# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/276 data_1 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jan 4 09:23:24 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 9.570(3) _cell_length_b 14.443(1) _cell_length_c 14.261(2) _cell_angle_alpha 90 _cell_angle_beta 104.57(1) _cell_angle_gamma 90 _cell_volume 1907.6(6) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 18.44 _cell_measurement_theta_max 25.44 #------------------------------------------------------------------------------ _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 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_measured ? _exptl_crystal_F000 1072.00 _exptl_absorpt_coefficient_mu_cm 22.893 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.913 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_\% -1.14 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3937 _diffrn_reflns_av_R_equivalents 1.96 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 11 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 16 _diffrn_reflns_l_min -13 _diffrn_reflns_l_max 13 _diffrn_theta_min ? _diffrn_theta_max 25.4946 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.01427 _diffrn_orient_matrix_12 0.03905 _diffrn_orient_matrix_13 0.05475 _diffrn_orient_matrix_21 0.10480 _diffrn_orient_matrix_22 0.01665 _diffrn_orient_matrix_23 0.01706 _diffrn_orient_matrix_31 -0.02171 _diffrn_orient_matrix_32 0.05470 _diffrn_orient_matrix_33 -0.04427 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 44 0.003 0.002 'International Tables' H 0 52 0.000 0.000 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 4 0.011 0.006 'International Tables' Cl 0 24 0.148 0.159 'International Tables' Sb 0 4 -0.587 1.546 '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 Sb 0.20738(3) 0.74834(2) 0.47646(2) 0.0421 Uij ? ? Cl1 0.2919(2) 0.76431(9) 0.64582(8) 0.0649 Uij ? ? Cl2 0.1219(2) 0.7338(1) 0.30708(9) 0.0819 Uij ? ? Cl3 0.3620(1) 0.86900(9) 0.45277(9) 0.0625 Uij ? ? Cl4 0.0510(2) 0.6266(1) 0.4992(1) 0.0768 Uij ? ? Cl5 0.3890(2) 0.63808(10) 0.4759(1) 0.0689 Uij ? ? Cl6 0.0251(1) 0.85812(10) 0.4789(1) 0.0717 Uij ? ? O 0.2711(4) 0.1318(3) 0.4131(3) 0.0874 Uij ? ? N1 0.1677(4) 0.1657(3) 0.3513(3) 0.0606 Uij ? ? N2 0.1472(4) 0.2546(3) 0.3399(3) 0.0551 Uij ? ? N3 0.0229(4) 0.2626(2) 0.2640(2) 0.0439 Uij ? ? N4 0.0371(4) 0.4255(3) 0.2594(3) 0.0532 Uij ? ? C1 0.0609(5) 0.1133(4) 0.2873(3) 0.0507 Uij ? ? C2 0.0471(6) 0.0180(4) 0.2795(4) 0.0665 Uij ? ? C3 -0.0681(7) -0.0129(4) 0.2080(4) 0.0761 Uij ? ? C4 -0.1642(6) 0.0489(4) 0.1496(4) 0.0651 Uij ? ? C5 -0.1508(5) 0.1438(3) 0.1592(3) 0.0562 Uij ? ? C6 -0.0317(5) 0.1748(3) 0.2312(3) 0.0432 Uij ? ? C7 -0.0249(5) 0.3478(3) 0.2297(3) 0.0449 Uij ? ? C8 -0.1610(5) 0.3599(3) 0.1526(3) 0.0533 Uij ? ? C9 -0.1724(6) 0.4641(4) 0.1369(4) 0.0787 Uij ? ? C10 -0.0427(7) 0.5052(4) 0.2064(4) 0.0788 Uij ? ? C11 0.1736(6) 0.4457(4) 0.3316(4) 0.0784 Uij ? ? H1 0.1084 -0.0301 0.3166 0.0860 Uij ? ? H2 -0.0808 -0.0784 0.1979 0.0860 Uij ? ? H3 -0.2440 0.0165 0.0875 0.0860 Uij ? ? H4 -0.2274 0.1944 0.1094 0.0860 Uij ? ? H5 -0.2434 0.3278 0.1842 0.0860 Uij ? ? H6 -0.1572 0.3170 0.0905 0.0860 Uij ? ? H7 -0.1784 0.4790 0.0612 0.0860 Uij ? ? H8 -0.2780 0.4950 0.1260 0.0860 Uij ? ? H9 -0.0696 0.5460 0.2491 0.0860 Uij ? ? H10 0.0166 0.5355 0.1710 0.0995 Uij ? ? H11 0.2677 0.3971 0.3317 0.0860 Uij ? ? H12 0.1702 0.4162 0.3949 0.0860 Uij ? ? H13 0.1940 0.5120 0.3393 0.0995 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 Sb 0.0395(2) 0.0494(2) 0.0366(2) -0.0022(1) 0.0082(1) 0.0026(1) Cl1 0.0759(9) 0.0790(9) 0.0371(6) 0.0071(7) 0.0093(6) 0.0003(6) Cl2 0.101(1) 0.093(1) 0.0401(7) -0.0137(9) -0.0050(7) -0.0037(7) Cl3 0.0625(8) 0.0640(8) 0.0666(8) -0.0150(7) 0.0264(7) -0.0021(6) Cl4 0.0685(9) 0.0673(9) 0.098(1) -0.0197(7) 0.0275(8) 0.0080(8) Cl5 0.0691(9) 0.0703(9) 0.0730(9) 0.0180(7) 0.0286(7) 0.0008(7) Cl6 0.0513(8) 0.0789(10) 0.0866(10) 0.0194(7) 0.0207(7) 0.0180(8) O 0.070(3) 0.107(3) 0.070(2) 0.018(2) -0.009(2) 0.027(2) N1 0.056(3) 0.077(3) 0.044(2) 0.006(2) 0.005(2) 0.014(2) N2 0.050(2) 0.068(3) 0.043(2) -0.004(2) 0.001(2) 0.002(2) N3 0.042(2) 0.048(2) 0.039(2) -0.002(2) 0.006(2) -0.001(2) N4 0.068(3) 0.046(2) 0.049(2) -0.012(2) 0.021(2) -0.005(2) C1 0.056(3) 0.055(3) 0.043(3) 0.005(3) 0.017(2) 0.004(2) C2 0.085(4) 0.050(3) 0.070(4) 0.016(3) 0.032(3) 0.017(3) C3 0.101(5) 0.054(3) 0.084(4) -0.005(3) 0.043(4) -0.005(3) C4 0.074(4) 0.061(3) 0.062(3) -0.014(3) 0.019(3) -0.012(3) C5 0.061(3) 0.052(3) 0.053(3) -0.013(3) 0.010(3) -0.008(2) C6 0.049(3) 0.044(2) 0.039(2) -0.004(2) 0.015(2) -0.003(2) C7 0.052(3) 0.048(3) 0.040(2) -0.010(2) 0.022(2) -0.009(2) C8 0.059(3) 0.047(3) 0.054(3) 0.006(2) 0.012(3) 0.011(2) C9 0.087(4) 0.056(3) 0.083(4) 0.011(3) 0.003(3) 0.015(3) C10 0.106(5) 0.052(3) 0.090(5) 0.004(3) 0.047(4) 0.002(3) C11 0.083(4) 0.067(4) 0.076(4) -0.036(3) 0.003(3) -0.012(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.95977 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2355 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0290 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0370 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.290 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.44990 _refine_diff_density_max -0.42280 #------------------------------------------------------------------------------ _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 Sb Cl(1) 2.358(1) ? ? yes Sb Cl(2) 2.357(1) ? ? yes Sb Cl(3) 2.365(1) ? ? yes Sb Cl(4) 2.383(1) ? ? yes Sb Cl(5) 2.359(1) ? ? yes Sb Cl(6) 2.364(1) ? ? yes O N(1) 1.248(5) ? ? yes N(1) N(2) 1.303(5) ? ? yes N(1) C(1) 1.407(6) ? ? yes N(2) N(3) 1.397(5) ? ? yes N(3) C(6) 1.406(5) ? ? yes N(3) C(7) 1.360(5) ? ? yes N(4) C(7) 1.291(5) ? ? yes N(4) C(10) 1.480(7) ? ? yes N(4) C(11) 1.475(6) ? ? yes C(1) C(2) 1.385(7) ? ? yes C(1) C(6) 1.363(6) ? ? yes C(2) C(3) 1.374(7) ? ? yes C(3) C(4) 1.397(8) ? ? yes C(4) C(5) 1.380(7) ? ? yes C(5) C(6) 1.401(6) ? ? yes C(7) C(8) 1.489(6) ? ? yes C(8) C(9) 1.522(7) ? ? yes C(9) C(10) 1.501(8) ? ? 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) Sb Cl(2) 179.45(5) ? ? ? yes Cl(1) Sb Cl(3) 90.48(5) ? ? ? yes Cl(1) Sb Cl(4) 89.89(5) ? ? ? yes Cl(1) Sb Cl(5) 90.36(5) ? ? ? yes Cl(1) Sb Cl(6) 89.06(5) ? ? ? yes Cl(2) Sb Cl(3) 89.30(5) ? ? ? yes Cl(2) Sb Cl(4) 90.33(6) ? ? ? yes Cl(2) Sb Cl(5) 90.14(5) ? ? ? yes Cl(2) Sb Cl(6) 90.44(6) ? ? ? yes Cl(3) Sb Cl(4) 179.63(5) ? ? ? yes Cl(3) Sb Cl(5) 90.52(5) ? ? ? yes Cl(3) Sb Cl(6) 89.90(5) ? ? ? yes Cl(4) Sb Cl(5) 89.47(6) ? ? ? yes Cl(4) Sb Cl(6) 90.12(5) ? ? ? yes Cl(5) Sb Cl(6) 179.28(5) ? ? ? yes O N(1) N(2) 122.9(4) ? ? ? yes O N(1) C(1) 124.4(5) ? ? ? yes N(2) N(1) C(1) 112.7(4) ? ? ? yes N(1) N(2) N(3) 104.5(4) ? ? ? yes N(2) N(3) C(6) 110.8(3) ? ? ? yes N(2) N(3) C(7) 119.8(4) ? ? ? yes C(6) N(3) C(7) 129.3(3) ? ? ? yes C(7) N(4) C(10) 111.9(4) ? ? ? yes C(7) N(4) C(11) 130.9(4) ? ? ? yes C(10) N(4) C(11) 117.2(4) ? ? ? yes N(1) C(1) C(2) 128.7(5) ? ? ? yes N(1) C(1) C(6) 106.9(4) ? ? ? yes C(2) C(1) C(6) 124.5(5) ? ? ? yes C(1) C(2) C(3) 115.2(5) ? ? ? yes C(2) C(3) C(4) 121.3(5) ? ? ? yes C(3) C(4) C(5) 123.0(5) ? ? ? yes C(4) C(5) C(6) 115.3(5) ? ? ? yes N(3) C(6) C(1) 105.1(4) ? ? ? yes N(3) C(6) C(5) 134.2(4) ? ? ? yes C(1) C(6) C(5) 120.7(4) ? ? ? yes N(3) C(7) N(4) 125.7(4) ? ? ? yes N(3) C(7) C(8) 121.6(4) ? ? ? yes N(4) C(7) C(8) 112.7(4) ? ? ? yes C(7) C(8) C(9) 104.0(4) ? ? ? yes C(8) C(9) C(10) 106.1(4) ? ? ? yes N(4) C(10) C(9) 105.4(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_2 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 3 09:05:30 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution ' DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 9.058(2) _cell_length_b 15.729(4) _cell_length_c 6.598(1) _cell_angle_alpha 94.21(2) _cell_angle_beta 98.99(2) _cell_angle_gamma 73.38(2) _cell_volume 889.4(4) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 14.23 _cell_measurement_theta_max 25.71 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_measured ? _exptl_crystal_F000 508.00 _exptl_absorpt_coefficient_mu_cm 24.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.666 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_\% 0.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2943 _diffrn_reflns_av_R_equivalents 7.65 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 9 _diffrn_reflns_k_min -16 _diffrn_reflns_k_max 10 _diffrn_reflns_l_min -2 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 24.9939 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 0.09597 _diffrn_orient_matrix_12 0.01833 _diffrn_orient_matrix_13 0.05496 _diffrn_orient_matrix_21 0.06234 _diffrn_orient_matrix_22 -0.06373 _diffrn_orient_matrix_23 0.00448 _diffrn_orient_matrix_31 0.02113 _diffrn_orient_matrix_32 0.00288 _diffrn_orient_matrix_33 -0.14326 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 18 0.003 0.002 'International Tables' H 0 22 0.000 0.000 'International Tables' N 0 8 0.006 0.003 'International Tables' O 0 2 0.011 0.006 'International Tables' Cl 0 12 0.148 0.159 'International Tables' Sb 0 2 -0.587 1.546 '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 Sb 0.15106(6) 0.17881(3) 0.15069(7) 0.0336 Uij ? ? Cl1 0.1356(3) 0.2629(1) 0.4627(3) 0.0540 Uij ? ? Cl2 0.1768(3) 0.0955(2) -0.1568(3) 0.0585 Uij ? ? Cl3 0.2368(3) 0.2903(2) 0.0144(3) 0.0549 Uij ? ? Cl4 0.0568(3) 0.0728(1) 0.2825(4) 0.0565 Uij ? ? Cl5 -0.1073(2) 0.2601(2) 0.0297(4) 0.0590 Uij ? ? Cl6 0.4111(2) 0.1034(2) 0.2788(4) 0.0598 Uij ? ? O 0.5363(6) 0.3824(4) 0.0437(8) 0.0480 Uij ? ? N1 0.5041(7) 0.3758(4) 0.2186(10) 0.0378 Uij ? ? N2 0.5680(7) 0.3062(4) 0.3317(9) 0.0381 Uij ? ? N3 0.4980(7) 0.3233(4) 0.5066(9) 0.0356 Uij ? ? N4 0.6267(7) 0.1894(4) 0.6777(9) 0.0384 Uij ? ? C1 0.3901(8) 0.4408(5) 0.315(1) 0.0369 Uij ? ? C2 0.2965(9) 0.5228(5) 0.247(1) 0.0454 Uij ? ? C3 0.1974(10) 0.5681(6) 0.380(1) 0.0506 Uij ? ? C4 0.1908(10) 0.5350(6) 0.567(1) 0.0532 Uij ? ? C5 0.2846(9) 0.4524(6) 0.631(1) 0.0433 Uij ? ? C6 0.3862(8) 0.4071(5) 0.501(1) 0.0351 Uij ? ? C7 0.5216(8) 0.2645(5) 0.655(1) 0.0363 Uij ? ? C8 0.7533(10) 0.1528(6) 0.551(1) 0.0543 Uij ? ? C9 0.624(1) 0.1328(6) 0.844(1) 0.0548 Uij ? ? H1 0.2959 0.5428 0.1048 0.0728 Uij ? ? H2 0.1289 0.6244 0.3410 0.0728 Uij ? ? H3 0.1202 0.5701 0.6539 0.0728 Uij ? ? H4 0.2674 0.4368 0.7558 0.0728 Uij ? ? H5 0.4683 0.2902 0.7931 0.0728 Uij ? ? H6 0.8165 0.1921 0.5593 0.0659 Uij ? ? H7 0.7093 0.1464 0.4120 0.0654 Uij ? ? H8 0.8147 0.0965 0.5999 0.0654 Uij ? ? H9 0.6175 0.0743 0.7789 0.0728 Uij ? ? H10 0.7341 0.1127 0.9029 0.0728 Uij ? ? H11 0.5888 0.1688 0.9497 0.0728 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 Sb 0.0272(3) 0.0339(3) 0.0414(3) -0.0102(2) 0.0053(2) 0.0037(2) Cl1 0.061(1) 0.051(1) 0.049(1) -0.013(1) 0.013(1) -0.0064(10) Cl2 0.068(2) 0.060(1) 0.051(1) -0.025(1) 0.013(1) -0.011(1) Cl3 0.063(1) 0.055(1) 0.060(1) -0.033(1) 0.014(1) 0.007(1) Cl4 0.056(1) 0.043(1) 0.080(1) -0.016(1) 0.027(1) 0.010(1) Cl5 0.035(1) 0.052(1) 0.083(2) -0.0060(10) -0.007(1) 0.011(1) Cl6 0.031(1) 0.059(1) 0.081(2) -0.004(1) -0.004(1) 0.002(1) O 0.044(3) 0.055(4) 0.049(3) -0.010(3) 0.018(3) 0.011(3) N1 0.031(4) 0.039(4) 0.048(4) -0.015(3) 0.008(3) 0.003(3) N2 0.031(4) 0.038(4) 0.045(4) -0.007(3) 0.010(3) 0.006(3) N3 0.032(4) 0.037(4) 0.038(3) -0.009(3) 0.007(3) 0.005(3) N4 0.032(4) 0.039(4) 0.043(3) -0.007(3) 0.007(3) 0.004(3) C1 0.029(4) 0.042(4) 0.044(4) -0.016(4) 0.003(3) 0.003(3) C2 0.039(5) 0.037(5) 0.062(5) -0.011(4) 0.006(4) 0.013(4) C3 0.046(5) 0.038(5) 0.065(5) -0.004(4) 0.006(4) 0.013(4) C4 0.045(5) 0.040(5) 0.070(6) 0.002(4) 0.018(4) 0.004(4) C5 0.042(5) 0.044(5) 0.041(4) -0.005(4) 0.008(4) 0.005(4) C6 0.027(4) 0.031(4) 0.048(4) -0.011(3) 0.003(3) 0.005(3) C7 0.031(4) 0.039(4) 0.041(4) -0.014(4) 0.006(3) 0.001(3) C8 0.039(5) 0.054(6) 0.065(5) 0.005(4) 0.020(4) 0.012(4) C9 0.056(6) 0.040(5) 0.070(6) -0.010(4) 0.013(5) 0.016(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 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2247 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0570 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.300 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.76770 _refine_diff_density_max -1.55960 #------------------------------------------------------------------------------ _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 Sb Cl(1) 2.365(2) ? ? yes Sb Cl(2) 2.339(2) ? ? yes Sb Cl(3) 2.391(2) ? ? yes Sb Cl(4) 2.351(2) ? ? yes Sb Cl(5) 2.367(2) ? ? yes Sb Cl(6) 2.366(2) ? ? yes O N(1) 1.251(7) ? ? yes N(1) N(2) 1.309(8) ? ? yes N(1) C(1) 1.423(10) ? ? yes N(2) N(3) 1.375(8) ? ? yes N(3) C(6) 1.413(9) ? ? yes N(3) C(7) 1.348(9) ? ? yes N(4) C(7) 1.289(10) ? ? yes N(4) C(8) 1.484(10) ? ? yes N(4) C(9) 1.470(10) ? ? yes C(1) C(2) 1.39(1) ? ? yes C(1) C(6) 1.379(10) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(3) C(4) 1.39(1) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(5) C(6) 1.37(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) Sb Cl(2) 177.73(8) ? ? ? yes Cl(1) Sb Cl(3) 88.62(8) ? ? ? yes Cl(1) Sb Cl(4) 90.93(8) ? ? ? yes Cl(1) Sb Cl(5) 89.41(8) ? ? ? yes Cl(1) Sb Cl(6) 88.59(8) ? ? ? yes Cl(2) Sb Cl(3) 90.16(8) ? ? ? yes Cl(2) Sb Cl(4) 90.36(8) ? ? ? yes Cl(2) Sb Cl(5) 92.45(9) ? ? ? yes Cl(2) Sb Cl(6) 89.51(9) ? ? ? yes Cl(3) Sb Cl(4) 177.76(8) ? ? ? yes Cl(3) Sb Cl(5) 87.90(8) ? ? ? yes Cl(3) Sb Cl(6) 90.54(9) ? ? ? yes Cl(4) Sb Cl(5) 89.90(8) ? ? ? yes Cl(4) Sb Cl(6) 91.65(9) ? ? ? yes Cl(5) Sb Cl(6) 177.49(8) ? ? ? yes O N(1) N(2) 123.7(6) ? ? ? yes O N(1) C(1) 124.6(6) ? ? ? yes N(2) N(1) C(1) 111.7(6) ? ? ? yes N(1) N(2) N(3) 105.8(6) ? ? ? yes N(2) N(3) C(6) 111.3(5) ? ? ? yes N(2) N(3) C(7) 124.5(6) ? ? ? yes C(6) N(3) C(7) 123.9(6) ? ? ? yes C(7) N(4) C(8) 126.4(7) ? ? ? yes C(7) N(4) C(9) 118.3(6) ? ? ? yes C(8) N(4) C(9) 115.3(6) ? ? ? yes N(1) C(1) C(2) 129.7(7) ? ? ? yes N(1) C(1) C(6) 106.5(6) ? ? ? yes C(2) C(1) C(6) 123.7(7) ? ? ? yes C(1) C(2) C(3) 114.2(7) ? ? ? yes C(2) C(3) C(4) 123.0(8) ? ? ? yes C(3) C(4) C(5) 121.7(8) ? ? ? yes C(4) C(5) C(6) 115.9(7) ? ? ? yes N(3) C(6) C(1) 104.7(6) ? ? ? yes N(3) C(6) C(5) 133.8(7) ? ? ? yes C(1) C(6) C(5) 121.5(7) ? ? ? yes N(3) C(7) N(4) 127.7(7) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_3 #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jan 4 09:23:24 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 9.570(3) _cell_length_b 14.443(1) _cell_length_c 14.261(2) _cell_angle_alpha 90 _cell_angle_beta 104.57(1) _cell_angle_gamma 90 _cell_volume 1907.6(6) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 18.44 _cell_measurement_theta_max 25.44 #------------------------------------------------------------------------------ _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 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.921 _exptl_crystal_density_measured ? _exptl_crystal_F000 1072.00 _exptl_absorpt_coefficient_mu_cm 22.893 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.913 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_\% -1.14 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 3937 _diffrn_reflns_av_R_equivalents 1.96 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 11 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 16 _diffrn_reflns_l_min -13 _diffrn_reflns_l_max 13 _diffrn_theta_min ? _diffrn_theta_max 25.4946 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.01427 _diffrn_orient_matrix_12 0.03905 _diffrn_orient_matrix_13 0.05475 _diffrn_orient_matrix_21 0.10480 _diffrn_orient_matrix_22 0.01665 _diffrn_orient_matrix_23 0.01706 _diffrn_orient_matrix_31 -0.02171 _diffrn_orient_matrix_32 0.05470 _diffrn_orient_matrix_33 -0.04427 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 44 0.003 0.002 'International Tables' H 0 52 0.000 0.000 'International Tables' N 0 16 0.006 0.003 'International Tables' O 0 4 0.011 0.006 'International Tables' Cl 0 24 0.148 0.159 'International Tables' Sb 0 4 -0.587 1.546 '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 Sb 0.20738(3) 0.74834(2) 0.47646(2) 0.0421 Uij ? ? Cl1 0.2919(2) 0.76431(9) 0.64582(8) 0.0649 Uij ? ? Cl2 0.1219(2) 0.7338(1) 0.30708(9) 0.0819 Uij ? ? Cl3 0.3620(1) 0.86900(9) 0.45277(9) 0.0625 Uij ? ? Cl4 0.0510(2) 0.6266(1) 0.4992(1) 0.0768 Uij ? ? Cl5 0.3890(2) 0.63808(10) 0.4759(1) 0.0689 Uij ? ? Cl6 0.0251(1) 0.85812(10) 0.4789(1) 0.0717 Uij ? ? O 0.2711(4) 0.1318(3) 0.4131(3) 0.0874 Uij ? ? N1 0.1677(4) 0.1657(3) 0.3513(3) 0.0606 Uij ? ? N2 0.1472(4) 0.2546(3) 0.3399(3) 0.0551 Uij ? ? N3 0.0229(4) 0.2626(2) 0.2640(2) 0.0439 Uij ? ? N4 0.0371(4) 0.4255(3) 0.2594(3) 0.0532 Uij ? ? C1 0.0609(5) 0.1133(4) 0.2873(3) 0.0507 Uij ? ? C2 0.0471(6) 0.0180(4) 0.2795(4) 0.0665 Uij ? ? C3 -0.0681(7) -0.0129(4) 0.2080(4) 0.0761 Uij ? ? C4 -0.1642(6) 0.0489(4) 0.1496(4) 0.0651 Uij ? ? C5 -0.1508(5) 0.1438(3) 0.1592(3) 0.0562 Uij ? ? C6 -0.0317(5) 0.1748(3) 0.2312(3) 0.0432 Uij ? ? C7 -0.0249(5) 0.3478(3) 0.2297(3) 0.0449 Uij ? ? C8 -0.1610(5) 0.3599(3) 0.1526(3) 0.0533 Uij ? ? C9 -0.1724(6) 0.4641(4) 0.1369(4) 0.0787 Uij ? ? C10 -0.0427(7) 0.5052(4) 0.2064(4) 0.0788 Uij ? ? C11 0.1736(6) 0.4457(4) 0.3316(4) 0.0784 Uij ? ? H1 0.1084 -0.0301 0.3166 0.0860 Uij ? ? H2 -0.0808 -0.0784 0.1979 0.0860 Uij ? ? H3 -0.2440 0.0165 0.0875 0.0860 Uij ? ? H4 -0.2274 0.1944 0.1094 0.0860 Uij ? ? H5 -0.2434 0.3278 0.1842 0.0860 Uij ? ? H6 -0.1572 0.3170 0.0905 0.0860 Uij ? ? H7 -0.1784 0.4790 0.0612 0.0860 Uij ? ? H8 -0.2780 0.4950 0.1260 0.0860 Uij ? ? H9 -0.0696 0.5460 0.2491 0.0860 Uij ? ? H10 0.0166 0.5355 0.1710 0.0995 Uij ? ? H11 0.2677 0.3971 0.3317 0.0860 Uij ? ? H12 0.1702 0.4162 0.3949 0.0860 Uij ? ? H13 0.1940 0.5120 0.3393 0.0995 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 Sb 0.0395(2) 0.0494(2) 0.0366(2) -0.0022(1) 0.0082(1) 0.0026(1) Cl1 0.0759(9) 0.0790(9) 0.0371(6) 0.0071(7) 0.0093(6) 0.0003(6) Cl2 0.101(1) 0.093(1) 0.0401(7) -0.0137(9) -0.0050(7) -0.0037(7) Cl3 0.0625(8) 0.0640(8) 0.0666(8) -0.0150(7) 0.0264(7) -0.0021(6) Cl4 0.0685(9) 0.0673(9) 0.098(1) -0.0197(7) 0.0275(8) 0.0080(8) Cl5 0.0691(9) 0.0703(9) 0.0730(9) 0.0180(7) 0.0286(7) 0.0008(7) Cl6 0.0513(8) 0.0789(10) 0.0866(10) 0.0194(7) 0.0207(7) 0.0180(8) O 0.070(3) 0.107(3) 0.070(2) 0.018(2) -0.009(2) 0.027(2) N1 0.056(3) 0.077(3) 0.044(2) 0.006(2) 0.005(2) 0.014(2) N2 0.050(2) 0.068(3) 0.043(2) -0.004(2) 0.001(2) 0.002(2) N3 0.042(2) 0.048(2) 0.039(2) -0.002(2) 0.006(2) -0.001(2) N4 0.068(3) 0.046(2) 0.049(2) -0.012(2) 0.021(2) -0.005(2) C1 0.056(3) 0.055(3) 0.043(3) 0.005(3) 0.017(2) 0.004(2) C2 0.085(4) 0.050(3) 0.070(4) 0.016(3) 0.032(3) 0.017(3) C3 0.101(5) 0.054(3) 0.084(4) -0.005(3) 0.043(4) -0.005(3) C4 0.074(4) 0.061(3) 0.062(3) -0.014(3) 0.019(3) -0.012(3) C5 0.061(3) 0.052(3) 0.053(3) -0.013(3) 0.010(3) -0.008(2) C6 0.049(3) 0.044(2) 0.039(2) -0.004(2) 0.015(2) -0.003(2) C7 0.052(3) 0.048(3) 0.040(2) -0.010(2) 0.022(2) -0.009(2) C8 0.059(3) 0.047(3) 0.054(3) 0.006(2) 0.012(3) 0.011(2) C9 0.087(4) 0.056(3) 0.083(4) 0.011(3) 0.003(3) 0.015(3) C10 0.106(5) 0.052(3) 0.090(5) 0.004(3) 0.047(4) 0.002(3) C11 0.083(4) 0.067(4) 0.076(4) -0.036(3) 0.003(3) -0.012(3) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 1.95977 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2355 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0290 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0370 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.290 _refine_ls_shift/esd_max 0.0030 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.44990 _refine_diff_density_max -0.42280 #------------------------------------------------------------------------------ _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 Sb Cl(1) 2.358(1) ? ? yes Sb Cl(2) 2.357(1) ? ? yes Sb Cl(3) 2.365(1) ? ? yes Sb Cl(4) 2.383(1) ? ? yes Sb Cl(5) 2.359(1) ? ? yes Sb Cl(6) 2.364(1) ? ? yes O N(1) 1.248(5) ? ? yes N(1) N(2) 1.303(5) ? ? yes N(1) C(1) 1.407(6) ? ? yes N(2) N(3) 1.397(5) ? ? yes N(3) C(6) 1.406(5) ? ? yes N(3) C(7) 1.360(5) ? ? yes N(4) C(7) 1.291(5) ? ? yes N(4) C(10) 1.480(7) ? ? yes N(4) C(11) 1.475(6) ? ? yes C(1) C(2) 1.385(7) ? ? yes C(1) C(6) 1.363(6) ? ? yes C(2) C(3) 1.374(7) ? ? yes C(3) C(4) 1.397(8) ? ? yes C(4) C(5) 1.380(7) ? ? yes C(5) C(6) 1.401(6) ? ? yes C(7) C(8) 1.489(6) ? ? yes C(8) C(9) 1.522(7) ? ? yes C(9) C(10) 1.501(8) ? ? 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) Sb Cl(2) 179.45(5) ? ? ? yes Cl(1) Sb Cl(3) 90.48(5) ? ? ? yes Cl(1) Sb Cl(4) 89.89(5) ? ? ? yes Cl(1) Sb Cl(5) 90.36(5) ? ? ? yes Cl(1) Sb Cl(6) 89.06(5) ? ? ? yes Cl(2) Sb Cl(3) 89.30(5) ? ? ? yes Cl(2) Sb Cl(4) 90.33(6) ? ? ? yes Cl(2) Sb Cl(5) 90.14(5) ? ? ? yes Cl(2) Sb Cl(6) 90.44(6) ? ? ? yes Cl(3) Sb Cl(4) 179.63(5) ? ? ? yes Cl(3) Sb Cl(5) 90.52(5) ? ? ? yes Cl(3) Sb Cl(6) 89.90(5) ? ? ? yes Cl(4) Sb Cl(5) 89.47(6) ? ? ? yes Cl(4) Sb Cl(6) 90.12(5) ? ? ? yes Cl(5) Sb Cl(6) 179.28(5) ? ? ? yes O N(1) N(2) 122.9(4) ? ? ? yes O N(1) C(1) 124.4(5) ? ? ? yes N(2) N(1) C(1) 112.7(4) ? ? ? yes N(1) N(2) N(3) 104.5(4) ? ? ? yes N(2) N(3) C(6) 110.8(3) ? ? ? yes N(2) N(3) C(7) 119.8(4) ? ? ? yes C(6) N(3) C(7) 129.3(3) ? ? ? yes C(7) N(4) C(10) 111.9(4) ? ? ? yes C(7) N(4) C(11) 130.9(4) ? ? ? yes C(10) N(4) C(11) 117.2(4) ? ? ? yes N(1) C(1) C(2) 128.7(5) ? ? ? yes N(1) C(1) C(6) 106.9(4) ? ? ? yes C(2) C(1) C(6) 124.5(5) ? ? ? yes C(1) C(2) C(3) 115.2(5) ? ? ? yes C(2) C(3) C(4) 121.3(5) ? ? ? yes C(3) C(4) C(5) 123.0(5) ? ? ? yes C(4) C(5) C(6) 115.3(5) ? ? ? yes N(3) C(6) C(1) 105.1(4) ? ? ? yes N(3) C(6) C(5) 134.2(4) ? ? ? yes C(1) C(6) C(5) 120.7(4) ? ? ? yes N(3) C(7) N(4) 125.7(4) ? ? ? yes N(3) C(7) C(8) 121.6(4) ? ? ? yes N(4) C(7) C(8) 112.7(4) ? ? ? yes C(7) C(8) C(9) 104.0(4) ? ? ? yes C(8) C(9) C(10) 106.1(4) ? ? ? yes N(4) C(10) C(9) 105.4(4) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; data_4 #------------------------------------------------------------------------------ _audit_creation_date 'Wed Mar 3 09:05:30 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution ' DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 9.058(2) _cell_length_b 15.729(4) _cell_length_c 6.598(1) _cell_angle_alpha 94.21(2) _cell_angle_beta 98.99(2) _cell_angle_gamma 73.38(2) _cell_volume 889.4(4) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 14.23 _cell_measurement_theta_max 25.71 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.963 _exptl_crystal_density_measured ? _exptl_crystal_F000 508.00 _exptl_absorpt_coefficient_mu_cm 24.496 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.666 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_\% 0.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2943 _diffrn_reflns_av_R_equivalents 7.65 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 9 _diffrn_reflns_k_min -16 _diffrn_reflns_k_max 10 _diffrn_reflns_l_min -2 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 24.9939 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 0.09597 _diffrn_orient_matrix_12 0.01833 _diffrn_orient_matrix_13 0.05496 _diffrn_orient_matrix_21 0.06234 _diffrn_orient_matrix_22 -0.06373 _diffrn_orient_matrix_23 0.00448 _diffrn_orient_matrix_31 0.02113 _diffrn_orient_matrix_32 0.00288 _diffrn_orient_matrix_33 -0.14326 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 18 0.003 0.002 'International Tables' H 0 22 0.000 0.000 'International Tables' N 0 8 0.006 0.003 'International Tables' O 0 2 0.011 0.006 'International Tables' Cl 0 12 0.148 0.159 'International Tables' Sb 0 2 -0.587 1.546 '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 Sb 0.15106(6) 0.17881(3) 0.15069(7) 0.0336 Uij ? ? Cl1 0.1356(3) 0.2629(1) 0.4627(3) 0.0540 Uij ? ? Cl2 0.1768(3) 0.0955(2) -0.1568(3) 0.0585 Uij ? ? Cl3 0.2368(3) 0.2903(2) 0.0144(3) 0.0549 Uij ? ? Cl4 0.0568(3) 0.0728(1) 0.2825(4) 0.0565 Uij ? ? Cl5 -0.1073(2) 0.2601(2) 0.0297(4) 0.0590 Uij ? ? Cl6 0.4111(2) 0.1034(2) 0.2788(4) 0.0598 Uij ? ? O 0.5363(6) 0.3824(4) 0.0437(8) 0.0480 Uij ? ? N1 0.5041(7) 0.3758(4) 0.2186(10) 0.0378 Uij ? ? N2 0.5680(7) 0.3062(4) 0.3317(9) 0.0381 Uij ? ? N3 0.4980(7) 0.3233(4) 0.5066(9) 0.0356 Uij ? ? N4 0.6267(7) 0.1894(4) 0.6777(9) 0.0384 Uij ? ? C1 0.3901(8) 0.4408(5) 0.315(1) 0.0369 Uij ? ? C2 0.2965(9) 0.5228(5) 0.247(1) 0.0454 Uij ? ? C3 0.1974(10) 0.5681(6) 0.380(1) 0.0506 Uij ? ? C4 0.1908(10) 0.5350(6) 0.567(1) 0.0532 Uij ? ? C5 0.2846(9) 0.4524(6) 0.631(1) 0.0433 Uij ? ? C6 0.3862(8) 0.4071(5) 0.501(1) 0.0351 Uij ? ? C7 0.5216(8) 0.2645(5) 0.655(1) 0.0363 Uij ? ? C8 0.7533(10) 0.1528(6) 0.551(1) 0.0543 Uij ? ? C9 0.624(1) 0.1328(6) 0.844(1) 0.0548 Uij ? ? H1 0.2959 0.5428 0.1048 0.0728 Uij ? ? H2 0.1289 0.6244 0.3410 0.0728 Uij ? ? H3 0.1202 0.5701 0.6539 0.0728 Uij ? ? H4 0.2674 0.4368 0.7558 0.0728 Uij ? ? H5 0.4683 0.2902 0.7931 0.0728 Uij ? ? H6 0.8165 0.1921 0.5593 0.0659 Uij ? ? H7 0.7093 0.1464 0.4120 0.0654 Uij ? ? H8 0.8147 0.0965 0.5999 0.0654 Uij ? ? H9 0.6175 0.0743 0.7789 0.0728 Uij ? ? H10 0.7341 0.1127 0.9029 0.0728 Uij ? ? H11 0.5888 0.1688 0.9497 0.0728 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 Sb 0.0272(3) 0.0339(3) 0.0414(3) -0.0102(2) 0.0053(2) 0.0037(2) Cl1 0.061(1) 0.051(1) 0.049(1) -0.013(1) 0.013(1) -0.0064(10) Cl2 0.068(2) 0.060(1) 0.051(1) -0.025(1) 0.013(1) -0.011(1) Cl3 0.063(1) 0.055(1) 0.060(1) -0.033(1) 0.014(1) 0.007(1) Cl4 0.056(1) 0.043(1) 0.080(1) -0.016(1) 0.027(1) 0.010(1) Cl5 0.035(1) 0.052(1) 0.083(2) -0.0060(10) -0.007(1) 0.011(1) Cl6 0.031(1) 0.059(1) 0.081(2) -0.004(1) -0.004(1) 0.002(1) O 0.044(3) 0.055(4) 0.049(3) -0.010(3) 0.018(3) 0.011(3) N1 0.031(4) 0.039(4) 0.048(4) -0.015(3) 0.008(3) 0.003(3) N2 0.031(4) 0.038(4) 0.045(4) -0.007(3) 0.010(3) 0.006(3) N3 0.032(4) 0.037(4) 0.038(3) -0.009(3) 0.007(3) 0.005(3) N4 0.032(4) 0.039(4) 0.043(3) -0.007(3) 0.007(3) 0.004(3) C1 0.029(4) 0.042(4) 0.044(4) -0.016(4) 0.003(3) 0.003(3) C2 0.039(5) 0.037(5) 0.062(5) -0.011(4) 0.006(4) 0.013(4) C3 0.046(5) 0.038(5) 0.065(5) -0.004(4) 0.006(4) 0.013(4) C4 0.045(5) 0.040(5) 0.070(6) 0.002(4) 0.018(4) 0.004(4) C5 0.042(5) 0.044(5) 0.041(4) -0.005(4) 0.008(4) 0.005(4) C6 0.027(4) 0.031(4) 0.048(4) -0.011(3) 0.003(3) 0.005(3) C7 0.031(4) 0.039(4) 0.041(4) -0.014(4) 0.006(3) 0.001(3) C8 0.039(5) 0.054(6) 0.065(5) 0.005(4) 0.020(4) 0.012(4) C9 0.056(6) 0.040(5) 0.070(6) -0.010(4) 0.013(5) 0.016(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 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2247 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0570 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 2.300 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 1.76770 _refine_diff_density_max -1.55960 #------------------------------------------------------------------------------ _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 Sb Cl(1) 2.365(2) ? ? yes Sb Cl(2) 2.339(2) ? ? yes Sb Cl(3) 2.391(2) ? ? yes Sb Cl(4) 2.351(2) ? ? yes Sb Cl(5) 2.367(2) ? ? yes Sb Cl(6) 2.366(2) ? ? yes O N(1) 1.251(7) ? ? yes N(1) N(2) 1.309(8) ? ? yes N(1) C(1) 1.423(10) ? ? yes N(2) N(3) 1.375(8) ? ? yes N(3) C(6) 1.413(9) ? ? yes N(3) C(7) 1.348(9) ? ? yes N(4) C(7) 1.289(10) ? ? yes N(4) C(8) 1.484(10) ? ? yes N(4) C(9) 1.470(10) ? ? yes C(1) C(2) 1.39(1) ? ? yes C(1) C(6) 1.379(10) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(3) C(4) 1.39(1) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(5) C(6) 1.37(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) Sb Cl(2) 177.73(8) ? ? ? yes Cl(1) Sb Cl(3) 88.62(8) ? ? ? yes Cl(1) Sb Cl(4) 90.93(8) ? ? ? yes Cl(1) Sb Cl(5) 89.41(8) ? ? ? yes Cl(1) Sb Cl(6) 88.59(8) ? ? ? yes Cl(2) Sb Cl(3) 90.16(8) ? ? ? yes Cl(2) Sb Cl(4) 90.36(8) ? ? ? yes Cl(2) Sb Cl(5) 92.45(9) ? ? ? yes Cl(2) Sb Cl(6) 89.51(9) ? ? ? yes Cl(3) Sb Cl(4) 177.76(8) ? ? ? yes Cl(3) Sb Cl(5) 87.90(8) ? ? ? yes Cl(3) Sb Cl(6) 90.54(9) ? ? ? yes Cl(4) Sb Cl(5) 89.90(8) ? ? ? yes Cl(4) Sb Cl(6) 91.65(9) ? ? ? yes Cl(5) Sb Cl(6) 177.49(8) ? ? ? yes O N(1) N(2) 123.7(6) ? ? ? yes O N(1) C(1) 124.6(6) ? ? ? yes N(2) N(1) C(1) 111.7(6) ? ? ? yes N(1) N(2) N(3) 105.8(6) ? ? ? yes N(2) N(3) C(6) 111.3(5) ? ? ? yes N(2) N(3) C(7) 124.5(6) ? ? ? yes C(6) N(3) C(7) 123.9(6) ? ? ? yes C(7) N(4) C(8) 126.4(7) ? ? ? yes C(7) N(4) C(9) 118.3(6) ? ? ? yes C(8) N(4) C(9) 115.3(6) ? ? ? yes N(1) C(1) C(2) 129.7(7) ? ? ? yes N(1) C(1) C(6) 106.5(6) ? ? ? yes C(2) C(1) C(6) 123.7(7) ? ? ? yes C(1) C(2) C(3) 114.2(7) ? ? ? yes C(2) C(3) C(4) 123.0(8) ? ? ? yes C(3) C(4) C(5) 121.7(8) ? ? ? yes C(4) C(5) C(6) 115.9(7) ? ? ? yes N(3) C(6) C(1) 104.7(6) ? ? ? yes N(3) C(6) C(5) 133.8(7) ? ? ? yes C(1) C(6) C(5) 121.5(7) ? ? ? yes N(3) C(7) N(4) 127.7(7) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;