1.398(3) . ? C15 C16 1.384(4) . ? C16 C17 1.391(3) . ? C17 C18 1.395(3) . ? C18 S 1.752(2) . ? N2 Si 1.7598(15) . ? N1 Si 1.9774(17) . ? N3 N4 1.178(2) . ? N3 Si 1.8051(17) . ? N4 N5 1.151(3) . ? S Si 2.2710(8) . ? C19 C25 1.415(10) . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 117.09(19) . . ? C2 C1 Si 123.07(15) . . ? C6 C1 Si 119.79(15) . . ? C1 C2 C3 120.8(2) . . ? C4 C3 C2 120.3(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 119.6(2) . . ? C5 C6 C1 122.1(2) . . ? N1 C7 C8 120.8(2) . . ? C7 C8 C9 119.3(2) . . ? C10 C9 C8 119.5(2) . . ? C9 C10 C11 118.9(2) . . ? N1 C11 C10 121.48(18) . . ? N1 C11 C12 113.16(16) . . ? C10 C11 C12 125.36(17) . . ? N2 C12 C11 107.86(14) . . ? C14 C13 N2 123.95(19) . . ? C14 C13 C18 118.89(18) . . ? N2 C13 C18 117.16(16) . . ? C15 C14 C13 119.9(2) . . ? C16 C15 C14 120.8(2) . . ? C15 C16 C17 119.8(2) . . ? C16 C17 C18 120.2(2) . . ? C17 C18 C13 120.40(19) . . ? C17 C18 S 123.24(18) . . ? C13 C18 S 116.36(14) . . ? C13 N2 C12 116.90(15) . . ? C13 N2 Si 122.16(13) . . ? C12 N2 Si 120.79(12) . . ? C11 N1 C7 120.01(17) . . ? C11 N1 Si 115.30(12) . . ? C7 N1 Si 124.58(13) . . ? N4 N3 Si 125.27(15) . . ? N5 N4 N3 175.5(3) . . ? C18 S Si 95.42(7) . . ? N2 Si N3 126.67(8) . . ? N2 Si C1 125.13(8) . . ? N3 Si C1 107.16(8) . . ? N2 Si N1 82.72(7) . . ? N3 Si N1 86.44(7) . . ? C1 Si N1 91.57(7) . . ? N2 Si S 88.91(6) . . ? N3 Si S 95.92(6) . . ? C1 Si S 96.03(6) . . ? N1 Si S 170.97(5) . . ? C21 C20 C25 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C20 120.0 . . ? C24 C25 C19 130.7(6) . . ? C20 C25 C19 109.3(6) . . ? 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 C6 C1 C2 C3 -1.7(3) . . . . ? Si C1 C2 C3 175.79(19) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C3 C4 C5 C6 -1.7(4) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C2 C1 C6 C5 0.7(3) . . . . ? Si C1 C6 C5 -176.85(17) . . . . ? N1 C7 C8 C9 -0.7(3) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C9 C10 C11 N1 -0.6(3) . . . . ? C9 C10 C11 C12 178.89(19) . . . . ? N1 C11 C12 N2 4.5(2) . . . . ? C10 C11 C12 N2 -175.05(18) . . . . ? N2 C13 C14 C15 -178.54(19) . . . . ? C18 C13 C14 C15 1.0(3) . . . . ? C13 C14 C15 C16 -0.8(3) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C13 -0.3(3) . . . . ? C16 C17 C18 S 178.62(17) . . . . ? C14 C13 C18 C17 -0.5(3) . . . . ? N2 C13 C18 C17 179.15(17) . . . . ? C14 C13 C18 S -179.47(15) . . . . ? N2 C13 C18 S 0.1(2) . . . . ? C14 C13 N2 C12 -5.1(3) . . . . ? C18 C13 N2 C12 175.32(16) . . . . ? C14 C13 N2 Si 179.27(15) . . . . ? C18 C13 N2 Si -0.3(2) . . . . ? C11 C12 N2 C13 -179.29(15) . . . . ? C11 C12 N2 Si -3.6(2) . . . . ? C10 C11 N1 C7 -0.5(3) . . . . ? C12 C11 N1 C7 179.93(16) . . . . ? C10 C11 N1 Si 175.79(15) . . . . ? C12 C11 N1 Si -3.77(19) . . . . ? C8 C7 N1 C11 1.2(3) . . . . ? C8 C7 N1 Si -174.77(16) . . . . ? Si N3 N4 N5 172(3) . . . . ? C17 C18 S Si -178.94(17) . . . . ? C13 C18 S Si 0.05(15) . . . . ? C13 N2 Si N3 96.84(16) . . . . ? C12 N2 Si N3 -78.61(16) . . . . ? C13 N2 Si C1 -96.34(16) . . . . ? C12 N2 Si C1 88.20(16) . . . . ? C13 N2 Si N1 176.87(15) . . . . ? C12 N2 Si N1 1.41(14) . . . . ? C13 N2 Si S 0.27(14) . . . . ? C12 N2 Si S -175.18(14) . . . . ? N4 N3 Si N2 -65.2(2) . . . . ? N4 N3 Si C1 126.03(18) . . . . ? N4 N3 Si N1 -143.42(19) . . . . ? N4 N3 Si S 27.83(19) . . . . ? C2 C1 Si N2 -38.1(2) . . . . ? C6 C1 Si N2 139.35(15) . . . . ? C2 C1 Si N3 130.87(17) . . . . ? C6 C1 Si N3 -51.69(17) . . . . ? C2 C1 Si N1 44.11(17) . . . . ? C6 C1 Si N1 -138.45(15) . . . . ? C2 C1 Si S -131.02(16) . . . . ? C6 C1 Si S 46.43(15) . . . . ? C11 N1 Si N2 1.46(13) . . . . ? C7 N1 Si N2 177.57(16) . . . . ? C11 N1 Si N3 129.13(14) . . . . ? C7 N1 Si N3 -54.76(16) . . . . ? C11 N1 Si C1 -123.77(14) . . . . ? C7 N1 Si C1 52.34(16) . . . . ? C11 N1 Si S 23.7(4) . . . . ? C7 N1 Si S -160.2(3) . . . . ? C18 S Si N2 -0.15(8) . . . . ? C18 S Si N3 -126.92(9) . . . . ? C18 S Si C1 125.07(9) . . . . ? C18 S Si N1 -22.2(3) . . . . ? C25 C20 C21 C22 0.0 . . . . ? C20 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C20 0.0 . . . . ? C23 C24 C25 C19 -179.4(9) . . . . ? C21 C20 C25 C24 0.0 . . . . ? C21 C20 C25 C19 179.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.556 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.052 ##***************************** compound 6 x 0.5 C7H8 ******* data_kob12cu_6 _database_code_depnum_ccdc_archive 'CCDC 832637' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H15 F3 N2 O3 S2 Si), C7 H8' _chemical_formula_sum 'C22.50 H19 F3 N2 O3 S2 Si' _chemical_formula_weight 514.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.972(2) _cell_length_b 11.273(2) _cell_length_c 11.806(2) _cell_angle_alpha 65.48(3) _cell_angle_beta 73.49(3) _cell_angle_gamma 74.68(3) _cell_volume 1141.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 6.85 _cell_measurement_theta_max 27.4 _exptl_crystal_description long_prism _exptl_crystal_colour colorless _exptl_crystal_size_max .48 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 0.339 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Stoe_image_plate _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16511 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 29.15 _reflns_number_total 5598 _reflns_number_gt 4307 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics OrteP/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob12b in P-1 CELL 0.71073 9.9717 11.2734 11.8063 65.476 73.489 74.681 ZERR 2.00 0.0020 0.0023 0.0024 0.030 0.030 0.030 LATT 1 SFAC C H O F N Si S UNIT 45 38 6 6 4 2 4 L.S. 12 TEMP -100 ACTA CONF HTAB 2.5 BOND FMAP 2 PLAN 20 WGHT 0.062800 0.255400 FVAR 0.36218 MOLE 1 C1 1 0.879102 0.045623 0.233877 11.00000 0.03413 0.02554 = 0.03215 -0.01022 -0.00778 -0.00800 C2 1 0.992295 -0.041070 0.193547 11.00000 0.04052 0.03371 = 0.05781 -0.02346 -0.00313 -0.00816 AFIX 43 H2 2 1.071878 -0.007436 0.132192 11.00000 -1.20000 AFIX 0 C3 1 0.989552 -0.176542 0.242521 11.00000 0.06225 0.03311 = 0.07401 -0.02979 -0.01437 -0.00340 AFIX 43 H3 2 1.066802 -0.234439 0.213961 11.00000 -1.20000 AFIX 0 C4 1 0.875828 -0.226253 0.331627 11.00000 0.08646 0.02772 = 0.05648 -0.01328 -0.01820 -0.01707 AFIX 43 H4 2 0.875001 -0.318674 0.365286 11.00000 -1.20000 AFIX 0 C5 1 0.762242 -0.142735 0.372872 11.00000 0.07386 0.03810 = 0.04015 -0.00875 -0.00127 -0.02903 AFIX 43 H5 2 0.683473 -0.177534 0.434653 11.00000 -1.20000 AFIX 0 C6 1 0.763831 -0.007341 0.323427 11.00000 0.04822 0.03214 = 0.03410 -0.01113 -0.00262 -0.01452 AFIX 43 H6 2 0.685038 0.049906 0.351182 11.00000 -1.20000 AFIX 0 C7 1 1.105168 0.120357 0.319217 11.00000 0.03515 0.03144 = 0.03091 -0.00558 -0.00775 -0.00907 AFIX 43 H7 2 1.034500 0.080997 0.388857 11.00000 -1.20000 AFIX 0 C8 1 1.242586 0.097422 0.335367 11.00000 0.04079 0.03672 = 0.03920 -0.00935 -0.01704 -0.00626 AFIX 43 H8 2 1.267054 0.041435 0.415242 11.00000 -1.20000 AFIX 0 C9 1 1.344464 0.156751 0.234102 11.00000 0.02978 0.04153 = 0.04654 -0.01768 -0.01328 -0.00353 AFIX 43 H9 2 1.439349 0.142187 0.244244 11.00000 -1.20000 AFIX 0 C10 1 1.307843 0.237127 0.118349 11.00000 0.02382 0.03524 = 0.03682 -0.01561 -0.00224 -0.00638 AFIX 43 H10 2 1.376241 0.279163 0.047917 11.00000 -1.20000 AFIX 0 C11 1 1.167701 0.254876 0.107714 11.00000 0.02363 0.02261 = 0.02994 -0.01374 -0.00197 -0.00286 C12 1 1.112524 0.335267 -0.011780 11.00000 0.02414 0.02719 = 0.02823 -0.01120 -0.00244 -0.00509 AFIX 23 H12A 2 1.125526 0.428320 -0.041758 11.00000 -1.20000 H12B 2 1.163889 0.299784 -0.079191 11.00000 -1.20000 AFIX 0 C13 1 0.886623 0.401862 -0.081116 11.00000 0.03051 0.02017 = 0.03040 -0.01173 -0.00840 -0.00115 C14 1 0.946604 0.479913 -0.202422 11.00000 0.03574 0.02639 = 0.03138 -0.01075 -0.00680 -0.00520 AFIX 43 H14 2 1.043929 0.487651 -0.222492 11.00000 -1.20000 AFIX 0 C15 1 0.863293 0.546968 -0.294768 11.00000 0.04911 0.03134 = 0.03294 -0.00921 -0.01394 -0.00261 AFIX 43 H15 2 0.904659 0.599440 -0.378056 11.00000 -1.20000 AFIX 0 C16 1 0.720857 0.537669 -0.266033 11.00000 0.04642 0.03484 = 0.04116 -0.01141 -0.02148 0.00065 AFIX 43 H16 2 0.665136 0.583275 -0.329626 11.00000 -1.20000 AFIX 0 C17 1 0.659723 0.462033 -0.144819 11.00000 0.03356 0.03392 = 0.04574 -0.01443 -0.01690 -0.00052 AFIX 43 H17 2 0.561807 0.456440 -0.125011 11.00000 -1.20000 AFIX 0 C18 1 0.741514 0.394026 -0.051713 11.00000 0.03191 0.02616 = 0.03532 -0.01266 -0.00967 -0.00261 C19 1 0.730166 0.340043 0.494732 11.00000 0.04253 0.04280 = 0.03610 -0.01933 0.00230 -0.00582 F1 4 0.616970 0.384902 0.565365 11.00000 0.05906 0.08677 = 0.05251 -0.04325 0.00705 0.00056 F2 4 0.828623 0.411980 0.463668 11.00000 0.07265 0.08342 = 0.05565 -0.03603 0.00083 -0.03904 F3 4 0.778872 0.217149 0.562302 11.00000 0.07838 0.05301 = 0.04567 -0.01284 -0.02213 0.00117 N2 5 0.961905 0.327407 0.017650 11.00000 0.02310 0.02330 = 0.02864 -0.00907 -0.00453 -0.00382 N1 5 1.069897 0.198327 0.205236 11.00000 0.02544 0.02313 = 0.02949 -0.00984 -0.00479 -0.00416 O1 3 0.821168 0.281620 0.297580 11.00000 0.02608 0.03375 = 0.03621 -0.01620 -0.00399 -0.00321 O2 3 0.649347 0.484535 0.279158 11.00000 0.05183 0.03582 = 0.04836 -0.01140 -0.00741 0.00765 O3 3 0.573140 0.268044 0.401047 11.00000 0.03146 0.06093 = 0.04944 -0.02094 0.00301 -0.01564 S1 7 0.674772 0.293212 0.102936 11.00000 0.02606 0.04686 = 0.03866 -0.00722 -0.00791 -0.01080 S2 7 0.679536 0.348340 0.353619 11.00000 0.02723 0.03272 = 0.03432 -0.01247 -0.00009 -0.00193 SI 6 0.881083 0.228360 0.167096 11.00000 0.02342 0.02280 = 0.02855 -0.00860 -0.00349 -0.00548 PART -1 ISOR .005 C20 C21 C22 C23 C24 C25 C26 DELU .005 C20 C21 DELU .005 C21 C22 DELU .005 C22 C23 DELU .005 C23 C24 DELU .005 C24 C25 DELU .005 C25 C26 DELU .005 C26 C21 C20 1 0.546254 -0.170055 1.198556 10.50000 0.08498 0.08117 = 0.08359 -0.03822 -0.00801 0.00037 AFIX 137 H20A 2 0.647734 -0.192201 1.200209 10.50000 -1.50000 H20B 2 0.512573 -0.248388 1.207800 10.50000 -1.50000 H20C 2 0.493863 -0.140439 1.268634 10.50000 -1.50000 AFIX 66 C21 1 0.465763 0.134425 0.849605 10.50000 0.07375 0.05748 = 0.05319 -0.02570 -0.00032 -0.00709 AFIX 43 H21 2 0.446175 0.202058 0.771972 10.50000 -1.20000 AFIX 65 C22 1 0.376777 0.041020 0.919118 10.50000 0.05745 0.05908 = 0.05265 -0.03434 0.00068 -0.01252 AFIX 43 H22 2 0.296371 0.044814 0.888995 10.50000 -1.20000 AFIX 65 C23 1 0.405437 -0.057938 1.032707 10.50000 0.04868 0.05400 = 0.05026 -0.02930 -0.00255 -0.00261 AFIX 43 H23 2 0.344618 -0.121776 1.080216 10.50000 -1.20000 AFIX 65 C24 1 0.523083 -0.063491 1.076783 10.50000 0.06013 0.05090 = 0.05156 -0.03194 -0.00125 0.00558 C25 1 0.612070 0.029914 1.007271 10.50000 0.04532 0.07188 = 0.06391 -0.04772 -0.01196 0.00082 AFIX 43 H25 2 0.692475 0.026118 1.037396 10.50000 -1.20000 AFIX 65 C26 1 0.583411 0.128872 0.893682 10.50000 0.06685 0.06804 = 0.06478 -0.04106 -0.00173 -0.00485 AFIX 43 H26 2 0.644230 0.192710 0.846173 10.50000 -1.20000 PART 0 HKLF 4 REM kob12b in P-1 REM R1 = 0.0383 for 4307 Fo > 4sig(Fo) and 0.0509 for all 5598 data REM 323 parameters refined using 48 restraints END WGHT 0.0628 0.2555 REM Highest difference peak 0.403, deepest hole -0.325, 1-sigma level 0.052 Q1 1 0.5674 0.1646 0.8608 11.00000 0.05 0.40 Q2 1 0.5855 -0.0041 1.0500 11.00000 0.05 0.40 Q3 1 0.7053 0.3410 0.4377 11.00000 0.05 0.36 Q4 1 0.7972 0.2659 0.3761 11.00000 0.05 0.35 Q5 1 0.4822 -0.0443 1.0435 11.00000 0.05 0.33 Q6 1 0.7761 0.2806 0.1248 11.00000 0.05 0.32 Q7 1 0.7623 0.2628 0.1553 11.00000 0.05 0.31 Q8 1 0.8747 0.1155 0.2044 11.00000 0.05 0.31 Q9 1 0.6655 0.3205 0.1686 11.00000 0.05 0.30 Q10 1 0.9250 0.3072 0.0785 11.00000 0.05 0.28 Q11 1 0.7996 0.5267 -0.2893 11.00000 0.05 0.27 Q12 1 0.3177 -0.1035 1.0405 11.00000 0.05 0.27 Q13 1 0.9953 0.2020 0.2037 11.00000 0.05 0.26 Q14 1 0.8660 0.2985 0.2943 11.00000 0.05 0.26 Q15 1 1.1306 0.2943 0.0453 11.00000 0.05 0.26 Q16 1 1.0131 0.3356 0.0140 11.00000 0.05 0.26 Q17 1 0.7986 0.3233 0.2883 11.00000 0.05 0.25 Q18 1 1.2400 0.2530 0.1047 11.00000 0.05 0.24 Q19 1 0.9195 0.4381 -0.1489 11.00000 0.05 0.23 Q20 1 1.0762 0.1748 0.2331 11.00000 0.05 0.23 ; _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^)+(0.0628P)^2^+0.2554P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5598 _refine_ls_number_parameters 323 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1045 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.87910(19) 0.04562(15) 0.23388(16) 0.0299(3) Uani 1 1 d . . . C2 C 0.9923(2) -0.04107(19) 0.1935(2) 0.0428(4) Uani 1 1 d . . . H2 H 1.0719 -0.0074 0.1322 0.051 Uiso 1 1 calc R . . C3 C 0.9896(3) -0.1765(2) 0.2425(2) 0.0537(6) Uani 1 1 d . . . H3 H 1.0668 -0.2344 0.2140 0.064 Uiso 1 1 calc R . . C4 C 0.8758(3) -0.2263(2) 0.3316(2) 0.0552(6) Uani 1 1 d . . . H4 H 0.8750 -0.3187 0.3653 0.066 Uiso 1 1 calc R . . C5 C 0.7622(3) -0.1427(2) 0.3729(2) 0.0508(5) Uani 1 1 d . . . H5 H 0.6835 -0.1775 0.4347 0.061 Uiso 1 1 calc R . . C6 C 0.7638(2) -0.00734(18) 0.32343(17) 0.0381(4) Uani 1 1 d . . . H6 H 0.6850 0.0499 0.3512 0.046 Uiso 1 1 calc R . . C7 C 1.1052(2) 0.12036(17) 0.31922(17) 0.0335(4) Uani 1 1 d . . . H7 H 1.0345 0.0810 0.3889 0.040 Uiso 1 1 calc R . . C8 C 1.2426(2) 0.09742(18) 0.33537(18) 0.0385(4) Uani 1 1 d . . . H8 H 1.2671 0.0414 0.4152 0.046 Uiso 1 1 calc R . . C9 C 1.3445(2) 0.15675(18) 0.23410(19) 0.0380(4) Uani 1 1 d . . . H9 H 1.4393 0.1422 0.2442 0.046 Uiso 1 1 calc R . . C10 C 1.30784(18) 0.23713(17) 0.11835(17) 0.0317(3) Uani 1 1 d . . . H10 H 1.3762 0.2792 0.0479 0.038 Uiso 1 1 calc R . . C11 C 1.16770(16) 0.25488(14) 0.10771(15) 0.0249(3) Uani 1 1 d . . . C12 C 1.11252(16) 0.33527(15) -0.01178(15) 0.0266(3) Uani 1 1 d . . . H12A H 1.1255 0.4283 -0.0418 0.032 Uiso 1 1 calc R . . H12B H 1.1639 0.2998 -0.0792 0.032 Uiso 1 1 calc R . . C13 C 0.88662(17) 0.40186(14) -0.08112(15) 0.0263(3) Uani 1 1 d . . . C14 C 0.94660(19) 0.47991(15) -0.20242(16) 0.0311(3) Uani 1 1 d . . . H14 H 1.0439 0.4877 -0.2225 0.037 Uiso 1 1 calc R . . C15 C 0.8633(2) 0.54697(17) -0.29477(17) 0.0383(4) Uani 1 1 d . . . H15 H 0.9047 0.5994 -0.3781 0.046 Uiso 1 1 calc R . . C16 C 0.7209(2) 0.53767(18) -0.26603(19) 0.0404(4) Uani 1 1 d . . . H16 H 0.6651 0.5833 -0.3296 0.048 Uiso 1 1 calc R . . C17 C 0.6597(2) 0.46203(17) -0.14482(19) 0.0369(4) Uani 1 1 d . . . H17 H 0.5618 0.4564 -0.1250 0.044 Uiso 1 1 calc R . . C18 C 0.74151(18) 0.39403(16) -0.05171(16) 0.0305(3) Uani 1 1 d . . . C19 C 0.7302(2) 0.3400(2) 0.49473(18) 0.0414(4) Uani 1 1 d . . . F1 F 0.61697(16) 0.38490(17) 0.56536(13) 0.0667(4) Uani 1 1 d . . . F2 F 0.82862(17) 0.41198(16) 0.46367(14) 0.0646(4) Uani 1 1 d . . . F3 F 0.77887(17) 0.21715(14) 0.56230(12) 0.0612(4) Uani 1 1 d . . . N2 N 0.96190(14) 0.32741(12) 0.01765(13) 0.0253(3) Uani 1 1 d . . . N1 N 1.06990(14) 0.19833(12) 0.20524(13) 0.0261(3) Uani 1 1 d . . . O1 O 0.82117(12) 0.28162(12) 0.29758(11) 0.0317(3) Uani 1 1 d . . . O2 O 0.64935(17) 0.48453(14) 0.27916(14) 0.0504(4) Uani 1 1 d . . . O3 O 0.57314(15) 0.26804(16) 0.40105(14) 0.0479(3) Uani 1 1 d . . . S1 S 0.67477(5) 0.29321(5) 0.10294(5) 0.03883(12) Uani 1 1 d . . . S2 S 0.67954(5) 0.34834(4) 0.35362(4) 0.03337(11) Uani 1 1 d . . . Si Si 0.88108(5) 0.22836(4) 0.16710(4) 0.02526(11) Uani 1 1 d . . . C20 C 0.5463(10) -0.1701(8) 1.1986(8) 0.085(2) Uani 0.50 1 d PU A -1 H20A H 0.6477 -0.1922 1.2002 0.128 Uiso 0.50 1 calc PR A -1 H20B H 0.5126 -0.2484 1.2078 0.128 Uiso 0.50 1 calc PR A -1 H20C H 0.4939 -0.1404 1.2686 0.128 Uiso 0.50 1 calc PR A -1 C21 C 0.4658(5) 0.1344(3) 0.8496(3) 0.0632(15) Uani 0.50 1 d PGU A -1 H21 H 0.4462 0.2021 0.7720 0.076 Uiso 0.50 1 calc PR A -1 C22 C 0.3768(3) 0.0410(4) 0.9191(3) 0.0537(11) Uani 0.50 1 d PGU A -1 H22 H 0.2964 0.0448 0.8890 0.064 Uiso 0.50 1 calc PR A -1 C23 C 0.4054(4) -0.0579(3) 1.0327(3) 0.0504(12) Uani 0.50 1 d PGU A -1 H23 H 0.3446 -0.1218 1.0802 0.060 Uiso 0.50 1 calc PR A -1 C24 C 0.5231(5) -0.0635(3) 1.0768(3) 0.0550(10) Uani 0.50 1 d PGU A -1 C25 C 0.6121(3) 0.0299(4) 1.0073(4) 0.0545(13) Uani 0.50 1 d PGU A -1 H25 H 0.6925 0.0261 1.0374 0.065 Uiso 0.50 1 calc PR A -1 C26 C 0.5834(4) 0.1289(3) 0.8937(4) 0.0647(13) Uani 0.50 1 d PGU A -1 H26 H 0.6442 0.1927 0.8462 0.078 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0341(9) 0.0255(7) 0.0321(8) -0.0102(6) -0.0078(7) -0.0080(6) C2 0.0405(10) 0.0337(9) 0.0578(12) -0.0235(9) -0.0031(9) -0.0082(8) C3 0.0622(14) 0.0331(9) 0.0740(15) -0.0298(10) -0.0144(13) -0.0034(10) C4 0.0865(19) 0.0277(9) 0.0565(12) -0.0133(9) -0.0182(13) -0.0171(10) C5 0.0739(16) 0.0381(10) 0.0402(10) -0.0088(8) -0.0013(11) -0.0290(10) C6 0.0482(11) 0.0321(8) 0.0341(8) -0.0111(7) -0.0026(8) -0.0145(8) C7 0.0352(9) 0.0314(8) 0.0309(8) -0.0056(6) -0.0078(7) -0.0091(7) C8 0.0408(10) 0.0367(9) 0.0392(9) -0.0094(7) -0.0170(8) -0.0063(8) C9 0.0298(9) 0.0415(9) 0.0465(10) -0.0177(8) -0.0133(8) -0.0035(8) C10 0.0238(8) 0.0352(8) 0.0368(8) -0.0156(7) -0.0022(7) -0.0064(7) C11 0.0236(7) 0.0226(6) 0.0299(7) -0.0137(6) -0.0020(6) -0.0029(6) C12 0.0241(7) 0.0272(7) 0.0282(7) -0.0112(6) -0.0024(6) -0.0051(6) C13 0.0305(8) 0.0202(6) 0.0304(7) -0.0117(6) -0.0084(6) -0.0012(6) C14 0.0357(9) 0.0264(7) 0.0314(8) -0.0108(6) -0.0068(7) -0.0052(7) C15 0.0491(11) 0.0313(8) 0.0329(8) -0.0092(7) -0.0139(8) -0.0026(8) C16 0.0464(11) 0.0348(8) 0.0412(9) -0.0114(7) -0.0215(9) 0.0007(8) C17 0.0336(9) 0.0339(8) 0.0457(10) -0.0144(7) -0.0169(8) -0.0005(7) C18 0.0319(8) 0.0262(7) 0.0353(8) -0.0127(6) -0.0097(7) -0.0026(6) C19 0.0425(10) 0.0428(10) 0.0361(9) -0.0193(8) 0.0023(8) -0.0058(8) F1 0.0591(9) 0.0868(11) 0.0525(8) -0.0433(8) 0.0070(7) 0.0006(8) F2 0.0727(10) 0.0834(10) 0.0557(8) -0.0360(7) 0.0008(7) -0.0390(8) F3 0.0784(10) 0.0530(7) 0.0457(7) -0.0128(6) -0.0221(7) 0.0012(7) N2 0.0231(6) 0.0233(6) 0.0286(6) -0.0091(5) -0.0045(5) -0.0038(5) N1 0.0254(7) 0.0231(6) 0.0295(6) -0.0098(5) -0.0048(5) -0.0042(5) O1 0.0261(6) 0.0338(6) 0.0362(6) -0.0162(5) -0.0040(5) -0.0032(5) O2 0.0518(9) 0.0358(7) 0.0484(8) -0.0114(6) -0.0074(7) 0.0076(7) O3 0.0315(7) 0.0609(9) 0.0494(8) -0.0209(7) 0.0030(6) -0.0156(7) S1 0.0261(2) 0.0469(3) 0.0387(2) -0.00722(19) -0.00791(19) -0.01080(19) S2 0.0272(2) 0.0327(2) 0.0343(2) -0.01247(17) -0.00009(17) -0.00193(17) Si 0.0234(2) 0.02280(19) 0.0286(2) -0.00860(16) -0.00349(17) -0.00548(16) C20 0.085(4) 0.081(4) 0.084(4) -0.038(3) -0.008(3) 0.000(3) C21 0.074(3) 0.057(3) 0.053(3) -0.026(2) 0.000(2) -0.007(2) C22 0.057(3) 0.059(2) 0.053(2) -0.0343(19) 0.001(2) -0.013(2) C23 0.049(2) 0.054(2) 0.050(3) -0.029(2) -0.003(2) -0.003(2) C24 0.060(2) 0.051(2) 0.052(2) -0.0319(19) -0.0012(19) 0.0056(19) C25 0.045(2) 0.072(3) 0.064(3) -0.048(2) -0.012(2) 0.001(2) C26 0.067(3) 0.068(3) 0.065(3) -0.041(2) -0.002(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.394(3) . ? C1 C2 1.398(3) . ? C1 Si 1.8789(17) . ? C2 C3 1.396(3) . ? C3 C4 1.369(4) . ? C4 C5 1.382(4) . ? C5 C6 1.392(3) . ? C7 N1 1.353(2) . ? C7 C8 1.379(3) . ? C8 C9 1.383(3) . ? C9 C10 1.379(3) . ? C10 C11 1.393(2) . ? C11 N1 1.328(2) . ? C11 C12 1.494(2) . ? C12 N2 1.460(2) . ? C13 C14 1.389(2) . ? C13 C18 1.407(2) . ? C13 N2 1.4071(19) . ? C14 C15 1.396(2) . ? C15 C16 1.385(3) . ? C16 C17 1.383(3) . ? C17 C18 1.393(2) . ? C18 S1 1.748(2) . ? C19 F2 1.313(3) . ? C19 F1 1.319(2) . ? C19 F3 1.319(2) . ? C19 S2 1.834(2) . ? N2 Si 1.7439(16) . ? N1 Si 1.9700(14) . ? O1 S2 1.5228(13) . ? O1 Si 1.7737(13) . ? O2 S2 1.4165(15) . ? O3 S2 1.4169(17) . ? S1 Si 2.2298(9) . ? C20 C24 1.474(8) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? 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 C6 C1 C2 118.00(16) . . ? C6 C1 Si 121.08(13) . . ? C2 C1 Si 120.92(15) . . ? C3 C2 C1 120.7(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 120.37(19) . . ? C4 C5 C6 119.7(2) . . ? C5 C6 C1 121.1(2) . . ? N1 C7 C8 120.71(18) . . ? C7 C8 C9 119.34(17) . . ? C10 C9 C8 119.79(16) . . ? C9 C10 C11 118.08(17) . . ? N1 C11 C10 122.02(15) . . ? N1 C11 C12 113.43(13) . . ? C10 C11 C12 124.53(15) . . ? N2 C12 C11 107.05(13) . . ? C14 C13 C18 119.55(14) . . ? C14 C13 N2 124.27(15) . . ? C18 C13 N2 116.18(15) . . ? C13 C14 C15 119.73(17) . . ? C16 C15 C14 120.59(18) . . ? C17 C16 C15 120.04(16) . . ? C16 C17 C18 120.10(17) . . ? C17 C18 C13 119.98(17) . . ? C17 C18 S1 123.42(14) . . ? C13 C18 S1 116.58(12) . . ? F2 C19 F1 108.88(17) . . ? F2 C19 F3 108.28(18) . . ? F1 C19 F3 108.73(18) . . ? F2 C19 S2 111.43(14) . . ? F1 C19 S2 108.57(15) . . ? F3 C19 S2 110.89(14) . . ? C13 N2 C12 116.60(13) . . ? C13 N2 Si 122.02(11) . . ? C12 N2 Si 121.37(10) . . ? C11 N1 C7 120.05(14) . . ? C11 N1 Si 115.38(10) . . ? C7 N1 Si 124.47(13) . . ? S2 O1 Si 134.32(8) . . ? C18 S1 Si 95.43(7) . . ? O2 S2 O3 120.44(10) . . ? O2 S2 O1 112.03(9) . . ? O3 S2 O1 112.25(8) . . ? O2 S2 C19 106.11(10) . . ? O3 S2 C19 105.22(10) . . ? O1 S2 C19 97.71(8) . . ? N2 Si O1 122.26(6) . . ? N2 Si C1 129.57(8) . . ? O1 Si C1 106.59(7) . . ? N2 Si N1 82.58(7) . . ? O1 Si N1 84.07(6) . . ? C1 Si N1 91.30(7) . . ? N2 Si S1 89.78(6) . . ? O1 Si S1 96.30(5) . . ? C1 Si S1 97.08(6) . . ? N1 Si S1 171.11(5) . . ? C22 C21 C26 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 C20 117.2(6) . . ? C25 C24 C20 122.8(5) . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? 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 C6 C1 C2 C3 -0.4(3) . . . . ? Si C1 C2 C3 -179.33(16) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C3 C4 C5 C6 -0.1(3) . . . . ? C4 C5 C6 C1 -0.8(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? Si C1 C6 C5 179.94(15) . . . . ? N1 C7 C8 C9 1.0(3) . . . . ? C7 C8 C9 C10 -0.4(3) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C9 C10 C11 N1 0.8(2) . . . . ? C9 C10 C11 C12 -178.06(15) . . . . ? N1 C11 C12 N2 0.67(17) . . . . ? C10 C11 C12 N2 179.59(14) . . . . ? C18 C13 C14 C15 -1.7(2) . . . . ? N2 C13 C14 C15 178.14(14) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C17 0.3(3) . . . . ? C15 C16 C17 C18 -0.6(3) . . . . ? C16 C17 C18 C13 -0.2(3) . . . . ? C16 C17 C18 S1 -178.55(14) . . . . ? C14 C13 C18 C17 1.4(2) . . . . ? N2 C13 C18 C17 -178.43(14) . . . . ? C14 C13 C18 S1 179.81(12) . . . . ? N2 C13 C18 S1 -0.01(18) . . . . ? C14 C13 N2 C12 0.4(2) . . . . ? C18 C13 N2 C12 -179.78(13) . . . . ? C14 C13 N2 Si -178.56(12) . . . . ? C18 C13 N2 Si 1.25(18) . . . . ? C11 C12 N2 C13 177.14(11) . . . . ? C11 C12 N2 Si -3.89(16) . . . . ? C10 C11 N1 C7 -0.2(2) . . . . ? C12 C11 N1 C7 178.75(13) . . . . ? C10 C11 N1 Si -176.72(12) . . . . ? C12 C11 N1 Si 2.23(16) . . . . ? C8 C7 N1 C11 -0.7(2) . . . . ? C8 C7 N1 Si 175.47(13) . . . . ? C17 C18 S1 Si 177.54(14) . . . . ? C13 C18 S1 Si -0.82(12) . . . . ? Si O1 S2 O2 -75.37(14) . . . . ? Si O1 S2 O3 63.75(14) . . . . ? Si O1 S2 C19 173.73(12) . . . . ? F2 C19 S2 O2 -50.84(17) . . . . ? F1 C19 S2 O2 69.07(17) . . . . ? F3 C19 S2 O2 -171.53(15) . . . . ? F2 C19 S2 O3 -179.53(14) . . . . ? F1 C19 S2 O3 -59.62(17) . . . . ? F3 C19 S2 O3 59.78(17) . . . . ? F2 C19 S2 O1 64.83(15) . . . . ? F1 C19 S2 O1 -175.27(15) . . . . ? F3 C19 S2 O1 -55.87(16) . . . . ? C13 N2 Si O1 -98.80(12) . . . . ? C12 N2 Si O1 82.28(13) . . . . ? C13 N2 Si C1 97.53(13) . . . . ? C12 N2 Si C1 -81.39(14) . . . . ? C13 N2 Si N1 -176.94(12) . . . . ? C12 N2 Si N1 4.14(11) . . . . ? C13 N2 Si S1 -1.49(11) . . . . ? C12 N2 Si S1 179.59(11) . . . . ? S2 O1 Si N2 94.15(13) . . . . ? S2 O1 Si C1 -98.92(12) . . . . ? S2 O1 Si N1 171.49(12) . . . . ? S2 O1 Si S1 0.43(12) . . . . ? C6 C1 Si N2 -149.26(13) . . . . ? C2 C1 Si N2 29.64(18) . . . . ? C6 C1 Si O1 45.11(15) . . . . ? C2 C1 Si O1 -135.99(14) . . . . ? C6 C1 Si N1 129.30(14) . . . . ? C2 C1 Si N1 -51.80(15) . . . . ? C6 C1 Si S1 -53.66(14) . . . . ? C2 C1 Si S1 125.24(14) . . . . ? C11 N1 Si N2 -3.54(11) . . . . ? C7 N1 Si N2 -179.88(14) . . . . ? C11 N1 Si O1 -127.23(11) . . . . ? C7 N1 Si O1 56.43(13) . . . . ? C11 N1 Si C1 126.22(12) . . . . ? C7 N1 Si C1 -50.12(14) . . . . ? C11 N1 Si S1 -34.4(4) . . . . ? C7 N1 Si S1 149.3(3) . . . . ? C18 S1 Si N2 1.13(7) . . . . ? C18 S1 Si O1 123.58(7) . . . . ? C18 S1 Si C1 -128.77(8) . . . . ? C18 S1 Si N1 31.7(3) . . . . ? C26 C21 C22 C23 0.0 . . . . ? C21 C22 C23 C24 0.0 . . . . ? C22 C23 C24 C25 0.0 . . . . ? C22 C23 C24 C20 179.3(5) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C20 C24 C25 C26 -179.3(5) . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 29.15 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.403 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.052 data_kob14lu_7 _database_code_depnum_ccdc_archive 'CCDC 832638' #TrackingRef 'kob14lu.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H13 Cl N2 S Si' _chemical_formula_sum 'C13 H13 Cl N2 S Si' _chemical_formula_weight 292.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1864(15) _cell_length_b 9.7269(19) _cell_length_c 18.971(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.328(5) _cell_angle_gamma 90.00 _cell_volume 1318.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9761 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 32.23 _exptl_crystal_description flat_needle _exptl_crystal_colour yellow _exptl_crystal_size_max .40 _exptl_crystal_size_mid .22 _exptl_crystal_size_min .17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .6666 _exptl_absorpt_correction_T_max .7463 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source rotating_anode _diffrn_radiation_monochromator Montel_multi_layer_optics _diffrn_measurement_device_type Bruker-Kappa_Apex2_CCD _diffrn_measurement_method omega_and_phi_scans _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35821 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 32.36 _reflns_number_total 4669 _reflns_number_gt 4218 _reflns_threshold_expression >2sigma(I) _computing_data_collection Bruker-SAINT _computing_cell_refinement Bruker-SAINT _computing_data_reduction Bruker-SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob14hu in P2(1)/c CELL 0.71073 7.1864 9.7269 18.9710 90.000 96.328 90.000 ZERR 4.00 0.0015 0.0019 0.0038 0.000 0.005 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Si S Cl UNIT 52 52 8 4 4 4 L.S. 28 ACTA BOND FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -173 WGHT 0.027000 0.916800 FVAR 0.13953 0.71130 2.10758 1.87088 0.01872 0.02173 0.02354 MOLE 1 S 5 0.264420 1.282771 0.215680 11.00000 0.02186 0.01474 = 0.02171 0.00074 0.00671 0.00040 EXYZ Si Sib EADP Si Sib DFIX 31. .002 Si Cl SiB Clb DFIX 41. .002 Si C1 Sib C1b PART 1 SI 4 0.255222 1.076773 0.161225 10.50000 0.01607 0.01552 = 0.01541 0.00129 0.00290 -0.00044 CL 6 0.494530 1.126761 0.109799 21.00000 51.00000 61.00000 = 71.00000 -0.00251 0.01196 -0.00457 C1 1 0.043292 1.106583 0.096658 21.00000 51.00000 61.00000 = 71.00000 0.00821 -0.00111 0.00438 AFIX 137 H1D 2 0.037626 1.036808 0.059218 21.00000 -1.50000 H1E 2 0.050380 1.198145 0.075566 21.00000 -1.50000 H1F 2 -0.069259 1.100427 0.121333 21.00000 -1.50000 AFIX 0 PART 2 SIB 4 0.255222 1.076773 0.161225 10.50000 0.01607 0.01552 = 0.01541 0.00129 0.00290 -0.00044 EADP C1 Clb EADP CL C1b CLB 6 0.017353 1.112371 0.089772 -21.00000 51.00000 61.00000 = 71.00000 0.00821 -0.00111 0.00438 C1B 1 0.464058 1.120957 0.114711 -21.00000 51.00000 61.00000 = 71.00000 -0.00251 0.01196 -0.00457 AFIX 137 H1A 2 0.578460 1.107035 0.147098 -21.00000 -1.50000 H1B 2 0.456107 1.217324 0.099607 -21.00000 -1.50000 H1C 2 0.466883 1.061632 0.073090 -21.00000 -1.50000 AFIX 0 PART 0 N2 3 0.236532 0.999476 0.243396 11.00000 0.01979 0.01404 = 0.01642 0.00070 0.00258 -0.00014 N1 3 0.279023 0.883435 0.130760 11.00000 0.01663 0.01815 = 0.01862 -0.00012 0.00436 -0.00005 C7 1 0.217974 1.075288 0.304833 11.00000 0.01484 0.01852 = 0.01641 -0.00004 0.00176 0.00078 C2 1 0.229693 1.218871 0.299386 11.00000 0.01453 0.01844 = 0.01923 -0.00083 0.00275 0.00095 C8 1 0.235892 0.851306 0.251362 11.00000 0.01874 0.01532 = 0.01782 0.00230 0.00246 -0.00037 AFIX 23 H8A 2 0.114090 0.820154 0.265385 11.00000 -1.20000 H8B 2 0.336031 0.822470 0.288455 11.00000 -1.20000 AFIX 0 C3 1 0.215255 1.301606 0.358014 11.00000 0.01980 0.02180 = 0.02491 -0.00593 0.00385 0.00170 AFIX 43 H3 2 0.224275 1.398651 0.353878 11.00000 -1.20000 AFIX 0 C9 1 0.268073 0.790630 0.182033 11.00000 0.01456 0.01711 = 0.01993 0.00028 0.00200 0.00004 C10 1 0.287784 0.650716 0.170351 11.00000 0.02199 0.01604 = 0.02617 -0.00058 0.00079 -0.00015 AFIX 43 H10 2 0.280002 0.586393 0.207595 11.00000 -1.20000 AFIX 0 C6 1 0.189663 1.017175 0.370144 11.00000 0.02113 0.02482 = 0.01776 0.00229 0.00301 -0.00015 AFIX 43 H6 2 0.181169 0.920192 0.374772 11.00000 -1.20000 AFIX 0 C11 1 0.318985 0.607160 0.103300 11.00000 0.02451 0.01993 = 0.03179 -0.00658 0.00354 -0.00064 AFIX 43 H11 2 0.334577 0.512148 0.093951 11.00000 -1.20000 AFIX 0 C12 1 0.327343 0.703539 0.049710 11.00000 0.02679 0.02543 = 0.02580 -0.00735 0.00764 -0.00112 AFIX 43 H12 2 0.347256 0.675146 0.003218 11.00000 -1.20000 AFIX 0 C5 1 0.173882 1.101834 0.428572 11.00000 0.02406 0.03412 = 0.01642 -0.00053 0.00429 0.00074 AFIX 43 H5 2 0.153464 1.061898 0.472767 11.00000 -1.20000 AFIX 0 C4 1 0.187560 1.242816 0.422961 11.00000 0.02438 0.03222 = 0.02047 -0.00677 0.00419 0.00210 AFIX 43 H4 2 0.178130 1.299478 0.463201 11.00000 -1.20000 AFIX 0 C13 1 0.306455 0.840367 0.064793 11.00000 0.02481 0.02367 = 0.01984 -0.00204 0.00742 -0.00028 AFIX 43 H13 2 0.311353 0.906349 0.028123 11.00000 -1.20000 HKLF 4 REM kob14hu in P2(1)/c REM R1 = 0.0337 for 4218 Fo > 4sig(Fo) and 0.0386 for all 4669 data REM 171 parameters refined using 4 restraints END WGHT 0.0269 0.9169 REM Highest difference peak 0.523, deepest hole -0.288, 1-sigma level 0.062 Q1 1 0.2447 1.0197 0.2113 11.00000 0.05 0.52 Q2 1 0.2573 1.2095 0.1708 11.00000 0.05 0.44 Q3 1 0.2677 0.7184 0.1746 11.00000 0.05 0.42 Q4 1 0.3233 0.7783 0.0583 11.00000 0.05 0.41 Q5 1 0.2266 1.2605 0.3276 11.00000 0.05 0.41 Q6 1 0.1922 1.2679 0.3900 11.00000 0.05 0.39 Q7 1 0.1368 1.1011 0.1226 11.00000 0.05 0.38 Q8 1 0.2278 1.1458 0.2989 11.00000 0.05 0.38 Q9 1 0.3279 0.6560 0.0804 11.00000 0.05 0.37 Q10 1 0.2005 1.1749 0.4226 11.00000 0.05 0.35 Q11 1 0.2366 0.9343 0.2509 11.00000 0.05 0.34 Q12 1 0.2703 0.8345 0.1554 11.00000 0.05 0.34 Q13 1 0.3239 0.6346 0.1414 11.00000 0.05 0.34 Q14 1 0.2663 0.8236 0.2196 11.00000 0.05 0.33 Q15 1 0.1849 1.0622 0.3980 11.00000 0.05 0.33 Q16 1 0.2062 1.0466 0.3384 11.00000 0.05 0.32 Q17 1 0.1634 1.3079 0.2009 11.00000 0.05 0.27 Q18 1 0.5803 1.1155 0.1158 11.00000 0.05 0.27 Q19 1 0.2163 1.0377 0.2755 11.00000 0.05 0.27 Q20 1 0.2337 1.2427 0.2697 11.00000 0.05 0.26 ; _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^)+(0.0270P)^2^+0.9168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4669 _refine_ls_number_parameters 171 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.26442(5) 1.28277(3) 0.215680(17) 0.01911(7) Uani 1 1 d . . . Si Si 0.25522(5) 1.07677(3) 0.161225(18) 0.01558(8) Uani 0.50 1 d PD A 1 Cl Cl 0.49453(10) 1.12676(10) 0.10980(5) 0.02061(12) Uani 0.7113(13) 1 d PD A 1 C1 C 0.0433(5) 1.1066(7) 0.0967(2) 0.02159(11) Uani 0.7113(13) 1 d PD A 1 H1D H 0.0376 1.0368 0.0592 0.032 Uiso 0.7113(13) 1 calc PR A 1 H1E H 0.0504 1.1981 0.0756 0.032 Uiso 0.7113(13) 1 calc PR A 1 H1F H -0.0693 1.1004 0.1213 0.032 Uiso 0.7113(13) 1 calc PR A 1 SiB Si 0.25522(5) 1.07677(3) 0.161225(18) 0.01558(8) Uani 0.50 1 d PD A 2 ClB Cl 0.0174(2) 1.1124(4) 0.08977(11) 0.02159(11) Uani 0.2887(13) 1 d PD A 2 C1B C 0.4641(13) 1.1210(13) 0.1147(6) 0.02061(12) Uani 0.2887(13) 1 d PD A 2 H1A H 0.5785 1.1070 0.1471 0.031 Uiso 0.2887(13) 1 calc PR A 2 H1B H 0.4561 1.2173 0.0996 0.031 Uiso 0.2887(13) 1 calc PR A 2 H1C H 0.4669 1.0616 0.0731 0.031 Uiso 0.2887(13) 1 calc PR A 2 N2 N 0.23653(15) 0.99948(11) 0.24340(5) 0.01671(19) Uani 1 1 d . . . N1 N 0.27902(15) 0.88344(11) 0.13076(6) 0.0176(2) Uani 1 1 d . . . C7 C 0.21797(17) 1.07529(13) 0.30483(6) 0.0166(2) Uani 1 1 d . A . C2 C 0.22969(17) 1.21887(13) 0.29939(7) 0.0173(2) Uani 1 1 d . A . C8 C 0.23589(18) 0.85131(12) 0.25136(6) 0.0173(2) Uani 1 1 d . A . H8A H 0.1141 0.8202 0.2654 0.021 Uiso 1 1 calc R . . H8B H 0.3360 0.8225 0.2885 0.021 Uiso 1 1 calc R . . C3 C 0.21526(19) 1.30161(14) 0.35801(7) 0.0221(2) Uani 1 1 d . . . H3 H 0.2243 1.3987 0.3539 0.026 Uiso 1 1 calc R A . C9 C 0.26807(17) 0.79063(13) 0.18203(7) 0.0172(2) Uani 1 1 d . A . C10 C 0.28778(19) 0.65072(13) 0.17035(7) 0.0215(2) Uani 1 1 d . . . H10 H 0.2800 0.5864 0.2076 0.026 Uiso 1 1 calc R A . C6 C 0.18966(19) 1.01717(15) 0.37014(7) 0.0212(2) Uani 1 1 d . . . H6 H 0.1812 0.9202 0.3748 0.025 Uiso 1 1 calc R A . C11 C 0.3190(2) 0.60716(15) 0.10330(8) 0.0254(3) Uani 1 1 d . A . H11 H 0.3346 0.5121 0.0940 0.030 Uiso 1 1 calc R . . C12 C 0.3273(2) 0.70354(15) 0.04971(8) 0.0257(3) Uani 1 1 d . . . H12 H 0.3473 0.6751 0.0032 0.031 Uiso 1 1 calc R A . C5 C 0.1739(2) 1.10183(16) 0.42857(7) 0.0247(3) Uani 1 1 d . A . H5 H 0.1535 1.0619 0.4728 0.030 Uiso 1 1 calc R . . C4 C 0.1876(2) 1.24282(16) 0.42296(7) 0.0256(3) Uani 1 1 d . A . H4 H 0.1781 1.2995 0.4632 0.031 Uiso 1 1 calc R . . C13 C 0.3065(2) 0.84037(14) 0.06479(7) 0.0224(2) Uani 1 1 d . A . H13 H 0.3114 0.9063 0.0281 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S 0.02186(15) 0.01474(13) 0.02171(14) 0.00074(10) 0.00671(11) 0.00040(10) Si 0.01607(16) 0.01552(15) 0.01541(15) 0.00129(11) 0.00290(11) -0.00044(11) Cl 0.0187(3) 0.0217(2) 0.0235(2) -0.00251(17) 0.0120(2) -0.0046(2) C1 0.0187(3) 0.0217(2) 0.0235(2) 0.0082(5) -0.0011(4) 0.0044(6) SiB 0.01607(16) 0.01552(15) 0.01541(15) 0.00129(11) 0.00290(11) -0.00044(11) ClB 0.0187(3) 0.0217(2) 0.0235(2) 0.0082(5) -0.0011(4) 0.0044(6) C1B 0.0187(3) 0.0217(2) 0.0235(2) -0.00251(17) 0.0120(2) -0.0046(2) N2 0.0198(5) 0.0140(4) 0.0164(4) 0.0007(3) 0.0026(4) -0.0001(4) N1 0.0166(5) 0.0182(5) 0.0186(5) -0.0001(4) 0.0044(4) 0.0000(4) C7 0.0148(5) 0.0185(5) 0.0164(5) 0.0000(4) 0.0018(4) 0.0008(4) C2 0.0145(5) 0.0184(5) 0.0192(5) -0.0008(4) 0.0028(4) 0.0010(4) C8 0.0187(6) 0.0153(5) 0.0178(5) 0.0023(4) 0.0025(4) -0.0004(4) C3 0.0198(6) 0.0218(6) 0.0249(6) -0.0059(5) 0.0038(5) 0.0017(5) C9 0.0146(5) 0.0171(5) 0.0199(5) 0.0003(4) 0.0020(4) 0.0000(4) C10 0.0220(6) 0.0160(5) 0.0262(6) -0.0006(4) 0.0008(5) -0.0001(4) C6 0.0211(6) 0.0248(6) 0.0178(5) 0.0023(4) 0.0030(4) -0.0001(5) C11 0.0245(7) 0.0199(6) 0.0318(7) -0.0066(5) 0.0035(5) -0.0006(5) C12 0.0268(7) 0.0254(6) 0.0258(6) -0.0074(5) 0.0076(5) -0.0011(5) C5 0.0241(6) 0.0341(7) 0.0164(5) -0.0005(5) 0.0043(5) 0.0007(5) C4 0.0244(7) 0.0322(7) 0.0205(6) -0.0068(5) 0.0042(5) 0.0021(5) C13 0.0248(6) 0.0237(6) 0.0198(6) -0.0020(5) 0.0074(5) -0.0003(5) _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 S C2 1.7486(13) . ? S Si 2.2520(6) . ? Si N2 1.7492(11) . ? Si C1 1.869(4) . ? Si N1 1.9803(12) . ? Si Cl 2.1250(6) . ? N2 C7 1.3980(16) . ? N2 C8 1.4492(16) . ? N1 C9 1.3357(16) . ? N1 C13 1.3546(16) . ? C7 C6 1.3970(17) . ? C7 C2 1.4036(17) . ? C2 C3 1.3860(18) . ? C8 C9 1.4828(17) . ? C3 C4 1.392(2) . ? C9 C10 1.3886(18) . ? C10 C11 1.382(2) . ? C6 C5 1.3955(19) . ? C11 C12 1.389(2) . ? C12 C13 1.373(2) . ? C5 C4 1.380(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 S Si 95.76(5) . . ? N2 Si C1 120.91(16) . . ? N2 Si N1 82.50(5) . . ? C1 Si N1 92.7(2) . . ? N2 Si Cl 130.77(5) . . ? C1 Si Cl 107.81(13) . . ? N1 Si Cl 89.03(4) . . ? N2 Si S 88.56(4) . . ? C1 Si S 98.2(2) . . ? N1 Si S 168.44(4) . . ? Cl Si S 91.30(3) . . ? C7 N2 C8 115.85(10) . . ? C7 N2 Si 122.69(9) . . ? C8 N2 Si 121.46(8) . . ? C9 N1 C13 119.34(11) . . ? C9 N1 Si 114.54(9) . . ? C13 N1 Si 126.11(9) . . ? C6 C7 N2 124.24(12) . . ? C6 C7 C2 118.93(12) . . ? N2 C7 C2 116.84(11) . . ? C3 C2 C7 120.55(12) . . ? C3 C2 S 123.59(10) . . ? C7 C2 S 115.86(9) . . ? N2 C8 C9 107.50(10) . . ? C2 C3 C4 120.15(13) . . ? N1 C9 C10 122.07(12) . . ? N1 C9 C8 113.85(11) . . ? C10 C9 C8 124.07(11) . . ? C11 C10 C9 118.49(13) . . ? C5 C6 C7 119.88(13) . . ? C10 C11 C12 119.42(13) . . ? C13 C12 C11 119.15(13) . . ? C4 C5 C6 120.83(13) . . ? C5 C4 C3 119.65(13) . . ? N1 C13 C12 121.51(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 S Si N2 -3.95(6) . . . . ? C2 S Si C1 117.09(15) . . . . ? C2 S Si N1 -43.21(19) . . . . ? C2 S Si Cl -134.70(5) . . . . ? C1 Si N2 C7 -93.3(3) . . . . ? N1 Si N2 C7 178.10(10) . . . . ? Cl Si N2 C7 95.93(11) . . . . ? S Si N2 C7 5.45(10) . . . . ? C1 Si N2 C8 85.5(3) . . . . ? N1 Si N2 C8 -3.09(10) . . . . ? Cl Si N2 C8 -85.27(11) . . . . ? S Si N2 C8 -175.74(10) . . . . ? N2 Si N1 C9 0.88(9) . . . . ? C1 Si N1 C9 -119.95(17) . . . . ? Cl Si N1 C9 132.26(9) . . . . ? S Si N1 C9 40.5(2) . . . . ? N2 Si N1 C13 -178.37(12) . . . . ? C1 Si N1 C13 60.79(18) . . . . ? Cl Si N1 C13 -47.00(11) . . . . ? S Si N1 C13 -138.72(16) . . . . ? C8 N2 C7 C6 -3.53(18) . . . . ? Si N2 C7 C6 175.34(10) . . . . ? C8 N2 C7 C2 176.22(11) . . . . ? Si N2 C7 C2 -4.91(16) . . . . ? C6 C7 C2 C3 0.63(19) . . . . ? N2 C7 C2 C3 -179.14(12) . . . . ? C6 C7 C2 S -179.79(10) . . . . ? N2 C7 C2 S 0.45(15) . . . . ? Si S C2 C3 -177.76(11) . . . . ? Si S C2 C7 2.67(10) . . . . ? C7 N2 C8 C9 -176.72(10) . . . . ? Si N2 C8 C9 4.39(14) . . . . ? C7 C2 C3 C4 -0.5(2) . . . . ? S C2 C3 C4 179.99(11) . . . . ? C13 N1 C9 C10 1.35(19) . . . . ? Si N1 C9 C10 -177.96(10) . . . . ? C13 N1 C9 C8 -179.39(11) . . . . ? Si N1 C9 C8 1.30(14) . . . . ? N2 C8 C9 N1 -3.29(15) . . . . ? N2 C8 C9 C10 175.95(12) . . . . ? N1 C9 C10 C11 -0.2(2) . . . . ? C8 C9 C10 C11 -179.43(12) . . . . ? N2 C7 C6 C5 179.64(12) . . . . ? C2 C7 C6 C5 -0.11(19) . . . . ? C9 C10 C11 C12 -0.8(2) . . . . ? C10 C11 C12 C13 0.7(2) . . . . ? C7 C6 C5 C4 -0.6(2) . . . . ? C6 C5 C4 C3 0.8(2) . . . . ? C2 C3 C4 C5 -0.2(2) . . . . ? C9 N1 C13 C12 -1.4(2) . . . . ? Si N1 C13 C12 177.80(11) . . . . ? C11 C12 C13 N1 0.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 32.36 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.523 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.062 ##***************************** compound 8 ************* data_kob19abs_8 _database_code_depnum_ccdc_archive 'CCDC 832639' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N2 O S Si' _chemical_formula_sum 'C19 H18 N2 O S Si' _chemical_formula_weight 350.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.258(2) _cell_length_b 7.6485(12) _cell_length_c 22.037(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.92(3) _cell_angle_gamma 90.00 _cell_volume 1722.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.45 _cell_measurement_theta_max 27.05 _exptl_crystal_description quadratic_prism _exptl_crystal_colour light_yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .5 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 0.266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8720 _exptl_absorpt_correction_T_max 0.9491 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26739 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 29.12 _reflns_number_total 4556 _reflns_number_gt 3694 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob19b in P2(1)/c CELL 0.71073 10.2584 7.6485 22.0369 90.000 94.922 90.000 ZERR 4 0.0022 0.0012 0.0054 0.000 0.027 0.000 REM CELL 0.71073 10.2661 7.6536 22.0407 90.000 94.802 90.000 REM ZERR 4.00 0.0021 0.0015 0.0044 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N O Si S UNIT 76 72 8 4 4 4 L.S. 12 ACTA BOND FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -100 WGHT 0.050200 0.556400 FVAR 0.92181 MOLE 1 C1 1 0.439201 0.669555 0.316225 11.00000 0.04125 0.03794 = 0.03834 -0.00978 0.00144 0.00182 AFIX 137 H1A 2 0.358327 0.669374 0.289104 11.00000 -1.50000 H1B 2 0.453778 0.552873 0.333893 11.00000 -1.50000 H1C 2 0.513018 0.701092 0.292987 11.00000 -1.50000 AFIX 0 C2 1 0.290983 1.107136 0.322173 11.00000 0.02884 0.03102 = 0.03640 0.00504 0.00040 -0.00112 C3 1 0.224991 1.241218 0.348706 11.00000 0.04703 0.04808 = 0.03899 -0.00258 -0.00442 0.01339 AFIX 43 H3 2 0.254589 1.282329 0.388182 11.00000 -1.20000 AFIX 0 C4 1 0.115127 1.315449 0.317276 11.00000 0.04569 0.05648 = 0.05406 0.00415 0.00225 0.01912 AFIX 43 H4 2 0.069579 1.406918 0.335564 11.00000 -1.20000 AFIX 0 C5 1 0.071704 1.257053 0.259582 11.00000 0.03210 0.05418 = 0.05409 0.01617 -0.00576 -0.00011 AFIX 43 H5 2 -0.004379 1.306247 0.238605 11.00000 -1.20000 AFIX 0 C6 1 0.140181 1.126481 0.232832 11.00000 0.04380 0.04730 = 0.04121 0.00450 -0.00914 -0.00847 AFIX 43 H6 2 0.112036 1.087866 0.192870 11.00000 -1.20000 AFIX 0 C7 1 0.249867 1.051035 0.263816 11.00000 0.03981 0.03711 = 0.03799 -0.00026 -0.00002 -0.00153 AFIX 43 H7 2 0.296449 0.961419 0.245080 11.00000 -1.20000 AFIX 0 C8 1 0.673744 0.968481 0.337795 11.00000 0.03756 0.04077 = 0.04864 0.00020 0.00906 0.00010 AFIX 43 H8 2 0.625671 0.988080 0.299612 11.00000 -1.20000 AFIX 0 C9 1 0.804010 1.013399 0.345165 11.00000 0.03966 0.04255 = 0.07073 -0.00583 0.01902 -0.00280 AFIX 43 H9 2 0.845498 1.063961 0.312468 11.00000 -1.20000 AFIX 0 C10 1 0.874134 0.983948 0.400971 11.00000 0.02964 0.04522 = 0.08350 -0.01279 0.00728 -0.00089 AFIX 43 H10 2 0.964393 1.012980 0.406694 11.00000 -1.20000 AFIX 0 C11 1 0.811712 0.912356 0.447885 11.00000 0.03101 0.04287 = 0.06228 -0.01101 -0.00476 0.00310 AFIX 43 H11 2 0.857914 0.892222 0.486479 11.00000 -1.20000 AFIX 0 C12 1 0.679191 0.869772 0.437788 11.00000 0.02862 0.03010 = 0.04401 -0.00900 -0.00338 0.00562 C13 1 0.597795 0.794344 0.484037 11.00000 0.03167 0.03460 = 0.03362 -0.00713 -0.00591 0.00667 AFIX 23 H13A 2 0.631410 0.677604 0.496934 11.00000 -1.20000 H13B 2 0.600689 0.870969 0.520335 11.00000 -1.20000 AFIX 0 C14 1 0.371373 0.713528 0.493372 11.00000 0.03612 0.02612 = 0.03019 -0.00385 0.00252 0.00529 C15 1 0.399404 0.660644 0.553964 11.00000 0.04589 0.03832 = 0.03199 -0.00390 0.00130 0.00686 AFIX 43 H15 2 0.486114 0.669950 0.572616 11.00000 -1.20000 AFIX 0 C16 1 0.300685 0.594606 0.586854 11.00000 0.06014 0.04511 = 0.03273 0.00172 0.00872 0.00672 AFIX 43 H16 2 0.320680 0.558697 0.627866 11.00000 -1.20000 AFIX 0 C17 1 0.173589 0.580493 0.560608 11.00000 0.05228 0.04582 = 0.04554 0.00286 0.01700 0.00020 AFIX 43 H17 2 0.107000 0.533593 0.583240 11.00000 -1.20000 AFIX 0 C18 1 0.144200 0.635440 0.500930 11.00000 0.03861 0.03841 = 0.04634 0.00007 0.00817 -0.00023 AFIX 43 H18 2 0.056788 0.627468 0.483045 11.00000 -1.20000 AFIX 0 C19 1 0.241136 0.701960 0.467049 11.00000 0.03570 0.02891 = 0.03452 -0.00210 0.00287 0.00333 N1 3 0.612869 0.897044 0.383803 11.00000 0.02863 0.03128 = 0.03949 -0.00396 0.00236 0.00199 N2 3 0.463891 0.779929 0.456394 11.00000 0.02759 0.03234 = 0.03037 -0.00290 -0.00215 0.00416 O 4 0.401499 1.038768 0.352688 11.00000 0.02930 0.03339 = 0.04290 0.00084 -0.00275 0.00120 S 6 0.210648 0.780073 0.392579 11.00000 0.02799 0.05137 = 0.03841 0.00710 -0.00166 -0.00111 SI 5 0.424781 0.833143 0.378903 11.00000 0.02750 0.02924 = 0.02923 -0.00288 -0.00025 0.00238 HKLF 4 REM kob19b in P2(1)/c REM R1 = 0.0382 for 3694 Fo > 4sig(Fo) and 0.0478 for all 4556 data REM 218 parameters refined using 0 restraints END WGHT 0.0502 0.5564 REM Highest difference peak 0.291, deepest hole -0.271, 1-sigma level 0.046 Q1 1 0.4529 0.7986 0.4276 11.00000 0.05 0.29 Q2 1 0.4407 0.7403 0.3419 11.00000 0.05 0.27 Q3 1 0.5498 0.8682 0.3794 11.00000 0.05 0.26 Q4 1 0.3872 0.7070 0.5262 11.00000 0.05 0.25 Q5 1 0.3094 0.8360 0.3912 11.00000 0.05 0.25 Q6 1 0.3059 0.7150 0.4815 11.00000 0.05 0.25 Q7 1 0.0763 1.2427 0.3030 11.00000 0.05 0.24 Q8 1 0.6359 0.8703 0.4123 11.00000 0.05 0.23 Q9 1 0.3472 1.0762 0.3388 11.00000 0.05 0.23 Q10 1 0.2009 0.6966 0.4840 11.00000 0.05 0.22 Q11 1 0.2180 0.7238 0.4401 11.00000 0.05 0.22 Q12 1 0.8350 0.9662 0.3704 11.00000 0.05 0.22 Q13 1 0.2370 0.6223 0.5801 11.00000 0.05 0.22 Q14 1 0.2562 1.0389 0.3019 11.00000 0.05 0.22 Q15 1 0.6491 0.8364 0.4599 11.00000 0.05 0.21 Q16 1 0.1529 0.5814 0.5296 11.00000 0.05 0.20 Q17 1 0.5152 0.7845 0.4623 11.00000 0.05 0.19 Q18 1 0.4306 0.7612 0.4698 11.00000 0.05 0.19 Q19 1 0.7426 0.8879 0.4431 11.00000 0.05 0.19 Q20 1 0.3693 1.0539 0.3671 11.00000 0.05 0.18 ; _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^)+(0.0502P)^2^+0.5564P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4556 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.43920(15) 0.6696(2) 0.31623(7) 0.0393(3) Uani 1 1 d . . . H1A H 0.3583 0.6694 0.2891 0.059 Uiso 1 1 calc R . . H1B H 0.4538 0.5529 0.3339 0.059 Uiso 1 1 calc R . . H1C H 0.5130 0.7011 0.2930 0.059 Uiso 1 1 calc R . . C2 C 0.29098(13) 1.1071(2) 0.32217(6) 0.0322(3) Uani 1 1 d . . . C3 C 0.22499(17) 1.2412(2) 0.34871(8) 0.0452(4) Uani 1 1 d . . . H3 H 0.2546 1.2823 0.3882 0.054 Uiso 1 1 calc R . . C4 C 0.11513(18) 1.3154(3) 0.31728(9) 0.0522(4) Uani 1 1 d . . . H4 H 0.0696 1.4069 0.3356 0.063 Uiso 1 1 calc R . . C5 C 0.07170(16) 1.2571(3) 0.25958(8) 0.0473(4) Uani 1 1 d . . . H5 H -0.0044 1.3062 0.2386 0.057 Uiso 1 1 calc R . . C6 C 0.14018(16) 1.1265(2) 0.23283(8) 0.0448(4) Uani 1 1 d . . . H6 H 0.1120 1.0879 0.1929 0.054 Uiso 1 1 calc R . . C7 C 0.24987(15) 1.0510(2) 0.26382(7) 0.0385(3) Uani 1 1 d . . . H7 H 0.2964 0.9614 0.2451 0.046 Uiso 1 1 calc R . . C8 C 0.67374(15) 0.9685(2) 0.33780(8) 0.0420(3) Uani 1 1 d . . . H8 H 0.6257 0.9881 0.2996 0.050 Uiso 1 1 calc R . . C9 C 0.80401(17) 1.0134(2) 0.34517(10) 0.0502(4) Uani 1 1 d . . . H9 H 0.8455 1.0640 0.3125 0.060 Uiso 1 1 calc R . . C10 C 0.87413(16) 0.9839(3) 0.40097(10) 0.0526(5) Uani 1 1 d . . . H10 H 0.9644 1.0130 0.4067 0.063 Uiso 1 1 calc R . . C11 C 0.81171(15) 0.9124(2) 0.44789(9) 0.0459(4) Uani 1 1 d . . . H11 H 0.8579 0.8922 0.4865 0.055 Uiso 1 1 calc R . . C12 C 0.67919(13) 0.8698(2) 0.43779(7) 0.0346(3) Uani 1 1 d . . . C13 C 0.59780(13) 0.7943(2) 0.48404(6) 0.0338(3) Uani 1 1 d . . . H13A H 0.6314 0.6776 0.4969 0.041 Uiso 1 1 calc R . . H13B H 0.6007 0.8710 0.5203 0.041 Uiso 1 1 calc R . . C14 C 0.37137(14) 0.71353(18) 0.49337(6) 0.0308(3) Uani 1 1 d . . . C15 C 0.39940(16) 0.6606(2) 0.55396(7) 0.0389(3) Uani 1 1 d . . . H15 H 0.4861 0.6700 0.5726 0.047 Uiso 1 1 calc R . . C16 C 0.30068(18) 0.5946(2) 0.58685(7) 0.0457(4) Uani 1 1 d . . . H16 H 0.3207 0.5587 0.6279 0.055 Uiso 1 1 calc R . . C17 C 0.17359(18) 0.5805(2) 0.56061(8) 0.0471(4) Uani 1 1 d . . . H17 H 0.1070 0.5336 0.5832 0.057 Uiso 1 1 calc R . . C18 C 0.14420(16) 0.6354(2) 0.50093(8) 0.0409(3) Uani 1 1 d . . . H18 H 0.0568 0.6275 0.4830 0.049 Uiso 1 1 calc R . . C19 C 0.24114(14) 0.70196(19) 0.46705(7) 0.0331(3) Uani 1 1 d . . . N1 N 0.61287(11) 0.89704(17) 0.38380(6) 0.0332(3) Uani 1 1 d . . . N2 N 0.46389(11) 0.77993(16) 0.45639(5) 0.0304(2) Uani 1 1 d . . . O O 0.40150(9) 1.03877(14) 0.35269(5) 0.0355(2) Uani 1 1 d . . . S S 0.21065(3) 0.78007(6) 0.392579(18) 0.03952(11) Uani 1 1 d . . . Si Si 0.42478(4) 0.83314(5) 0.378903(17) 0.02881(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0413(8) 0.0379(8) 0.0383(7) -0.0098(6) 0.0014(6) 0.0018(6) C2 0.0288(6) 0.0310(7) 0.0364(7) 0.0050(5) 0.0004(5) -0.0011(5) C3 0.0470(8) 0.0481(10) 0.0390(8) -0.0026(7) -0.0044(6) 0.0134(7) C4 0.0457(9) 0.0565(12) 0.0541(10) 0.0042(8) 0.0022(7) 0.0191(8) C5 0.0321(7) 0.0542(11) 0.0541(10) 0.0162(8) -0.0058(6) -0.0001(7) C6 0.0438(8) 0.0473(10) 0.0412(8) 0.0045(7) -0.0091(6) -0.0085(7) C7 0.0398(7) 0.0371(8) 0.0380(7) -0.0003(6) 0.0000(6) -0.0015(6) C8 0.0376(7) 0.0408(9) 0.0486(9) 0.0002(7) 0.0091(6) 0.0001(6) C9 0.0397(8) 0.0425(10) 0.0707(12) -0.0058(8) 0.0190(8) -0.0028(7) C10 0.0296(7) 0.0452(10) 0.0835(13) -0.0128(9) 0.0073(8) -0.0009(7) C11 0.0310(7) 0.0429(9) 0.0623(10) -0.0110(8) -0.0048(7) 0.0031(6) C12 0.0286(6) 0.0301(7) 0.0440(8) -0.0090(6) -0.0034(5) 0.0056(5) C13 0.0317(6) 0.0346(8) 0.0336(7) -0.0071(5) -0.0059(5) 0.0067(5) C14 0.0361(7) 0.0261(7) 0.0302(6) -0.0039(5) 0.0025(5) 0.0053(5) C15 0.0459(8) 0.0383(8) 0.0320(7) -0.0039(6) 0.0013(6) 0.0069(6) C16 0.0601(10) 0.0451(9) 0.0327(7) 0.0017(6) 0.0087(7) 0.0067(8) C17 0.0523(9) 0.0458(10) 0.0455(9) 0.0029(7) 0.0170(7) 0.0002(7) C18 0.0386(7) 0.0384(9) 0.0463(8) 0.0001(6) 0.0082(6) -0.0002(6) C19 0.0357(7) 0.0289(7) 0.0345(7) -0.0021(5) 0.0029(5) 0.0033(5) N1 0.0286(5) 0.0313(6) 0.0395(6) -0.0040(5) 0.0024(4) 0.0020(4) N2 0.0276(5) 0.0323(6) 0.0304(5) -0.0029(4) -0.0021(4) 0.0042(4) O 0.0293(5) 0.0334(5) 0.0429(5) 0.0008(4) -0.0028(4) 0.0012(4) S 0.02799(17) 0.0514(2) 0.03841(19) 0.00710(16) -0.00166(13) -0.00111(15) Si 0.02750(18) 0.0292(2) 0.02923(18) -0.00288(14) -0.00025(13) 0.00238(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si 1.8789(15) . ? C2 O 1.3712(16) . ? C2 C3 1.386(2) . ? C2 C7 1.387(2) . ? C3 C4 1.392(2) . ? C4 C5 1.385(3) . ? C5 C6 1.382(3) . ? C6 C7 1.390(2) . ? C8 N1 1.351(2) . ? C8 C9 1.376(2) . ? C9 C10 1.389(3) . ? C10 C11 1.376(3) . ? C11 C12 1.397(2) . ? C12 N1 1.3352(19) . ? C12 C13 1.488(2) . ? C13 N2 1.4583(17) . ? C14 N2 1.3984(19) . ? C14 C15 1.401(2) . ? C14 C19 1.413(2) . ? C15 C16 1.390(2) . ? C16 C17 1.384(3) . ? C17 C18 1.389(2) . ? C18 C19 1.390(2) . ? C19 S 1.7492(15) . ? N1 Si 1.9844(13) . ? N2 Si 1.7678(13) . ? O Si 1.6854(12) . ? S Si 2.2792(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O C2 C3 119.25(13) . . ? O C2 C7 120.65(14) . . ? C3 C2 C7 119.98(14) . . ? C2 C3 C4 119.73(16) . . ? C5 C4 C3 120.54(17) . . ? C6 C5 C4 119.31(15) . . ? C5 C6 C7 120.67(16) . . ? C2 C7 C6 119.73(16) . . ? N1 C8 C9 121.28(17) . . ? C8 C9 C10 119.21(17) . . ? C11 C10 C9 119.40(15) . . ? C10 C11 C12 118.85(17) . . ? N1 C12 C11 121.33(16) . . ? N1 C12 C13 113.44(12) . . ? C11 C12 C13 125.22(14) . . ? N2 C13 C12 107.88(11) . . ? N2 C14 C15 124.48(13) . . ? N2 C14 C19 116.66(12) . . ? C15 C14 C19 118.86(14) . . ? C16 C15 C14 120.18(15) . . ? C17 C16 C15 120.84(15) . . ? C16 C17 C18 119.48(16) . . ? C17 C18 C19 120.81(15) . . ? C18 C19 C14 119.81(14) . . ? C18 C19 S 123.39(12) . . ? C14 C19 S 116.77(11) . . ? C12 N1 C8 119.92(13) . . ? C12 N1 Si 115.39(10) . . ? C8 N1 Si 124.66(11) . . ? C14 N2 C13 116.50(12) . . ? C14 N2 Si 122.51(9) . . ? C13 N2 Si 120.91(10) . . ? C2 O Si 127.65(9) . . ? C19 S Si 95.05(6) . . ? O Si N2 124.03(6) . . ? O Si C1 112.78(7) . . ? N2 Si C1 122.08(7) . . ? O Si N1 84.11(5) . . ? N2 Si N1 82.25(6) . . ? C1 Si N1 93.81(7) . . ? O Si S 95.84(4) . . ? N2 Si S 88.44(5) . . ? C1 Si S 96.67(6) . . ? N1 Si S 168.62(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 O C2 C3 C4 177.92(16) . . . . ? C7 C2 C3 C4 1.9(3) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 -1.3(3) . . . . ? C4 C5 C6 C7 1.5(3) . . . . ? O C2 C7 C6 -177.71(14) . . . . ? C3 C2 C7 C6 -1.8(2) . . . . ? C5 C6 C7 C2 0.1(3) . . . . ? N1 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 -0.7(3) . . . . ? C9 C10 C11 C12 0.5(3) . . . . ? C10 C11 C12 N1 0.1(2) . . . . ? C10 C11 C12 C13 -179.00(15) . . . . ? N1 C12 C13 N2 -2.70(17) . . . . ? C11 C12 C13 N2 176.44(14) . . . . ? N2 C14 C15 C16 -179.37(14) . . . . ? C19 C14 C15 C16 1.4(2) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C16 C17 C18 C19 0.9(3) . . . . ? C17 C18 C19 C14 0.2(2) . . . . ? C17 C18 C19 S -177.89(13) . . . . ? N2 C14 C19 C18 179.32(13) . . . . ? C15 C14 C19 C18 -1.4(2) . . . . ? N2 C14 C19 S -2.45(17) . . . . ? C15 C14 C19 S 176.88(11) . . . . ? C11 C12 N1 C8 -0.5(2) . . . . ? C13 C12 N1 C8 178.63(14) . . . . ? C11 C12 N1 Si -178.68(12) . . . . ? C13 C12 N1 Si 0.50(16) . . . . ? C9 C8 N1 C12 0.4(2) . . . . ? C9 C8 N1 Si 178.33(13) . . . . ? C15 C14 N2 C13 -0.3(2) . . . . ? C19 C14 N2 C13 179.03(12) . . . . ? C15 C14 N2 Si 176.35(11) . . . . ? C19 C14 N2 Si -4.36(18) . . . . ? C12 C13 N2 C14 -179.08(12) . . . . ? C12 C13 N2 Si 4.25(16) . . . . ? C3 C2 O Si 116.44(15) . . . . ? C7 C2 O Si -67.62(17) . . . . ? C18 C19 S Si -175.98(13) . . . . ? C14 C19 S Si 5.85(11) . . . . ? C2 O Si N2 -120.12(12) . . . . ? C2 O Si C1 71.70(13) . . . . ? C2 O Si N1 163.38(12) . . . . ? C2 O Si S -28.06(12) . . . . ? C14 N2 Si O 102.78(12) . . . . ? C13 N2 Si O -80.76(12) . . . . ? C14 N2 Si C1 -90.10(13) . . . . ? C13 N2 Si C1 86.36(13) . . . . ? C14 N2 Si N1 -179.75(12) . . . . ? C13 N2 Si N1 -3.29(11) . . . . ? C14 N2 Si S 6.79(11) . . . . ? C13 N2 Si S -176.75(11) . . . . ? C12 N1 Si O 127.06(11) . . . . ? C8 N1 Si O -50.97(13) . . . . ? C12 N1 Si N2 1.48(11) . . . . ? C8 N1 Si N2 -176.56(14) . . . . ? C12 N1 Si C1 -120.40(12) . . . . ? C8 N1 Si C1 61.56(14) . . . . ? C12 N1 Si S 36.8(3) . . . . ? C8 N1 Si S -141.3(2) . . . . ? C19 S Si O -130.23(6) . . . . ? C19 S Si N2 -6.17(6) . . . . ? C19 S Si C1 115.95(7) . . . . ? C19 S Si N1 -41.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 29.12 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.291 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.046 ##***************************** compound 9 **************** data_kob15h_9 _database_code_depnum_ccdc_archive 'CCDC 832640' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N2 S2 Si' _chemical_formula_sum 'C19 H18 N2 S2 Si' _chemical_formula_weight 366.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5524(15) _cell_length_b 16.297(3) _cell_length_c 14.284(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.34(3) _cell_angle_gamma 90.00 _cell_volume 1743.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 7.05 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22364 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 29.21 _reflns_number_total 4684 _reflns_number_gt 3714 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob15d in P2(1)/c CELL 0.71073 7.5524 16.2966 14.2838 90.000 97.338 90.000 ZERR 4.00 0.0015 0.0033 0.0029 0.000 0.030 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Si S UNIT 76 72 8 4 8 L.S. 12 ACTA BOND FMAP 2 PLAN 20 HTAB 2.5 CONF TEMP -100 WGHT 0.062400 0.521400 FVAR 0.22982 C1 1 0.703822 0.371590 0.242279 11.00000 0.03747 0.04500 = 0.03409 0.00631 0.00788 -0.00548 AFIX 137 H1A 2 0.580972 0.388262 0.220017 11.00000 -1.50000 H1B 2 0.727361 0.379018 0.310824 11.00000 -1.50000 H1C 2 0.719974 0.313724 0.226730 11.00000 -1.50000 AFIX 0 C2 1 1.226118 0.479530 0.321396 11.00000 0.02930 0.02941 = 0.02936 0.00027 -0.00002 0.00260 C3 1 1.342039 0.542201 0.302560 11.00000 0.03852 0.03999 = 0.04419 -0.00374 0.01002 -0.00644 AFIX 43 H3 2 1.375726 0.548012 0.241059 11.00000 -1.20000 AFIX 0 C4 1 1.407803 0.595784 0.373325 11.00000 0.04658 0.04808 = 0.06925 -0.01646 0.01356 -0.01721 AFIX 43 H4 2 1.485774 0.638850 0.360224 11.00000 -1.20000 AFIX 0 C5 1 1.361151 0.587185 0.462548 11.00000 0.04491 0.05656 = 0.05427 -0.02330 -0.00306 -0.00202 AFIX 43 H5 2 1.406356 0.624474 0.510895 11.00000 -1.20000 AFIX 0 C6 1 1.248889 0.524594 0.482196 11.00000 0.05368 0.05430 = 0.03076 -0.00565 -0.00062 0.00549 AFIX 43 H6 2 1.217281 0.518582 0.544105 11.00000 -1.20000 AFIX 0 C7 1 1.182007 0.470331 0.411488 11.00000 0.04647 0.03801 = 0.03088 0.00306 0.00327 -0.00275 AFIX 43 H7 2 1.105730 0.426799 0.425223 11.00000 -1.20000 AFIX 0 C8 1 0.962974 0.270899 0.107209 11.00000 0.04361 0.02987 = 0.03370 0.00101 0.00093 -0.00281 AFIX 43 H8 2 0.982988 0.252995 0.170979 11.00000 -1.20000 AFIX 0 C9 1 1.000701 0.218615 0.037216 11.00000 0.05026 0.03021 = 0.04430 -0.00662 0.00134 -0.00396 AFIX 43 H9 2 1.046733 0.165297 0.052168 11.00000 -1.20000 AFIX 0 C10 1 0.970387 0.245007 -0.056132 11.00000 0.04705 0.04010 = 0.03819 -0.01063 0.00388 -0.00604 AFIX 43 H10 2 0.998649 0.210440 -0.105686 11.00000 -1.20000 AFIX 0 C11 1 0.898864 0.321897 -0.075914 11.00000 0.03820 0.04181 = 0.02908 -0.00500 0.00150 -0.00743 AFIX 43 H11 2 0.874181 0.340348 -0.139328 11.00000 -1.20000 AFIX 0 C12 1 0.863349 0.372083 -0.001681 11.00000 0.02776 0.03463 = 0.02790 -0.00039 0.00198 -0.00782 C13 1 0.785062 0.455855 -0.013084 11.00000 0.02860 0.03849 = 0.02438 0.00239 -0.00008 -0.00560 AFIX 23 H13A 2 0.856287 0.490150 -0.051607 11.00000 -1.20000 H13B 2 0.661377 0.452743 -0.045606 11.00000 -1.20000 AFIX 0 C14 1 0.720078 0.571846 0.083716 11.00000 0.02369 0.03335 = 0.03246 0.00616 0.00155 -0.00181 C15 1 0.644966 0.616472 0.004696 11.00000 0.03100 0.03956 = 0.03458 0.00829 -0.00120 -0.00163 AFIX 43 H15 2 0.637324 0.592868 -0.056501 11.00000 -1.20000 AFIX 0 C16 1 0.581208 0.695987 0.016255 11.00000 0.03969 0.04156 = 0.04774 0.01590 -0.00207 0.00547 AFIX 43 H16 2 0.529239 0.725870 -0.037437 11.00000 -1.20000 AFIX 0 C17 1 0.592658 0.731625 0.104376 11.00000 0.04624 0.03701 = 0.05457 0.00831 0.00445 0.01136 AFIX 43 H17 2 0.548041 0.785503 0.111227 11.00000 -1.20000 AFIX 0 C18 1 0.669614 0.688505 0.183069 11.00000 0.04077 0.03734 = 0.04154 0.00163 0.00764 0.00734 AFIX 43 H18 2 0.678817 0.713106 0.243794 11.00000 -1.20000 AFIX 0 C19 1 0.733484 0.608997 0.172987 11.00000 0.02937 0.03331 = 0.03348 0.00417 0.00393 0.00259 N1 3 0.897921 0.347423 0.087993 11.00000 0.03209 0.02999 = 0.02831 -0.00146 0.00154 -0.00463 N2 3 0.785585 0.491828 0.079821 11.00000 0.02947 0.03190 = 0.02462 0.00288 0.00134 -0.00058 SI 4 0.863164 0.436288 0.183387 11.00000 0.02890 0.02989 = 0.02446 0.00320 0.00206 -0.00047 S1 5 0.843513 0.552960 0.267408 11.00000 0.04692 0.03687 = 0.02718 -0.00049 0.00104 0.01116 S2 5 1.147163 0.409229 0.230451 11.00000 0.03123 0.03270 = 0.03042 -0.00383 -0.00086 0.00233 HKLF 4 REM kob15d in P2(1)/c REM R1 = 0.0404 for 3714 Fo > 4sig(Fo) and 0.0504 for all 4684 data REM 218 parameters refined using 0 restraints END WGHT 0.0624 0.5215 REM Highest difference peak 0.338, deepest hole -0.351, 1-sigma level 0.057 Q1 1 0.7665 0.3965 0.2164 11.00000 0.05 0.34 Q2 1 0.8282 0.4711 0.1207 11.00000 0.05 0.33 Q3 1 1.1902 0.4528 0.2860 11.00000 0.05 0.32 Q4 1 1.0004 0.4087 0.2270 11.00000 0.05 0.31 Q5 1 1.0194 0.4327 0.1835 11.00000 0.05 0.31 Q6 1 0.7594 0.5164 0.2589 11.00000 0.05 0.31 Q7 1 0.8280 0.4997 0.2190 11.00000 0.05 0.29 Q8 1 0.8971 0.4913 0.2406 11.00000 0.05 0.28 Q9 1 0.8855 0.3794 0.1235 11.00000 0.05 0.27 Q10 1 0.6926 0.5985 0.0443 11.00000 0.05 0.25 Q11 1 0.8251 0.4116 -0.0145 11.00000 0.05 0.25 Q12 1 0.7909 0.5947 0.2133 11.00000 0.05 0.24 Q13 1 0.7998 0.4707 0.0383 11.00000 0.05 0.24 Q14 1 0.7384 0.5899 0.1310 11.00000 0.05 0.23 Q15 1 1.1817 0.4787 0.3612 11.00000 0.05 0.23 Q16 1 0.9418 0.2817 -0.0791 11.00000 0.05 0.22 Q17 1 0.7149 0.6390 0.1763 11.00000 0.05 0.22 Q18 1 0.9765 0.2350 -0.0035 11.00000 0.05 0.22 Q19 1 0.9754 0.5406 0.3236 11.00000 0.05 0.21 Q20 1 0.8724 0.3502 -0.0394 11.00000 0.05 0.21 ; _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^)+(0.0624P)^2^+0.5214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4684 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1134 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7038(2) 0.37159(12) 0.24228(13) 0.0386(4) Uani 1 1 d . . . H1A H 0.5810 0.3883 0.2200 0.058 Uiso 1 1 calc R . . H1B H 0.7274 0.3790 0.3108 0.058 Uiso 1 1 calc R . . H1C H 0.7200 0.3137 0.2267 0.058 Uiso 1 1 calc R . . C2 C 1.2261(2) 0.47953(10) 0.32140(11) 0.0297(3) Uani 1 1 d . . . C3 C 1.3420(2) 0.54220(12) 0.30256(15) 0.0405(4) Uani 1 1 d . . . H3 H 1.3757 0.5480 0.2411 0.049 Uiso 1 1 calc R . . C4 C 1.4078(3) 0.59578(14) 0.37332(18) 0.0541(5) Uani 1 1 d . . . H4 H 1.4858 0.6389 0.3602 0.065 Uiso 1 1 calc R . . C5 C 1.3612(3) 0.58719(14) 0.46255(17) 0.0527(5) Uani 1 1 d . . . H5 H 1.4064 0.6245 0.5109 0.063 Uiso 1 1 calc R . . C6 C 1.2489(3) 0.52459(14) 0.48220(14) 0.0468(5) Uani 1 1 d . . . H6 H 1.2173 0.5186 0.5441 0.056 Uiso 1 1 calc R . . C7 C 1.1820(3) 0.47033(12) 0.41149(13) 0.0386(4) Uani 1 1 d . . . H7 H 1.1057 0.4268 0.4252 0.046 Uiso 1 1 calc R . . C8 C 0.9630(2) 0.27090(10) 0.10721(13) 0.0361(4) Uani 1 1 d . . . H8 H 0.9830 0.2530 0.1710 0.043 Uiso 1 1 calc R . . C9 C 1.0007(3) 0.21861(11) 0.03722(14) 0.0420(4) Uani 1 1 d . . . H9 H 1.0467 0.1653 0.0522 0.050 Uiso 1 1 calc R . . C10 C 0.9704(3) 0.24501(12) -0.05613(14) 0.0419(4) Uani 1 1 d . . . H10 H 0.9986 0.2104 -0.1057 0.050 Uiso 1 1 calc R . . C11 C 0.8989(2) 0.32190(11) -0.07591(12) 0.0366(4) Uani 1 1 d . . . H11 H 0.8742 0.3403 -0.1393 0.044 Uiso 1 1 calc R . . C12 C 0.8633(2) 0.37208(10) -0.00168(11) 0.0302(3) Uani 1 1 d . . . C13 C 0.7851(2) 0.45585(10) -0.01308(11) 0.0308(3) Uani 1 1 d . . . H13A H 0.8563 0.4902 -0.0516 0.037 Uiso 1 1 calc R . . H13B H 0.6614 0.4527 -0.0456 0.037 Uiso 1 1 calc R . . C14 C 0.7201(2) 0.57185(10) 0.08372(12) 0.0300(3) Uani 1 1 d . . . C15 C 0.6450(2) 0.61647(11) 0.00470(13) 0.0355(3) Uani 1 1 d . . . H15 H 0.6373 0.5929 -0.0565 0.043 Uiso 1 1 calc R . . C16 C 0.5812(3) 0.69599(12) 0.01626(15) 0.0437(4) Uani 1 1 d . . . H16 H 0.5292 0.7259 -0.0374 0.052 Uiso 1 1 calc R . . C17 C 0.5927(3) 0.73162(12) 0.10438(16) 0.0461(4) Uani 1 1 d . . . H17 H 0.5480 0.7855 0.1112 0.055 Uiso 1 1 calc R . . C18 C 0.6696(3) 0.68851(11) 0.18307(14) 0.0397(4) Uani 1 1 d . . . H18 H 0.6788 0.7131 0.2438 0.048 Uiso 1 1 calc R . . C19 C 0.7335(2) 0.60900(10) 0.17299(12) 0.0321(3) Uani 1 1 d . . . N1 N 0.89792(18) 0.34742(8) 0.08799(10) 0.0303(3) Uani 1 1 d . . . N2 N 0.78559(17) 0.49183(8) 0.07982(9) 0.0288(3) Uani 1 1 d . . . Si Si 0.86316(6) 0.43629(3) 0.18339(3) 0.02786(11) Uani 1 1 d . . . S1 S 0.84351(6) 0.55296(3) 0.26741(3) 0.03731(12) Uani 1 1 d . . . S2 S 1.14716(5) 0.40923(3) 0.23045(3) 0.03187(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0375(8) 0.0450(9) 0.0341(8) 0.0063(7) 0.0079(7) -0.0055(7) C2 0.0293(7) 0.0294(7) 0.0294(7) 0.0003(6) 0.0000(6) 0.0026(6) C3 0.0385(9) 0.0400(9) 0.0442(10) -0.0037(8) 0.0100(7) -0.0064(7) C4 0.0466(11) 0.0481(11) 0.0692(15) -0.0165(10) 0.0136(10) -0.0172(9) C5 0.0449(10) 0.0566(12) 0.0543(12) -0.0233(10) -0.0031(9) -0.0020(9) C6 0.0537(11) 0.0543(11) 0.0308(9) -0.0056(8) -0.0006(8) 0.0055(9) C7 0.0465(9) 0.0380(9) 0.0309(8) 0.0031(7) 0.0033(7) -0.0027(7) C8 0.0436(9) 0.0299(8) 0.0337(8) 0.0010(6) 0.0009(7) -0.0028(6) C9 0.0503(10) 0.0302(8) 0.0443(10) -0.0066(7) 0.0013(8) -0.0040(7) C10 0.0471(10) 0.0401(9) 0.0382(9) -0.0106(7) 0.0039(8) -0.0060(8) C11 0.0382(8) 0.0418(9) 0.0291(8) -0.0050(7) 0.0015(6) -0.0074(7) C12 0.0278(7) 0.0346(8) 0.0279(7) -0.0004(6) 0.0020(5) -0.0078(6) C13 0.0286(7) 0.0385(8) 0.0244(7) 0.0024(6) -0.0001(5) -0.0056(6) C14 0.0237(6) 0.0333(7) 0.0325(7) 0.0062(6) 0.0015(5) -0.0018(5) C15 0.0310(7) 0.0396(8) 0.0346(8) 0.0083(7) -0.0012(6) -0.0016(6) C16 0.0397(9) 0.0416(9) 0.0477(10) 0.0159(8) -0.0021(8) 0.0055(7) C17 0.0462(10) 0.0370(9) 0.0546(12) 0.0083(8) 0.0044(9) 0.0114(8) C18 0.0408(9) 0.0373(9) 0.0415(9) 0.0016(7) 0.0076(7) 0.0073(7) C19 0.0294(7) 0.0333(8) 0.0335(8) 0.0042(6) 0.0039(6) 0.0026(6) N1 0.0321(6) 0.0300(6) 0.0283(6) -0.0015(5) 0.0015(5) -0.0046(5) N2 0.0295(6) 0.0319(6) 0.0246(6) 0.0029(5) 0.0013(5) -0.0006(5) Si 0.0289(2) 0.0299(2) 0.0245(2) 0.00320(15) 0.00206(15) -0.00047(15) S1 0.0469(2) 0.0369(2) 0.0272(2) -0.00049(15) 0.00104(17) 0.01116(17) S2 0.03123(19) 0.0327(2) 0.0304(2) -0.00383(14) -0.00086(14) 0.00233(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si 1.8778(18) . ? C2 C7 1.378(2) . ? C2 C3 1.394(2) . ? C2 S2 1.7770(16) . ? C3 C4 1.379(3) . ? C4 C5 1.372(4) . ? C5 C6 1.378(3) . ? C6 C7 1.388(3) . ? C8 N1 1.356(2) . ? C8 C9 1.371(3) . ? C9 C10 1.392(3) . ? C10 C11 1.379(3) . ? C11 C12 1.392(2) . ? C12 N1 1.336(2) . ? C12 C13 1.488(2) . ? C13 N2 1.450(2) . ? C14 N2 1.398(2) . ? C14 C15 1.400(2) . ? C14 C19 1.403(2) . ? C15 C16 1.399(3) . ? C16 C17 1.379(3) . ? C17 C18 1.389(3) . ? C18 C19 1.396(2) . ? C19 S1 1.7485(17) . ? N1 Si 2.0284(15) . ? N2 Si 1.7690(14) . ? Si S2 2.2087(8) . ? Si S1 2.2634(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 C2 C3 119.52(16) . . ? C7 C2 S2 120.93(13) . . ? C3 C2 S2 119.46(13) . . ? C4 C3 C2 119.92(19) . . ? C5 C4 C3 120.3(2) . . ? C4 C5 C6 120.16(19) . . ? C5 C6 C7 119.97(19) . . ? C2 C7 C6 120.08(18) . . ? N1 C8 C9 121.86(17) . . ? C8 C9 C10 118.85(18) . . ? C11 C10 C9 119.28(18) . . ? C10 C11 C12 119.09(17) . . ? N1 C12 C11 121.36(16) . . ? N1 C12 C13 114.02(14) . . ? C11 C12 C13 124.61(15) . . ? N2 C13 C12 108.42(13) . . ? N2 C14 C15 124.14(16) . . ? N2 C14 C19 116.97(14) . . ? C15 C14 C19 118.88(16) . . ? C16 C15 C14 119.72(18) . . ? C17 C16 C15 121.02(17) . . ? C16 C17 C18 119.79(18) . . ? C17 C18 C19 120.03(18) . . ? C18 C19 C14 120.54(16) . . ? C18 C19 S1 122.78(14) . . ? C14 C19 S1 116.59(12) . . ? C12 N1 C8 119.49(15) . . ? C12 N1 Si 113.77(11) . . ? C8 N1 Si 126.55(12) . . ? C14 N2 C13 116.98(13) . . ? C14 N2 Si 121.66(11) . . ? C13 N2 Si 121.35(11) . . ? N2 Si C1 119.94(8) . . ? N2 Si N1 82.01(6) . . ? C1 Si N1 92.60(8) . . ? N2 Si S2 124.17(5) . . ? C1 Si S2 113.86(6) . . ? N1 Si S2 81.83(5) . . ? N2 Si S1 88.65(5) . . ? C1 Si S1 98.34(7) . . ? N1 Si S1 168.19(5) . . ? S2 Si S1 97.66(3) . . ? C19 S1 Si 94.97(6) . . ? C2 S2 Si 108.42(6) . . ? 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 C7 C2 C3 C4 -1.8(3) . . . . ? S2 C2 C3 C4 -178.30(16) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C4 C5 C6 C7 -0.3(3) . . . . ? C3 C2 C7 C6 1.8(3) . . . . ? S2 C2 C7 C6 178.27(15) . . . . ? C5 C6 C7 C2 -0.7(3) . . . . ? N1 C8 C9 C10 -0.3(3) . . . . ? C8 C9 C10 C11 -1.8(3) . . . . ? C9 C10 C11 C12 1.8(3) . . . . ? C10 C11 C12 N1 0.3(2) . . . . ? C10 C11 C12 C13 -179.46(16) . . . . ? N1 C12 C13 N2 6.10(18) . . . . ? C11 C12 C13 N2 -174.09(15) . . . . ? N2 C14 C15 C16 179.24(16) . . . . ? C19 C14 C15 C16 -1.5(2) . . . . ? C14 C15 C16 C17 0.6(3) . . . . ? C15 C16 C17 C18 0.5(3) . . . . ? C16 C17 C18 C19 -0.7(3) . . . . ? C17 C18 C19 C14 -0.2(3) . . . . ? C17 C18 C19 S1 176.21(15) . . . . ? N2 C14 C19 C18 -179.37(15) . . . . ? C15 C14 C19 C18 1.3(2) . . . . ? N2 C14 C19 S1 3.96(19) . . . . ? C15 C14 C19 S1 -175.35(12) . . . . ? C11 C12 N1 C8 -2.4(2) . . . . ? C13 C12 N1 C8 177.43(14) . . . . ? C11 C12 N1 Si 172.90(12) . . . . ? C13 C12 N1 Si -7.29(17) . . . . ? C9 C8 N1 C12 2.4(3) . . . . ? C9 C8 N1 Si -172.25(14) . . . . ? C15 C14 N2 C13 4.1(2) . . . . ? C19 C14 N2 C13 -175.14(14) . . . . ? C15 C14 N2 Si -175.10(12) . . . . ? C19 C14 N2 Si 5.62(19) . . . . ? C12 C13 N2 C14 178.68(12) . . . . ? C12 C13 N2 Si -2.07(17) . . . . ? C14 N2 Si C1 89.50(14) . . . . ? C13 N2 Si C1 -89.71(14) . . . . ? C14 N2 Si N1 177.90(13) . . . . ? C13 N2 Si N1 -1.31(12) . . . . ? C14 N2 Si S2 -107.69(12) . . . . ? C13 N2 Si S2 73.10(13) . . . . ? C14 N2 Si S1 -9.35(12) . . . . ? C13 N2 Si S1 171.44(12) . . . . ? C12 N1 Si N2 4.95(11) . . . . ? C8 N1 Si N2 179.84(15) . . . . ? C12 N1 Si C1 124.83(12) . . . . ? C8 N1 Si C1 -60.28(15) . . . . ? C12 N1 Si S2 -121.43(11) . . . . ? C8 N1 Si S2 53.46(14) . . . . ? C12 N1 Si S1 -33.1(3) . . . . ? C8 N1 Si S1 141.81(19) . . . . ? C18 C19 S1 Si 174.81(14) . . . . ? C14 C19 S1 Si -8.60(13) . . . . ? N2 Si S1 C19 8.80(7) . . . . ? C1 Si S1 C19 -111.27(8) . . . . ? N1 Si S1 C19 46.4(2) . . . . ? S2 Si S1 C19 133.12(6) . . . . ? C7 C2 S2 Si 75.95(14) . . . . ? C3 C2 S2 Si -107.55(14) . . . . ? N2 Si S2 C2 100.89(8) . . . . ? C1 Si S2 C2 -95.37(9) . . . . ? N1 Si S2 C2 175.40(7) . . . . ? S1 Si S2 C2 7.31(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.338 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.057 ##************************** compound 10 **************** data_kob17cabsu_10 _database_code_depnum_ccdc_archive 'CCDC 832641' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N2 S Se Si' _chemical_formula_sum 'C19 H18 N2 S Se Si' _chemical_formula_weight 413.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5484(12) _cell_length_b 16.447(4) _cell_length_c 14.428(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.973(19) _cell_angle_gamma 90.00 _cell_volume 1773.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.9 _cell_measurement_theta_max 27.55 _exptl_crystal_description irregular_piece _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 2.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3469 _exptl_absorpt_correction_T_max 0.4146 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24275 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 29.18 _reflns_number_total 4716 _reflns_number_gt 3849 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDs _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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. TITL kob17b in P2(1)/c CELL 0.71073 7.5484 16.4467 14.4277 90.000 97.973 90.000 ZERR 4.0 0.0012 0.0035 0.0024 0.000 0.019 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N Si S Se UNIT 76 72 8 4 4 4 L.S. 8 ACTA BOND FMAP 2 PLAN 20 CONF HTAB 2.5 TEMP -100 WGHT 0.052100 0.044500 FVAR 0.28291 C1 1 0.789816 0.636612 0.259968 11.00000 0.03047 0.04371 = 0.02838 0.00520 0.00583 -0.00502 AFIX 137 H1A 2 0.765790 0.693960 0.271829 11.00000 -1.50000 H1B 2 0.771745 0.626511 0.192373 11.00000 -1.50000 H1C 2 0.913639 0.623642 0.285662 11.00000 -1.50000 AFIX 0 C2 1 0.257784 0.516213 0.169422 11.00000 0.02632 0.02874 = 0.02505 -0.00118 -0.00116 0.00071 C3 1 0.302347 0.523529 0.079999 11.00000 0.05369 0.03662 = 0.02717 0.00154 0.00413 -0.00265 AFIX 43 H3 2 0.375172 0.567501 0.065302 11.00000 -1.20000 AFIX 0 C4 1 0.241206 0.466958 0.011649 11.00000 0.06163 0.05828 = 0.02810 -0.01013 0.00127 0.00465 AFIX 43 H4 2 0.271936 0.472305 -0.049721 11.00000 -1.20000 AFIX 0 C5 1 0.136582 0.403433 0.032682 11.00000 0.04828 0.05890 = 0.06088 -0.03134 -0.00237 -0.00307 AFIX 43 H5 2 0.095233 0.364571 -0.014070 11.00000 -1.20000 AFIX 0 C6 1 0.091098 0.395730 0.121543 11.00000 0.05430 0.05309 = 0.07833 -0.02389 0.01971 -0.02493 AFIX 43 H6 2 0.018556 0.351486 0.135750 11.00000 -1.20000 AFIX 0 C7 1 0.150480 0.452106 0.190345 11.00000 0.04101 0.04499 = 0.04656 -0.00679 0.01352 -0.01260 AFIX 43 H7 2 0.117961 0.446894 0.251360 11.00000 -1.20000 AFIX 0 C8 1 0.525351 0.734042 0.391316 11.00000 0.03778 0.02898 = 0.03020 -0.00022 0.00132 -0.00238 AFIX 43 H8 2 0.506918 0.751776 0.328045 11.00000 -1.20000 AFIX 0 C9 1 0.483229 0.785294 0.459914 11.00000 0.04565 0.02911 = 0.03832 -0.00838 0.00209 -0.00077 AFIX 43 H9 2 0.434931 0.837684 0.444460 11.00000 -1.20000 AFIX 0 C10 1 0.512610 0.759115 0.553313 11.00000 0.04255 0.03869 = 0.03278 -0.01333 0.00518 -0.00465 AFIX 43 H10 2 0.481854 0.793219 0.601780 11.00000 -1.20000 AFIX 0 C11 1 0.586327 0.683655 0.574225 11.00000 0.03471 0.03971 = 0.02470 -0.00767 0.00302 -0.00670 AFIX 43 H11 2 0.609897 0.665473 0.637229 11.00000 -1.20000 AFIX 0 C12 1 0.625681 0.634479 0.501174 11.00000 0.02347 0.03311 = 0.02213 -0.00143 0.00171 -0.00711 C13 1 0.706596 0.551823 0.513693 11.00000 0.02403 0.03354 = 0.01962 0.00169 0.00046 -0.00371 AFIX 23 H13A 2 0.829439 0.555560 0.547888 11.00000 -1.20000 H13B 2 0.634504 0.517162 0.550318 11.00000 -1.20000 AFIX 0 C14 1 0.779169 0.437946 0.418280 11.00000 0.01930 0.03019 = 0.02724 0.00440 0.00215 -0.00232 C15 1 0.854416 0.394073 0.497332 11.00000 0.02682 0.03561 = 0.02950 0.00778 -0.00129 -0.00295 AFIX 43 H15 2 0.860435 0.417581 0.557833 11.00000 -1.20000 AFIX 0 C16 1 0.920375 0.315949 0.487094 11.00000 0.03526 0.03591 = 0.04281 0.01370 -0.00318 0.00030 AFIX 43 H16 2 0.971635 0.286462 0.540817 11.00000 -1.20000 AFIX 0 C17 1 0.911880 0.280785 0.399075 11.00000 0.04241 0.03112 = 0.05088 0.00494 0.00145 0.00843 AFIX 43 H17 2 0.958520 0.227741 0.392690 11.00000 -1.20000 AFIX 0 C18 1 0.835341 0.323115 0.320588 11.00000 0.03630 0.03308 = 0.03739 0.00007 0.00420 0.00508 AFIX 43 H18 2 0.828416 0.298789 0.260472 11.00000 -1.20000 AFIX 0 C19 1 0.768624 0.401105 0.329542 11.00000 0.02532 0.03179 = 0.02945 0.00355 0.00355 0.00128 N2 3 0.710671 0.516782 0.421383 11.00000 0.02610 0.02966 = 0.01935 0.00172 0.00161 0.00021 N1 3 0.592861 0.658449 0.411529 11.00000 0.02586 0.02744 = 0.02371 -0.00214 0.00233 -0.00371 S 5 0.658895 0.456029 0.234303 11.00000 0.04782 0.03689 = 0.02246 -0.00191 0.00012 0.01505 SE 6 0.330700 0.596373 0.263822 11.00000 0.02644 0.03119 = 0.02590 -0.00380 0.00017 0.00246 SI 4 0.633187 0.570917 0.317543 11.00000 0.02496 0.02774 = 0.01899 0.00213 0.00229 0.00083 HKLF 4 REM kob17b in P2(1)/c REM R1 = 0.0294 for 3849 Fo > 4sig(Fo) and 0.0401 for all 4716 data REM 218 parameters refined using 0 restraints END WGHT 0.0521 0.0445 REM Highest difference peak 0.566, deepest hole -0.327, 1-sigma level 0.070 Q1 1 0.4838 0.5897 0.2756 11.00000 0.05 0.57 Q2 1 0.7337 0.4845 0.2364 11.00000 0.05 0.45 Q3 1 0.6785 0.5391 0.3844 11.00000 0.05 0.36 Q4 1 0.6767 0.5958 0.5151 11.00000 0.05 0.34 Q5 1 0.7969 0.4076 0.4559 11.00000 0.05 0.34 Q6 1 0.5479 0.6961 0.4099 11.00000 0.05 0.34 Q7 1 0.6022 0.6596 0.5384 11.00000 0.05 0.33 Q8 1 0.7052 0.6186 0.2793 11.00000 0.05 0.33 Q9 1 0.5000 0.7708 0.5005 11.00000 0.05 0.31 Q10 1 0.7725 0.3599 0.3207 11.00000 0.05 0.30 Q11 1 0.6711 0.5174 0.2601 11.00000 0.05 0.30 Q12 1 0.8676 0.3103 0.3601 11.00000 0.05 0.29 Q13 1 0.7191 0.4106 0.2924 11.00000 0.05 0.28 Q14 1 0.6159 0.4610 0.2362 11.00000 0.05 0.28 Q15 1 0.4683 0.7492 0.4223 11.00000 0.05 0.28 Q16 1 0.2842 0.5461 0.1993 11.00000 0.05 0.28 Q17 1 0.1786 0.6119 0.2619 11.00000 0.05 0.28 Q18 1 0.4440 0.6409 0.2384 11.00000 0.05 0.28 Q19 1 0.3957 0.5978 0.3423 11.00000 0.05 0.27 Q20 1 0.3422 0.6669 0.2530 11.00000 0.05 0.27 ; _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^)+(0.0521P)^2^+0.0445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4716 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7898(3) 0.63661(14) 0.25997(14) 0.0340(4) Uani 1 1 d . . . H1A H 0.7658 0.6940 0.2718 0.051 Uiso 1 1 calc R . . H1B H 0.7717 0.6265 0.1924 0.051 Uiso 1 1 calc R . . H1C H 0.9136 0.6236 0.2857 0.051 Uiso 1 1 calc R . . C2 C 0.2578(3) 0.51621(12) 0.16942(13) 0.0271(4) Uani 1 1 d . . . C3 C 0.3023(3) 0.52353(14) 0.08000(14) 0.0393(5) Uani 1 1 d . . . H3 H 0.3752 0.5675 0.0653 0.047 Uiso 1 1 calc R . . C4 C 0.2412(4) 0.46696(17) 0.01165(16) 0.0498(6) Uani 1 1 d . . . H4 H 0.2719 0.4723 -0.0497 0.060 Uiso 1 1 calc R . . C5 C 0.1366(4) 0.40343(18) 0.0327(2) 0.0570(7) Uani 1 1 d . . . H5 H 0.0952 0.3646 -0.0141 0.068 Uiso 1 1 calc R . . C6 C 0.0911(4) 0.39573(18) 0.1215(2) 0.0609(8) Uani 1 1 d . . . H6 H 0.0186 0.3515 0.1358 0.073 Uiso 1 1 calc R . . C7 C 0.1505(3) 0.45211(15) 0.19034(18) 0.0435(5) Uani 1 1 d . . . H7 H 0.1180 0.4469 0.2514 0.052 Uiso 1 1 calc R . . C8 C 0.5254(3) 0.73404(12) 0.39132(14) 0.0326(4) Uani 1 1 d . . . H8 H 0.5069 0.7518 0.3280 0.039 Uiso 1 1 calc R . . C9 C 0.4832(3) 0.78529(13) 0.45991(16) 0.0380(5) Uani 1 1 d . . . H9 H 0.4349 0.8377 0.4445 0.046 Uiso 1 1 calc R . . C10 C 0.5126(3) 0.75912(14) 0.55331(15) 0.0380(5) Uani 1 1 d . . . H10 H 0.4819 0.7932 0.6018 0.046 Uiso 1 1 calc R . . C11 C 0.5863(3) 0.68366(13) 0.57423(14) 0.0331(4) Uani 1 1 d . . . H11 H 0.6099 0.6655 0.6372 0.040 Uiso 1 1 calc R . . C12 C 0.6257(2) 0.63448(12) 0.50117(12) 0.0264(4) Uani 1 1 d . . . C13 C 0.7066(3) 0.55182(11) 0.51369(12) 0.0260(4) Uani 1 1 d . . . H13A H 0.8294 0.5556 0.5479 0.031 Uiso 1 1 calc R . . H13B H 0.6345 0.5172 0.5503 0.031 Uiso 1 1 calc R . . C14 C 0.7792(2) 0.43795(11) 0.41828(13) 0.0257(3) Uani 1 1 d . . . C15 C 0.8544(3) 0.39407(12) 0.49733(14) 0.0311(4) Uani 1 1 d . . . H15 H 0.8604 0.4176 0.5578 0.037 Uiso 1 1 calc R . . C16 C 0.9204(3) 0.31595(14) 0.48709(16) 0.0388(5) Uani 1 1 d . . . H16 H 0.9716 0.2865 0.5408 0.047 Uiso 1 1 calc R . . C17 C 0.9119(3) 0.28078(13) 0.39907(18) 0.0419(5) Uani 1 1 d . . . H17 H 0.9585 0.2277 0.3927 0.050 Uiso 1 1 calc R . . C18 C 0.8353(3) 0.32311(13) 0.32059(16) 0.0357(4) Uani 1 1 d . . . H18 H 0.8284 0.2988 0.2605 0.043 Uiso 1 1 calc R . . C19 C 0.7686(3) 0.40111(12) 0.32954(14) 0.0289(4) Uani 1 1 d . . . N2 N 0.7107(2) 0.51678(10) 0.42138(10) 0.0252(3) Uani 1 1 d . . . N1 N 0.5929(2) 0.65845(9) 0.41153(11) 0.0258(3) Uani 1 1 d . . . S S 0.65889(8) 0.45603(3) 0.23430(3) 0.03617(13) Uani 1 1 d . . . Se Se 0.33070(3) 0.596373(12) 0.263822(13) 0.02817(7) Uani 1 1 d . . . Si Si 0.63319(7) 0.57092(3) 0.31754(3) 0.02397(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0305(10) 0.0437(12) 0.0284(9) 0.0052(8) 0.0058(8) -0.0050(8) C2 0.0263(9) 0.0287(9) 0.0250(8) -0.0012(7) -0.0012(7) 0.0007(7) C3 0.0537(14) 0.0366(11) 0.0272(10) 0.0015(8) 0.0041(9) -0.0027(10) C4 0.0616(17) 0.0583(15) 0.0281(10) -0.0101(10) 0.0013(11) 0.0046(12) C5 0.0483(16) 0.0589(16) 0.0609(17) -0.0313(13) -0.0024(13) -0.0031(12) C6 0.0543(17) 0.0531(16) 0.078(2) -0.0239(14) 0.0197(16) -0.0249(13) C7 0.0410(13) 0.0450(13) 0.0466(13) -0.0068(10) 0.0135(10) -0.0126(10) C8 0.0378(11) 0.0290(9) 0.0302(9) -0.0002(7) 0.0013(8) -0.0024(8) C9 0.0457(13) 0.0291(10) 0.0383(11) -0.0084(8) 0.0021(10) -0.0008(8) C10 0.0426(12) 0.0387(11) 0.0328(10) -0.0133(8) 0.0052(9) -0.0046(9) C11 0.0347(11) 0.0397(11) 0.0247(9) -0.0077(8) 0.0030(8) -0.0067(8) C12 0.0235(9) 0.0331(9) 0.0221(8) -0.0014(7) 0.0017(7) -0.0071(7) C13 0.0240(9) 0.0335(9) 0.0196(8) 0.0017(6) 0.0005(7) -0.0037(7) C14 0.0193(8) 0.0302(9) 0.0272(8) 0.0044(7) 0.0022(7) -0.0023(7) C15 0.0268(10) 0.0356(10) 0.0295(9) 0.0078(7) -0.0013(8) -0.0029(7) C16 0.0353(12) 0.0359(11) 0.0428(11) 0.0137(9) -0.0032(9) 0.0003(9) C17 0.0424(13) 0.0311(11) 0.0509(13) 0.0049(9) 0.0014(11) 0.0084(9) C18 0.0363(11) 0.0331(10) 0.0374(10) 0.0001(8) 0.0042(9) 0.0051(8) C19 0.0253(9) 0.0318(9) 0.0294(9) 0.0035(7) 0.0036(7) 0.0013(7) N2 0.0261(8) 0.0297(8) 0.0194(7) 0.0017(6) 0.0016(6) 0.0002(6) N1 0.0259(8) 0.0274(7) 0.0237(7) -0.0021(6) 0.0023(6) -0.0037(6) S 0.0478(3) 0.0369(3) 0.0225(2) -0.00191(18) 0.0001(2) 0.0150(2) Se 0.02644(11) 0.03119(10) 0.02590(10) -0.00380(7) 0.00017(7) 0.00246(7) Si 0.0250(3) 0.0277(2) 0.0190(2) 0.00213(18) 0.00229(18) 0.00083(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si 1.878(2) . ? C2 C3 1.383(3) . ? C2 C7 1.388(3) . ? C2 Se 1.9204(19) . ? C3 C4 1.387(3) . ? C4 C5 1.369(4) . ? C5 C6 1.378(5) . ? C6 C7 1.387(4) . ? C8 N1 1.360(3) . ? C8 C9 1.371(3) . ? C9 C10 1.403(3) . ? C10 C11 1.376(3) . ? C11 C12 1.393(3) . ? C12 N1 1.342(2) . ? C12 C13 1.491(3) . ? C13 N2 1.455(2) . ? C14 N2 1.399(2) . ? C14 C15 1.402(3) . ? C14 C19 1.409(3) . ? C15 C16 1.393(3) . ? C16 C17 1.389(3) . ? C17 C18 1.385(3) . ? C18 C19 1.391(3) . ? C19 S 1.753(2) . ? N2 Si 1.7709(16) . ? N1 Si 2.0294(16) . ? S Si 2.2616(8) . ? Se Si 2.3449(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C7 119.6(2) . . ? C3 C2 Se 121.27(16) . . ? C7 C2 Se 119.06(15) . . ? C2 C3 C4 120.3(2) . . ? C5 C4 C3 120.0(2) . . ? C4 C5 C6 120.1(2) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C2 119.5(2) . . ? N1 C8 C9 121.67(19) . . ? C8 C9 C10 118.9(2) . . ? C11 C10 C9 119.51(19) . . ? C10 C11 C12 118.68(19) . . ? N1 C12 C11 121.90(19) . . ? N1 C12 C13 113.73(16) . . ? C11 C12 C13 124.37(17) . . ? N2 C13 C12 108.09(15) . . ? N2 C14 C15 124.13(17) . . ? N2 C14 C19 116.95(16) . . ? C15 C14 C19 118.92(18) . . ? C16 C15 C14 119.9(2) . . ? C17 C16 C15 120.6(2) . . ? C18 C17 C16 120.0(2) . . ? C17 C18 C19 120.2(2) . . ? C18 C19 C14 120.38(18) . . ? C18 C19 S 122.70(16) . . ? C14 C19 S 116.85(14) . . ? C14 N2 C13 116.82(15) . . ? C14 N2 Si 121.27(12) . . ? C13 N2 Si 121.91(13) . . ? C12 N1 C8 119.27(16) . . ? C12 N1 Si 114.26(13) . . ? C8 N1 Si 126.28(13) . . ? C19 S Si 94.60(7) . . ? C2 Se Si 106.38(6) . . ? N2 Si C1 120.60(9) . . ? N2 Si N1 81.60(7) . . ? C1 Si N1 92.83(8) . . ? N2 Si S 89.23(6) . . ? C1 Si S 98.06(7) . . ? N1 Si S 168.34(5) . . ? N2 Si Se 124.16(6) . . ? C1 Si Se 113.26(7) . . ? N1 Si Se 82.23(5) . . ? S Si Se 97.18(3) . . ? 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 C7 C2 C3 C4 -0.4(4) . . . . ? Se C2 C3 C4 -176.96(19) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 0.3(5) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 C2 -0.6(5) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? Se C2 C7 C6 177.4(2) . . . . ? N1 C8 C9 C10 0.7(3) . . . . ? C8 C9 C10 C11 1.4(3) . . . . ? C9 C10 C11 C12 -1.6(3) . . . . ? C10 C11 C12 N1 -0.4(3) . . . . ? C10 C11 C12 C13 179.61(19) . . . . ? N1 C12 C13 N2 -5.6(2) . . . . ? C11 C12 C13 N2 174.41(17) . . . . ? N2 C14 C15 C16 -179.55(18) . . . . ? C19 C14 C15 C16 1.2(3) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C15 C16 C17 C18 -0.8(4) . . . . ? C16 C17 C18 C19 0.7(4) . . . . ? C17 C18 C19 C14 0.4(3) . . . . ? C17 C18 C19 S -176.34(18) . . . . ? N2 C14 C19 C18 179.39(18) . . . . ? C15 C14 C19 C18 -1.3(3) . . . . ? N2 C14 C19 S -3.7(2) . . . . ? C15 C14 C19 S 175.57(14) . . . . ? C15 C14 N2 C13 -4.7(3) . . . . ? C19 C14 N2 C13 174.49(16) . . . . ? C15 C14 N2 Si 175.18(15) . . . . ? C19 C14 N2 Si -5.6(2) . . . . ? C12 C13 N2 C14 -178.72(15) . . . . ? C12 C13 N2 Si 1.4(2) . . . . ? C11 C12 N1 C8 2.5(3) . . . . ? C13 C12 N1 C8 -177.52(17) . . . . ? C11 C12 N1 Si -172.81(14) . . . . ? C13 C12 N1 Si 7.2(2) . . . . ? C9 C8 N1 C12 -2.6(3) . . . . ? C9 C8 N1 Si 172.02(16) . . . . ? C18 C19 S Si -174.90(17) . . . . ? C14 C19 S Si 8.28(15) . . . . ? C3 C2 Se Si -77.74(18) . . . . ? C7 C2 Se Si 105.66(18) . . . . ? C14 N2 Si C1 -89.74(17) . . . . ? C13 N2 Si C1 90.18(16) . . . . ? C14 N2 Si N1 -178.06(15) . . . . ? C13 N2 Si N1 1.86(14) . . . . ? C14 N2 Si S 9.17(14) . . . . ? C13 N2 Si S -170.91(14) . . . . ? C14 N2 Si Se 107.33(13) . . . . ? C13 N2 Si Se -72.75(15) . . . . ? C12 N1 Si N2 -5.19(13) . . . . ? C8 N1 Si N2 179.92(17) . . . . ? C12 N1 Si C1 -125.72(15) . . . . ? C8 N1 Si C1 59.40(18) . . . . ? C12 N1 Si S 33.3(4) . . . . ? C8 N1 Si S -141.6(2) . . . . ? C12 N1 Si Se 121.18(13) . . . . ? C8 N1 Si Se -53.70(16) . . . . ? C19 S Si N2 -8.56(8) . . . . ? C19 S Si C1 112.26(10) . . . . ? C19 S Si N1 -46.6(3) . . . . ? C19 S Si Se -132.92(7) . . . . ? C2 Se Si N2 -99.06(9) . . . . ? C2 Se Si C1 96.90(10) . . . . ? C2 Se Si N1 -173.35(7) . . . . ? C2 Se Si S -5.09(6) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 29.18 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.566 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.070 ##*********************** compound 11 ************ data_kob20k_11 _database_code_depnum_ccdc_archive 'CCDC 832642' #TrackingRef '- Kobelt Crystaldata.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N2 S Si Te' _chemical_formula_sum 'C19 H18 N2 S Si Te' _chemical_formula_weight 462.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 18.327(2) _cell_length_b 18.327(2) _cell_length_c 18.327(2) _cell_angle_alpha 116.627(17) _cell_angle_beta 116.627(17) _cell_angle_gamma 116.627(17) _cell_volume 2869.9(6) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.3 _cell_measurement_theta_max 26.8 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max .5 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 1.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4685 _exptl_absorpt_correction_T_max 0.7051 _exptl_special_details ; TITL kob20b in R-3 CELL 0.71073 18.3271 18.3271 18.3271 116.627 116.627 116.627 ZERR 6 0.0021 0.0021 0.0021 0.017 0.017 0.017 LATT 1 SYMM +Z,+X,+Y SYMM +Y,+Z,+X SFAC C H N Si S Te UNIT 114 108 12 6 6 6 L.S. 20 PLAN 20 ACTA TEMP -100 BOND CONF HTAB 2.5 FMAP 2 LIST 3 REM E:/xray_daten/daten51/kobelt/kob20a/kob20k.hkl WGHT 0.009500 9.544300 FVAR 0.45258 0.94430 0.03908 PART 1 C1 1 0.744673 0.225153 -0.191167 21.00000 0.06422 0.08574 = 0.06411 0.06542 0.05429 0.06595 AFIX 137 H1A 2 0.770108 0.215979 -0.228288 21.00000 -1.50000 H1B 2 0.799758 0.320230 -0.120847 21.00000 -1.50000 H1C 2 0.644855 0.157669 -0.267530 21.00000 -1.50000 AFIX 0 C2 1 0.626435 -0.094088 -0.301337 21.00000 0.04157 0.04017 = 0.03659 0.02879 0.03210 0.02974 C3 1 0.539925 -0.232257 -0.399015 21.00000 0.05078 0.03953 = 0.04018 0.02825 0.03659 0.02907 AFIX 43 H3 2 0.442062 -0.304825 -0.468772 21.00000 -1.20000 AFIX 0 C4 1 0.595074 -0.265117 -0.395590 21.00000 0.08139 0.04430 = 0.06462 0.04420 0.06449 0.04752 AFIX 43 H4 2 0.534284 -0.360359 -0.464851 21.00000 -1.20000 AFIX 0 C5 1 0.738126 -0.160729 -0.292249 21.00000 0.08205 0.05515 = 0.07621 0.05674 0.07148 0.05865 AFIX 43 H5 2 0.775563 -0.183869 -0.289648 21.00000 -1.20000 AFIX 0 C6 1 0.826171 -0.021350 -0.192251 21.00000 0.05532 0.04528 = 0.05357 0.04236 0.04789 0.04238 AFIX 43 H6 2 0.924295 0.050640 -0.120563 21.00000 -1.20000 AFIX 0 C7 1 0.772356 0.014124 -0.195811 21.00000 0.04420 0.03980 = 0.03827 0.03231 0.03588 0.03392 C8 1 1.004005 0.261060 0.009162 21.00000 0.03441 0.03893 = 0.03922 0.03213 0.03062 0.03101 AFIX 23 H8A 2 1.027156 0.253813 -0.030932 21.00000 -1.20000 H8B 2 1.037922 0.252849 0.060474 21.00000 -1.20000 AFIX 0 C9 1 1.071980 0.397762 0.105873 21.00000 0.03641 0.04024 = 0.03897 0.03382 0.03273 0.03202 C10 1 1.214435 0.526958 0.224884 21.00000 0.03873 0.04271 = 0.04308 0.03321 0.03273 0.03201 AFIX 43 H10 2 1.277390 0.533734 0.250077 21.00000 -1.20000 AFIX 0 C11 1 1.264401 0.646598 0.307100 21.00000 0.04587 0.03982 = 0.04807 0.03368 0.03807 0.03109 AFIX 43 H11 2 1.362083 0.736545 0.389868 21.00000 -1.20000 AFIX 0 C12 1 1.169513 0.633006 0.266661 21.00000 0.06398 0.04454 = 0.06077 0.04403 0.05479 0.04459 AFIX 43 H12 2 1.201495 0.713660 0.321559 21.00000 -1.20000 AFIX 0 C13 1 1.029348 0.502118 0.146814 21.00000 0.05599 0.04947 = 0.06083 0.04864 0.05190 0.04596 AFIX 43 H13 2 0.964304 0.492758 0.118596 21.00000 -1.20000 AFIX 0 C14 1 0.931286 0.415632 0.221847 21.00000 0.04676 0.04643 = 0.04865 0.04132 0.04179 0.03907 C15 1 1.040346 0.449504 0.297771 21.00000 0.05834 0.06722 = 0.05942 0.05626 0.05099 0.05371 AFIX 43 H15 2 1.024024 0.379260 0.254579 21.00000 -1.20000 AFIX 0 C16 1 1.171688 0.584086 0.435011 21.00000 0.06269 0.09333 = 0.05986 0.06525 0.05221 0.06299 AFIX 43 H16 2 1.246108 0.606872 0.485459 21.00000 -1.20000 AFIX 0 C17 1 1.195512 0.686181 0.499588 21.00000 0.05670 0.06657 = 0.04792 0.03945 0.04340 0.03813 AFIX 43 H17 2 1.286690 0.779422 0.593714 21.00000 -1.20000 AFIX 0 C18 1 1.086883 0.652763 0.427398 21.00000 0.07453 0.05002 = 0.06715 0.04582 0.06157 0.04762 AFIX 43 H18 2 1.102679 0.722241 0.473011 21.00000 -1.20000 AFIX 0 C19 1 0.954086 0.517180 0.287665 21.00000 0.05987 0.05264 = 0.05969 0.04725 0.05244 0.04823 AFIX 43 H19 2 0.879531 0.494315 0.237677 21.00000 -1.20000 AFIX 0 N1 3 0.981728 0.386282 0.068040 21.00000 0.03988 0.04205 = 0.04434 0.03740 0.03613 0.03510 N2 3 0.854141 0.150616 -0.101455 21.00000 0.03384 0.03828 = 0.03708 0.02989 0.02912 0.02994 SI 4 0.781532 0.189967 -0.108717 21.00000 0.03636 0.04459 = 0.04019 0.03474 0.03154 0.03435 S 5 0.564788 -0.043577 -0.303968 21.00000 0.03343 0.04870 = 0.04356 0.02762 0.02593 0.02980 TE 6 0.734013 0.210438 0.006130 21.00000 0.04382 0.04502 = 0.05338 0.03927 0.04226 0.03604 PART 0 PART 2 AFIX 9 C1B 1 0.898621 0.379626 -0.036426 -21.00000 31.00000 AFIX 137 H1BA 2 0.798188 0.309118 -0.117292 -21.00000 -1.50000 H1BB 2 0.949236 0.451175 -0.019386 -21.00000 -1.50000 H1BC 2 0.931517 0.423412 0.046234 -21.00000 -1.50000 AFIX 5 C2B 1 1.175682 0.427176 0.178011 -21.00000 31.00000 C3B 1 1.298115 0.501607 0.298210 -21.00000 31.00000 AFIX 43 H3B 2 1.385005 0.591583 0.359240 -21.00000 -1.20000 AFIX 5 C4B 1 1.296190 0.446943 0.331270 -21.00000 31.00000 AFIX 43 H4B 2 1.379652 0.503634 0.420427 -21.00000 -1.20000 AFIX 0 C5B 1 1.180571 0.318687 0.240485 -21.00000 31.00000 AFIX 43 H5B 2 1.183966 0.276105 0.255189 -21.00000 -1.20000 AFIX 5 C6B 1 1.047792 0.237633 0.119022 -21.00000 31.00000 AFIX 43 H6B 2 0.963369 0.149958 0.063262 -21.00000 -1.20000 AFIX 5 C7B 1 1.046507 0.291959 0.085110 -21.00000 31.00000 C8B 1 0.795997 0.082892 -0.129309 -21.00000 31.00000 AFIX 23 H8BA 2 0.778845 0.085664 -0.084616 -21.00000 -1.20000 H8BB 2 0.799362 0.025267 -0.155522 -21.00000 -1.20000 AFIX 5 C9B 1 0.681956 0.020916 -0.255781 -21.00000 31.00000 C10B 1 0.543636 -0.111010 -0.369599 -21.00000 31.00000 AFIX 43 H10A 2 0.513415 -0.170705 -0.371803 -21.00000 -1.20000 AFIX 5 C11B 1 0.448442 -0.156128 -0.481462 -21.00000 31.00000 AFIX 43 H11A 2 0.351901 -0.247817 -0.562490 -21.00000 -1.20000 AFIX 5 C12B 1 0.496593 -0.065091 -0.473020 -21.00000 31.00000 AFIX 43 H12A 2 0.433220 -0.093468 -0.548323 -21.00000 -1.20000 AFIX 5 C13B 1 0.635177 0.065161 -0.356226 -21.00000 31.00000 AFIX 43 H13A 2 0.667778 0.127670 -0.350484 -21.00000 -1.20000 AFIX 5 C14B 1 0.772610 0.068537 -0.406830 -21.00000 31.00000 C15B 1 0.711572 -0.045281 -0.448228 -21.00000 31.00000 AFIX 43 H15A 2 0.762065 -0.031187 -0.381671 -21.00000 -1.20000 AFIX 5 C16B 1 0.579095 -0.178135 -0.584157 -21.00000 31.00000 AFIX 43 H16A 2 0.537077 -0.255758 -0.611418 -21.00000 -1.20000 AFIX 5 C17B 1 0.507151 -0.198772 -0.680989 -21.00000 31.00000 AFIX 43 H17A 2 0.414615 -0.290944 -0.775023 -21.00000 -1.20000 AFIX 5 C18B 1 0.567502 -0.087564 -0.643417 -21.00000 31.00000 AFIX 43 H18A 2 0.518165 -0.103058 -0.711744 -21.00000 -1.20000 AFIX 5 C19B 1 0.700939 0.047481 -0.505068 -21.00000 31.00000 AFIX 43 H19A 2 0.742884 0.125044 -0.477900 -21.00000 -1.20000 AFIX 5 N1B 3 0.726965 0.107591 -0.248972 -21.00000 31.00000 N2B 3 0.926039 0.221851 -0.033778 -21.00000 31.00000 SI1B 4 0.930815 0.294346 -0.072260 -21.00000 31.00000 S1B 5 1.166843 0.491825 0.132989 -21.00000 31.00000 TE1B 6 0.971053 0.272170 -0.192901 -21.00000 0.04167 HKLF 4 REM kob20b in R-3 REM R1 = 0.0471 for 4170 Fo > 4sig(Fo) and 0.0574 for all 5129 data REM 232 parameters refined using 0 restraints END WGHT 0.0093 9.5498 REM Highest difference peak 0.698, deepest hole -1.064, 1-sigma level 0.092 Q1 1 1.0116 0.3333 -0.1315 11.00000 0.05 0.70 Q2 1 0.7796 0.2166 -0.0303 11.00000 0.05 0.63 Q3 1 0.7576 0.2038 -0.0476 11.00000 0.05 0.57 Q4 1 0.8576 0.3301 0.1179 11.00000 0.05 0.56 Q5 1 0.6214 0.1575 -0.0600 11.00000 0.05 0.54 Q6 1 1.0428 0.3285 -0.1027 11.00000 0.05 0.53 Q7 1 0.9180 0.2007 -0.2612 11.00000 0.05 0.53 Q8 1 0.7556 0.2541 0.0195 11.00000 0.05 0.50 Q9 1 0.8249 0.3249 0.1262 11.00000 0.05 0.50 Q10 1 0.8055 0.2504 -0.0018 11.00000 0.05 0.49 Q11 1 0.8080 0.3012 0.0306 11.00000 0.05 0.48 Q12 1 0.7428 0.1422 -0.0386 11.00000 0.05 0.48 Q13 1 0.6046 0.1112 -0.1106 11.00000 0.05 0.48 Q14 1 0.9305 0.2802 -0.2312 11.00000 0.05 0.47 Q15 1 0.8301 0.2427 0.0410 11.00000 0.05 0.45 Q16 1 0.8996 0.2280 -0.2964 11.00000 0.05 0.45 Q17 1 0.6828 0.1531 -0.0514 11.00000 0.05 0.45 Q18 1 0.9893 0.3410 -0.1798 11.00000 0.05 0.44 Q19 1 0.6991 0.1486 -0.0967 11.00000 0.05 0.43 Q20 1 0.7912 0.3100 0.0409 11.00000 0.05 0.41 ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45772 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 29.21 _reflns_number_total 5129 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/POVRAY _computing_publication_material Bruker-SHELXTL _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^)+(0.0095P)^2^+9.5443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5129 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7447(6) 0.2252(6) -0.1912(6) 0.0584(12) Uani 0.9443(15) 1 d P A 1 H1A H 0.7701 0.2160 -0.2283 0.088 Uiso 0.9443(15) 1 calc PR A 1 H1B H 0.7998 0.3202 -0.1208 0.088 Uiso 0.9443(15) 1 calc PR A 1 H1C H 0.6449 0.1577 -0.2675 0.088 Uiso 0.9443(15) 1 calc PR A 1 C2 C 0.6264(4) -0.0941(4) -0.3013(4) 0.0455(10) Uani 0.9443(15) 1 d P A 1 C3 C 0.5399(5) -0.2323(5) -0.3990(5) 0.0568(12) Uani 0.9443(15) 1 d P A 1 H3 H 0.4421 -0.3048 -0.4688 0.068 Uiso 0.9443(15) 1 calc PR A 1 C4 C 0.5951(6) -0.2651(5) -0.3956(6) 0.0616(14) Uani 0.9443(15) 1 d P A 1 H4 H 0.5343 -0.3604 -0.4649 0.074 Uiso 0.9443(15) 1 calc PR A 1 C5 C 0.7381(6) -0.1607(5) -0.2922(6) 0.0563(12) Uani 0.9443(15) 1 d P A 1 H5 H 0.7756 -0.1839 -0.2896 0.068 Uiso 0.9443(15) 1 calc PR A 1 C6 C 0.8262(5) -0.0213(5) -0.1923(5) 0.0432(9) Uani 0.9443(15) 1 d P A 1 H6 H 0.9243 0.0506 -0.1206 0.052 Uiso 0.9443(15) 1 calc PR A 1 C7 C 0.7724(4) 0.0141(4) -0.1958(4) 0.0377(8) Uani 0.9443(15) 1 d P A 1 C8 C 1.0040(4) 0.2611(4) 0.0092(4) 0.0349(7) Uani 0.9443(15) 1 d P A 1 H8A H 1.0272 0.2538 -0.0309 0.042 Uiso 0.9443(15) 1 calc PR A 1 H8B H 1.0379 0.2528 0.0605 0.042 Uiso 0.9443(15) 1 calc PR A 1 C9 C 1.0720(4) 0.3978(4) 0.1059(4) 0.0334(7) Uani 0.9443(15) 1 d P A 1 C10 C 1.2144(4) 0.5270(4) 0.2249(4) 0.0450(9) Uani 0.9443(15) 1 d P A 1 H10 H 1.2774 0.5337 0.2501 0.054 Uiso 0.9443(15) 1 calc PR A 1 C11 C 1.2644(5) 0.6466(5) 0.3071(5) 0.0509(11) Uani 0.9443(15) 1 d P A 1 H11 H 1.3621 0.7365 0.3899 0.061 Uiso 0.9443(15) 1 calc PR A 1 C12 C 1.1695(5) 0.6330(5) 0.2667(5) 0.0499(11) Uani 0.9443(15) 1 d P A 1 H12 H 1.2015 0.7137 0.3216 0.060 Uiso 0.9443(15) 1 calc PR A 1 C13 C 1.0293(5) 0.5021(4) 0.1468(5) 0.0428(9) Uani 0.9443(15) 1 d P A 1 H13 H 0.9643 0.4928 0.1186 0.051 Uiso 0.9443(15) 1 calc PR A 1 C14 C 0.9313(4) 0.4156(4) 0.2218(4) 0.0396(8) Uani 0.9443(15) 1 d P A 1 C15 C 1.0403(5) 0.4495(5) 0.2978(5) 0.0499(10) Uani 0.9443(15) 1 d P A 1 H15 H 1.0240 0.3793 0.2546 0.060 Uiso 0.9443(15) 1 calc PR A 1 C16 C 1.1717(6) 0.5841(7) 0.4350(6) 0.0663(15) Uani 0.9443(15) 1 d P A 1 H16 H 1.2461 0.6069 0.4855 0.080 Uiso 0.9443(15) 1 calc PR A 1 C17 C 1.1955(6) 0.6862(7) 0.4996(6) 0.0769(19) Uani 0.9443(15) 1 d P A 1 H17 H 1.2867 0.7794 0.5937 0.092 Uiso 0.9443(15) 1 calc PR A 1 C18 C 1.0869(6) 0.6528(6) 0.4274(6) 0.0647(14) Uani 0.9443(15) 1 d P A 1 H18 H 1.1027 0.7222 0.4730 0.078 Uiso 0.9443(15) 1 calc PR A 1 C19 C 0.9541(5) 0.5172(5) 0.2877(5) 0.0486(10) Uani 0.9443(15) 1 d P A 1 H19 H 0.8795 0.4943 0.2377 0.058 Uiso 0.9443(15) 1 calc PR A 1 N1 N 0.9817(3) 0.3863(3) 0.0680(3) 0.0354(7) Uani 0.9443(15) 1 d P A 1 N2 N 0.8541(3) 0.1506(3) -0.1015(3) 0.0361(7) Uani 0.9443(15) 1 d P A 1 Si Si 0.78153(11) 0.18997(12) -0.10872(12) 0.0379(2) Uani 0.9443(15) 1 d P A 1 S S 0.56479(12) -0.04358(13) -0.30397(13) 0.0625(4) Uani 0.9443(15) 1 d P A 1 Te Te 0.73401(3) 0.21044(3) 0.00613(4) 0.04514(11) Uani 0.9443(15) 1 d P A 1 C1B C 0.8986(15) 0.3796(15) -0.0364(14) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H1BA H 0.7982 0.3091 -0.1173 0.059 Uiso 0.0557(15) 1 calc PR A 2 H1BB H 0.9492 0.4512 -0.0194 0.059 Uiso 0.0557(15) 1 calc PR A 2 H1BC H 0.9315 0.4234 0.0462 0.059 Uiso 0.0557(15) 1 calc PR A 2 C2B C 1.1757(14) 0.4272(15) 0.1780(14) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 C3B C 1.2981(18) 0.5016(19) 0.2982(18) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H3B H 1.3850 0.5916 0.3592 0.047 Uiso 0.0557(15) 1 calc PR A 2 C4B C 1.296(2) 0.447(2) 0.331(2) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H4B H 1.3797 0.5036 0.4204 0.047 Uiso 0.0557(15) 1 calc PR A 2 C5B C 1.181(7) 0.319(7) 0.240(7) 0.039(3) Uiso 0.0557(15) 1 d P A 2 H5B H 1.1840 0.2761 0.2552 0.047 Uiso 0.0557(15) 1 calc PR A 2 C6B C 1.048(2) 0.2376(19) 0.1190(19) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H6B H 0.9634 0.1500 0.0633 0.047 Uiso 0.0557(15) 1 calc PR A 2 C7B C 1.0465(15) 0.2920(15) 0.0851(14) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 C8B C 0.7960(15) 0.0829(15) -0.1293(15) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H8BA H 0.7788 0.0857 -0.0846 0.047 Uiso 0.0557(15) 1 calc PR A 2 H8BB H 0.7994 0.0253 -0.1555 0.047 Uiso 0.0557(15) 1 calc PR A 2 C9B C 0.6820(14) 0.0209(15) -0.2558(14) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 C10B C 0.5436(18) -0.1110(19) -0.3696(18) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H10A H 0.5134 -0.1707 -0.3718 0.047 Uiso 0.0557(15) 1 calc PR A 2 C11B C 0.4484(19) -0.156(2) -0.4815(19) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H11A H 0.3519 -0.2478 -0.5625 0.047 Uiso 0.0557(15) 1 calc PR A 2 C12B C 0.4966(16) -0.065(2) -0.4730(18) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H12A H 0.4332 -0.0935 -0.5483 0.047 Uiso 0.0557(15) 1 calc PR A 2 C13B C 0.6352(13) 0.0652(16) -0.3562(14) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H13A H 0.6678 0.1277 -0.3505 0.047 Uiso 0.0557(15) 1 calc PR A 2 C14B C 0.7726(10) 0.0685(10) -0.4068(10) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 C15B C 0.7116(13) -0.0453(12) -0.4482(12) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H15A H 0.7621 -0.0312 -0.3817 0.047 Uiso 0.0557(15) 1 calc PR A 2 C16B C 0.5791(17) -0.1781(16) -0.5842(17) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H16A H 0.5371 -0.2558 -0.6114 0.047 Uiso 0.0557(15) 1 calc PR A 2 C17B C 0.5072(18) -0.1988(19) -0.6810(18) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H17A H 0.4146 -0.2909 -0.7750 0.047 Uiso 0.0557(15) 1 calc PR A 2 C18B C 0.5675(16) -0.0876(18) -0.6434(17) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H18A H 0.5182 -0.1031 -0.7117 0.047 Uiso 0.0557(15) 1 calc PR A 2 C19B C 0.7009(12) 0.0475(14) -0.5051(13) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 H19A H 0.7429 0.1250 -0.4779 0.047 Uiso 0.0557(15) 1 calc PR A 2 N1B N 0.7270(11) 0.1076(13) -0.2490(12) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 N2B N 0.9260(12) 0.2219(12) -0.0338(12) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 Si1B Si 0.9308(8) 0.2943(9) -0.0723(8) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 S1B S 1.1668(11) 0.4918(11) 0.1330(10) 0.039(3) Uiso 0.0557(15) 1 d PG A 2 Te1B Te 0.9711(5) 0.2722(6) -0.1929(6) 0.0417(16) Uiso 0.0557(15) 1 d PG A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.064(3) 0.086(4) 0.064(3) 0.065(3) 0.054(3) 0.066(3) C2 0.042(2) 0.040(2) 0.037(2) 0.0288(19) 0.0321(19) 0.0297(19) C3 0.051(3) 0.040(2) 0.040(2) 0.028(2) 0.037(2) 0.029(2) C4 0.081(4) 0.044(2) 0.065(3) 0.044(3) 0.064(3) 0.048(3) C5 0.082(4) 0.055(3) 0.076(3) 0.057(3) 0.071(3) 0.059(3) C6 0.055(2) 0.045(2) 0.054(2) 0.042(2) 0.048(2) 0.042(2) C7 0.044(2) 0.0398(19) 0.0383(19) 0.0323(18) 0.0359(18) 0.0339(18) C8 0.0344(18) 0.0389(19) 0.0392(19) 0.0321(17) 0.0306(17) 0.0310(17) C9 0.0364(18) 0.0402(19) 0.0390(18) 0.0338(17) 0.0327(17) 0.0320(17) C10 0.039(2) 0.043(2) 0.043(2) 0.033(2) 0.0327(19) 0.0320(19) C11 0.046(2) 0.040(2) 0.048(2) 0.034(2) 0.038(2) 0.031(2) C12 0.064(3) 0.045(2) 0.061(3) 0.044(2) 0.055(3) 0.045(2) C13 0.056(2) 0.049(2) 0.061(3) 0.049(2) 0.052(2) 0.046(2) C14 0.047(2) 0.046(2) 0.049(2) 0.041(2) 0.042(2) 0.039(2) C15 0.058(3) 0.067(3) 0.059(3) 0.056(3) 0.051(3) 0.054(3) C16 0.063(3) 0.093(4) 0.060(3) 0.065(3) 0.052(3) 0.063(3) C17 0.057(3) 0.067(4) 0.048(3) 0.039(3) 0.043(3) 0.038(3) C18 0.075(4) 0.050(3) 0.067(3) 0.046(3) 0.062(3) 0.048(3) C19 0.060(3) 0.053(2) 0.060(3) 0.047(2) 0.052(3) 0.048(2) N1 0.0399(16) 0.0421(17) 0.0443(17) 0.0374(16) 0.0361(16) 0.0351(15) N2 0.0338(15) 0.0383(16) 0.0371(16) 0.0299(15) 0.0291(15) 0.0299(15) Si 0.0364(5) 0.0446(6) 0.0402(6) 0.0347(5) 0.0315(5) 0.0343(5) S 0.0334(5) 0.0487(6) 0.0436(6) 0.0276(6) 0.0259(5) 0.0298(5) Te 0.04382(15) 0.04502(16) 0.05338(18) 0.03927(15) 0.04226(15) 0.03604(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 Si 1.872(5) . ? C2 C3 1.387(7) . ? C2 C7 1.413(6) . ? C2 S 1.751(5) . ? C3 C4 1.382(8) . ? C4 C5 1.388(8) . ? C5 C6 1.395(6) . ? C6 C7 1.398(6) . ? C7 N2 1.390(5) . ? C8 N2 1.449(5) . ? C8 C9 1.488(5) . ? C9 N1 1.338(5) . ? C9 C10 1.380(6) . ? C10 C11 1.385(6) . ? C11 C12 1.388(7) . ? C12 C13 1.369(7) . ? C13 N1 1.347(5) . ? C14 C19 1.390(6) . ? C14 C15 1.392(6) . ? C14 Te 2.125(7) . ? C15 C16 1.376(8) . ? C16 C17 1.383(9) . ? C17 C18 1.382(9) . ? C18 C19 1.394(8) . ? N1 Si 1.992(6) . ? N2 Si 1.760(3) . ? Si S 2.279(6) . ? Si Te 2.5608(12) . ? C1B Si1B 1.864(6) . ? C2B C3B 1.371(5) . ? C2B C7B 1.411(5) . ? C2B S1B 1.743(6) . ? C3B C4B 1.380(4) . ? C4B C5B 1.29(8) . ? C5B C6B 1.42(7) . ? C6B C7B 1.393(4) . ? C7B N2B 1.382(5) . ? C8B N2B 1.433(5) . ? C8B C9B 1.483(5) . ? C9B N1B 1.332(4) . ? C9B C10B 1.367(6) . ? C10B C11B 1.383(5) . ? C11B C12B 1.383(4) . ? C12B C13B 1.358(5) . ? C13B N1B 1.339(4) . ? C14B C15B 1.381(4) . ? C14B C19B 1.385(5) . ? C14B Te1B 2.113(9) . ? C15B C16B 1.368(6) . ? C16B C17B 1.373(5) . ? C17B C18B 1.375(5) . ? C18B C19B 1.388(5) . ? N1B Si1B 1.979(8) . ? N2B Si1B 1.750(6) . ? Si1B S1B 2.267(9) . ? Si1B Te1B 2.554(8) . ? 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 C3 C2 C7 119.8(5) . . ? C3 C2 S 123.6(4) . . ? C7 C2 S 116.6(3) . . ? C4 C3 C2 120.5(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C6 119.1(5) . . ? C5 C6 C7 121.1(5) . . ? N2 C7 C6 123.8(4) . . ? N2 C7 C2 117.5(4) . . ? C6 C7 C2 118.7(4) . . ? N2 C8 C9 108.2(3) . . ? N1 C9 C10 121.2(4) . . ? N1 C9 C8 113.8(3) . . ? C10 C9 C8 124.9(4) . . ? C9 C10 C11 119.1(4) . . ? C10 C11 C12 119.0(4) . . ? C13 C12 C11 119.3(4) . . ? N1 C13 C12 121.4(4) . . ? C19 C14 C15 119.5(5) . . ? C19 C14 Te 121.3(3) . . ? C15 C14 Te 119.3(3) . . ? C16 C15 C14 120.4(5) . . ? C15 C16 C17 120.1(5) . . ? C18 C17 C16 120.1(6) . . ? C17 C18 C19 120.1(5) . . ? C14 C19 C18 119.7(5) . . ? C9 N1 C13 120.0(4) . . ? C9 N1 Si 114.2(3) . . ? C13 N1 Si 125.7(3) . . ? C7 N2 C8 117.0(3) . . ? C7 N2 Si 122.0(3) . . ? C8 N2 Si 120.9(3) . . ? N2 Si C1 122.2(2) . . ? N2 Si N1 82.78(14) . . ? C1 Si N1 90.9(2) . . ? N2 Si S 89.10(12) . . ? C1 Si S 96.1(2) . . ? N1 Si S 171.28(12) . . ? N2 Si Te 119.23(12) . . ? C1 Si Te 118.56(17) . . ? N1 Si Te 94.22(11) . . ? S Si Te 86.97(7) . . ? C2 S Si 94.70(15) . . ? C14 Te Si 104.51(11) . . ? C3B C2B C7B 120.0 . . ? C3B C2B S1B 123.9 . . ? C7B C2B S1B 116.1 . . ? C2B C3B C4B 120.57(10) . . ? C5B C4B C3B 119(3) . . ? C4B C5B C6B 123(6) . . ? C7B C6B C5B 117(3) . . ? N2B C7B C6B 124.0 . . ? N2B C7B C2B 117.8 . . ? C6B C7B C2B 118.3 . . ? N2B C8B C9B 108.7 . . ? N1B C9B C10B 121.8 . . ? N1B C9B C8B 113.2 . . ? C10B C9B C8B 125.0 . . ? C9B C10B C11B 118.9 . . ? C10B C11B C12B 118.7 . . ? C13B C12B C11B 119.4 . . ? N1B C13B C12B 121.6 . . ? C15B C14B C19B 119.6 . . ? C15B C14B Te1B 119.1 . . ? C19B C14B Te1B 121.2 . . ? C16B C15B C14B 120.6 . . ? C15B C16B C17B 119.7 . . ? C16B C17B C18B 120.7 . . ? C17B C18B C19B 119.6 . . ? C14B C19B C18B 119.6 . . ? C9B N1B C13B 119.6 . . ? C9B N1B Si1B 114.5 . . ? C13B N1B Si1B 125.9 . . ? C7B N2B C8B 117.1 . . ? C7B N2B Si1B 122.0 . . ? C8B N2B Si1B 120.8 . . ? N2B Si1B C1B 122.3 . . ? N2B Si1B N1B 82.7 . . ? C1B Si1B N1B 90.6 . . ? N2B Si1B S1B 89.1 . . ? C1B Si1B S1B 96.5 . . ? N1B Si1B S1B 171.2 . . ? N2B Si1B Te1B 119.0 . . ? C1B Si1B Te1B 118.6 . . ? N1B Si1B Te1B 94.2 . . ? S1B Si1B Te1B 86.9 . . ? C2B S1B Si1B 94.9 . . ? C14B Te1B Si1B 104.5 . . ? 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 C7 C2 C3 C4 -1.3(7) . . . . ? S C2 C3 C4 176.1(4) . . . . ? C2 C3 C4 C5 1.9(7) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? C4 C5 C6 C7 -0.8(7) . . . . ? C5 C6 C7 N2 -178.3(4) . . . . ? C5 C6 C7 C2 1.4(6) . . . . ? C3 C2 C7 N2 179.3(4) . . . . ? S C2 C7 N2 1.8(5) . . . . ? C3 C2 C7 C6 -0.3(6) . . . . ? S C2 C7 C6 -177.9(3) . . . . ? N2 C8 C9 N1 -0.7(4) . . . . ? N2 C8 C9 C10 179.2(4) . . . . ? N1 C9 C10 C11 0.7(6) . . . . ? C8 C9 C10 C11 -179.2(4) . . . . ? C9 C10 C11 C12 -0.5(7) . . . . ? C10 C11 C12 C13 -0.1(7) . . . . ? C11 C12 C13 N1 0.6(7) . . . . ? C19 C14 C15 C16 -3.2(6) . . . . ? Te C14 C15 C16 175.6(4) . . . . ? C14 C15 C16 C17 1.5(7) . . . . ? C15 C16 C17 C18 1.3(8) . . . . ? C16 C17 C18 C19 -2.3(8) . . . . ? C15 C14 C19 C18 2.2(6) . . . . ? Te C14 C19 C18 -176.6(3) . . . . ? C17 C18 C19 C14 0.6(7) . . . . ? C10 C9 N1 C13 -0.2(6) . . . . ? C8 C9 N1 C13 179.7(3) . . . . ? C10 C9 N1 Si 179.1(3) . . . . ? C8 C9 N1 Si -1.0(4) . . . . ? C12 C13 N1 C9 -0.5(6) . . . . ? C12 C13 N1 Si -179.6(3) . . . . ? C6 C7 N2 C8 -2.4(5) . . . . ? C2 C7 N2 C8 177.9(3) . . . . ? C6 C7 N2 Si -178.9(3) . . . . ? C2 C7 N2 Si 1.4(5) . . . . ? C9 C8 N2 C7 -174.1(3) . . . . ? C9 C8 N2 Si 2.5(4) . . . . ? C7 N2 Si C1 -99.5(4) . . . . ? C8 N2 Si C1 84.0(4) . . . . ? C7 N2 Si N1 174.0(3) . . . . ? C8 N2 Si N1 -2.5(3) . . . . ? C7 N2 Si S -2.9(3) . . . . ? C8 N2 Si S -179.3(3) . . . . ? C7 N2 Si Te 83.1(3) . . . . ? C8 N2 Si Te -93.3(3) . . . . ? C9 N1 Si N2 1.9(3) . . . . ? C13 N1 Si N2 -178.9(3) . . . . ? C9 N1 Si C1 -120.4(3) . . . . ? C13 N1 Si C1 58.8(4) . . . . ? C9 N1 Si S 23.4(9) . . . . ? C13 N1 Si S -157.4(6) . . . . ? C9 N1 Si Te 120.9(3) . . . . ? C13 N1 Si Te -59.9(3) . . . . ? C3 C2 S Si 179.5(4) . . . . ? C7 C2 S Si -3.1(3) . . . . ? N2 Si S C2 2.95(19) . . . . ? C1 Si S C2 125.2(2) . . . . ? N1 Si S C2 -18.3(8) . . . . ? Te Si S C2 -116.38(15) . . . . ? C19 C14 Te Si 113.7(3) . . . . ? C15 C14 Te Si -65.0(3) . . . . ? N2 Si Te C14 81.11(18) . . . . ? C1 Si Te C14 -96.3(2) . . . . ? N1 Si Te C14 -2.97(15) . . . . ? S Si Te C14 168.37(13) . . . . ? C7B C2B C3B C4B -1.7 . . . . ? S1B C2B C3B C4B 175.7 . . . . ? C2B C3B C4B C5B 9(4) . . . . ? C3B C4B C5B C6B -14(8) . . . . ? C4B C5B C6B C7B 12(7) . . . . ? C5B C6B C7B N2B 176(3) . . . . ? C5B C6B C7B C2B -5(3) . . . . ? C3B C2B C7B N2B 179.3 . . . . ? S1B C2B C7B N2B 1.7 . . . . ? C3B C2B C7B C6B -0.2 . . . . ? S1B C2B C7B C6B -177.8 . . . . ? N2B C8B C9B N1B -0.7 . . . . ? N2B C8B C9B C10B 179.5 . . . . ? N1B C9B C10B C11B 1.0 . . . . ? C8B C9B C10B C11B -179.1 . . . . ? C9B C10B C11B C12B -1.0 . . . . ? C10B C11B C12B C13B 0.3 . . . . ? C11B C12B C13B N1B 0.5 . . . . ? C19B C14B C15B C16B -2.5 . . . . ? Te1B C14B C15B C16B 175.3 . . . . ? C14B C15B C16B C17B 1.3 . . . . ? C15B C16B C17B C18B 1.0 . . . . ? C16B C17B C18B C19B -2.1 . . . . ? C15B C14B C19B C18B 1.3 . . . . ? Te1B C14B C19B C18B -176.4 . . . . ? C17B C18B C19B C14B 1.0 . . . . ? C10B C9B N1B C13B -0.3 . . . . ? C8B C9B N1B C13B 179.8 . . . . ? C10B C9B N1B Si1B 178.7 . . . . ? C8B C9B N1B Si1B -1.2 . . . . ? C12B C13B N1B C9B -0.5 . . . . ? C12B C13B N1B Si1B -179.4 . . . . ? C6B C7B N2B C8B -2.5 . . . . ? C2B C7B N2B C8B 178.0 . . . . ? C6B C7B N2B Si1B -179.1 . . . . ? C2B C7B N2B Si1B 1.4 . . . . ? C9B C8B N2B C7B -174.1 . . . . ? C9B C8B N2B Si1B 2.6 . . . . ? C7B N2B Si1B C1B -100.0 . . . . ? C8B N2B Si1B C1B 83.5 . . . . ? C7B N2B Si1B N1B 173.9 . . . . ? C8B N2B Si1B N1B -2.6 . . . . ? C7B N2B Si1B S1B -2.8 . . . . ? C8B N2B Si1B S1B -179.3 . . . . ? C7B N2B Si1B Te1B 83.2 . . . . ? C8B N2B Si1B Te1B -93.3 . . . . ? C9B N1B Si1B N2B 2.1 . . . . ? C13B N1B Si1B N2B -179.0 . . . . ? C9B N1B Si1B C1B -120.4 . . . . ? C13B N1B Si1B C1B 58.5 . . . . ? C9B N1B Si1B S1B 23.9 . . . . ? C13B N1B Si1B S1B -157.1 . . . . ? C9B N1B Si1B Te1B 120.8 . . . . ? C13B N1B Si1B Te1B -60.2 . . . . ? C3B C2B S1B Si1B 179.5 . . . . ? C7B C2B S1B Si1B -3.0 . . . . ? N2B Si1B S1B C2B 2.9 . . . . ? C1B Si1B S1B C2B 125.3 . . . . ? N1B Si1B S1B C2B -18.8 . . . . ? Te1B Si1B S1B C2B -116.2 . . . . ? C15B C14B Te1B Si1B -64.0 . . . . ? C19B C14B Te1B Si1B 113.8 . . . . ? N2B Si1B Te1B C14B 81.0 . . . . ? C1B Si1B Te1B C14B -96.0 . . . . ? N1B Si1B Te1B C14B -3.0 . . . . ? S1B Si1B Te1B C14B 168.3 . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.21 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.698 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.092 # Attachment '- kob21abs.cif' data_kob21abs _database_code_depnum_ccdc_archive 'CCDC 845196' #TrackingRef '- kob21abs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H10 Cl F5 N2 S Si' _chemical_formula_sum 'C18 H10 Cl F5 N2 S Si' _chemical_formula_weight 444.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.7449(10) _cell_length_b 15.308(2) _cell_length_c 15.082(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.831(15) _cell_angle_gamma 90.00 _cell_volume 1767.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5.85 _cell_measurement_theta_max 26.65 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max .6 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8180 _exptl_absorpt_correction_T_max 0.8858 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate_Stoe-IPDS _diffrn_measurement_method omega_scan _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23304 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 29.07 _reflns_number_total 4706 _reflns_number_gt 3784 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Ortep/Povray _computing_publication_material Bruker-SHELXTL _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^)+(0.0522P)^2^+0.4979P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4706 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0912 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.90263(19) 0.10152(9) 0.80481(9) 0.0240(3) Uani 1 1 d . . . C2 C 0.7840(2) 0.10762(10) 0.86463(10) 0.0267(3) Uani 1 1 d . . . C3 C 0.8315(2) 0.11008(11) 0.95729(10) 0.0308(3) Uani 1 1 d . . . C4 C 1.0066(2) 0.10473(10) 0.99323(10) 0.0310(3) Uani 1 1 d . . . C5 C 1.1296(2) 0.09592(10) 0.93683(11) 0.0308(3) Uani 1 1 d . . . C6 C 1.0767(2) 0.09497(10) 0.84442(10) 0.0265(3) Uani 1 1 d . . . C7 C 0.7358(2) -0.09099(10) 0.62752(10) 0.0275(3) Uani 1 1 d . . . C8 C 0.7187(2) -0.18039(11) 0.60958(11) 0.0346(4) Uani 1 1 d . . . H7 H 0.8196 -0.2165 0.6159 0.041 Uiso 1 1 calc R . . C9 C 0.5543(3) -0.21675(11) 0.58256(11) 0.0368(4) Uani 1 1 d . . . H8 H 0.5426 -0.2776 0.5710 0.044 Uiso 1 1 calc R . . C10 C 0.4075(2) -0.16348(11) 0.57259(11) 0.0335(3) Uani 1 1 d . . . H9 H 0.2955 -0.1883 0.5539 0.040 Uiso 1 1 calc R . . C11 C 0.4224(2) -0.07372(10) 0.58975(9) 0.0267(3) Uani 1 1 d . . . H10 H 0.3210 -0.0379 0.5821 0.032 Uiso 1 1 calc R . . C12 C 0.58664(19) -0.03696(9) 0.61812(9) 0.0230(3) Uani 1 1 d . . . C13 C 0.46289(18) 0.10855(9) 0.62939(9) 0.0230(3) Uani 1 1 d . . . H12A H 0.3798 0.0883 0.6688 0.028 Uiso 1 1 calc R . . H12B H 0.4027 0.1076 0.5665 0.028 Uiso 1 1 calc R . . C14 C 0.52396(18) 0.19917(9) 0.65502(9) 0.0230(3) Uani 1 1 d . . . C15 C 0.4162(2) 0.27207(10) 0.65469(10) 0.0288(3) Uani 1 1 d . . . H14 H 0.2937 0.2670 0.6361 0.035 Uiso 1 1 calc R . . C16 C 0.4901(2) 0.35199(10) 0.68178(10) 0.0310(3) Uani 1 1 d . . . H15 H 0.4189 0.4025 0.6820 0.037 Uiso 1 1 calc R . . C17 C 0.6701(2) 0.35741(10) 0.70864(10) 0.0302(3) Uani 1 1 d . . . H16 H 0.7232 0.4116 0.7277 0.036 Uiso 1 1 calc R . . C18 C 0.7699(2) 0.28321(10) 0.70717(10) 0.0274(3) Uani 1 1 d . . . H17 H 0.8926 0.2868 0.7253 0.033 Uiso 1 1 calc R . . Si Si 0.82315(5) 0.09282(3) 0.67783(2) 0.02219(10) Uani 1 1 d . . . Cl Cl 0.99827(5) 0.15676(3) 0.60441(3) 0.03432(11) Uani 1 1 d . . . F1 F 0.61065(12) 0.10958(7) 0.83363(6) 0.0358(2) Uani 1 1 d . . . F2 F 0.71054(16) 0.11602(8) 1.01158(7) 0.0458(3) Uani 1 1 d . . . F3 F 1.05536(16) 0.10543(7) 1.08257(6) 0.0422(3) Uani 1 1 d . . . F4 F 1.29881(14) 0.08737(8) 0.97181(7) 0.0435(3) Uani 1 1 d . . . F5 F 1.20296(12) 0.08557(7) 0.79305(7) 0.0378(2) Uani 1 1 d . . . N2 N 0.61509(15) 0.05188(8) 0.63916(8) 0.0224(2) Uani 1 1 d . . . N1 N 0.69723(16) 0.20500(8) 0.68040(8) 0.0225(2) Uani 1 1 d . . . S S 0.93709(5) -0.03912(3) 0.66021(3) 0.03745(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0249(7) 0.0227(6) 0.0232(6) 0.0005(5) -0.0003(5) 0.0010(5) C2 0.0267(7) 0.0271(7) 0.0255(7) 0.0002(5) 0.0012(5) 0.0048(6) C3 0.0395(9) 0.0297(8) 0.0241(7) 0.0011(5) 0.0074(6) 0.0056(6) C4 0.0445(9) 0.0234(7) 0.0221(6) 0.0015(5) -0.0044(6) -0.0019(6) C5 0.0304(8) 0.0267(7) 0.0315(7) 0.0049(6) -0.0071(6) -0.0054(6) C6 0.0247(7) 0.0262(7) 0.0279(7) 0.0012(5) 0.0015(5) -0.0020(6) C7 0.0304(8) 0.0275(7) 0.0237(6) -0.0009(5) 0.0014(5) 0.0029(6) C8 0.0431(9) 0.0271(8) 0.0328(8) -0.0017(6) 0.0035(7) 0.0054(7) C9 0.0530(11) 0.0238(7) 0.0339(8) -0.0007(6) 0.0070(7) -0.0042(7) C10 0.0405(9) 0.0303(8) 0.0303(7) -0.0011(6) 0.0068(6) -0.0108(7) C11 0.0286(7) 0.0283(7) 0.0234(6) 0.0008(5) 0.0049(5) -0.0035(6) C12 0.0268(7) 0.0228(6) 0.0192(6) 0.0003(5) 0.0031(5) -0.0014(5) C13 0.0182(6) 0.0251(7) 0.0252(6) 0.0002(5) 0.0017(5) 0.0010(5) C14 0.0216(6) 0.0269(7) 0.0201(6) 0.0013(5) 0.0023(5) 0.0010(5) C15 0.0258(7) 0.0292(7) 0.0303(7) -0.0002(6) 0.0007(6) 0.0042(6) C16 0.0366(8) 0.0263(7) 0.0291(7) -0.0011(5) 0.0024(6) 0.0053(6) C17 0.0384(9) 0.0245(7) 0.0268(7) -0.0015(5) 0.0013(6) -0.0031(6) C18 0.0273(7) 0.0281(7) 0.0259(6) 0.0004(5) 0.0008(5) -0.0043(6) Si 0.01780(18) 0.0261(2) 0.02212(18) -0.00137(14) 0.00116(13) 0.00045(14) Cl 0.02421(18) 0.0461(2) 0.03406(19) 0.00423(15) 0.00888(14) -0.00160(15) F1 0.0242(5) 0.0553(6) 0.0282(4) 0.0031(4) 0.0055(4) 0.0082(4) F2 0.0505(7) 0.0626(7) 0.0265(5) 0.0022(4) 0.0128(4) 0.0129(6) F3 0.0581(7) 0.0418(6) 0.0225(4) 0.0008(4) -0.0073(4) -0.0036(5) F4 0.0311(5) 0.0541(7) 0.0395(5) 0.0089(5) -0.0128(4) -0.0082(5) F5 0.0223(4) 0.0550(6) 0.0357(5) 0.0037(4) 0.0027(4) 0.0003(4) N2 0.0190(5) 0.0240(6) 0.0237(5) -0.0015(4) 0.0014(4) 0.0012(4) N1 0.0211(5) 0.0250(6) 0.0210(5) 0.0007(4) 0.0018(4) -0.0001(5) S 0.02442(19) 0.0347(2) 0.0503(2) -0.01260(17) -0.00325(17) 0.00830(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(2) . ? C1 C6 1.392(2) . ? C1 Si 1.9242(14) . ? C2 F1 1.3528(17) . ? C2 C3 1.390(2) . ? C3 F2 1.338(2) . ? C3 C4 1.384(2) . ? C4 F3 1.3424(17) . ? C4 C5 1.378(3) . ? C5 F4 1.3417(18) . ? C5 C6 1.391(2) . ? C6 F5 1.3453(19) . ? C7 C8 1.397(2) . ? C7 C12 1.410(2) . ? C7 S 1.7518(16) . ? C8 C9 1.392(3) . ? C9 C10 1.388(3) . ? C10 C11 1.400(2) . ? C11 C12 1.397(2) . ? C12 N2 1.4062(18) . ? C13 N2 1.4527(18) . ? C13 C14 1.497(2) . ? C14 N1 1.3407(18) . ? C14 C15 1.393(2) . ? C15 C16 1.386(2) . ? C16 C17 1.393(2) . ? C17 C18 1.376(2) . ? C18 N1 1.3577(19) . ? Si N2 1.7438(13) . ? Si N1 1.9781(13) . ? Si Cl 2.1178(6) . ? Si S 2.2362(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 114.87(13) . . ? C2 C1 Si 120.65(11) . . ? C6 C1 Si 124.26(12) . . ? F1 C2 C1 119.90(12) . . ? F1 C2 C3 116.22(14) . . ? C1 C2 C3 123.86(14) . . ? F2 C3 C4 120.02(14) . . ? F2 C3 C2 121.02(15) . . ? C4 C3 C2 118.95(15) . . ? F3 C4 C5 120.41(15) . . ? F3 C4 C3 120.01(16) . . ? C5 C4 C3 119.54(14) . . ? F4 C5 C4 119.53(14) . . ? F4 C5 C6 120.83(16) . . ? C4 C5 C6 119.64(14) . . ? F5 C6 C5 116.73(13) . . ? F5 C6 C1 120.16(13) . . ? C5 C6 C1 123.10(15) . . ? C8 C7 C12 120.21(15) . . ? C8 C7 S 123.52(13) . . ? C12 C7 S 116.25(11) . . ? C9 C8 C7 120.24(16) . . ? C10 C9 C8 119.59(15) . . ? C9 C10 C11 120.93(16) . . ? C12 C11 C10 119.82(15) . . ? C11 C12 N2 124.23(13) . . ? C11 C12 C7 119.20(14) . . ? N2 C12 C7 116.56(13) . . ? N2 C13 C14 107.93(11) . . ? N1 C14 C15 121.38(14) . . ? N1 C14 C13 113.46(12) . . ? C15 C14 C13 125.16(13) . . ? C16 C15 C14 119.08(14) . . ? C15 C16 C17 119.21(15) . . ? C18 C17 C16 119.05(14) . . ? N1 C18 C17 121.65(14) . . ? N2 Si C1 119.72(7) . . ? N2 Si N1 83.42(5) . . ? C1 Si N1 90.22(6) . . ? N2 Si Cl 128.63(5) . . ? C1 Si Cl 110.84(5) . . ? N1 Si Cl 88.07(4) . . ? N2 Si S 89.83(4) . . ? C1 Si S 96.26(5) . . ? N1 Si S 172.36(4) . . ? Cl Si S 93.39(3) . . ? C12 N2 C13 117.26(12) . . ? C12 N2 Si 121.85(10) . . ? C13 N2 Si 120.87(10) . . ? C14 N1 C18 119.63(13) . . ? C14 N1 Si 114.30(10) . . ? C18 N1 Si 126.04(10) . . ? C7 S Si 95.30(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 C6 C1 C2 F1 -176.49(13) . . . . ? Si C1 C2 F1 -1.58(19) . . . . ? C6 C1 C2 C3 2.0(2) . . . . ? Si C1 C2 C3 176.95(12) . . . . ? F1 C2 C3 F2 -1.4(2) . . . . ? C1 C2 C3 F2 180.00(15) . . . . ? F1 C2 C3 C4 177.45(14) . . . . ? C1 C2 C3 C4 -1.1(2) . . . . ? F2 C3 C4 F3 0.1(2) . . . . ? C2 C3 C4 F3 -178.83(14) . . . . ? F2 C3 C4 C5 178.00(15) . . . . ? C2 C3 C4 C5 -0.9(2) . . . . ? F3 C4 C5 F4 0.5(2) . . . . ? C3 C4 C5 F4 -177.46(14) . . . . ? F3 C4 C5 C6 179.74(14) . . . . ? C3 C4 C5 C6 1.8(2) . . . . ? F4 C5 C6 F5 -0.3(2) . . . . ? C4 C5 C6 F5 -179.55(14) . . . . ? F4 C5 C6 C1 178.44(14) . . . . ? C4 C5 C6 C1 -0.8(2) . . . . ? C2 C1 C6 F5 177.64(13) . . . . ? Si C1 C6 F5 2.9(2) . . . . ? C2 C1 C6 C5 -1.1(2) . . . . ? Si C1 C6 C5 -175.76(12) . . . . ? C12 C7 C8 C9 -0.2(2) . . . . ? S C7 C8 C9 -179.02(13) . . . . ? C7 C8 C9 C10 0.7(3) . . . . ? C8 C9 C10 C11 -0.3(2) . . . . ? C9 C10 C11 C12 -0.6(2) . . . . ? C10 C11 C12 N2 -178.39(14) . . . . ? C10 C11 C12 C7 1.1(2) . . . . ? C8 C7 C12 C11 -0.7(2) . . . . ? S C7 C12 C11 178.19(11) . . . . ? C8 C7 C12 N2 178.81(14) . . . . ? S C7 C12 N2 -2.27(17) . . . . ? N2 C13 C14 N1 -0.53(16) . . . . ? N2 C13 C14 C15 -179.77(13) . . . . ? N1 C14 C15 C16 -0.4(2) . . . . ? C13 C14 C15 C16 178.74(14) . . . . ? C14 C15 C16 C17 0.0(2) . . . . ? C15 C16 C17 C18 0.3(2) . . . . ? C16 C17 C18 N1 -0.1(2) . . . . ? C2 C1 Si N2 -24.18(14) . . . . ? C6 C1 Si N2 150.23(12) . . . . ? C2 C1 Si N1 58.37(12) . . . . ? C6 C1 Si N1 -127.22(13) . . . . ? C2 C1 Si Cl 146.38(11) . . . . ? C6 C1 Si Cl -39.21(14) . . . . ? C2 C1 Si S -117.56(12) . . . . ? C6 C1 Si S 56.85(13) . . . . ? C11 C12 N2 C13 -0.8(2) . . . . ? C7 C12 N2 C13 179.68(12) . . . . ? C11 C12 N2 Si 177.81(11) . . . . ? C7 C12 N2 Si -1.70(17) . . . . ? C14 C13 N2 C12 -179.89(11) . . . . ? C14 C13 N2 Si 1.48(15) . . . . ? C1 Si N2 C12 -93.50(12) . . . . ? N1 Si N2 C12 -179.98(11) . . . . ? Cl Si N2 C12 97.81(11) . . . . ? S Si N2 C12 3.61(11) . . . . ? C1 Si N2 C13 85.07(12) . . . . ? N1 Si N2 C13 -1.41(11) . . . . ? Cl Si N2 C13 -83.62(11) . . . . ? S Si N2 C13 -177.82(10) . . . . ? C15 C14 N1 C18 0.6(2) . . . . ? C13 C14 N1 C18 -178.67(12) . . . . ? C15 C14 N1 Si 178.83(11) . . . . ? C13 C14 N1 Si -0.44(15) . . . . ? C17 C18 N1 C14 -0.3(2) . . . . ? C17 C18 N1 Si -178.32(11) . . . . ? N2 Si N1 C14 1.01(10) . . . . ? C1 Si N1 C14 -118.89(11) . . . . ? Cl Si N1 C14 130.26(10) . . . . ? S Si N1 C14 29.1(4) . . . . ? N2 Si N1 C18 179.12(13) . . . . ? C1 Si N1 C18 59.21(13) . . . . ? Cl Si N1 C18 -51.64(12) . . . . ? S Si N1 C18 -152.8(3) . . . . ? C8 C7 S Si -177.19(13) . . . . ? C12 C7 S Si 3.92(12) . . . . ? N2 Si S C7 -3.73(7) . . . . ? C1 Si S C7 116.16(7) . . . . ? N1 Si S C7 -31.6(3) . . . . ? Cl Si S C7 -132.43(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.07 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.420 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.054