Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 207 _publ_requested_journal 'Perkin Transactions 1' loop_ _publ_author_name 'Shen, Yanchang' 'Sun, Jie' 'Wang, Guoping' _publ_contact_author_name 'Prof Yanchang Shen' _publ_contact_author_address ; Prof Yanchang Shen Laboratory of Organometallic Chemistry Shanghai Institute of Organic Chemistry Academia Sinica 354 Fenglin Lu Shanghai 200032 CHINA ; data_master_file_afc7*.xtl _database_code_CSD 152496 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jul 5 10:21:12 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 24.847(4) _cell_length_b 5.433(1) _cell_length_c 13.118(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1770(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 13.87 _cell_measurement_theta_max 21.81 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_Int_Tables_number 33 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y,1/2+z' '1/2-x,1/2+y,1/2+z' '1/2+x,1/2-y, +z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_measured ? _exptl_crystal_F000 752.00 _exptl_absorpt_coefficient_mu_cm 2.210 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_\% 0.63 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 1806 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 29 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 0 _diffrn_reflns_l_min 0 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 24.9718 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.01959 _diffrn_orient_matrix_12 -0.15949 _diffrn_orient_matrix_13 0.00840 _diffrn_orient_matrix_21 -0.03505 _diffrn_orient_matrix_22 0.08669 _diffrn_orient_matrix_23 -0.01078 _diffrn_orient_matrix_31 0.00280 _diffrn_orient_matrix_32 -0.03040 _diffrn_orient_matrix_33 -0.07499 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 76 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' F 0 12 0.017 0.010 'International Tables' O 0 8 0.011 0.006 'International Tables' S 0 4 0.125 0.123 'International Tables' #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom S 0.6353(1) 0.0662(5) 0.7499 0.0901 Uij ? ? F1 0.5878(3) 0.120(1) 0.9890(5) 0.1200 Uij ? ? F2 0.5654(3) 0.484(1) 1.0292(6) 0.1404 Uij ? ? F3 0.6436(3) 0.408(1) 0.9698(7) 0.1469 Uij ? ? O1 0.6118(3) -0.121(1) 0.6848(8) 0.1313 Uij ? ? O2 0.6572(3) -0.004(2) 0.8389(7) 0.1364 Uij ? ? C1 0.5863(3) 0.295(1) 0.7664(7) 0.0687 Uij ? ? C2 0.5714(3) 0.403(2) 0.8541(8) 0.0671 Uij ? ? C3 0.5300(3) 0.584(2) 0.8529(8) 0.0691 Uij ? ? C4 0.4971(4) 0.741(2) 0.8486(8) 0.0683 Uij ? ? C5 0.4566(3) 0.932(2) 0.8386(7) 0.0600 Uij ? ? C6 0.4384(4) 1.069(2) 0.9212(7) 0.0786 Uij ? ? C7 0.3993(4) 1.244(2) 0.907(1) 0.0886 Uij ? ? C8 0.3783(3) 1.292(2) 0.811(1) 0.0816 Uij ? ? C9 0.3960(4) 1.158(2) 0.7317(9) 0.0947 Uij ? ? C10 0.4350(4) 0.976(2) 0.7418(9) 0.0856 Uij ? ? C11 0.5601(4) 0.352(2) 0.6682(9) 0.0920 Uij ? ? C12 0.5930(5) 0.357(2) 0.9622(9) 0.0940 Uij ? ? C13 0.3354(5) 1.486(2) 0.799(2) 0.1359 Uij ? ? C14 0.6848(4) 0.218(1) 0.6798(9) 0.0761 Uij ? ? C15 0.7121(5) 0.420(2) 0.714(1) 0.1196 Uij ? ? C16 0.7517(6) 0.520(3) 0.649(2) 0.1727 Uij ? ? C17 0.7644(8) 0.433(5) 0.565(2) 0.1906 Uij ? ? C18 0.7387(5) 0.237(4) 0.528(1) 0.1385 Uij ? ? C19 0.6980(4) 0.131(2) 0.587(1) 0.1072 Uij ? ? H1 0.4535 1.0339 0.9862 0.1399 Uij ? ? H2 0.3862 1.3332 0.9645 0.1399 Uij ? ? H3 0.3817 1.1835 0.6638 0.1399 Uij ? ? H4 0.4475 0.8805 0.6843 0.1399 Uij ? ? H5 0.5351 0.2274 0.6516 0.1230 Uij ? ? H6 0.5875 0.3563 0.6157 0.1399 Uij ? ? H7 0.5430 0.5068 0.6707 0.1065 Uij ? ? H8 0.3052 1.4464 0.8396 0.1256 Uij ? ? H9 0.3498 1.6409 0.8212 0.1643 Uij ? ? H10 0.3249 1.5004 0.7297 0.1643 Uij ? ? H11 0.7063 0.4854 0.7770 0.1489 Uij ? ? H12 0.7708 0.6594 0.6671 0.2116 Uij ? ? H13 0.7914 0.4941 0.5178 0.2282 Uij ? ? H14 0.7456 0.1696 0.4627 0.1708 Uij ? ? H15 0.6795 -0.0043 0.5599 0.1256 Uij ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S 0.094(2) 0.066(1) 0.111(2) 0.004(1) 0.031(2) 0.019(2) F1 0.158(6) 0.116(5) 0.086(4) 0.032(4) 0.015(4) 0.032(4) F2 0.191(7) 0.154(6) 0.077(4) 0.072(5) -0.024(4) -0.032(4) F3 0.110(5) 0.171(7) 0.159(7) -0.015(5) -0.069(5) 0.034(6) O1 0.139(6) 0.064(4) 0.191(8) -0.032(4) 0.055(6) -0.043(5) O2 0.117(6) 0.173(8) 0.119(7) 0.059(6) 0.015(5) 0.030(6) C1 0.072(5) 0.057(4) 0.078(7) -0.011(4) 0.021(5) 0.017(5) C2 0.070(5) 0.060(5) 0.071(6) -0.010(4) 0.003(4) 0.007(5) C3 0.060(5) 0.071(5) 0.075(6) 0.006(5) 0.000(5) 0.006(5) C4 0.057(5) 0.075(5) 0.072(5) -0.008(5) 0.002(4) 0.009(5) C5 0.056(4) 0.066(5) 0.058(5) -0.015(4) 0.004(4) 0.004(4) C6 0.090(7) 0.087(6) 0.059(6) -0.015(6) 0.007(5) 0.005(5) C7 0.074(6) 0.070(6) 0.122(9) 0.011(5) 0.025(6) -0.009(6) C8 0.058(5) 0.066(6) 0.121(9) 0.006(5) 0.007(6) 0.014(6) C9 0.091(7) 0.099(7) 0.094(8) 0.011(6) 0.001(7) 0.025(7) C10 0.071(6) 0.102(7) 0.084(7) 0.011(5) 0.001(6) 0.002(6) C11 0.112(8) 0.086(7) 0.079(7) -0.016(6) 0.008(6) -0.008(6) C12 0.117(9) 0.087(7) 0.077(7) 0.013(7) -0.010(7) -0.001(6) C13 0.099(8) 0.099(7) 0.21(1) 0.033(7) 0.015(10) 0.034(9) C14 0.078(6) 0.052(5) 0.098(7) 0.008(4) 0.007(5) -0.003(5) C15 0.097(8) 0.082(6) 0.18(1) -0.013(6) -0.010(8) -0.030(8) C16 0.067(9) 0.11(1) 0.34(3) -0.043(8) 0.01(1) 0.03(2) C17 0.08(1) 0.21(2) 0.28(3) 0.01(1) 0.08(2) 0.13(2) C18 0.077(8) 0.21(2) 0.13(1) 0.005(10) 0.030(8) 0.04(1) C19 0.080(7) 0.101(7) 0.14(1) -0.013(6) 0.001(8) -0.005(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1071 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0660 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0760 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.760 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.43960 _refine_diff_density_max -0.27220 #------------------------------------------------------------------------------ _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S O(1) 1.450(9) ? ? yes S O(2) 1.343(9) ? ? yes S C(1) 1.753(9) ? ? yes S C(14) 1.743(10) ? ? yes F(1) C(12) 1.34(1) ? ? yes F(2) C(12) 1.31(1) ? ? yes F(3) C(12) 1.29(1) ? ? yes C(1) C(2) 1.34(1) ? ? yes C(1) C(11) 1.48(1) ? ? yes C(2) C(3) 1.42(1) ? ? yes C(2) C(12) 1.54(1) ? ? yes C(3) C(4) 1.18(1) ? ? yes C(4) C(5) 1.45(1) ? ? yes C(5) C(6) 1.39(1) ? ? yes C(5) C(10) 1.40(1) ? ? yes C(6) C(7) 1.37(1) ? ? yes C(7) C(8) 1.39(2) ? ? yes C(8) C(9) 1.34(1) ? ? yes C(8) C(13) 1.50(1) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(14) C(15) 1.36(1) ? ? yes C(14) C(19) 1.34(2) ? ? yes C(15) C(16) 1.40(2) ? ? yes C(16) C(17) 1.24(3) ? ? yes C(17) C(18) 1.33(3) ? ? yes C(18) C(19) 1.39(2) ? ? yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_bond_publ_flag O(1) S O(2) 118.5(6) ? ? ? yes O(1) S C(1) 106.7(5) ? ? ? yes O(1) S C(14) 107.8(5) ? ? ? yes O(2) S C(1) 112.0(5) ? ? ? yes O(2) S C(14) 107.9(5) ? ? ? yes C(1) S C(14) 102.7(4) ? ? ? yes S C(1) C(2) 127.4(7) ? ? ? yes S C(1) C(11) 110.3(7) ? ? ? yes C(2) C(1) C(11) 122.3(8) ? ? ? yes C(1) C(2) C(3) 119.5(9) ? ? ? yes C(1) C(2) C(12) 128.5(8) ? ? ? yes C(3) C(2) C(12) 112.0(9) ? ? ? yes C(2) C(3) C(4) 176.7(9) ? ? ? yes C(3) C(4) C(5) 177.5(10) ? ? ? yes C(4) C(5) C(6) 122.6(8) ? ? ? yes C(4) C(5) C(10) 118.0(8) ? ? ? yes C(6) C(5) C(10) 119.4(8) ? ? ? yes C(5) C(6) C(7) 119.6(9) ? ? ? yes C(6) C(7) C(8) 121.4(9) ? ? ? yes C(7) C(8) C(9) 118.4(9) ? ? ? yes C(7) C(8) C(13) 119(1) ? ? ? yes C(9) C(8) C(13) 122(1) ? ? ? yes C(8) C(9) C(10) 122(1) ? ? ? yes C(5) C(10) C(9) 118.4(9) ? ? ? yes F(1) C(12) F(2) 106(1) ? ? ? yes F(1) C(12) F(3) 106.2(10) ? ? ? yes F(1) C(12) C(2) 111.3(9) ? ? ? yes F(2) C(12) F(3) 110(1) ? ? ? yes F(2) C(12) C(2) 110.5(9) ? ? ? yes F(3) C(12) C(2) 112.2(10) ? ? ? yes S C(14) C(15) 124.1(10) ? ? ? yes S C(14) C(19) 118.9(8) ? ? ? yes C(15) C(14) C(19) 116(1) ? ? ? yes C(14) C(15) C(16) 117(1) ? ? ? yes C(15) C(16) C(17) 124(1) ? ? ? yes C(16) C(17) C(18) 120(1) ? ? ? yes C(17) C(18) C(19) 118(1) ? ? ? yes C(14) C(19) C(18) 122(1) ? ? ? yes #------------------------------------------------------------------------------ END