data_c:\crystal\x-red\ebokt05 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl2 N4 O2 Pt' _chemical_formula_weight 484.21 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'N' 'N' 0.0061 0.0033 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 17.4566(6) _cell_length_b 17.4566(6) _cell_length_c 9.0567(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2759.87(16) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23934 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 28.283 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 10.557 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'X-Shape (Stoe & Cie, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; 'Kappa CCD (Nonius)' ; _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14292 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 28.29 _reflns_number_total 3409 _reflns_number_gt 3236 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; 'Collect (Nonius BV, 1997-2000)' ; _computing_cell_refinement ; 'HKL Scalepack (Otwinowski & Minor 1997)' ; _computing_data_reduction ; 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+34.4517P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00029(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.026(10) _refine_ls_number_reflns 3409 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0601 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Pt Pt 0.841005(13) 0.201740(13) 0.76326(2) 0.01960(8) Uani 1 1 d . . . Cl1 Cl 0.90542(10) 0.28716(11) 0.6157(2) 0.0254(4) Uani 1 1 d . . . Cl2 Cl 0.92715(10) 0.10676(9) 0.7078(2) 0.0281(4) Uani 1 1 d . . . O1 O 0.6056(4) 0.0914(4) 0.7449(12) 0.074(2) Uani 1 1 d . . . O2 O 0.6029(3) 0.2298(4) 0.6341(7) 0.0409(15) Uani 1 1 d . . . N1 N 0.7862(4) 0.1280(3) 0.8958(7) 0.0218(12) Uani 1 1 d . . . N2 N 0.6997(4) 0.0523(4) 0.9943(7) 0.0294(14) Uani 1 1 d . . . N3 N 0.7665(3) 0.2838(3) 0.8233(6) 0.0206(12) Uani 1 1 d . . . N4 N 0.6583(3) 0.3472(3) 0.8397(7) 0.0234(13) Uani 1 1 d . . . C1 C 0.7126(4) 0.1079(4) 0.8911(8) 0.0233(14) Uani 1 1 d . . . C2 C 0.7674(5) 0.0379(4) 1.0613(8) 0.0334(19) Uani 1 1 d . . . H2A H 0.7755 0.0024 1.1361 0.040 Uiso 1 1 calc R . . C3 C 0.8210(5) 0.0839(4) 1.0012(8) 0.0284(17) Uani 1 1 d . . . H3A H 0.8726 0.0854 1.0268 0.034 Uiso 1 1 calc R . . C4 C 0.6260(5) 0.0177(5) 1.0318(10) 0.0360(19) Uani 1 1 d . . . H4C H 0.6310 -0.0110 1.1217 0.043 Uiso 1 1 calc R . . H4B H 0.6103 -0.0159 0.9536 0.043 Uiso 1 1 calc R . . H4A H 0.5884 0.0573 1.0447 0.043 Uiso 1 1 calc R . . C5 C 0.6548(4) 0.1344(4) 0.7858(10) 0.0329(18) Uani 1 1 d . . . C6 C 0.6912(4) 0.2813(4) 0.7985(8) 0.0242(15) Uani 1 1 d . . . C7 C 0.7141(4) 0.3937(4) 0.8930(8) 0.0263(16) Uani 1 1 d . . . H7A H 0.7077 0.4429 0.9308 0.032 Uiso 1 1 calc R . . C8 C 0.7816(4) 0.3542(4) 0.8804(8) 0.0233(14) Uani 1 1 d . . . H8A H 0.8298 0.3725 0.9066 0.028 Uiso 1 1 calc R . . C9 C 0.5768(4) 0.3660(5) 0.8306(9) 0.0319(17) Uani 1 1 d . . . H9C H 0.5698 0.4197 0.8493 0.038 Uiso 1 1 calc R . . H9B H 0.5491 0.3368 0.9029 0.038 Uiso 1 1 calc R . . H9A H 0.5581 0.3538 0.7338 0.038 Uiso 1 1 calc R . . C10 C 0.6498(4) 0.2173(4) 0.7299(9) 0.0273(14) Uani 1 1 d . . . 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 Pt 0.01818(13) 0.01938(13) 0.02123(11) -0.00182(11) -0.00194(10) 0.00252(10) Cl1 0.0206(8) 0.0231(9) 0.0327(9) 0.0014(7) 0.0016(7) -0.0018(7) Cl2 0.0250(8) 0.0206(7) 0.0387(10) -0.0061(7) 0.0033(7) 0.0042(6) O1 0.078(5) 0.041(3) 0.102(6) 0.021(5) -0.047(6) -0.030(3) O2 0.038(3) 0.039(4) 0.045(4) 0.008(3) -0.017(3) -0.002(3) N1 0.025(3) 0.019(3) 0.021(3) 0.002(2) 0.000(2) 0.002(2) N2 0.041(4) 0.018(3) 0.030(3) 0.002(3) 0.007(3) 0.001(3) N3 0.019(3) 0.021(3) 0.021(3) 0.005(2) -0.003(2) -0.002(2) N4 0.021(3) 0.024(3) 0.025(3) 0.009(2) 0.004(2) 0.008(2) C1 0.028(4) 0.017(3) 0.025(3) 0.001(3) 0.002(3) -0.004(3) C2 0.058(6) 0.018(4) 0.024(4) 0.004(3) -0.007(4) 0.006(4) C3 0.042(5) 0.023(4) 0.020(3) 0.005(3) -0.007(3) 0.008(3) C4 0.042(5) 0.022(4) 0.043(5) 0.000(3) 0.018(4) -0.002(3) C5 0.025(3) 0.021(3) 0.053(5) 0.009(3) -0.010(4) -0.008(3) C6 0.021(3) 0.021(3) 0.030(4) 0.008(3) 0.001(3) 0.001(3) C7 0.025(4) 0.027(4) 0.026(4) -0.002(3) 0.004(3) 0.000(3) C8 0.020(3) 0.019(3) 0.030(4) -0.001(3) 0.002(3) 0.001(3) C9 0.024(4) 0.037(4) 0.035(4) 0.012(3) 0.004(3) 0.002(3) C10 0.025(3) 0.030(3) 0.027(4) 0.006(3) -0.007(3) 0.000(3) _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 Pt N1 2.003(6) . ? Pt N3 2.009(6) . ? Pt Cl2 2.2942(16) . ? Pt Cl1 2.2966(18) . ? O1 C5 1.199(9) . ? O2 C10 1.213(9) . ? N1 C1 1.333(10) . ? N1 C3 1.369(9) . ? N2 C2 1.352(11) . ? N2 C1 1.366(9) . ? N2 C4 1.460(10) . ? N3 C6 1.334(9) . ? N3 C8 1.360(9) . ? N4 C6 1.338(9) . ? N4 C7 1.358(10) . ? N4 C9 1.462(9) . ? C1 C5 1.463(10) . ? C2 C3 1.348(12) . ? C5 C10 1.536(9) . ? C6 C10 1.469(10) . ? C7 C8 1.371(10) . ? 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 N1 Pt N3 89.2(2) . . ? N1 Pt Cl2 88.86(17) . . ? N3 Pt Cl2 176.94(18) . . ? N1 Pt Cl1 178.73(19) . . ? N3 Pt Cl1 90.68(17) . . ? Cl2 Pt Cl1 91.20(6) . . ? C1 N1 C3 107.5(6) . . ? C1 N1 Pt 127.7(5) . . ? C3 N1 Pt 124.6(5) . . ? C2 N2 C1 107.1(7) . . ? C2 N2 C4 126.1(7) . . ? C1 N2 C4 126.7(7) . . ? C6 N3 C8 106.5(6) . . ? C6 N3 Pt 124.7(5) . . ? C8 N3 Pt 128.4(5) . . ? C6 N4 C7 107.8(6) . . ? C6 N4 C9 126.5(7) . . ? C7 N4 C9 125.7(6) . . ? N1 C1 N2 109.0(7) . . ? N1 C1 C5 127.0(6) . . ? N2 C1 C5 123.8(7) . . ? C3 C2 N2 108.4(7) . . ? C2 C3 N1 107.9(7) . . ? O1 C5 C1 119.8(7) . . ? O1 C5 C10 116.6(7) . . ? C1 C5 C10 123.5(6) . . ? N3 C6 N4 110.4(7) . . ? N3 C6 C10 125.4(6) . . ? N4 C6 C10 124.1(6) . . ? N4 C7 C8 106.6(7) . . ? N3 C8 C7 108.7(6) . . ? O2 C10 C6 119.8(7) . . ? O2 C10 C5 116.4(6) . . ? C6 C10 C5 123.3(6) . . ? 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 N3 Pt N1 C1 58.0(6) . . . . ? Cl2 Pt N1 C1 -124.3(6) . . . . ? Cl1 Pt N1 C1 143(8) . . . . ? N3 Pt N1 C3 -128.0(6) . . . . ? Cl2 Pt N1 C3 49.6(6) . . . . ? Cl1 Pt N1 C3 -43(9) . . . . ? N1 Pt N3 C6 -62.3(6) . . . . ? Cl2 Pt N3 C6 -113(3) . . . . ? Cl1 Pt N3 C6 119.0(6) . . . . ? N1 Pt N3 C8 125.4(6) . . . . ? Cl2 Pt N3 C8 75(3) . . . . ? Cl1 Pt N3 C8 -53.3(6) . . . . ? C3 N1 C1 N2 1.0(8) . . . . ? Pt N1 C1 N2 175.8(5) . . . . ? C3 N1 C1 C5 -173.7(7) . . . . ? Pt N1 C1 C5 1.0(11) . . . . ? C2 N2 C1 N1 -0.8(8) . . . . ? C4 N2 C1 N1 175.9(7) . . . . ? C2 N2 C1 C5 174.2(7) . . . . ? C4 N2 C1 C5 -9.1(12) . . . . ? C1 N2 C2 C3 0.2(9) . . . . ? C4 N2 C2 C3 -176.6(7) . . . . ? N2 C2 C3 N1 0.5(9) . . . . ? C1 N1 C3 C2 -0.9(8) . . . . ? Pt N1 C3 C2 -175.9(5) . . . . ? N1 C1 C5 O1 144.7(10) . . . . ? N2 C1 C5 O1 -29.4(13) . . . . ? N1 C1 C5 C10 -39.3(12) . . . . ? N2 C1 C5 C10 146.7(7) . . . . ? C8 N3 C6 N4 -0.8(8) . . . . ? Pt N3 C6 N4 -174.5(4) . . . . ? C8 N3 C6 C10 176.7(7) . . . . ? Pt N3 C6 C10 3.0(10) . . . . ? C7 N4 C6 N3 -0.1(8) . . . . ? C9 N4 C6 N3 -179.6(6) . . . . ? C7 N4 C6 C10 -177.6(7) . . . . ? C9 N4 C6 C10 2.9(11) . . . . ? C6 N4 C7 C8 0.9(8) . . . . ? C9 N4 C7 C8 -179.6(6) . . . . ? C6 N3 C8 C7 1.4(8) . . . . ? Pt N3 C8 C7 174.8(5) . . . . ? N4 C7 C8 N3 -1.4(8) . . . . ? N3 C6 C10 O2 -134.0(8) . . . . ? N4 C6 C10 O2 43.1(11) . . . . ? N3 C6 C10 C5 54.0(11) . . . . ? N4 C6 C10 C5 -128.9(8) . . . . ? O1 C5 C10 O2 -9.5(13) . . . . ? C1 C5 C10 O2 174.4(8) . . . . ? O1 C5 C10 C6 162.8(9) . . . . ? C1 C5 C10 C6 -13.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.849 _refine_diff_density_min -1.665 _refine_diff_density_rms 0.154