Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Rainer Streubel' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie der Technischen Universitat Braunschweig Postfach 3329 Braunschweig 38106 GERMANY ; _publ_contact_author_email R.STREUBEL@TU-BS.DE #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Report on a very unconventional access to [(Me_3Si)_2HCPCl_2W(CO)_5] and its reaction to various structurally characterized organo chalcogenophosphonic derivatives ; loop_ _publ_author_name _publ_author_address A.A.Khan ; Institut fur Anorganische und Analytische Chemie Technische Universitat Braunschweig Postfach 3329 38023 Braunschweig Germany ; C.Wismach ; Institut fur Anorganische und Analytische Chemie Technische Universitat Braunschweig Postfach 3329 38023 Braunschweig Germany ; P.G.Jones ; Institut fur Anorganische und Analytische Chemie Technische Universitat Braunschweig Postfach 3329 38023 Braunschweig Germany ; R.Streubel ; Institut fur Anorganische und Analytische Chemie Technische Universitat Braunschweig Postfach 3329 38023 Braunschweig Germany ; data_lanchi _database_code_CSD 197414 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H19 Cl2 O5 P Si2 W' _chemical_formula_weight 585.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.8271(8) _cell_length_b 9.6096(6) _cell_length_c 14.8458(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.063(3) _cell_angle_gamma 90.00 _cell_volume 2082.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 40209 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'cut tablet' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method ? _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 6.011 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.4287 _exptl_absorpt_correction_T_max 0.6949 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker Samrt 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 38893 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6084 _reflns_number_gt 5890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0485P)^2^+2.0392P] 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 'methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6084 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0828 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W W 0.593022(6) 0.530503(10) 0.234681(7) 0.01625(5) Uani 1 1 d . . . P P 0.54115(4) 0.30872(7) 0.29062(5) 0.01628(12) Uani 1 1 d . . . Si1 Si 0.40630(5) 0.15599(8) 0.13545(5) 0.01987(14) Uani 1 1 d . . . Si2 Si 0.35811(5) 0.17127(9) 0.33908(5) 0.02152(15) Uani 1 1 d . . . O1 O 0.46584(18) 0.6702(3) 0.36066(17) 0.0359(5) Uani 1 1 d . . . O2 O 0.75669(18) 0.5517(3) 0.40569(19) 0.0284(5) Uani 1 1 d . . . O3 O 0.65116(19) 0.8269(3) 0.1738(2) 0.0365(5) Uani 1 1 d . . . O4 O 0.72318(18) 0.3790(3) 0.11469(19) 0.0360(5) Uani 1 1 d . . . O5 O 0.42528(19) 0.5436(3) 0.06929(19) 0.0313(5) Uani 1 1 d . . . C1 C 0.5115(2) 0.6216(3) 0.3146(2) 0.0231(5) Uani 1 1 d . . . C2 C 0.6999(2) 0.5399(3) 0.3447(2) 0.0207(6) Uani 1 1 d . . . C3 C 0.6311(2) 0.7187(3) 0.1954(2) 0.0252(5) Uani 1 1 d . . . C4 C 0.6767(2) 0.4325(3) 0.1568(2) 0.0235(5) Uani 1 1 d . . . C5 C 0.4866(2) 0.5361(3) 0.1287(2) 0.0208(6) Uani 1 1 d . . . C6 C 0.42475(18) 0.2521(3) 0.25235(18) 0.0167(4) Uani 1 1 d . . . H6 H 0.3917 0.3419 0.2367 0.020 Uiso 1 1 calc R . . C7 C 0.4952(2) 0.1898(4) 0.0630(2) 0.0282(6) Uani 1 1 d . . . H7A H 0.5547 0.1560 0.0947 0.034 Uiso 1 1 calc R . . H7B H 0.4989 0.2900 0.0519 0.034 Uiso 1 1 calc R . . H7C H 0.4785 0.1411 0.0045 0.034 Uiso 1 1 calc R . . C8 C 0.2955(2) 0.2236(4) 0.0702(2) 0.0311(6) Uani 1 1 d . . . H8A H 0.2996 0.3247 0.0634 0.037 Uiso 1 1 calc R . . H8B H 0.2458 0.2013 0.1034 0.037 Uiso 1 1 calc R . . H8C H 0.2832 0.1801 0.0096 0.037 Uiso 1 1 calc R . . C9 C 0.4047(3) -0.0370(3) 0.1517(3) 0.0313(8) Uani 1 1 d . . . H9A H 0.4640 -0.0676 0.1858 0.038 Uiso 1 1 calc R . . H9B H 0.3930 -0.0828 0.0918 0.038 Uiso 1 1 calc R . . H9C H 0.3562 -0.0616 0.1860 0.038 Uiso 1 1 calc R . . C10 C 0.2407(2) 0.1239(4) 0.2796(3) 0.0337(7) Uani 1 1 d . . . H10A H 0.2098 0.2071 0.2510 0.040 Uiso 1 1 calc R . . H10B H 0.2056 0.0857 0.3240 0.040 Uiso 1 1 calc R . . H10C H 0.2450 0.0541 0.2324 0.040 Uiso 1 1 calc R . . C11 C 0.4155(3) 0.0124(4) 0.3924(3) 0.0394(9) Uani 1 1 d . . . H11A H 0.4775 0.0359 0.4234 0.047 Uiso 1 1 calc R . . H11B H 0.4189 -0.0573 0.3449 0.047 Uiso 1 1 calc R . . H11C H 0.3804 -0.0252 0.4370 0.047 Uiso 1 1 calc R . . C12 C 0.3395(2) 0.3007(4) 0.4279(2) 0.0346(7) Uani 1 1 d . . . H12A H 0.3088 0.3831 0.3981 0.041 Uiso 1 1 calc R . . H12B H 0.3987 0.3278 0.4639 0.041 Uiso 1 1 calc R . . H12C H 0.3013 0.2591 0.4683 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.56100(5) 0.31480(8) 0.43130(5) 0.02726(14) Uani 1 1 d . . . Cl2 Cl 0.61680(5) 0.13171(8) 0.27954(6) 0.02749(14) 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 W 0.01610(7) 0.01565(7) 0.01706(8) -0.00038(3) 0.00306(5) -0.00095(3) P 0.0151(3) 0.0173(3) 0.0159(3) 0.0003(2) 0.0013(2) -0.0007(2) Si1 0.0196(3) 0.0219(3) 0.0181(3) -0.0043(3) 0.0030(3) -0.0022(3) Si2 0.0189(3) 0.0269(4) 0.0194(3) 0.0007(3) 0.0049(3) -0.0030(3) O1 0.0341(12) 0.0453(14) 0.0284(12) -0.0059(10) 0.0058(9) 0.0142(11) O2 0.0249(11) 0.0310(11) 0.0275(12) -0.0057(10) -0.0003(9) 0.0019(9) O3 0.0397(13) 0.0258(11) 0.0431(14) 0.0070(10) 0.0048(11) -0.0090(9) O4 0.0341(12) 0.0397(13) 0.0370(13) -0.0087(11) 0.0137(10) 0.0038(10) O5 0.0272(12) 0.0409(14) 0.0231(12) 0.0038(9) -0.0029(10) -0.0001(9) C1 0.0220(12) 0.0239(13) 0.0219(13) -0.0002(10) -0.0008(10) 0.0013(10) C2 0.0220(14) 0.0189(12) 0.0218(14) -0.0021(9) 0.0058(11) 0.0009(9) C3 0.0254(13) 0.0231(13) 0.0271(14) 0.0004(11) 0.0041(11) -0.0011(10) C4 0.0217(12) 0.0241(13) 0.0247(14) -0.0018(11) 0.0038(10) -0.0029(11) C5 0.0216(13) 0.0208(14) 0.0208(14) 0.0005(9) 0.0062(11) -0.0013(9) C6 0.0176(10) 0.0174(11) 0.0149(10) -0.0017(9) 0.0022(8) 0.0008(8) C7 0.0290(14) 0.0335(15) 0.0242(14) -0.0073(12) 0.0105(11) -0.0062(12) C8 0.0256(14) 0.0422(17) 0.0224(14) -0.0036(13) -0.0041(11) 0.0015(13) C9 0.0315(17) 0.0243(16) 0.040(2) -0.0081(12) 0.0123(15) -0.0034(11) C10 0.0222(13) 0.0454(19) 0.0343(17) -0.0067(14) 0.0070(12) -0.0089(13) C11 0.047(2) 0.0311(17) 0.039(2) 0.0151(16) 0.0045(17) -0.0048(16) C12 0.0292(15) 0.050(2) 0.0259(15) -0.0101(14) 0.0081(12) 0.0001(14) Cl1 0.0278(3) 0.0369(4) 0.0152(3) 0.0023(3) -0.0015(2) -0.0075(3) Cl2 0.0204(3) 0.0218(3) 0.0397(4) 0.0023(3) 0.0035(3) 0.0052(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 W C3 2.012(3) . ? W C5 2.026(4) . ? W C1 2.034(3) . ? W C4 2.065(3) . ? W C2 2.070(3) . ? W P 2.4589(7) . ? P C6 1.804(3) . ? P Cl1 2.0584(9) . ? P Cl2 2.0598(9) . ? Si1 C7 1.869(3) . ? Si1 C9 1.871(3) . ? Si1 C8 1.871(3) . ? Si1 C6 1.943(3) . ? Si2 C11 1.856(4) . ? Si2 C10 1.865(3) . ? Si2 C12 1.867(3) . ? Si2 C6 1.919(3) . ? O1 C1 1.142(4) . ? O2 C2 1.129(4) . ? O3 C3 1.142(4) . ? O4 C4 1.132(4) . ? O5 C5 1.152(4) . ? 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 W C5 88.33(12) . . ? C3 W C1 90.44(12) . . ? C5 W C1 88.86(12) . . ? C3 W C4 91.20(12) . . ? C5 W C4 92.28(12) . . ? C1 W C4 178.02(12) . . ? C3 W C2 88.55(12) . . ? C5 W C2 175.82(11) . . ? C1 W C2 88.39(12) . . ? C4 W C2 90.56(12) . . ? C3 W P 176.00(9) . . ? C5 W P 92.18(8) . . ? C1 W P 85.61(9) . . ? C4 W P 92.74(9) . . ? C2 W P 90.74(8) . . ? C6 P Cl1 106.70(9) . . ? C6 P Cl2 103.30(9) . . ? Cl1 P Cl2 96.96(4) . . ? C6 P W 119.57(9) . . ? Cl1 P W 108.68(3) . . ? Cl2 P W 118.81(4) . . ? C7 Si1 C9 105.82(16) . . ? C7 Si1 C8 106.57(16) . . ? C9 Si1 C8 112.37(18) . . ? C7 Si1 C6 115.34(13) . . ? C9 Si1 C6 111.05(16) . . ? C8 Si1 C6 105.75(13) . . ? C11 Si2 C10 108.8(2) . . ? C11 Si2 C12 111.1(2) . . ? C10 Si2 C12 104.85(16) . . ? C11 Si2 C6 111.55(17) . . ? C10 Si2 C6 109.16(14) . . ? C12 Si2 C6 111.16(15) . . ? O1 C1 W 178.5(3) . . ? O2 C2 W 176.5(3) . . ? O3 C3 W 178.5(3) . . ? O4 C4 W 179.4(3) . . ? O5 C5 W 177.7(3) . . ? P C6 Si2 119.16(14) . . ? P C6 Si1 113.72(14) . . ? Si2 C6 Si1 113.48(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 W P C6 79.7(13) . . . . ? C5 W P C6 -17.66(14) . . . . ? C1 W P C6 71.03(13) . . . . ? C4 W P C6 -110.05(13) . . . . ? C2 W P C6 159.35(13) . . . . ? C3 W P Cl1 -43.0(13) . . . . ? C5 W P Cl1 -140.39(10) . . . . ? C1 W P Cl1 -51.70(9) . . . . ? C4 W P Cl1 127.22(9) . . . . ? C2 W P Cl1 36.63(9) . . . . ? C3 W P Cl2 -152.4(13) . . . . ? C5 W P Cl2 110.22(10) . . . . ? C1 W P Cl2 -161.09(9) . . . . ? C4 W P Cl2 17.83(9) . . . . ? C2 W P Cl2 -72.76(9) . . . . ? C3 W C1 O1 -157(10) . . . . ? C5 W C1 O1 115(10) . . . . ? C4 W C1 O1 -10(13) . . . . ? C2 W C1 O1 -68(10) . . . . ? P W C1 O1 23(10) . . . . ? C3 W C2 O2 50(5) . . . . ? C5 W C2 O2 8(6) . . . . ? C1 W C2 O2 -41(5) . . . . ? C4 W C2 O2 141(5) . . . . ? P W C2 O2 -126(5) . . . . ? C5 W C3 O3 75(12) . . . . ? C1 W C3 O3 -14(12) . . . . ? C4 W C3 O3 168(12) . . . . ? C2 W C3 O3 -102(12) . . . . ? P W C3 O3 -22(13) . . . . ? C3 W C4 O4 81(32) . . . . ? C5 W C4 O4 169(100) . . . . ? C1 W C4 O4 -65(33) . . . . ? C2 W C4 O4 -8(32) . . . . ? P W C4 O4 -98(32) . . . . ? C3 W C5 O5 -50(7) . . . . ? C1 W C5 O5 40(7) . . . . ? C4 W C5 O5 -142(7) . . . . ? C2 W C5 O5 -9(8) . . . . ? P W C5 O5 126(7) . . . . ? Cl1 P C6 Si2 -14.38(17) . . . . ? Cl2 P C6 Si2 87.21(14) . . . . ? W P C6 Si2 -138.07(11) . . . . ? Cl1 P C6 Si1 -152.41(11) . . . . ? Cl2 P C6 Si1 -50.82(14) . . . . ? W P C6 Si1 83.89(14) . . . . ? C11 Si2 C6 P -59.9(2) . . . . ? C10 Si2 C6 P 179.87(17) . . . . ? C12 Si2 C6 P 64.7(2) . . . . ? C11 Si2 C6 Si1 78.2(2) . . . . ? C10 Si2 C6 Si1 -42.0(2) . . . . ? C12 Si2 C6 Si1 -157.17(15) . . . . ? C7 Si1 C6 P -20.4(2) . . . . ? C9 Si1 C6 P 99.92(18) . . . . ? C8 Si1 C6 P -137.92(16) . . . . ? C7 Si1 C6 Si2 -160.90(15) . . . . ? C9 Si1 C6 Si2 -40.5(2) . . . . ? C8 Si1 C6 Si2 81.63(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.939 _refine_diff_density_min -1.792 _refine_diff_density_rms 0.199 data_pota _database_code_CSD 197415 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H20 Cl O2 P Si2' _chemical_formula_weight 258.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7903(6) _cell_length_b 8.7696(8) _cell_length_c 12.5541(10) _cell_angle_alpha 75.307(3) _cell_angle_beta 77.234(3) _cell_angle_gamma 72.823(3) _cell_volume 682.19(10) _cell_formula_units_Z 2 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5325 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'cut tablet' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7154 _exptl_absorpt_correction_T_max 0.9281 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker Smart 1000 CCD' _diffrn_measurement_method '\w and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9764 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3379 _reflns_number_gt 2830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'O-H free, methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3379 _refine_ls_number_parameters 128 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0869 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.22202(6) 0.38458(4) 0.10009(3) 0.01947(10) Uani 1 1 d . . . Si1 Si 0.23367(6) 0.63389(4) 0.22238(3) 0.02166(11) Uani 1 1 d . . . Si2 Si 0.42435(6) 0.24634(5) 0.31757(3) 0.02203(11) Uani 1 1 d . . . Cl Cl 0.32094(7) 0.14637(5) 0.08610(3) 0.03465(12) Uani 1 1 d . . . O1 O -0.00893(16) 0.40670(14) 0.15551(9) 0.0260(2) Uani 1 1 d D . . H01 H -0.082(4) 0.446(3) 0.1098(18) 0.072(8) Uiso 1 1 d D . . O2 O 0.25412(15) 0.48059(13) -0.01592(8) 0.0235(2) Uani 1 1 d . . . C1 C 0.3585(2) 0.41825(16) 0.19195(11) 0.0180(3) Uani 1 1 d . . . H1 H 0.4975 0.4252 0.1464 0.022 Uiso 1 1 calc R . . C2 C 0.1199(3) 0.78010(18) 0.10159(13) 0.0309(4) Uani 1 1 d . . . H2A H 0.0693 0.8897 0.1182 0.037 Uiso 1 1 calc R . . H2B H 0.0034 0.7467 0.0882 0.037 Uiso 1 1 calc R . . H2C H 0.2272 0.7806 0.0350 0.037 Uiso 1 1 calc R . . C3 C 0.0201(3) 0.62731(19) 0.34443(13) 0.0334(4) Uani 1 1 d . . . H3A H 0.0775 0.5559 0.4101 0.040 Uiso 1 1 calc R . . H3B H -0.0863 0.5852 0.3283 0.040 Uiso 1 1 calc R . . H3C H -0.0430 0.7374 0.3590 0.040 Uiso 1 1 calc R . . C4 C 0.4445(3) 0.70862(19) 0.24990(13) 0.0313(4) Uani 1 1 d . . . H4A H 0.5544 0.7106 0.1845 0.038 Uiso 1 1 calc R . . H4B H 0.5036 0.6357 0.3147 0.038 Uiso 1 1 calc R . . H4C H 0.3863 0.8189 0.2649 0.038 Uiso 1 1 calc R . . C5 C 0.5038(3) 0.3213(2) 0.42432(13) 0.0345(4) Uani 1 1 d . . . H5A H 0.3889 0.4084 0.4503 0.041 Uiso 1 1 calc R . . H5B H 0.6270 0.3635 0.3911 0.041 Uiso 1 1 calc R . . H5C H 0.5372 0.2313 0.4875 0.041 Uiso 1 1 calc R . . C6 C 0.1950(3) 0.15991(19) 0.38284(13) 0.0320(4) Uani 1 1 d . . . H6A H 0.2303 0.0737 0.4478 0.038 Uiso 1 1 calc R . . H6B H 0.1582 0.1144 0.3285 0.038 Uiso 1 1 calc R . . H6C H 0.0761 0.2463 0.4065 0.038 Uiso 1 1 calc R . . C7 C 0.6590(3) 0.08770(19) 0.27217(14) 0.0333(4) Uani 1 1 d . . . H7A H 0.7741 0.1385 0.2360 0.040 Uiso 1 1 calc R . . H7B H 0.6257 0.0372 0.2194 0.040 Uiso 1 1 calc R . . H7C H 0.7004 0.0042 0.3373 0.040 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 P 0.01913(18) 0.02205(18) 0.01673(18) -0.00262(14) -0.00320(13) -0.00531(14) Si1 0.0249(2) 0.01725(19) 0.0203(2) -0.00262(14) -0.00507(15) -0.00151(15) Si2 0.0251(2) 0.01817(19) 0.0208(2) -0.00152(15) -0.00811(15) -0.00124(15) Cl 0.0471(3) 0.02494(19) 0.0361(2) -0.01042(16) -0.01401(18) -0.00643(17) O1 0.0198(5) 0.0372(6) 0.0193(5) 0.0006(4) -0.0037(4) -0.0095(4) O2 0.0201(5) 0.0321(5) 0.0170(5) -0.0011(4) -0.0034(4) -0.0073(4) C1 0.0169(6) 0.0182(6) 0.0184(6) -0.0029(5) -0.0039(5) -0.0036(5) C2 0.0375(9) 0.0206(7) 0.0305(8) 0.0008(6) -0.0122(7) -0.0013(6) C3 0.0338(9) 0.0280(8) 0.0283(8) -0.0059(6) 0.0006(7) 0.0032(7) C4 0.0400(9) 0.0246(7) 0.0333(8) -0.0065(6) -0.0124(7) -0.0088(7) C5 0.0457(10) 0.0290(8) 0.0292(8) -0.0035(6) -0.0196(7) -0.0020(7) C6 0.0383(9) 0.0272(8) 0.0258(8) 0.0033(6) -0.0042(7) -0.0095(7) C7 0.0315(8) 0.0257(8) 0.0389(9) -0.0059(7) -0.0133(7) 0.0035(6) _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 P O2 1.4912(10) . ? P O1 1.5452(11) . ? P C1 1.7557(14) . ? P Cl 2.0375(5) . ? Si1 C3 1.8645(16) . ? Si1 C2 1.8673(15) . ? Si1 C4 1.8673(18) . ? Si1 C1 1.9280(13) . ? Si2 C6 1.8683(17) . ? Si2 C7 1.8685(16) . ? Si2 C5 1.8696(17) . ? Si2 C1 1.9150(13) . ? 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 O2 P O1 114.46(6) . . ? O2 P C1 114.49(6) . . ? O1 P C1 107.72(6) . . ? O2 P Cl 105.55(5) . . ? O1 P Cl 104.50(5) . . ? C1 P Cl 109.58(5) . . ? C3 Si1 C2 107.87(8) . . ? C3 Si1 C4 111.32(8) . . ? C2 Si1 C4 107.97(7) . . ? C3 Si1 C1 110.00(7) . . ? C2 Si1 C1 112.26(7) . . ? C4 Si1 C1 107.44(7) . . ? C6 Si2 C7 111.98(8) . . ? C6 Si2 C5 109.19(8) . . ? C7 Si2 C5 104.84(8) . . ? C6 Si2 C1 110.51(7) . . ? C7 Si2 C1 109.23(7) . . ? C5 Si2 C1 110.97(7) . . ? P C1 Si2 117.04(7) . . ? P C1 Si1 108.98(7) . . ? Si2 C1 Si1 116.51(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 P C1 Si2 -154.59(7) . . . . ? O1 P C1 Si2 76.87(9) . . . . ? Cl P C1 Si2 -36.25(8) . . . . ? O2 P C1 Si1 70.55(8) . . . . ? O1 P C1 Si1 -58.00(8) . . . . ? Cl P C1 Si1 -171.11(5) . . . . ? C6 Si2 C1 P -43.73(10) . . . . ? C7 Si2 C1 P 79.89(10) . . . . ? C5 Si2 C1 P -165.01(8) . . . . ? C6 Si2 C1 Si1 87.77(9) . . . . ? C7 Si2 C1 Si1 -148.61(8) . . . . ? C5 Si2 C1 Si1 -33.51(10) . . . . ? C3 Si1 C1 P 88.85(9) . . . . ? C2 Si1 C1 P -31.27(10) . . . . ? C4 Si1 C1 P -149.82(7) . . . . ? C3 Si1 C1 Si2 -46.28(10) . . . . ? C2 Si1 C1 Si2 -166.40(8) . . . . ? C4 Si1 C1 Si2 75.05(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H01 O2 0.786(16) 1.718(17) 2.5017(15) 174(3) 2_565 C1 H1 O2 1.00 2.26 3.2256(17) 161.0 2_665 C4 H4A O2 0.98 2.88 3.658(2) 137.3 2_665 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.555 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.063 data_jhinga _database_code_CSD 197416 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H19 Cl2 P S Si2' _chemical_formula_weight 293.33 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 8.619(4) _cell_length_b 14.482(7) _cell_length_c 12.031(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.926(10) _cell_angle_gamma 90.00 _cell_volume 1444.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5473 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'cut tablet' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method ? _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker Samrt 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23211 _diffrn_reflns_av_R_equivalents 0.1682 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 31.11 _reflns_number_total 4504 _reflns_number_gt 3749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material ShelXL-97 _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^)+(0.1130P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'Methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4504 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0690 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.40124(5) 0.16185(3) 0.81625(4) 0.01828(14) Uani 1 1 d . . . S S 0.47398(6) 0.16750(3) 0.67939(5) 0.02440(15) Uani 1 1 d . . . Cl1 Cl 0.58564(6) 0.16578(4) 0.96439(5) 0.02787(15) Uani 1 1 d . . . Cl2 Cl 0.31262(6) 0.03520(3) 0.83883(5) 0.03041(15) Uani 1 1 d . . . Si1 Si 0.03867(6) 0.21645(4) 0.75288(5) 0.02010(14) Uani 1 1 d . . . Si2 Si 0.32957(6) 0.36907(3) 0.80837(5) 0.01891(14) Uani 1 1 d . . . C1 C 0.2594(2) 0.24553(12) 0.83371(16) 0.0172(3) Uani 1 1 d . . . H1 H 0.268(3) 0.2392(16) 0.912(2) 0.018(5) Uiso 1 1 d . . . C2 C -0.0905(2) 0.32184(16) 0.7335(2) 0.0319(5) Uani 1 1 d . . . H2A H -0.0486 0.3683 0.6899 0.038 Uiso 1 1 calc R . . H2B H -0.0894 0.3469 0.8094 0.038 Uiso 1 1 calc R . . H2C H -0.2013 0.3057 0.6910 0.038 Uiso 1 1 calc R . . C3 C -0.0465(2) 0.13617(14) 0.8424(2) 0.0284(4) Uani 1 1 d . . . H3A H -0.0422 0.1655 0.9166 0.034 Uiso 1 1 calc R . . H3B H 0.0168 0.0790 0.8559 0.034 Uiso 1 1 calc R . . H3C H -0.1588 0.1219 0.8015 0.034 Uiso 1 1 calc R . . C4 C 0.0251(3) 0.16716(15) 0.60755(19) 0.0284(4) Uani 1 1 d . . . H4A H -0.0884 0.1633 0.5628 0.034 Uiso 1 1 calc R . . H4B H 0.0728 0.1052 0.6163 0.034 Uiso 1 1 calc R . . H4C H 0.0837 0.2070 0.5670 0.034 Uiso 1 1 calc R . . C5 C 0.2772(3) 0.39677(14) 0.65110(18) 0.0266(4) Uani 1 1 d . . . H5A H 0.1616 0.3865 0.6165 0.032 Uiso 1 1 calc R . . H5B H 0.3391 0.3568 0.6133 0.032 Uiso 1 1 calc R . . H5C H 0.3033 0.4615 0.6409 0.032 Uiso 1 1 calc R . . C6 C 0.2298(3) 0.45050(13) 0.88719(19) 0.0271(4) Uani 1 1 d . . . H6A H 0.2731 0.5128 0.8846 0.033 Uiso 1 1 calc R . . H6B H 0.2506 0.4306 0.9678 0.033 Uiso 1 1 calc R . . H6C H 0.1132 0.4508 0.8505 0.033 Uiso 1 1 calc R . . C7 C 0.5509(2) 0.38383(14) 0.8720(2) 0.0270(4) Uani 1 1 d . . . H7A H 0.6090 0.3424 0.8329 0.032 Uiso 1 1 calc R . . H7B H 0.5792 0.3689 0.9546 0.032 Uiso 1 1 calc R . . H7C H 0.5809 0.4479 0.8619 0.032 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 P 0.0198(2) 0.0206(2) 0.0153(3) -0.00021(15) 0.00630(18) 0.00162(14) S 0.0267(3) 0.0319(3) 0.0176(3) -0.00279(16) 0.0110(2) 0.00107(16) Cl1 0.0244(2) 0.0394(3) 0.0180(3) 0.00340(17) 0.00270(18) 0.00726(16) Cl2 0.0387(3) 0.0201(2) 0.0374(3) 0.00156(17) 0.0188(2) 0.00061(16) Si1 0.0184(2) 0.0272(3) 0.0148(3) -0.00090(18) 0.00460(19) -0.00162(16) Si2 0.0244(3) 0.0197(2) 0.0132(3) -0.00021(16) 0.00627(19) -0.00164(16) C1 0.0191(7) 0.0201(7) 0.0131(8) -0.0006(6) 0.0058(6) 0.0010(6) C2 0.0235(9) 0.0397(11) 0.0305(12) 0.0014(9) 0.0042(8) 0.0069(8) C3 0.0247(9) 0.0379(10) 0.0241(11) -0.0009(8) 0.0095(8) -0.0077(8) C4 0.0302(10) 0.0385(11) 0.0163(10) -0.0040(7) 0.0063(8) -0.0075(8) C5 0.0375(10) 0.0283(9) 0.0147(9) 0.0023(7) 0.0084(8) -0.0016(8) C6 0.0396(10) 0.0230(8) 0.0202(10) -0.0029(7) 0.0107(8) 0.0024(7) C7 0.0277(9) 0.0310(9) 0.0225(10) -0.0014(8) 0.0071(8) -0.0085(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 P C1 1.7744(18) . ? P S 1.9176(10) . ? P Cl2 2.0336(10) . ? P Cl1 2.0374(10) . ? Si1 C4 1.862(2) . ? Si1 C2 1.866(2) . ? Si1 C3 1.866(2) . ? Si1 C1 1.9304(19) . ? Si2 C7 1.863(2) . ? Si2 C5 1.864(2) . ? Si2 C6 1.865(2) . ? Si2 C1 1.9394(19) . ? 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 P S 118.08(7) . . ? C1 P Cl2 107.69(7) . . ? S P Cl2 112.11(3) . . ? C1 P Cl1 105.95(7) . . ? S P Cl1 112.93(5) . . ? Cl2 P Cl1 98.03(3) . . ? C4 Si1 C2 108.34(11) . . ? C4 Si1 C3 111.67(10) . . ? C2 Si1 C3 105.43(11) . . ? C4 Si1 C1 110.86(9) . . ? C2 Si1 C1 110.87(9) . . ? C3 Si1 C1 109.55(9) . . ? C7 Si2 C5 109.14(10) . . ? C7 Si2 C6 106.37(10) . . ? C5 Si2 C6 111.28(10) . . ? C7 Si2 C1 111.70(9) . . ? C5 Si2 C1 111.03(9) . . ? C6 Si2 C1 107.23(9) . . ? P C1 Si1 114.03(10) . . ? P C1 Si2 110.89(9) . . ? Si1 C1 Si2 115.40(9) . . ? 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 S P C1 Si1 82.46(10) . . . . ? Cl2 P C1 Si1 -45.71(11) . . . . ? Cl1 P C1 Si1 -149.82(8) . . . . ? S P C1 Si2 -49.83(11) . . . . ? Cl2 P C1 Si2 -178.00(6) . . . . ? Cl1 P C1 Si2 77.89(9) . . . . ? C4 Si1 C1 P -40.40(13) . . . . ? C2 Si1 C1 P -160.76(11) . . . . ? C3 Si1 C1 P 83.29(13) . . . . ? C4 Si1 C1 Si2 89.69(12) . . . . ? C2 Si1 C1 Si2 -30.68(14) . . . . ? C3 Si1 C1 Si2 -146.62(10) . . . . ? C7 Si2 C1 P -39.87(13) . . . . ? C5 Si2 C1 P 82.21(12) . . . . ? C6 Si2 C1 P -156.04(10) . . . . ? C7 Si2 C1 Si1 -171.45(10) . . . . ? C5 Si2 C1 Si1 -49.37(13) . . . . ? C6 Si2 C1 Si1 72.38(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2C Cl1 0.98 2.87 3.653(3) 137.7 4_465 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.262 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.181 data_matsya _database_code_CSD 197417 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H19 Cl2 P Se Si2' _chemical_formula_weight 340.23 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' P P 0.1023 0.0942 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 8.6576(10) _cell_length_b 14.5623(16) _cell_length_c 12.1849(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.019(3) _cell_angle_gamma 90.00 _cell_volume 1476.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7166 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description 'cut prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method ? _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 3.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3131 _exptl_absorpt_correction_T_max 0.4935 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker Samrt 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17609 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.28 _reflns_number_total 3665 _reflns_number_gt 2925 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Samrt' _computing_cell_refinement 'Bruker Saint' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'methyls rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3665 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se Se 0.98055(3) 0.167922(18) 0.67312(2) 0.02226(10) Uani 1 1 d . . . P P 0.90259(7) 0.16291(4) 0.81869(6) 0.01666(14) Uani 1 1 d . . . Si1 Si 0.54049(8) 0.21694(5) 0.75560(6) 0.01946(16) Uani 1 1 d . . . Si2 Si 0.82894(8) 0.36978(5) 0.80845(6) 0.01765(15) Uani 1 1 d . . . Cl1 Cl 0.81514(8) 0.03600(4) 0.84300(6) 0.02701(16) Uani 1 1 d . . . Cl2 Cl 1.08790(7) 0.16797(4) 0.96610(5) 0.02317(14) Uani 1 1 d . . . C1 C 0.7607(3) 0.24652(15) 0.8347(2) 0.0154(4) Uani 1 1 d . . . H1 H 0.7654 0.2449 0.9176 0.019 Uiso 1 1 calc R . . C2 C 0.4112(3) 0.3214(2) 0.7363(3) 0.0306(6) Uani 1 1 d . . . H2A H 0.4486 0.3662 0.6894 0.037 Uiso 1 1 calc R . . H2B H 0.4174 0.3484 0.8111 0.037 Uiso 1 1 calc R . . H2C H 0.2997 0.3045 0.6984 0.037 Uiso 1 1 calc R . . C3 C 0.4581(3) 0.1376(2) 0.8455(3) 0.0290(6) Uani 1 1 d . . . H3A H 0.3446 0.1252 0.8076 0.035 Uiso 1 1 calc R . . H3B H 0.4679 0.1660 0.9200 0.035 Uiso 1 1 calc R . . H3C H 0.5184 0.0798 0.8561 0.035 Uiso 1 1 calc R . . C4 C 0.5255(3) 0.16708(19) 0.6121(2) 0.0281(6) Uani 1 1 d . . . H4A H 0.4124 0.1559 0.5721 0.034 Uiso 1 1 calc R . . H4B H 0.5849 0.1090 0.6210 0.034 Uiso 1 1 calc R . . H4C H 0.5713 0.2101 0.5678 0.034 Uiso 1 1 calc R . . C5 C 0.7752(3) 0.39770(18) 0.6532(2) 0.0262(6) Uani 1 1 d . . . H5A H 0.6599 0.3878 0.6195 0.031 Uiso 1 1 calc R . . H5B H 0.8360 0.3579 0.6153 0.031 Uiso 1 1 calc R . . H5C H 0.8015 0.4621 0.6432 0.031 Uiso 1 1 calc R . . C6 C 0.7292(3) 0.45046(17) 0.8864(2) 0.0254(6) Uani 1 1 d . . . H6A H 0.7749 0.5120 0.8865 0.030 Uiso 1 1 calc R . . H6B H 0.7467 0.4293 0.9653 0.030 Uiso 1 1 calc R . . H6C H 0.6137 0.4524 0.8484 0.030 Uiso 1 1 calc R . . C7 C 1.0500(3) 0.38563(18) 0.8705(2) 0.0254(6) Uani 1 1 d . . . H7A H 1.0784 0.4498 0.8616 0.030 Uiso 1 1 calc R . . H7B H 1.1079 0.3457 0.8306 0.030 Uiso 1 1 calc R . . H7C H 1.0797 0.3697 0.9517 0.030 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 Se 0.02302(15) 0.02488(16) 0.02138(16) -0.00247(9) 0.01033(11) 0.00087(10) P 0.0170(3) 0.0141(3) 0.0194(3) 0.0002(2) 0.0060(2) 0.0010(2) Si1 0.0153(3) 0.0214(4) 0.0213(4) -0.0006(3) 0.0045(3) -0.0018(2) Si2 0.0210(3) 0.0140(3) 0.0181(3) -0.0001(2) 0.0058(3) -0.0010(2) Cl1 0.0328(3) 0.0133(3) 0.0397(4) 0.0020(2) 0.0179(3) -0.0001(2) Cl2 0.0208(3) 0.0281(3) 0.0189(3) 0.0024(2) 0.0028(2) 0.0067(2) C1 0.0155(10) 0.0156(11) 0.0153(12) -0.0008(8) 0.0043(9) 0.0002(8) C2 0.0197(12) 0.0317(16) 0.0395(17) 0.0012(12) 0.0064(12) 0.0035(11) C3 0.0196(12) 0.0357(16) 0.0332(16) 0.0041(12) 0.0100(11) -0.0061(11) C4 0.0260(13) 0.0348(16) 0.0216(14) -0.0046(11) 0.0034(11) -0.0085(11) C5 0.0354(14) 0.0210(13) 0.0236(14) 0.0030(10) 0.0106(11) 0.0001(11) C6 0.0319(14) 0.0159(12) 0.0291(15) -0.0022(10) 0.0096(12) 0.0015(10) C7 0.0229(12) 0.0251(14) 0.0283(15) -0.0001(11) 0.0071(11) -0.0058(10) _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 Se P 2.0659(7) . ? P C1 1.778(2) . ? P Cl1 2.0495(9) . ? P Cl2 2.0531(9) . ? Si1 C4 1.864(3) . ? Si1 C3 1.864(3) . ? Si1 C2 1.864(3) . ? Si1 C1 1.932(2) . ? Si2 C5 1.864(3) . ? Si2 C6 1.866(3) . ? Si2 C7 1.868(3) . ? Si2 C1 1.944(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 C1 P Cl1 107.91(8) . . ? C1 P Cl2 106.04(8) . . ? Cl1 P Cl2 97.85(4) . . ? C1 P Se 117.99(8) . . ? Cl1 P Se 112.16(3) . . ? Cl2 P Se 112.85(4) . . ? C4 Si1 C3 111.75(13) . . ? C4 Si1 C2 108.39(14) . . ? C3 Si1 C2 105.43(14) . . ? C4 Si1 C1 111.00(12) . . ? C3 Si1 C1 109.26(12) . . ? C2 Si1 C1 110.87(12) . . ? C5 Si2 C6 111.00(12) . . ? C5 Si2 C7 108.93(13) . . ? C6 Si2 C7 106.42(12) . . ? C5 Si2 C1 111.50(11) . . ? C6 Si2 C1 107.05(11) . . ? C7 Si2 C1 111.82(11) . . ? P C1 Si1 114.14(12) . . ? P C1 Si2 111.31(12) . . ? Si1 C1 Si2 115.26(12) . . ? 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 Cl1 P C1 Si1 -45.59(14) . . . . ? Cl2 P C1 Si1 -149.61(10) . . . . ? Se P C1 Si1 82.77(13) . . . . ? Cl1 P C1 Si2 -178.19(9) . . . . ? Cl2 P C1 Si2 77.80(12) . . . . ? Se P C1 Si2 -49.82(14) . . . . ? C4 Si1 C1 P -40.82(18) . . . . ? C3 Si1 C1 P 82.87(17) . . . . ? C2 Si1 C1 P -161.35(14) . . . . ? C4 Si1 C1 Si2 89.86(15) . . . . ? C3 Si1 C1 Si2 -146.45(14) . . . . ? C2 Si1 C1 Si2 -30.67(18) . . . . ? C5 Si2 C1 P 82.80(15) . . . . ? C6 Si2 C1 P -155.62(13) . . . . ? C7 Si2 C1 P -39.43(17) . . . . ? C5 Si2 C1 Si1 -49.23(17) . . . . ? C6 Si2 C1 Si1 72.35(16) . . . . ? C7 Si2 C1 Si1 -171.46(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2C Cl2 0.98 2.94 3.690(3) 133.7 4_465 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.117 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.107