# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 188/161 data_GLOBAL # 1. SUBMISSION DETAILS _publ_contact_author_name 'Gleiter, Rolf' _publ_contact_author_address ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email 'rolf.gleiter@urz.uni-heidelberg.de' _publ_requested_journal 'J. Chem. Soc., Perkin 2' _publ_requested_coeditor_name ? _publ_contact_letter ; paper to be submitted for publication in J. Chem. Soc., Perkin 2 ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; 1,1,2,2-Tetramethyl-1,2-disilacycloocta-3,7-diyne - Structure and Bonding Properties of a Highly Stained Diyne ; loop_ _publ_author_name _publ_author_address 'Haberhauer, Gebhard' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Gleiter, Rolf' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================= data_gh13 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H16 Si2' _chemical_formula_weight 192.41 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.36050(10) _cell_length_b 13.2811(2) _cell_length_c 12.3457(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.4960(10) _cell_angle_gamma 90.00 _cell_volume 1206.82(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .34 _exptl_crystal_size_mid .26 _exptl_crystal_size_min .18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.247 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8781 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.56 _reflns_number_total 2088 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.1815P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2088 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.010 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 0.70498(6) 0.23623(3) 0.15169(3) 0.03498(15) Uani 1 1 d . . . C11 C 0.4770(3) 0.29020(19) 0.1817(2) 0.0589(5) Uani 1 1 d . . . H11A H 0.483(3) 0.320(2) 0.250(2) 0.095(8) Uiso 1 1 d . . . H11B H 0.442(3) 0.336(2) 0.128(2) 0.092(8) Uiso 1 1 d . . . H11C H 0.387(4) 0.235(2) 0.192(2) 0.091(8) Uiso 1 1 d . . . C12 C 0.8810(4) 0.33709(17) 0.1475(2) 0.0590(6) Uani 1 1 d . . . H12A H 0.830(3) 0.3883(19) 0.104(2) 0.088(8) Uiso 1 1 d . . . H12B H 0.889(4) 0.3614(19) 0.209(2) 0.092(9) Uiso 1 1 d . . . H12C H 0.999(3) 0.3100(18) 0.122(2) 0.080(8) Uiso 1 1 d . . . Si2 Si 0.78410(6) 0.10706(3) 0.27576(3) 0.03610(15) Uani 1 1 d . . . C21 C 0.6002(3) 0.08487(18) 0.37623(17) 0.0549(5) Uani 1 1 d . . . H21A H 0.579(3) 0.1433(18) 0.4189(19) 0.077(7) Uiso 1 1 d . . . H21B H 0.490(3) 0.0613(18) 0.3402(18) 0.082(7) Uiso 1 1 d . . . H21C H 0.633(3) 0.0349(19) 0.420(2) 0.078(8) Uiso 1 1 d . . . C22 C 1.0041(3) 0.13514(19) 0.34559(19) 0.0548(5) Uani 1 1 d . . . H22A H 0.995(3) 0.1919(18) 0.3884(19) 0.069(6) Uiso 1 1 d . . . H22B H 1.093(3) 0.1473(17) 0.297(2) 0.073(7) Uiso 1 1 d . . . H22C H 1.041(3) 0.0834(18) 0.3917(19) 0.073(7) Uiso 1 1 d . . . C3 C 0.8055(2) -0.00299(12) 0.18641(13) 0.0381(4) Uani 1 1 d . . . C4 C 0.8013(2) -0.04821(11) 0.10225(13) 0.0355(4) Uani 1 1 d . . . C5 C 0.7911(2) -0.08439(13) -0.00967(14) 0.0402(4) Uani 1 1 d . . . H5A H 0.718(3) -0.1428(16) -0.0127(17) 0.064(6) Uiso 1 1 d . . . H5B H 0.911(3) -0.0992(14) -0.0345(15) 0.054(5) Uiso 1 1 d . . . C6 C 0.7112(2) -0.00374(13) -0.08761(13) 0.0391(4) Uani 1 1 d . . . H6A H 0.588(3) -0.0241(14) -0.1054(15) 0.054(5) Uiso 1 1 d . . . H6B H 0.783(3) -0.0025(15) -0.1493(16) 0.063(6) Uiso 1 1 d . . . C7 C 0.7026(2) 0.09602(12) -0.03720(12) 0.0335(4) Uani 1 1 d . . . C8 C 0.6970(2) 0.16852(11) 0.02134(12) 0.0351(4) 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 Si1 0.0437(3) 0.0280(2) 0.0332(2) -0.00306(18) -0.00061(19) -0.00091(18) C11 0.0644(14) 0.0541(13) 0.0583(13) -0.0112(11) 0.0030(10) 0.0209(11) C12 0.0824(17) 0.0470(12) 0.0474(12) -0.0025(10) -0.0066(11) -0.0239(11) Si2 0.0442(3) 0.0356(3) 0.0285(2) -0.00039(18) 0.00143(18) -0.00074(19) C21 0.0708(15) 0.0531(13) 0.0411(10) -0.0033(10) 0.0158(10) -0.0120(11) C22 0.0557(13) 0.0614(14) 0.0472(11) -0.0063(11) -0.0091(10) 0.0031(10) C3 0.0450(9) 0.0313(8) 0.0379(9) 0.0035(7) -0.0007(7) 0.0033(7) C4 0.0328(8) 0.0292(8) 0.0445(9) 0.0028(7) 0.0008(7) 0.0010(6) C5 0.0372(10) 0.0357(9) 0.0477(10) -0.0131(8) -0.0002(7) -0.0009(7) C6 0.0386(10) 0.0439(10) 0.0349(9) -0.0101(7) 0.0024(7) -0.0020(7) C7 0.0304(8) 0.0403(9) 0.0298(7) 0.0010(7) -0.0014(6) -0.0017(7) C8 0.0382(9) 0.0336(9) 0.0334(8) 0.0030(7) -0.0040(7) 0.0005(7) _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 C8 1.8440(16) . ? Si1 C12 1.864(2) . ? Si1 C11 1.865(2) . ? Si1 Si2 2.3691(6) . ? Si2 C3 1.8387(16) . ? Si2 C22 1.865(2) . ? Si2 C21 1.8675(19) . ? C3 C4 1.200(2) . ? C4 C5 1.464(2) . ? C5 C6 1.552(2) . ? C6 C7 1.465(2) . ? C7 C8 1.205(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 Si1 C12 110.06(10) . . ? C8 Si1 C11 109.79(9) . . ? C12 Si1 C11 110.86(12) . . ? C8 Si1 Si2 102.53(5) . . ? C12 Si1 Si2 111.80(8) . . ? C11 Si1 Si2 111.50(9) . . ? C3 Si2 C22 110.96(9) . . ? C3 Si2 C21 109.84(9) . . ? C22 Si2 C21 110.85(11) . . ? C3 Si2 Si1 102.10(5) . . ? C22 Si2 Si1 111.20(8) . . ? C21 Si2 Si1 111.60(9) . . ? C4 C3 Si2 156.26(14) . . ? C3 C4 C5 169.06(16) . . ? C4 C5 C6 112.00(13) . . ? C7 C6 C5 112.22(13) . . ? C8 C7 C6 168.27(16) . . ? C7 C8 Si1 155.81(13) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.56 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.238 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.036 #=======================================================================