# Copyright The Royal Society of Chemistry, 1998 data_ptpiret2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common trans-[PtCl2(h2-C2H4)(Hpir)]x0.5C6H6 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H20 Cl2 N3 O4 Pt S' _chemical_formula_weight 664.39 _chemical_melting_point ? _chemical_compound_source ? 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' 'S' 'S' 0.1246 0.1234 '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 ? _symmetry_space_group_name_H-M 'P(-1), no. 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9290(10) _cell_length_b 11.3950(10) _cell_length_c 14.948(2) _cell_angle_alpha 87.920(10) _cell_angle_beta 83.920(10) _cell_angle_gamma 79.570(10) _cell_volume 1154.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 10 _cell_measurement_theta_max 40 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method ? _exptl_crystal_F_000 642 _exptl_absorpt_coefficient_mu 6.49 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.91 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'SIEMENS P4' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no appreciable decay' _diffrn_reflns_number 4435 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4071 _reflns_number_observed 3533 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SIEMENS XSCANS' _computing_cell_refinement 'SIEMENS XSCANS' _computing_data_reduction 'SIEMENS XSCANS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XPMA-ZORTEP (Zsolnai, 1994)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or 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 w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary PATTERSON _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom + difmap' _refine_ls_hydrogen_treatment ; H(16), H(17) and ethene free, all others free to ride on the atoms to which they are bound ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4069 _refine_ls_number_parameters 298 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_obs 0.0419 _refine_ls_wR_factor_all 0.1119 _refine_ls_wR_factor_obs 0.1019 _refine_ls_goodness_of_fit_all 1.053 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.099 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max 0.126 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.12905(4) 0.49984(2) 0.13376(2) 0.04084(13) Uani 1 d . . Cl1 Cl -0.1796(3) 0.5969(2) 0.1055(2) 0.0616(5) Uani 1 d . . Cl2 Cl 0.4354(3) 0.3993(3) 0.1612(2) 0.0716(7) Uani 1 d . . S1 S -0.1455(3) 0.7802(2) 0.36864(13) 0.0460(4) Uani 1 d . . O11 O 0.0600(8) 0.7303(5) 0.3643(4) 0.0570(14) Uani 1 d . . O12 O -0.2110(10) 0.8766(5) 0.3099(4) 0.064(2) Uani 1 d . . O15 O -0.2085(9) 0.3706(5) 0.4440(4) 0.0547(14) Uani 1 d . . O17 O -0.2448(9) 0.5236(5) 0.5756(4) 0.0581(14) Uani 1 d D . H17 H -0.2182(141) 0.4585(53) 0.5437(55) 0.070 Uiso 1 d D . N2 N -0.2655(9) 0.6723(5) 0.3535(4) 0.0407(13) Uani 1 d . . N16 N -0.1556(10) 0.4432(5) 0.3004(4) 0.0427(15) Uani 1 d . . H16 H -0.1535(125) 0.4995(78) 0.2732(58) 0.051 Uiso 1 d . . N1' N 0.0215(9) 0.3449(5) 0.1771(4) 0.0443(14) Uani 1 d . . C3 C -0.2434(11) 0.5783(6) 0.4209(5) 0.043(2) Uani 1 d . . C4 C -0.2564(10) 0.6055(7) 0.5095(5) 0.044(2) Uani 1 d . . C5 C -0.3327(13) 0.7556(9) 0.6312(6) 0.061(2) Uani 1 d . . H5 H -0.3619(13) 0.6964(9) 0.6722(6) 0.073 Uiso 1 calc R . C6 C -0.3458(15) 0.8718(10) 0.6584(7) 0.073(3) Uani 1 d . . H6 H -0.3865(15) 0.8907(10) 0.7182(7) 0.087 Uiso 1 calc R . C7 C -0.3000(16) 0.9597(9) 0.5990(8) 0.078(3) Uani 1 d . . H7 H -0.3083(16) 1.0368(9) 0.6193(8) 0.093 Uiso 1 calc R . C8 C -0.2410(14) 0.9344(7) 0.5085(7) 0.063(2) Uani 1 d . . H8 H -0.2096(14) 0.9936(7) 0.4679(7) 0.075 Uiso 1 calc R . C9 C -0.2309(11) 0.8190(7) 0.4814(5) 0.046(2) Uani 1 d . . C10 C -0.2743(10) 0.7290(7) 0.5403(5) 0.045(2) Uani 1 d . . C13 C -0.4660(14) 0.7054(7) 0.3278(6) 0.059(2) Uani 1 d . . H131 H -0.4703(14) 0.7680(7) 0.2829(6) 0.071 Uiso 1 calc R . H132 H -0.5544(14) 0.7328(7) 0.3797(6) 0.071 Uiso 1 calc R . H133 H -0.5052(14) 0.6372(7) 0.3039(6) 0.071 Uiso 1 calc R . C14 C -0.2033(10) 0.4560(6) 0.3906(5) 0.042(2) Uani 1 d . . C2' C -0.0971(10) 0.3368(6) 0.2528(5) 0.039(2) Uani 1 d . . C3' C -0.1535(12) 0.2302(7) 0.2809(6) 0.051(2) Uani 1 d . . H3' H -0.2335(12) 0.2255(7) 0.3345(6) 0.062 Uiso 1 calc R . C4' C -0.0899(14) 0.1310(7) 0.2288(7) 0.061(2) Uani 1 d . . H4' H -0.1265(14) 0.0584(7) 0.2467(7) 0.073 Uiso 1 calc R . C5' C 0.0292(14) 0.1403(7) 0.1495(6) 0.060(2) Uani 1 d . . H5' H 0.0743(14) 0.0738(7) 0.1138(6) 0.072 Uiso 1 calc R . C6' C 0.0799(13) 0.2477(7) 0.1239(6) 0.054(2) Uani 1 d . . H6' H 0.1555(13) 0.2546(7) 0.0694(6) 0.064 Uiso 1 calc R . C1E C 0.2154(17) 0.6737(9) 0.1399(7) 0.072(3) Uani 1 d D . H1E1 H 0.0831(88) 0.7371(73) 0.1488(69) 0.086 Uiso 1 d D . H2E1 H 0.3519(84) 0.6296(83) 0.1620(68) 0.086 Uiso 1 d D . C2E C 0.2594(15) 0.6290(8) 0.0514(6) 0.058(2) Uani 1 d D . H1E2 H 0.1996(126) 0.6264(81) -0.0096(34) 0.070 Uiso 1 d D . H2E2 H 0.3998(67) 0.5748(70) 0.0424(60) 0.070 Uiso 1 d D . C1B C 0.4831(16) 0.1094(9) 0.9616(10) 0.085(3) Uani 1 d . . H1B H 0.4716(16) 0.1850(9) 0.9349(10) 0.103 Uiso 1 calc R . C2B C 0.5781(19) 0.0858(10) 1.0348(10) 0.094(4) Uani 1 d . . H2B H 0.6319(19) 0.1452(10) 1.0591(10) 0.113 Uiso 1 calc R . C3B C 0.4029(18) 0.0244(11) 0.9257(9) 0.091(3) Uani 1 d . . H3B H 0.3358(18) 0.0412(11) 0.8747(9) 0.109 Uiso 1 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 0.0464(2) 0.0413(2) 0.0391(2) 0.00578(11) -0.00348(11) -0.02095(12) Cl1 0.0552(12) 0.0540(12) 0.0755(14) 0.0187(10) -0.0088(10) -0.0118(9) Cl2 0.0448(11) 0.096(2) 0.0753(15) 0.0316(13) -0.0085(10) -0.0219(11) S1 0.0485(11) 0.0393(10) 0.0519(11) 0.0077(8) -0.0027(8) -0.0155(8) O11 0.043(3) 0.065(4) 0.065(4) 0.001(3) 0.006(3) -0.019(3) O12 0.089(5) 0.038(3) 0.066(4) 0.019(3) -0.012(3) -0.019(3) O15 0.069(4) 0.041(3) 0.054(3) 0.014(2) 0.002(3) -0.016(3) O17 0.073(4) 0.057(3) 0.044(3) 0.016(3) -0.003(3) -0.018(3) N2 0.043(3) 0.033(3) 0.048(3) 0.009(2) -0.007(3) -0.011(3) N16 0.050(4) 0.027(3) 0.050(4) 0.009(3) 0.002(3) -0.008(3) N1' 0.045(3) 0.035(3) 0.055(4) 0.009(3) -0.013(3) -0.010(3) C3 0.039(4) 0.040(4) 0.048(4) 0.010(3) 0.004(3) -0.012(3) C4 0.031(4) 0.049(4) 0.048(4) 0.013(3) 0.001(3) -0.008(3) C5 0.048(5) 0.080(6) 0.052(5) -0.001(4) -0.002(4) -0.003(4) C6 0.062(6) 0.083(7) 0.069(6) -0.027(6) -0.005(5) 0.004(5) C7 0.078(7) 0.058(6) 0.095(8) -0.034(6) -0.021(6) 0.008(5) C8 0.069(6) 0.041(4) 0.080(6) -0.001(4) -0.021(5) -0.005(4) C9 0.034(4) 0.046(4) 0.057(5) -0.008(3) -0.005(3) -0.002(3) C10 0.031(4) 0.052(4) 0.053(4) -0.004(3) -0.003(3) -0.005(3) C13 0.071(6) 0.044(4) 0.070(6) 0.008(4) -0.028(5) -0.018(4) C14 0.035(4) 0.040(4) 0.051(4) 0.017(3) -0.006(3) -0.012(3) C2' 0.039(4) 0.034(4) 0.048(4) 0.011(3) -0.011(3) -0.015(3) C3' 0.050(5) 0.038(4) 0.068(5) 0.013(4) -0.008(4) -0.015(3) C4' 0.069(6) 0.033(4) 0.088(7) 0.011(4) -0.022(5) -0.021(4) C5' 0.072(6) 0.037(4) 0.075(6) -0.004(4) -0.011(5) -0.015(4) C6' 0.065(5) 0.049(5) 0.047(4) -0.005(4) -0.005(4) -0.013(4) C1E 0.089(7) 0.052(5) 0.083(7) 0.003(5) -0.007(6) -0.037(5) C2E 0.074(6) 0.064(5) 0.044(4) 0.015(4) -0.007(4) -0.033(5) C1B 0.067(7) 0.053(6) 0.134(10) 0.024(6) -0.005(7) -0.011(5) C2B 0.098(9) 0.066(7) 0.128(11) -0.020(7) -0.029(8) -0.027(6) C3B 0.092(8) 0.090(9) 0.097(9) 0.011(7) -0.024(7) -0.025(7) _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 N1' 2.093(6) . ? Pt1 C2E 2.148(8) . ? Pt1 C1E 2.178(9) . ? Pt1 Cl2 2.293(2) . ? Pt1 Cl1 2.297(2) . ? S1 O12 1.421(6) . ? S1 O11 1.430(6) . ? S1 N2 1.639(6) . ? S1 C9 1.770(8) . ? O15 C14 1.239(8) . ? O17 C4 1.334(9) . ? N2 C3 1.442(9) . ? N2 C13 1.461(10) . ? N16 C14 1.362(10) . ? N16 C2' 1.401(9) . ? N1' C2' 1.336(10) . ? N1' C6' 1.363(10) . ? C3 C4 1.361(11) . ? C3 C14 1.450(10) . ? C4 C10 1.476(11) . ? C5 C6 1.383(14) . ? C5 C10 1.404(12) . ? C6 C7 1.372(15) . ? C7 C8 1.396(14) . ? C8 C9 1.378(11) . ? C9 C10 1.382(11) . ? C2' C3' 1.381(10) . ? C3' C4' 1.374(12) . ? C4' C5' 1.384(13) . ? C5' C6' 1.363(12) . ? C1E C2E 1.418(14) . ? C1B C2B 1.33(2) . ? C1B C3B 1.35(2) . ? C2B C3B 1.36(2) 2_657 ? C3B C2B 1.36(2) 2_657 ? 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' Pt1 C2E 162.3(3) . . ? N1' Pt1 C1E 159.3(3) . . ? C2E Pt1 C1E 38.3(4) . . ? N1' Pt1 Cl2 87.1(2) . . ? C2E Pt1 Cl2 90.7(3) . . ? C1E Pt1 Cl2 92.9(3) . . ? N1' Pt1 Cl1 91.9(2) . . ? C2E Pt1 Cl1 90.1(3) . . ? C1E Pt1 Cl1 88.3(3) . . ? Cl2 Pt1 Cl1 178.80(8) . . ? O12 S1 O11 119.5(4) . . ? O12 S1 N2 108.0(4) . . ? O11 S1 N2 107.9(3) . . ? O12 S1 C9 109.8(4) . . ? O11 S1 C9 108.5(4) . . ? N2 S1 C9 101.6(3) . . ? C3 N2 C13 113.8(6) . . ? C3 N2 S1 114.0(5) . . ? C13 N2 S1 117.7(5) . . ? C14 N16 C2' 127.8(6) . . ? C2' N1' C6' 119.5(7) . . ? C2' N1' Pt1 124.0(5) . . ? C6' N1' Pt1 116.6(5) . . ? C4 C3 N2 120.2(7) . . ? C4 C3 C14 122.0(6) . . ? N2 C3 C14 117.8(6) . . ? O17 C4 C3 123.4(7) . . ? O17 C4 C10 114.0(7) . . ? C3 C4 C10 122.5(7) . . ? C6 C5 C10 118.5(9) . . ? C7 C6 C5 121.5(9) . . ? C6 C7 C8 120.6(9) . . ? C9 C8 C7 117.8(9) . . ? C8 C9 C10 122.4(8) . . ? C8 C9 S1 119.7(7) . . ? C10 C9 S1 117.7(6) . . ? C9 C10 C5 119.2(8) . . ? C9 C10 C4 121.0(7) . . ? C5 C10 C4 119.8(8) . . ? O15 C14 N16 123.3(7) . . ? O15 C14 C3 121.8(7) . . ? N16 C14 C3 114.9(6) . . ? N1' C2' C3' 121.4(7) . . ? N1' C2' N16 114.9(6) . . ? C3' C2' N16 123.6(7) . . ? C4' C3' C2' 119.2(8) . . ? C3' C4' C5' 119.2(8) . . ? C6' C5' C4' 119.6(8) . . ? N1' C6' C5' 121.0(8) . . ? C2E C1E Pt1 69.7(5) . . ? C1E C2E Pt1 72.0(5) . . ? C2B C1B C3B 120.6(10) . . ? C1B C2B C3B 120.4(11) . 2_657 ? C1B C3B C2B 119.0(11) . 2_657 ? _refine_diff_density_max 2.354 _refine_diff_density_min -2.941 _refine_diff_density_rms 0.169