# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Iwona Lakomska' _publ_contact_author_email DZIUBEK@UMK.PL _publ_section_title ; Mono- and dinucler platinum(II) compounds with 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine. Structure, cytotoxic activity and reaction with 5'-GMP ; loop_ _publ_author_name 'Iwona Lakomska' 'Huub Kooijman' 'Jan Reedijk' 'Wei-Zheng Shen' 'A Spek' # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF # Attachment 'iwona_spek_publ.cif' # CIF-file generated for s2166a R = 0.03 #============================================================================== data_s2166a _database_code_depnum_ccdc_archive 'CCDC 728067' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_formula_moiety 'C14 H16 Cl2 N8 Pt' _chemical_formula_sum 'C14 H16 Cl2 N8 Pt' _chemical_formula_weight 562.33 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 8.2733(12) _cell_length_b 9.3493(12) _cell_length_c 12.7502(12) _cell_angle_alpha 78.721(10) _cell_angle_beta 75.241(10) _cell_angle_gamma 72.229(10) _cell_volume 900.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 681 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 20.0 _cell_special_details ; Least Squares Treatment of 25 SET4 setting angles. ; _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 8.101 # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type refdelf # Example: '(North et al., 1968)' _exptl_absorpt_process_details PLATON/DELABS _exptl_absorpt_correction_T_min 0.394 _exptl_absorpt_correction_T_max 0.912 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean 18.4 # number of measured reflections (redundant set) _diffrn_reflns_number 11275 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 4100 # number of observed reflections (> n sig(I)) _reflns_number_gt 3840 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Locally modified CAD4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement DENZO' _computing_data_reduction DENZO _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+1.0765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 4100 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0651 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.029 _refine_diff_density_min -1.963 _refine_diff_density_rms 0.131 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pt1 Pt Uani 0.28878(2) -0.28351(1) 0.77959(1) 1.000 0.0259(1) . . Cl1 Cl Uani 0.32832(14) -0.49467(12) 0.90659(10) 1.000 0.0396(3) . . Cl2 Cl Uani 0.26740(15) -0.42716(12) 0.65951(10) 1.000 0.0407(3) . . N1 N Uani 0.1379(4) 0.0577(4) 0.5297(3) 1.000 0.0320(10) . . N3 N Uani 0.2575(4) -0.1028(3) 0.6629(3) 1.000 0.0245(9) . . N4 N Uani 0.4602(4) 0.0317(4) 0.6750(2) 1.000 0.0251(9) . . N8 N Uani 0.2639(4) 0.1071(4) 0.5532(2) 1.000 0.0255(9) . . N11 N Uani 0.3463(4) -0.1010(4) 1.0411(3) 1.000 0.0305(10) . . N31 N Uani 0.2906(4) -0.1559(3) 0.8903(3) 1.000 0.0252(9) . . N41 N Uani 0.1007(4) 0.0887(3) 0.8397(3) 1.000 0.0249(9) . . N81 N Uani 0.2379(4) 0.0224(4) 0.9923(3) 1.000 0.0264(9) . . C2 C Uani 0.1411(5) -0.0670(4) 0.5980(3) 1.000 0.0278(11) . . C3A C Uani 0.3365(4) 0.0096(4) 0.6348(3) 1.000 0.0227(9) . . C5 C Uani 0.5092(5) 0.1574(4) 0.6308(3) 1.000 0.0265(11) . . C6 C Uani 0.4404(5) 0.2584(4) 0.5443(3) 1.000 0.0291(11) . . C7 C Uani 0.3164(5) 0.2327(4) 0.5035(3) 1.000 0.0281(11) . . C9 C Uani 0.6387(6) 0.1951(5) 0.6768(4) 1.000 0.0367(12) . . C10 C Uani 0.2369(7) 0.3260(6) 0.4112(4) 1.000 0.0439(16) . . C21 C Uani 0.3727(5) -0.2033(5) 0.9765(3) 1.000 0.0302(11) . . C31A C Uani 0.2037(4) -0.0105(4) 0.9018(3) 1.000 0.0239(10) . . C51 C Uani 0.0363(5) 0.2272(4) 0.8693(3) 1.000 0.0281(10) . . C61 C Uani 0.0666(5) 0.2653(5) 0.9629(4) 1.000 0.0326(11) . . C71 C Uani 0.1678(5) 0.1611(5) 1.0279(4) 1.000 0.0311(11) . . C91 C Uani -0.0714(6) 0.3457(5) 0.7980(4) 1.000 0.0381(14) . . C101 C Uani 0.1995(6) 0.1840(6) 1.1316(4) 1.000 0.0432(16) . . H2 H Uiso 0.06640 -0.12830 0.60170 1.000 0.0330 calc R H6 H Uiso 0.48160 0.34520 0.51440 1.000 0.0350 calc R H9A H Uiso 0.68170 0.11120 0.73090 1.000 0.0550 calc R H9B H Uiso 0.58300 0.28730 0.71200 1.000 0.0550 calc R H9C H Uiso 0.73590 0.21150 0.61760 1.000 0.0550 calc R H10A H Uiso 0.26620 0.26580 0.35080 1.000 0.0660 calc R H10B H Uiso 0.28170 0.41530 0.38620 1.000 0.0660 calc R H10C H Uiso 0.11050 0.35840 0.43590 1.000 0.0660 calc R H10D H Uiso 0.12990 0.13390 1.19330 1.000 0.0650 calc R H10E H Uiso 0.16680 0.29270 1.13710 1.000 0.0650 calc R H10F H Uiso 0.32280 0.14080 1.13320 1.000 0.0650 calc R H21 H Uiso 0.44400 -0.30340 0.98880 1.000 0.0360 calc R H61 H Uiso 0.01560 0.36530 0.98140 1.000 0.0390 calc R H91A H Uiso -0.00580 0.41790 0.75760 1.000 0.0570 calc R H91B H Uiso -0.17880 0.39940 0.84380 1.000 0.0570 calc R H91C H Uiso -0.09980 0.29700 0.74620 1.000 0.0570 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0228(1) 0.0216(1) 0.0323(1) -0.0032(1) -0.0036(1) -0.0062(1) Cl1 0.0392(5) 0.0228(5) 0.0512(6) 0.0055(4) -0.0106(5) -0.0057(4) Cl2 0.0473(6) 0.0338(5) 0.0448(6) -0.0140(4) -0.0003(5) -0.0187(4) N1 0.0304(16) 0.0399(19) 0.0313(18) -0.0042(14) -0.0116(14) -0.0135(14) N3 0.0244(14) 0.0239(15) 0.0273(16) -0.0046(12) -0.0063(12) -0.0080(12) N4 0.0230(14) 0.0291(16) 0.0248(15) -0.0032(12) -0.0073(12) -0.0075(12) N8 0.0253(14) 0.0285(16) 0.0235(15) -0.0035(12) -0.0059(12) -0.0077(12) N11 0.0266(15) 0.0339(18) 0.0283(17) 0.0035(13) -0.0084(13) -0.0068(13) N31 0.0235(14) 0.0212(15) 0.0268(16) 0.0012(12) -0.0051(12) -0.0029(11) N41 0.0216(14) 0.0227(15) 0.0271(16) -0.0013(12) -0.0021(12) -0.0048(11) N81 0.0229(14) 0.0274(16) 0.0270(16) -0.0007(12) -0.0039(12) -0.0069(12) C2 0.0249(17) 0.034(2) 0.0291(19) -0.0061(16) -0.0095(14) -0.0103(15) C3A 0.0218(15) 0.0239(17) 0.0214(17) -0.0041(13) -0.0036(13) -0.0046(13) C5 0.0284(18) 0.0302(19) 0.0231(18) -0.0067(14) -0.0038(14) -0.0105(15) C6 0.0338(19) 0.0238(18) 0.029(2) -0.0026(15) -0.0027(15) -0.0103(15) C7 0.0328(19) 0.0278(19) 0.0228(18) -0.0008(14) -0.0064(15) -0.0077(15) C9 0.043(2) 0.045(2) 0.034(2) -0.0033(18) -0.0150(18) -0.0242(19) C10 0.052(3) 0.042(3) 0.039(2) 0.011(2) -0.020(2) -0.016(2) C21 0.0256(17) 0.031(2) 0.032(2) 0.0024(15) -0.0078(15) -0.0073(15) C31A 0.0213(15) 0.0259(18) 0.0249(18) -0.0008(14) -0.0044(13) -0.0088(13) C51 0.0228(16) 0.0245(18) 0.033(2) -0.0016(15) -0.0003(15) -0.0063(14) C61 0.0269(18) 0.028(2) 0.041(2) -0.0070(17) -0.0010(16) -0.0082(15) C71 0.0243(18) 0.032(2) 0.037(2) -0.0086(17) 0.0005(16) -0.0107(15) C91 0.037(2) 0.025(2) 0.047(3) 0.0033(17) -0.0132(19) -0.0019(16) C101 0.038(2) 0.054(3) 0.041(3) -0.017(2) -0.0077(19) -0.011(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; 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 Pt1 Cl1 2.2916(12) . . yes Pt1 Cl2 2.2949(12) . . yes Pt1 N3 2.020(3) . . yes Pt1 N31 2.024(3) . . yes N1 N8 1.377(5) . . yes N1 C2 1.309(5) . . yes N3 C2 1.351(5) . . yes N3 C3A 1.346(5) . . yes N4 C3A 1.338(5) . . yes N4 C5 1.334(5) . . yes N8 C3A 1.374(5) . . yes N8 C7 1.360(5) . . yes N11 N81 1.376(5) . . yes N11 C21 1.315(6) . . yes N31 C21 1.368(5) . . yes N31 C31A 1.347(5) . . yes N41 C31A 1.337(5) . . yes N41 C51 1.331(5) . . yes N81 C31A 1.366(5) . . yes N81 C71 1.364(6) . . yes C5 C6 1.420(5) . . no C5 C9 1.499(7) . . no C6 C7 1.361(6) . . no C7 C10 1.490(7) . . no C51 C61 1.410(6) . . no C51 C91 1.505(6) . . no C61 C71 1.370(7) . . no C71 C101 1.478(7) . . no C2 H2 0.9500 . . no C6 H6 0.9500 . . no C9 H9A 0.9800 . . no C9 H9B 0.9800 . . no C9 H9C 0.9800 . . no C10 H10A 0.9800 . . no C10 H10B 0.9800 . . no C10 H10C 0.9800 . . no C21 H21 0.9500 . . no C61 H61 0.9500 . . no C91 H91A 0.9800 . . no C91 H91B 0.9800 . . no C91 H91C 0.9800 . . no C101 H10D 0.9800 . . no C101 H10E 0.9800 . . no C101 H10F 0.9800 . . 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 Cl1 Pt1 Cl2 89.43(4) . . . yes Cl1 Pt1 N3 177.72(10) . . . yes Cl1 Pt1 N31 89.98(10) . . . yes Cl2 Pt1 N3 88.49(10) . . . yes Cl2 Pt1 N31 176.12(11) . . . yes N3 Pt1 N31 92.16(13) . . . yes N8 N1 C2 102.0(3) . . . yes Pt1 N3 C2 125.2(3) . . . yes Pt1 N3 C3A 129.9(3) . . . yes C2 N3 C3A 104.9(3) . . . yes C3A N4 C5 115.3(3) . . . yes N1 N8 C3A 110.9(3) . . . yes N1 N8 C7 126.6(3) . . . yes C3A N8 C7 122.5(3) . . . yes N81 N11 C21 101.6(3) . . . yes Pt1 N31 C21 126.9(3) . . . yes Pt1 N31 C31A 129.0(3) . . . yes C21 N31 C31A 104.0(3) . . . yes C31A N41 C51 115.4(3) . . . yes N11 N81 C31A 111.4(3) . . . yes N11 N81 C71 126.1(4) . . . yes C31A N81 C71 122.4(4) . . . yes N1 C2 N3 115.6(4) . . . yes N3 C3A N4 129.9(3) . . . yes N3 C3A N8 106.7(3) . . . yes N4 C3A N8 123.4(3) . . . yes N4 C5 C6 122.7(4) . . . yes N4 C5 C9 118.3(3) . . . yes C6 C5 C9 118.9(4) . . . no C5 C6 C7 121.0(4) . . . no N8 C7 C6 114.9(3) . . . yes N8 C7 C10 118.3(4) . . . yes C6 C7 C10 126.8(4) . . . no N11 C21 N31 115.6(4) . . . yes N31 C31A N41 128.9(3) . . . yes N31 C31A N81 107.4(3) . . . yes N41 C31A N81 123.8(3) . . . yes N41 C51 C61 122.6(4) . . . yes N41 C51 C91 117.5(4) . . . yes C61 C51 C91 120.0(4) . . . no C51 C61 C71 121.4(4) . . . no N81 C71 C61 114.4(4) . . . yes N81 C71 C101 119.1(4) . . . yes C61 C71 C101 126.5(4) . . . no N1 C2 H2 122.00 . . . no N3 C2 H2 122.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 119.00 . . . no C5 C9 H9A 109.00 . . . no C5 C9 H9B 109.00 . . . no C5 C9 H9C 109.00 . . . no H9A C9 H9B 109.00 . . . no H9A C9 H9C 110.00 . . . no H9B C9 H9C 109.00 . . . no C7 C10 H10A 110.00 . . . no C7 C10 H10B 109.00 . . . no C7 C10 H10C 109.00 . . . no H10A C10 H10B 109.00 . . . no H10A C10 H10C 109.00 . . . no H10B C10 H10C 109.00 . . . no N11 C21 H21 122.00 . . . no N31 C21 H21 122.00 . . . no C51 C61 H61 119.00 . . . no C71 C61 H61 119.00 . . . no C51 C91 H91A 109.00 . . . no C51 C91 H91B 109.00 . . . no C51 C91 H91C 109.00 . . . no H91A C91 H91B 109.00 . . . no H91A C91 H91C 109.00 . . . no H91B C91 H91C 109.00 . . . no C71 C101 H10D 110.00 . . . no C71 C101 H10E 109.00 . . . no C71 C101 H10F 110.00 . . . no H10D C101 H10E 109.00 . . . no H10D C101 H10F 109.00 . . . no H10E C101 H10F 109.00 . . . 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 Cl2 Pt1 N3 C2 43.2(3) . . . . no Cl2 Pt1 N3 C3A -140.0(3) . . . . no N31 Pt1 N3 C2 -133.0(3) . . . . no N31 Pt1 N3 C3A 43.8(3) . . . . no Cl1 Pt1 N31 C21 27.3(3) . . . . no Cl1 Pt1 N31 C31A -147.5(3) . . . . no N3 Pt1 N31 C21 -151.9(4) . . . . no N3 Pt1 N31 C31A 33.3(4) . . . . no C2 N1 N8 C3A -0.1(4) . . . . no C2 N1 N8 C7 178.7(4) . . . . no N8 N1 C2 N3 -0.2(4) . . . . no Pt1 N3 C2 N1 178.0(3) . . . . no C3A N3 C2 N1 0.5(5) . . . . no Pt1 N3 C3A N4 1.4(6) . . . . no Pt1 N3 C3A N8 -177.8(3) . . . . no C2 N3 C3A N4 178.7(4) . . . . no C2 N3 C3A N8 -0.5(4) . . . . no C5 N4 C3A N3 -178.6(4) . . . . no C5 N4 C3A N8 0.5(5) . . . . no C3A N4 C5 C6 -2.3(5) . . . . no C3A N4 C5 C9 176.0(4) . . . . no N1 N8 C3A N3 0.4(4) . . . . no N1 N8 C3A N4 -178.8(3) . . . . no C7 N8 C3A N3 -178.5(3) . . . . no C7 N8 C3A N4 2.3(6) . . . . no N1 N8 C7 C6 178.3(4) . . . . no N1 N8 C7 C10 -2.4(6) . . . . no C3A N8 C7 C6 -3.0(5) . . . . no C3A N8 C7 C10 176.3(4) . . . . no C21 N11 N81 C31A 0.2(4) . . . . no C21 N11 N81 C71 179.0(4) . . . . no N81 N11 C21 N31 0.1(5) . . . . no Pt1 N31 C21 N11 -176.1(3) . . . . no C31A N31 C21 N11 -0.3(5) . . . . no Pt1 N31 C31A N41 -3.6(6) . . . . no Pt1 N31 C31A N81 176.1(3) . . . . no C21 N31 C31A N41 -179.3(4) . . . . no C21 N31 C31A N81 0.4(4) . . . . no C51 N41 C31A N31 -177.9(4) . . . . no C51 N41 C31A N81 2.5(6) . . . . no C31A N41 C51 C61 -3.2(6) . . . . no C31A N41 C51 C91 176.3(4) . . . . no N11 N81 C31A N31 -0.4(4) . . . . no N11 N81 C31A N41 179.4(4) . . . . no C71 N81 C31A N31 -179.3(4) . . . . no C71 N81 C31A N41 0.5(6) . . . . no N11 N81 C71 C61 178.8(4) . . . . no N11 N81 C71 C101 -3.7(7) . . . . no C31A N81 C71 C61 -2.5(6) . . . . no C31A N81 C71 C101 175.0(4) . . . . no N4 C5 C6 C7 1.5(6) . . . . no C9 C5 C6 C7 -176.8(4) . . . . no C5 C6 C7 N8 1.2(5) . . . . no C5 C6 C7 C10 -178.0(4) . . . . no N41 C51 C61 C71 1.2(7) . . . . no C91 C51 C61 C71 -178.3(4) . . . . no C51 C61 C71 N81 1.7(7) . . . . no C51 C61 C71 C101 -175.6(5) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C2 H2 N1 0.9500 2.5400 3.118(6) 120.00 2_556 yes C6 H6 Cl2 0.9500 2.7900 3.551(4) 138.00 2_656 yes C21 H21 Cl1 0.9500 2.7400 3.175(5) 109.00 . yes C21 H21 Cl1 0.9500 2.6500 3.505(5) 150.00 2_647 yes #===END # Attachment 'iwona_new.cif' data_n _database_code_depnum_ccdc_archive 'CCDC 728846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H32 Cl2 N16 Pt2)2+, 3(N O3)-, H+, 6(H2 O)' _chemical_formula_sum 'C28 H45 Cl2 N19 O15 Pt2' _chemical_formula_weight 1348.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.974(5) _cell_length_b 11.294(2) _cell_length_c 20.317(4) _cell_angle_alpha 90.00 _cell_angle_beta 130.84(3) _cell_angle_gamma 90.00 _cell_volume 4682.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1500 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27.5 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2624 _exptl_absorpt_coefficient_mu 6.165 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'Omega and phi scans' _diffrn_reflns_number 8082 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.1232 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.33 _reflns_number_total 4235 _reflns_number_gt 2397 _reflns_threshold_expression I>2\s(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4235 _refine_ls_number_parameters 303 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 0.888 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.054600(13) 0.44864(3) 0.349976(18) 0.03823(12) Uani 1 1 d . . . Cl1 Cl 0.02588(9) 0.29584(18) 0.39636(12) 0.0474(5) Uani 1 1 d . . . N3 N 0.1157(3) 0.3390(6) 0.3555(4) 0.0387(16) Uani 1 1 d . . . N4 N 0.2164(3) 0.4499(6) 0.4439(4) 0.0482(17) Uani 1 1 d . . . N1 N 0.1512(4) 0.1773(6) 0.3307(4) 0.062(2) Uani 1 1 d . . . N8 N 0.2002(3) 0.2609(6) 0.3802(4) 0.0509(18) Uani 1 1 d . . . N1N N 0.0000 0.9017(16) 0.2500 0.090(5) Uani 1 2 d S . . N4X N -0.0051(3) 0.5662(5) 0.3458(4) 0.0360(15) Uani 1 1 d . . . N8X N -0.0959(3) 0.6959(6) 0.2607(4) 0.0448(17) Uani 1 1 d . . . N1X N 0.1439(3) 0.7285(6) 0.3254(5) 0.0525(19) Uani 1 1 d . . . N2N N 0.1911(7) 0.4581(17) 0.2385(7) 0.119(5) Uani 1 1 d . . . N3X N 0.0816(3) 0.5810(5) 0.3124(4) 0.0356(16) Uani 1 1 d . . . C9X C -0.1318(4) 0.8351(8) 0.3127(6) 0.084(3) Uani 1 1 d . . . H91 H -0.1184 0.8637 0.3668 0.126 Uiso 1 1 calc R . . H92 H -0.1751 0.8024 0.2782 0.126 Uiso 1 1 calc R . . H93 H -0.1319 0.8994 0.2817 0.126 Uiso 1 1 calc R . . C3 C 0.1789(4) 0.3580(8) 0.3958(5) 0.042(2) Uani 1 1 d . . . C7 C 0.2640(4) 0.2513(9) 0.4127(6) 0.059(3) Uani 1 1 d . . . C5 C 0.2774(4) 0.4446(9) 0.4761(5) 0.059(2) Uani 1 1 d . . . C5X C 0.0070(4) 0.6100(7) 0.4167(5) 0.048(2) Uani 1 1 d . . . C9 C 0.2823(4) 0.1428(9) 0.3915(5) 0.077(3) Uani 1 1 d . . . H9A H 0.3224 0.1565 0.4028 0.116 Uiso 1 1 calc R . . H9B H 0.2481 0.1234 0.3312 0.116 Uiso 1 1 calc R . . H9C H 0.2883 0.0784 0.4269 0.116 Uiso 1 1 calc R . . C2 C 0.1019(4) 0.2301(8) 0.3178(5) 0.053(2) Uani 1 1 d . . . H2A H 0.0606 0.1956 0.2855 0.064 Uiso 1 1 calc R . . C6 C 0.3026(4) 0.3452(10) 0.4613(6) 0.063(3) Uani 1 1 d . . . H6A H 0.3461 0.3456 0.4855 0.076 Uiso 1 1 calc R . . C2X C 0.1330(3) 0.6578(7) 0.3660(5) 0.045(2) Uani 1 1 d . . . H2X H 0.1579 0.6596 0.4259 0.054 Uiso 1 1 calc R . . C3X C -0.0581(4) 0.6094(7) 0.2677(5) 0.039(2) Uani 1 1 d . . . C10X C 0.0662(4) 0.5704(7) 0.5038(5) 0.061(3) Uani 1 1 d . . . H10A H 0.0673 0.4855 0.5059 0.091 Uiso 1 1 calc R . . H10B H 0.0651 0.6006 0.5470 0.091 Uiso 1 1 calc R . . H10C H 0.1045 0.5996 0.5150 0.091 Uiso 1 1 calc R . . C7X C -0.0857(4) 0.7424(8) 0.3303(6) 0.052(2) Uani 1 1 d . . . C6X C -0.0345(4) 0.6970(7) 0.4067(6) 0.055(2) Uani 1 1 d . . . H6X H -0.0258 0.7248 0.4565 0.066 Uiso 1 1 calc R . . C10 C 0.3209(4) 0.5454(8) 0.5297(7) 0.096(4) Uani 1 1 d . . . H10D H 0.3081 0.5795 0.5599 0.144 Uiso 1 1 calc R . . H10E H 0.3176 0.6041 0.4928 0.144 Uiso 1 1 calc R . . H10F H 0.3654 0.5180 0.5712 0.144 Uiso 1 1 calc R . . O1W O 0.2817(4) -0.1841(9) 0.4169(6) 0.166(4) Uani 1 1 d . . . O13 O 0.0000 1.0053(11) 0.2500 0.163(7) Uani 1 2 d S . . O11 O 0.0128(4) 0.8455(9) 0.3091(6) 0.134(3) Uani 1 1 d . . . O23 O 0.1416(5) 0.4265(11) 0.2203(6) 0.153(4) Uani 1 1 d . . . O21 O 0.2077(7) 0.5609(12) 0.2698(9) 0.193(6) Uani 1 1 d . . . O22 O 0.2241(6) 0.4025(11) 0.2343(7) 0.204(6) Uani 1 1 d . . . O2W O 0.0236(6) 1.0041(9) 0.4295(9) 0.210(5) Uani 1 1 d . . . O3W O 0.1690(8) 0.1513(16) 0.1457(10) 0.176(9) Uiso 0.595(15) 1 d P . . O3W' O 0.0707(11) 0.122(2) 0.0879(15) 0.164(12) Uiso 0.405(15) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.03330(16) 0.0394(2) 0.03632(17) 0.00179(19) 0.02028(13) 0.00114(19) Cl1 0.0488(12) 0.0496(14) 0.0447(11) 0.0073(10) 0.0309(10) 0.0040(10) N3 0.031(4) 0.040(5) 0.043(4) 0.003(4) 0.023(3) 0.004(3) N4 0.037(4) 0.046(5) 0.053(4) -0.006(4) 0.025(3) -0.005(4) N1 0.057(5) 0.058(6) 0.059(5) -0.009(4) 0.033(4) 0.005(5) N8 0.048(4) 0.048(5) 0.044(4) -0.001(4) 0.024(4) 0.007(4) N1N 0.070(9) 0.071(13) 0.116(14) 0.000 0.055(11) 0.000 N4X 0.033(3) 0.039(4) 0.033(3) 0.001(4) 0.020(3) 0.001(3) N8X 0.037(4) 0.046(5) 0.048(4) -0.002(4) 0.026(4) 0.001(4) N1X 0.042(4) 0.046(5) 0.058(5) 0.000(4) 0.028(4) -0.007(4) N2N 0.096(9) 0.191(16) 0.087(8) 0.037(10) 0.068(8) 0.046(12) N3X 0.037(4) 0.032(4) 0.042(4) -0.001(3) 0.028(3) -0.002(3) C9X 0.086(7) 0.081(8) 0.092(7) -0.018(6) 0.061(6) 0.019(6) C3 0.047(5) 0.041(6) 0.039(5) 0.009(4) 0.028(4) 0.016(5) C7 0.049(6) 0.077(8) 0.050(6) 0.019(5) 0.032(5) 0.023(6) C5 0.047(5) 0.064(7) 0.056(5) 0.013(6) 0.029(5) 0.010(6) C5X 0.043(5) 0.050(6) 0.050(5) -0.007(5) 0.030(5) -0.009(4) C9 0.078(7) 0.092(8) 0.074(6) 0.013(6) 0.055(6) 0.042(6) C2 0.045(5) 0.055(7) 0.056(5) -0.001(5) 0.031(5) -0.001(5) C6 0.043(5) 0.083(8) 0.064(6) 0.017(6) 0.036(5) 0.005(6) C2X 0.035(5) 0.041(6) 0.042(5) -0.005(5) 0.018(4) 0.000(4) C3X 0.038(5) 0.034(5) 0.056(6) -0.005(4) 0.036(5) -0.005(4) C10X 0.060(6) 0.064(7) 0.043(5) -0.014(5) 0.027(5) -0.007(5) C7X 0.047(5) 0.049(6) 0.064(6) -0.011(5) 0.039(5) -0.003(5) C6X 0.061(6) 0.056(7) 0.063(6) -0.018(5) 0.047(5) -0.008(5) C10 0.050(6) 0.064(7) 0.113(8) -0.025(7) 0.027(6) -0.018(6) O1W 0.111(7) 0.183(10) 0.147(8) 0.016(7) 0.059(6) -0.025(6) O13 0.125(11) 0.042(8) 0.243(17) 0.000 0.086(12) 0.000 O11 0.110(7) 0.125(9) 0.163(9) 0.008(7) 0.088(7) -0.029(6) O23 0.123(8) 0.241(14) 0.109(7) 0.042(7) 0.082(7) 0.019(9) O21 0.227(15) 0.197(14) 0.207(14) 0.011(10) 0.165(13) 0.050(11) O22 0.170(10) 0.280(15) 0.203(11) 0.032(9) 0.141(10) 0.122(10) O2W 0.255(13) 0.126(9) 0.346(17) -0.089(9) 0.239(13) -0.066(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N3 2.005(6) . ? Pt1 N3X 2.019(6) . ? Pt1 N4X 2.046(6) . ? Pt1 Cl1 2.328(2) . ? N3 C3 1.339(9) . ? N3 C2 1.366(9) . ? N4 C5 1.314(9) . ? N4 C3 1.328(9) . ? N1 C2 1.319(9) . ? N1 N8 1.382(8) . ? N8 C3 1.368(9) . ? N8 C7 1.387(10) . ? N1N O13 1.170(16) . ? N1N O11 1.192(10) . ? N1N O11 1.192(10) 2 ? N4X C5X 1.347(9) . ? N4X C3X 1.354(9) . ? N8X C3X 1.351(9) . ? N8X C7X 1.356(9) . ? N8X N1X 1.383(8) 2 ? N1X C2X 1.310(9) . ? N1X N8X 1.383(8) 2 ? N2N O22 1.138(13) . ? N2N O23 1.183(14) . ? N2N O21 1.257(17) . ? N3X C3X 1.342(9) 2 ? N3X C2X 1.373(8) . ? C9X C7X 1.481(10) . ? C9X H91 0.9600 . ? C9X H92 0.9600 . ? C9X H93 0.9600 . ? C7 C6 1.356(11) . ? C7 C9 1.486(11) . ? C5 C6 1.443(12) . ? C5 C10 1.480(11) . ? C5X C6X 1.402(10) . ? C5X C10X 1.477(10) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C2 H2A 0.9300 . ? C6 H6A 0.9300 . ? C2X H2X 0.9300 . ? C3X N3X 1.342(9) 2 ? C10X H10A 0.9600 . ? C10X H10B 0.9600 . ? C10X H10C 0.9600 . ? C7X C6X 1.333(10) . ? C6X H6X 0.9300 . ? C10 H10D 0.9600 . ? C10 H10E 0.9600 . ? C10 H10F 0.9600 . ? 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_3 _geom_angle_publ_flag N3 Pt1 N3X 89.5(2) . . ? N3 Pt1 N4X 177.6(2) . . ? N3X Pt1 N4X 88.5(2) . . ? N3 Pt1 Cl1 89.92(18) . . ? N3X Pt1 Cl1 178.70(18) . . ? N4X Pt1 Cl1 92.10(17) . . ? N3 Pt1 Pt1 96.66(17) . 2 ? N3X Pt1 Pt1 76.81(17) . 2 ? N4X Pt1 Pt1 84.11(16) . 2 ? Cl1 Pt1 Pt1 104.41(5) . 2 ? C3 N3 C2 105.0(7) . . ? C3 N3 Pt1 127.3(6) . . ? C2 N3 Pt1 127.7(5) . . ? C5 N4 C3 115.7(8) . . ? C2 N1 N8 101.3(7) . . ? C3 N8 N1 111.7(7) . . ? C3 N8 C7 122.1(8) . . ? N1 N8 C7 126.2(8) . . ? O13 N1N O11 122.1(10) . . ? O13 N1N O11 122.1(10) . 2 ? O11 N1N O11 116(2) . 2 ? C5X N4X C3X 117.0(7) . . ? C5X N4X Pt1 124.0(5) . . ? C3X N4X Pt1 118.8(5) . . ? C3X N8X C7X 123.0(7) . . ? C3X N8X N1X 110.0(7) . 2 ? C7X N8X N1X 126.9(7) . 2 ? C2X N1X N8X 103.0(6) . 2 ? O22 N2N O23 126(2) . . ? O22 N2N O21 120.6(19) . . ? O23 N2N O21 113.0(16) . . ? C3X N3X C2X 104.0(6) 2 . ? C3X N3X Pt1 129.4(5) 2 . ? C2X N3X Pt1 126.5(5) . . ? C7X C9X H91 109.5 . . ? C7X C9X H92 109.5 . . ? H91 C9X H92 109.5 . . ? C7X C9X H93 109.5 . . ? H91 C9X H93 109.5 . . ? H92 C9X H93 109.5 . . ? N4 C3 N3 128.9(8) . . ? N4 C3 N8 124.3(7) . . ? N3 C3 N8 106.8(7) . . ? C6 C7 N8 114.1(8) . . ? C6 C7 C9 127.8(9) . . ? N8 C7 C9 118.0(9) . . ? N4 C5 C6 122.6(9) . . ? N4 C5 C10 117.7(9) . . ? C6 C5 C10 119.7(8) . . ? N4X C5X C6X 119.3(7) . . ? N4X C5X C10X 119.2(7) . . ? C6X C5X C10X 121.4(8) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C2 N3 115.2(7) . . ? N1 C2 H2A 122.4 . . ? N3 C2 H2A 122.4 . . ? C7 C6 C5 121.1(8) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? N1X C2X N3X 114.3(7) . . ? N1X C2X H2X 122.9 . . ? N3X C2X H2X 122.9 . . ? N3X C3X N8X 108.7(7) 2 . ? N3X C3X N4X 129.3(7) 2 . ? N8X C3X N4X 122.0(7) . . ? C5X C10X H10A 109.5 . . ? C5X C10X H10B 109.5 . . ? H10A C10X H10B 109.5 . . ? C5X C10X H10C 109.5 . . ? H10A C10X H10C 109.5 . . ? H10B C10X H10C 109.5 . . ? C6X C7X N8X 114.5(8) . . ? C6X C7X C9X 128.3(8) . . ? N8X C7X C9X 117.1(8) . . ? C7X C6X C5X 124.0(8) . . ? C7X C6X H6X 118.0 . . ? C5X C6X H6X 118.0 . . ? C5 C10 H10D 109.5 . . ? C5 C10 H10E 109.5 . . ? H10D C10 H10E 109.5 . . ? C5 C10 H10F 109.5 . . ? H10D C10 H10F 109.5 . . ? H10E C10 H10F 109.5 . . ? 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 N3X Pt1 N3 C3 50.0(6) . . . . ? Cl1 Pt1 N3 C3 -128.9(6) . . . . ? Pt1 Pt1 N3 C3 126.6(6) 2 . . . ? N3X Pt1 N3 C2 -128.6(6) . . . . ? Cl1 Pt1 N3 C2 52.5(6) . . . . ? Pt1 Pt1 N3 C2 -52.0(6) 2 . . . ? C2 N1 N8 C3 0.7(8) . . . . ? C2 N1 N8 C7 -180.0(7) . . . . ? N3X Pt1 N4X C5X -107.8(6) . . . . ? Cl1 Pt1 N4X C5X 71.0(6) . . . . ? Pt1 Pt1 N4X C5X 175.3(6) 2 . . . ? N3X Pt1 N4X C3X 67.8(5) . . . . ? Cl1 Pt1 N4X C3X -113.4(5) . . . . ? Pt1 Pt1 N4X C3X -9.1(5) 2 . . . ? N3 Pt1 N3X C3X 85.6(6) . . . 2 ? N4X Pt1 N3X C3X -95.7(6) . . . 2 ? Pt1 Pt1 N3X C3X -11.4(6) 2 . . 2 ? N3 Pt1 N3X C2X -88.9(6) . . . . ? N4X Pt1 N3X C2X 89.8(6) . . . . ? Pt1 Pt1 N3X C2X 174.1(6) 2 . . . ? C5 N4 C3 N3 179.6(7) . . . . ? C5 N4 C3 N8 1.2(11) . . . . ? C2 N3 C3 N4 -178.1(8) . . . . ? Pt1 N3 C3 N4 3.1(11) . . . . ? C2 N3 C3 N8 0.5(8) . . . . ? Pt1 N3 C3 N8 -178.3(4) . . . . ? N1 N8 C3 N4 177.9(7) . . . . ? C7 N8 C3 N4 -1.5(11) . . . . ? N1 N8 C3 N3 -0.8(8) . . . . ? C7 N8 C3 N3 179.9(7) . . . . ? C3 N8 C7 C6 0.8(11) . . . . ? N1 N8 C7 C6 -178.4(7) . . . . ? C3 N8 C7 C9 -179.5(7) . . . . ? N1 N8 C7 C9 1.3(12) . . . . ? C3 N4 C5 C6 -0.5(12) . . . . ? C3 N4 C5 C10 179.6(7) . . . . ? C3X N4X C5X C6X -0.6(10) . . . . ? Pt1 N4X C5X C6X 175.1(5) . . . . ? C3X N4X C5X C10X -176.9(7) . . . . ? Pt1 N4X C5X C10X -1.2(10) . . . . ? N8 N1 C2 N3 -0.4(9) . . . . ? C3 N3 C2 N1 0.0(9) . . . . ? Pt1 N3 C2 N1 178.8(5) . . . . ? N8 C7 C6 C5 -0.1(12) . . . . ? C9 C7 C6 C5 -179.8(8) . . . . ? N4 C5 C6 C7 -0.1(13) . . . . ? C10 C5 C6 C7 179.8(8) . . . . ? N8X N1X C2X N3X 0.4(9) 2 . . . ? C3X N3X C2X N1X -1.7(9) 2 . . . ? Pt1 N3X C2X N1X 173.8(5) . . . . ? C7X N8X C3X N3X 178.7(7) . . . 2 ? N1X N8X C3X N3X -2.3(8) 2 . . 2 ? C7X N8X C3X N4X -2.9(11) . . . . ? N1X N8X C3X N4X 176.1(6) 2 . . . ? C5X N4X C3X N3X -179.3(7) . . . 2 ? Pt1 N4X C3X N3X 4.8(10) . . . 2 ? C5X N4X C3X N8X 2.6(10) . . . . ? Pt1 N4X C3X N8X -173.3(5) . . . . ? C3X N8X C7X C6X 0.9(11) . . . . ? N1X N8X C7X C6X -177.9(7) 2 . . . ? C3X N8X C7X C9X -178.8(7) . . . . ? N1X N8X C7X C9X 2.4(12) 2 . . . ? N8X C7X C6X C5X 1.2(12) . . . . ? C9X C7X C6X C5X -179.1(8) . . . . ? N4X C5X C6X C7X -1.4(13) . . . . ? C10X C5X C6X C7X 174.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.246 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.136