Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Barbara Gehrhus' 'Mahmood Delawar' 'P. B. Hitchcock' _publ_contact_author_name 'Dr Barbara Gehrhus' _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email B.GEHRHUS@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reactions of a stable silylene with halocarbons ; _publ_requested_category FO data_(2a)-apr1703 _database_code_depnum_ccdc_archive 'CCDC 273147' _audit_creation_date 2003-04-14T13:42:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C35 H59 Cl1 N4 Si2' _chemical_formula_sum 'C35 H59 Cl1 N4 Si2' _chemical_formula_weight 627.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 37.6052(5) _cell_length_b 10.2296(1) _cell_length_c 19.9346(2) _cell_angle_alpha 90 _cell_angle_beta 105.446(1) _cell_angle_gamma 90 _cell_volume 7391.59(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22738 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.197 _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 0.9001 _exptl_absorpt_correction_T_max 0.9735 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.11569E-1 _diffrn_orient_matrix_ub_12 -0.80347E-1 _diffrn_orient_matrix_ub_13 0.251502E-1 _diffrn_orient_matrix_ub_21 0.3929E-3 _diffrn_orient_matrix_ub_22 0.420873E-1 _diffrn_orient_matrix_ub_23 0.454685E-1 _diffrn_orient_matrix_ub_31 -0.250425E-1 _diffrn_orient_matrix_ub_32 -0.364578E-1 _diffrn_orient_matrix_ub_33 -0.29375E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_unetI/netI 0.0276 _diffrn_reflns_number 38024 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6480 _reflns_number_gt 5583 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+12.0550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6480 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1005 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.524 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.042 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Si1 Si 0.131645(13) 0.10637(5) 0.48251(2) 0.02121(13) Uani 1 1 d . . . Si2 Si 0.147045(13) 0.09040(5) 0.60525(2) 0.02112(13) Uani 1 1 d . . . Cl Cl 0.195563(14) 0.19617(5) 0.64473(3) 0.03712(14) Uani 1 1 d . . . N1 N 0.12708(4) 0.26630(15) 0.45041(8) 0.0235(3) Uani 1 1 d . . . N2 N 0.08478(4) 0.07213(14) 0.45148(7) 0.0215(3) Uani 1 1 d . . . N3 N 0.11088(4) 0.13851(14) 0.63768(7) 0.0213(3) Uani 1 1 d . . . N4 N 0.15036(4) -0.06263(15) 0.64279(8) 0.0234(3) Uani 1 1 d . . . C1 C 0.08969(5) 0.28994(18) 0.41529(9) 0.0223(4) Uani 1 1 d . . . C2 C 0.06623(5) 0.18227(17) 0.41542(9) 0.0222(4) Uani 1 1 d . . . C3 C 0.02878(5) 0.19320(19) 0.38391(10) 0.0286(4) Uani 1 1 d . . . H3 H 0.0129 0.121 0.3839 0.034 Uiso 1 1 calc R . . C4 C 0.01450(6) 0.3105(2) 0.35223(11) 0.0358(5) Uani 1 1 d . . . H4 H -0.0112 0.3177 0.3304 0.043 Uiso 1 1 calc R . . C5 C 0.03722(6) 0.4155(2) 0.35237(11) 0.0359(5) Uani 1 1 d . . . H5 H 0.0272 0.495 0.3308 0.043 Uiso 1 1 calc R . . C6 C 0.07498(6) 0.40599(19) 0.38401(10) 0.0299(4) Uani 1 1 d . . . H6 H 0.0906 0.479 0.3841 0.036 Uiso 1 1 calc R . . C7 C 0.15161(5) 0.37751(19) 0.47697(10) 0.0289(4) Uani 1 1 d . . . H7A H 0.1658 0.3565 0.5252 0.035 Uiso 1 1 calc R . . H7B H 0.1359 0.454 0.4796 0.035 Uiso 1 1 calc R . . C8 C 0.17928(6) 0.4191(2) 0.43657(11) 0.0349(5) Uani 1 1 d . . . C9 C 0.20046(8) 0.5359(3) 0.47584(14) 0.0636(8) Uani 1 1 d . . . H9A H 0.1832 0.6073 0.4765 0.095 Uiso 1 1 calc R . . H9B H 0.2189 0.5652 0.4524 0.095 Uiso 1 1 calc R . . H9C H 0.2128 0.5099 0.5237 0.095 Uiso 1 1 calc R . . C10 C 0.20593(7) 0.3081(3) 0.43542(14) 0.0535(7) Uani 1 1 d . . . H10A H 0.2182 0.2816 0.4832 0.08 Uiso 1 1 calc R . . H10B H 0.2245 0.3374 0.4122 0.08 Uiso 1 1 calc R . . H10C H 0.1923 0.2336 0.41 0.08 Uiso 1 1 calc R . . C11 C 0.16036(7) 0.4589(3) 0.36188(11) 0.0457(6) Uani 1 1 d . . . H11A H 0.143 0.5303 0.3621 0.069 Uiso 1 1 calc R . . H11B H 0.1469 0.3839 0.3367 0.069 Uiso 1 1 calc R . . H11C H 0.179 0.488 0.3388 0.069 Uiso 1 1 calc R . . C12 C 0.06400(5) -0.02232(18) 0.48200(10) 0.0262(4) Uani 1 1 d . . . H12A H 0.04 0.018 0.4815 0.031 Uiso 1 1 calc R . . H12B H 0.0776 -0.035 0.5314 0.031 Uiso 1 1 calc R . . C13 C 0.05624(5) -0.15814(19) 0.44818(10) 0.0302(4) Uani 1 1 d . . . C14 C 0.03671(7) -0.1485(2) 0.37095(12) 0.0480(6) Uani 1 1 d . . . H14A H 0.0137 -0.0994 0.3647 0.072 Uiso 1 1 calc R . . H14B H 0.0312 -0.2365 0.3516 0.072 Uiso 1 1 calc R . . H14C H 0.0527 -0.1033 0.3468 0.072 Uiso 1 1 calc R . . C15 C 0.09200(7) -0.2344(2) 0.45826(15) 0.0510(6) Uani 1 1 d . . . H15A H 0.1045 -0.2402 0.508 0.077 Uiso 1 1 calc R . . H15B H 0.108 -0.1896 0.4341 0.077 Uiso 1 1 calc R . . H15C H 0.0865 -0.3226 0.4391 0.077 Uiso 1 1 calc R . . C16 C 0.03168(7) -0.2294(2) 0.48652(14) 0.0510(6) Uani 1 1 d . . . H16A H 0.0084 -0.1815 0.4802 0.076 Uiso 1 1 calc R . . H16B H 0.0444 -0.2344 0.5362 0.076 Uiso 1 1 calc R . . H16C H 0.0265 -0.3179 0.4677 0.076 Uiso 1 1 calc R . . C17 C 0.09984(5) 0.03352(18) 0.67343(9) 0.0216(4) Uani 1 1 d . . . C18 C 0.12201(5) -0.07872(18) 0.67681(9) 0.0224(4) Uani 1 1 d . . . C19 C 0.11398(6) -0.19112(19) 0.70878(10) 0.0294(4) Uani 1 1 d . . . H19 H 0.1291 -0.2664 0.7119 0.035 Uiso 1 1 calc R . . C20 C 0.08359(6) -0.1932(2) 0.73626(10) 0.0334(5) Uani 1 1 d . . . H20 H 0.078 -0.2702 0.7581 0.04 Uiso 1 1 calc R . . C21 C 0.06158(6) -0.0845(2) 0.73194(10) 0.0335(5) Uani 1 1 d . . . H21 H 0.0407 -0.0873 0.7503 0.04 Uiso 1 1 calc R . . C22 C 0.06958(5) 0.0297(2) 0.70090(10) 0.0279(4) Uani 1 1 d . . . H22 H 0.0544 0.1048 0.6985 0.033 Uiso 1 1 calc R . . C23 C 0.08564(5) 0.24654(19) 0.60906(10) 0.0270(4) Uani 1 1 d . . . H23A H 0.0601 0.2143 0.6021 0.032 Uiso 1 1 calc R . . H23B H 0.0887 0.2681 0.5625 0.032 Uiso 1 1 calc R . . C24 C 0.08958(6) 0.3744(2) 0.65146(11) 0.0348(5) Uani 1 1 d . . . C25 C 0.12908(7) 0.4242(2) 0.66840(15) 0.0515(6) Uani 1 1 d . . . H25A H 0.1364 0.4361 0.6252 0.077 Uiso 1 1 calc R . . H25B H 0.1455 0.3607 0.6981 0.077 Uiso 1 1 calc R . . H25C H 0.1307 0.5081 0.6928 0.077 Uiso 1 1 calc R . . C26 C 0.06368(8) 0.4734(2) 0.60550(15) 0.0623(8) Uani 1 1 d . . . H26A H 0.0707 0.4849 0.5619 0.094 Uiso 1 1 calc R . . H26B H 0.0656 0.5573 0.6299 0.094 Uiso 1 1 calc R . . H26C H 0.0382 0.4413 0.5953 0.094 Uiso 1 1 calc R . . C27 C 0.07874(8) 0.3568(2) 0.71943(13) 0.0545(7) Uani 1 1 d . . . H27A H 0.0533 0.3251 0.7093 0.082 Uiso 1 1 calc R . . H27B H 0.0807 0.4408 0.7438 0.082 Uiso 1 1 calc R . . H27C H 0.0953 0.2932 0.7489 0.082 Uiso 1 1 calc R . . C28 C 0.17174(5) -0.17619(19) 0.63090(10) 0.0288(4) Uani 1 1 d . . . H28A H 0.1762 -0.1661 0.5844 0.035 Uiso 1 1 calc R . . H28B H 0.1562 -0.2549 0.629 0.035 Uiso 1 1 calc R . . C29 C 0.20942(5) -0.2030(2) 0.68403(10) 0.0308(4) Uani 1 1 d . . . C30 C 0.23962(7) -0.1253(3) 0.6659(2) 0.0829(11) Uani 1 1 d . . . H30A H 0.2407 -0.1475 0.6187 0.124 Uiso 1 1 calc R . . H30B H 0.2633 -0.146 0.6989 0.124 Uiso 1 1 calc R . . H30C H 0.2345 -0.0317 0.6684 0.124 Uiso 1 1 calc R . . C31 C 0.21805(8) -0.3469(3) 0.68012(19) 0.0783(10) Uani 1 1 d . . . H31A H 0.1987 -0.399 0.692 0.117 Uiso 1 1 calc R . . H31B H 0.2419 -0.3664 0.713 0.117 Uiso 1 1 calc R . . H31C H 0.2191 -0.3686 0.6328 0.117 Uiso 1 1 calc R . . C32 C 0.20880(7) -0.1676(4) 0.75728(12) 0.0777(11) Uani 1 1 d . . . H32A H 0.1894 -0.2178 0.7703 0.117 Uiso 1 1 calc R . . H32B H 0.2038 -0.074 0.7596 0.117 Uiso 1 1 calc R . . H32C H 0.2328 -0.1881 0.7895 0.117 Uiso 1 1 calc R . . C33 C 0.16280(5) -0.00095(19) 0.44836(9) 0.0266(4) Uani 1 1 d . . . H33A H 0.1881 0.0357 0.463 0.032 Uiso 1 1 calc R . . H33B H 0.1635 -0.0882 0.4702 0.032 Uiso 1 1 calc R . . C34 C 0.15205(6) -0.0185(2) 0.36883(10) 0.0358(5) Uani 1 1 d . . . H34A H 0.1259 -0.0465 0.3531 0.043 Uiso 1 1 calc R . . H34B H 0.1543 0.0666 0.3467 0.043 Uiso 1 1 calc R . . C35 C 0.17598(8) -0.1186(3) 0.34509(13) 0.0563(7) Uani 1 1 d . . . H35A H 0.1681 -0.1261 0.2943 0.084 Uiso 1 1 calc R . . H35B H 0.1735 -0.2036 0.366 0.084 Uiso 1 1 calc R . . H35C H 0.2018 -0.0905 0.3596 0.084 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 Si1 0.0214(3) 0.0225(3) 0.0199(2) 0.0012(2) 0.00589(19) -0.0001(2) Si2 0.0209(3) 0.0227(3) 0.0193(2) 0.0017(2) 0.00460(19) -0.0006(2) Cl 0.0272(3) 0.0417(3) 0.0376(3) 0.0032(2) 0.0000(2) -0.0103(2) N1 0.0234(8) 0.0225(8) 0.0241(8) 0.0010(6) 0.0057(6) -0.0032(6) N2 0.0219(8) 0.0190(8) 0.0235(8) 0.0003(6) 0.0059(6) -0.0010(6) N3 0.0231(8) 0.0190(8) 0.0219(7) 0.0002(6) 0.0062(6) 0.0005(6) N4 0.0236(8) 0.0236(8) 0.0236(8) 0.0036(6) 0.0075(6) 0.0034(6) C1 0.0267(10) 0.0217(9) 0.0192(9) -0.0021(7) 0.0072(7) 0.0014(8) C2 0.0269(10) 0.0209(9) 0.0192(8) -0.0029(7) 0.0066(7) 0.0026(8) C3 0.0256(10) 0.0274(10) 0.0319(10) -0.0031(8) 0.0063(8) -0.0002(8) C4 0.0277(11) 0.0355(12) 0.0402(12) -0.0012(9) 0.0020(9) 0.0087(9) C5 0.0398(12) 0.0261(11) 0.0382(12) 0.0019(9) 0.0041(9) 0.0119(9) C6 0.0366(11) 0.0212(10) 0.0319(10) -0.0012(8) 0.0093(9) 0.0007(8) C7 0.0324(11) 0.0288(11) 0.0241(9) -0.0002(8) 0.0050(8) -0.0082(9) C8 0.0339(11) 0.0382(12) 0.0316(11) 0.0042(9) 0.0067(9) -0.0123(9) C9 0.0692(18) 0.0696(19) 0.0532(15) -0.0088(14) 0.0183(13) -0.0444(16) C10 0.0346(13) 0.0715(18) 0.0584(15) 0.0170(13) 0.0191(11) -0.0005(12) C11 0.0479(14) 0.0573(15) 0.0334(12) 0.0121(11) 0.0134(10) -0.0099(12) C12 0.0275(10) 0.0245(10) 0.0269(9) -0.0009(8) 0.0077(8) -0.0040(8) C13 0.0304(11) 0.0221(10) 0.0359(11) -0.0007(8) 0.0052(8) -0.0049(8) C14 0.0610(16) 0.0339(12) 0.0405(13) -0.0094(10) -0.0012(11) -0.0096(11) C15 0.0453(14) 0.0276(12) 0.0773(18) -0.0088(12) 0.0112(13) 0.0015(10) C16 0.0545(15) 0.0350(13) 0.0655(16) 0.0034(12) 0.0195(13) -0.0159(11) C17 0.0238(9) 0.0227(9) 0.0168(8) -0.0030(7) 0.0027(7) -0.0040(8) C18 0.0224(9) 0.0242(10) 0.0186(9) -0.0007(7) 0.0022(7) -0.0032(8) C19 0.0335(11) 0.0247(10) 0.0277(10) 0.0024(8) 0.0039(8) -0.0026(8) C20 0.0373(12) 0.0328(11) 0.0295(10) 0.0040(9) 0.0077(9) -0.0130(9) C21 0.0304(11) 0.0428(13) 0.0297(10) -0.0029(9) 0.0121(8) -0.0129(10) C22 0.0261(10) 0.0321(11) 0.0263(10) -0.0042(8) 0.0085(8) -0.0027(8) C23 0.0310(10) 0.0246(10) 0.0250(9) -0.0001(8) 0.0068(8) 0.0056(8) C24 0.0445(13) 0.0232(10) 0.0383(11) -0.0050(9) 0.0140(9) 0.0034(9) C25 0.0585(16) 0.0282(12) 0.0714(17) -0.0179(12) 0.0237(13) -0.0096(11) C26 0.079(2) 0.0337(14) 0.0701(18) -0.0012(13) 0.0134(15) 0.0244(13) C27 0.0789(19) 0.0424(14) 0.0514(15) -0.0229(12) 0.0334(14) -0.0075(13) C28 0.0341(11) 0.0284(11) 0.0238(9) 0.0011(8) 0.0075(8) 0.0076(9) C29 0.0293(10) 0.0327(11) 0.0314(10) 0.0046(9) 0.0099(8) 0.0093(9) C30 0.0359(15) 0.094(2) 0.114(3) 0.049(2) 0.0121(16) -0.0008(16) C31 0.0590(18) 0.0476(17) 0.106(3) -0.0099(16) -0.0161(17) 0.0259(14) C32 0.0406(15) 0.154(3) 0.0314(13) -0.0058(17) -0.0022(11) 0.0337(18) C33 0.0269(10) 0.0296(10) 0.0243(9) 0.0040(8) 0.0086(8) 0.0051(8) C34 0.0407(12) 0.0427(13) 0.0267(10) 0.0013(9) 0.0137(9) 0.0088(10) C35 0.0760(19) 0.0583(17) 0.0427(14) -0.0006(12) 0.0302(13) 0.0195(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N2 1.7408(15) . ? Si1 N1 1.7484(16) . ? Si1 C33 1.8618(19) . ? Si1 Si2 2.3652(7) . ? Si2 N4 1.7252(16) . ? Si2 N3 1.7256(15) . ? Si2 Cl 2.0866(7) . ? N1 C1 1.415(2) . ? N1 C7 1.472(2) . ? N2 C2 1.416(2) . ? N2 C12 1.472(2) . ? N3 C17 1.411(2) . ? N3 C23 1.469(2) . ? N4 C18 1.417(2) . ? N4 C28 1.468(2) . ? C1 C6 1.386(3) . ? C1 C2 1.411(3) . ? C2 C3 1.385(3) . ? C3 C4 1.395(3) . ? C4 C5 1.372(3) . ? C5 C6 1.395(3) . ? C7 C8 1.536(3) . ? C8 C10 1.519(3) . ? C8 C11 1.525(3) . ? C8 C9 1.530(3) . ? C12 C13 1.538(3) . ? C13 C15 1.521(3) . ? C13 C14 1.522(3) . ? C13 C16 1.531(3) . ? C17 C22 1.389(3) . ? C17 C18 1.410(3) . ? C18 C19 1.386(3) . ? C19 C20 1.393(3) . ? C20 C21 1.375(3) . ? C21 C22 1.392(3) . ? C23 C24 1.543(3) . ? C24 C25 1.521(3) . ? C24 C27 1.526(3) . ? C24 C26 1.529(3) . ? C28 C29 1.551(3) . ? C29 C30 1.507(3) . ? C29 C32 1.510(3) . ? C29 C31 1.514(3) . ? C33 C34 1.539(3) . ? C34 C35 1.519(3) . ? 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 N2 Si1 N1 93.82(7) . . ? N2 Si1 C33 115.31(8) . . ? N1 Si1 C33 115.34(8) . . ? N2 Si1 Si2 107.43(5) . . ? N1 Si1 Si2 114.60(5) . . ? C33 Si1 Si2 109.45(6) . . ? N4 Si2 N3 93.98(7) . . ? N4 Si2 Cl 110.60(6) . . ? N3 Si2 Cl 114.08(6) . . ? N4 Si2 Si1 118.74(6) . . ? N3 Si2 Si1 111.57(5) . . ? Cl Si2 Si1 107.64(3) . . ? C1 N1 C7 119.42(15) . . ? C1 N1 Si1 109.20(12) . . ? C7 N1 Si1 126.91(12) . . ? C2 N2 C12 119.20(15) . . ? C2 N2 Si1 109.60(12) . . ? C12 N2 Si1 125.71(12) . . ? C17 N3 C23 121.46(15) . . ? C17 N3 Si2 109.84(12) . . ? C23 N3 Si2 124.12(12) . . ? C18 N4 C28 119.97(15) . . ? C18 N4 Si2 109.65(12) . . ? C28 N4 Si2 128.87(12) . . ? C6 C1 C2 119.65(17) . . ? C6 C1 N1 126.45(17) . . ? C2 C1 N1 113.88(15) . . ? C3 C2 C1 119.77(17) . . ? C3 C2 N2 126.74(17) . . ? C1 C2 N2 113.47(15) . . ? C2 C3 C4 119.80(19) . . ? C5 C4 C3 120.54(19) . . ? C4 C5 C6 120.29(19) . . ? C1 C6 C5 119.96(19) . . ? N1 C7 C8 118.23(16) . . ? C10 C8 C11 108.8(2) . . ? C10 C8 C9 109.6(2) . . ? C11 C8 C9 109.6(2) . . ? C10 C8 C7 110.05(18) . . ? C11 C8 C7 112.39(17) . . ? C9 C8 C7 106.32(18) . . ? N2 C12 C13 118.12(15) . . ? C15 C13 C14 109.8(2) . . ? C15 C13 C16 108.62(19) . . ? C14 C13 C16 110.07(18) . . ? C15 C13 C12 110.35(17) . . ? C14 C13 C12 111.63(17) . . ? C16 C13 C12 106.30(17) . . ? C22 C17 C18 119.65(17) . . ? C22 C17 N3 127.05(17) . . ? C18 C17 N3 113.21(15) . . ? C19 C18 C17 119.93(17) . . ? C19 C18 N4 126.87(17) . . ? C17 C18 N4 113.15(15) . . ? C18 C19 C20 119.69(19) . . ? C21 C20 C19 120.42(18) . . ? C20 C21 C22 120.58(18) . . ? C17 C22 C21 119.71(19) . . ? N3 C23 C24 117.83(16) . . ? C25 C24 C27 108.6(2) . . ? C25 C24 C26 109.9(2) . . ? C27 C24 C26 109.4(2) . . ? C25 C24 C23 110.58(17) . . ? C27 C24 C23 112.14(18) . . ? C26 C24 C23 106.27(18) . . ? N4 C28 C29 118.02(16) . . ? C30 C29 C32 108.2(2) . . ? C30 C29 C31 108.4(2) . . ? C32 C29 C31 110.0(2) . . ? C30 C29 C28 110.66(18) . . ? C32 C29 C28 111.80(17) . . ? C31 C29 C28 107.83(19) . . ? C34 C33 Si1 115.31(13) . . ? C35 C34 C33 112.64(18) . . ? #===END data_(3a)-mar2403 _database_code_depnum_ccdc_archive 'CCDC 273148' _audit_creation_date 2003-03-31T11:20:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[{C6H4(NCH2tBu)2}Si(Cl)Si(CH2Cl){(NCH2tBu)2C6H4}' ; _chemical_formula_moiety 'C33 H54 Cl2 N4 Si2' _chemical_formula_sum 'C33 H54 Cl2 N4 Si2' _chemical_formula_weight 633.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2646(5) _cell_length_b 18.5123(10) _cell_length_c 10.6180(5) _cell_angle_alpha 99.309(3) _cell_angle_beta 70.322(3) _cell_angle_gamma 82.774(3) _cell_volume 1839.18(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 24551 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.268 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_unetI/netI 0.059 _diffrn_reflns_number 9307 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 23.04 _diffrn_reflns_theta_full 23.04 _diffrn_measured_fraction_theta_full 0.924 _diffrn_measured_fraction_theta_max 0.924 _reflns_number_total 4765 _reflns_number_gt 4133 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Diffraction was weak and limited. ***************************************************************************** There is unresolved 50:50 disorder of the Cl and CH2Cl groups attached to the Si atoms. Bond lengths and angles involving these groups are unreal. ***************************************************************************** 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^)+(0.0000P)^2^+6.2443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4765 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1954 _refine_ls_goodness_of_fit_ref 1.239 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.332 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.062 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Cl1 Cl 0.3972(3) 0.10933(13) -0.2014(3) 0.0502(6) Uani 0.5 1 d P A . Cl2 Cl 0.0517(3) 0.16942(16) 0.1890(3) 0.0568(7) Uani 0.5 1 d P B . Cl3 Cl 0.4756(4) 0.07499(18) -0.3702(3) 0.0538(8) Uani 0.5 1 d P . . Cl4 Cl -0.0389(4) 0.1893(2) 0.3527(3) 0.0562(9) Uani 0.5 1 d P . . Si1 Si 0.17191(17) 0.23756(8) 0.10389(15) 0.0353(4) Uani 1 1 d . . . Si2 Si 0.24745(17) 0.19996(9) -0.13699(15) 0.0355(4) Uani 1 1 d . A . N1 N 0.0933(5) 0.3305(3) 0.1546(5) 0.0388(11) Uani 1 1 d . B . N2 N 0.3013(4) 0.2499(2) 0.1708(5) 0.0336(11) Uani 1 1 d . B . N3 N 0.2950(5) 0.2746(3) -0.2082(5) 0.0369(11) Uani 1 1 d . . . N4 N 0.1188(5) 0.1902(2) -0.2061(5) 0.0361(11) Uani 1 1 d . . . C1 C 0.1669(6) 0.3715(3) 0.2214(5) 0.0324(12) Uani 1 1 d . . . C2 C 0.2849(6) 0.3260(3) 0.2291(5) 0.0335(13) Uani 1 1 d . B . C3 C 0.3714(6) 0.3595(3) 0.2860(6) 0.0421(14) Uani 1 1 d . . . H3 H 0.4501 0.3295 0.2924 0.05 Uiso 1 1 calc R B . C4 C 0.3450(7) 0.4354(4) 0.3332(7) 0.0484(16) Uani 1 1 d . B . H4 H 0.4059 0.4577 0.371 0.058 Uiso 1 1 calc R . . C5 C 0.2296(7) 0.4796(3) 0.3257(6) 0.0472(15) Uani 1 1 d . . . H5 H 0.2116 0.5321 0.3586 0.057 Uiso 1 1 calc R B . C6 C 0.1399(6) 0.4476(3) 0.2705(6) 0.0413(14) Uani 1 1 d . B . H6 H 0.0603 0.4781 0.2666 0.05 Uiso 1 1 calc R . . C7 C 0.0061(6) 0.3693(4) 0.0903(6) 0.0468(15) Uani 1 1 d . . . H7A H 0.0305 0.3396 -0.0037 0.056 Uiso 1 1 calc R B . H7B H 0.0344 0.4179 0.0816 0.056 Uiso 1 1 calc R . . C8 C -0.1543(6) 0.3839(3) 0.1612(7) 0.0489(16) Uani 1 1 d . B . C9 C -0.2053(8) 0.3107(5) 0.1521(12) 0.106(4) Uani 1 1 d . . . H9A H -0.1745 0.2849 0.0558 0.16 Uiso 1 1 calc R B . H9B H -0.3085 0.3204 0.1931 0.16 Uiso 1 1 calc R . . H9C H -0.1659 0.2793 0.2017 0.16 Uiso 1 1 calc R . . C10 C -0.2158(9) 0.4333(6) 0.0859(9) 0.099(3) Uani 1 1 d . . . H10A H -0.186 0.408 -0.0106 0.149 Uiso 1 1 calc R B . H10B H -0.1821 0.4805 0.092 0.149 Uiso 1 1 calc R . . H10C H -0.319 0.4433 0.1277 0.149 Uiso 1 1 calc R . . C11 C -0.1996(7) 0.4229(5) 0.3099(7) 0.067(2) Uani 1 1 d . . . H11A H -0.3026 0.4311 0.353 0.101 Uiso 1 1 calc R B . H11B H -0.1691 0.4709 0.3158 0.101 Uiso 1 1 calc R . . H11C H -0.1567 0.3918 0.3574 0.101 Uiso 1 1 calc R . . C12 C 0.4366(6) 0.1992(3) 0.1368(6) 0.0425(14) Uani 1 1 d . . . H12A H 0.5104 0.2298 0.1283 0.051 Uiso 1 1 calc R B . H12B H 0.4597 0.1666 0.0455 0.051 Uiso 1 1 calc R . . C13 C 0.4464(6) 0.1487(3) 0.2374(6) 0.0433(14) Uani 1 1 d . B . C14 C 0.3550(9) 0.0902(4) 0.2328(9) 0.080(2) Uani 1 1 d . . . H14A H 0.3847 0.0612 0.1386 0.119 Uiso 1 1 calc R B . H14B H 0.256 0.1151 0.2637 0.119 Uiso 1 1 calc R . . H14C H 0.3655 0.0568 0.2929 0.119 Uiso 1 1 calc R . . C15 C 0.6003(8) 0.1092(5) 0.1856(10) 0.088(3) Uani 1 1 d . . . H15A H 0.6273 0.0804 0.0916 0.132 Uiso 1 1 calc R B . H15B H 0.6121 0.0755 0.2449 0.132 Uiso 1 1 calc R . . H15C H 0.6603 0.1463 0.1868 0.132 Uiso 1 1 calc R . . C16 C 0.4011(10) 0.1928(4) 0.3814(7) 0.078(3) Uani 1 1 d . . . H16A H 0.3025 0.2181 0.412 0.117 Uiso 1 1 calc R B . H16B H 0.4607 0.2299 0.3848 0.117 Uiso 1 1 calc R . . H16C H 0.4104 0.1591 0.4415 0.117 Uiso 1 1 calc R . . C17 C 0.2065(5) 0.2950(3) -0.2792(5) 0.0335(13) Uani 1 1 d . B . C18 C 0.1091(6) 0.2471(3) -0.2803(5) 0.0350(13) Uani 1 1 d . B . C19 C 0.0152(6) 0.2600(3) -0.3440(6) 0.0452(15) Uani 1 1 d . . . H19 H -0.0498 0.2278 -0.3452 0.054 Uiso 1 1 calc R B . C20 C 0.0152(7) 0.3200(4) -0.4066(7) 0.0513(16) Uani 1 1 d . B . H20 H -0.0496 0.3287 -0.4512 0.062 Uiso 1 1 calc R . . C21 C 0.1075(7) 0.3669(3) -0.4050(6) 0.0476(16) Uani 1 1 d . . . H21 H 0.106 0.4081 -0.4478 0.057 Uiso 1 1 calc R B . C22 C 0.2041(6) 0.3546(3) -0.3407(6) 0.0396(14) Uani 1 1 d . B . H22 H 0.268 0.3875 -0.3397 0.047 Uiso 1 1 calc R . . C23 C 0.3676(6) 0.3292(3) -0.1547(6) 0.0425(15) Uani 1 1 d . B . H23A H 0.356 0.3246 -0.0601 0.051 Uiso 1 1 calc R . . H23B H 0.3176 0.3798 -0.1485 0.051 Uiso 1 1 calc R . . C24 C 0.5258(7) 0.3245(4) -0.2342(7) 0.0575(18) Uani 1 1 d . . . C25 C 0.5510(8) 0.3429(5) -0.3754(7) 0.076(2) Uani 1 1 d . B . H25A H 0.498 0.3929 -0.3639 0.114 Uiso 1 1 calc R . . H25B H 0.5193 0.3062 -0.4302 0.114 Uiso 1 1 calc R . . H25C H 0.6518 0.3413 -0.4223 0.114 Uiso 1 1 calc R . . C26 C 0.5721(9) 0.3830(6) -0.1478(9) 0.087(3) Uani 1 1 d . B . H26A H 0.5563 0.3713 -0.0576 0.13 Uiso 1 1 calc R . . H26B H 0.5171 0.4324 -0.1364 0.13 Uiso 1 1 calc R . . H26C H 0.6726 0.3826 -0.194 0.13 Uiso 1 1 calc R . . C27 C 0.6060(8) 0.2480(5) -0.2496(12) 0.100(3) Uani 1 1 d . B . H27A H 0.5886 0.2368 -0.1588 0.15 Uiso 1 1 calc R . . H27B H 0.7071 0.246 -0.2956 0.15 Uiso 1 1 calc R . . H27C H 0.5748 0.211 -0.3043 0.15 Uiso 1 1 calc R . . C28 C 0.0043(6) 0.1485(3) -0.1684(6) 0.0438(15) Uani 1 1 d . B . H28A H -0.0818 0.1795 -0.168 0.053 Uiso 1 1 calc R . . H28B H -0.0136 0.1429 -0.0732 0.053 Uiso 1 1 calc R . . C29 C 0.0243(6) 0.0700(3) -0.2580(6) 0.0439(15) Uani 1 1 d . . . C30 C 0.1237(9) 0.0136(4) -0.2248(10) 0.081(3) Uani 1 1 d . B . H30A H 0.0858 0.0142 -0.1267 0.121 Uiso 1 1 calc R . . H30B H 0.217 0.0271 -0.249 0.121 Uiso 1 1 calc R . . H30C H 0.1318 -0.0364 -0.2776 0.121 Uiso 1 1 calc R . . C31 C -0.1195(8) 0.0477(4) -0.2199(9) 0.076(2) Uani 1 1 d . B . H31A H -0.1568 0.0484 -0.1217 0.114 Uiso 1 1 calc R . . H31B H -0.11 -0.0026 -0.2723 0.114 Uiso 1 1 calc R . . H31C H -0.1843 0.083 -0.2413 0.114 Uiso 1 1 calc R . . C32 C 0.0842(10) 0.0699(4) -0.4077(7) 0.076(2) Uani 1 1 d . B . H32A H 0.0209 0.1059 -0.4295 0.114 Uiso 1 1 calc R . . H32B H 0.094 0.0199 -0.4615 0.114 Uiso 1 1 calc R . . H32C H 0.177 0.084 -0.43 0.114 Uiso 1 1 calc R . . C1A C 0.3972(3) 0.10933(13) -0.2014(3) 0.0502(6) Uani 0.5 1 d P A 1 H1A1 H 0.4714 0.1202 -0.165 0.06 Uiso 0.5 1 calc PR A 1 H1A2 H 0.3561 0.0695 -0.1593 0.06 Uiso 0.5 1 calc PR A 1 C2A C 0.0517(3) 0.16942(16) 0.1890(3) 0.0568(7) Uani 0.5 1 d P B 1 H2A1 H -0.0158 0.1634 0.1417 0.068 Uiso 0.5 1 calc PR B 1 H2A2 H 0.1135 0.12 0.1674 0.068 Uiso 0.5 1 calc PR B 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 Cl1 0.0510(14) 0.0368(14) 0.0605(16) 0.0061(12) -0.0217(12) -0.0019(11) Cl2 0.0603(16) 0.0559(17) 0.0629(17) 0.0282(14) -0.0197(13) -0.0298(13) Cl3 0.065(2) 0.0446(18) 0.0380(17) 0.0003(14) -0.0132(15) 0.0102(15) Cl4 0.074(2) 0.061(2) 0.0342(16) 0.0141(15) -0.0144(15) -0.0271(17) Si1 0.0451(9) 0.0278(9) 0.0333(9) 0.0077(7) -0.0144(7) -0.0060(7) Si2 0.0465(9) 0.0292(9) 0.0320(8) 0.0075(7) -0.0130(7) -0.0149(7) N1 0.043(3) 0.030(3) 0.047(3) 0.008(2) -0.021(2) -0.002(2) N2 0.035(2) 0.027(3) 0.040(3) 0.006(2) -0.016(2) -0.0022(19) N3 0.045(3) 0.035(3) 0.037(3) 0.012(2) -0.017(2) -0.019(2) N4 0.042(3) 0.031(3) 0.037(3) 0.012(2) -0.012(2) -0.015(2) C1 0.038(3) 0.029(3) 0.030(3) 0.008(2) -0.011(2) -0.008(2) C2 0.037(3) 0.030(3) 0.031(3) 0.011(2) -0.008(2) -0.006(2) C3 0.034(3) 0.040(4) 0.052(4) 0.018(3) -0.012(3) -0.007(3) C4 0.048(4) 0.044(4) 0.057(4) 0.010(3) -0.021(3) -0.017(3) C5 0.057(4) 0.031(3) 0.051(4) 0.009(3) -0.014(3) -0.016(3) C6 0.040(3) 0.034(3) 0.045(3) 0.009(3) -0.011(3) -0.001(3) C7 0.054(4) 0.045(4) 0.039(3) 0.003(3) -0.020(3) 0.004(3) C8 0.042(3) 0.043(4) 0.057(4) -0.004(3) -0.023(3) 0.006(3) C9 0.053(5) 0.056(5) 0.185(11) -0.023(6) -0.036(6) -0.004(4) C10 0.074(6) 0.131(9) 0.084(6) 0.011(6) -0.041(5) 0.032(5) C11 0.053(4) 0.075(5) 0.057(4) 0.002(4) -0.006(3) -0.010(4) C12 0.044(3) 0.035(3) 0.038(3) 0.006(3) -0.006(3) 0.002(3) C13 0.041(3) 0.038(3) 0.046(4) 0.009(3) -0.014(3) 0.001(3) C14 0.104(6) 0.056(5) 0.106(7) 0.042(5) -0.056(6) -0.033(5) C15 0.058(5) 0.080(6) 0.118(7) 0.044(6) -0.021(5) 0.012(4) C16 0.128(7) 0.054(5) 0.047(4) 0.011(4) -0.037(5) 0.013(5) C17 0.036(3) 0.028(3) 0.030(3) 0.004(2) -0.005(2) -0.006(2) C18 0.038(3) 0.025(3) 0.036(3) 0.004(2) -0.006(3) -0.008(2) C19 0.050(4) 0.033(3) 0.060(4) 0.014(3) -0.026(3) -0.010(3) C20 0.045(4) 0.047(4) 0.061(4) 0.009(3) -0.024(3) 0.002(3) C21 0.055(4) 0.034(3) 0.045(4) 0.011(3) -0.010(3) 0.001(3) C22 0.045(3) 0.029(3) 0.038(3) 0.009(3) -0.006(3) -0.008(3) C23 0.058(4) 0.044(4) 0.036(3) 0.014(3) -0.020(3) -0.031(3) C24 0.057(4) 0.069(5) 0.064(4) 0.034(4) -0.027(4) -0.035(4) C25 0.061(5) 0.119(7) 0.055(5) 0.029(5) -0.015(4) -0.052(5) C26 0.086(6) 0.131(8) 0.082(6) 0.053(6) -0.048(5) -0.073(6) C27 0.047(4) 0.097(7) 0.164(10) 0.061(7) -0.028(5) -0.029(5) C28 0.050(4) 0.036(3) 0.046(4) 0.010(3) -0.013(3) -0.020(3) C29 0.050(4) 0.030(3) 0.059(4) 0.012(3) -0.023(3) -0.019(3) C30 0.103(6) 0.035(4) 0.131(8) 0.020(4) -0.074(6) -0.022(4) C31 0.070(5) 0.053(5) 0.104(6) 0.007(4) -0.029(5) -0.033(4) C32 0.119(7) 0.050(5) 0.052(5) -0.004(4) -0.026(4) -0.030(4) C1A 0.0510(14) 0.0368(14) 0.0605(16) 0.0061(12) -0.0217(12) -0.0019(11) C2A 0.0603(16) 0.0559(17) 0.0629(17) 0.0282(14) -0.0197(13) -0.0298(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 Cl3 1.673(4) . ? Cl1 Si2 1.980(3) . ? Cl2 Cl4 1.625(4) . ? Cl2 Si1 1.985(3) . ? Si1 N1 1.720(5) . ? Si1 N2 1.727(5) . ? Si1 Si2 2.362(2) . ? Si2 N3 1.727(4) . ? Si2 N4 1.728(5) . ? N1 C1 1.407(7) . ? N1 C7 1.480(7) . ? N2 C2 1.410(7) . ? N2 C12 1.470(7) . ? N3 C17 1.415(7) . ? N3 C23 1.479(7) . ? N4 C18 1.427(7) . ? N4 C28 1.465(7) . ? C1 C6 1.379(8) . ? C1 C2 1.420(7) . ? C2 C3 1.384(8) . ? C3 C4 1.374(9) . ? C4 C5 1.385(9) . ? C5 C6 1.389(9) . ? C7 C8 1.529(8) . ? C8 C11 1.511(9) . ? C8 C9 1.514(10) . ? C8 C10 1.518(10) . ? C12 C13 1.549(8) . ? C13 C16 1.496(9) . ? C13 C14 1.525(10) . ? C13 C15 1.525(9) . ? C17 C22 1.372(8) . ? C17 C18 1.419(8) . ? C18 C19 1.370(8) . ? C19 C20 1.384(9) . ? C20 C21 1.366(9) . ? C21 C22 1.396(8) . ? C23 C24 1.541(9) . ? C24 C27 1.501(11) . ? C24 C26 1.530(11) . ? C24 C25 1.536(9) . ? C28 C29 1.551(8) . ? C29 C32 1.498(9) . ? C29 C31 1.522(9) . ? C29 C30 1.532(9) . ? 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 Cl3 Cl1 Si2 118.22(18) . . ? Cl4 Cl2 Si1 120.6(2) . . ? N1 Si1 N2 93.9(2) . +. ? N1 Si1 Cl2 114.9(2) . . ? N2 Si1 Cl2 112.46(18) . . ? N1 Si1 Si2 109.47(17) . . ? N2 Si1 Si2 116.57(17) . . ? Cl2 Si1 Si2 109.00(11) . . ? N3 Si2 N4 94.3(2) . . ? N3 Si2 Cl1 114.98(19) . . ? N4 Si2 Cl1 111.90(19) . . ? N3 Si2 Si1 108.77(17) . . ? N4 Si2 Si1 117.20(17) . . ? Cl1 Si2 Si1 109.17(11) . . ? C1 N1 C7 119.3(5) . . ? C1 N1 Si1 110.5(3) . . ? C7 N1 Si1 125.4(4) . . ? C2 N2 C12 119.7(5) . . ? C2 N2 Si1 109.7(3) . . ? C12 N2 Si1 127.6(4) . . ? C17 N3 C23 121.0(4) . . ? C17 N3 Si2 110.0(3) . . ? C23 N3 Si2 123.9(4) . . ? C18 N4 C28 119.4(5) . . ? C18 N4 Si2 109.5(3) . . ? C28 N4 Si2 128.8(4) . . ? C6 C1 N1 127.4(5) . . ? C6 C1 C2 119.9(5) . . ? N1 C1 C2 112.6(5) . . ? C3 C2 N2 127.7(5) . . ? C3 C2 C1 118.9(5) . . ? N2 C2 C1 113.4(5) . . ? C4 C3 C2 120.9(5) . . ? C3 C4 C5 120.1(6) . . ? C4 C5 C6 120.4(6) . . ? C1 C6 C5 119.8(5) . . ? N1 C7 C8 118.2(5) . . ? C11 C8 C9 109.4(7) . . ? C11 C8 C10 109.6(6) . . ? C9 C8 C10 110.0(7) . . ? C11 C8 C7 111.2(5) . . ? C9 C8 C7 109.6(5) . . ? C10 C8 C7 107.1(6) . . ? N2 C12 C13 117.5(5) . . ? C16 C13 C14 109.3(6) . . ? C16 C13 C15 110.9(7) . . ? C14 C13 C15 108.7(6) . . ? C16 C13 C12 111.9(5) . . ? C14 C13 C12 109.8(5) . . ? C15 C13 C12 106.1(5) . . ? C22 C17 N3 127.6(5) . . ? C22 C17 C18 119.3(5) . . ? N3 C17 C18 113.0(4) . . ? C19 C18 C17 120.1(5) . . ? C19 C18 N4 126.8(5) . . ? C17 C18 N4 113.1(5) . . ? C18 C19 C20 119.7(6) . . ? C21 C20 C19 120.7(6) . . ? C20 C21 C22 120.4(6) . . ? C17 C22 C21 119.8(5) . . ? N3 C23 C24 118.4(5) . . ? C27 C24 C26 110.3(7) . . ? C27 C24 C25 110.3(7) . . ? C26 C24 C25 109.3(6) . . ? C27 C24 C23 109.8(5) . . ? C26 C24 C23 105.9(6) . . ? C25 C24 C23 111.1(5) . . ? N4 C28 C29 118.2(5) . . ? C32 C29 C31 110.9(6) . . ? C32 C29 C30 109.1(6) . . ? C31 C29 C30 108.4(6) . . ? C32 C29 C28 111.4(5) . . ? C31 C29 C28 107.4(5) . . ? C30 C29 C28 109.6(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 Cl4 Cl2 Si1 N1 -45.8(3) . . . . ? Cl4 Cl2 Si1 N2 60.1(3) . . . . ? Cl4 Cl2 Si1 Si2 -169.0(2) . . . . ? Cl3 Cl1 Si2 N3 -53.5(3) . . . . ? Cl3 Cl1 Si2 N4 52.6(3) . . . . ? Cl3 Cl1 Si2 Si1 -176.04(19) . . . . ? N1 Si1 Si2 N3 32.2(3) . . . . ? N2 Si1 Si2 N3 -72.8(3) . . . . ? Cl2 Si1 Si2 N3 158.61(19) . . . . ? N1 Si1 Si2 N4 -73.1(3) . . . . ? N2 Si1 Si2 N4 -178.1(2) . . . . ? Cl2 Si1 Si2 N4 53.3(2) . . . . ? N1 Si1 Si2 Cl1 158.4(2) . . . . ? N2 Si1 Si2 Cl1 53.4(2) . . . . ? Cl2 Si1 Si2 Cl1 -75.20(15) . . . . ? N2 Si1 N1 C1 0.8(4) . . . . ? Cl2 Si1 N1 C1 117.8(3) . . . . ? Si2 Si1 N1 C1 -119.2(3) . . . . ? N2 Si1 N1 C7 155.5(5) . . . . ? Cl2 Si1 N1 C7 -87.5(5) . . . . ? Si2 Si1 N1 C7 35.5(5) . . . . ? N1 Si1 N2 C2 -1.4(4) . . . . ? Cl2 Si1 N2 C2 -120.4(3) . . . . ? Si2 Si1 N2 C2 112.7(3) . . . . ? N1 Si1 N2 C12 -161.3(5) . . . . ? Cl2 Si1 N2 C12 79.6(5) . . . . ? Si2 Si1 N2 C12 -47.3(5) . . . . ? N4 Si2 N3 C17 3.3(4) . . . . ? Cl1 Si2 N3 C17 119.9(3) . . . . ? Si1 Si2 N3 C17 -117.3(3) . . . . ? N4 Si2 N3 C23 158.0(5) . . . . ? Cl1 Si2 N3 C23 -85.4(5) . . . . ? Si1 Si2 N3 C23 37.4(5) . . . . ? N3 Si2 N4 C18 -2.3(4) . . . . ? Cl1 Si2 N4 C18 -121.5(3) . . . . ? Si1 Si2 N4 C18 111.3(3) . . . . ? N3 Si2 N4 C28 -164.4(5) . . . . ? Cl1 Si2 N4 C28 76.5(5) . . . . ? Si1 Si2 N4 C28 -50.7(5) . . . . ? C7 N1 C1 C6 20.1(8) . . . . ? Si1 N1 C1 C6 176.6(5) . . . . ? C7 N1 C1 C2 -156.4(5) . . . . ? Si1 N1 C1 C2 0.1(6) . . . . ? C12 N2 C2 C3 -14.2(8) . . . . ? Si1 N2 C2 C3 -176.0(5) . . . . ? C12 N2 C2 C1 163.4(5) . . . . ? Si1 N2 C2 C1 1.7(5) . . . . ? C6 C1 C2 C3 -0.2(8) . . . . ? N1 C1 C2 C3 176.7(5) . . . . ? C6 C1 C2 N2 -178.0(5) . . . . ? N1 C1 C2 N2 -1.1(6) . . . . ? N2 C2 C3 C4 176.9(5) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? C2 C3 C4 C5 0.7(9) . . . . ? C3 C4 C5 C6 -0.1(9) . . . . ? N1 C1 C6 C5 -175.5(5) . . . . ? C2 C1 C6 C5 0.8(8) . . . . ? C4 C5 C6 C1 -0.7(9) . . . . ? C1 N1 C7 C8 -106.3(6) . . . . ? Si1 N1 C7 C8 101.0(6) . . . . ? N1 C7 C8 C11 52.4(8) . . . . ? N1 C7 C8 C9 -68.6(8) . . . . ? N1 C7 C8 C10 172.1(6) . . . . ? C2 N2 C12 C13 101.2(6) . . . . ? Si1 N2 C12 C13 -100.6(6) . . . . ? N2 C12 C13 C16 -52.9(8) . . . . ? N2 C12 C13 C14 68.7(7) . . . . ? N2 C12 C13 C15 -174.0(6) . . . . ? C23 N3 C17 C22 19.4(8) . . . . ? Si2 N3 C17 C22 175.0(5) . . . . ? C23 N3 C17 C18 -159.0(5) . . . . ? Si2 N3 C17 C18 -3.5(5) . . . . ? C22 C17 C18 C19 0.9(8) . . . . ? N3 C17 C18 C19 179.4(5) . . . . ? C22 C17 C18 N4 -176.8(5) . . . . ? N3 C17 C18 N4 1.8(6) . . . . ? C28 N4 C18 C19 -12.7(8) . . . . ? Si2 N4 C18 C19 -176.7(5) . . . . ? C28 N4 C18 C17 164.7(5) . . . . ? Si2 N4 C18 C17 0.7(6) . . . . ? C17 C18 C19 C20 -0.3(9) . . . . ? N4 C18 C19 C20 177.0(5) . . . . ? C18 C19 C20 C21 -0.3(9) . . . . ? C19 C20 C21 C22 0.4(9) . . . . ? N3 C17 C22 C21 -179.1(5) . . . . ? C18 C17 C22 C21 -0.8(8) . . . . ? C20 C21 C22 C17 0.1(9) . . . . ? C17 N3 C23 C24 -102.8(6) . . . . ? Si2 N3 C23 C24 105.1(5) . . . . ? N3 C23 C24 C27 -56.2(8) . . . . ? N3 C23 C24 C26 -175.2(6) . . . . ? N3 C23 C24 C25 66.2(8) . . . . ? C18 N4 C28 C29 99.8(6) . . . . ? Si2 N4 C28 C29 -99.7(6) . . . . ? N4 C28 C29 C32 -44.6(8) . . . . ? N4 C28 C29 C31 -166.2(6) . . . . ? N4 C28 C29 C30 76.3(7) . . . . ? #===END data_(4b)-oct1704 _database_code_depnum_ccdc_archive 'CCDC 273149' _audit_creation_date 2004-10-19T14:06:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C35 H58 Cl2 N4 Si2' _chemical_formula_sum 'C35 H58 Cl2 N4 Si2' _chemical_formula_weight 661.93 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5407(3) _cell_length_b 11.9325(4) _cell_length_c 17.3185(5) _cell_angle_alpha 90.626(2) _cell_angle_beta 98.687(2) _cell_angle_gamma 104.831(1) _cell_volume 1881.53(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15530 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.402147E-1 _diffrn_orient_matrix_ub_12 -0.186248E-1 _diffrn_orient_matrix_ub_13 -0.472258E-1 _diffrn_orient_matrix_ub_21 -0.603994E-1 _diffrn_orient_matrix_ub_22 -0.82156E-1 _diffrn_orient_matrix_ub_23 -0.13006E-2 _diffrn_orient_matrix_ub_31 -0.824409E-1 _diffrn_orient_matrix_ub_32 0.209641E-1 _diffrn_orient_matrix_ub_33 -0.344846E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0525 _diffrn_reflns_number 27787 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 26.08 _diffrn_reflns_theta_full 26.08 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 7412 _reflns_number_gt 5578 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+1.2395P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7412 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1055 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.546 _refine_diff_density_min -0.33 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Si1 Si 0.16364(7) 0.35155(5) 0.27928(3) 0.01906(15) Uani 1 1 d . . . Si2 Si 0.32227(7) 0.45436(5) 0.19790(3) 0.01875(15) Uani 1 1 d . . . Cl1 Cl 0.29672(7) 0.38406(5) 0.38770(3) 0.03106(15) Uani 1 1 d . . . Cl2 Cl 0.50327(6) 0.38432(5) 0.20659(4) 0.03107(16) Uani 1 1 d . . . N1 N 0.0960(2) 0.20526(15) 0.25817(11) 0.0208(4) Uani 1 1 d . . . N2 N -0.1036(2) 0.30864(15) 0.31427(10) 0.0200(4) Uani 1 1 d . . . N3 N 0.2475(2) 0.46142(15) 0.10223(10) 0.0207(4) Uani 1 1 d . . . N4 N 0.37914(19) 0.60273(14) 0.21532(10) 0.0193(4) Uani 1 1 d . . . C1 C -0.0569(2) 0.16176(18) 0.22935(12) 0.0199(5) Uani 1 1 d . . . C2 C -0.1584(2) 0.21139(18) 0.25941(12) 0.0198(5) Uani 1 1 d . . . C3 C -0.3076(3) 0.16411(19) 0.23265(14) 0.0250(5) Uani 1 1 d . . . H3 H -0.377 0.1958 0.2531 0.03 Uiso 1 1 calc R . . C4 C -0.3578(3) 0.0723(2) 0.17712(14) 0.0294(6) Uani 1 1 d . . . H4 H -0.4602 0.0408 0.1607 0.035 Uiso 1 1 calc R . . C5 C -0.2582(3) 0.02712(19) 0.14609(14) 0.0297(6) Uani 1 1 d . . . H5 H -0.2916 -0.0348 0.1073 0.036 Uiso 1 1 calc R . . C6 C -0.1097(3) 0.07197(19) 0.17135(14) 0.0268(5) Uani 1 1 d . . . H6 H -0.0417 0.0412 0.1488 0.032 Uiso 1 1 calc R . . C7 C 0.1952(3) 0.12905(19) 0.25627(15) 0.0270(5) Uani 1 1 d . . . H7A H 0.2971 0.1787 0.2625 0.032 Uiso 1 1 calc R . . H7B H 0.1732 0.0891 0.2037 0.032 Uiso 1 1 calc R . . C8 C 0.1898(3) 0.0358(2) 0.31771(16) 0.0322(6) Uani 1 1 d . . . C9 C 0.2220(6) 0.0919(3) 0.3997(2) 0.1032(18) Uani 1 1 d . . . H9A H 0.3163 0.1507 0.4065 0.155 Uiso 1 1 calc R . . H9B H 0.2264 0.0325 0.438 0.155 Uiso 1 1 calc R . . H9C H 0.144 0.1286 0.4075 0.155 Uiso 1 1 calc R . . C10 C 0.0458(4) -0.0544(3) 0.3082(3) 0.0792(13) Uani 1 1 d . . . H10A H -0.0323 -0.0176 0.3158 0.119 Uiso 1 1 calc R . . H10B H 0.0508 -0.1129 0.3471 0.119 Uiso 1 1 calc R . . H10C H 0.0246 -0.0918 0.2556 0.119 Uiso 1 1 calc R . . C11 C 0.3095(4) -0.0223(3) 0.3073(3) 0.0891(15) Uani 1 1 d . . . H11A H 0.4042 0.0361 0.3135 0.134 Uiso 1 1 calc R . . H11B H 0.2886 -0.0605 0.2549 0.134 Uiso 1 1 calc R . . H11C H 0.3133 -0.0803 0.3467 0.134 Uiso 1 1 calc R . . C12 C -0.2026(3) 0.33354(19) 0.36550(13) 0.0239(5) Uani 1 1 d . . . H12A H -0.3038 0.313 0.3361 0.029 Uiso 1 1 calc R . . H12B H -0.1746 0.418 0.3789 0.029 Uiso 1 1 calc R . . C13 C -0.2021(3) 0.2688(2) 0.44185(14) 0.0295(6) Uani 1 1 d . . . C14 C -0.3075(3) 0.3092(3) 0.48733(16) 0.0459(7) Uani 1 1 d . . . H14A H -0.4063 0.289 0.4565 0.069 Uiso 1 1 calc R . . H14B H -0.2739 0.3936 0.4975 0.069 Uiso 1 1 calc R . . H14C H -0.3098 0.2711 0.5371 0.069 Uiso 1 1 calc R . . C15 C -0.0484(3) 0.3001(2) 0.48977(15) 0.0379(6) Uani 1 1 d . . . H15A H -0.0497 0.2584 0.5382 0.057 Uiso 1 1 calc R . . H15B H -0.0169 0.3839 0.5026 0.057 Uiso 1 1 calc R . . H15C H 0.02 0.2782 0.4594 0.057 Uiso 1 1 calc R . . C16 C -0.2543(4) 0.1372(2) 0.42623(16) 0.0492(8) Uani 1 1 d . . . H16A H -0.3532 0.1167 0.3955 0.074 Uiso 1 1 calc R . . H16B H -0.2564 0.0993 0.4761 0.074 Uiso 1 1 calc R . . H16C H -0.1869 0.1113 0.3971 0.074 Uiso 1 1 calc R . . C17 C 0.2821(2) 0.57814(18) 0.08068(13) 0.0205(5) Uani 1 1 d . . . C18 C 0.3553(2) 0.65732(18) 0.14429(13) 0.0207(5) Uani 1 1 d . . . C19 C 0.3943(3) 0.77555(19) 0.13274(14) 0.0269(5) Uani 1 1 d . . . H19 H 0.4433 0.8293 0.1752 0.032 Uiso 1 1 calc R . . C20 C 0.3609(3) 0.8147(2) 0.05858(15) 0.0347(6) Uani 1 1 d . . . H20 H 0.3873 0.8956 0.0506 0.042 Uiso 1 1 calc R . . C21 C 0.2901(3) 0.7375(2) -0.00357(15) 0.0354(6) Uani 1 1 d . . . H21 H 0.2682 0.7655 -0.0539 0.042 Uiso 1 1 calc R . . C22 C 0.2505(3) 0.6187(2) 0.00737(14) 0.0283(5) Uani 1 1 d . . . H22 H 0.2019 0.5657 -0.0355 0.034 Uiso 1 1 calc R . . C23 C 0.1417(2) 0.37072(19) 0.04937(13) 0.0246(5) Uani 1 1 d . . . H23A H 0.0787 0.4089 0.014 0.03 Uiso 1 1 calc R . . H23B H 0.0775 0.3192 0.0815 0.03 Uiso 1 1 calc R . . C24 C 0.2036(3) 0.2933(2) -0.00185(14) 0.0282(5) Uani 1 1 d . . . C25 C 0.2456(4) 0.1975(2) 0.04607(17) 0.0499(8) Uani 1 1 d . . . H25A H 0.3243 0.2319 0.0894 0.075 Uiso 1 1 calc R . . H25B H 0.2796 0.1465 0.0127 0.075 Uiso 1 1 calc R . . H25C H 0.1598 0.1522 0.067 0.075 Uiso 1 1 calc R . . C26 C 0.0799(4) 0.2389(3) -0.06919(18) 0.0548(8) Uani 1 1 d . . . H26A H 0.0529 0.3005 -0.1004 0.082 Uiso 1 1 calc R . . H26B H -0.0057 0.1943 -0.0479 0.082 Uiso 1 1 calc R . . H26C H 0.1135 0.1873 -0.1024 0.082 Uiso 1 1 calc R . . C27 C 0.3364(3) 0.3628(2) -0.03467(18) 0.0473(8) Uani 1 1 d . . . H27A H 0.3094 0.4244 -0.0658 0.071 Uiso 1 1 calc R . . H27B H 0.3701 0.3113 -0.0679 0.071 Uiso 1 1 calc R . . H27C H 0.4153 0.3974 0.0085 0.071 Uiso 1 1 calc R . . C28 C 0.4346(2) 0.67287(19) 0.28923(13) 0.0224(5) Uani 1 1 d . . . H28A H 0.3835 0.6309 0.3303 0.027 Uiso 1 1 calc R . . H28B H 0.4049 0.7464 0.2831 0.027 Uiso 1 1 calc R . . C29 C 0.6024(3) 0.70436(19) 0.32012(13) 0.0261(5) Uani 1 1 d . . . C30 C 0.6929(3) 0.7184(2) 0.25389(15) 0.0360(6) Uani 1 1 d . . . H30A H 0.6696 0.7788 0.2202 0.054 Uiso 1 1 calc R . . H30B H 0.6696 0.6448 0.2231 0.054 Uiso 1 1 calc R . . H30C H 0.7976 0.7408 0.2758 0.054 Uiso 1 1 calc R . . C31 C 0.6397(3) 0.6109(2) 0.37293(16) 0.0406(7) Uani 1 1 d . . . H31A H 0.5817 0.6019 0.4157 0.061 Uiso 1 1 calc R . . H31B H 0.7445 0.6337 0.3946 0.061 Uiso 1 1 calc R . . H31C H 0.6166 0.537 0.3424 0.061 Uiso 1 1 calc R . . C32 C 0.6396(3) 0.8191(2) 0.36893(18) 0.0460(7) Uani 1 1 d . . . H32A H 0.6165 0.8799 0.3357 0.069 Uiso 1 1 calc R . . H32B H 0.7445 0.841 0.3906 0.069 Uiso 1 1 calc R . . H32C H 0.5817 0.8097 0.4117 0.069 Uiso 1 1 calc R . . C33 C -0.0032(2) 0.40883(18) 0.28058(13) 0.0204(5) Uani 1 1 d . . . C34 C 0.0406(3) 0.5205(2) 0.33274(15) 0.0299(6) Uani 1 1 d . . . H34A H 0.0837 0.505 0.3852 0.045 Uiso 1 1 calc R . . H34B H -0.0467 0.5483 0.336 0.045 Uiso 1 1 calc R . . H34C H 0.1126 0.5798 0.3104 0.045 Uiso 1 1 calc R . . C35 C -0.0709(3) 0.4367(2) 0.19924(13) 0.0258(5) Uani 1 1 d . . . H35A H -0.0999 0.3663 0.1646 0.039 Uiso 1 1 calc R . . H35B H 0.0015 0.4967 0.1776 0.039 Uiso 1 1 calc R . . H35C H -0.1575 0.4648 0.2036 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0202(3) 0.0161(3) 0.0198(3) 0.0003(2) 0.0029(2) 0.0030(2) Si2 0.0191(3) 0.0168(3) 0.0197(3) -0.0009(2) 0.0037(2) 0.0032(2) Cl1 0.0294(3) 0.0341(3) 0.0237(3) -0.0003(2) -0.0032(2) 0.0020(3) Cl2 0.0252(3) 0.0295(3) 0.0410(4) 0.0009(3) 0.0053(3) 0.0118(2) N1 0.0206(10) 0.0153(9) 0.0261(10) 0.0003(7) 0.0029(8) 0.0042(7) N2 0.0225(10) 0.0170(9) 0.0196(10) -0.0027(7) 0.0065(8) 0.0018(8) N3 0.0217(10) 0.0188(9) 0.0198(10) -0.0023(7) 0.0037(8) 0.0021(8) N4 0.0227(10) 0.0168(9) 0.0166(9) -0.0021(7) 0.0016(8) 0.0028(7) C1 0.0231(12) 0.0156(10) 0.0194(11) 0.0027(8) 0.0030(9) 0.0024(9) C2 0.0234(12) 0.0163(11) 0.0182(11) 0.0020(8) 0.0040(9) 0.0019(9) C3 0.0244(13) 0.0208(12) 0.0296(13) 0.0005(10) 0.0032(10) 0.0059(10) C4 0.0256(13) 0.0234(12) 0.0327(14) -0.0021(10) -0.0034(11) -0.0006(10) C5 0.0374(15) 0.0166(11) 0.0295(13) -0.0064(10) -0.0004(11) 0.0009(10) C6 0.0325(14) 0.0208(12) 0.0265(13) -0.0061(9) 0.0041(11) 0.0063(10) C7 0.0224(13) 0.0205(12) 0.0391(14) 0.0019(10) 0.0090(11) 0.0051(10) C8 0.0297(14) 0.0238(13) 0.0447(16) 0.0062(11) 0.0046(12) 0.0108(11) C9 0.214(6) 0.055(2) 0.049(2) 0.0183(18) 0.004(3) 0.058(3) C10 0.055(2) 0.062(2) 0.107(3) 0.055(2) 0.001(2) -0.0033(18) C11 0.069(3) 0.064(2) 0.158(4) 0.056(3) 0.043(3) 0.045(2) C12 0.0235(12) 0.0253(12) 0.0234(12) -0.0019(9) 0.0064(10) 0.0060(10) C13 0.0325(14) 0.0329(13) 0.0217(12) 0.0002(10) 0.0084(11) 0.0037(11) C14 0.0368(16) 0.071(2) 0.0289(15) -0.0016(14) 0.0140(13) 0.0076(14) C15 0.0389(16) 0.0508(17) 0.0246(14) 0.0014(12) 0.0051(12) 0.0130(13) C16 0.076(2) 0.0333(15) 0.0310(15) 0.0097(12) 0.0115(15) -0.0012(14) C17 0.0185(11) 0.0196(11) 0.0226(12) -0.0005(9) 0.0034(9) 0.0034(9) C18 0.0195(12) 0.0220(11) 0.0214(12) 0.0017(9) 0.0042(9) 0.0059(9) C19 0.0296(13) 0.0198(12) 0.0279(13) -0.0012(10) 0.0014(11) 0.0023(10) C20 0.0396(15) 0.0234(13) 0.0381(15) 0.0078(11) 0.0020(12) 0.0050(11) C21 0.0407(16) 0.0341(14) 0.0295(14) 0.0100(11) 0.0003(12) 0.0090(12) C22 0.0290(13) 0.0302(13) 0.0226(12) -0.0007(10) -0.0008(10) 0.0050(10) C23 0.0228(12) 0.0233(12) 0.0240(12) -0.0051(9) 0.0047(10) -0.0011(9) C24 0.0320(14) 0.0269(13) 0.0240(13) -0.0063(10) 0.0055(11) 0.0041(10) C25 0.079(2) 0.0357(16) 0.0406(17) -0.0029(13) 0.0119(16) 0.0240(15) C26 0.055(2) 0.0548(19) 0.0486(19) -0.0276(15) -0.0050(15) 0.0135(16) C27 0.0557(19) 0.0427(16) 0.0481(18) -0.0070(13) 0.0311(15) 0.0084(14) C28 0.0258(12) 0.0194(11) 0.0200(12) -0.0039(9) 0.0025(10) 0.0033(9) C29 0.0243(13) 0.0246(12) 0.0246(12) -0.0057(9) -0.0007(10) 0.0007(10) C30 0.0265(14) 0.0396(15) 0.0387(15) 0.0001(12) 0.0078(12) 0.0013(11) C31 0.0304(15) 0.0479(17) 0.0376(15) 0.0042(13) -0.0060(12) 0.0062(12) C32 0.0345(16) 0.0432(17) 0.0507(18) -0.0234(14) -0.0018(13) -0.0014(13) C33 0.0235(12) 0.0157(11) 0.0212(12) -0.0017(9) 0.0055(9) 0.0028(9) C34 0.0299(14) 0.0231(12) 0.0353(14) -0.0083(10) 0.0101(11) 0.0017(10) C35 0.0272(13) 0.0247(12) 0.0270(13) 0.0062(10) 0.0067(10) 0.0082(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.7133(18) . ? Si1 C33 1.889(2) . ? Si1 Cl1 2.0737(8) . ? Si1 Si2 2.3481(8) . ? Si2 N3 1.7139(19) . ? Si2 N4 1.7225(18) . ? Si2 Cl2 2.0896(8) . ? N1 C1 1.426(3) . ? N1 C7 1.474(3) . ? N2 C2 1.428(3) . ? N2 C12 1.469(3) . ? N2 C33 1.511(3) . ? N3 C17 1.415(3) . ? N3 C23 1.472(3) . ? N4 C18 1.414(3) . ? N4 C28 1.471(3) . ? C1 C6 1.399(3) . ? C1 C2 1.414(3) . ? C2 C3 1.393(3) . ? C3 C4 1.387(3) . ? C4 C5 1.376(3) . ? C5 C6 1.380(3) . ? C7 C8 1.545(3) . ? C8 C10 1.498(4) . ? C8 C11 1.512(4) . ? C8 C9 1.516(4) . ? C12 C13 1.539(3) . ? C13 C15 1.524(4) . ? C13 C16 1.529(4) . ? C13 C14 1.531(3) . ? C17 C22 1.382(3) . ? C17 C18 1.414(3) . ? C18 C19 1.389(3) . ? C19 C20 1.391(3) . ? C20 C21 1.380(4) . ? C21 C22 1.393(3) . ? C23 C24 1.552(3) . ? C24 C27 1.518(4) . ? C24 C25 1.520(4) . ? C24 C26 1.533(4) . ? C28 C29 1.556(3) . ? C29 C30 1.522(3) . ? C29 C31 1.528(4) . ? C29 C32 1.533(3) . ? C33 C34 1.530(3) . ? C33 C35 1.535(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C33 105.32(9) . . ? N1 Si1 Cl1 110.79(7) . . ? C33 Si1 Cl1 110.08(7) . . ? N1 Si1 Si2 116.57(7) . . ? C33 Si1 Si2 112.55(7) . . ? Cl1 Si1 Si2 101.57(3) . . ? N3 Si2 N4 94.39(9) . . ? N3 Si2 Cl2 111.43(7) . . ? N4 Si2 Cl2 110.41(7) . . ? N3 Si2 Si1 116.58(7) . . ? N4 Si2 Si1 116.13(6) . . ? Cl2 Si2 Si1 107.50(3) . . ? C1 N1 C7 119.87(17) . . ? C1 N1 Si1 118.12(14) . . ? C7 N1 Si1 121.15(15) . . ? C2 N2 C12 118.01(17) . . ? C2 N2 C33 111.58(16) . . ? C12 N2 C33 118.86(16) . . ? C17 N3 C23 120.25(18) . . ? C17 N3 Si2 109.65(14) . . ? C23 N3 Si2 129.33(15) . . ? C18 N4 C28 120.16(17) . . ? C18 N4 Si2 109.28(14) . . ? C28 N4 Si2 130.41(15) . . ? C6 C1 C2 118.8(2) . . ? C6 C1 N1 121.9(2) . . ? C2 C1 N1 119.28(19) . . ? C3 C2 C1 118.12(19) . . ? C3 C2 N2 123.20(19) . . ? C1 C2 N2 118.66(19) . . ? C4 C3 C2 122.1(2) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 119.9(2) . . ? C5 C6 C1 121.5(2) . . ? N1 C7 C8 117.27(18) . . ? C10 C8 C11 108.9(3) . . ? C10 C8 C9 108.9(3) . . ? C11 C8 C9 108.7(3) . . ? C10 C8 C7 113.4(2) . . ? C11 C8 C7 106.4(2) . . ? C9 C8 C7 110.4(2) . . ? N2 C12 C13 114.67(19) . . ? C15 C13 C16 109.2(2) . . ? C15 C13 C14 109.6(2) . . ? C16 C13 C14 109.4(2) . . ? C15 C13 C12 110.3(2) . . ? C16 C13 C12 111.9(2) . . ? C14 C13 C12 106.4(2) . . ? C22 C17 C18 119.9(2) . . ? C22 C17 N3 127.2(2) . . ? C18 C17 N3 112.88(19) . . ? C19 C18 N4 127.1(2) . . ? C19 C18 C17 119.7(2) . . ? N4 C18 C17 113.20(18) . . ? C18 C19 C20 119.5(2) . . ? C21 C20 C19 120.8(2) . . ? C20 C21 C22 120.1(2) . . ? C17 C22 C21 119.9(2) . . ? N3 C23 C24 117.84(19) . . ? C27 C24 C25 109.4(2) . . ? C27 C24 C26 109.6(2) . . ? C25 C24 C26 109.2(2) . . ? C27 C24 C23 112.04(19) . . ? C25 C24 C23 109.8(2) . . ? C26 C24 C23 106.7(2) . . ? N4 C28 C29 118.44(18) . . ? C30 C29 C31 109.4(2) . . ? C30 C29 C32 109.6(2) . . ? C31 C29 C32 108.6(2) . . ? C30 C29 C28 112.09(19) . . ? C31 C29 C28 110.06(19) . . ? C32 C29 C28 106.95(19) . . ? N2 C33 C34 113.29(17) . . ? N2 C33 C35 112.39(18) . . ? C34 C33 C35 107.85(18) . . ? N2 C33 Si1 100.91(13) . . ? C34 C33 Si1 109.10(16) . . ? C35 C33 Si1 113.27(14) . . ? #===END data_(11d)-sep1504 _database_code_depnum_ccdc_archive 'CCDC 273150' _audit_creation_date 2004-09-10T16:39:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C65 H106 Br2 N8 Si4, 1.5(C6 H6)' _chemical_formula_sum 'C74 H115 Br2 N8 Si4' _chemical_formula_weight 1388.92 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.8293(3) _cell_length_b 15.1696(3) _cell_length_c 19.1719(3) _cell_angle_alpha 87.796(1) _cell_angle_beta 67.561(1) _cell_angle_gamma 76.029(1) _cell_volume 3861.41(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34268 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1482 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.156 _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 0.7024 _exptl_absorpt_correction_T_max 0.8304 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.736879E-1 _diffrn_orient_matrix_ub_12 -0.23609E-1 _diffrn_orient_matrix_ub_13 -0.121091E-1 _diffrn_orient_matrix_ub_21 -0.152519E-1 _diffrn_orient_matrix_ub_22 -0.36216E-1 _diffrn_orient_matrix_ub_23 0.459599E-1 _diffrn_orient_matrix_ub_31 0.13337E-2 _diffrn_orient_matrix_ub_32 -0.525568E-1 _diffrn_orient_matrix_ub_33 -0.306128E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0446 _diffrn_reflns_number 52154 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 13561 _reflns_number_gt 10267 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+3.5470P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13561 _refine_ls_number_parameters 793 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.34 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.053 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' 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 Br1 Br 0.98302(2) 0.48993(2) 0.147019(16) 0.04346(10) Uani 1 1 d . . . Br2 Br 0.43426(2) 0.86343(2) 0.373863(16) 0.04686(10) Uani 1 1 d . . . Si1 Si 0.52002(6) 0.85982(5) 0.24775(4) 0.02872(17) Uani 1 1 d . . . Si2 Si 0.69798(5) 0.83567(5) 0.21489(4) 0.02509(17) Uani 1 1 d . . . Si3 Si 0.83208(5) 0.67651(5) 0.29309(4) 0.02465(16) Uani 1 1 d . . . Si4 Si 0.88218(6) 0.51420(5) 0.27207(4) 0.02769(17) Uani 1 1 d . . . N1 N 0.47848(16) 0.95019(15) 0.20076(12) 0.0312(5) Uani 1 1 d . . . N2 N 0.48142(17) 0.78433(15) 0.20660(12) 0.0322(5) Uani 1 1 d . . . N3 N 0.73861(16) 0.85255(15) 0.11838(12) 0.0297(5) Uani 1 1 d . . . N4 N 0.74876(16) 0.92002(14) 0.23290(12) 0.0300(5) Uani 1 1 d . . . N5 N 0.93882(16) 0.71517(14) 0.27910(12) 0.0284(5) Uani 1 1 d . . . N6 N 0.77513(16) 0.71461(15) 0.38754(11) 0.0293(5) Uani 1 1 d . . . N7 N 0.93103(16) 0.46245(14) 0.33602(12) 0.0292(5) Uani 1 1 d . . . N8 N 0.79905(17) 0.44627(14) 0.28909(12) 0.0313(5) Uani 1 1 d . . . C1 C 0.4454(2) 0.91970(19) 0.14782(15) 0.0331(7) Uani 1 1 d . . . C2 C 0.4463(2) 0.8261(2) 0.15174(15) 0.0342(7) Uani 1 1 d . . . C3 C 0.4195(2) 0.7847(2) 0.10215(17) 0.0444(8) Uani 1 1 d . . . H3 H 0.42 0.7219 0.1048 0.053 Uiso 1 1 calc R . . C4 C 0.3922(3) 0.8350(3) 0.04868(18) 0.0545(9) Uani 1 1 d . . . H4 H 0.3723 0.8069 0.0153 0.065 Uiso 1 1 calc R . . C5 C 0.3934(3) 0.9253(3) 0.04331(18) 0.0519(9) Uani 1 1 d . . . H5 H 0.3757 0.9589 0.0056 0.062 Uiso 1 1 calc R . . C6 C 0.4205(2) 0.9679(2) 0.09279(16) 0.0421(7) Uani 1 1 d . . . H6 H 0.4218 1.0302 0.0885 0.051 Uiso 1 1 calc R . . C7 C 0.5067(2) 1.03765(18) 0.19463(17) 0.0391(7) Uani 1 1 d . . . H7A H 0.5334 1.05 0.1404 0.047 Uiso 1 1 calc R . . H7B H 0.5626 1.0302 0.2122 0.047 Uiso 1 1 calc R . . C8 C 0.4245(3) 1.1229(2) 0.2378(2) 0.0489(8) Uani 1 1 d . . . C9 C 0.4784(4) 1.1988(3) 0.2289(3) 0.0969(16) Uani 1 1 d . . . H9A H 0.5322 1.1803 0.2482 0.145 Uiso 1 1 calc R . . H9B H 0.4303 1.2541 0.2574 0.145 Uiso 1 1 calc R . . H9C H 0.5075 1.2109 0.1753 0.145 Uiso 1 1 calc R . . C10 C 0.3751(4) 1.1068(3) 0.3207(2) 0.0902(15) Uani 1 1 d . . . H10A H 0.4268 1.088 0.3421 0.135 Uiso 1 1 calc R . . H10B H 0.3393 1.0589 0.3262 0.135 Uiso 1 1 calc R . . H10C H 0.3274 1.1631 0.3477 0.135 Uiso 1 1 calc R . . C11 C 0.3439(3) 1.1519(3) 0.2052(3) 0.0790(13) Uani 1 1 d . . . H11A H 0.2938 1.2059 0.2343 0.118 Uiso 1 1 calc R . . H11B H 0.3111 1.1023 0.2079 0.118 Uiso 1 1 calc R . . H11C H 0.3749 1.166 0.1523 0.118 Uiso 1 1 calc R . . C12 C 0.4973(2) 0.68560(19) 0.21303(18) 0.0390(7) Uani 1 1 d . . . H12A H 0.5497 0.6655 0.2342 0.047 Uiso 1 1 calc R . . H12B H 0.5251 0.6568 0.1612 0.047 Uiso 1 1 calc R . . C13 C 0.4055(2) 0.6467(2) 0.26127(18) 0.0423(7) Uani 1 1 d . . . C14 C 0.3059(3) 0.7172(3) 0.2824(2) 0.0718(12) Uani 1 1 d . . . H14A H 0.2972 0.7403 0.2364 0.108 Uiso 1 1 calc R . . H14B H 0.3054 0.7676 0.3132 0.108 Uiso 1 1 calc R . . H14C H 0.2508 0.6892 0.3114 0.108 Uiso 1 1 calc R . . C15 C 0.4057(4) 0.5667(3) 0.2155(2) 0.0920(16) Uani 1 1 d . . . H15A H 0.3988 0.5877 0.1684 0.138 Uiso 1 1 calc R . . H15B H 0.3493 0.5404 0.245 0.138 Uiso 1 1 calc R . . H15C H 0.4691 0.5203 0.2037 0.138 Uiso 1 1 calc R . . C16 C 0.4164(3) 0.6145(3) 0.3340(2) 0.0745(12) Uani 1 1 d . . . H16A H 0.4802 0.5687 0.3222 0.112 Uiso 1 1 calc R . . H16B H 0.3605 0.5876 0.3633 0.112 Uiso 1 1 calc R . . H16C H 0.4155 0.6662 0.3635 0.112 Uiso 1 1 calc R . . C17 C 0.7819(2) 0.92757(18) 0.10250(16) 0.0388(7) Uani 1 1 d . . . C18 C 0.7922(2) 0.96239(18) 0.16550(16) 0.0366(7) Uani 1 1 d . . . C19 C 0.8449(3) 1.0290(2) 0.15659(19) 0.0599(10) Uani 1 1 d . . . H19 H 0.8566 1.0495 0.1979 0.072 Uiso 1 1 calc R . . C20 C 0.8804(4) 1.0652(3) 0.0862(2) 0.0906(17) Uani 1 1 d . . . H20 H 0.917 1.1104 0.0794 0.109 Uiso 1 1 calc R . . C21 C 0.8630(4) 1.0363(3) 0.0271(2) 0.0927(17) Uani 1 1 d . . . H21 H 0.8843 1.0643 -0.0196 0.111 Uiso 1 1 calc R . . C22 C 0.8147(3) 0.9664(2) 0.03403(18) 0.0611(11) Uani 1 1 d . . . H22 H 0.8044 0.9458 -0.0079 0.073 Uiso 1 1 calc R . . C23 C 0.7040(2) 0.8194(2) 0.06442(15) 0.0408(7) Uani 1 1 d . . . H23A H 0.6855 0.8715 0.0357 0.049 Uiso 1 1 calc R . . H23B H 0.6416 0.8 0.0939 0.049 Uiso 1 1 calc R . . C24 C 0.7765(2) 0.7401(2) 0.00644(15) 0.0421(7) Uani 1 1 d . . . C25 C 0.8760(3) 0.7604(3) -0.0424(2) 0.0701(12) Uani 1 1 d . . . H25A H 0.9111 0.7704 -0.0104 0.105 Uiso 1 1 calc R . . H25B H 0.8637 0.8152 -0.0695 0.105 Uiso 1 1 calc R . . H25C H 0.9175 0.7089 -0.0789 0.105 Uiso 1 1 calc R . . C26 C 0.7987(3) 0.6543(2) 0.04623(19) 0.0677(11) Uani 1 1 d . . . H26A H 0.8338 0.6643 0.0783 0.102 Uiso 1 1 calc R . . H26B H 0.8413 0.6042 0.0086 0.102 Uiso 1 1 calc R . . H26C H 0.7354 0.6389 0.0776 0.102 Uiso 1 1 calc R . . C27 C 0.7221(4) 0.7255(4) -0.0429(2) 0.0964(17) Uani 1 1 d . . . H27A H 0.7643 0.6754 -0.0807 0.145 Uiso 1 1 calc R . . H27B H 0.7081 0.7812 -0.0686 0.145 Uiso 1 1 calc R . . H27C H 0.6586 0.7106 -0.0116 0.145 Uiso 1 1 calc R . . C28 C 0.7718(2) 0.93374(18) 0.29938(16) 0.0359(7) Uani 1 1 d . . . H28A H 0.8406 0.9434 0.2808 0.043 Uiso 1 1 calc R . . H28B H 0.7735 0.8763 0.3258 0.043 Uiso 1 1 calc R . . C29 C 0.7017(2) 1.01185(18) 0.35860(16) 0.0372(7) Uani 1 1 d . . . C30 C 0.6940(3) 1.10514(19) 0.32539(18) 0.0531(9) Uani 1 1 d . . . H30A H 0.7612 1.1167 0.3025 0.08 Uiso 1 1 calc R . . H30B H 0.6503 1.1521 0.3656 0.08 Uiso 1 1 calc R . . H30C H 0.6656 1.1065 0.2867 0.08 Uiso 1 1 calc R . . C31 C 0.7468(3) 1.0106(3) 0.4183(2) 0.0714(12) Uani 1 1 d . . . H31A H 0.8149 1.02 0.3945 0.107 Uiso 1 1 calc R . . H31B H 0.7498 0.9517 0.4413 0.107 Uiso 1 1 calc R . . H31C H 0.7046 1.0593 0.4575 0.107 Uiso 1 1 calc R . . C32 C 0.5973(3) 0.9955(2) 0.3938(2) 0.0593(10) Uani 1 1 d . . . H32A H 0.5698 0.9955 0.3546 0.089 Uiso 1 1 calc R . . H32B H 0.5535 1.0439 0.4327 0.089 Uiso 1 1 calc R . . H32C H 0.6008 0.9366 0.4167 0.089 Uiso 1 1 calc R . . C33 C 0.7460(2) 0.71831(17) 0.24206(14) 0.0284(6) Uani 1 1 d . . . H33A H 0.6844 0.6978 0.2716 0.034 Uiso 1 1 calc R . . H33B H 0.7779 0.6807 0.1939 0.034 Uiso 1 1 calc R . . C34 C 0.9330(2) 0.74936(18) 0.34922(15) 0.0323(6) Uani 1 1 d . . . C35 C 0.8424(2) 0.74746(18) 0.40969(15) 0.0314(6) Uani 1 1 d . . . C36 C 0.8257(3) 0.7784(2) 0.48170(16) 0.0427(8) Uani 1 1 d . . . H36 H 0.7646 0.7773 0.5228 0.051 Uiso 1 1 calc R . . C37 C 0.8988(3) 0.8110(2) 0.49340(19) 0.0522(9) Uani 1 1 d . . . H37 H 0.8875 0.8324 0.5427 0.063 Uiso 1 1 calc R . . C38 C 0.9865(3) 0.8128(2) 0.4350(2) 0.0534(9) Uani 1 1 d . . . H38 H 1.036 0.8351 0.444 0.064 Uiso 1 1 calc R . . C39 C 1.0049(2) 0.7823(2) 0.36198(18) 0.0432(8) Uani 1 1 d . . . H39 H 1.0661 0.7841 0.3214 0.052 Uiso 1 1 calc R . . C40 C 1.0391(2) 0.68573(19) 0.21761(16) 0.0356(7) Uani 1 1 d . . . H40A H 1.0441 0.6257 0.196 0.043 Uiso 1 1 calc R . . H40B H 1.0903 0.6767 0.2403 0.043 Uiso 1 1 calc R . . C41 C 1.0675(2) 0.7490(2) 0.15200(16) 0.0386(7) Uani 1 1 d . . . C42 C 1.0725(3) 0.8403(2) 0.17923(19) 0.0536(9) Uani 1 1 d . . . H42A H 1.1214 0.83 0.2034 0.08 Uiso 1 1 calc R . . H42B H 1.006 0.8716 0.2158 0.08 Uiso 1 1 calc R . . H42C H 1.0934 0.8779 0.136 0.08 Uiso 1 1 calc R . . C43 C 0.9924(2) 0.7631(2) 0.11407(18) 0.0493(8) Uani 1 1 d . . . H43A H 0.9255 0.794 0.1503 0.074 Uiso 1 1 calc R . . H43B H 0.9903 0.7039 0.0968 0.074 Uiso 1 1 calc R . . H43C H 1.0131 0.8004 0.0707 0.074 Uiso 1 1 calc R . . C44 C 1.1721(2) 0.6999(3) 0.09525(19) 0.0582(10) Uani 1 1 d . . . H44A H 1.2208 0.6911 0.1195 0.087 Uiso 1 1 calc R . . H44B H 1.1927 0.7367 0.0515 0.087 Uiso 1 1 calc R . . H44C H 1.1696 0.6406 0.0786 0.087 Uiso 1 1 calc R . . C45 C 0.6678(2) 0.73392(19) 0.43771(15) 0.0362(7) Uani 1 1 d . . . H45A H 0.6277 0.7542 0.4064 0.043 Uiso 1 1 calc R . . H45B H 0.6536 0.7856 0.4734 0.043 Uiso 1 1 calc R . . C46 C 0.6297(2) 0.6557(2) 0.48427(16) 0.0371(7) Uani 1 1 d . . . C47 C 0.7038(3) 0.6026(3) 0.5170(2) 0.0649(11) Uani 1 1 d . . . H47A H 0.7673 0.5742 0.4758 0.097 Uiso 1 1 calc R . . H47B H 0.6757 0.5554 0.5479 0.097 Uiso 1 1 calc R . . H47C H 0.716 0.6441 0.5485 0.097 Uiso 1 1 calc R . . C48 C 0.5301(3) 0.6990(3) 0.5478(2) 0.0693(11) Uani 1 1 d . . . H48A H 0.4826 0.7326 0.5262 0.104 Uiso 1 1 calc R . . H48B H 0.541 0.7409 0.5797 0.104 Uiso 1 1 calc R . . H48C H 0.5025 0.6514 0.5783 0.104 Uiso 1 1 calc R . . C49 C 0.6113(3) 0.5933(3) 0.4343(2) 0.0632(10) Uani 1 1 d . . . H49A H 0.5629 0.6281 0.4141 0.095 Uiso 1 1 calc R . . H49B H 0.5843 0.5448 0.464 0.095 Uiso 1 1 calc R . . H49C H 0.6748 0.5663 0.3925 0.095 Uiso 1 1 calc R . . C50 C 0.8743(2) 0.40029(17) 0.37696(15) 0.0313(6) Uani 1 1 d . . . C51 C 0.8009(2) 0.39134(18) 0.35004(16) 0.0340(7) Uani 1 1 d . . . C52 C 0.7368(2) 0.3360(2) 0.38542(18) 0.0437(8) Uani 1 1 d . . . H52 H 0.6881 0.3285 0.3667 0.052 Uiso 1 1 calc R . . C53 C 0.7443(3) 0.2916(2) 0.44851(19) 0.0525(9) Uani 1 1 d . . . H53 H 0.7003 0.2538 0.473 0.063 Uiso 1 1 calc R . . C54 C 0.8143(3) 0.3019(2) 0.47565(18) 0.0484(8) Uani 1 1 d . . . H54 H 0.8177 0.2717 0.5193 0.058 Uiso 1 1 calc R . . C55 C 0.8807(2) 0.35608(19) 0.44003(17) 0.0404(7) Uani 1 1 d . . . H55 H 0.9296 0.3626 0.4588 0.048 Uiso 1 1 calc R . . C56 C 0.9959(2) 0.49669(19) 0.36405(16) 0.0357(7) Uani 1 1 d . . . H56A H 0.9673 0.4966 0.4199 0.043 Uiso 1 1 calc R . . H56B H 0.9916 0.5609 0.351 0.043 Uiso 1 1 calc R . . C57 C 1.1082(2) 0.4469(2) 0.33624(18) 0.0413(7) Uani 1 1 d . . . C58 C 1.1571(3) 0.5044(3) 0.3683(2) 0.0631(10) Uani 1 1 d . . . H58A H 1.1256 0.5084 0.4237 0.095 Uiso 1 1 calc R . . H58B H 1.1477 0.5656 0.3497 0.095 Uiso 1 1 calc R . . H58C H 1.2292 0.4759 0.3522 0.095 Uiso 1 1 calc R . . C59 C 1.1575(3) 0.4394(3) 0.25033(19) 0.0605(10) Uani 1 1 d . . . H59A H 1.1255 0.4031 0.2301 0.091 Uiso 1 1 calc R . . H59B H 1.2293 0.4098 0.2345 0.091 Uiso 1 1 calc R . . H59C H 1.1495 0.5003 0.2311 0.091 Uiso 1 1 calc R . . C60 C 1.1238(3) 0.3516(2) 0.3657(2) 0.0576(10) Uani 1 1 d . . . H60A H 1.0924 0.3144 0.3458 0.086 Uiso 1 1 calc R . . H60B H 1.093 0.3559 0.421 0.086 Uiso 1 1 calc R . . H60C H 1.196 0.3234 0.349 0.086 Uiso 1 1 calc R . . C61 C 0.7243(2) 0.44873(19) 0.25639(18) 0.0403(7) Uani 1 1 d . . . H61A H 0.7132 0.5083 0.234 0.048 Uiso 1 1 calc R . . H61B H 0.6602 0.4465 0.2982 0.048 Uiso 1 1 calc R . . C62 C 0.7475(3) 0.3729(2) 0.19494(19) 0.0493(8) Uani 1 1 d . . . C63 C 0.7702(4) 0.4135(3) 0.1182(2) 0.0883(15) Uani 1 1 d . . . H63A H 0.83 0.4374 0.105 0.132 Uiso 1 1 calc R . . H63B H 0.7127 0.4629 0.1201 0.132 Uiso 1 1 calc R . . H63C H 0.7825 0.3663 0.0799 0.132 Uiso 1 1 calc R . . C64 C 0.8379(3) 0.2950(2) 0.1907(2) 0.0699(11) Uani 1 1 d . . . H64A H 0.8979 0.3186 0.1771 0.105 Uiso 1 1 calc R . . H64B H 0.8493 0.2482 0.1523 0.105 Uiso 1 1 calc R . . H64C H 0.824 0.2683 0.2399 0.105 Uiso 1 1 calc R . . C65 C 0.6554(3) 0.3341(3) 0.2145(3) 0.0843(14) Uani 1 1 d . . . H65A H 0.597 0.3831 0.2175 0.126 Uiso 1 1 calc R . . H65B H 0.6418 0.3063 0.2633 0.126 Uiso 1 1 calc R . . H65C H 0.6683 0.2879 0.1752 0.126 Uiso 1 1 calc R . . C66 C 1.1088(7) 1.0107(5) 0.3443(5) 0.128(2) Uani 1 1 d . . . H66 H 1.1301 0.9775 0.3806 0.154 Uiso 1 1 calc R . . C67 C 1.1638(4) 0.9906(4) 0.2655(6) 0.118(2) Uani 1 1 d . . . H67 H 1.2235 0.9429 0.2473 0.142 Uiso 1 1 calc R . . C68 C 1.1300(5) 1.0400(5) 0.2175(4) 0.120(2) Uani 1 1 d . . . H68 H 1.1666 1.0266 0.1647 0.143 Uiso 1 1 calc R . . C69 C 1.0472(5) 1.1073(5) 0.2404(4) 0.1131(18) Uani 1 1 d . . . H69 H 1.0256 1.141 0.2045 0.136 Uiso 1 1 calc R . . C70 C 0.9950(4) 1.1271(4) 0.3134(4) 0.1037(17) Uani 1 1 d . . . H70 H 0.9362 1.1758 0.3289 0.124 Uiso 1 1 calc R . . C71 C 1.0210(5) 1.0823(5) 0.3659(3) 0.1079(19) Uani 1 1 d . . . H71 H 0.9809 1.0982 0.4179 0.129 Uiso 1 1 calc R . . C72 C 1.4350(5) 0.5664(5) -0.0200(4) 0.119(2) Uani 1 1 d . . . H72 H 1.3899 0.613 -0.0335 0.143 Uiso 1 1 calc R . . C73 C 1.4043(4) 0.4939(6) 0.0142(4) 0.123(2) Uani 1 1 d . . . H73 H 1.338 0.489 0.0237 0.147 Uiso 1 1 calc R . . C74 C 1.4677(5) 0.4267(4) 0.0357(4) 0.121(2) Uani 1 1 d . . . H74 H 1.4451 0.3763 0.061 0.145 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 Br1 0.0512(2) 0.04180(18) 0.03002(16) -0.00565(13) -0.00596(14) -0.01303(15) Br2 0.0476(2) 0.0605(2) 0.02803(16) 0.00177(14) -0.00520(14) -0.02064(16) Si1 0.0276(4) 0.0286(4) 0.0266(4) 0.0010(3) -0.0075(3) -0.0057(3) Si2 0.0267(4) 0.0227(4) 0.0223(4) 0.0011(3) -0.0071(3) -0.0033(3) Si3 0.0273(4) 0.0220(4) 0.0229(4) 0.0021(3) -0.0081(3) -0.0057(3) Si4 0.0303(4) 0.0228(4) 0.0287(4) 0.0006(3) -0.0109(3) -0.0050(3) N1 0.0308(13) 0.0293(12) 0.0329(12) 0.0014(10) -0.0129(11) -0.0048(10) N2 0.0310(13) 0.0295(12) 0.0355(13) 0.0013(10) -0.0121(11) -0.0073(10) N3 0.0306(13) 0.0315(12) 0.0235(11) 0.0037(9) -0.0087(10) -0.0043(10) N4 0.0322(13) 0.0249(12) 0.0290(12) -0.0001(9) -0.0066(10) -0.0082(10) N5 0.0298(12) 0.0250(12) 0.0302(12) 0.0024(9) -0.0101(10) -0.0089(10) N6 0.0310(13) 0.0332(12) 0.0228(11) 0.0000(9) -0.0083(10) -0.0095(10) N7 0.0307(13) 0.0244(12) 0.0338(12) 0.0043(10) -0.0145(11) -0.0060(10) N8 0.0340(13) 0.0258(12) 0.0368(13) 0.0024(10) -0.0160(11) -0.0084(10) C1 0.0249(15) 0.0385(17) 0.0313(15) -0.0004(12) -0.0076(12) -0.0042(13) C2 0.0267(15) 0.0435(17) 0.0294(15) -0.0008(13) -0.0074(12) -0.0086(13) C3 0.0469(19) 0.0516(19) 0.0389(17) 0.0009(15) -0.0175(15) -0.0177(16) C4 0.058(2) 0.076(3) 0.0416(19) 0.0005(18) -0.0262(17) -0.026(2) C5 0.050(2) 0.071(2) 0.0395(18) 0.0089(17) -0.0242(16) -0.0136(18) C6 0.0386(18) 0.0457(18) 0.0378(17) 0.0048(14) -0.0146(14) -0.0033(14) C7 0.0388(17) 0.0322(16) 0.0471(18) 0.0064(13) -0.0178(15) -0.0085(13) C8 0.055(2) 0.0317(17) 0.063(2) -0.0024(15) -0.0303(18) -0.0015(15) C9 0.101(4) 0.040(2) 0.163(5) -0.008(3) -0.065(4) -0.015(2) C10 0.109(4) 0.061(3) 0.062(3) -0.020(2) -0.022(3) 0.033(2) C11 0.076(3) 0.056(2) 0.106(3) -0.023(2) -0.057(3) 0.024(2) C12 0.0339(17) 0.0312(16) 0.0508(18) -0.0026(13) -0.0149(15) -0.0075(13) C13 0.0401(18) 0.0394(17) 0.0491(18) 0.0050(14) -0.0151(15) -0.0169(15) C14 0.039(2) 0.086(3) 0.082(3) 0.024(2) -0.013(2) -0.023(2) C15 0.106(4) 0.084(3) 0.081(3) -0.015(2) -0.004(3) -0.064(3) C16 0.070(3) 0.085(3) 0.066(3) 0.026(2) -0.022(2) -0.023(2) C17 0.0379(17) 0.0259(15) 0.0342(16) 0.0034(12) 0.0008(14) 0.0008(13) C18 0.0388(17) 0.0236(14) 0.0339(16) -0.0006(12) -0.0004(13) -0.0058(13) C19 0.067(2) 0.0415(19) 0.048(2) -0.0100(16) 0.0116(18) -0.0264(18) C20 0.119(4) 0.046(2) 0.064(3) -0.008(2) 0.029(3) -0.047(2) C21 0.144(4) 0.044(2) 0.048(2) 0.0098(19) 0.016(3) -0.035(3) C22 0.086(3) 0.0395(19) 0.0341(18) 0.0079(15) -0.0032(18) -0.0066(19) C23 0.0359(17) 0.056(2) 0.0252(14) -0.0004(13) -0.0115(13) -0.0013(15) C24 0.0442(18) 0.0526(19) 0.0251(15) -0.0036(13) -0.0095(14) -0.0095(15) C25 0.061(2) 0.056(2) 0.057(2) -0.0153(18) 0.0134(19) -0.0065(19) C26 0.097(3) 0.047(2) 0.0388(19) -0.0075(16) -0.008(2) -0.010(2) C27 0.090(3) 0.135(4) 0.067(3) -0.046(3) -0.047(3) 0.004(3) C28 0.0413(17) 0.0255(15) 0.0429(17) -0.0032(12) -0.0194(14) -0.0053(13) C29 0.0469(18) 0.0284(15) 0.0335(15) -0.0027(12) -0.0127(14) -0.0080(13) C30 0.065(2) 0.0265(16) 0.0493(19) -0.0059(14) -0.0058(17) -0.0040(15) C31 0.105(3) 0.056(2) 0.062(2) -0.0173(19) -0.048(2) -0.005(2) C32 0.059(2) 0.051(2) 0.051(2) -0.0092(16) 0.0021(18) -0.0182(18) C33 0.0310(15) 0.0282(14) 0.0278(14) 0.0021(11) -0.0127(12) -0.0080(12) C34 0.0413(17) 0.0260(14) 0.0364(16) 0.0066(12) -0.0212(14) -0.0109(13) C35 0.0427(17) 0.0265(14) 0.0317(15) 0.0044(12) -0.0198(14) -0.0120(13) C36 0.062(2) 0.0414(18) 0.0304(16) 0.0059(13) -0.0197(15) -0.0200(16) C37 0.085(3) 0.048(2) 0.0422(19) 0.0090(15) -0.038(2) -0.0298(19) C38 0.075(3) 0.056(2) 0.059(2) 0.0156(17) -0.048(2) -0.0350(19) C39 0.051(2) 0.0426(18) 0.0481(19) 0.0094(15) -0.0262(16) -0.0228(16) C40 0.0272(15) 0.0345(16) 0.0412(16) -0.0012(13) -0.0103(13) -0.0049(13) C41 0.0305(16) 0.0429(17) 0.0365(16) 0.0041(13) -0.0050(13) -0.0118(14) C42 0.063(2) 0.048(2) 0.0485(19) 0.0145(16) -0.0134(17) -0.0278(18) C43 0.0416(19) 0.060(2) 0.0472(19) 0.0140(16) -0.0159(16) -0.0175(16) C44 0.0341(18) 0.080(3) 0.048(2) -0.0024(18) -0.0020(16) -0.0118(18) C45 0.0351(16) 0.0378(16) 0.0286(15) -0.0010(12) -0.0082(13) -0.0025(13) C46 0.0305(16) 0.0416(17) 0.0325(15) 0.0017(13) -0.0054(13) -0.0080(13) C47 0.062(2) 0.068(2) 0.072(2) 0.037(2) -0.029(2) -0.028(2) C48 0.048(2) 0.081(3) 0.053(2) -0.009(2) 0.0094(18) -0.016(2) C49 0.065(2) 0.063(2) 0.057(2) -0.0052(18) -0.0105(19) -0.027(2) C50 0.0339(16) 0.0237(14) 0.0326(15) 0.0005(12) -0.0103(13) -0.0043(12) C51 0.0366(17) 0.0264(15) 0.0354(15) 0.0004(12) -0.0114(13) -0.0052(13) C52 0.0390(18) 0.0440(18) 0.0501(19) 0.0079(15) -0.0144(15) -0.0191(15) C53 0.052(2) 0.049(2) 0.052(2) 0.0181(16) -0.0100(18) -0.0237(17) C54 0.052(2) 0.0470(19) 0.0411(18) 0.0160(15) -0.0133(16) -0.0132(16) C55 0.0437(18) 0.0357(16) 0.0417(17) 0.0094(14) -0.0165(15) -0.0104(14) C56 0.0409(17) 0.0305(15) 0.0402(16) 0.0061(13) -0.0203(14) -0.0096(13) C57 0.0342(17) 0.0402(17) 0.0508(19) 0.0127(14) -0.0201(15) -0.0068(14) C58 0.053(2) 0.070(2) 0.084(3) 0.019(2) -0.041(2) -0.0248(19) C59 0.0379(19) 0.075(3) 0.053(2) 0.0102(18) -0.0118(17) 0.0044(18) C60 0.041(2) 0.048(2) 0.077(3) 0.0176(18) -0.0235(19) -0.0016(16) C61 0.0426(18) 0.0311(16) 0.0543(19) 0.0040(14) -0.0256(16) -0.0103(14) C62 0.067(2) 0.0452(19) 0.052(2) 0.0040(15) -0.0307(18) -0.0291(18) C63 0.146(5) 0.089(3) 0.058(2) 0.012(2) -0.051(3) -0.061(3) C64 0.089(3) 0.047(2) 0.068(2) -0.0202(18) -0.023(2) -0.015(2) C65 0.100(3) 0.089(3) 0.090(3) -0.002(2) -0.044(3) -0.057(3) C66 0.136(6) 0.120(5) 0.188(8) 0.069(5) -0.100(6) -0.085(5) C67 0.070(4) 0.062(3) 0.204(8) -0.015(4) -0.029(5) -0.021(3) C68 0.095(5) 0.115(5) 0.120(5) -0.033(4) 0.000(4) -0.038(4) C69 0.104(5) 0.131(5) 0.105(5) 0.011(4) -0.034(4) -0.041(4) C70 0.086(4) 0.114(4) 0.104(4) -0.021(4) -0.030(4) -0.017(3) C71 0.101(5) 0.148(6) 0.082(4) -0.023(4) -0.024(3) -0.055(4) C72 0.088(5) 0.119(5) 0.154(6) -0.076(5) -0.071(4) 0.023(4) C73 0.073(4) 0.128(5) 0.162(6) -0.079(5) -0.050(4) 0.005(4) C74 0.102(5) 0.113(5) 0.142(5) -0.061(4) -0.047(4) -0.002(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Si4 2.2769(8) . ? Br2 Si1 2.2574(8) . ? Si1 N1 1.729(2) . ? Si1 N2 1.730(2) . ? Si1 Si2 2.4036(10) . ? Si2 N4 1.738(2) . ? Si2 N3 1.743(2) . ? Si2 C33 1.884(3) . ? Si3 N6 1.733(2) . ? Si3 N5 1.742(2) . ? Si3 C33 1.871(3) . ? Si3 Si4 2.3962(10) . ? Si4 N8 1.723(2) . ? Si4 N7 1.724(2) . ? N1 C1 1.418(4) . ? N1 C7 1.472(3) . ? N2 C2 1.410(4) . ? N2 C12 1.467(3) . ? N3 C17 1.406(4) . ? N3 C23 1.469(4) . ? N4 C18 1.414(3) . ? N4 C28 1.473(3) . ? N5 C34 1.424(3) . ? N5 C40 1.477(3) . ? N6 C35 1.416(3) . ? N6 C45 1.474(3) . ? N7 C50 1.426(3) . ? N7 C56 1.463(3) . ? N8 C51 1.414(3) . ? N8 C61 1.460(4) . ? C1 C6 1.376(4) . ? C1 C2 1.416(4) . ? C2 C3 1.382(4) . ? C3 C4 1.380(4) . ? C4 C5 1.374(5) . ? C5 C6 1.394(4) . ? C7 C8 1.548(4) . ? C8 C10 1.514(5) . ? C8 C11 1.518(5) . ? C8 C9 1.523(5) . ? C12 C13 1.562(4) . ? C13 C16 1.513(5) . ? C13 C14 1.518(5) . ? C13 C15 1.524(5) . ? C17 C22 1.378(4) . ? C17 C18 1.410(4) . ? C18 C19 1.388(4) . ? C19 C20 1.393(5) . ? C20 C21 1.363(6) . ? C21 C22 1.392(6) . ? C23 C24 1.551(4) . ? C24 C27 1.510(5) . ? C24 C25 1.514(5) . ? C24 C26 1.514(5) . ? C28 C29 1.543(4) . ? C29 C32 1.514(4) . ? C29 C30 1.526(4) . ? C29 C31 1.528(5) . ? C34 C39 1.382(4) . ? C34 C35 1.406(4) . ? C35 C36 1.386(4) . ? C36 C37 1.387(4) . ? C37 C38 1.360(5) . ? C38 C39 1.395(4) . ? C40 C41 1.542(4) . ? C41 C43 1.517(4) . ? C41 C42 1.527(4) . ? C41 C44 1.537(4) . ? C45 C46 1.543(4) . ? C46 C49 1.511(4) . ? C46 C47 1.520(5) . ? C46 C48 1.521(4) . ? C50 C55 1.384(4) . ? C50 C51 1.405(4) . ? C51 C52 1.385(4) . ? C52 C53 1.390(4) . ? C53 C54 1.367(5) . ? C54 C55 1.395(4) . ? C56 C57 1.541(4) . ? C57 C59 1.522(4) . ? C57 C60 1.529(4) . ? C57 C58 1.533(5) . ? C61 C62 1.560(4) . ? C62 C63 1.520(5) . ? C62 C65 1.528(5) . ? C62 C64 1.536(5) . ? C66 C71 1.409(9) . ? C66 C67 1.420(9) . ? C67 C68 1.334(9) . ? C68 C69 1.326(8) . ? C69 C70 1.320(7) . ? C70 C71 1.319(8) . ? C72 C73 1.343(9) . ? C72 C74 1.386(8) 2_865 ? C73 C74 1.377(9) . ? C74 C72 1.386(8) 2_865 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 N2 92.78(11) . . ? N1 Si1 Br2 116.70(8) . . ? N2 Si1 Br2 107.15(8) . . ? N1 Si1 Si2 109.86(8) . . ? N2 Si1 Si2 117.06(8) . . ? Br2 Si1 Si2 112.15(4) . . ? N4 Si2 N3 93.12(11) . . ? N4 Si2 C33 115.69(12) . . ? N3 Si2 C33 116.34(11) . . ? N4 Si2 Si1 121.46(8) . . ? N3 Si2 Si1 100.77(8) . . ? C33 Si2 Si1 107.96(9) . . ? N6 Si3 N5 93.17(10) . . ? N6 Si3 C33 111.32(12) . . ? N5 Si3 C33 123.80(11) . . ? N6 Si3 Si4 114.34(8) . . ? N5 Si3 Si4 108.13(8) . . ? C33 Si3 Si4 106.07(9) . . ? N8 Si4 N7 93.39(11) . . ? N8 Si4 Br1 106.35(8) . . ? N7 Si4 Br1 117.67(8) . . ? N8 Si4 Si3 123.94(8) . . ? N7 Si4 Si3 111.85(8) . . ? Br1 Si4 Si3 104.34(3) . . ? C1 N1 C7 121.6(2) . . ? C1 N1 Si1 110.49(18) . . ? C7 N1 Si1 124.45(19) . . ? C2 N2 C12 120.0(2) . . ? C2 N2 Si1 110.97(18) . . ? C12 N2 Si1 128.1(2) . . ? C17 N3 C23 120.3(2) . . ? C17 N3 Si2 110.02(18) . . ? C23 N3 Si2 126.44(19) . . ? C18 N4 C28 120.0(2) . . ? C18 N4 Si2 109.87(18) . . ? C28 N4 Si2 128.20(18) . . ? C34 N5 C40 118.2(2) . . ? C34 N5 Si3 109.79(17) . . ? C40 N5 Si3 127.38(18) . . ? C35 N6 C45 119.4(2) . . ? C35 N6 Si3 110.25(17) . . ? C45 N6 Si3 128.93(19) . . ? C50 N7 C56 121.5(2) . . ? C50 N7 Si4 110.05(18) . . ? C56 N7 Si4 125.44(17) . . ? C51 N8 C61 120.6(2) . . ? C51 N8 Si4 110.26(18) . . ? C61 N8 Si4 128.62(18) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 N1 128.0(3) . . ? C2 C1 N1 112.7(2) . . ? C3 C2 N2 127.2(3) . . ? C3 C2 C1 120.2(3) . . ? N2 C2 C1 112.5(2) . . ? C4 C3 C2 119.7(3) . . ? C5 C4 C3 120.6(3) . . ? C4 C5 C6 120.4(3) . . ? C1 C6 C5 120.0(3) . . ? N1 C7 C8 118.1(2) . . ? C10 C8 C11 109.1(3) . . ? C10 C8 C9 109.8(4) . . ? C11 C8 C9 108.5(3) . . ? C10 C8 C7 110.9(3) . . ? C11 C8 C7 112.6(3) . . ? C9 C8 C7 105.8(3) . . ? N2 C12 C13 118.6(2) . . ? C16 C13 C14 107.5(3) . . ? C16 C13 C15 109.7(3) . . ? C14 C13 C15 109.8(3) . . ? C16 C13 C12 109.3(3) . . ? C14 C13 C12 112.6(3) . . ? C15 C13 C12 107.9(3) . . ? C22 C17 N3 126.9(3) . . ? C22 C17 C18 119.9(3) . . ? N3 C17 C18 113.2(2) . . ? C19 C18 C17 119.9(3) . . ? C19 C18 N4 126.6(3) . . ? C17 C18 N4 113.4(2) . . ? C18 C19 C20 119.0(4) . . ? C21 C20 C19 120.6(4) . . ? C20 C21 C22 121.2(3) . . ? C17 C22 C21 119.1(4) . . ? N3 C23 C24 118.4(2) . . ? C27 C24 C25 109.4(3) . . ? C27 C24 C26 109.9(3) . . ? C25 C24 C26 107.8(3) . . ? C27 C24 C23 105.7(3) . . ? C25 C24 C23 113.2(3) . . ? C26 C24 C23 110.8(2) . . ? N4 C28 C29 118.8(2) . . ? C32 C29 C30 108.6(3) . . ? C32 C29 C31 110.4(3) . . ? C30 C29 C31 108.8(3) . . ? C32 C29 C28 109.5(2) . . ? C30 C29 C28 113.0(2) . . ? C31 C29 C28 106.4(3) . . ? Si3 C33 Si2 131.38(15) . . ? C39 C34 C35 119.7(3) . . ? C39 C34 N5 127.2(3) . . ? C35 C34 N5 113.1(2) . . ? C36 C35 C34 119.9(3) . . ? C36 C35 N6 126.8(3) . . ? C34 C35 N6 113.3(2) . . ? C35 C36 C37 119.5(3) . . ? C38 C37 C36 120.7(3) . . ? C37 C38 C39 120.8(3) . . ? C34 C39 C38 119.4(3) . . ? N5 C40 C41 117.5(2) . . ? C43 C41 C42 110.5(3) . . ? C43 C41 C44 109.3(3) . . ? C42 C41 C44 109.2(3) . . ? C43 C41 C40 109.9(2) . . ? C42 C41 C40 111.5(2) . . ? C44 C41 C40 106.3(2) . . ? N6 C45 C46 117.3(2) . . ? C49 C46 C47 110.3(3) . . ? C49 C46 C48 108.9(3) . . ? C47 C46 C48 110.0(3) . . ? C49 C46 C45 108.9(2) . . ? C47 C46 C45 111.8(2) . . ? C48 C46 C45 106.8(3) . . ? C55 C50 C51 120.1(3) . . ? C55 C50 N7 127.2(3) . . ? C51 C50 N7 112.5(2) . . ? C52 C51 C50 119.9(3) . . ? C52 C51 N8 126.9(3) . . ? C50 C51 N8 113.2(2) . . ? C51 C52 C53 119.4(3) . . ? C54 C53 C52 120.7(3) . . ? C53 C54 C55 120.7(3) . . ? C50 C55 C54 119.1(3) . . ? N7 C56 C57 118.5(2) . . ? C59 C57 C60 108.9(3) . . ? C59 C57 C58 109.8(3) . . ? C60 C57 C58 108.8(3) . . ? C59 C57 C56 111.4(2) . . ? C60 C57 C56 111.9(2) . . ? C58 C57 C56 105.9(3) . . ? N8 C61 C62 118.0(3) . . ? C63 C62 C65 109.3(3) . . ? C63 C62 C64 108.8(3) . . ? C65 C62 C64 108.5(3) . . ? C63 C62 C61 109.5(3) . . ? C65 C62 C61 108.9(3) . . ? C64 C62 C61 111.8(3) . . ? C71 C66 C67 116.7(6) . . ? C68 C67 C66 118.6(6) . . ? C69 C68 C67 122.6(7) . . ? C70 C69 C68 119.7(7) . . ? C71 C70 C69 122.8(6) . . ? C70 C71 C66 119.6(6) . . ? C73 C72 C74 120.2(6) . 2_865 ? C72 C73 C74 120.8(6) . . ? C73 C74 C72 119.0(7) . 2_865 ? #===END