# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1650 data_master_file_afc7*.xtl #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jan 14 16:07:15 2000' _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 SHELXS86 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 14.633(2) _cell_length_b 19.668(4) _cell_length_c 7.749(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2230.0(8) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 18.40 _cell_measurement_theta_max 21.59 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_measured ? _exptl_crystal_F000 912.00 _exptl_absorpt_coefficient_mu_cm 1.657 #------------------------------------------------------------------------------ _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_\% 0.21 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2938 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 19 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 25 _diffrn_reflns_l_min 0 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 27.4862 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.04983 _diffrn_orient_matrix_12 -0.03443 _diffrn_orient_matrix_13 0.01272 _diffrn_orient_matrix_21 0.04647 _diffrn_orient_matrix_22 -0.03563 _diffrn_orient_matrix_23 0.02785 _diffrn_orient_matrix_31 -0.00527 _diffrn_orient_matrix_32 0.01141 _diffrn_orient_matrix_33 0.12537 #------------------------------------------------------------------------------ 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 0 112 0.003 0.002 'International Tables' H 0 116 0.000 0.000 'International Tables' N 0 4 0.006 0.003 'International Tables' O 0 4 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 -0.17164(5) -0.85862(3) -0.0126(1) 0.0437 Uij ? ? O -0.4562(1) -0.81022(10) 0.1318(3) 0.0467 Uij ? ? N -0.3157(1) -0.8150(1) 0.2492(3) 0.0366 Uij ? ? C1 -0.1340(2) -0.7390(1) 0.1621(4) 0.0403 Uij ? ? C2 -0.1709(2) -0.7655(1) -0.0177(4) 0.0346 Uij ? ? C3 -0.2594(2) -0.7314(1) -0.0735(3) 0.0298 Uij ? ? C4 -0.3439(1) -0.7348(1) 0.0136(3) 0.0292 Uij ? ? C5 -0.4050(2) -0.6804(1) -0.0012(4) 0.0340 Uij ? ? C6 -0.3840(2) -0.6229(1) -0.0983(4) 0.0374 Uij ? ? C7 -0.3123(2) -0.6283(1) -0.2132(4) 0.0413 Uij ? ? C8 -0.2513(2) -0.6820(1) -0.2025(3) 0.0358 Uij ? ? C9 -0.4244(2) -0.5541(1) -0.0507(5) 0.0511 Uij ? ? C10 -0.3697(3) -0.5164(2) 0.0948(6) 0.0688 Uij ? ? C11 -0.2903(2) -0.5574(2) 0.1656(4) 0.0490 Uij ? ? C12 -0.2054(2) -0.5578(2) 0.0824(4) 0.0502 Uij ? ? C13 -0.1470(2) -0.6123(2) 0.0995(4) 0.0451 Uij ? ? C14 -0.1710(2) -0.6679(1) 0.2000(3) 0.0367 Uij ? ? C15 -0.2439(2) -0.6597(1) 0.3127(4) 0.0403 Uij ? ? C16 -0.3028(2) -0.6046(2) 0.2946(4) 0.0465 Uij ? ? C17 -0.3667(2) -0.7887(1) 0.1386(3) 0.0302 Uij ? ? C18 -0.4615(2) -0.8659(1) 0.2542(4) 0.0441 Uij ? ? C19 -0.3698(2) -0.8639(1) 0.3506(4) 0.0373 Uij ? ? C20 -0.3745(2) -0.8420(2) 0.5391(4) 0.0413 Uij ? ? C21 -0.4152(3) -0.8985(2) 0.6512(5) 0.0730 Uij ? ? C22 -0.4272(2) -0.7757(2) 0.5623(4) 0.0512 Uij ? ? C23 -0.1431(2) -0.8841(1) -0.2250(4) 0.0360 Uij ? ? C24 -0.0934(2) -0.8472(1) -0.3452(4) 0.0454 Uij ? ? C25 -0.0723(3) -0.8752(2) -0.5040(5) 0.0582 Uij ? ? C26 -0.1002(3) -0.9407(2) -0.5455(5) 0.0624 Uij ? ? C27 -0.1493(3) -0.9769(2) -0.4272(5) 0.0595 Uij ? ? C28 -0.1711(2) -0.9495(1) -0.2690(5) 0.0499 Uij ? ? H1 -0.1504 -0.7706 0.2607 0.0688 Uij ? ? H2 -0.0645 -0.7399 0.1438 0.0688 Uij ? ? H3 -0.1287 -0.7538 -0.1135 0.0688 Uij ? ? H4 -0.4561 -0.6775 0.0850 0.0688 Uij ? ? H5 -0.3010 -0.5970 -0.2869 0.0688 Uij ? ? H6 -0.2013 -0.6779 -0.2797 0.0688 Uij ? ? H7 -0.4316 -0.5266 -0.1597 0.0688 Uij ? ? H8 -0.4858 -0.5544 0.0017 0.0688 Uij ? ? H9 -0.3558 -0.4752 0.0452 0.0688 Uij ? ? H10 -0.4138 -0.5084 0.1868 0.0688 Uij ? ? H11 -0.1913 -0.5288 -0.0019 0.0688 Uij ? ? H12 -0.0956 -0.6117 0.0056 0.0688 Uij ? ? H13 -0.2574 -0.6875 0.3945 0.0688 Uij ? ? H14 -0.3516 -0.6055 0.3702 0.0688 Uij ? ? H15 -0.5131 -0.8543 0.3338 0.0688 Uij ? ? H16 -0.4711 -0.9129 0.1869 0.0688 Uij ? ? H17 -0.3358 -0.9081 0.3430 0.0688 Uij ? ? H18 -0.3136 -0.8319 0.5897 0.0688 Uij ? ? H19 -0.4754 -0.9043 0.6212 0.0688 Uij ? ? H20 -0.3810 -0.9426 0.6315 0.0688 Uij ? ? H21 -0.4111 -0.8832 0.7818 0.0688 Uij ? ? H22 -0.4294 -0.7581 0.6905 0.0688 Uij ? ? H23 -0.4065 -0.7444 0.4619 0.0688 Uij ? ? H24 -0.4909 -0.7807 0.5433 0.0688 Uij ? ? H25 -0.0696 -0.7979 -0.3245 0.0688 Uij ? ? H26 -0.0465 -0.8483 -0.5901 0.0688 Uij ? ? H27 -0.0815 -0.9582 -0.6595 0.0688 Uij ? ? H28 -0.1713 -1.0205 -0.4386 0.0688 Uij ? ? H29 -0.2090 -0.9720 -0.1821 0.0688 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 0.0507(4) 0.0339(3) 0.0465(4) 0.0067(3) 0.0125(4) 0.0036(3) O 0.0369(10) 0.046(1) 0.058(1) -0.0176(8) -0.0153(10) 0.017(1) N 0.0287(10) 0.044(1) 0.037(1) -0.0001(9) 0.0030(10) 0.008(1) C1 0.028(1) 0.046(1) 0.047(2) 0.002(1) -0.008(1) 0.000(1) C2 0.031(1) 0.033(1) 0.040(1) 0.0017(10) 0.002(1) -0.002(1) C3 0.032(1) 0.030(1) 0.027(1) -0.0020(10) -0.0014(10) -0.004(1) C4 0.030(1) 0.030(1) 0.028(1) -0.0033(9) -0.004(1) -0.003(1) C5 0.028(1) 0.036(1) 0.038(1) -0.0016(9) -0.003(1) -0.002(1) C6 0.037(1) 0.034(1) 0.042(1) 0.001(1) -0.010(1) 0.002(1) C7 0.048(2) 0.036(1) 0.039(1) -0.005(1) -0.006(1) 0.007(1) C8 0.037(1) 0.041(1) 0.029(1) -0.005(1) 0.001(1) 0.000(1) C9 0.045(2) 0.035(1) 0.073(2) 0.008(1) -0.004(2) 0.006(1) C10 0.077(2) 0.042(2) 0.088(3) 0.019(2) -0.014(2) -0.014(2) C11 0.058(2) 0.038(1) 0.051(2) 0.002(1) -0.005(2) -0.015(1) C12 0.066(2) 0.039(2) 0.045(2) -0.010(1) 0.002(2) -0.005(1) C13 0.044(2) 0.048(2) 0.044(2) -0.014(1) 0.003(1) -0.007(1) C14 0.032(1) 0.043(1) 0.036(1) -0.006(1) -0.007(1) -0.007(1) C15 0.045(1) 0.044(1) 0.032(1) -0.009(1) -0.002(1) -0.008(1) C16 0.047(2) 0.047(2) 0.045(2) -0.003(1) 0.008(1) -0.018(1) C17 0.028(1) 0.032(1) 0.031(1) -0.0020(10) 0.002(1) -0.003(1) C18 0.044(1) 0.043(1) 0.045(2) -0.016(1) -0.006(1) 0.008(1) C19 0.036(1) 0.032(1) 0.044(1) 0.002(1) 0.001(1) 0.005(1) C20 0.035(1) 0.052(2) 0.037(1) -0.002(1) 0.000(1) 0.010(1) C21 0.063(2) 0.090(3) 0.066(2) -0.004(2) 0.010(2) 0.042(2) C22 0.048(2) 0.060(2) 0.046(2) -0.002(1) 0.008(1) -0.010(2) C23 0.031(1) 0.034(1) 0.042(1) 0.007(1) -0.002(1) 0.001(1) C24 0.048(2) 0.040(2) 0.048(2) -0.004(1) 0.004(1) -0.002(1) C25 0.077(2) 0.054(2) 0.044(2) -0.004(2) 0.006(2) 0.001(2) C26 0.089(3) 0.053(2) 0.045(2) 0.001(2) -0.003(2) -0.010(2) C27 0.076(2) 0.042(2) 0.061(2) -0.004(2) -0.010(2) -0.011(2) C28 0.051(2) 0.037(1) 0.061(2) -0.002(1) 0.000(2) 0.003(1) #------------------------------------------------------------------------------ _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 17.86539 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2555 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0430 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0540 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.800 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.43080 _refine_diff_density_max -0.34400 #------------------------------------------------------------------------------ _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 C(2) 1.833(3) ? ? yes S C(23) 1.770(3) ? ? yes O C(17) 1.376(3) ? ? yes O C(18) 1.451(3) ? ? yes N C(17) 1.249(3) ? ? yes N C(19) 1.473(3) ? ? yes C(1) C(2) 1.583(4) ? ? yes C(1) C(14) 1.528(4) ? ? yes C(2) C(3) 1.521(3) ? ? yes C(3) C(4) 1.410(3) ? ? yes C(3) C(8) 1.400(4) ? ? yes C(4) C(5) 1.398(3) ? ? yes C(4) C(17) 1.475(3) ? ? yes C(5) C(6) 1.393(4) ? ? yes C(6) C(7) 1.380(4) ? ? yes C(6) C(9) 1.522(4) ? ? yes C(7) C(8) 1.386(4) ? ? yes C(9) C(10) 1.568(5) ? ? yes C(10) C(11) 1.517(5) ? ? yes C(11) C(12) 1.400(5) ? ? yes C(11) C(16) 1.376(4) ? ? yes C(12) C(13) 1.377(4) ? ? yes C(13) C(14) 1.387(4) ? ? yes C(14) C(15) 1.388(4) ? ? yes C(15) C(16) 1.393(4) ? ? yes C(18) C(19) 1.536(4) ? ? yes C(19) C(20) 1.525(4) ? ? yes C(20) C(21) 1.531(4) ? ? yes C(20) C(22) 1.526(4) ? ? yes C(23) C(24) 1.386(4) ? ? yes C(23) C(28) 1.393(4) ? ? yes C(24) C(25) 1.382(5) ? ? yes C(25) C(26) 1.391(4) ? ? yes C(26) C(27) 1.364(5) ? ? yes C(27) C(28) 1.377(5) ? ? 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_angle_publ_flag C(2) S C(23) 105.1(1) ? ? ? yes C(17) O C(18) 104.9(2) ? ? ? yes C(17) N C(19) 108.3(2) ? ? ? yes C(2) C(1) C(14) 110.4(2) ? ? ? yes S C(2) C(1) 108.2(2) ? ? ? yes S C(2) C(3) 116.2(2) ? ? ? yes C(1) C(2) C(3) 113.3(2) ? ? ? yes C(2) C(3) C(4) 126.2(2) ? ? ? yes C(2) C(3) C(8) 115.9(2) ? ? ? yes C(4) C(3) C(8) 116.6(2) ? ? ? yes C(3) C(4) C(5) 119.0(2) ? ? ? yes C(3) C(4) C(17) 123.1(2) ? ? ? yes C(5) C(4) C(17) 117.4(2) ? ? ? yes C(4) C(5) C(6) 121.6(2) ? ? ? yes C(5) C(6) C(7) 117.0(2) ? ? ? yes C(5) C(6) C(9) 120.4(3) ? ? ? yes C(7) C(6) C(9) 121.3(2) ? ? ? yes C(6) C(7) C(8) 120.6(2) ? ? ? yes C(3) C(8) C(7) 121.2(2) ? ? ? yes C(6) C(9) C(10) 113.4(2) ? ? ? yes C(9) C(10) C(11) 113.6(3) ? ? ? yes C(10) C(11) C(12) 121.1(3) ? ? ? yes C(10) C(11) C(16) 121.2(3) ? ? ? yes C(12) C(11) C(16) 116.7(3) ? ? ? yes C(11) C(12) C(13) 120.7(3) ? ? ? yes C(12) C(13) C(14) 120.7(3) ? ? ? yes C(1) C(14) C(13) 121.6(2) ? ? ? yes C(1) C(14) C(15) 119.9(2) ? ? ? yes C(13) C(14) C(15) 117.2(3) ? ? ? yes C(14) C(15) C(16) 120.2(3) ? ? ? yes C(11) C(16) C(15) 121.0(3) ? ? ? yes O C(17) N 117.9(2) ? ? ? yes O C(17) C(4) 114.3(2) ? ? ? yes N C(17) C(4) 127.8(2) ? ? ? yes O C(18) C(19) 104.6(2) ? ? ? yes N C(19) C(18) 103.1(2) ? ? ? yes N C(19) C(20) 110.6(2) ? ? ? yes C(18) C(19) C(20) 115.7(2) ? ? ? yes C(19) C(20) C(21) 110.9(3) ? ? ? yes C(19) C(20) C(22) 112.2(2) ? ? ? yes C(21) C(20) C(22) 111.0(3) ? ? ? yes S C(23) C(24) 126.9(2) ? ? ? yes S C(23) C(28) 114.8(2) ? ? ? yes C(24) C(23) C(28) 118.2(3) ? ? ? yes C(23) C(24) C(25) 120.5(3) ? ? ? yes C(24) C(25) C(26) 120.6(3) ? ? ? yes C(25) C(26) C(27) 118.9(3) ? ? ? yes C(26) C(27) C(28) 121.1(3) ? ? ? yes C(23) C(28) C(27) 120.7(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;