data_publication_text _publ_contact_author_name 'Aaron D. Sadow' _publ_contact_author_address ;1605 Gilman Hall Department of Chemistry Iowa State University Ames IA 50011 ; _publ_contact_author_email sadow@iastate.edu _publ_contact_author_phone 5152948069 _publ_contact_author_fax 5152940105 loop_ _publ_author_name _publ_author_address 'Yan, K.' ;1605 Gilman Hall Department of Chemistry Iowa State University Ames IA 50011 ; 'Upton, B.' ;1605 Gilman Hall Department of Chemistry Iowa State University Ames IA 50011 ; 'Ellern, A.' ;1605 Gilman Hall Department of Chemistry Iowa State University Ames IA 50011 ; 'Sadow, A. D. ' ;1605 Gilman Hall Department of Chemistry Iowa State University Ames IA 50011 ; data_disilacyclobutane _vrf_RINTA01_disilacyclobutane ; PROBLEM: The value of Rint is greater than 0.20 RESPONSE: Weakly diffracted sample with high mosaisity. No significant reflections at high angles ; _vrf_THETM01_disilacyclobutane ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Weakly diffracted sample with high mosaisity. No significant reflections at high angles ; _vrf_PLAT020_disilacyclobutane ; PROBLEM: The value of Rint is greater than 0.10 ......... 0.30 RESPONSE: Weakly diffracted sample with high mosaisity. No significant reflections at high angles ; _vrf_PLAT023_disilacyclobutane ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 21.00 Deg. RESPONSE: Weakly diffracted sample with high mosaisity. No significant reflections at high angles ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H40 Si6' _chemical_formula_weight 377.00 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 8.512(7) _cell_length_b 8.569(7) _cell_length_c 9.253(9) _cell_angle_alpha 104.555(19) _cell_angle_beta 91.47(2) _cell_angle_gamma 114.49(2) _cell_volume 588.0(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 715 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.94 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 208 _exptl_absorpt_coefficient_mu 0.348 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 3026 _diffrn_reflns_av_R_equivalents 0.3013 _diffrn_reflns_av_sigmaI/netI 0.2229 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 21.00 _reflns_number_total 1275 _reflns_number_gt 859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1379P)^2^+0.6066P] 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 1275 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2429 _refine_ls_wR_factor_gt 0.1992 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.57907(19) 1.10749(18) 0.91908(18) 0.0233(8) Uani 1 1 d . . . Si2 Si 0.4023(2) 0.6925(2) 0.7369(2) 0.0294(8) Uani 1 1 d . . . Si3 Si 0.1668(2) 0.89442(19) 0.8257(2) 0.0294(8) Uani 1 1 d . . . C1 C 0.3766(7) 0.8816(7) 0.8752(7) 0.0216(15) Uani 1 1 d . . . C2 C 0.5343(9) 1.2956(7) 0.8893(8) 0.0385(18) Uani 1 1 d . . . H2A H 0.4896 1.2675 0.7828 0.058 Uiso 1 1 calc R . . H2B H 0.6426 1.4068 0.9179 0.058 Uiso 1 1 calc R . . H2C H 0.4475 1.3104 0.9519 0.058 Uiso 1 1 calc R . . C3 C 0.7587(8) 1.1071(8) 0.8090(8) 0.0383(17) Uani 1 1 d . . . H3A H 0.8631 1.2205 0.8504 0.057 Uiso 1 1 calc R . . H3B H 0.7229 1.0929 0.7032 0.057 Uiso 1 1 calc R . . H3C H 0.7847 1.0076 0.8154 0.057 Uiso 1 1 calc R . . C4 C 0.2247(8) 0.4617(7) 0.7196(8) 0.0426(19) Uani 1 1 d . . . H4A H 0.2037 0.4489 0.8206 0.064 Uiso 1 1 calc R . . H4B H 0.2611 0.3711 0.6659 0.064 Uiso 1 1 calc R . . H4C H 0.1171 0.4454 0.6635 0.064 Uiso 1 1 calc R . . C5 C 0.4123(10) 0.7122(9) 0.5396(8) 0.052(2) Uani 1 1 d . . . H5A H 0.4545 0.6289 0.4810 0.077 Uiso 1 1 calc R . . H5B H 0.4921 0.8349 0.5426 0.077 Uiso 1 1 calc R . . H5C H 0.2955 0.6830 0.4920 0.077 Uiso 1 1 calc R . . C6 C 0.1417(9) 0.9344(10) 0.6392(8) 0.053(2) Uani 1 1 d . . . H6A H 0.2531 1.0240 0.6248 0.080 Uiso 1 1 calc R . . H6B H 0.0523 0.9781 0.6363 0.080 Uiso 1 1 calc R . . H6C H 0.1065 0.8222 0.5585 0.080 Uiso 1 1 calc R . . C7 C -0.0340(7) 0.6886(9) 0.8276(9) 0.047(2) Uani 1 1 d . . . H7A H -0.1381 0.7076 0.8108 0.071 Uiso 1 1 calc R . . H7B H -0.0278 0.6655 0.9256 0.071 Uiso 1 1 calc R . . H7C H -0.0406 0.5856 0.7474 0.071 Uiso 1 1 calc R . . H3S H 0.158(7) 1.025(7) 0.916(7) 0.038(16) Uiso 1 1 d . . . H2S H 0.558(8) 0.703(8) 0.802(7) 0.044(17) Uiso 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 0.0201(12) 0.0157(11) 0.0370(14) 0.0141(9) 0.0010(10) 0.0069(8) Si2 0.0280(13) 0.0219(11) 0.0436(14) 0.0118(9) 0.0017(10) 0.0148(9) Si3 0.0213(12) 0.0250(11) 0.0472(15) 0.0140(10) -0.0015(10) 0.0136(9) C1 0.009(3) 0.016(3) 0.040(4) 0.017(3) 0.000(3) 0.001(3) C2 0.042(4) 0.023(3) 0.054(4) 0.022(3) -0.005(4) 0.011(3) C3 0.024(3) 0.037(4) 0.049(4) 0.021(3) 0.008(3) 0.004(3) C4 0.038(4) 0.016(3) 0.061(5) -0.001(3) -0.003(4) 0.006(3) C5 0.070(5) 0.045(4) 0.041(4) 0.005(4) 0.008(4) 0.030(4) C6 0.043(4) 0.073(5) 0.059(5) 0.030(4) -0.005(4) 0.034(4) C7 0.013(3) 0.045(4) 0.080(6) 0.020(4) 0.007(4) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C3 1.859(7) . ? Si1 C2 1.883(5) . ? Si1 C1 1.902(6) 2_677 ? Si1 C1 1.920(5) . ? Si1 Si1 2.623(3) 2_677 ? Si2 C5 1.876(7) . ? Si2 C1 1.892(6) . ? Si2 C4 1.890(6) . ? Si2 H2S 1.40(6) . ? Si3 C6 1.865(7) . ? Si3 C7 1.885(6) . ? Si3 C1 1.886(5) . ? Si3 H3S 1.25(6) . ? C1 Si1 1.902(6) 2_677 ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Si1 C2 105.2(3) . . ? C3 Si1 C1 114.4(3) . 2_677 ? C2 Si1 C1 114.7(3) . 2_677 ? C3 Si1 C1 115.1(3) . . ? C2 Si1 C1 114.4(3) . . ? C1 Si1 C1 93.3(2) 2_677 . ? C3 Si1 Si1 127.6(2) . 2_677 ? C2 Si1 Si1 127.2(3) . 2_677 ? C1 Si1 Si1 46.93(17) 2_677 2_677 ? C1 Si1 Si1 46.37(19) . 2_677 ? C5 Si2 C1 114.1(3) . . ? C5 Si2 C4 105.8(3) . . ? C1 Si2 C4 114.7(3) . . ? C5 Si2 H2S 112(3) . . ? C1 Si2 H2S 103(3) . . ? C4 Si2 H2S 108(2) . . ? C6 Si3 C7 107.0(3) . . ? C6 Si3 C1 114.9(3) . . ? C7 Si3 C1 113.2(3) . . ? C6 Si3 H3S 103(3) . . ? C7 Si3 H3S 107(3) . . ? C1 Si3 H3S 111(3) . . ? Si3 C1 Si2 113.1(3) . . ? Si3 C1 Si1 113.6(3) . 2_677 ? Si2 C1 Si1 113.8(2) . 2_677 ? Si3 C1 Si1 113.5(3) . . ? Si2 C1 Si1 113.6(3) . . ? Si1 C1 Si1 86.7(2) 2_677 . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si3 C6 H6A 109.5 . . ? Si3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si3 C7 H7A 109.5 . . ? Si3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.641 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.133