Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Wendt, Ola F.' 'Kuznik, Nikodem' _publ_contact_author_name 'Dr Ola F Wendt' _publ_contact_author_address ; Dr Ola F Wendt Inorganic Chemistry 1, Department of Chemistry Lund University PO Box 124 221 00 Lund SWEDEN ; _publ_contact_author_email 'OLA.WENDT@INORG.LU.SE' _publ_section_title ; Trans Effect and trans influence of triphenyl arsine in platinum(II) complexes. A comparative mechanistic and structural study. ; data_paperB202100P _database_code_CSD 180736 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound1' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H51 As I3 N Pt' _chemical_formula_weight 1124.47 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.788(2) _cell_length_b 18.474(4) _cell_length_c 21.956(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.67(3) _cell_angle_gamma 90.00 _cell_volume 3924.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7680 _cell_measurement_theta_min 2.176 _cell_measurement_theta_max 26.304 _exptl_crystal_description 'plate' _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.903 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 6.793 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.296734 _exptl_absorpt_correction_T_max 0.596846 _exptl_absorpt_process_details 'absorption corrections using SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 38894 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.0946 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 31.80 _reflns_number_total 12008 _reflns_number_gt 6247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg)' _computing_publication_material '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^)+(0.0465P)^2^+1.1000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12008 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0453 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _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 Pt1 Pt 0.59936(3) 0.292920(13) 0.388669(11) 0.04071(8) Uani 1 1 d . . . I1 I 0.79470(5) 0.33540(3) 0.47566(2) 0.06086(15) Uani 1 1 d . . . I2 I 0.42761(6) 0.24591(3) 0.29391(2) 0.06233(15) Uani 1 1 d . . . I3 I 0.61113(6) 0.41892(3) 0.33120(3) 0.06528(16) Uani 1 1 d . . . As1 As 0.56250(7) 0.18248(4) 0.43915(3) 0.04257(16) Uani 1 1 d . . . C11 C 0.5937(8) 0.0960(4) 0.3909(3) 0.0496(17) Uani 1 1 d . . . C12 C 0.5083(8) 0.0350(4) 0.3870(3) 0.0532(18) Uani 1 1 d . . . H12 H 0.4282 0.0350 0.4050 0.069 Uiso 1 1 calc R . . C13 C 0.5457(10) -0.0258(4) 0.3557(4) 0.069(2) Uani 1 1 d . . . H13 H 0.4905 -0.0669 0.3537 0.089 Uiso 1 1 calc R . . C14 C 0.6632(10) -0.0265(5) 0.3272(4) 0.069(2) Uani 1 1 d . . . H14 H 0.6869 -0.0676 0.3068 0.089 Uiso 1 1 calc R . . C15 C 0.7420(9) 0.0335(5) 0.3298(4) 0.071(2) Uani 1 1 d . . . H15 H 0.8203 0.0334 0.3105 0.092 Uiso 1 1 calc R . . C16 C 0.7098(8) 0.0953(4) 0.3605(4) 0.063(2) Uani 1 1 d . . . H16 H 0.7652 0.1362 0.3609 0.082 Uiso 1 1 calc R . . C21 C 0.3766(7) 0.1737(4) 0.4607(3) 0.0459(16) Uani 1 1 d . . . C22 C 0.2739(8) 0.2222(4) 0.4402(3) 0.0538(18) Uani 1 1 d . . . H22 H 0.2920 0.2592 0.4137 0.070 Uiso 1 1 calc R . . C23 C 0.1441(9) 0.2177(5) 0.4577(4) 0.069(2) Uani 1 1 d . . . H23 H 0.0780 0.2526 0.4441 0.090 Uiso 1 1 calc R . . C24 C 0.1118(9) 0.1627(5) 0.4947(4) 0.071(2) Uani 1 1 d . . . H24 H 0.0242 0.1598 0.5061 0.092 Uiso 1 1 calc R . . C25 C 0.2095(10) 0.1125(5) 0.5144(4) 0.081(3) Uani 1 1 d . . . H25 H 0.1877 0.0745 0.5389 0.106 Uiso 1 1 calc R . . C26 C 0.3425(9) 0.1168(5) 0.4986(4) 0.070(2) Uani 1 1 d . . . H26 H 0.4084 0.0821 0.5131 0.090 Uiso 1 1 calc R . . C31 C 0.6722(7) 0.1580(4) 0.5189(3) 0.0520(18) Uani 1 1 d . . . C32 C 0.7615(8) 0.0995(4) 0.5261(4) 0.063(2) Uani 1 1 d . . . H32 H 0.7699 0.0699 0.4926 0.082 Uiso 1 1 calc R . . C33 C 0.8389(10) 0.0850(5) 0.5834(4) 0.086(3) Uani 1 1 d . . . H33 H 0.9005 0.0463 0.5880 0.112 Uiso 1 1 calc R . . C34 C 0.8240(10) 0.1287(6) 0.6343(4) 0.086(3) Uani 1 1 d . . . H34 H 0.8766 0.1193 0.6724 0.112 Uiso 1 1 calc R . . C35 C 0.7334(12) 0.1842(6) 0.6280(4) 0.089(3) Uani 1 1 d . . . H35 H 0.7218 0.2119 0.6622 0.115 Uiso 1 1 calc R . . C36 C 0.6562(9) 0.2006(5) 0.5702(3) 0.070(2) Uani 1 1 d . . . H36 H 0.5951 0.2395 0.5661 0.090 Uiso 1 1 calc R . . N1 N 0.8626(5) 0.5053(3) 0.6502(2) 0.0431(13) Uani 1 1 d . . . C1A C 0.9970(7) 0.4634(4) 0.6693(3) 0.0486(16) Uani 1 1 d . . . H1A1 H 1.0718 0.4910 0.6563 0.063 Uiso 1 1 calc R . . H1A2 H 1.0142 0.4611 0.7139 0.063 Uiso 1 1 calc R . . C2A C 1.0037(8) 0.3874(4) 0.6448(3) 0.0547(18) Uani 1 1 d . . . H2A1 H 0.9318 0.3585 0.6589 0.071 Uiso 1 1 calc R . . H2A2 H 0.9857 0.3887 0.6001 0.071 Uiso 1 1 calc R . . C3A C 1.1412(8) 0.3518(4) 0.6649(3) 0.063(2) Uani 1 1 d . . . H3A1 H 1.1565 0.3476 0.7094 0.082 Uiso 1 1 calc R . . H3A2 H 1.2137 0.3822 0.6531 0.082 Uiso 1 1 calc R . . C4A C 1.1505(11) 0.2778(5) 0.6371(4) 0.090(3) Uani 1 1 d . . . H4A1 H 1.2407 0.2580 0.6503 0.117 Uiso 1 1 calc R . . H4A2 H 1.1347 0.2816 0.5930 0.117 Uiso 1 1 calc R . . H4A3 H 1.0820 0.2467 0.6503 0.117 Uiso 1 1 calc R . . C1B C 0.8725(7) 0.5768(4) 0.6852(3) 0.0503(17) Uani 1 1 d . . . H1B1 H 0.7843 0.6014 0.6756 0.065 Uiso 1 1 calc R . . H1B2 H 0.8863 0.5661 0.7289 0.065 Uiso 1 1 calc R . . C2B C 0.9839(8) 0.6283(4) 0.6729(4) 0.0598(19) Uani 1 1 d . . . H2B1 H 0.9646 0.6450 0.6306 0.078 Uiso 1 1 calc R . . H2B2 H 1.0720 0.6032 0.6782 0.078 Uiso 1 1 calc R . . C3B C 0.9934(9) 0.6940(4) 0.7167(5) 0.083(3) Uani 1 1 d . . . H3B1 H 0.9099 0.7226 0.7069 0.108 Uiso 1 1 calc R . . H3B2 H 0.9971 0.6765 0.7586 0.108 Uiso 1 1 calc R . . C4B C 1.1128(11) 0.7408(6) 0.7139(6) 0.110(4) Uani 1 1 d . . . H4B1 H 1.1112 0.7804 0.7421 0.143 Uiso 1 1 calc R . . H4B2 H 1.1093 0.7591 0.6728 0.143 Uiso 1 1 calc R . . H4B3 H 1.1963 0.7134 0.7250 0.143 Uiso 1 1 calc R . . C1C C 0.8481(8) 0.5186(4) 0.5804(3) 0.0545(18) Uani 1 1 d . . . H1C1 H 0.9303 0.5435 0.5718 0.071 Uiso 1 1 calc R . . H1C2 H 0.8446 0.4721 0.5597 0.071 Uiso 1 1 calc R . . C2C C 0.7222(9) 0.5623(4) 0.5531(3) 0.063(2) Uani 1 1 d . . . H2C1 H 0.7245 0.6093 0.5728 0.081 Uiso 1 1 calc R . . H2C2 H 0.6388 0.5375 0.5604 0.081 Uiso 1 1 calc R . . C3C C 0.7208(10) 0.5719(6) 0.4840(4) 0.086(3) Uani 1 1 d . . . H3C1 H 0.8028 0.5983 0.4773 0.111 Uiso 1 1 calc R . . H3C2 H 0.7243 0.5246 0.4651 0.111 Uiso 1 1 calc R . . C4C C 0.5939(9) 0.6119(5) 0.4529(4) 0.076(2) Uani 1 1 d . . . H4C1 H 0.5983 0.6166 0.4096 0.098 Uiso 1 1 calc R . . H4C2 H 0.5907 0.6591 0.4708 0.098 Uiso 1 1 calc R . . H4C3 H 0.5124 0.5853 0.4584 0.098 Uiso 1 1 calc R . . C1D C 0.7376(7) 0.4629(4) 0.6657(3) 0.0514(17) Uani 1 1 d . . . H1D1 H 0.6544 0.4896 0.6500 0.067 Uiso 1 1 calc R . . H1D2 H 0.7334 0.4169 0.6443 0.067 Uiso 1 1 calc R . . C2D C 0.7378(8) 0.4485(4) 0.7336(3) 0.066(2) Uani 1 1 d . . . H2D1 H 0.7382 0.4943 0.7552 0.086 Uiso 1 1 calc R . . H2D2 H 0.8216 0.4228 0.7500 0.086 Uiso 1 1 calc R . . C3D C 0.6138(9) 0.4045(5) 0.7458(4) 0.074(2) Uani 1 1 d . . . H3D1 H 0.6205 0.3561 0.7294 0.096 Uiso 1 1 calc R . . H3D2 H 0.5302 0.4266 0.7244 0.096 Uiso 1 1 calc R . . C4D C 0.6033(10) 0.3992(5) 0.8163(5) 0.094(3) Uani 1 1 d . . . H4D1 H 0.5239 0.3708 0.8218 0.122 Uiso 1 1 calc R . . H4D2 H 0.5944 0.4469 0.8326 0.122 Uiso 1 1 calc R . . H4D3 H 0.6851 0.3766 0.8376 0.122 Uiso 1 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 0.04182(15) 0.03891(14) 0.04164(14) 0.00171(11) 0.00713(10) -0.00077(11) I1 0.0580(3) 0.0598(3) 0.0616(3) -0.0098(2) -0.0012(2) -0.0120(2) I2 0.0669(3) 0.0735(3) 0.0423(3) 0.0044(2) -0.0056(2) -0.0081(3) I3 0.0609(3) 0.0478(3) 0.0900(4) 0.0210(3) 0.0205(3) 0.0070(2) As1 0.0474(4) 0.0413(3) 0.0378(3) 0.0029(3) 0.0023(3) -0.0043(3) C11 0.061(5) 0.039(3) 0.047(4) 0.006(3) -0.001(3) -0.001(3) C12 0.059(5) 0.050(4) 0.049(4) 0.013(3) 0.002(3) -0.012(4) C13 0.098(7) 0.035(4) 0.068(5) -0.007(4) -0.004(5) -0.014(4) C14 0.083(6) 0.057(5) 0.065(5) -0.012(4) 0.008(5) 0.012(5) C15 0.082(6) 0.066(5) 0.067(5) -0.015(4) 0.025(4) 0.004(5) C16 0.070(6) 0.050(4) 0.073(5) -0.001(4) 0.023(4) -0.013(4) C21 0.055(4) 0.047(4) 0.035(3) -0.001(3) 0.004(3) 0.000(3) C22 0.066(5) 0.052(4) 0.046(4) 0.001(3) 0.017(4) -0.002(4) C23 0.066(6) 0.073(6) 0.073(5) 0.004(4) 0.026(4) 0.008(4) C24 0.063(5) 0.084(6) 0.069(5) -0.001(5) 0.020(4) 0.000(5) C25 0.092(7) 0.086(7) 0.076(6) 0.024(5) 0.043(5) -0.011(6) C26 0.060(5) 0.078(6) 0.071(5) 0.027(5) 0.009(4) 0.000(4) C31 0.050(4) 0.062(4) 0.042(4) 0.009(3) -0.001(3) -0.013(4) C32 0.059(5) 0.061(5) 0.067(5) 0.009(4) -0.002(4) 0.006(4) C33 0.083(7) 0.088(7) 0.081(7) 0.043(6) -0.007(5) 0.006(5) C34 0.077(7) 0.115(8) 0.057(6) 0.032(6) -0.017(5) -0.021(6) C35 0.112(8) 0.110(8) 0.041(5) 0.004(5) 0.002(5) -0.033(7) C36 0.078(6) 0.078(6) 0.051(5) 0.003(4) 0.002(4) -0.008(5) N1 0.040(3) 0.046(3) 0.042(3) -0.001(2) 0.005(2) 0.002(3) C1A 0.041(4) 0.050(4) 0.053(4) -0.001(3) 0.003(3) 0.002(3) C2A 0.061(5) 0.046(4) 0.056(4) -0.006(3) 0.005(4) 0.007(4) C3A 0.060(5) 0.069(5) 0.058(5) -0.007(4) 0.005(4) 0.016(4) C4A 0.107(8) 0.073(6) 0.090(7) -0.007(5) 0.013(6) 0.035(6) C1B 0.051(4) 0.049(4) 0.050(4) -0.008(3) 0.003(3) 0.001(3) C2B 0.051(4) 0.053(4) 0.077(5) -0.007(4) 0.015(4) -0.008(4) C3B 0.063(6) 0.050(5) 0.138(9) -0.021(5) 0.023(6) -0.007(4) C4B 0.093(8) 0.094(8) 0.150(10) -0.041(7) 0.041(7) -0.021(6) C1C 0.066(5) 0.052(4) 0.044(4) -0.003(3) 0.003(3) 0.008(4) C2C 0.071(5) 0.059(5) 0.057(5) 0.005(4) 0.007(4) 0.009(4) C3C 0.091(7) 0.106(7) 0.056(5) 0.009(5) -0.004(5) 0.032(6) C4C 0.077(6) 0.079(6) 0.069(5) 0.011(5) 0.005(4) 0.015(5) C1D 0.045(4) 0.052(4) 0.055(4) 0.001(3) 0.001(3) -0.004(3) C2D 0.066(5) 0.070(5) 0.062(5) 0.015(4) 0.008(4) -0.011(4) C3D 0.075(6) 0.070(5) 0.078(6) 0.021(5) 0.018(5) -0.007(5) C4D 0.087(7) 0.082(7) 0.116(8) 0.015(6) 0.024(6) 0.004(6) _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 As1 2.3753(8) . ? Pt1 I1 2.6112(9) . ? Pt1 I2 2.6181(9) . ? Pt1 I3 2.6585(7) . ? As1 C21 1.954(7) . ? As1 C31 1.964(6) . ? As1 C11 1.965(7) . ? C11 C12 1.398(9) . ? C11 C16 1.402(10) . ? C12 C13 1.396(11) . ? C13 C14 1.388(12) . ? C14 C15 1.347(11) . ? C15 C16 1.386(11) . ? C21 C22 1.371(10) . ? C21 C26 1.413(10) . ? C22 C23 1.385(11) . ? C23 C24 1.367(11) . ? C24 C25 1.356(12) . ? C25 C26 1.399(12) . ? C31 C32 1.383(10) . ? C31 C36 1.402(11) . ? C32 C33 1.394(11) . ? C33 C34 1.403(14) . ? C34 C35 1.349(14) . ? C35 C36 1.409(11) . ? N1 C1B 1.524(8) . ? N1 C1A 1.529(8) . ? N1 C1D 1.533(9) . ? N1 C1C 1.536(8) . ? C1A C2A 1.509(9) . ? C2A C3A 1.503(10) . ? C3A C4A 1.504(10) . ? C1B C2B 1.502(10) . ? C2B C3B 1.543(11) . ? C3B C4B 1.463(12) . ? C1C C2C 1.519(10) . ? C2C C3C 1.526(11) . ? C3C C4C 1.516(11) . ? C1D C2D 1.513(10) . ? C2D C3D 1.517(11) . ? C3D C4D 1.570(12) . ? 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 As1 Pt1 I1 93.60(2) . . ? As1 Pt1 I2 87.79(2) . . ? I1 Pt1 I2 173.02(2) . . ? As1 Pt1 I3 173.75(2) . . ? I1 Pt1 I3 90.27(2) . . ? I2 Pt1 I3 88.96(2) . . ? C21 As1 C31 99.7(3) . . ? C21 As1 C11 106.8(3) . . ? C31 As1 C11 100.6(3) . . ? C21 As1 Pt1 113.4(2) . . ? C31 As1 Pt1 120.9(2) . . ? C11 As1 Pt1 113.5(2) . . ? C12 C11 C16 118.9(7) . . ? C12 C11 As1 123.2(6) . . ? C16 C11 As1 117.9(5) . . ? C13 C12 C11 118.7(8) . . ? C14 C13 C12 121.8(7) . . ? C15 C14 C13 118.8(8) . . ? C14 C15 C16 121.8(8) . . ? C15 C16 C11 120.0(7) . . ? C22 C21 C26 117.0(7) . . ? C22 C21 As1 122.0(5) . . ? C26 C21 As1 121.0(6) . . ? C21 C22 C23 121.8(7) . . ? C24 C23 C22 121.0(8) . . ? C25 C24 C23 118.9(8) . . ? C24 C25 C26 121.3(8) . . ? C25 C26 C21 120.0(8) . . ? C32 C31 C36 119.5(7) . . ? C32 C31 As1 122.2(6) . . ? C36 C31 As1 118.3(6) . . ? C31 C32 C33 120.1(8) . . ? C32 C33 C34 120.0(9) . . ? C35 C34 C33 120.1(8) . . ? C34 C35 C36 120.8(9) . . ? C31 C36 C35 119.5(9) . . ? C1B N1 C1A 108.3(5) . . ? C1B N1 C1D 108.8(5) . . ? C1A N1 C1D 111.3(5) . . ? C1B N1 C1C 110.7(5) . . ? C1A N1 C1C 107.5(5) . . ? C1D N1 C1C 110.3(5) . . ? C2A C1A N1 117.0(5) . . ? C3A C2A C1A 112.8(6) . . ? C2A C3A C4A 112.7(7) . . ? C2B C1B N1 116.8(6) . . ? C1B C2B C3B 111.2(6) . . ? C4B C3B C2B 114.3(8) . . ? C2C C1C N1 115.2(6) . . ? C1C C2C C3C 109.9(7) . . ? C4C C3C C2C 112.9(8) . . ? C2D C1D N1 115.3(5) . . ? C1D C2D C3D 112.7(6) . . ? C2D C3D C4D 112.4(7) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 31.80 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.632 _refine_diff_density_min -1.544 _refine_diff_density_rms 0.187 _publ_requested_journal 'test' #===END data_compound2 _database_code_CSD 180737 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'compound2' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H20 As I2 N Pt' _chemical_formula_weight 834.21 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.869(3) _cell_length_b 11.283(2) _cell_length_c 16.842(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.83(3) _cell_angle_gamma 90.00 _cell_volume 2393.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5858 _cell_measurement_theta_min 2.188 _cell_measurement_theta_max 29.544 _exptl_crystal_description 'prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 9.822 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.13726 _exptl_absorpt_correction_T_max 0.27807 _exptl_absorpt_process_details 'absorption corrections using SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 23939 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 31.54 _reflns_number_total 7407 _reflns_number_gt 4408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg)' _computing_publication_material '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^)+(0.0657P)^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 'riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7407 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Pt1 Pt 0.848984(19) 0.76721(2) 0.616016(14) 0.04376(10) Uani 1 1 d . . . I1 I 1.05269(4) 0.76946(6) 0.62913(3) 0.07285(18) Uani 1 1 d . . . I2 I 0.64638(4) 0.74993(5) 0.61348(3) 0.0792(2) Uani 1 1 d . . . As As 0.81774(5) 0.76069(6) 0.47323(4) 0.04198(16) Uani 1 1 d . . . N1 N 0.8754(5) 0.7748(5) 0.7437(3) 0.0530(14) Uani 1 1 d . . . C1 C 0.9160(6) 0.6873(9) 0.7897(4) 0.071(2) Uani 1 1 d . . . H1 H 0.9310 0.6176 0.7649 0.085 Uiso 1 1 calc R . . C2 C 0.9374(7) 0.6916(11) 0.8707(5) 0.095(3) Uani 1 1 d . . . H2 H 0.9657 0.6260 0.9010 0.114 Uiso 1 1 calc R . . C3 C 0.9171(7) 0.7935(11) 0.9083(5) 0.094(3) Uani 1 1 d . . . H3 H 0.9313 0.7990 0.9645 0.112 Uiso 1 1 calc R . . C4 C 0.8762(7) 0.8855(10) 0.8620(5) 0.087(3) Uani 1 1 d . . . H4 H 0.8631 0.9568 0.8859 0.104 Uiso 1 1 calc R . . C5 C 0.8537(6) 0.8740(7) 0.7790(4) 0.068(2) Uani 1 1 d . . . H5 H 0.8228 0.9371 0.7471 0.082 Uiso 1 1 calc R . . C11 C 0.7362(5) 0.8922(6) 0.4172(4) 0.0461(14) Uani 1 1 d . . . C12 C 0.7266(5) 0.9019(6) 0.3338(4) 0.0544(17) Uani 1 1 d . . . H12 H 0.7602 0.8480 0.3058 0.065 Uiso 1 1 calc R . . C13 C 0.6654(6) 0.9941(7) 0.2928(4) 0.065(2) Uani 1 1 d . . . H13 H 0.6575 1.0008 0.2369 0.078 Uiso 1 1 calc R . . C14 C 0.6179(7) 1.0734(7) 0.3336(5) 0.080(3) Uani 1 1 d . . . H14 H 0.5767 1.1338 0.3057 0.096 Uiso 1 1 calc R . . C15 C 0.6302(7) 1.0651(7) 0.4176(5) 0.077(2) Uani 1 1 d . . . H15 H 0.5979 1.1201 0.4458 0.092 Uiso 1 1 calc R . . C16 C 0.6906(5) 0.9749(6) 0.4585(4) 0.0576(18) Uani 1 1 d . . . H16 H 0.7005 0.9702 0.5147 0.069 Uiso 1 1 calc R . . C21 C 0.7456(5) 0.6164(6) 0.4313(4) 0.0487(15) Uani 1 1 d . . . C22 C 0.7745(6) 0.5126(7) 0.4728(4) 0.067(2) Uani 1 1 d . . . H22 H 0.8239 0.5148 0.5216 0.081 Uiso 1 1 calc R . . C23 C 0.7319(7) 0.4060(7) 0.4439(5) 0.079(2) Uani 1 1 d . . . H23 H 0.7527 0.3362 0.4721 0.095 Uiso 1 1 calc R . . C24 C 0.6567(7) 0.4042(9) 0.3713(6) 0.085(3) Uani 1 1 d . . . H24 H 0.6263 0.3326 0.3512 0.102 Uiso 1 1 calc R . . C25 C 0.6276(6) 0.5056(8) 0.3298(5) 0.076(2) Uani 1 1 d . . . H25 H 0.5776 0.5031 0.2814 0.091 Uiso 1 1 calc R . . C26 C 0.6714(5) 0.6122(7) 0.3585(4) 0.0601(18) Uani 1 1 d . . . H26 H 0.6515 0.6814 0.3294 0.072 Uiso 1 1 calc R . . C31 C 0.9390(5) 0.7620(6) 0.4211(4) 0.0470(15) Uani 1 1 d . . . C32 C 0.9797(5) 0.6608(7) 0.3937(4) 0.0608(19) Uani 1 1 d . . . H32 H 0.9485 0.5877 0.3990 0.073 Uiso 1 1 calc R . . C33 C 1.0685(7) 0.6686(9) 0.3578(4) 0.076(2) Uani 1 1 d . . . H33 H 1.0965 0.6002 0.3396 0.092 Uiso 1 1 calc R . . C34 C 1.1141(7) 0.7752(10) 0.3492(5) 0.084(3) Uani 1 1 d . . . H34 H 1.1723 0.7793 0.3245 0.101 Uiso 1 1 calc R . . C35 C 1.0755(6) 0.8758(10) 0.3765(5) 0.085(3) Uani 1 1 d . . . H35 H 1.1084 0.9480 0.3718 0.102 Uiso 1 1 calc R . . C36 C 0.9868(6) 0.8711(8) 0.4114(4) 0.066(2) Uani 1 1 d . . . H36 H 0.9591 0.9405 0.4284 0.079 Uiso 1 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 0.04314(15) 0.05827(18) 0.03071(13) 0.00102(10) 0.00950(10) 0.00598(10) I1 0.0446(3) 0.1298(5) 0.0429(3) 0.0058(3) 0.0062(2) 0.0098(3) I2 0.0467(3) 0.1418(6) 0.0518(3) 0.0024(3) 0.0168(2) -0.0015(3) As 0.0417(3) 0.0534(4) 0.0313(3) 0.0006(2) 0.0088(2) 0.0045(3) N1 0.052(3) 0.071(4) 0.039(3) -0.003(3) 0.017(3) 0.000(3) C1 0.070(5) 0.104(7) 0.040(4) 0.008(4) 0.012(3) 0.032(5) C2 0.084(6) 0.153(10) 0.049(5) 0.019(5) 0.017(4) 0.046(6) C3 0.068(6) 0.172(11) 0.038(4) -0.004(5) 0.005(4) 0.008(6) C4 0.089(6) 0.121(9) 0.056(5) -0.031(5) 0.029(5) -0.028(6) C5 0.085(5) 0.073(5) 0.050(4) -0.011(4) 0.020(4) -0.006(4) C11 0.044(3) 0.048(4) 0.043(3) 0.004(3) 0.002(3) 0.004(3) C12 0.065(4) 0.060(5) 0.037(3) 0.005(3) 0.009(3) 0.005(3) C13 0.076(5) 0.065(5) 0.052(4) 0.009(4) 0.008(4) -0.003(4) C14 0.089(6) 0.048(5) 0.089(6) 0.014(4) -0.016(5) -0.004(4) C15 0.089(6) 0.062(5) 0.075(5) -0.009(4) 0.007(5) 0.017(4) C16 0.070(5) 0.053(4) 0.050(4) -0.008(3) 0.011(3) 0.012(3) C21 0.052(4) 0.056(4) 0.041(3) 0.005(3) 0.016(3) 0.003(3) C22 0.079(5) 0.070(5) 0.053(4) 0.006(4) 0.013(4) -0.004(4) C23 0.104(7) 0.059(5) 0.084(6) 0.013(4) 0.044(5) 0.007(5) C24 0.095(7) 0.072(7) 0.099(8) -0.024(5) 0.046(6) -0.011(5) C25 0.074(5) 0.077(6) 0.074(6) -0.021(5) 0.011(4) -0.003(4) C26 0.060(4) 0.062(5) 0.056(4) -0.010(3) 0.007(4) 0.000(3) C31 0.040(3) 0.068(5) 0.032(3) 0.003(3) 0.006(3) 0.008(3) C32 0.051(4) 0.082(6) 0.050(4) -0.017(4) 0.011(3) 0.009(4) C33 0.067(5) 0.110(8) 0.056(5) -0.013(5) 0.022(4) 0.020(5) C34 0.062(5) 0.136(10) 0.059(5) 0.007(5) 0.026(4) 0.012(6) C35 0.056(5) 0.135(9) 0.068(5) 0.034(5) 0.023(4) -0.002(5) C36 0.053(4) 0.087(6) 0.061(5) 0.004(4) 0.020(4) 0.010(4) _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 2.109(5) . ? Pt1 As 2.3567(8) . ? Pt1 I1 2.5855(8) . ? Pt1 I2 2.6062(8) . ? As C21 1.935(7) . ? As C31 1.941(6) . ? As C11 1.946(6) . ? N1 C1 1.297(9) . ? N1 C5 1.324(9) . ? C1 C2 1.336(10) . ? C2 C3 1.363(15) . ? C3 C4 1.339(13) . ? C4 C5 1.373(10) . ? C11 C16 1.366(8) . ? C11 C12 1.389(8) . ? C12 C13 1.399(9) . ? C13 C14 1.350(11) . ? C14 C15 1.394(12) . ? C15 C16 1.377(10) . ? C21 C22 1.376(10) . ? C21 C26 1.392(9) . ? C22 C23 1.369(11) . ? C23 C24 1.395(11) . ? C24 C25 1.353(12) . ? C25 C26 1.373(10) . ? C31 C32 1.375(9) . ? C31 C36 1.401(10) . ? C32 C33 1.401(10) . ? C33 C34 1.359(13) . ? C34 C35 1.356(13) . ? C35 C36 1.387(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 Pt1 As 179.24(16) . . ? N1 Pt1 I1 87.94(16) . . ? As Pt1 I1 92.60(4) . . ? N1 Pt1 I2 88.34(16) . . ? As Pt1 I2 91.15(4) . . ? I1 Pt1 I2 174.63(2) . . ? C21 As C31 102.2(3) . . ? C21 As C11 107.1(3) . . ? C31 As C11 100.3(3) . . ? C21 As Pt1 111.57(18) . . ? C31 As Pt1 118.46(19) . . ? C11 As Pt1 115.66(18) . . ? C1 N1 C5 118.1(7) . . ? C1 N1 Pt1 122.6(5) . . ? C5 N1 Pt1 119.2(5) . . ? N1 C1 C2 123.8(9) . . ? C1 C2 C3 119.0(10) . . ? C4 C3 C2 118.3(8) . . ? C3 C4 C5 119.6(9) . . ? N1 C5 C4 121.1(8) . . ? C16 C11 C12 120.2(6) . . ? C16 C11 As 121.3(5) . . ? C12 C11 As 118.5(5) . . ? C11 C12 C13 118.9(6) . . ? C14 C13 C12 120.6(7) . . ? C13 C14 C15 120.2(7) . . ? C16 C15 C14 119.6(7) . . ? C11 C16 C15 120.5(7) . . ? C22 C21 C26 118.9(7) . . ? C22 C21 As 118.1(5) . . ? C26 C21 As 122.8(5) . . ? C23 C22 C21 121.3(8) . . ? C22 C23 C24 118.7(8) . . ? C25 C24 C23 120.6(9) . . ? C24 C25 C26 120.6(8) . . ? C25 C26 C21 119.9(8) . . ? C32 C31 C36 118.9(7) . . ? C32 C31 As 122.8(6) . . ? C36 C31 As 118.2(5) . . ? C31 C32 C33 119.6(8) . . ? C34 C33 C32 120.6(8) . . ? C35 C34 C33 120.6(9) . . ? C34 C35 C36 120.1(9) . . ? C35 C36 C31 120.2(8) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 31.54 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.589 _refine_diff_density_min -2.422 _refine_diff_density_rms 0.214