# Copyright The Royal Society of Chemistry, 1998 data_Complex_5a #------------------------------------------------------------------------------ _audit_creation_date 'Tue Feb 24 11:10:54 1998' _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' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.89(1) _cell_length_b 14.11(2) _cell_length_c 12.358(4) _cell_angle_alpha 90.46(7) _cell_angle_beta 109.19(4) _cell_angle_gamma 68.0(1) _cell_volume 1951(3) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 43.1 _cell_measurement_theta_max 47.7 #------------------------------------------------------------------------------ _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 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 2.065 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 606.54 _chemical_formula_analytical ? _chemical_formula_sum 'C15 H20 Cl I N2 O2 W ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1136.00 _exptl_absorpt_coefficient_mu 7.654 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.344 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _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 scans with profile analysis' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_decay_% -0.93 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 7992 _reflns_number_total 7632 _reflns_number_observed 5541 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 3.79 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.06279 _diffrn_orient_matrix_UB_12 0.02133 _diffrn_orient_matrix_UB_13 -0.07891 _diffrn_orient_matrix_UB_21 -0.06357 _diffrn_orient_matrix_UB_22 0.01908 _diffrn_orient_matrix_UB_23 0.03520 _diffrn_orient_matrix_UB_31 -0.00222 _diffrn_orient_matrix_UB_32 0.07158 _diffrn_orient_matrix_UB_33 0.00191 #------------------------------------------------------------------------------ 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 W 0 4 -0.849 6.872 'International Tables' I 0 4 -0.474 1.812 'International Tables' Cl 0 4 0.148 0.159 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 8 0.006 0.003 'International Tables' C 0 60 0.003 0.002 'International Tables' H 0 80 0.000 0.000 '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 W(1) 0.18200(3) 0.48669(3) 0.29312(3) 0.0476 Uij ? ? W(2) 0.19248(3) -0.01970(3) 0.32617(3) 0.0498 Uij ? ? I(1) 0.41367(6) 0.66669(6) -0.17459(5) 0.0737 Uij ? ? I(2) 0.41508(7) 0.17635(6) 0.94797(5) 0.0829 Uij ? ? Cl(1) 0.1277(2) 0.3758(2) 0.4073(2) 0.0696 Uij ? ? Cl(2) 0.1213(3) -0.1247(2) 0.1738(2) 0.0759 Uij ? ? O(1) 0.4197(7) 0.2977(6) 0.3197(7) 0.0971 Uij ? ? O(2) 0.0672(8) 0.3959(6) 0.0774(6) 0.1066 Uij ? ? O(3) 0.4330(8) -0.2148(6) 0.4153(8) 0.1114 Uij ? ? O(4) 0.1051(9) -0.1167(6) 0.4858(7) 0.1201 Uij ? ? N(1) 0.0112(6) 0.6260(5) 0.2870(6) 0.0562 Uij ? ? N(2) 0.2491(7) 0.5507(6) 0.4633(6) 0.0606 Uij ? ? N(3) 0.0135(7) 0.1192(5) 0.2341(6) 0.0608 Uij ? ? N(4) 0.2391(7) 0.0560(6) 0.1948(6) 0.0661 Uij ? ? C(1) 0.3331(9) 0.3659(7) 0.3136(8) 0.0629 Uij ? ? C(2) 0.1089(9) 0.4303(7) 0.1590(8) 0.0672 Uij ? ? C(3) 0.2268(8) 0.5444(6) 0.1958(7) 0.0544 Uij ? ? C(4) 0.2677(7) 0.5723(6) 0.1082(7) 0.0511 Uij ? ? C(5) 0.2541(9) 0.5318(8) 0.0046(7) 0.0738 Uij ? ? C(6) 0.2962(9) 0.5580(8) -0.0762(7) 0.0688 Uij ? ? C(7) 0.3508(8) 0.6256(7) -0.0543(7) 0.0551 Uij ? ? C(8) 0.367(1) 0.6663(7) 0.0486(9) 0.0758 Uij ? ? C(9) 0.3253(9) 0.6407(7) 0.1299(8) 0.0681 Uij ? ? C(10) -0.0413(9) 0.6970(7) 0.1755(8) 0.0738 Uij ? ? C(11) -0.0871(9) 0.5985(9) 0.2962(9) 0.0837 Uij ? ? C(12) 0.046(1) 0.6851(8) 0.3814(9) 0.0867 Uij ? ? C(13) 0.139(1) 0.6188(8) 0.4856(8) 0.0818 Uij ? ? C(14) 0.318(1) 0.6105(10) 0.4519(9) 0.0959 Uij ? ? C(15) 0.323(1) 0.4704(8) 0.5653(8) 0.0882 Uij ? ? C(16) 0.345(1) -0.1423(8) 0.3830(8) 0.0738 Uij ? ? C(17) 0.135(1) -0.0811(8) 0.4236(8) 0.0756 Uij ? ? C(18) 0.2495(8) 0.0330(6) 0.4567(7) 0.0557 Uij ? ? C(19) 0.2918(8) 0.0616(7) 0.5706(7) 0.0578 Uij ? ? C(20) 0.292(1) 0.0137(8) 0.6684(8) 0.0806 Uij ? ? C(21) 0.328(1) 0.0446(9) 0.7757(8) 0.0816 Uij ? ? C(22) 0.3644(8) 0.1260(7) 0.7876(7) 0.0605 Uij ? ? C(23) 0.3666(8) 0.1736(7) 0.6932(8) 0.0636 Uij ? ? C(24) 0.3316(9) 0.1417(7) 0.5859(7) 0.0636 Uij ? ? C(25) -0.019(1) 0.1903(8) 0.318(1) 0.0953 Uij ? ? C(26) -0.089(1) 0.091(1) 0.180(1) 0.1252 Uij ? ? C(27) 0.032(1) 0.175(1) 0.148(1) 0.1408 Uij ? ? C(28) 0.130(1) 0.140(1) 0.125(1) 0.1699 Uij ? ? C(29) 0.332(1) 0.095(1) 0.252(1) 0.1076 Uij ? ? C(30) 0.285(1) -0.0144(10) 0.1156(9) 0.1023 Uij ? ? H(1) 0.2152 0.4851 -0.0118 0.0886 Uij ? ? H(2) 0.2868 0.5288 -0.1465 0.0826 Uij ? ? H(3) 0.4077 0.7119 0.0643 0.0909 Uij ? ? H(4) 0.3358 0.6698 0.2003 0.0817 Uij ? ? H(5) 0.0181 0.7166 0.1651 0.0886 Uij ? ? H(6) -0.0686 0.6624 0.1130 0.0886 Uij ? ? H(7) -0.1064 0.7566 0.1780 0.0886 Uij ? ? H(8) -0.1520 0.6594 0.2966 0.1005 Uij ? ? H(9) -0.1131 0.5650 0.2321 0.1005 Uij ? ? H(10) -0.0586 0.5536 0.3658 0.1005 Uij ? ? H(11) 0.0756 0.7298 0.3557 0.1040 Uij ? ? H(12) -0.0222 0.7248 0.3997 0.1040 Uij ? ? H(13) 0.1080 0.5766 0.5138 0.0981 Uij ? ? H(14) 0.1594 0.6608 0.5422 0.0981 Uij ? ? H(15) 0.3892 0.5660 0.4413 0.1151 Uij ? ? H(16) 0.2714 0.6625 0.3872 0.1151 Uij ? ? H(17) 0.3375 0.6417 0.5200 0.1151 Uij ? ? H(18) 0.2802 0.4307 0.5733 0.1058 Uij ? ? H(19) 0.3951 0.4266 0.5548 0.1058 Uij ? ? H(20) 0.3421 0.5024 0.6328 0.1058 Uij ? ? H(21) 0.2664 -0.0419 0.6612 0.0968 Uij ? ? H(22) 0.3286 0.0099 0.8414 0.0979 Uij ? ? H(23) 0.3923 0.2290 0.7012 0.0763 Uij ? ? H(24) 0.3347 0.1751 0.5213 0.0763 Uij ? ? H(25) 0.0439 0.2115 0.3554 0.1144 Uij ? ? H(26) -0.0899 0.2490 0.2783 0.1144 Uij ? ? H(27) -0.0333 0.1557 0.3741 0.1144 Uij ? ? H(28) -0.1581 0.1507 0.1419 0.1503 Uij ? ? H(29) -0.0724 0.0445 0.1259 0.1503 Uij ? ? H(30) -0.1024 0.0579 0.2382 0.1503 Uij ? ? H(31) -0.0303 0.1819 0.0767 0.1690 Uij ? ? H(32) 0.0236 0.2406 0.1709 0.1690 Uij ? ? H(33) 0.1514 0.1974 0.1225 0.2039 Uij ? ? H(34) 0.1095 0.1197 0.0501 0.2039 Uij ? ? H(35) 0.4038 0.0385 0.2946 0.1292 Uij ? ? H(36) 0.3443 0.1301 0.1963 0.1292 Uij ? ? H(37) 0.3063 0.1406 0.3040 0.1292 Uij ? ? H(38) 0.2275 -0.0416 0.0757 0.1227 Uij ? ? H(39) 0.2981 0.0227 0.0614 0.1227 Uij ? ? H(40) 0.3576 -0.0694 0.1592 0.1227 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 W(1) 0.0542(2) 0.0477(2) 0.0489(2) -0.0227(2) 0.0228(2) -0.0072(1) W(2) 0.0589(2) 0.0494(2) 0.0483(2) -0.0259(2) 0.0206(2) -0.0072(1) I(1) 0.0755(5) 0.1005(5) 0.0655(4) -0.0413(4) 0.0399(3) -0.0111(3) I(2) 0.0776(5) 0.1231(6) 0.0597(4) -0.0508(5) 0.0236(3) -0.0298(4) Cl(1) 0.086(2) 0.065(1) 0.073(1) -0.039(1) 0.032(1) 0.002(1) Cl(2) 0.095(2) 0.069(2) 0.074(1) -0.041(2) 0.032(1) -0.029(1) O(1) 0.084(6) 0.076(5) 0.118(6) 0.000(4) 0.051(5) 0.002(4) O(2) 0.168(9) 0.085(5) 0.060(4) -0.065(6) 0.011(5) -0.010(4) O(3) 0.088(6) 0.077(6) 0.138(7) -0.002(5) 0.029(5) 0.028(5) O(4) 0.20(1) 0.124(7) 0.122(7) -0.112(8) 0.104(7) -0.040(5) N(1) 0.053(5) 0.054(4) 0.064(4) -0.019(4) 0.024(4) -0.009(3) N(2) 0.069(5) 0.064(5) 0.056(4) -0.031(4) 0.022(4) -0.012(3) N(3) 0.058(5) 0.062(5) 0.062(4) -0.017(4) 0.026(4) -0.016(4) N(4) 0.076(6) 0.068(5) 0.070(5) -0.036(5) 0.034(4) -0.003(4) C(1) 0.068(7) 0.062(6) 0.064(5) -0.020(5) 0.034(5) -0.005(4) C(2) 0.082(7) 0.057(6) 0.064(6) -0.028(5) 0.024(5) 0.001(4) C(3) 0.054(5) 0.054(5) 0.067(5) -0.025(4) 0.028(4) -0.014(4) C(4) 0.048(5) 0.044(5) 0.063(5) -0.011(4) 0.027(4) -0.001(4) C(5) 0.089(8) 0.110(8) 0.053(5) -0.066(7) 0.029(5) -0.019(5) C(6) 0.086(7) 0.088(7) 0.055(5) -0.050(6) 0.032(5) -0.025(5) C(7) 0.052(5) 0.067(6) 0.050(5) -0.019(5) 0.027(4) -0.002(4) C(8) 0.107(9) 0.063(6) 0.091(7) -0.050(6) 0.055(7) -0.020(5) C(9) 0.090(8) 0.067(6) 0.080(6) -0.043(6) 0.055(6) -0.030(5) C(10) 0.067(7) 0.065(6) 0.082(7) -0.016(5) 0.024(5) 0.006(5) C(11) 0.066(7) 0.103(8) 0.096(8) -0.036(7) 0.037(6) 0.010(6) C(12) 0.099(9) 0.074(7) 0.084(7) -0.019(7) 0.043(7) -0.036(6) C(13) 0.098(9) 0.080(7) 0.065(6) -0.025(7) 0.035(6) -0.026(5) C(14) 0.12(1) 0.14(1) 0.078(7) -0.100(9) 0.029(7) -0.032(7) C(15) 0.100(9) 0.088(8) 0.063(6) -0.041(7) 0.004(6) -0.013(5) C(16) 0.084(8) 0.070(7) 0.072(6) -0.033(6) 0.027(6) 0.001(5) C(17) 0.108(9) 0.075(7) 0.073(6) -0.054(7) 0.045(6) -0.028(5) C(18) 0.061(6) 0.051(5) 0.060(5) -0.026(5) 0.021(4) -0.002(4) C(19) 0.058(6) 0.058(5) 0.054(5) -0.022(5) 0.015(4) -0.001(4) C(20) 0.120(10) 0.088(8) 0.056(6) -0.070(8) 0.022(6) -0.004(5) C(21) 0.109(9) 0.111(9) 0.047(5) -0.064(8) 0.029(6) -0.005(5) C(22) 0.062(6) 0.076(6) 0.049(5) -0.028(5) 0.025(4) -0.013(4) C(23) 0.067(6) 0.054(5) 0.077(6) -0.026(5) 0.028(5) -0.011(4) C(24) 0.071(7) 0.062(6) 0.056(5) -0.025(5) 0.019(5) -0.001(4) C(25) 0.109(10) 0.081(8) 0.110(9) -0.032(7) 0.060(8) -0.045(7) C(26) 0.049(7) 0.11(1) 0.19(1) -0.024(7) 0.009(8) -0.061(9) C(27) 0.12(1) 0.14(1) 0.12(1) 0.015(10) 0.062(10) 0.069(9) C(28) 0.12(1) 0.15(1) 0.20(2) 0.04(1) 0.10(1) 0.12(1) C(29) 0.14(1) 0.15(1) 0.098(8) -0.11(1) 0.058(8) -0.026(8) C(30) 0.14(1) 0.13(1) 0.088(8) -0.082(10) 0.074(8) -0.041(7) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.10288 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5541 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0351 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0406 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.733 _refine_ls_shift/esd_max 0.0120 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.81 _refine_diff_density_max 2.30 #------------------------------------------------------------------------------ _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 W(1) Cl(1) 2.536(2) ? ? yes W(1) N(1) 2.317(7) ? ? yes W(1) N(2) 2.312(7) ? ? yes W(1) C(1) 1.990(10) ? ? yes W(1) C(2) 1.94(1) ? ? yes W(1) C(3) 1.807(8) ? ? yes W(2) Cl(2) 2.534(2) ? ? yes W(2) N(3) 2.320(7) ? ? yes W(2) N(4) 2.300(7) ? ? yes W(2) C(16) 1.98(1) ? ? yes W(2) C(17) 1.958(10) ? ? yes W(2) C(18) 1.818(8) ? ? yes I(1) C(7) 2.088(7) ? ? yes I(2) C(22) 2.082(8) ? ? yes O(1) C(1) 1.15(1) ? ? yes O(2) C(2) 1.17(1) ? ? yes O(3) C(16) 1.16(1) ? ? yes O(4) C(17) 1.16(1) ? ? yes N(1) C(10) 1.50(1) ? ? yes N(1) C(11) 1.49(1) ? ? yes N(1) C(12) 1.48(1) ? ? yes N(2) C(13) 1.50(1) ? ? yes N(2) C(14) 1.47(1) ? ? yes N(2) C(15) 1.49(1) ? ? yes N(3) C(25) 1.49(1) ? ? yes N(3) C(26) 1.47(1) ? ? yes N(3) C(27) 1.46(1) ? ? yes N(4) C(28) 1.45(1) ? ? yes N(4) C(29) 1.47(1) ? ? yes N(4) C(30) 1.49(1) ? ? yes C(3) C(4) 1.46(1) ? ? yes C(4) C(5) 1.38(1) ? ? yes C(4) C(9) 1.40(1) ? ? yes C(5) C(6) 1.39(1) ? ? yes C(6) C(7) 1.36(1) ? ? yes C(7) C(8) 1.38(1) ? ? yes C(8) C(9) 1.39(1) ? ? yes C(12) C(13) 1.46(1) ? ? yes C(18) C(19) 1.45(1) ? ? yes C(19) C(20) 1.39(1) ? ? yes C(19) C(24) 1.39(1) ? ? yes C(20) C(21) 1.38(1) ? ? yes C(21) C(22) 1.38(1) ? ? yes C(22) C(23) 1.36(1) ? ? yes C(23) C(24) 1.38(1) ? ? yes C(27) C(28) 1.29(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_angle_publ_flag Cl(1) W(1) N(1) 88.9(2) ? ? ? yes Cl(1) W(1) N(2) 87.0(2) ? ? ? yes Cl(1) W(1) C(1) 88.3(3) ? ? ? yes Cl(1) W(1) C(2) 85.7(3) ? ? ? yes Cl(1) W(1) C(3) 168.7(3) ? ? ? yes N(1) W(1) N(2) 78.0(3) ? ? ? yes N(1) W(1) C(1) 174.9(3) ? ? ? yes N(1) W(1) C(2) 97.7(3) ? ? ? yes N(1) W(1) C(3) 99.1(3) ? ? ? yes N(2) W(1) C(1) 97.6(3) ? ? ? yes N(2) W(1) C(2) 171.6(3) ? ? ? yes N(2) W(1) C(3) 102.4(3) ? ? ? yes C(1) W(1) C(2) 86.4(4) ? ? ? yes C(1) W(1) C(3) 84.2(4) ? ? ? yes C(2) W(1) C(3) 85.3(4) ? ? ? yes Cl(2) W(2) N(3) 88.0(2) ? ? ? yes Cl(2) W(2) N(4) 89.0(2) ? ? ? yes Cl(2) W(2) C(16) 85.9(3) ? ? ? yes Cl(2) W(2) C(17) 86.4(3) ? ? ? yes Cl(2) W(2) C(18) 167.9(2) ? ? ? yes N(3) W(2) N(4) 78.1(3) ? ? ? yes N(3) W(2) C(16) 172.1(3) ? ? ? yes N(3) W(2) C(17) 96.9(4) ? ? ? yes N(3) W(2) C(18) 99.5(3) ? ? ? yes N(4) W(2) C(16) 96.7(3) ? ? ? yes N(4) W(2) C(17) 173.3(4) ? ? ? yes N(4) W(2) C(18) 101.8(3) ? ? ? yes C(16) W(2) C(17) 87.8(4) ? ? ? yes C(16) W(2) C(18) 87.3(4) ? ? ? yes C(17) W(2) C(18) 83.3(4) ? ? ? yes W(1) N(1) C(10) 111.0(5) ? ? ? yes W(1) N(1) C(11) 114.8(6) ? ? ? yes W(1) N(1) C(12) 107.7(6) ? ? ? yes C(10) N(1) C(11) 106.0(7) ? ? ? yes C(10) N(1) C(12) 107.2(7) ? ? ? yes C(11) N(1) C(12) 110.0(8) ? ? ? yes W(1) N(2) C(13) 105.6(6) ? ? ? yes W(1) N(2) C(14) 111.1(5) ? ? ? yes W(1) N(2) C(15) 114.0(5) ? ? ? yes C(13) N(2) C(14) 110.3(8) ? ? ? yes C(13) N(2) C(15) 107.2(7) ? ? ? yes C(14) N(2) C(15) 108.5(8) ? ? ? yes W(2) N(3) C(25) 110.5(6) ? ? ? yes W(2) N(3) C(26) 114.1(7) ? ? ? yes W(2) N(3) C(27) 107.1(7) ? ? ? yes C(25) N(3) C(26) 105.9(8) ? ? ? yes C(25) N(3) C(27) 108.5(10) ? ? ? yes C(26) N(3) C(27) 110(1) ? ? ? yes W(2) N(4) C(28) 107.0(6) ? ? ? yes W(2) N(4) C(29) 111.5(6) ? ? ? yes W(2) N(4) C(30) 114.0(6) ? ? ? yes C(28) N(4) C(29) 110(1) ? ? ? yes C(28) N(4) C(30) 107(1) ? ? ? yes C(29) N(4) C(30) 106.2(8) ? ? ? yes W(1) C(1) O(1) 176.5(8) ? ? ? yes W(1) C(2) O(2) 178.4(10) ? ? ? yes W(1) C(3) C(4) 169.1(6) ? ? ? yes C(3) C(4) C(5) 122.5(8) ? ? ? yes C(3) C(4) C(9) 119.4(8) ? ? ? yes C(5) C(4) C(9) 118.1(7) ? ? ? yes C(4) C(5) C(6) 121.3(8) ? ? ? yes C(5) C(6) C(7) 119.9(8) ? ? ? yes I(1) C(7) C(6) 120.6(6) ? ? ? yes I(1) C(7) C(8) 119.1(7) ? ? ? yes C(6) C(7) C(8) 120.3(7) ? ? ? yes C(7) C(8) C(9) 120.2(9) ? ? ? yes C(4) C(9) C(8) 120.2(8) ? ? ? yes N(1) C(12) C(13) 112.6(8) ? ? ? yes N(2) C(13) C(12) 112.1(8) ? ? ? yes W(2) C(16) O(3) 179(1) ? ? ? yes W(2) C(17) O(4) 176.7(10) ? ? ? yes W(2) C(18) C(19) 170.1(6) ? ? ? yes C(18) C(19) C(20) 122.5(8) ? ? ? yes C(18) C(19) C(24) 120.5(8) ? ? ? yes C(20) C(19) C(24) 117.0(8) ? ? ? yes C(19) C(20) C(21) 121.7(9) ? ? ? yes C(20) C(21) C(22) 120.0(8) ? ? ? yes I(2) C(22) C(21) 120.6(6) ? ? ? yes I(2) C(22) C(23) 119.9(7) ? ? ? yes C(21) C(22) C(23) 119.5(8) ? ? ? yes C(22) C(23) C(24) 120.5(9) ? ? ? yes C(19) C(24) C(23) 121.3(8) ? ? ? yes N(3) C(27) C(28) 122(1) ? ? ? yes N(4) C(28) C(27) 124(1) ? ? ? 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 OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #==END data_Complex_10 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Feb 24 11:13:19 1998' _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' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 38.685(4) _cell_length_b 8.229(2) _cell_length_c 17.227(2) _cell_angle_alpha 90 _cell_angle_beta 106.43(2) _cell_angle_gamma 90 _cell_volume 5260(1) _cell_formula_units_Z 8 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' +x, +y, +z' ' -x, +y,1/2-z' ' -x, +y,1/2-z' ' -x, -y, -z' ' -x, -y, -z' ' +x, -y,1/2+z' ' +x, -y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 651.24 _chemical_formula_analytical ? _chemical_formula_sum 'C24.50 H26 Cl2 N2 O3 W ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 2552.00 _exptl_absorpt_coefficient_mu 4.627 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.755 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _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 'unknown' _diffrn_measurement_method 'omega scans with profile analysis' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% -12.31 _diffrn_reflns_number 5057 _reflns_number_total 4987 _reflns_number_observed 2768 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.95 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00773 _diffrn_orient_matrix_UB_12 0.00669 _diffrn_orient_matrix_UB_13 0.06042 _diffrn_orient_matrix_UB_21 -0.02581 _diffrn_orient_matrix_UB_22 0.00027 _diffrn_orient_matrix_UB_23 0.00027 _diffrn_orient_matrix_UB_31 0.00035 _diffrn_orient_matrix_UB_32 -0.12134 _diffrn_orient_matrix_UB_33 0.00335 #------------------------------------------------------------------------------ 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 W 0 8 -0.849 6.872 'International Tables' Cl 0 16 0.148 0.159 'International Tables' O 0 24 0.011 0.006 'International Tables' N 0 16 0.006 0.003 'International Tables' C 0 196 0.003 0.002 'International Tables' H 0 208 0.000 0.000 '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 W(1) 0.156007(7) -0.00675(4) 0.28006(2) 0.0432 Uij ? ? Cl(1) 0.19262(6) 0.1440(3) 0.1981(1) 0.0731 Uij ? ? Cl(2) 0.0150(2) 0.1920(9) 0.1850(5) 0.3071 Uij ? ? O(1) 0.1167(2) 0.3172(7) 0.2994(4) 0.0849 Uij ? ? O(2) 0.0937(2) -0.0387(9) 0.1193(4) 0.1028 Uij ? ? O(3) -0.1741(2) -0.5067(9) 0.5197(4) 0.1077 Uij ? ? N(1) 0.1874(2) -0.2414(9) 0.2681(4) 0.0675 Uij ? ? N(2) 0.2053(2) 0.0125(10) 0.3913(4) 0.0696 Uij ? ? C(1) 0.1320(2) 0.2020(10) 0.2928(5) 0.0557 Uij ? ? C(2) 0.1172(2) -0.0290(10) 0.1772(5) 0.0619 Uij ? ? C(3) 0.1235(2) -0.0956(9) 0.3243(4) 0.0445 Uij ? ? C(4) 0.0930(2) -0.1555(8) 0.3495(4) 0.0440 Uij ? ? C(5) 0.0832(2) -0.088(1) 0.4137(5) 0.0587 Uij ? ? C(6) 0.0530(2) -0.143(1) 0.4350(5) 0.0652 Uij ? ? C(7) 0.0326(2) -0.2686(10) 0.3930(5) 0.0534 Uij ? ? C(8) 0.0433(2) -0.341(1) 0.3310(5) 0.0673 Uij ? ? C(9) 0.0723(2) -0.285(1) 0.3087(5) 0.0646 Uij ? ? C(10) 0.0006(2) -0.323(1) 0.4123(5) 0.0627 Uij ? ? C(11) -0.0254(2) -0.368(1) 0.4279(5) 0.0612 Uij ? ? C(12) -0.0586(2) -0.421(1) 0.4430(5) 0.0528 Uij ? ? C(13) -0.0715(2) -0.348(1) 0.5009(5) 0.0704 Uij ? ? C(14) -0.1035(2) -0.396(1) 0.5131(5) 0.0686 Uij ? ? C(15) -0.1231(2) -0.519(1) 0.4693(4) 0.0574 Uij ? ? C(16) -0.1097(2) -0.598(1) 0.4132(5) 0.0689 Uij ? ? C(17) -0.0779(2) -0.548(1) 0.3998(5) 0.0693 Uij ? ? C(18) -0.1582(2) -0.573(1) 0.4798(6) 0.0809 Uij ? ? C(19) 0.1656(3) -0.386(1) 0.2731(6) 0.0957 Uij ? ? C(20) 0.1979(3) -0.255(1) 0.1921(7) 0.1062 Uij ? ? C(21) 0.2206(3) -0.239(2) 0.3391(9) 0.1403 Uij ? ? C(22) 0.2282(4) -0.126(2) 0.386(1) 0.2203 Uij ? ? C(23) 0.2258(3) 0.166(2) 0.3977(7) 0.1206 Uij ? ? C(24) 0.1950(3) 0.000(2) 0.4671(6) 0.1287 Uij ? ? C(25) 0.0000 0.088(3) 0.2500 0.1968 Uij ? ? H(1) 0.0974 -0.0036 0.4440 0.0704 Uij ? ? H(2) 0.0464 -0.0925 0.4785 0.0785 Uij ? ? H(3) 0.0300 -0.4304 0.3031 0.0807 Uij ? ? H(4) 0.0786 -0.3361 0.2651 0.0773 Uij ? ? H(5) -0.0582 -0.2625 0.5327 0.0841 Uij ? ? H(6) -0.1121 -0.3425 0.5528 0.0823 Uij ? ? H(7) -0.1225 -0.6872 0.3835 0.0827 Uij ? ? H(8) -0.0693 -0.6017 0.3601 0.0834 Uij ? ? H(9) -0.1687 -0.6681 0.4520 0.0973 Uij ? ? H(10) 0.1582 -0.3811 0.3213 0.1150 Uij ? ? H(11) 0.1448 -0.3889 0.2276 0.1150 Uij ? ? H(12) 0.1795 -0.4813 0.2738 0.1150 Uij ? ? H(13) 0.2116 -0.3510 0.1933 0.1278 Uij ? ? H(14) 0.1769 -0.2591 0.1473 0.1278 Uij ? ? H(15) 0.2119 -0.1630 0.1867 0.1278 Uij ? ? H(16) 0.2188 -0.3316 0.3709 0.1680 Uij ? ? H(17) 0.2404 -0.2528 0.3173 0.1680 Uij ? ? H(18) 0.2491 -0.0781 0.3764 0.2649 Uij ? ? H(19) 0.2345 -0.1728 0.4383 0.2649 Uij ? ? H(20) 0.2464 0.1609 0.4434 0.1448 Uij ? ? H(21) 0.2332 0.1808 0.3501 0.1448 Uij ? ? H(22) 0.2109 0.2541 0.4037 0.1448 Uij ? ? H(23) 0.1806 0.0911 0.4718 0.1544 Uij ? ? H(24) 0.1817 -0.0969 0.4666 0.1544 Uij ? ? H(25) 0.2161 -0.0017 0.5117 0.1544 Uij ? ? H(26) 0.0191 0.0159 0.2791 0.2237 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 W(1) 0.0396(1) 0.0473(2) 0.0469(2) -0.0048(2) 0.0190(1) -0.0006(2) Cl(1) 0.058(1) 0.084(2) 0.086(2) -0.003(1) 0.036(1) 0.026(1) Cl(2) 0.239(7) 0.277(8) 0.43(1) -0.059(6) 0.131(7) 0.095(7) O(1) 0.111(5) 0.056(4) 0.098(5) 0.020(4) 0.046(4) -0.002(3) O(2) 0.096(5) 0.114(6) 0.071(4) -0.012(4) -0.021(4) -0.010(4) O(3) 0.076(4) 0.153(7) 0.115(5) -0.020(5) 0.060(4) -0.014(6) N(1) 0.053(4) 0.072(5) 0.089(5) 0.014(4) 0.040(4) 0.002(4) N(2) 0.057(4) 0.079(5) 0.067(4) -0.008(5) 0.007(3) -0.010(5) C(1) 0.064(5) 0.052(5) 0.060(5) -0.006(4) 0.031(4) 0.001(4) C(2) 0.066(5) 0.060(6) 0.062(5) -0.008(5) 0.023(4) -0.007(4) C(3) 0.044(4) 0.044(4) 0.045(4) 0.000(4) 0.013(3) -0.001(3) C(4) 0.039(4) 0.045(4) 0.052(4) -0.002(3) 0.018(3) 0.004(3) C(5) 0.055(5) 0.064(5) 0.062(5) -0.020(4) 0.024(4) -0.012(4) C(6) 0.058(5) 0.086(6) 0.063(5) -0.005(5) 0.035(4) -0.001(5) C(7) 0.044(4) 0.057(5) 0.058(5) -0.002(4) 0.014(4) 0.015(4) C(8) 0.057(5) 0.061(5) 0.085(6) -0.018(4) 0.022(5) -0.010(5) C(9) 0.054(5) 0.078(6) 0.070(5) -0.016(5) 0.031(4) -0.021(5) C(10) 0.047(5) 0.080(6) 0.064(5) -0.002(4) 0.021(4) 0.017(5) C(11) 0.045(5) 0.069(6) 0.071(5) 0.003(4) 0.019(4) 0.020(5) C(12) 0.037(4) 0.066(5) 0.057(5) 0.003(4) 0.015(4) 0.019(4) C(13) 0.056(5) 0.084(6) 0.070(6) -0.016(5) 0.017(5) -0.013(5) C(14) 0.063(5) 0.087(7) 0.068(5) -0.015(5) 0.039(5) -0.012(5) C(15) 0.047(4) 0.070(6) 0.058(4) -0.005(5) 0.019(3) 0.015(5) C(16) 0.055(5) 0.073(6) 0.088(6) -0.012(5) 0.036(5) -0.012(5) C(17) 0.064(5) 0.076(7) 0.084(6) -0.017(5) 0.046(5) -0.021(5) C(18) 0.070(6) 0.103(8) 0.083(7) -0.022(5) 0.044(6) -0.009(5) C(19) 0.117(9) 0.056(6) 0.133(9) 0.015(6) 0.066(8) 0.009(6) C(20) 0.116(9) 0.117(9) 0.110(8) 0.026(8) 0.072(7) -0.018(7) C(21) 0.081(8) 0.17(1) 0.15(1) 0.062(9) -0.007(8) -0.04(1) C(22) 0.14(1) 0.19(2) 0.22(2) 0.10(1) -0.12(1) -0.11(1) C(23) 0.108(10) 0.16(1) 0.091(8) -0.073(9) 0.022(7) -0.026(8) C(24) 0.126(9) 0.19(1) 0.055(5) -0.061(9) -0.001(6) 0.014(8) C(25) 0.31(3) 0.08(1) 0.19(2) 0.0000 0.06(2) 0.0000 #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2768 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0280 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0339 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.530 _refine_ls_shift/esd_max 1.6880 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.67 _refine_diff_density_max 0.65 #------------------------------------------------------------------------------ _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 ? ? ? ? ? ? # -- ENTER BONDS HERE, ONE PER LINE -- # e.g. C1 C2 1.541(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 # -- ENTER ANGLES HERE, ONE PER LINE -- # e.g. C1 C2 C3 109.4(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 OTHER REFERENCES Molecular Structure Corporation (1985, 1992). teXsan. Crystal Structure Analysis Package, The Woodlands, TX, USA 77381 ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;