# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 207/370 data_master_file_afc7*.xtl #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jul 15 14:54:23 1997' _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 8.614(2) _cell_length_b 17.667(5) _cell_length_c 8.446(3) _cell_angle_alpha 97.02(3) _cell_angle_beta 91.42(2) _cell_angle_gamma 79.31(2) _cell_volume 1253.7(7) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 18.36 _cell_measurement_theta_max 21.70 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -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 1.627 _exptl_crystal_density_measured ? _exptl_crystal_F000 624.00 _exptl_absorpt_coefficient_mu_cm 32.952 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.651 #------------------------------------------------------------------------------ _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_\% -5.48 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3942 _diffrn_reflns_av_R_equivalents 3.97 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 9 _diffrn_reflns_k_min -19 _diffrn_reflns_k_max 21 _diffrn_reflns_l_min -1 _diffrn_reflns_l_max 10 _diffrn_theta_min ? _diffrn_theta_max 24.9932 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 0.08653 _diffrn_orient_matrix_12 0.03065 _diffrn_orient_matrix_13 0.02106 _diffrn_orient_matrix_21 0.08015 _diffrn_orient_matrix_22 -0.04912 _diffrn_orient_matrix_23 -0.01268 _diffrn_orient_matrix_31 0.00664 _diffrn_orient_matrix_32 0.00377 _diffrn_orient_matrix_33 -0.11673 #------------------------------------------------------------------------------ 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 44 0.003 0.002 'International Tables' H 0 60 0.000 0.000 'International Tables' O 0 20 0.011 0.006 'International Tables' Br 0 4 -0.290 2.459 '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 Br1 0.3358(1) 0.09472(4) 0.25215(7) 0.0878(3) Uij ? ? Br2 0.24089(8) 0.34464(5) 0.3649(1) 0.1024(3) Uij ? ? O1 0.1261(5) -0.0190(2) 0.6383(5) 0.069(1) Uij ? ? O2 0.1887(5) 0.0231(2) 0.8845(4) 0.063(1) Uij ? ? O3 0.5855(5) 0.1043(3) 0.5380(7) 0.070(2) Uij ? ? O4 0.3581(5) 0.2681(2) 0.8448(5) 0.057(1) Uij ? ? O5 0.0980(5) 0.2953(2) 0.8134(4) 0.058(1) Uij ? ? O6 -0.3899(5) 0.4917(2) 0.2155(6) 0.079(2) Uij ? ? O7 -0.1845(4) 0.4561(2) 0.0531(4) 0.049(1) Uij ? ? O8 -0.3294(5) 0.2972(2) 0.5943(5) 0.070(1) Uij ? ? O9 -0.3363(5) 0.2258(3) 0.3621(6) 0.072(2) Uij ? ? O10 0.0035(7) 0.4246(3) 0.6437(6) 0.089(2) Uij ? ? C1 0.2358(6) 0.1591(3) 0.8068(6) 0.036(1) Uij ? ? C2 0.1177(5) 0.1191(3) 0.7087(6) 0.038(1) Uij ? ? C3 0.1447(7) 0.1236(3) 0.5309(6) 0.043(2) Uij ? ? C4 0.3128(7) 0.0917(3) 0.4821(6) 0.044(2) Uij ? ? C5 0.4258(6) 0.1366(3) 0.5726(6) 0.041(1) Uij ? ? C6 0.4074(6) 0.1358(3) 0.7519(6) 0.040(1) Uij ? ? C7 0.4815(8) 0.1992(3) 0.8446(9) 0.057(2) Uij ? ? C8 0.2159(7) 0.2474(3) 0.8195(5) 0.044(1) Uij ? ? C9 -0.0548(7) 0.1522(4) 0.7532(10) 0.061(2) Uij ? ? C10 0.1444(5) 0.0330(3) 0.7372(6) 0.041(1) Uij ? ? C11 0.208(1) -0.0554(4) 0.924(1) 0.082(3) Uij ? ? C12 -0.3157(6) 0.3645(3) 0.3756(6) 0.042(1) Uij ? ? C13 -0.2378(6) 0.3626(3) 0.2145(5) 0.035(1) Uij ? ? C14 -0.0583(6) 0.3359(3) 0.2276(6) 0.040(1) Uij ? ? C15 0.0113(6) 0.3836(3) 0.3604(7) 0.046(2) Uij ? ? C16 -0.0587(7) 0.3782(3) 0.5181(6) 0.050(2) Uij ? ? C17 -0.2365(7) 0.4046(3) 0.5169(6) 0.050(2) Uij ? ? C18 -0.310(1) 0.3765(4) 0.6558(8) 0.082(2) Uij ? ? C19 -0.3277(6) 0.2875(4) 0.4349(7) 0.051(2) Uij ? ? C20 -0.305(1) 0.3106(4) 0.0799(8) 0.065(2) Uij ? ? C21 -0.2793(6) 0.4442(3) 0.1655(6) 0.040(1) Uij ? ? C22 -0.2236(10) 0.5299(4) -0.0109(9) 0.060(2) Uij ? ? H1 0.229(6) 0.149(3) 0.912(7) 0.05(1) Uij ? ? H2 0.090(6) 0.099(3) 0.480(6) 0.03(1) Uij ? ? H3 0.114(6) 0.179(3) 0.515(6) 0.04(1) Uij ? ? H4 0.334(6) 0.039(3) 0.501(5) 0.04(1) Uij ? ? H5 0.398(5) 0.187(3) 0.551(5) 0.03(1) Uij ? ? H6 0.454(6) 0.086(3) 0.782(5) 0.04(1) Uij ? ? H7 0.508(7) 0.192(3) 0.943(7) 0.06(2) Uij ? ? H8 0.563(9) 0.212(4) 0.796(8) 0.09(2) Uij ? ? H9 -0.089(7) 0.199(4) 0.710(7) 0.06(2) Uij ? ? H10 -0.12(1) 0.118(5) 0.71(1) 0.13(2) Uij ? ? H11 -0.061(6) 0.154(3) 0.874(7) 0.05(1) Uij ? ? H12 0.259(9) -0.091(5) 0.849(9) 0.10(2) Uij ? ? H13 0.09(1) -0.075(6) 0.89(1) 0.14(2) Uij ? ? H14 0.234(9) -0.049(4) 1.028(10) 0.10(2) Uij ? ? H15 0.611(9) 0.126(4) 0.482(9) 0.08(2) Uij ? ? H16 -0.418(7) 0.386(3) 0.362(6) 0.05(2) Uij ? ? H17 -0.038(5) 0.283(3) 0.244(5) 0.04(1) Uij ? ? H18 -0.015(6) 0.338(3) 0.122(7) 0.05(1) Uij ? ? H19 -0.002(6) 0.436(3) 0.344(6) 0.05(1) Uij ? ? H20 -0.037(5) 0.325(3) 0.539(5) 0.03(1) Uij ? ? H21 -0.256(6) 0.453(3) 0.516(6) 0.05(1) Uij ? ? H22 -0.416(9) 0.403(4) 0.672(8) 0.08(2) Uij ? ? H23 -0.249(10) 0.378(5) 0.76(1) 0.12(2) Uij ? ? H24 -0.291(6) 0.266(4) 0.103(6) 0.05(2) Uij ? ? H25 -0.415(9) 0.335(4) 0.075(8) 0.09(2) Uij ? ? H26 -0.254(9) 0.317(5) -0.02(1) 0.11(2) Uij ? ? H27 -0.239(9) 0.564(5) 0.075(10) 0.10(2) Uij ? ? H28 -0.144(9) 0.526(4) -0.082(9) 0.10(2) Uij ? ? H29 -0.315(9) 0.532(4) -0.063(9) 0.09(2) Uij ? ? H30 0.045(8) 0.400(4) 0.700(8) 0.07(2) 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 Br1 0.1445(8) 0.0753(5) 0.0463(4) -0.0294(5) 0.0189(4) 0.0000(3) Br2 0.0375(4) 0.1010(7) 0.1847(10) -0.0177(4) -0.0257(4) 0.0774(6) O1 0.092(3) 0.039(2) 0.083(3) -0.032(2) -0.029(2) 0.009(2) O2 0.104(3) 0.034(2) 0.054(2) -0.017(2) -0.004(2) 0.014(2) O3 0.048(3) 0.045(2) 0.120(4) -0.010(2) 0.027(2) 0.017(3) O4 0.077(3) 0.029(2) 0.067(2) -0.020(2) -0.017(2) -0.002(2) O5 0.078(3) 0.030(2) 0.061(2) 0.006(2) -0.005(2) 0.005(2) O6 0.075(3) 0.058(3) 0.098(3) 0.025(2) 0.029(3) 0.036(2) O7 0.054(2) 0.037(2) 0.057(2) -0.005(2) 0.008(2) 0.015(2) O8 0.080(3) 0.054(3) 0.078(3) 0.000(2) 0.033(2) 0.027(2) O9 0.082(3) 0.051(3) 0.096(3) -0.033(2) 0.006(2) 0.019(2) O10 0.155(5) 0.038(2) 0.075(3) -0.026(3) -0.067(3) 0.011(2) C1 0.047(3) 0.024(2) 0.037(3) -0.004(2) -0.002(2) 0.006(2) C2 0.036(3) 0.032(3) 0.048(3) -0.009(2) -0.003(2) 0.008(2) C3 0.051(3) 0.035(3) 0.047(3) -0.020(3) -0.016(3) 0.006(2) C4 0.064(4) 0.029(3) 0.043(3) -0.014(3) 0.005(2) 0.003(2) C5 0.042(3) 0.023(3) 0.059(3) -0.007(2) 0.006(2) 0.007(2) C6 0.037(3) 0.025(3) 0.060(3) -0.012(2) -0.008(2) 0.012(2) C7 0.065(4) 0.044(3) 0.065(4) -0.019(3) -0.020(3) 0.006(3) C8 0.068(4) 0.027(3) 0.036(3) -0.010(3) -0.007(2) 0.002(2) C9 0.044(3) 0.053(4) 0.089(5) -0.002(3) 0.003(3) 0.026(4) C10 0.031(3) 0.040(3) 0.057(3) -0.013(2) -0.004(2) 0.013(3) C11 0.134(7) 0.039(4) 0.077(5) -0.016(4) 0.001(5) 0.026(4) C12 0.031(3) 0.035(3) 0.060(3) -0.002(2) 0.004(2) 0.014(2) C13 0.041(3) 0.027(2) 0.038(2) -0.011(2) -0.003(2) 0.000(2) C14 0.039(3) 0.029(3) 0.050(3) 0.000(2) 0.007(2) 0.007(2) C15 0.038(3) 0.031(3) 0.074(4) -0.013(2) -0.017(3) 0.021(3) C16 0.075(4) 0.022(3) 0.054(3) -0.011(3) -0.029(3) 0.007(2) C17 0.076(4) 0.023(3) 0.045(3) 0.005(3) 0.009(3) 0.006(2) C18 0.121(7) 0.061(4) 0.052(4) 0.020(4) 0.033(4) 0.013(3) C19 0.036(3) 0.051(4) 0.071(4) -0.007(3) 0.015(3) 0.018(3) C20 0.095(6) 0.042(4) 0.063(4) -0.030(4) -0.024(4) 0.005(3) C21 0.041(3) 0.037(3) 0.043(3) -0.007(3) -0.008(2) 0.004(2) C22 0.074(5) 0.047(4) 0.062(4) -0.009(3) -0.001(4) 0.025(3) #------------------------------------------------------------------------------ _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 27.62231 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2980 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0510 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0720 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.600 _refine_ls_shift/esd_max 0.0220 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.22850 _refine_diff_density_max -1.13370 #------------------------------------------------------------------------------ _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 Br(1) C(4) 1.965(5) ? ? yes Br(2) C(15) 1.971(5) ? ? yes O(1) C(10) 1.195(6) ? ? yes O(2) C(10) 1.314(6) ? ? yes O(2) C(11) 1.445(7) ? ? yes O(3) C(5) 1.411(6) ? ? yes O(4) C(7) 1.460(7) ? ? yes O(4) C(8) 1.346(7) ? ? yes O(5) C(8) 1.200(6) ? ? yes O(6) C(21) 1.194(6) ? ? yes O(7) C(21) 1.329(6) ? ? yes O(7) C(22) 1.452(7) ? ? yes O(8) C(18) 1.471(9) ? ? yes O(8) C(19) 1.337(7) ? ? yes O(9) C(19) 1.199(7) ? ? yes O(10) C(16) 1.416(7) ? ? yes C(1) C(2) 1.517(7) ? ? yes C(1) C(6) 1.527(7) ? ? yes C(1) C(8) 1.529(7) ? ? yes C(2) C(3) 1.539(7) ? ? yes C(2) C(9) 1.531(8) ? ? yes C(2) C(10) 1.542(7) ? ? yes C(3) C(4) 1.502(8) ? ? yes C(4) C(5) 1.504(7) ? ? yes C(5) C(6) 1.529(7) ? ? yes C(6) C(7) 1.516(7) ? ? yes C(12) C(13) 1.526(7) ? ? yes C(12) C(17) 1.525(8) ? ? yes C(12) C(19) 1.526(7) ? ? yes C(13) C(14) 1.536(7) ? ? yes C(13) C(20) 1.544(7) ? ? yes C(13) C(21) 1.525(7) ? ? yes C(14) C(15) 1.501(7) ? ? yes C(15) C(16) 1.496(8) ? ? yes C(16) C(17) 1.516(8) ? ? yes C(17) C(18) 1.522(9) ? ? 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(10) O(2) C(11) 115.9(5) ? ? ? yes C(7) O(4) C(8) 110.2(4) ? ? ? yes C(21) O(7) C(22) 116.6(5) ? ? ? yes C(18) O(8) C(19) 110.6(4) ? ? ? yes C(2) C(1) C(6) 115.8(4) ? ? ? yes C(2) C(1) C(8) 119.0(4) ? ? ? yes C(6) C(1) C(8) 100.2(4) ? ? ? yes C(1) C(2) C(3) 108.8(4) ? ? ? yes C(1) C(2) C(9) 113.9(5) ? ? ? yes C(1) C(2) C(10) 109.4(4) ? ? ? yes C(3) C(2) C(9) 110.2(5) ? ? ? yes C(3) C(2) C(10) 108.8(4) ? ? ? yes C(9) C(2) C(10) 105.7(4) ? ? ? yes C(2) C(3) C(4) 112.0(4) ? ? ? yes Br(1) C(4) C(3) 109.7(4) ? ? ? yes Br(1) C(4) C(5) 109.5(3) ? ? ? yes C(3) C(4) C(5) 111.7(4) ? ? ? yes O(3) C(5) C(4) 112.9(4) ? ? ? yes O(3) C(5) C(6) 105.8(4) ? ? ? yes C(4) C(5) C(6) 110.0(4) ? ? ? yes C(1) C(6) C(5) 112.8(4) ? ? ? yes C(1) C(6) C(7) 101.5(4) ? ? ? yes C(5) C(6) C(7) 110.4(5) ? ? ? yes O(4) C(7) C(6) 103.4(4) ? ? ? yes O(4) C(8) O(5) 121.2(5) ? ? ? yes O(4) C(8) C(1) 109.2(4) ? ? ? yes O(5) C(8) C(1) 129.6(5) ? ? ? yes O(1) C(10) O(2) 123.4(5) ? ? ? yes O(1) C(10) C(2) 124.4(5) ? ? ? yes O(2) C(10) C(2) 112.2(4) ? ? ? yes C(13) C(12) C(17) 114.9(4) ? ? ? yes C(13) C(12) C(19) 118.5(4) ? ? ? yes C(17) C(12) C(19) 101.7(4) ? ? ? yes C(12) C(13) C(14) 110.1(4) ? ? ? yes C(12) C(13) C(20) 112.9(5) ? ? ? yes C(12) C(13) C(21) 107.2(4) ? ? ? yes C(14) C(13) C(20) 110.0(5) ? ? ? yes C(14) C(13) C(21) 111.6(4) ? ? ? yes C(20) C(13) C(21) 104.8(4) ? ? ? yes C(13) C(14) C(15) 111.7(4) ? ? ? yes Br(2) C(15) C(14) 108.0(4) ? ? ? yes Br(2) C(15) C(16) 109.5(4) ? ? ? yes C(14) C(15) C(16) 111.4(4) ? ? ? yes O(10) C(16) C(15) 111.8(5) ? ? ? yes O(10) C(16) C(17) 107.7(5) ? ? ? yes C(15) C(16) C(17) 111.1(4) ? ? ? yes C(12) C(17) C(16) 112.6(4) ? ? ? yes C(12) C(17) C(18) 100.9(5) ? ? ? yes C(16) C(17) C(18) 110.0(5) ? ? ? yes O(8) C(18) C(17) 103.9(5) ? ? ? yes O(8) C(19) O(9) 120.7(5) ? ? ? yes O(8) C(19) C(12) 108.9(5) ? ? ? yes O(9) C(19) C(12) 130.4(5) ? ? ? yes O(6) C(21) O(7) 122.7(5) ? ? ? yes O(6) C(21) C(13) 124.3(5) ? ? ? yes O(7) C(21) C(13) 112.8(4) ? ? ? 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 ;