# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Wai-Yeung, Wong' 'Lee, Albert W. M.' 'Lu, G. L.' 'Mo, T.' 'Wong, C. K.' 'Zhang, H.' _publ_contact_author_name 'Dr Wong Wai-Yeung' _publ_contact_author_address ; Dr Wong Wai-Yeung Department of Chemistry Hong Kong Baptist University Waterloo Road Kowloon Tong Hong Kong CHINA ; _publ_contact_author_email 'RWYWONG@HKBU.EDU.HK' _publ_section_title ; Synthesis and characterisation of new oligoacetylenic silanes ; data_wy0382wm _database_code_CSD 177961 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H34 Si2' _chemical_formula_weight 738.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0001(7) _cell_length_b 9.4959(9) _cell_length_c 14.7690(13) _cell_angle_alpha 80.960(2) _cell_angle_beta 74.773(2) _cell_angle_gamma 82.454(2) _cell_volume 1064.35(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 386 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Smart CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6216 _diffrn_reflns_av_R_equivalents 0.0188 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4519 _reflns_number_gt 3508 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1281P)^2^+0.0375P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4519 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1890 _refine_ls_wR_factor_gt 0.1741 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 4.079 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0426(5) 1.2164(4) 0.4939(2) 0.1259(13) Uani 1 1 d . . . C2 C 0.1734(4) 1.1650(3) 0.45056(18) 0.0938(8) Uani 1 1 d . . . C3 C 0.3353(3) 1.0974(2) 0.40113(15) 0.0778(6) Uani 1 1 d . . . C4 C 0.3381(3) 0.9877(3) 0.34875(17) 0.0820(6) Uani 1 1 d . . . H4A H 0.2343 0.9614 0.3422 0.098 Uiso 1 1 calc R . . C5 C 0.4937(3) 0.9178(2) 0.30650(15) 0.0756(6) Uani 1 1 d . . . H5A H 0.4946 0.8447 0.2711 0.091 Uiso 1 1 calc R . . C6 C 0.6493(3) 0.9551(2) 0.31599(13) 0.0664(5) Uani 1 1 d . . . C7 C 0.6469(3) 1.0670(2) 0.36720(16) 0.0804(6) Uani 1 1 d . . . H7A H 0.7508 1.0939 0.3730 0.096 Uiso 1 1 calc R . . C8 C 0.4912(4) 1.1379(3) 0.40917(17) 0.0874(7) Uani 1 1 d . . . H8A H 0.4902 1.2129 0.4430 0.105 Uiso 1 1 calc R . . C9 C 0.8082(3) 0.8745(2) 0.27639(13) 0.0681(5) Uani 1 1 d . . . C10 C 0.9384(3) 0.8003(2) 0.24504(13) 0.0693(5) Uani 1 1 d . . . C11 C 1.2360(2) 0.6175(2) 0.29899(13) 0.0644(5) Uani 1 1 d . . . C12 C 1.3141(2) 0.5792(2) 0.35877(13) 0.0625(5) Uani 1 1 d . . . C13 C 1.0318(2) 0.5075(2) 0.18866(12) 0.0603(4) Uani 1 1 d . . . C14 C 0.9145(4) 0.5162(3) 0.13360(18) 0.0927(7) Uani 1 1 d . . . H14A H 0.8764 0.6053 0.1059 0.111 Uiso 1 1 calc R . . C15 C 0.8525(4) 0.3934(4) 0.1190(2) 0.1125(10) Uani 1 1 d . . . H15A H 0.7724 0.4015 0.0825 0.135 Uiso 1 1 calc R . . C16 C 0.9082(4) 0.2617(3) 0.1578(2) 0.1030(9) Uani 1 1 d . . . H16A H 0.8675 0.1798 0.1472 0.124 Uiso 1 1 calc R . . C17 C 1.0213(4) 0.2513(3) 0.2109(2) 0.1021(8) Uani 1 1 d . . . H17A H 1.0598 0.1615 0.2373 0.123 Uiso 1 1 calc R . . C18 C 1.0826(3) 0.3719(3) 0.22751(17) 0.0820(6) Uani 1 1 d . . . H18A H 1.1601 0.3614 0.2658 0.098 Uiso 1 1 calc R . . C19 C 1.2703(2) 0.7474(2) 0.09717(12) 0.0627(5) Uani 1 1 d . . . C20 C 1.2247(3) 0.8731(2) 0.04298(15) 0.0791(6) Uani 1 1 d . . . H20A H 1.1179 0.9249 0.0634 0.095 Uiso 1 1 calc R . . C21 C 1.3387(4) 0.9214(3) -0.04180(18) 0.1012(8) Uani 1 1 d . . . H21A H 1.3071 1.0049 -0.0781 0.121 Uiso 1 1 calc R . . C22 C 1.4968(4) 0.8467(4) -0.07196(19) 0.1070(9) Uani 1 1 d . . . H22A H 1.5725 0.8796 -0.1286 0.128 Uiso 1 1 calc R . . C23 C 1.5432(4) 0.7254(4) -0.0199(2) 0.1059(9) Uani 1 1 d . . . H23A H 1.6507 0.6749 -0.0409 0.127 Uiso 1 1 calc R . . C24 C 1.4323(3) 0.6756(3) 0.06437(17) 0.0867(6) Uani 1 1 d . . . H24A H 1.4669 0.5923 0.0998 0.104 Uiso 1 1 calc R . . C25 C 1.4088(2) 0.53799(19) 0.43050(12) 0.0584(4) Uani 1 1 d . . . C26 C 1.3208(3) 0.5010(2) 0.52458(13) 0.0686(5) Uani 1 1 d . . . H26 H 1.2003 0.5016 0.5410 0.082 Uiso 1 1 calc R . . C27 C 1.5877(3) 0.5362(2) 0.40698(13) 0.0680(5) Uani 1 1 d . . . H27 H 1.6469 0.5604 0.3443 0.082 Uiso 1 1 calc R . . H1 H -0.066(7) 1.244(6) 0.544(3) 0.202(17) Uiso 1 1 d . . . Si1 Si 1.11938(6) 0.66972(5) 0.20643(3) 0.0571(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.118(2) 0.114(2) 0.109(2) -0.0079(18) 0.0084(19) 0.036(2) C2 0.0988(16) 0.0828(15) 0.0781(14) -0.0011(12) -0.0041(12) 0.0219(13) C3 0.0860(14) 0.0669(12) 0.0640(12) -0.0008(9) -0.0055(10) 0.0156(11) C4 0.0793(13) 0.0803(14) 0.0800(14) -0.0074(11) -0.0158(11) 0.0045(11) C5 0.0828(13) 0.0675(12) 0.0731(13) -0.0139(10) -0.0175(10) 0.0075(10) C6 0.0749(11) 0.0595(10) 0.0568(10) -0.0030(8) -0.0101(8) 0.0042(9) C7 0.0841(14) 0.0754(13) 0.0773(14) -0.0155(10) -0.0103(11) -0.0046(11) C8 0.1044(18) 0.0672(13) 0.0810(15) -0.0185(11) -0.0053(12) 0.0018(12) C9 0.0781(12) 0.0669(11) 0.0552(10) -0.0048(8) -0.0154(9) 0.0025(10) C10 0.0749(11) 0.0751(12) 0.0573(10) -0.0107(9) -0.0193(9) 0.0038(10) C11 0.0710(11) 0.0730(12) 0.0555(10) -0.0144(8) -0.0262(8) -0.0007(9) C12 0.0698(11) 0.0682(11) 0.0553(10) -0.0127(8) -0.0270(8) 0.0018(9) C13 0.0610(9) 0.0769(12) 0.0461(8) -0.0103(8) -0.0175(7) -0.0054(8) C14 0.1143(18) 0.0929(16) 0.0924(16) -0.0085(13) -0.0630(15) -0.0138(14) C15 0.129(2) 0.135(3) 0.104(2) -0.0173(18) -0.0691(18) -0.037(2) C16 0.126(2) 0.101(2) 0.0955(18) -0.0104(15) -0.0362(16) -0.0460(18) C17 0.115(2) 0.0812(16) 0.119(2) 0.0050(15) -0.0453(17) -0.0292(15) C18 0.0859(14) 0.0817(14) 0.0872(15) 0.0025(11) -0.0394(12) -0.0184(12) C19 0.0706(11) 0.0719(11) 0.0532(9) -0.0128(8) -0.0236(8) -0.0112(9) C20 0.0907(14) 0.0813(14) 0.0716(13) -0.0012(10) -0.0336(11) -0.0141(12) C21 0.132(2) 0.1021(19) 0.0757(15) 0.0163(13) -0.0376(16) -0.0425(18) C22 0.113(2) 0.136(3) 0.0719(15) -0.0030(16) -0.0107(15) -0.048(2) C23 0.0927(17) 0.132(2) 0.0817(16) -0.0157(16) 0.0005(13) -0.0140(17) C24 0.0781(13) 0.0950(16) 0.0768(14) -0.0070(12) -0.0080(11) 0.0003(12) C25 0.0710(10) 0.0589(10) 0.0526(9) -0.0094(7) -0.0302(8) 0.0008(8) C26 0.0630(10) 0.0856(13) 0.0602(11) -0.0056(9) -0.0249(8) -0.0026(9) C27 0.0695(11) 0.0853(13) 0.0492(9) -0.0042(8) -0.0207(8) -0.0009(10) Si1 0.0619(3) 0.0673(3) 0.0469(3) -0.0108(2) -0.0235(2) 0.0018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.164(4) . ? C2 C3 1.433(3) . ? C3 C4 1.387(3) . ? C3 C8 1.391(4) . ? C4 C5 1.373(3) . ? C5 C6 1.385(3) . ? C6 C7 1.393(3) . ? C6 C9 1.427(3) . ? C7 C8 1.376(3) . ? C9 C10 1.206(3) . ? C10 Si1 1.810(2) . ? C11 C12 1.197(2) . ? C11 Si1 1.8221(18) . ? C12 C25 1.436(2) . ? C13 C18 1.380(3) . ? C13 C14 1.381(3) . ? C13 Si1 1.855(2) . ? C14 C15 1.392(4) . ? C15 C16 1.361(4) . ? C16 C17 1.331(4) . ? C17 C18 1.382(3) . ? C19 C24 1.386(3) . ? C19 C20 1.391(3) . ? C19 Si1 1.855(2) . ? C20 C21 1.393(4) . ? C21 C22 1.367(4) . ? C22 C23 1.347(4) . ? C23 C24 1.380(4) . ? C25 C27 1.380(3) . ? C25 C26 1.395(3) . ? C26 C27 1.375(2) 2_866 ? C27 C26 1.375(2) 2_866 ? 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 C1 C2 C3 177.3(3) . . ? C4 C3 C8 119.6(2) . . ? C4 C3 C2 120.7(3) . . ? C8 C3 C2 119.7(2) . . ? C5 C4 C3 120.1(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 C7 119.2(2) . . ? C5 C6 C9 119.38(19) . . ? C7 C6 C9 121.3(2) . . ? C8 C7 C6 120.2(2) . . ? C7 C8 C3 120.1(2) . . ? C10 C9 C6 176.7(2) . . ? C9 C10 Si1 172.72(19) . . ? C12 C11 Si1 177.97(18) . . ? C11 C12 C25 178.1(2) . . ? C18 C13 C14 116.42(19) . . ? C18 C13 Si1 122.23(14) . . ? C14 C13 Si1 121.34(16) . . ? C13 C14 C15 120.9(2) . . ? C16 C15 C14 120.6(2) . . ? C17 C16 C15 119.3(2) . . ? C16 C17 C18 121.1(3) . . ? C13 C18 C17 121.7(2) . . ? C24 C19 C20 117.6(2) . . ? C24 C19 Si1 119.72(16) . . ? C20 C19 Si1 122.59(17) . . ? C19 C20 C21 120.2(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 120.1(3) . . ? C22 C23 C24 120.5(3) . . ? C23 C24 C19 121.2(2) . . ? C27 C25 C26 119.47(15) . . ? C27 C25 C12 120.15(16) . . ? C26 C25 C12 120.38(17) . . ? C27 C26 C25 119.99(18) 2_866 . ? C26 C27 C25 120.54(17) 2_866 . ? C10 Si1 C11 109.44(9) . . ? C10 Si1 C13 108.42(9) . . ? C11 Si1 C13 107.52(9) . . ? C10 Si1 C19 110.06(9) . . ? C11 Si1 C19 109.20(9) . . ? C13 Si1 C19 112.15(8) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.463 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.049 #==================End of compound 4b=====================