# Copyright The Royal Society of Chemistry, 1998. data_afc379 #---------------------------------------------------------------- _audit_creation_date 'Mon Sep 8 16:30:28 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' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #---------------------------------------------------------------- _cell_length_a 11.756(4) _cell_length_b 12.972(5) _cell_length_c 14.510(4) _cell_angle_alpha 90 _cell_angle_beta 112.17(2) _cell_angle_gamma 90 _cell_volume 2049(1) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 13.5 _cell_measurement_theta_max 19.5 #---------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #---------------------------------------------------------------- _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 537.70 _chemical_formula_analytical ? _chemical_formula_sum 'C17 H24 Cl N3 O3 W ' _chemical_formula_moiety 'C17 H24 Cl N3 O3 W ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1048.00 _exptl_absorpt_coefficient_mu 5.793 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.533 #---------------------------------------------------------------- _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_% -0.31 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3548 _reflns_number_total 3368 _reflns_number_observed 2722 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.86 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.08898 _diffrn_orient_matrix_UB_12 0.00344 _diffrn_orient_matrix_UB_13 -0.01041 _diffrn_orient_matrix_UB_21 -0.02233 _diffrn_orient_matrix_UB_22 0.00139 _diffrn_orient_matrix_UB_23 -0.07367 _diffrn_orient_matrix_UB_31 -0.00458 _diffrn_orient_matrix_UB_32 -0.07700 _diffrn_orient_matrix_UB_33 -0.00180 #---------------------------------------------------------------- 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' Cl 0 4 0.148 0.159 'International Tables' O 0 12 0.011 0.006 'International Tables' N 0 12 0.006 0.003 'International Tables' C 0 68 0.003 0.002 'International Tables' H 0 96 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) 0.36353(3) 0.10977(2) 0.15556(2) 0.03827(9) Uij ? ? Cl(1) 0.1480(1) 0.0717(1) 0.1564(1) 0.0418(5) Uij ? ? O(1) 0.4135(7) -0.1261(4) 0.1571(5) 0.093(3) Uij ? ? O(2) 0.4812(6) 0.0890(5) 0.3875(4) 0.091(2) Uij ? ? O(3) 1.0681(5) 0.1420(4) 0.4976(4) 0.064(2) Uij ? ? N(1) 1.0448(6) 0.1271(5) 0.3370(4) 0.046(2) Uij ? ? N(2) 0.3164(6) 0.2835(4) 0.1399(4) 0.048(2) Uij ? ? N(3) 0.2726(6) 0.1277(4) -0.0140(4) 0.045(2) Uij ? ? C(1) 0.3914(7) -0.0401(7) 0.1556(5) 0.056(2) Uij ? ? C(2) 0.4316(7) 0.0986(6) 0.3025(6) 0.057(3) Uij ? ? C(3) 0.5242(7) 0.1201(5) 0.1771(5) 0.041(2) Uij ? ? C(4) 0.6589(6) 0.1197(5) 0.2157(5) 0.039(2) Uij ? ? C(5) 0.7240(6) 0.1870(5) 0.1792(5) 0.046(2) Uij ? ? C(6) 0.8491(6) 0.1890(5) 0.2192(5) 0.045(2) Uij ? ? C(7) 0.9141(6) 0.1229(5) 0.2970(5) 0.040(2) Uij ? ? C(8) 0.8515(6) 0.0537(5) 0.3328(5) 0.044(2) Uij ? ? C(9) 0.7252(7) 0.0524(5) 0.2924(5) 0.047(2) Uij ? ? C(10) 1.1128(7) 0.1376(5) 0.4341(5) 0.049(2) Uij ? ? C(11) 1.2492(7) 0.1466(7) 0.4585(6) 0.074(3) Uij ? ? C(12) 0.4264(9) 0.3463(6) 0.1982(7) 0.077(3) Uij ? ? C(13) 0.2162(9) 0.3180(7) 0.1709(7) 0.084(3) Uij ? ? C(14) 0.2849(9) 0.3098(6) 0.0335(6) 0.074(3) Uij ? ? C(15) 0.2098(8) 0.2296(6) -0.0342(5) 0.067(3) Uij ? ? C(16) 0.1799(8) 0.0489(7) -0.0646(5) 0.068(3) Uij ? ? C(17) 0.3647(8) 0.1234(6) -0.0601(6) 0.068(3) Uij ? ? H(1) 1.080(7) 0.123(5) 0.295(5) 0.06(2) Uij ? ? H(2) 0.6808 0.2321 0.1259 0.0548 Uij ? ? H(3) 0.8924 0.2358 0.1939 0.0540 Uij ? ? H(4) 0.8952 0.0075 0.3849 0.0525 Uij ? ? H(5) 0.6822 0.0048 0.3172 0.0563 Uij ? ? H(6) 1.2772 0.0860 0.4371 0.0862 Uij ? ? H(7) 1.2646 0.2049 0.4259 0.0862 Uij ? ? H(8) 1.2903 0.1540 0.5285 0.0862 Uij ? ? H(9) 0.4469 0.3350 0.2672 0.0925 Uij ? ? H(10) 0.4936 0.3267 0.1808 0.0925 Uij ? ? H(11) 0.4088 0.4173 0.1835 0.0925 Uij ? ? H(12) 0.2007 0.3893 0.1563 0.1011 Uij ? ? H(13) 0.1439 0.2796 0.1360 0.1011 Uij ? ? H(14) 0.2397 0.3074 0.2404 0.1011 Uij ? ? H(15) 0.2404 0.3728 0.0194 0.0882 Uij ? ? H(16) 0.3589 0.3181 0.0221 0.0882 Uij ? ? H(17) 0.1950 0.2492 -0.1008 0.0809 Uij ? ? H(18) 0.1340 0.2239 -0.0255 0.0809 Uij ? ? H(19) 0.1182 0.0486 -0.0371 0.0816 Uij ? ? H(20) 0.1436 0.0643 -0.1336 0.0816 Uij ? ? H(21) 0.2180 -0.0168 -0.0556 0.0816 Uij ? ? H(22) 0.4006 0.0566 -0.0507 0.0811 Uij ? ? H(23) 0.3262 0.1372 -0.1293 0.0811 Uij ? ? H(24) 0.4267 0.1733 -0.0301 0.0811 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) 0.0385(2) 0.0392(2) 0.0384(2) -0.0009(1) 0.0160(1) -0.0002(1) Cl(1) 0.0358(9) 0.0515(10) 0.0457(9) -0.0075(8) 0.0241(8) -0.0002(8) O(1) 0.115(6) 0.039(4) 0.147(7) 0.014(4) 0.076(5) 0.012(3) O(2) 0.075(4) 0.148(6) 0.042(3) 0.001(4) 0.014(3) 0.012(3) O(3) 0.059(4) 0.084(4) 0.048(3) 0.001(3) 0.019(3) -0.006(3) N(1) 0.041(4) 0.056(4) 0.044(4) 0.002(3) 0.019(3) -0.005(3) N(2) 0.056(4) 0.040(3) 0.049(3) 0.001(3) 0.021(3) -0.003(3) N(3) 0.057(4) 0.046(3) 0.036(3) -0.005(3) 0.020(3) -0.003(3) C(1) 0.054(5) 0.055(5) 0.063(5) -0.004(4) 0.029(4) 0.004(4) C(2) 0.054(5) 0.069(5) 0.057(5) -0.005(4) 0.031(4) 0.001(4) C(3) 0.050(4) 0.037(4) 0.041(4) -0.001(3) 0.022(3) 0.003(3) C(4) 0.038(4) 0.040(4) 0.037(3) -0.006(3) 0.014(3) -0.004(3) C(5) 0.043(4) 0.054(4) 0.038(3) -0.003(4) 0.013(3) 0.009(3) C(6) 0.047(4) 0.047(4) 0.044(4) -0.007(3) 0.022(3) 0.007(3) C(7) 0.040(4) 0.042(4) 0.040(4) 0.003(3) 0.017(3) -0.009(3) C(8) 0.043(4) 0.045(4) 0.047(4) 0.006(3) 0.022(3) 0.006(3) C(9) 0.049(5) 0.049(4) 0.048(4) 0.000(4) 0.023(3) 0.004(3) C(10) 0.052(5) 0.046(4) 0.047(4) 0.003(4) 0.018(4) -0.005(3) C(11) 0.043(5) 0.101(7) 0.067(5) 0.002(5) 0.010(4) -0.007(5) C(12) 0.080(7) 0.052(5) 0.092(6) -0.015(5) 0.024(5) -0.018(5) C(13) 0.092(7) 0.064(6) 0.123(8) 0.005(5) 0.069(6) -0.013(5) C(14) 0.098(7) 0.054(5) 0.068(5) 0.015(5) 0.029(5) 0.009(4) C(15) 0.082(6) 0.059(5) 0.053(4) 0.018(5) 0.015(4) 0.006(4) C(16) 0.066(6) 0.079(6) 0.050(4) -0.012(5) 0.012(4) -0.016(4) C(17) 0.075(6) 0.087(6) 0.048(4) -0.001(5) 0.031(4) -0.007(4) #---------------------------------------------------------------- _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 1.23838 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2722 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0288 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0363 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.130 _refine_ls_shift/esd_max 0.0430 _refine_ls_shift/esd_mean ? _refine_diff_density_min -1.29 _refine_diff_density_max 1.13 #---------------------------------------------------------------- _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) 2.585(2) ? ? yes W(1) N(2) 2.312(6) ? ? yes W(1) N(3) 2.295(5) ? ? yes W(1) C(1) 1.972(9) ? ? yes W(1) C(2) 1.980(8) ? ? yes W(1) C(3) 1.799(7) ? ? yes O(1) C(1) 1.143(9) ? ? yes O(2) C(2) 1.155(9) ? ? yes O(3) C(10) 1.222(8) ? ? yes N(1) C(7) 1.424(9) ? ? yes N(1) C(10) 1.340(9) ? ? yes N(2) C(12) 1.492(10) ? ? yes N(2) C(13) 1.480(10) ? ? yes N(2) C(14) 1.486(9) ? ? yes N(3) C(15) 1.488(9) ? ? yes N(3) C(16) 1.472(9) ? ? yes N(3) C(17) 1.474(10) ? ? yes C(3) C(4) 1.467(9) ? ? yes C(4) C(5) 1.390(9) ? ? yes C(4) C(9) 1.398(9) ? ? yes C(5) C(6) 1.363(9) ? ? yes C(6) C(7) 1.393(9) ? ? yes C(7) C(8) 1.380(9) ? ? yes C(8) C(9) 1.375(9) ? ? yes C(10) C(11) 1.51(1) ? ? yes C(14) C(15) 1.47(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 Cl(1) W(1) N(2) 89.3(2) ? ? ? yes Cl(1) W(1) N(3) 87.9(2) ? ? ? yes Cl(1) W(1) C(1) 88.5(2) ? ? ? yes Cl(1) W(1) C(2) 88.8(2) ? ? ? yes Cl(1) W(1) C(3) 168.4(2) ? ? ? yes N(2) W(1) N(3) 78.4(2) ? ? ? yes N(2) W(1) C(1) 174.3(2) ? ? ? yes N(2) W(1) C(2) 99.3(3) ? ? ? yes N(2) W(1) C(3) 98.1(2) ? ? ? yes N(3) W(1) C(1) 96.3(2) ? ? ? yes N(3) W(1) C(2) 176.0(3) ? ? ? yes N(3) W(1) C(3) 102.3(2) ? ? ? yes C(1) W(1) C(2) 85.9(3) ? ? ? yes C(1) W(1) C(3) 84.8(3) ? ? ? yes C(2) W(1) C(3) 81.2(3) ? ? ? yes C(7) N(1) C(10) 123.8(6) ? ? ? yes W(1) N(2) C(12) 110.6(5) ? ? ? yes W(1) N(2) C(13) 117.0(5) ? ? ? yes W(1) N(2) C(14) 106.4(4) ? ? ? yes C(12) N(2) C(13) 106.4(6) ? ? ? yes C(12) N(2) C(14) 106.6(6) ? ? ? yes C(13) N(2) C(14) 109.4(6) ? ? ? yes W(1) N(3) C(15) 107.2(4) ? ? ? yes W(1) N(3) C(16) 114.9(4) ? ? ? yes W(1) N(3) C(17) 111.0(5) ? ? ? yes C(15) N(3) C(16) 107.5(6) ? ? ? yes C(15) N(3) C(17) 109.9(6) ? ? ? yes C(16) N(3) C(17) 106.3(6) ? ? ? yes W(1) C(1) O(1) 176.7(7) ? ? ? yes W(1) C(2) O(2) 173.7(7) ? ? ? yes W(1) C(3) C(4) 167.7(5) ? ? ? yes C(3) C(4) C(5) 121.5(6) ? ? ? yes C(3) C(4) C(9) 120.2(6) ? ? ? yes C(5) C(4) C(9) 118.2(6) ? ? ? yes C(4) C(5) C(6) 120.7(6) ? ? ? yes C(5) C(6) C(7) 120.4(6) ? ? ? yes N(1) C(7) C(6) 118.9(6) ? ? ? yes N(1) C(7) C(8) 121.2(6) ? ? ? yes C(6) C(7) C(8) 119.8(6) ? ? ? yes C(7) C(8) C(9) 119.4(6) ? ? ? yes C(4) C(9) C(8) 121.3(6) ? ? ? yes O(3) C(10) N(1) 122.8(7) ? ? ? yes O(3) C(10) C(11) 122.7(7) ? ? ? yes N(1) C(10) C(11) 114.5(7) ? ? ? yes N(2) C(14) C(15) 112.4(7) ? ? ? yes N(3) C(15) C(14) 111.6(6) ? ? ? 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_Afc392 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 8 16:33:20 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' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.642(5) _cell_length_b 13.764(6) _cell_length_c 15.915(5) _cell_angle_alpha 90 _cell_angle_beta 95.71(3) _cell_angle_gamma 90 _cell_volume 2319(1) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 22 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 18.3 #------------------------------------------------------------------------------ _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 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 599.77 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H26 Cl N3 O3 W ' _chemical_formula_moiety 'C22 H26 Cl N3 O3 W ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1176.00 _exptl_absorpt_coefficient_mu 5.128 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.867 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 301.2 _diffrn_radiation_wavelength 0.6323 _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_% -2.02 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3436 _reflns_number_total 3237 _reflns_number_observed 2621 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.56 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 20.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.07108 _diffrn_orient_matrix_UB_12 0.03311 _diffrn_orient_matrix_UB_13 0.00349 _diffrn_orient_matrix_UB_21 0.04291 _diffrn_orient_matrix_UB_22 0.05547 _diffrn_orient_matrix_UB_23 -0.00003 _diffrn_orient_matrix_UB_31 -0.01282 _diffrn_orient_matrix_UB_32 0.00203 _diffrn_orient_matrix_UB_33 -0.05607 #------------------------------------------------------------------------------ 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' O 0 12 0.011 0.006 'International Tables' N 0 12 0.006 0.003 'International Tables' C 0 88 0.003 0.002 'International Tables' H 0 104 0.000 0.000 'International Tables' Cl 0 4 0.148 0.159 '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) 0.22925(3) 0.16332(3) 0.02704(2) 0.0380(1) Uij ? ? Cl(1) 0.2260(2) -0.0178(2) -0.0145(2) 0.0488(7) Uij ? ? O(1) 0.4364(9) 0.1178(8) 0.1760(6) 0.114(4) Uij ? ? O(2) 0.0374(8) 0.1285(6) 0.1605(5) 0.083(3) Uij ? ? O(3) 0.3362(7) 0.7301(5) 0.1828(5) 0.071(3) Uij ? ? N(1) 0.0888(7) 0.1980(6) -0.0877(5) 0.049(2) Uij ? ? N(2) 0.3650(7) 0.1900(6) -0.0756(5) 0.050(3) Uij ? ? N(3) 0.2270(8) 0.6327(5) 0.2624(5) 0.052(3) Uij ? ? C(1) 0.361(1) 0.1322(8) 0.1218(7) 0.065(4) Uij ? ? C(2) 0.107(1) 0.1379(7) 0.1107(7) 0.055(3) Uij ? ? C(3) 0.2320(9) 0.2834(7) 0.0736(5) 0.045(3) Uij ? ? C(4) 0.2297(9) 0.3742(6) 0.1192(5) 0.042(3) Uij ? ? C(5) 0.1168(8) 0.4131(6) 0.1431(5) 0.041(3) Uij ? ? C(6) 0.1167(9) 0.4985(7) 0.1887(6) 0.051(3) Uij ? ? C(7) 0.2290(9) 0.5484(6) 0.2112(5) 0.044(3) Uij ? ? C(8) 0.3400(9) 0.5117(7) 0.1867(6) 0.048(3) Uij ? ? C(9) 0.3431(9) 0.4267(7) 0.1419(6) 0.050(3) Uij ? ? C(10) 0.2837(8) 0.7179(7) 0.2471(6) 0.045(3) Uij ? ? C(11) 0.2765(9) 0.7968(7) 0.3104(6) 0.048(3) Uij ? ? C(12) 0.2833(10) 0.8913(7) 0.2815(7) 0.057(3) Uij ? ? C(13) 0.279(1) 0.9684(8) 0.3374(8) 0.074(4) Uij ? ? C(14) 0.266(1) 0.9509(9) 0.4226(8) 0.079(5) Uij ? ? C(15) 0.262(1) 0.8583(10) 0.4509(7) 0.076(4) Uij ? ? C(16) 0.268(1) 0.7791(8) 0.3963(6) 0.062(4) Uij ? ? C(17) -0.008(1) 0.272(1) -0.0658(8) 0.098(5) Uij ? ? C(18) 0.016(1) 0.1143(8) -0.1261(7) 0.068(4) Uij ? ? C(19) 0.164(1) 0.2429(10) -0.1500(7) 0.084(5) Uij ? ? C(20) 0.279(1) 0.195(1) -0.1592(7) 0.087(5) Uij ? ? C(21) 0.457(1) 0.1137(10) -0.0877(8) 0.093(5) Uij ? ? C(22) 0.430(1) 0.2828(8) -0.0608(7) 0.070(4) Uij ? ? H(1) 0.1672 0.6246 0.3104 0.0659 Uij ? ? H(2) 0.0392 0.3804 0.1275 0.0490 Uij ? ? H(3) 0.0395 0.5235 0.2050 0.0617 Uij ? ? H(4) 0.4164 0.5464 0.2010 0.0574 Uij ? ? H(5) 0.4214 0.4027 0.1265 0.0607 Uij ? ? H(6) 0.2906 0.9038 0.2238 0.0693 Uij ? ? H(7) 0.2840 1.0332 0.3176 0.0886 Uij ? ? H(8) 0.2602 1.0039 0.4603 0.0945 Uij ? ? H(9) 0.2558 0.8468 0.5094 0.0909 Uij ? ? H(10) 0.2660 0.7143 0.4170 0.0748 Uij ? ? H(11) 0.0344 0.3270 -0.0412 0.1182 Uij ? ? H(12) -0.0589 0.2899 -0.1154 0.1182 Uij ? ? H(13) -0.0591 0.2437 -0.0265 0.1182 Uij ? ? H(14) -0.0359 0.0885 -0.0863 0.0824 Uij ? ? H(15) -0.0350 0.1353 -0.1749 0.0824 Uij ? ? H(16) 0.0731 0.0657 -0.1411 0.0824 Uij ? ? H(17) 0.1147 0.2429 -0.2034 0.1000 Uij ? ? H(18) 0.1821 0.3080 -0.1332 0.1000 Uij ? ? H(19) 0.3216 0.2295 -0.1997 0.1041 Uij ? ? H(20) 0.2608 0.1311 -0.1789 0.1041 Uij ? ? H(21) 0.4140 0.0535 -0.0973 0.1103 Uij ? ? H(22) 0.5010 0.1290 -0.1349 0.1103 Uij ? ? H(23) 0.5150 0.1087 -0.0385 0.1103 Uij ? ? H(24) 0.4884 0.2782 -0.0119 0.0847 Uij ? ? H(25) 0.4738 0.2985 -0.1083 0.0847 Uij ? ? H(26) 0.3698 0.3322 -0.0529 0.0847 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) 0.0419(3) 0.0358(3) 0.0368(3) 0.0008(2) 0.0068(2) -0.0008(2) Cl(1) 0.055(1) 0.027(1) 0.067(2) -0.001(1) 0.019(1) -0.007(1) O(1) 0.105(8) 0.144(9) 0.082(6) 0.036(7) -0.048(6) 0.017(6) O(2) 0.089(6) 0.100(7) 0.067(5) -0.038(5) 0.041(5) -0.023(5) O(3) 0.098(6) 0.051(5) 0.069(5) -0.003(4) 0.035(5) 0.001(4) N(1) 0.051(5) 0.051(5) 0.045(5) 0.009(4) -0.001(4) -0.002(4) N(2) 0.053(5) 0.046(5) 0.054(5) -0.004(4) 0.021(4) -0.003(4) N(3) 0.065(6) 0.041(5) 0.054(5) -0.013(4) 0.023(4) -0.006(4) C(1) 0.070(8) 0.060(7) 0.065(8) -0.003(6) 0.009(6) 0.000(6) C(2) 0.064(7) 0.056(7) 0.049(6) -0.008(5) 0.020(6) -0.011(5) C(3) 0.051(6) 0.050(6) 0.037(5) -0.012(5) 0.013(4) 0.001(5) C(4) 0.051(6) 0.041(5) 0.035(5) -0.007(5) 0.010(4) -0.005(4) C(5) 0.036(5) 0.044(6) 0.042(5) -0.004(4) 0.004(4) -0.003(5) C(6) 0.060(6) 0.044(6) 0.052(6) -0.003(5) 0.019(5) -0.009(5) C(7) 0.056(6) 0.036(5) 0.040(5) -0.013(5) 0.011(5) -0.015(4) C(8) 0.050(6) 0.044(6) 0.049(6) -0.015(5) 0.007(5) -0.005(5) C(9) 0.050(6) 0.059(7) 0.043(6) -0.004(5) 0.010(5) -0.007(5) C(10) 0.039(6) 0.048(6) 0.047(6) -0.001(5) 0.001(5) -0.006(5) C(11) 0.051(6) 0.039(6) 0.056(6) -0.003(5) 0.011(5) -0.006(5) C(12) 0.064(7) 0.047(6) 0.061(7) 0.001(5) 0.007(5) 0.006(5) C(13) 0.097(10) 0.041(7) 0.082(9) 0.003(6) 0.002(7) -0.009(6) C(14) 0.094(10) 0.063(8) 0.078(9) -0.004(7) 0.004(7) -0.023(7) C(15) 0.086(9) 0.087(10) 0.056(7) -0.017(7) 0.017(6) -0.013(7) C(16) 0.081(8) 0.058(7) 0.048(6) -0.011(6) 0.010(6) -0.008(5) C(17) 0.10(1) 0.11(1) 0.080(9) 0.057(9) -0.017(8) 0.007(8) C(18) 0.059(7) 0.080(8) 0.061(7) -0.016(6) -0.021(6) -0.014(6) C(19) 0.10(1) 0.09(1) 0.048(7) -0.016(8) -0.015(7) 0.021(7) C(20) 0.11(1) 0.10(1) 0.052(7) -0.008(9) 0.041(8) 0.007(7) C(21) 0.091(10) 0.089(10) 0.11(1) 0.044(8) 0.059(8) 0.022(8) C(22) 0.062(7) 0.072(8) 0.082(8) -0.025(6) 0.030(6) -0.023(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 0.64601 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2621 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0313 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0463 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.496 _refine_ls_shift/esd_max 0.0070 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.47 _refine_diff_density_max 0.98 #------------------------------------------------------------------------------ _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) 2.579(2) ? ? yes W(1) N(1) 2.292(7) ? ? yes W(1) N(2) 2.315(7) ? ? yes W(1) C(1) 2.00(1) ? ? yes W(1) C(2) 1.98(1) ? ? yes W(1) C(3) 1.810(9) ? ? yes O(1) C(1) 1.13(1) ? ? yes O(2) C(2) 1.15(1) ? ? yes O(3) C(10) 1.23(1) ? ? yes N(1) C(17) 1.51(1) ? ? yes N(1) C(18) 1.49(1) ? ? yes N(1) C(19) 1.47(1) ? ? yes N(2) C(20) 1.54(2) ? ? yes N(2) C(21) 1.46(1) ? ? yes N(2) C(22) 1.46(1) ? ? yes N(3) C(7) 1.42(1) ? ? yes N(3) C(10) 1.35(1) ? ? yes C(3) C(4) 1.45(1) ? ? yes C(4) C(5) 1.40(1) ? ? yes C(4) C(9) 1.42(1) ? ? yes C(5) C(6) 1.38(1) ? ? yes C(6) C(7) 1.39(1) ? ? yes C(7) C(8) 1.38(1) ? ? yes C(8) C(9) 1.37(1) ? ? yes C(10) C(11) 1.49(1) ? ? yes C(11) C(12) 1.38(1) ? ? yes C(11) C(16) 1.40(1) ? ? yes C(12) C(13) 1.39(1) ? ? yes C(13) C(14) 1.40(2) ? ? yes C(14) C(15) 1.35(2) ? ? yes C(15) C(16) 1.40(1) ? ? yes C(19) C(20) 1.41(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) 90.3(2) ? ? ? yes Cl(1) W(1) N(2) 88.0(2) ? ? ? yes Cl(1) W(1) C(1) 88.7(3) ? ? ? yes Cl(1) W(1) C(2) 90.5(3) ? ? ? yes Cl(1) W(1) C(3) 170.7(3) ? ? ? yes N(1) W(1) N(2) 78.9(3) ? ? ? yes N(1) W(1) C(1) 176.1(4) ? ? ? yes N(1) W(1) C(2) 98.8(4) ? ? ? yes N(1) W(1) C(3) 96.8(3) ? ? ? yes N(2) W(1) C(1) 97.2(4) ? ? ? yes N(2) W(1) C(2) 177.3(3) ? ? ? yes N(2) W(1) C(3) 99.1(3) ? ? ? yes C(1) W(1) C(2) 85.0(5) ? ? ? yes C(1) W(1) C(3) 84.6(4) ? ? ? yes C(2) W(1) C(3) 82.6(4) ? ? ? yes W(1) N(1) C(17) 111.2(6) ? ? ? yes W(1) N(1) C(18) 116.0(6) ? ? ? yes W(1) N(1) C(19) 105.6(6) ? ? ? yes C(17) N(1) C(18) 106.1(9) ? ? ? yes C(17) N(1) C(19) 107.6(10) ? ? ? yes C(18) N(1) C(19) 110.1(8) ? ? ? yes W(1) N(2) C(20) 105.1(6) ? ? ? yes W(1) N(2) C(21) 116.9(7) ? ? ? yes W(1) N(2) C(22) 110.1(6) ? ? ? yes C(20) N(2) C(21) 105.4(9) ? ? ? yes C(20) N(2) C(22) 109.2(9) ? ? ? yes C(21) N(2) C(22) 109.8(9) ? ? ? yes C(7) N(3) C(10) 124.9(8) ? ? ? yes W(1) C(1) O(1) 177(1) ? ? ? yes W(1) C(2) O(2) 176.2(9) ? ? ? yes W(1) C(3) C(4) 173.5(7) ? ? ? yes C(3) C(4) C(5) 121.6(8) ? ? ? yes C(3) C(4) C(9) 120.7(8) ? ? ? yes C(5) C(4) C(9) 117.7(8) ? ? ? yes C(4) C(5) C(6) 120.8(8) ? ? ? yes C(5) C(6) C(7) 120.6(9) ? ? ? yes N(3) C(7) C(6) 119.3(8) ? ? ? yes N(3) C(7) C(8) 121.7(8) ? ? ? yes C(6) C(7) C(8) 118.9(8) ? ? ? yes C(7) C(8) C(9) 121.8(8) ? ? ? yes C(4) C(9) C(8) 120.1(9) ? ? ? yes O(3) C(10) N(3) 121.2(9) ? ? ? yes O(3) C(10) C(11) 121.5(9) ? ? ? yes N(3) C(10) C(11) 117.2(8) ? ? ? yes C(10) C(11) C(12) 116.9(9) ? ? ? yes C(10) C(11) C(16) 123.0(9) ? ? ? yes C(12) C(11) C(16) 120.0(9) ? ? ? yes C(11) C(12) C(13) 119.9(10) ? ? ? yes C(12) C(13) C(14) 120(1) ? ? ? yes C(13) C(14) C(15) 119(1) ? ? ? yes C(14) C(15) C(16) 121(1) ? ? ? yes C(11) C(16) C(15) 118(1) ? ? ? yes N(1) C(19) C(20) 114(1) ? ? ? yes N(2) C(20) C(19) 112.2(9) ? ? ? 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_AFC461 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 8 16:37:08 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' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 15.563(6) _cell_length_b 10.855(6) _cell_length_c 13.592(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2296(2) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 37.0 _cell_measurement_theta_max 47.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a ' _symmetry_Int_Tables_number 62 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y,1/2-z' ' -x,1/2+y, -z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y,1/2+z' ' +x,1/2-y, +z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 629.21 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H25 Br N4 O2 W ' _chemical_formula_moiety 'C21 H25 Br N4 O2 W ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1216.00 _exptl_absorpt_coefficient_mu 6.805 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.491 #------------------------------------------------------------------------------ _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_% 2.41 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2320 _reflns_number_total 2320 _reflns_number_observed 1525 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.02 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.00354 _diffrn_orient_matrix_UB_12 -0.07364 _diffrn_orient_matrix_UB_13 -0.04402 _diffrn_orient_matrix_UB_21 -0.00510 _diffrn_orient_matrix_UB_22 0.05534 _diffrn_orient_matrix_UB_23 -0.05853 _diffrn_orient_matrix_UB_31 0.06395 _diffrn_orient_matrix_UB_32 0.00033 _diffrn_orient_matrix_UB_33 -0.00710 #------------------------------------------------------------------------------ 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' Br 0 4 -0.290 2.459 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 16 0.006 0.003 'International Tables' C 0 84 0.003 0.002 'International Tables' H 0 100 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) 0.52311(3) 0.2500 0.33413(3) 0.0520(1) Uij ? ? Br(1) 0.49518(9) 0.2500 0.52991(9) 0.0877(5) Uij ? ? O(1) 0.6656(4) 0.0513(6) 0.3674(5) 0.103(2) Uij ? ? N(1) 0.4098(4) 0.3852(7) 0.3102(5) 0.079(2) Uij ? ? N(2) 0.7144(7) 0.2500 -0.1676(8) 0.113(5) Uij ? ? N(3) 0.8774(10) 0.2500 -0.4862(9) 0.128(6) Uij ? ? C(1) 0.6128(5) 0.1233(8) 0.3579(5) 0.066(2) Uij ? ? C(2) 0.4270(8) 0.468(1) 0.2288(9) 0.192(6) Uij ? ? C(3) 0.3844(7) 0.4603(9) 0.3978(8) 0.112(4) Uij ? ? C(4) 0.3357(6) 0.309(1) 0.2839(10) 0.177(6) Uij ? ? C(5) 0.5645(6) 0.2500 0.2105(7) 0.050(3) Uij ? ? C(6) 0.6073(6) 0.2500 0.1161(7) 0.051(3) Uij ? ? C(7) 0.6286(5) 0.3584(8) 0.0695(5) 0.067(3) Uij ? ? C(8) 0.6690(5) 0.3594(8) -0.0222(6) 0.079(3) Uij ? ? C(9) 0.6867(8) 0.2500 -0.0687(8) 0.078(4) Uij ? ? C(10) 0.7858(8) 0.2500 -0.1890(10) 0.085(5) Uij ? ? C(11) 0.8192(9) 0.2500 -0.2943(9) 0.082(4) Uij ? ? C(12) 0.7638(9) 0.2500 -0.3744(10) 0.091(5) Uij ? ? C(13) 0.7969(9) 0.2500 -0.4666(10) 0.102(6) Uij ? ? C(14) 0.9320(9) 0.2500 -0.409(1) 0.116(6) Uij ? ? C(15) 0.9090(8) 0.2500 -0.3147(9) 0.098(5) Uij ? ? H(1) 0.4750 0.5177 0.2436 0.2296 Uij ? ? H(2) 0.4386 0.4204 0.1712 0.2296 Uij ? ? H(3) 0.3780 0.5180 0.2173 0.2296 Uij ? ? H(4) 0.4313 0.5107 0.4171 0.1355 Uij ? ? H(5) 0.3366 0.5102 0.3816 0.1355 Uij ? ? H(6) 0.3697 0.4065 0.4505 0.1355 Uij ? ? H(7) 0.2910 0.3325 0.3271 0.2133 Uij ? ? H(8) 0.3210 0.3325 0.2183 0.2133 Uij ? ? H(9) 0.6156 0.4349 0.1004 0.0801 Uij ? ? H(10) 0.6841 0.4349 -0.0526 0.0954 Uij ? ? H(11) 0.8290 0.2500 -0.1348 0.1011 Uij ? ? H(12) 0.7042 0.2500 -0.3645 0.1082 Uij ? ? H(13) 0.7581 0.2500 -0.5203 0.1229 Uij ? ? H(14) 0.9920 0.2500 -0.4226 0.1393 Uij ? ? H(15) 0.9508 0.2500 -0.2633 0.1178 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) 0.0436(2) 0.0765(3) 0.0359(2) 0.0000 0.0014(2) 0.0000 Br(1) 0.0908(9) 0.128(1) 0.0441(7) 0.0000 0.0072(7) 0.0000 O(1) 0.086(4) 0.111(5) 0.112(5) 0.039(4) 0.014(4) 0.030(4) N(1) 0.062(4) 0.111(5) 0.063(4) 0.026(4) -0.003(4) 0.003(4) N(2) 0.084(8) 0.19(1) 0.061(7) 0.0000 0.029(7) 0.0000 N(3) 0.12(1) 0.19(1) 0.074(9) 0.0000 0.027(9) 0.0000 C(1) 0.061(5) 0.092(6) 0.046(4) 0.000(5) 0.009(4) 0.010(4) C(2) 0.17(1) 0.27(2) 0.14(1) 0.14(1) 0.077(10) 0.13(1) C(3) 0.108(8) 0.117(8) 0.111(8) 0.039(7) -0.015(7) -0.032(7) C(4) 0.076(6) 0.21(2) 0.24(1) 0.065(8) -0.083(8) -0.11(1) C(5) 0.041(5) 0.069(6) 0.041(5) 0.0000 -0.001(5) 0.0000 C(6) 0.043(6) 0.073(7) 0.039(6) 0.0000 -0.002(5) 0.0000 C(7) 0.064(5) 0.091(6) 0.046(4) 0.002(4) 0.001(4) -0.004(4) C(8) 0.080(6) 0.105(7) 0.053(5) -0.019(5) 0.008(5) 0.012(5) C(9) 0.066(8) 0.13(1) 0.036(7) 0.0000 0.015(6) 0.0000 C(10) 0.065(8) 0.12(1) 0.07(1) 0.0000 -0.006(8) 0.0000 C(11) 0.088(10) 0.108(10) 0.051(7) 0.0000 0.007(7) 0.0000 C(12) 0.087(10) 0.12(1) 0.060(8) 0.0000 0.003(8) 0.0000 C(13) 0.09(1) 0.17(1) 0.047(8) 0.0000 0.007(8) 0.0000 C(14) 0.065(9) 0.21(2) 0.072(10) 0.0000 0.020(9) 0.0000 C(15) 0.069(8) 0.18(1) 0.049(8) 0.0000 0.024(7) 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 Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 3.22553 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1525 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0295 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0342 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.671 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.61 _refine_diff_density_max 0.79 #------------------------------------------------------------------------------ _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) Br(1) 2.696(1) ? ? yes W(1) N(1) 2.318(6) ? ? yes W(1) N(1) 2.318(6) ? ? yes W(1) C(1) 1.986(9) ? ? yes W(1) C(1) 1.986(9) ? ? yes W(1) C(5) 1.799(9) ? ? yes O(1) C(1) 1.141(8) ? ? yes N(1) C(2) 1.45(1) ? ? yes N(1) C(3) 1.50(1) ? ? yes N(1) C(4) 1.46(1) ? ? yes N(2) C(9) 1.41(1) ? ? yes N(2) C(10) 1.15(1) ? ? yes N(3) C(13) 1.28(2) ? ? yes N(3) C(14) 1.35(2) ? ? yes C(4) C(4) 1.28(2) ? ? yes C(5) C(6) 1.45(1) ? ? yes C(6) C(7) 1.377(9) ? ? yes C(6) C(7) 1.377(9) ? ? yes C(7) C(8) 1.396(10) ? ? yes C(8) C(9) 1.373(10) ? ? yes C(10) C(11) 1.52(2) ? ? yes C(11) C(12) 1.39(2) ? ? yes C(11) C(15) 1.42(2) ? ? yes C(12) C(13) 1.36(2) ? ? yes C(14) C(15) 1.33(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 Br(1) W(1) N(1) 90.9(2) ? ? ? yes Br(1) W(1) N(1) 90.9(2) ? ? ? yes Br(1) W(1) C(1) 87.3(2) ? ? ? yes Br(1) W(1) C(1) 87.3(2) ? ? ? yes Br(1) W(1) C(5) 168.3(3) ? ? ? yes N(1) W(1) N(1) 78.6(4) ? ? ? yes N(1) W(1) C(1) 175.1(3) ? ? ? yes N(1) W(1) C(1) 96.8(3) ? ? ? yes N(1) W(1) C(5) 98.1(3) ? ? ? yes N(1) W(1) C(1) 96.8(3) ? ? ? yes N(1) W(1) C(1) 175.1(3) ? ? ? yes N(1) W(1) C(5) 98.1(3) ? ? ? yes C(1) W(1) C(1) 87.6(5) ? ? ? yes C(1) W(1) C(5) 84.3(3) ? ? ? yes C(1) W(1) C(5) 84.3(3) ? ? ? yes W(1) N(1) C(2) 111.0(6) ? ? ? yes W(1) N(1) C(3) 115.8(5) ? ? ? yes W(1) N(1) C(4) 106.0(5) ? ? ? yes C(2) N(1) C(3) 108.5(8) ? ? ? yes C(2) N(1) C(4) 108.0(9) ? ? ? yes C(3) N(1) C(4) 107.2(8) ? ? ? yes C(9) N(2) C(10) 122(1) ? ? ? yes C(13) N(3) C(14) 117(1) ? ? ? yes W(1) C(1) O(1) 177.0(7) ? ? ? yes N(1) C(4) C(4) 124.5(5) ? ? ? yes W(1) C(5) C(6) 173.6(7) ? ? ? yes C(5) C(6) C(7) 121.3(5) ? ? ? yes C(5) C(6) C(7) 121.3(5) ? ? ? yes C(7) C(6) C(7) 117.4(9) ? ? ? yes C(6) C(7) C(8) 121.7(8) ? ? ? yes C(7) C(8) C(9) 119.7(9) ? ? ? yes N(2) C(9) C(8) 120.0(5) ? ? ? yes N(2) C(9) C(8) 120.0(5) ? ? ? yes C(8) C(9) C(8) 119(1) ? ? ? yes N(2) C(10) C(11) 124(1) ? ? ? yes C(10) C(11) C(12) 121(1) ? ? ? yes C(10) C(11) C(15) 121(1) ? ? ? yes C(12) C(11) C(15) 117(1) ? ? ? yes C(11) C(12) C(13) 119(1) ? ? ? yes N(3) C(13) C(12) 124(1) ? ? ? yes N(3) C(14) C(15) 125(1) ? ? ? yes C(11) C(15) C(14) 116(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_IPDS_096 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 8 16:26:00 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' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 10.680(3) _cell_length_b 13.549(4) _cell_length_c 16.015(4) _cell_angle_alpha 90 _cell_angle_beta 95.73(2) _cell_angle_gamma 90 _cell_volume 2305.8(10) _cell_formula_units_Z 4 _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 '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 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 645.21 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H25 Br N4 O3 W ' _chemical_formula_moiety 'C21 H25 Br N4 O3 W ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1248.00 _exptl_absorpt_coefficient_mu 6.782 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ _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_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 4397 _reflns_number_total 4397 _reflns_number_observed 3210 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.63 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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' O 0 12 0.011 0.006 'International Tables' N 0 16 0.006 0.003 'International Tables' C 0 84 0.003 0.002 'International Tables' H 0 100 0.000 0.000 '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 W(1) 0.27064(3) 0.16652(2) 0.47242(2) 0.02973(9) Uij ? ? Br(1) 0.2764(1) -0.02544(6) 0.51729(7) 0.0584(3) Uij ? ? O(1) 0.4624(7) 0.1269(5) 0.3407(4) 0.072(2) Uij ? ? O(2) 0.0640(8) 0.1149(7) 0.3289(6) 0.104(3) Uij ? ? O(3) 0.1615(8) 0.7321(4) 0.3161(5) 0.086(3) Uij ? ? N(1) 0.1378(7) 0.1972(5) 0.5733(4) 0.045(2) Uij ? ? N(2) 0.4110(6) 0.2081(5) 0.5845(4) 0.039(2) Uij ? ? N(3) 0.2677(7) 0.6377(5) 0.2333(4) 0.045(2) Uij ? ? N(4) 0.2397(9) 0.9763(6) 0.0963(7) 0.079(3) Uij ? ? C(1) 0.3923(8) 0.1376(5) 0.3906(5) 0.042(2) Uij ? ? C(2) 0.1397(9) 0.1326(7) 0.3822(6) 0.054(3) Uij ? ? C(3) 0.2680(8) 0.2867(5) 0.4234(5) 0.035(2) Uij ? ? C(4) 0.2672(7) 0.3764(5) 0.3751(5) 0.033(2) Uij ? ? C(5) 0.3777(8) 0.4146(5) 0.3489(5) 0.040(2) Uij ? ? C(6) 0.3782(8) 0.5005(6) 0.3031(5) 0.041(2) Uij ? ? C(7) 0.2663(8) 0.5499(5) 0.2823(5) 0.039(2) Uij ? ? C(8) 0.1559(8) 0.5161(6) 0.3080(5) 0.045(3) Uij ? ? C(9) 0.1571(8) 0.4297(5) 0.3549(5) 0.042(2) Uij ? ? C(10) 0.2147(8) 0.7229(5) 0.2534(6) 0.045(3) Uij ? ? C(11) 0.2256(8) 0.8087(5) 0.1953(6) 0.042(2) Uij ? ? C(12) 0.2401(9) 0.8008(6) 0.1116(6) 0.052(3) Uij ? ? C(13) 0.245(1) 0.8872(8) 0.0647(7) 0.071(4) Uij ? ? C(14) 0.224(1) 0.9816(6) 0.1774(8) 0.071(4) Uij ? ? C(15) 0.2163(10) 0.9022(6) 0.2311(6) 0.058(3) Uij ? ? C(16) 0.0708(9) 0.2917(7) 0.5562(7) 0.062(3) Uij ? ? C(17) 0.0423(10) 0.1189(7) 0.5850(7) 0.069(4) Uij ? ? C(18) 0.219(1) 0.2048(8) 0.6552(5) 0.065(3) Uij ? ? C(19) 0.339(1) 0.2599(7) 0.6440(6) 0.065(3) Uij ? ? C(20) 0.4832(9) 0.1257(7) 0.6275(6) 0.056(3) Uij ? ? C(21) 0.507(1) 0.2793(8) 0.5583(7) 0.077(4) Uij ? ? H(1) 0.3361 0.6427 0.2032 0.0584 Uij ? ? H(2) 0.4544 0.3804 0.3631 0.0479 Uij ? ? H(3) 0.4548 0.5258 0.2862 0.0491 Uij ? ? H(4) 0.0790 0.5508 0.2930 0.0537 Uij ? ? H(5) 0.0807 0.4062 0.3730 0.0498 Uij ? ? H(6) 0.2469 0.7380 0.0861 0.0621 Uij ? ? H(7) 0.2534 0.8804 0.0065 0.0845 Uij ? ? H(8) 0.2142 1.0453 0.2006 0.0855 Uij ? ? H(9) 0.2059 0.9105 0.2888 0.0686 Uij ? ? H(10) 0.1307 0.3425 0.5493 0.0749 Uij ? ? H(11) 0.0149 0.2859 0.5072 0.0749 Uij ? ? H(12) 0.0255 0.3079 0.6027 0.0749 Uij ? ? H(13) -0.0061 0.1376 0.6294 0.0821 Uij ? ? H(14) -0.0110 0.1105 0.5350 0.0821 Uij ? ? H(15) 0.0843 0.0581 0.5999 0.0821 Uij ? ? H(16) 0.1731 0.2374 0.6952 0.0774 Uij ? ? H(17) 0.2393 0.1394 0.6755 0.0774 Uij ? ? H(18) 0.3899 0.2660 0.6971 0.0752 Uij ? ? H(19) 0.3199 0.3256 0.6240 0.0752 Uij ? ? H(20) 0.4263 0.0782 0.6456 0.0680 Uij ? ? H(21) 0.5342 0.0956 0.5891 0.0680 Uij ? ? H(22) 0.5350 0.1504 0.6742 0.0680 Uij ? ? H(23) 0.5607 0.2995 0.6062 0.0925 Uij ? ? H(24) 0.5548 0.2489 0.5190 0.0925 Uij ? ? H(25) 0.4651 0.3360 0.5334 0.0925 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) 0.0401(2) 0.0247(2) 0.0247(2) 0.0004(1) 0.0048(1) -0.0001(1) Br(1) 0.0733(7) 0.0325(5) 0.0716(7) 0.0021(4) 0.0179(5) 0.0044(4) O(1) 0.080(5) 0.090(5) 0.052(4) 0.033(4) 0.036(4) 0.010(4) O(2) 0.096(7) 0.130(7) 0.076(6) -0.025(6) -0.038(5) -0.017(5) O(3) 0.145(8) 0.037(4) 0.088(6) 0.009(4) 0.072(6) 0.007(3) N(1) 0.060(5) 0.035(3) 0.041(4) -0.010(3) 0.018(4) 0.001(3) N(2) 0.046(4) 0.039(3) 0.029(4) -0.001(3) -0.001(3) -0.003(3) N(3) 0.056(5) 0.036(3) 0.044(4) 0.014(3) 0.019(4) 0.015(3) N(4) 0.104(8) 0.045(5) 0.093(8) 0.014(4) 0.036(6) 0.022(5) C(1) 0.056(6) 0.032(4) 0.036(5) 0.011(4) -0.006(4) 0.009(3) C(2) 0.053(6) 0.056(5) 0.053(6) -0.004(4) 0.003(5) -0.005(4) C(3) 0.048(5) 0.034(4) 0.023(4) 0.005(3) 0.006(3) -0.001(3) C(4) 0.046(5) 0.027(4) 0.025(4) 0.001(3) 0.006(3) 0.002(3) C(5) 0.043(5) 0.040(4) 0.036(5) 0.011(3) 0.009(4) 0.010(3) C(6) 0.048(5) 0.035(4) 0.041(5) -0.003(4) 0.015(4) 0.007(3) C(7) 0.062(6) 0.029(4) 0.028(4) 0.004(4) 0.016(4) 0.004(3) C(8) 0.049(5) 0.041(5) 0.046(5) 0.009(4) 0.006(4) 0.011(4) C(9) 0.043(5) 0.042(5) 0.040(5) -0.001(3) 0.005(4) 0.009(3) C(10) 0.058(6) 0.030(4) 0.049(5) 0.005(4) 0.026(5) 0.004(3) C(11) 0.040(5) 0.029(4) 0.059(6) 0.000(3) 0.011(4) 0.009(3) C(12) 0.065(6) 0.034(4) 0.058(6) 0.007(4) 0.011(5) 0.009(4) C(13) 0.093(9) 0.063(7) 0.059(7) 0.009(6) 0.021(6) 0.020(5) C(14) 0.097(9) 0.022(5) 0.099(9) 0.007(4) 0.033(7) 0.004(5) C(15) 0.071(7) 0.046(5) 0.059(6) -0.002(4) 0.020(5) 0.002(4) C(16) 0.059(6) 0.055(5) 0.077(7) 0.023(5) 0.025(6) 0.005(5) C(17) 0.061(7) 0.060(6) 0.095(9) -0.019(5) 0.047(6) -0.011(5) C(18) 0.104(9) 0.074(6) 0.023(5) 0.007(6) 0.030(5) -0.008(4) C(19) 0.087(8) 0.060(6) 0.043(6) 0.010(5) -0.013(5) -0.018(4) C(20) 0.058(6) 0.068(6) 0.040(5) 0.012(5) -0.010(5) 0.007(4) C(21) 0.081(8) 0.083(7) 0.063(7) -0.042(6) -0.019(6) 0.006(6) #------------------------------------------------------------------------------ _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 3210 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0381 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0473 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.634 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean ? _refine_diff_density_min -2.38 _refine_diff_density_max 1.07 #------------------------------------------------------------------------------ _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) Br(1) 2.6975(9) ? ? yes W(1) N(1) 2.292(7) ? ? yes W(1) N(2) 2.291(6) ? ? yes W(1) C(1) 1.974(9) ? ? yes W(1) C(2) 1.96(1) ? ? yes W(1) C(3) 1.807(7) ? ? yes O(1) C(1) 1.16(1) ? ? yes O(2) C(2) 1.14(1) ? ? yes O(3) C(10) 1.208(10) ? ? yes N(1) C(16) 1.48(1) ? ? yes N(1) C(17) 1.50(1) ? ? yes N(1) C(18) 1.50(1) ? ? yes N(2) C(19) 1.46(1) ? ? yes N(2) C(20) 1.49(1) ? ? yes N(2) C(21) 1.50(1) ? ? yes N(3) C(7) 1.426(9) ? ? yes N(3) C(10) 1.339(9) ? ? yes N(4) C(13) 1.31(1) ? ? yes N(4) C(14) 1.33(1) ? ? yes C(3) C(4) 1.440(10) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(4) C(9) 1.39(1) ? ? yes C(5) C(6) 1.375(10) ? ? yes C(6) C(7) 1.38(1) ? ? yes C(7) C(8) 1.37(1) ? ? yes C(8) C(9) 1.39(1) ? ? yes C(10) C(11) 1.50(1) ? ? yes C(11) C(12) 1.37(1) ? ? yes C(11) C(15) 1.40(1) ? ? yes C(12) C(13) 1.39(1) ? ? yes C(14) C(15) 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 Br(1) W(1) N(1) 89.2(2) ? ? ? yes Br(1) W(1) N(2) 91.9(2) ? ? ? yes Br(1) W(1) C(1) 89.2(2) ? ? ? yes Br(1) W(1) C(2) 88.1(3) ? ? ? yes Br(1) W(1) C(3) 169.6(2) ? ? ? yes N(1) W(1) N(2) 78.8(3) ? ? ? yes N(1) W(1) C(1) 176.8(3) ? ? ? yes N(1) W(1) C(2) 96.6(3) ? ? ? yes N(1) W(1) C(3) 99.1(3) ? ? ? yes N(2) W(1) C(1) 98.4(3) ? ? ? yes N(2) W(1) C(2) 175.4(3) ? ? ? yes N(2) W(1) C(3) 95.7(3) ? ? ? yes C(1) W(1) C(2) 86.2(4) ? ? ? yes C(1) W(1) C(3) 82.7(3) ? ? ? yes C(2) W(1) C(3) 84.9(4) ? ? ? yes W(1) N(1) C(16) 110.4(5) ? ? ? yes W(1) N(1) C(17) 116.0(5) ? ? ? yes W(1) N(1) C(18) 106.4(5) ? ? ? yes C(16) N(1) C(17) 108.3(8) ? ? ? yes C(16) N(1) C(18) 109.2(7) ? ? ? yes C(17) N(1) C(18) 106.3(7) ? ? ? yes W(1) N(2) C(19) 106.4(5) ? ? ? yes W(1) N(2) C(20) 116.5(5) ? ? ? yes W(1) N(2) C(21) 110.6(5) ? ? ? yes C(19) N(2) C(20) 110.0(7) ? ? ? yes C(19) N(2) C(21) 107.0(7) ? ? ? yes C(20) N(2) C(21) 105.9(8) ? ? ? yes C(7) N(3) C(10) 123.9(6) ? ? ? yes C(13) N(4) C(14) 116.2(8) ? ? ? yes W(1) C(1) O(1) 175.6(7) ? ? ? yes W(1) C(2) O(2) 178.4(9) ? ? ? yes W(1) C(3) C(4) 173.2(6) ? ? ? yes C(3) C(4) C(5) 121.1(7) ? ? ? yes C(3) C(4) C(9) 121.5(7) ? ? ? yes C(5) C(4) C(9) 117.4(7) ? ? ? yes C(4) C(5) C(6) 121.6(7) ? ? ? yes C(5) C(6) C(7) 119.4(7) ? ? ? yes N(3) C(7) C(6) 118.8(7) ? ? ? yes N(3) C(7) C(8) 120.1(7) ? ? ? yes C(6) C(7) C(8) 121.1(7) ? ? ? yes C(7) C(8) C(9) 118.9(8) ? ? ? yes C(4) C(9) C(8) 121.7(7) ? ? ? yes O(3) C(10) N(3) 122.3(7) ? ? ? yes O(3) C(10) C(11) 120.5(7) ? ? ? yes N(3) C(10) C(11) 117.2(7) ? ? ? yes C(10) C(11) C(12) 124.8(7) ? ? ? yes C(10) C(11) C(15) 115.8(8) ? ? ? yes C(12) C(11) C(15) 119.4(8) ? ? ? yes C(11) C(12) C(13) 118.4(9) ? ? ? yes N(4) C(13) C(12) 123(1) ? ? ? yes N(4) C(14) C(15) 125.9(8) ? ? ? yes C(11) C(15) C(14) 116.0(9) ? ? ? yes N(1) C(18) C(19) 110.7(7) ? ? ? yes N(2) C(19) C(18) 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 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_C35H30Cl1N1O2P2W1.CH2Cl2 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Sep 8 16:23:34 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' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 19.851(2) _cell_length_b 9.089(3) _cell_length_c 21.874(2) _cell_angle_alpha 90.06(2) _cell_angle_beta 113.155(7) _cell_angle_gamma 90.05(2) _cell_volume 3628.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 301.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 22.0 #------------------------------------------------------------------------------ _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 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 862.81 _chemical_formula_analytical ? _chemical_formula_sum 'C36 H32 Cl3 N O2 P2 W ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1704.00 _exptl_absorpt_coefficient_mu 3.528 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.912 #------------------------------------------------------------------------------ _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 3 _diffrn_standards_interval_count 3 _diffrn_standards_decay_% -21.98 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 6288 _reflns_number_total 6204 _reflns_number_observed 4409 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 2.08 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 23.97 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.03076 _diffrn_orient_matrix_UB_12 -0.05151 _diffrn_orient_matrix_UB_13 -0.02021 _diffrn_orient_matrix_UB_21 -0.03867 _diffrn_orient_matrix_UB_22 0.01735 _diffrn_orient_matrix_UB_23 -0.04535 _diffrn_orient_matrix_UB_31 0.02366 _diffrn_orient_matrix_UB_32 0.09566 _diffrn_orient_matrix_UB_33 -0.00257 #------------------------------------------------------------------------------ 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' P 0 8 0.102 0.094 'International Tables' Cl 0 12 0.148 0.159 'International Tables' O 0 8 0.011 0.006 'International Tables' N 0 4 0.006 0.003 'International Tables' C 0 144 0.003 0.002 'International Tables' H 0 128 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) 0.25118(2) 0.08579(3) 0.20732(1) 0.03775(8) Uij ? ? Cl(1) 0.22087(9) -0.0083(2) 0.08787(7) 0.0370(5) Uij ? ? Cl(2) 0.2358(3) -0.1772(6) 0.4454(2) 0.197(2) Uij ? ? Cl(3) 0.2041(3) 0.0135(5) 0.5368(2) 0.163(2) Uij ? ? P(1) 0.3295(1) -0.1452(2) 0.23981(9) 0.0405(5) Uij ? ? P(2) 0.1573(1) -0.0973(2) 0.21303(9) 0.0432(5) Uij ? ? O(1) 0.3697(3) 0.2847(7) 0.1847(3) 0.090(3) Uij ? ? O(2) 0.1382(4) 0.3449(8) 0.1579(3) 0.087(2) Uij ? ? N(1) 0.3502(4) 0.5215(9) 0.5184(3) 0.073(2) Uij ? ? C(1) 0.3270(4) 0.2114(9) 0.1926(4) 0.053(3) Uij ? ? C(2) 0.1786(4) 0.2474(10) 0.1735(4) 0.053(2) Uij ? ? C(3) 0.2761(4) 0.1692(8) 0.2886(3) 0.043(2) Uij ? ? C(4) 0.2959(4) 0.2584(8) 0.3483(3) 0.041(2) Uij ? ? C(5) 0.3369(4) 0.3845(8) 0.3566(4) 0.051(2) Uij ? ? C(6) 0.3548(5) 0.4725(9) 0.4123(4) 0.061(3) Uij ? ? C(7) 0.3308(4) 0.4368(9) 0.4620(4) 0.054(2) Uij ? ? C(8) 0.2912(5) 0.3081(10) 0.4554(4) 0.063(3) Uij ? ? C(9) 0.2742(4) 0.2197(9) 0.3999(4) 0.059(3) Uij ? ? C(10) 0.2660(4) -0.3033(8) 0.2238(4) 0.052(2) Uij ? ? C(11) 0.2041(4) -0.2715(8) 0.2465(4) 0.051(2) Uij ? ? C(12) 0.3926(4) -0.1672(8) 0.3268(3) 0.043(2) Uij ? ? C(13) 0.3751(4) -0.1096(9) 0.3775(4) 0.054(2) Uij ? ? C(14) 0.4225(5) -0.1261(10) 0.4436(4) 0.067(3) Uij ? ? C(15) 0.4881(5) -0.200(1) 0.4592(4) 0.067(3) Uij ? ? C(16) 0.5062(4) -0.256(1) 0.4103(4) 0.067(3) Uij ? ? C(17) 0.4589(4) -0.2396(10) 0.3445(4) 0.055(2) Uij ? ? C(18) 0.3872(4) -0.1974(9) 0.1958(3) 0.046(2) Uij ? ? C(19) 0.4381(5) -0.0972(9) 0.1925(4) 0.061(3) Uij ? ? C(20) 0.4880(5) -0.134(1) 0.1657(5) 0.076(3) Uij ? ? C(21) 0.4875(5) -0.272(1) 0.1412(5) 0.077(4) Uij ? ? C(22) 0.4376(6) -0.370(1) 0.1422(5) 0.085(4) Uij ? ? C(23) 0.3876(5) -0.334(1) 0.1699(4) 0.071(3) Uij ? ? C(24) 0.0816(4) -0.1438(10) 0.1345(4) 0.057(3) Uij ? ? C(25) 0.0835(5) -0.262(1) 0.0959(4) 0.078(3) Uij ? ? C(26) 0.0241(7) -0.287(2) 0.0360(5) 0.106(5) Uij ? ? C(27) -0.0365(8) -0.199(2) 0.0159(6) 0.116(5) Uij ? ? C(28) -0.0385(6) -0.083(2) 0.0543(6) 0.113(4) Uij ? ? C(29) 0.0192(5) -0.054(1) 0.1120(5) 0.079(3) Uij ? ? C(30) 0.1084(4) -0.0596(9) 0.2668(4) 0.052(2) Uij ? ? C(31) 0.0675(5) -0.171(1) 0.2793(5) 0.081(4) Uij ? ? C(32) 0.0280(6) -0.143(1) 0.3174(6) 0.106(5) Uij ? ? C(33) 0.0307(6) -0.008(2) 0.3451(5) 0.095(4) Uij ? ? C(34) 0.0708(5) 0.102(1) 0.3339(5) 0.080(4) Uij ? ? C(35) 0.1097(4) 0.078(1) 0.2937(4) 0.063(3) Uij ? ? C(36) 0.201(1) -0.154(2) 0.4993(10) 0.208(10) Uij ? ? H(1) 0.3866 0.5973 0.5296 0.0747 Uij ? ? H(2) 0.3190 0.4824 0.5423 0.0747 Uij ? ? H(3) 0.3535 0.4120 0.3230 0.0610 Uij ? ? H(4) 0.3837 0.5582 0.4165 0.0737 Uij ? ? H(5) 0.2755 0.2801 0.4895 0.0754 Uij ? ? H(6) 0.2475 0.1313 0.3967 0.0707 Uij ? ? H(7) 0.2456 -0.3237 0.1774 0.0628 Uij ? ? H(8) 0.2926 -0.3867 0.2471 0.0628 Uij ? ? H(9) 0.2239 -0.2665 0.2936 0.0617 Uij ? ? H(10) 0.1694 -0.3493 0.2319 0.0617 Uij ? ? H(11) 0.3302 -0.0583 0.3669 0.0649 Uij ? ? H(12) 0.4098 -0.0871 0.4779 0.0798 Uij ? ? H(13) 0.5206 -0.2108 0.5044 0.0801 Uij ? ? H(14) 0.5513 -0.3063 0.4212 0.0804 Uij ? ? H(15) 0.4723 -0.2789 0.3106 0.0661 Uij ? ? H(16) 0.4386 -0.0004 0.2091 0.0730 Uij ? ? H(17) 0.5227 -0.0635 0.1644 0.0910 Uij ? ? H(18) 0.5225 -0.2992 0.1234 0.0929 Uij ? ? H(19) 0.4363 -0.4654 0.1238 0.1020 Uij ? ? H(20) 0.3531 -0.4061 0.1709 0.0852 Uij ? ? H(21) 0.1246 -0.3256 0.1099 0.0934 Uij ? ? H(22) 0.0258 -0.3666 0.0085 0.1278 Uij ? ? H(23) -0.0770 -0.2181 -0.0246 0.1394 Uij ? ? H(24) -0.0805 -0.0217 0.0406 0.1354 Uij ? ? H(25) 0.0172 0.0285 0.1378 0.0950 Uij ? ? H(26) 0.0669 -0.2670 0.2614 0.0975 Uij ? ? H(27) -0.0013 -0.2187 0.3245 0.1275 Uij ? ? H(28) 0.0044 0.0090 0.3725 0.1142 Uij ? ? H(29) 0.0723 0.1962 0.3536 0.0962 Uij ? ? H(30) 0.1367 0.1561 0.2850 0.0753 Uij ? ? H(31) 0.1503 -0.1792 0.4777 0.2501 Uij ? ? H(32) 0.2242 -0.2225 0.5339 0.2501 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) 0.0421(2) 0.0351(2) 0.0380(2) -0.0015(2) 0.0178(1) -0.0013(2) Cl(1) 0.0406(9) 0.047(1) 0.0239(8) -0.0020(8) 0.0130(7) -0.0060(8) Cl(2) 0.288(6) 0.179(4) 0.189(4) 0.094(4) 0.163(4) 0.078(4) Cl(3) 0.215(4) 0.124(3) 0.180(4) 0.019(3) 0.111(3) 0.029(3) P(1) 0.046(1) 0.037(1) 0.040(1) 0.0027(9) 0.0185(9) -0.0005(9) P(2) 0.044(1) 0.045(1) 0.044(1) -0.006(1) 0.0203(8) -0.0032(10) O(1) 0.080(5) 0.077(5) 0.124(6) -0.018(4) 0.054(4) 0.019(4) O(2) 0.088(5) 0.074(5) 0.105(5) 0.030(4) 0.046(4) 0.020(4) N(1) 0.080(5) 0.075(5) 0.062(4) -0.011(4) 0.025(4) -0.028(4) C(1) 0.062(5) 0.045(5) 0.055(5) 0.000(4) 0.025(4) 0.002(4) C(2) 0.053(5) 0.051(5) 0.057(5) 0.002(5) 0.025(4) 0.004(4) C(3) 0.041(4) 0.038(4) 0.051(4) -0.007(4) 0.021(3) 0.010(4) C(4) 0.050(4) 0.039(4) 0.039(4) -0.001(4) 0.021(3) -0.004(4) C(5) 0.062(5) 0.048(5) 0.050(4) -0.006(4) 0.030(4) -0.005(4) C(6) 0.072(6) 0.046(5) 0.063(5) -0.016(4) 0.024(5) -0.010(4) C(7) 0.055(5) 0.058(6) 0.044(4) 0.003(4) 0.016(4) -0.010(4) C(8) 0.080(6) 0.066(6) 0.051(5) -0.016(5) 0.036(4) -0.009(4) C(9) 0.075(6) 0.050(5) 0.056(5) -0.021(5) 0.031(4) -0.008(4) C(10) 0.059(5) 0.032(4) 0.068(5) 0.001(4) 0.027(4) -0.006(4) C(11) 0.058(5) 0.042(5) 0.057(5) -0.008(4) 0.025(4) 0.000(4) C(12) 0.047(4) 0.039(4) 0.045(4) 0.001(4) 0.020(3) 0.003(4) C(13) 0.067(5) 0.048(5) 0.046(4) 0.002(4) 0.021(4) 0.000(4) C(14) 0.100(7) 0.059(6) 0.041(5) -0.007(5) 0.028(5) -0.005(4) C(15) 0.072(6) 0.061(6) 0.049(5) -0.008(5) 0.005(5) 0.008(4) C(16) 0.057(5) 0.079(6) 0.060(5) 0.008(5) 0.018(4) 0.020(5) C(17) 0.056(5) 0.059(5) 0.050(4) 0.003(4) 0.019(4) 0.003(4) C(18) 0.050(4) 0.051(5) 0.036(4) 0.005(4) 0.018(3) -0.002(4) C(19) 0.068(5) 0.055(5) 0.071(5) 0.013(5) 0.039(5) 0.005(5) C(20) 0.070(6) 0.079(7) 0.098(7) 0.013(5) 0.055(6) 0.016(6) C(21) 0.079(7) 0.100(9) 0.072(6) 0.028(7) 0.050(5) 0.005(6) C(22) 0.096(8) 0.081(8) 0.091(7) 0.019(6) 0.051(6) -0.024(6) C(23) 0.070(6) 0.064(6) 0.090(7) -0.010(5) 0.045(5) -0.023(5) C(24) 0.060(5) 0.064(6) 0.050(5) -0.025(5) 0.024(4) -0.003(4) C(25) 0.080(6) 0.089(8) 0.067(6) -0.027(6) 0.032(5) -0.029(6) C(26) 0.121(10) 0.13(1) 0.068(7) -0.072(9) 0.040(7) -0.041(7) C(27) 0.11(1) 0.15(1) 0.065(7) -0.07(1) 0.002(7) 0.008(8) C(28) 0.082(8) 0.12(1) 0.090(8) -0.016(8) -0.016(7) 0.040(8) C(29) 0.070(6) 0.074(7) 0.076(6) -0.005(5) 0.008(5) 0.003(5) C(30) 0.044(4) 0.061(6) 0.053(5) -0.004(4) 0.021(4) -0.005(4) C(31) 0.099(7) 0.072(7) 0.102(7) -0.028(6) 0.071(6) -0.017(6) C(32) 0.128(10) 0.101(9) 0.14(1) -0.026(8) 0.110(9) -0.021(8) C(33) 0.089(8) 0.13(1) 0.096(8) 0.001(8) 0.069(7) -0.003(8) C(34) 0.083(7) 0.091(8) 0.078(6) 0.009(6) 0.045(6) -0.019(6) C(35) 0.059(5) 0.067(6) 0.067(5) -0.001(5) 0.030(4) -0.004(5) C(36) 0.35(3) 0.13(1) 0.26(2) 0.06(2) 0.24(2) 0.08(1) #------------------------------------------------------------------------------ _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 2.28518 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4409 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0326 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0415 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.512 _refine_ls_shift/esd_max 0.0280 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.66 _refine_diff_density_max 1.30 #------------------------------------------------------------------------------ _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) 2.584(2) ? ? yes W(1) P(1) 2.544(2) ? ? yes W(1) P(2) 2.537(2) ? ? yes W(1) C(1) 2.013(8) ? ? yes W(1) C(2) 1.986(9) ? ? yes W(1) C(3) 1.812(7) ? ? yes Cl(2) C(36) 1.60(1) ? ? yes Cl(3) C(36) 1.72(2) ? ? yes P(1) C(10) 1.850(8) ? ? yes P(1) C(12) 1.832(7) ? ? yes P(1) C(18) 1.825(7) ? ? yes P(2) C(11) 1.837(8) ? ? yes P(2) C(24) 1.832(8) ? ? yes P(2) C(30) 1.828(8) ? ? yes O(1) C(1) 1.144(9) ? ? yes O(2) C(2) 1.154(9) ? ? yes N(1) C(7) 1.373(9) ? ? yes C(3) C(4) 1.453(9) ? ? yes C(4) C(5) 1.376(10) ? ? yes C(4) C(9) 1.402(9) ? ? yes C(5) C(6) 1.38(1) ? ? yes C(6) C(7) 1.39(1) ? ? yes C(7) C(8) 1.38(1) ? ? yes C(8) C(9) 1.38(1) ? ? yes C(10) C(11) 1.523(10) ? ? yes C(12) C(13) 1.389(10) ? ? yes C(12) C(17) 1.385(10) ? ? yes C(13) C(14) 1.39(1) ? ? yes C(14) C(15) 1.38(1) ? ? yes C(15) C(16) 1.36(1) ? ? yes C(16) C(17) 1.383(10) ? ? yes C(18) C(19) 1.38(1) ? ? yes C(18) C(23) 1.37(1) ? ? yes C(19) C(20) 1.38(1) ? ? yes C(20) C(21) 1.37(1) ? ? yes C(21) C(22) 1.34(1) ? ? yes C(22) C(23) 1.39(1) ? ? yes C(24) C(25) 1.37(1) ? ? yes C(24) C(29) 1.40(1) ? ? yes C(25) C(26) 1.39(1) ? ? yes C(26) C(27) 1.37(2) ? ? yes C(27) C(28) 1.35(2) ? ? yes C(28) C(29) 1.35(1) ? ? yes C(30) C(31) 1.39(1) ? ? yes C(30) C(35) 1.38(1) ? ? yes C(31) C(32) 1.38(1) ? ? yes C(32) C(33) 1.36(2) ? ? yes C(33) C(34) 1.36(1) ? ? yes C(34) C(35) 1.40(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 Cl(1) W(1) P(1) 83.33(6) ? ? ? yes Cl(1) W(1) P(2) 87.15(6) ? ? ? yes Cl(1) W(1) C(1) 85.2(2) ? ? ? yes Cl(1) W(1) C(2) 91.2(2) ? ? ? yes Cl(1) W(1) C(3) 173.9(2) ? ? ? yes P(1) W(1) P(2) 79.91(6) ? ? ? yes P(1) W(1) C(1) 95.7(2) ? ? ? yes P(1) W(1) C(2) 171.8(2) ? ? ? yes P(1) W(1) C(3) 99.7(2) ? ? ? yes P(2) W(1) C(1) 171.6(2) ? ? ? yes P(2) W(1) C(2) 93.7(2) ? ? ? yes P(2) W(1) C(3) 98.5(2) ? ? ? yes C(1) W(1) C(2) 89.9(3) ? ? ? yes C(1) W(1) C(3) 89.3(3) ? ? ? yes C(2) W(1) C(3) 86.3(3) ? ? ? yes W(1) P(1) C(10) 107.0(2) ? ? ? yes W(1) P(1) C(12) 118.4(2) ? ? ? yes W(1) P(1) C(18) 120.6(3) ? ? ? yes C(10) P(1) C(12) 104.4(3) ? ? ? yes C(10) P(1) C(18) 102.7(3) ? ? ? yes C(12) P(1) C(18) 101.8(3) ? ? ? yes W(1) P(2) C(11) 108.6(2) ? ? ? yes W(1) P(2) C(24) 116.9(2) ? ? ? yes W(1) P(2) C(30) 119.7(3) ? ? ? yes C(11) P(2) C(24) 106.0(4) ? ? ? yes C(11) P(2) C(30) 102.6(4) ? ? ? yes C(24) P(2) C(30) 101.5(4) ? ? ? yes W(1) C(1) O(1) 178.9(7) ? ? ? yes W(1) C(2) O(2) 175.6(7) ? ? ? yes W(1) C(3) C(4) 170.7(6) ? ? ? yes C(3) C(4) C(5) 121.3(6) ? ? ? yes C(3) C(4) C(9) 121.6(7) ? ? ? yes C(5) C(4) C(9) 117.1(6) ? ? ? yes C(4) C(5) C(6) 122.2(7) ? ? ? yes C(5) C(6) C(7) 120.5(7) ? ? ? yes N(1) C(7) C(6) 120.7(8) ? ? ? yes N(1) C(7) C(8) 121.0(7) ? ? ? yes C(6) C(7) C(8) 118.1(7) ? ? ? yes C(7) C(8) C(9) 121.0(7) ? ? ? yes C(4) C(9) C(8) 121.0(7) ? ? ? yes P(1) C(10) C(11) 111.5(5) ? ? ? yes P(2) C(11) C(10) 112.4(5) ? ? ? yes P(1) C(12) C(13) 120.2(6) ? ? ? yes P(1) C(12) C(17) 122.0(5) ? ? ? yes C(13) C(12) C(17) 117.8(7) ? ? ? yes C(12) C(13) C(14) 120.7(8) ? ? ? yes C(13) C(14) C(15) 119.9(8) ? ? ? yes C(14) C(15) C(16) 120.2(7) ? ? ? yes C(15) C(16) C(17) 120.0(8) ? ? ? yes C(12) C(17) C(16) 121.5(7) ? ? ? yes P(1) C(18) C(19) 118.7(6) ? ? ? yes P(1) C(18) C(23) 124.1(6) ? ? ? yes C(19) C(18) C(23) 117.0(7) ? ? ? yes C(18) C(19) C(20) 121.7(8) ? ? ? yes C(19) C(20) C(21) 119.8(9) ? ? ? yes C(20) C(21) C(22) 119.6(8) ? ? ? yes C(21) C(22) C(23) 120.9(9) ? ? ? yes C(18) C(23) C(22) 120.9(9) ? ? ? yes P(2) C(24) C(25) 123.0(7) ? ? ? yes P(2) C(24) C(29) 118.8(7) ? ? ? yes C(25) C(24) C(29) 118.1(8) ? ? ? yes C(24) C(25) C(26) 119(1) ? ? ? yes C(25) C(26) C(27) 121(1) ? ? ? yes C(26) C(27) C(28) 119(1) ? ? ? yes C(27) C(28) C(29) 120(1) ? ? ? yes C(24) C(29) C(28) 121(1) ? ? ? yes P(2) C(30) C(31) 119.2(7) ? ? ? yes P(2) C(30) C(35) 121.2(6) ? ? ? yes C(31) C(30) C(35) 119.6(7) ? ? ? yes C(30) C(31) C(32) 119.9(9) ? ? ? yes C(31) C(32) C(33) 120.4(10) ? ? ? yes C(32) C(33) C(34) 120.6(9) ? ? ? yes C(33) C(34) C(35) 120.3(9) ? ? ? yes C(30) C(35) C(34) 119.2(9) ? ? ? yes Cl(2) C(36) Cl(3) 121(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 ;