Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 ---------- X-Sun-Charset: us-ascii X-Sun-Content-Lines: 563 data_TCH1 _database_code_CSD 164932 #-------------------------------------------------------------------------- _audit_creation_date '1999-11-09' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #-------------------------------------------------------------------------- _publ_requested_journal ' Journal of the Chemical Society, Dalton Transactions' _journal_coden_Cambridge 186 _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_contact_author_name ' Dr Trevor W. Hambley' _publ_contact_author ; Dr Trevor W. Hambley School of Chemistry University of Sydney ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 61-2-9351-2830 ' _publ_contact_author_fax ' 61-2-9351-3329 ' _publ_contact_author_email ' t.hambley@chem.usyd.edu.au ' loop_ _publ_author_name _publ_author_address 'S. Tsuey Cham' ; School of Chemistry University of Sydney ; 'Connie I. Diakos' ; School of Chemistry University of Sydney ; 'Leanne T. Ellis' ; School of Chemistry University of Sydney ; 'Ronald R. Fenton' ; School of Chemistry University of Sydney ; 'Vivienne P. Munk' ; School of Chemistry University of Sydney ; 'Barbara A. Messerle' ; School of Chemistry University of New South Wales ; 'Trevor W. Hambley' ; School of Chemistry University of Sydney ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. de Meulenaer, J. & Tompa, H. (1965), Acta Cryst. 19, 1014. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #-------------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #-------------------------------------------------------------------------- _cell_length_a 7.690(1) _cell_length_b 8.358(2) _cell_length_c 12.149(4) _cell_angle_alpha 70.00(2) _cell_angle_beta 80.87(2) _cell_angle_gamma 83.58(2) _cell_volume 723.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #-------------------------------------------------------------------------- #--- _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 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.00 _exptl_crystal_size_mid 0.00 _exptl_crystal_size_min 0.00 _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 453.28 _chemical_formula_analytical ? _chemical_formula_sum 'C9 H21 Cl2 N3 O Pt ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 432.00 _exptl_absorpt_coefficient_mu 10.020 _exptl_absorpt_correction_type ; analytical (de Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_max 0.448 _exptl_absorpt_correction_T_min 0.346 _exptl_special_details ; ? ; #--------------------------------------------------------------------------= #--- _diffrn_special_details ; ? ; _diffrn_ambient_temperature 273.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'unknown' _diffrn_measurement_method ? _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 2663 _reflns_number_total 2531 _reflns_number_observed 2411 _reflns_observed_criterion >2.50\s(I) _diffrn_reflns_av_R_equivalents 0.00928 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.02040 _diffrn_orient_matrix_UB_12 0.11983 _diffrn_orient_matrix_UB_13 0.00099 _diffrn_orient_matrix_UB_21 -0.01590 _diffrn_orient_matrix_UB_22 -0.04347 _diffrn_orient_matrix_UB_23 0.08839 _diffrn_orient_matrix_UB_31 0.12927 _diffrn_orient_matrix_UB_32 0.00549 _diffrn_orient_matrix_UB_33 -0.00059 #--------------------------------------------------------------------------= #--- 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 Pt 0 2 -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 18 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 6 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 42 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 2 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------= #--- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.09724(3) 0.44841(3) 0.12674(2) 0.02820(7) 1.000 . Uani d ? Cl(1) 0.3027(2) 0.6557(2) 0.0585(1) 0.0435(4) 1.000 . Uani d ? Cl(2) -0.1031(2) 0.6153(2) 0.2109(1) 0.0424(4) 1.000 . Uani d ? O(1) -0.3635(6) 0.2419(6) 0.3770(5) 0.070(2) 1.000 . Uani d ? N(1) 0.2686(7) 0.3058(6) 0.0457(5) 0.036(2) 1.000 . Uani d ? N(2) -0.0846(6) 0.2685(6) 0.1825(5) 0.035(1) 1.000 . Uani d ? N(3) -0.6135(6) 0.3728(7) 0.4393(5) 0.045(2) 1.000 . Uani d ? C(1) 0.2802(8) 0.1159(7) 0.0968(6) 0.040(2) 1.000 . Uani d ? C(2) 0.0970(8) 0.0529(8) 0.1104(6) 0.043(2) 1.000 . Uani d ? C(3) -0.0244(8) 0.0827(7) 0.2130(6) 0.038(2) 1.000 . Uani d ? C(4) 0.0575(10) 0.0199(9) 0.3281(6) 0.051(2) 1.000 . Uani d ? C(5) 0.2395(10) 0.0812(10) 0.3149(6) 0.054(2) 1.000 . Uani d ? C(6) 0.3602(10) 0.0524(9) 0.2128(7) 0.054(2) 1.000 . Uani d ? C(7) -0.4772(10) 0.3582(9) 0.3632(6) 0.058(2) 1.000 . Uani d ? C(8) -0.746(1) 0.514(1) 0.4163(8) 0.085(3) 1.000 . Uani d ? C(9) -0.644(1) 0.240(1) 0.5533(7) 0.078(3) 1.000 . Uani d ? H(1) 0.246(7) 0.341(6) -0.042(5) 0.04(2) 1.000 . Uiso d ? H(2) 0.350(7) 0.338(7) 0.050(5) 0.03(2) 1.000 . Uiso d ? H(3) -0.140(8) 0.276(7) 0.242(5) 0.04(2) 1.000 . Uiso d ? H(4) -0.165(8) 0.303(7) 0.107(6) 0.06(2) 1.000 . Uiso d ? H(5) 0.352(7) 0.078(6) 0.049(5) 0.03(2) 1.000 . Uiso d ? H(6) 0.032(8) 0.113(7) 0.021(6) 0.06(2) 1.000 . Uiso d ? H(7) 0.113(9) -0.053(8) 0.119(6) 0.07(2) 1.000 . Uiso d ? H(8) -0.128(7) 0.022(6) 0.225(5) 0.03(1) 1.000 . Uiso d ? H(9) -0.046(8) 0.044(7) 0.396(5) 0.06(2) 1.000 . Uiso d ? H(10) 0.076(8) -0.099(8) 0.339(5) 0.05(2) 1.000 . Uiso d ? H(11) 0.232(7) 0.202(7) 0.309(5) 0.04(2) 1.000 . Uiso d ? H(12) 0.303(8) 0.015(8) 0.388(6) 0.06(2) 1.000 . Uiso d ? H(13) 0.392(8) -0.068(8) 0.215(6) 0.06(2) 1.000 . Uiso d ? H(14) 0.464(9) 0.111(8) 0.205(6) 0.06(2) 1.000 . Uiso d ? H(15) -0.4656 0.4480 0.2896 0.070 1.000 . Uiso c ? H(16) -0.6921 0.6168 0.3972 0.103 1.000 . Uiso c ? H(17) -0.8035 0.5138 0.3523 0.103 1.000 . Uiso c ? H(18) -0.8307 0.4981 0.4849 0.103 1.000 . Uiso c ? H(19) -0.7461 0.2719 0.5978 0.093 1.000 . Uiso c ? H(20) -0.6618 0.1364 0.5411 0.093 1.000 . Uiso c ? H(21) -0.5450 0.2240 0.5939 0.093 1.000 . Uiso c ? 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 Pt(1) 0.0269(1) 0.0255(1) 0.0280(2) -0.00374(8) 0.00038(9) -0.00450(10) Cl(1) 0.0340(8) 0.0329(8) 0.060(1) -0.0106(6) 0.0047(7) -0.0127(7) Cl(2) 0.0410(9) 0.0389(8) 0.0451(9) -0.0021(6) 0.0063(7) -0.0164(7) O(1) 0.052(3) 0.066(3) 0.070(4) 0.002(3) 0.022(3) -0.010(3) N(1) 0.031(3) 0.031(3) 0.044(4) -0.005(2) 0.001(3) -0.011(2) N(2) 0.033(3) 0.033(3) 0.033(3) -0.005(2) 0.004(2) -0.006(2) N(3) 0.036(3) 0.051(3) 0.043(3) 0.002(2) -0.001(3) -0.011(3) C(1) 0.040(4) 0.030(3) 0.045(4) 0.000(3) 0.005(3) -0.012(3) C(2) 0.045(4) 0.030(3) 0.053(4) -0.007(3) -0.002(3) -0.015(3) C(3) 0.037(4) 0.026(3) 0.047(4) -0.010(3) -0.004(3) -0.005(3) C(4) 0.057(5) 0.042(4) 0.041(4) -0.003(3) -0.005(3) 0.004(3) C(5) 0.061(5) 0.048(4) 0.045(4) 0.004(4) -0.021(4) -0.002(4) C(6) 0.043(4) 0.044(4) 0.064(5) 0.007(3) -0.018(4) -0.005(4) C(7) 0.054(5) 0.064(5) 0.046(5) -0.014(4) 0.006(4) -0.006(4) C(8) 0.084(6) 0.087(6) 0.085(7) 0.030(5) -0.026(5) -0.037(5) C(9) 0.075(6) 0.076(6) 0.063(6) -0.010(4) 0.025(4) -0.009(4) #-------------------------------------------------------------------------- _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w == 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_extinction_coef 0.0000128(3) _refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2411 _refine_ls_number_parameters 202 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_obs 0.0229 _refine_ls_wR_factor_all 0.0232 _refine_ls_wR_factor_obs 0.0232 _refine_ls_goodness_of_fit_all 2.758 _refine_ls_goodness_of_fit_obs 2.758 _refine_ls_shift/esd_max 0.0056 _refine_ls_shift/esd_mean 0.0353 _refine_diff_density_min -1.13 _refine_diff_density_max 1.88 #--------------------------------------------------------------------------= #--- _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 Pt(1) Cl(1) 2.323(1) . . yes Pt(1) Cl(2) 2.315(1) . . yes Pt(1) N(1) 2.041(5) . . yes Pt(1) N(2) 2.037(5) . . yes O(1) C(7) 1.218(8) . . yes N(1) C(1) 1.492(7) . . yes N(1) H(1) 1.04(6) . . no N(1) H(2) 0.72(5) . . no N(2) C(3) 1.504(7) . . yes N(2) H(3) 0.80(6) . . no N(2) H(4) 1.12(6) . . no N(3) C(7) 1.308(8) . . yes N(3) C(8) 1.446(8) . . yes N(3) C(9) 1.452(9) . . yes C(1) C(2) 1.524(8) . . yes C(1) C(6) 1.528(9) . . yes C(1) H(5) 0.85(5) . . no C(2) C(3) 1.510(9) . . yes C(2) H(6) 1.19(6) . . no C(2) H(7) 0.85(6) . . no C(3) C(4) 1.527(9) . . yes C(3) H(8) 0.96(5) . . no C(4) C(5) 1.510(9) . . yes C(4) H(9) 1.11(6) . . no C(4) H(10) 0.95(6) . . no C(5) C(6) 1.50(1) . . yes C(5) H(11) 0.98(5) . . no C(5) H(12) 1.04(6) . . no C(6) H(13) 1.00(6) . . no C(6) H(14) 0.96(6) . . no C(7) H(15) 0.95 . . no C(8) H(16) 0.94 . . no C(8) H(17) 0.95 . . no C(8) H(18) 0.95 . . no C(9) H(19) 0.95 . . no C(9) H(20) 0.95 . . no C(9) H(21) 0.94 . . no #--------------------------------------------------------------------------= #--- 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) Pt(1) Cl(2) 92.65(5) . . . yes Cl(1) Pt(1) N(1) 87.4(1) . . . yes Cl(1) Pt(1) N(2) 178.6(2) . . . yes Cl(2) Pt(1) N(1) 177.4(2) . . . yes Cl(2) Pt(1) N(2) 87.6(1) . . . yes N(1) Pt(1) N(2) 92.2(2) . . . yes Pt(1) N(1) C(1) 120.6(4) . . . yes Pt(1) N(1) H(1) 108(2) . . . no Pt(1) N(1) H(2) 98(4) . . . no C(1) N(1) H(1) 108(2) . . . no C(1) N(1) H(2) 108(4) . . . no H(1) N(1) H(2) 111(5) . . . no Pt(1) N(2) C(3) 119.7(4) . . . yes Pt(1) N(2) H(3) 107(4) . . . no Pt(1) N(2) H(4) 103(3) . . . no C(3) N(2) H(3) 104(4) . . . no C(3) N(2) H(4) 108(2) . . . no H(3) N(2) H(4) 113(5) . . . no C(7) N(3) C(8) 124.0(6) . . . yes C(7) N(3) C(9) 120.3(6) . . . yes C(8) N(3) C(9) 115.7(6) . . . yes N(1) C(1) C(2) 108.4(5) . . . yes N(1) C(1) C(6) 112.1(5) . . . yes N(1) C(1) H(5) 107(3) . . . no C(2) C(1) C(6) 112.5(6) . . . yes C(2) C(1) H(5) 110(3) . . . no C(6) C(1) H(5) 105(3) . . . no C(1) C(2) C(3) 112.8(5) . . . yes C(1) C(2) H(6) 111(2) . . . no C(1) C(2) H(7) 105(4) . . . no C(3) C(2) H(6) 110(2) . . . no C(3) C(2) H(7) 111(4) . . . no H(6) C(2) H(7) 104(5) . . . no N(2) C(3) C(2) 110.0(5) . . . yes N(2) C(3) C(4) 110.9(5) . . . yes N(2) C(3) H(8) 106(2) . . . no C(2) C(3) C(4) 113.3(6) . . . yes C(2) C(3) H(8) 107(3) . . . no C(4) C(3) H(8) 108(3) . . . no C(3) C(4) C(5) 113.2(6) . . . yes C(3) C(4) H(9) 105(3) . . . no C(3) C(4) H(10) 100(3) . . . no C(5) C(4) H(9) 119(3) . . . no C(5) C(4) H(10) 105(3) . . . no H(9) C(4) H(10) 111(4) . . . no C(4) C(5) C(6) 113.1(6) . . . yes C(4) C(5) H(11) 110(3) . . . no C(4) C(5) H(12) 111(3) . . . no C(6) C(5) H(11) 110(3) . . . no C(6) C(5) H(12) 104(3) . . . no H(11) C(5) H(12) 106(4) . . . no C(1) C(6) C(5) 113.8(6) . . . yes C(1) C(6) H(13) 97(3) . . . no C(1) C(6) H(14) 110(4) . . . no C(5) C(6) H(13) 118(3) . . . no C(5) C(6) H(14) 105(4) . . . no H(13) C(6) H(14) 111(5) . . . no O(1) C(7) N(3) 126.8(7) . . . yes O(1) C(7) H(15) 116.7 . . . no N(3) C(7) H(15) 116.5 . . . no N(3) C(8) H(16) 109.9 . . . no N(3) C(8) H(17) 108.8 . . . no N(3) C(8) H(18) 109.1 . . . no H(16) C(8) H(17) 110.2 . . . no H(16) C(8) H(18) 110.1 . . . no H(17) C(8) H(18) 108.7 . . . no N(3) C(9) H(19) 109.3 . . . no N(3) C(9) H(20) 108.8 . . . no N(3) C(9) H(21) 109.7 . . . no H(19) C(9) H(20) 109.2 . . . no H(19) C(9) H(21) 110.2 . . . no H(20) C(9) H(21) 109.6 . . . no #--------------------------------------------------------------------------= #--- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt(1) Pt(1) 3.4378(4) . 2_565 no Cl(1) N(1) 3.349(5) . 2_665 no Cl(1) N(2) 3.440(6) . 2_565 no Cl(2) N(1) 3.382(6) . 2_565 no O(1) N(2) 2.893(7) . . no O(1) C(3) 3.454(8) . . no C(5) C(7) 3.59(1) . 1_655 no #--------------------------------------------------------------------------= #--- loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Pt(1) N(1) C(1) C(2) . . . . 56.1(7) no Pt(1) N(1) C(1) C(6) . . . . -68.7(6) no Pt(1) N(2) C(3) C(2) . . . . -54.6(6) no Pt(1) N(2) C(3) C(4) . . . . 71.5(6) no Cl(1) Pt(1) N(1) C(1) . . . . 147.1(5) no Cl(1) Pt(1) N(2) C(3) . . . . 109(5) no Cl(2) Pt(1) N(1) C(1) . . . . -120(3) no Cl(2) Pt(1) N(2) C(3) . . . . -149.9(4) no O(1) C(7) N(3) C(8) . . . . -178.9(7) no O(1) C(7) N(3) C(9) . . . . -1(1) no N(1) Pt(1) N(2) C(3) . . . . 32.7(5) no N(1) C(1) C(2) C(3) . . . . -74.9(7) no N(1) C(1) C(6) C(5) . . . . 72.7(8) no N(2) Pt(1) N(1) C(1) . . . . -34.2(5) no N(2) C(3) C(2) C(1) . . . . 74.8(7) no N(2) C(3) C(4) C(5) . . . . -74.5(7) no C(1) C(2) C(3) C(4) . . . . -49.9(7) no C(1) C(6) C(5) C(4) . . . . 49.8(8) no C(2) C(1) C(6) C(5) . . . . -49.9(8) no C(2) C(3) C(4) C(5) . . . . 49.8(8) no C(3) C(2) C(1) C(6) . . . . 49.7(7) no C(3) C(4) C(5) C(6) . . . . -49.4(8) no #------------------------------------------------------