# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 207/364 data_master_file_afc7*.xtl #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 6 09:33:32 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 SHELXS86 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 7.943(3) _cell_length_b 27.493(3) _cell_length_c 8.752(2) _cell_angle_alpha 90 _cell_angle_beta 103.73(3) _cell_angle_gamma 90 _cell_volume 1856(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 13.82 _cell_measurement_theta_max 24.29 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+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 1.221 _exptl_crystal_density_measured ? _exptl_crystal_F000 720.00 _exptl_absorpt_coefficient_mu_cm 1.632 #------------------------------------------------------------------------------ _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_\% 0.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3615 _diffrn_reflns_av_R_equivalents 4.00 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 9 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 32 _diffrn_reflns_l_min -10 _diffrn_reflns_l_max 10 _diffrn_theta_min 2.25 _diffrn_theta_max 24.9938 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.02700 _diffrn_orient_matrix_12 -0.00016 _diffrn_orient_matrix_13 -0.11756 _diffrn_orient_matrix_21 0.01389 _diffrn_orient_matrix_22 0.03615 _diffrn_orient_matrix_23 -0.00013 _diffrn_orient_matrix_31 0.12599 _diffrn_orient_matrix_32 -0.00402 _diffrn_orient_matrix_33 0.00352 #------------------------------------------------------------------------------ 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 80 0.000 0.000 'International Tables' O 0 12 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' P 0 4 0.102 0.094 '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 P 0.3209(2) 0.52219(8) 0.2499(3) 0.0597 Uij ? ? O1 0.2356(6) 0.5378(2) 0.0933(5) 0.0718 Uij ? ? O2 0.2765(7) 0.5526(2) 0.3869(6) 0.0865 Uij ? ? O3 0.5231(7) 0.5264(2) 0.3004(7) 0.0966 Uij ? ? N 0.237(1) 0.3534(3) 0.501(1) 0.1324 Uij ? ? C1 0.2681(8) 0.4622(2) 0.2969(8) 0.0536 Uij ? ? C2 0.1451(8) 0.4371(3) 0.2000(8) 0.0565 Uij ? ? C3 0.0807(10) 0.3894(3) 0.2319(9) 0.0585 Uij ? ? C4 0.165(1) 0.3676(3) 0.380(1) 0.0852 Uij ? ? C5 -0.0575(9) 0.3697(3) 0.1337(8) 0.0619 Uij ? ? C6 -0.146(1) 0.3232(3) 0.1544(9) 0.0678 Uij ? ? C7 -0.056(1) 0.2843(3) 0.231(1) 0.0978 Uij ? ? C8 -0.147(1) 0.2411(3) 0.256(1) 0.1292 Uij ? ? C9 -0.322(2) 0.2385(3) 0.203(1) 0.1077 Uij ? ? C10 -0.416(1) 0.2769(3) 0.120(1) 0.0824 Uij ? ? C11 -0.598(1) 0.2729(4) 0.063(1) 0.1118 Uij ? ? C12 -0.687(1) 0.3106(5) -0.016(2) 0.1442 Uij ? ? C13 -0.605(1) 0.3532(4) -0.038(1) 0.1230 Uij ? ? C14 -0.431(1) 0.3586(3) 0.016(1) 0.0810 Uij ? ? C15 -0.329(1) 0.3203(3) 0.0954(9) 0.0626 Uij ? ? C16 0.285(1) 0.6040(4) 0.387(1) 0.1186 Uij ? ? C17 0.287(2) 0.6230(4) 0.533(2) 0.1724 Uij ? ? C18 0.627(1) 0.5106(4) 0.206(1) 0.1077 Uij ? ? C19 0.814(1) 0.5230(4) 0.279(1) 0.1079 Uij ? ? H1 0.3348 0.4455 0.4063 0.1012 Uij ? ? H2 0.0499 0.4532 0.0894 0.1012 Uij ? ? H3 -0.1238 0.3903 0.0204 0.1012 Uij ? ? H4 0.0905 0.2776 0.2669 0.1012 Uij ? ? H5 -0.0812 0.2128 0.3118 0.1626 Uij ? ? H6 -0.3810 0.2083 0.2214 0.1300 Uij ? ? H7 -0.6567 0.2427 0.0797 0.1310 Uij ? ? H8 -0.8157 0.3076 -0.0581 0.1593 Uij ? ? H9 -0.6710 0.3806 -0.0995 0.1468 Uij ? ? H10 -0.3659 0.3926 -0.0270 0.1012 Uij ? ? H11 0.1836 0.6182 0.3089 0.1343 Uij ? ? H12 0.3845 0.6161 0.3528 0.1343 Uij ? ? H13 0.1815 0.6136 0.5639 0.1864 Uij ? ? H14 0.2894 0.6582 0.5350 0.1864 Uij ? ? H15 0.3824 0.6112 0.6083 0.1864 Uij ? ? H16 0.6000 0.5245 0.1032 0.1382 Uij ? ? H17 0.6223 0.4751 0.1912 0.1382 Uij ? ? H18 0.8242 0.5571 0.2954 0.1626 Uij ? ? H19 0.8912 0.5120 0.2210 0.1229 Uij ? ? H20 0.8464 0.5077 0.3837 0.1229 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 P 0.048(1) 0.058(1) 0.069(1) -0.003(1) 0.0061(10) -0.001(1) O1 0.082(3) 0.067(4) 0.058(3) -0.015(3) -0.001(3) 0.007(3) O2 0.123(5) 0.059(4) 0.077(4) -0.009(4) 0.021(3) -0.007(3) O3 0.069(4) 0.116(5) 0.102(5) -0.016(4) 0.015(3) -0.006(4) N 0.173(9) 0.079(6) 0.108(7) -0.024(6) -0.039(6) 0.020(5) C1 0.041(4) 0.046(5) 0.070(5) 0.003(4) 0.004(4) 0.002(4) C2 0.039(4) 0.059(5) 0.066(5) 0.002(4) 0.000(4) 0.002(4) C3 0.063(5) 0.054(5) 0.052(5) 0.000(4) 0.003(4) 0.005(4) C4 0.093(7) 0.067(6) 0.085(7) -0.017(5) 0.000(6) -0.005(6) C5 0.060(5) 0.058(5) 0.064(5) -0.002(4) 0.007(4) 0.002(4) C6 0.078(6) 0.059(6) 0.059(5) -0.004(5) 0.003(4) -0.005(4) C7 0.094(7) 0.061(6) 0.118(8) 0.004(6) -0.016(6) 0.018(6) C8 0.129(10) 0.060(7) 0.17(1) -0.013(6) -0.023(8) 0.037(7) C9 0.122(8) 0.062(7) 0.123(9) -0.025(6) -0.003(7) 0.005(6) C10 0.090(7) 0.062(6) 0.093(7) -0.022(6) 0.017(6) -0.018(5) C11 0.097(9) 0.085(9) 0.16(1) -0.038(7) 0.035(7) -0.015(7) C12 0.079(8) 0.102(10) 0.23(1) -0.033(7) 0.005(8) -0.011(10) C13 0.082(8) 0.090(8) 0.18(1) -0.003(6) -0.010(7) -0.003(7) C14 0.069(6) 0.066(6) 0.106(7) 0.000(5) 0.017(5) 0.003(5) C15 0.071(6) 0.054(6) 0.058(5) -0.014(5) 0.006(4) -0.011(4) C16 0.17(1) 0.077(8) 0.108(9) 0.008(7) 0.040(8) -0.020(6) C17 0.30(2) 0.094(9) 0.15(1) -0.013(10) 0.11(1) -0.048(8) C18 0.117(8) 0.140(9) 0.081(7) 0.018(7) 0.054(6) -0.040(6) C19 0.052(5) 0.165(10) 0.103(7) 0.008(6) 0.012(5) -0.010(7) #------------------------------------------------------------------------------ _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 1247 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0700 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0660 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.680 _refine_ls_shift/esd_max 0.0070 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.37730 _refine_diff_density_max -0.25560 #------------------------------------------------------------------------------ _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 P O(1) 1.442(5) ? ? yes P O(2) 1.570(6) ? ? yes P O(3) 1.566(5) ? ? yes P C(1) 1.774(7) ? ? yes O(2) C(16) 1.414(10) ? ? yes O(3) C(18) 1.367(9) ? ? yes N C(4) 1.148(10) ? ? yes C(1) C(2) 1.326(8) ? ? yes C(2) C(3) 1.460(9) ? ? yes C(3) C(4) 1.44(1) ? ? yes C(3) C(5) 1.337(9) ? ? yes C(5) C(6) 1.488(9) ? ? yes C(6) C(7) 1.370(9) ? ? yes C(6) C(15) 1.424(10) ? ? yes C(7) C(8) 1.43(1) ? ? yes C(8) C(9) 1.36(1) ? ? yes C(9) C(10) 1.39(1) ? ? yes C(10) C(11) 1.42(1) ? ? yes C(10) C(15) 1.423(10) ? ? yes C(11) C(12) 1.35(1) ? ? yes C(12) C(13) 1.38(1) ? ? yes C(13) C(14) 1.36(1) ? ? yes C(14) C(15) 1.405(10) ? ? yes C(16) C(17) 1.38(1) ? ? yes C(18) C(19) 1.51(1) ? ? 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 O(1) P O(2) 115.3(3) ? ? ? yes O(1) P O(3) 117.7(3) ? ? ? yes O(1) P C(1) 114.4(3) ? ? ? yes O(2) P O(3) 98.4(3) ? ? ? yes O(2) P C(1) 102.1(3) ? ? ? yes O(3) P C(1) 106.6(3) ? ? ? yes P O(2) C(16) 121.0(6) ? ? ? yes P O(3) C(18) 122.0(6) ? ? ? yes P C(1) C(2) 121.0(5) ? ? ? yes C(1) C(2) C(3) 125.8(7) ? ? ? yes C(2) C(3) C(4) 115.8(7) ? ? ? yes C(2) C(3) C(5) 120.8(7) ? ? ? yes C(4) C(3) C(5) 123.2(7) ? ? ? yes N C(4) C(3) 175.2(9) ? ? ? yes C(3) C(5) C(6) 127.4(7) ? ? ? yes C(5) C(6) C(7) 121.8(7) ? ? ? yes C(5) C(6) C(15) 118.2(7) ? ? ? yes C(7) C(6) C(15) 119.9(8) ? ? ? yes C(6) C(7) C(8) 120.0(8) ? ? ? yes C(7) C(8) C(9) 120.4(8) ? ? ? yes C(8) C(9) C(10) 120.9(9) ? ? ? yes C(9) C(10) C(11) 119.9(10) ? ? ? yes C(9) C(10) C(15) 119.9(8) ? ? ? yes C(11) C(10) C(15) 120.2(9) ? ? ? yes C(10) C(11) C(12) 119.2(10) ? ? ? yes C(11) C(12) C(13) 120(1) ? ? ? yes C(12) C(13) C(14) 121.6(10) ? ? ? yes C(13) C(14) C(15) 120.7(8) ? ? ? yes C(6) C(15) C(10) 118.9(8) ? ? ? yes C(6) C(15) C(14) 123.8(8) ? ? ? yes C(10) C(15) C(14) 117.3(8) ? ? ? yes O(2) C(16) C(17) 111.6(10) ? ? ? yes O(3) C(18) C(19) 110.3(7) ? ? ? 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 ;