# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Doerrer, Linda' 'Baddour, Frederick' 'Kahn, Michael' 'Golen, James' 'Rheingold, Arnold' _publ_contact_author_name 'Linda Doerrer' _publ_contact_author_address ; Contact Address: 590 Commonwealth Ave SCI 383 Boston Massachusetts United States 02215 ; _publ_contact_author_email doerrer@bu.edu _publ_section_title ;Synthesis, Solution and Structural Characterization of Platinum(IV)-terpyridine Complexes ; data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 768818' #TrackingRef 'Baddour-Doerrer-et-al---five-CIFs-and-CheckCIF-report.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H39 Cl6 N3 Pt' _chemical_formula_weight 837.42 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' 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 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 12.6476(8) _cell_length_b 18.6217(12) _cell_length_c 14.8974(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.1010(10) _cell_angle_gamma 90.00 _cell_volume 3402.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9903 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.47 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 4.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2956 _exptl_absorpt_correction_T_max 0.3170 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 20063 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.47 _reflns_number_total 6302 _reflns_number_gt 5570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; SQUEEZE used to render one molecule of CH2Cl2 per Pt complex. One also found and refined. 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. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 274 89 2 0.500 0.000 0.500 274 90 _platon_squeeze_details ; SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent contributions. Total electron count found = 179/unit cell. calculated for 4 CH2Cl2 (the re'xtal solvent) = 168/unit cell. The intensive properties (density, F(000), etc.) reflect these contributions. ; _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^)+(0.1000P)^2^+2.6500P] 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 6302 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1437 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 2.109 _refine_ls_shift/su_mean 0.085 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 0.327960(6) 0.971283(4) 0.042866(6) 0.01485(3) Uani 1 1 d . . . Cl1 Cl 0.22484(4) 1.05984(3) 0.08822(5) 0.02304(16) Uani 1 1 d . . . Cl2 Cl 0.30406(4) 0.71557(3) -0.30025(4) 0.02149(15) Uani 1 1 d . . . Cl3 Cl 0.92082(8) 1.24023(5) -0.04532(7) 0.0582(3) Uani 1 1 d . . . Cl4 Cl 0.92641(7) 1.10283(4) -0.13712(6) 0.0479(2) Uani 1 1 d . . . N1 N 0.47024(15) 0.98974(11) 0.13573(15) 0.0176(5) Uani 1 1 d . . . N2 N 0.41479(14) 0.89816(10) 0.00449(14) 0.0159(5) Uani 1 1 d . . . N3 N 0.21143(15) 0.92546(10) -0.05797(14) 0.0178(5) Uani 1 1 d . . . C1 C 0.4929(2) 1.03847(12) 0.2025(2) 0.0217(7) Uani 1 1 d . . . H1A H 0.4394 1.0737 0.2051 0.026 Uiso 1 1 calc R . . C2 C 0.5894(2) 1.04025(13) 0.2676(2) 0.0224(7) Uani 1 1 d . . . H2A H 0.6018 1.0764 0.3139 0.027 Uiso 1 1 calc R . . C3 C 0.66976(19) 0.98973(13) 0.26682(18) 0.0195(6) Uani 1 1 d . . . C4 C 0.65038(17) 0.94149(12) 0.19276(17) 0.0157(6) Uani 1 1 d . . . H4A H 0.7047 0.9071 0.1892 0.019 Uiso 1 1 calc R . . C5 C 0.55308(18) 0.94249(13) 0.12368(16) 0.0169(6) Uani 1 1 d . . . C6 C 0.52106(17) 0.89227(11) 0.04880(17) 0.0140(6) Uani 1 1 d . . . C7 C 0.58754(17) 0.84213(12) 0.01830(17) 0.0161(6) Uani 1 1 d . . . H7A H 0.6623 0.8373 0.0494 0.019 Uiso 1 1 calc R . . C8 C 0.54158(17) 0.79915(12) -0.05906(17) 0.0156(6) Uani 1 1 d . . . C9 C 0.42888(18) 0.80653(12) -0.10177(18) 0.0179(6) Uani 1 1 d . . . H9A H 0.3961 0.7775 -0.1535 0.021 Uiso 1 1 calc R . . C10 C 0.36710(17) 0.85588(11) -0.06795(18) 0.0167(6) Uani 1 1 d . . . C11 C 0.24839(17) 0.86966(12) -0.10092(16) 0.0150(6) Uani 1 1 d . . . C12 C 0.17892(19) 0.82826(13) -0.16602(18) 0.0204(6) Uani 1 1 d . . . H12A H 0.2074 0.7909 -0.1968 0.024 Uiso 1 1 calc R . . C13 C 0.06650(18) 0.84091(13) -0.18714(17) 0.0195(6) Uani 1 1 d . . . C14 C 0.03188(19) 0.89855(13) -0.14342(19) 0.0235(7) Uani 1 1 d . . . H14A H -0.0435 0.9103 -0.1577 0.028 Uiso 1 1 calc R . . C15 C 0.10392(18) 0.93931(13) -0.07975(18) 0.0192(6) Uani 1 1 d . . . H15A H 0.0771 0.9782 -0.0504 0.023 Uiso 1 1 calc R . . C16 C 0.7742(2) 0.98375(13) 0.3443(2) 0.0237(7) Uani 1 1 d . . . C17 C 0.7857(2) 1.04641(16) 0.4136(2) 0.0340(8) Uani 1 1 d . . . H17A H 0.7909 1.0918 0.3816 0.051 Uiso 1 1 calc R . . H17B H 0.8517 1.0396 0.4634 0.051 Uiso 1 1 calc R . . H17C H 0.7219 1.0477 0.4400 0.051 Uiso 1 1 calc R . . C18 C 0.7666(2) 0.91258(15) 0.3970(2) 0.0329(8) Uani 1 1 d . . . H18A H 0.7603 0.8720 0.3541 0.049 Uiso 1 1 calc R . . H18B H 0.7024 0.9140 0.4228 0.049 Uiso 1 1 calc R . . H18C H 0.8323 0.9068 0.4473 0.049 Uiso 1 1 calc R . . C19 C 0.8742(2) 0.98160(14) 0.3046(2) 0.0262(8) Uani 1 1 d . . . H19A H 0.8791 1.0265 0.2716 0.039 Uiso 1 1 calc R . . H19B H 0.8680 0.9411 0.2616 0.039 Uiso 1 1 calc R . . H19C H 0.9397 0.9758 0.3551 0.039 Uiso 1 1 calc R . . C20 C 0.60834(17) 0.74429(12) -0.09978(17) 0.0163(6) Uani 1 1 d . . . C21 C 0.72659(19) 0.73936(13) -0.0417(2) 0.0237(7) Uani 1 1 d . . . H21A H 0.7618 0.7863 -0.0404 0.036 Uiso 1 1 calc R . . H21B H 0.7664 0.7038 -0.0692 0.036 Uiso 1 1 calc R . . H21C H 0.7269 0.7248 0.0216 0.036 Uiso 1 1 calc R . . C22 C 0.60705(19) 0.76711(13) -0.19764(17) 0.0206(6) Uani 1 1 d . . . H22A H 0.6414 0.8144 -0.1964 0.031 Uiso 1 1 calc R . . H22B H 0.5315 0.7697 -0.2345 0.031 Uiso 1 1 calc R . . H22C H 0.6474 0.7320 -0.2253 0.031 Uiso 1 1 calc R . . C23 C 0.5545(2) 0.67001(12) -0.10119(19) 0.0224(7) Uani 1 1 d . . . H23A H 0.5963 0.6345 -0.1268 0.034 Uiso 1 1 calc R . . H23B H 0.4798 0.6721 -0.1397 0.034 Uiso 1 1 calc R . . H23C H 0.5533 0.6562 -0.0380 0.034 Uiso 1 1 calc R . . C24 C -0.01115(18) 0.79338(14) -0.25732(18) 0.0229(7) Uani 1 1 d . . . C25 C 0.0012(2) 0.81214(17) -0.3547(2) 0.0347(8) Uani 1 1 d . . . H25A H -0.0179 0.8627 -0.3681 0.052 Uiso 1 1 calc R . . H25B H -0.0474 0.7816 -0.4004 0.052 Uiso 1 1 calc R . . H25C H 0.0768 0.8041 -0.3577 0.052 Uiso 1 1 calc R . . C26 C 0.0186(2) 0.71437(14) -0.2377(2) 0.0342(8) Uani 1 1 d . . . H26A H 0.0112 0.7019 -0.1756 0.051 Uiso 1 1 calc R . . H26B H 0.0940 0.7064 -0.2413 0.051 Uiso 1 1 calc R . . H26C H -0.0304 0.6842 -0.2836 0.051 Uiso 1 1 calc R . . C27 C -0.1300(2) 0.80434(18) -0.2524(3) 0.0437(9) Uani 1 1 d . . . H27A H -0.1505 0.8548 -0.2651 0.066 Uiso 1 1 calc R . . H27B H -0.1376 0.7916 -0.1904 0.066 Uiso 1 1 calc R . . H27C H -0.1779 0.7737 -0.2985 0.066 Uiso 1 1 calc R . . C28 C 1.0046(2) 1.17385(16) -0.0758(2) 0.0367(9) Uani 1 1 d . . . H28A H 1.0545 1.1547 -0.0190 0.044 Uiso 1 1 calc R . . H28B H 1.0495 1.1955 -0.1146 0.044 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 0.01178(5) 0.01405(5) 0.01900(5) -0.00071(3) 0.00427(4) 0.00173(3) Cl1 0.0170(2) 0.0201(3) 0.0327(3) -0.0056(2) 0.0075(2) 0.0031(2) Cl2 0.0157(2) 0.0257(3) 0.0210(3) -0.0048(2) 0.0004(2) -0.0016(2) Cl3 0.0780(5) 0.0570(5) 0.0432(5) 0.0044(4) 0.0216(4) 0.0233(4) Cl4 0.0502(4) 0.0441(4) 0.0453(5) 0.0084(4) 0.0039(4) -0.0072(3) N1 0.0183(8) 0.0165(8) 0.0222(11) -0.0058(8) 0.0128(7) 0.0030(8) N2 0.0115(8) 0.0156(8) 0.0194(10) -0.0009(8) 0.0017(7) 0.0036(7) N3 0.0150(8) 0.0221(9) 0.0163(10) -0.0009(8) 0.0037(7) -0.0001(8) C1 0.0183(11) 0.0151(10) 0.0328(15) -0.0035(10) 0.0083(10) 0.0015(9) C2 0.0232(11) 0.0214(11) 0.0215(13) -0.0066(10) 0.0035(10) -0.0018(10) C3 0.0180(10) 0.0199(10) 0.0205(12) 0.0045(10) 0.0046(9) -0.0081(9) C4 0.0103(9) 0.0145(10) 0.0220(12) 0.0064(9) 0.0033(8) -0.0016(8) C5 0.0196(10) 0.0219(11) 0.0128(11) -0.0085(9) 0.0110(8) 0.0033(9) C6 0.0125(9) 0.0103(9) 0.0187(11) 0.0021(9) 0.0028(8) 0.0003(8) C7 0.0108(9) 0.0185(10) 0.0187(12) 0.0007(9) 0.0032(8) -0.0008(8) C8 0.0128(9) 0.0151(10) 0.0178(12) -0.0013(9) 0.0012(8) 0.0025(8) C9 0.0141(9) 0.0161(10) 0.0223(12) -0.0021(10) 0.0021(9) -0.0012(9) C10 0.0107(9) 0.0133(9) 0.0256(13) 0.0021(9) 0.0039(9) -0.0004(8) C11 0.0140(9) 0.0193(10) 0.0141(11) -0.0024(9) 0.0080(8) 0.0005(8) C12 0.0161(10) 0.0210(11) 0.0230(13) -0.0024(10) 0.0028(9) 0.0031(9) C13 0.0160(9) 0.0247(11) 0.0191(12) 0.0019(10) 0.0066(9) 0.0042(9) C14 0.0135(9) 0.0255(12) 0.0321(14) 0.0015(11) 0.0065(9) 0.0027(9) C15 0.0133(9) 0.0213(11) 0.0220(13) -0.0060(10) 0.0023(9) 0.0072(9) C16 0.0222(12) 0.0248(11) 0.0208(14) -0.0076(11) -0.0010(11) -0.0013(10) C17 0.0276(14) 0.0377(13) 0.0296(16) -0.0133(13) -0.0068(12) -0.0011(12) C18 0.0323(13) 0.0333(14) 0.0286(15) 0.0029(13) -0.0013(12) -0.0043(12) C19 0.0212(12) 0.0242(11) 0.0316(16) -0.0035(11) 0.0034(11) -0.0034(10) C20 0.0115(9) 0.0141(10) 0.0229(12) -0.0016(9) 0.0036(9) 0.0009(8) C21 0.0153(10) 0.0236(11) 0.0292(14) -0.0033(11) -0.0004(10) 0.0046(9) C22 0.0170(10) 0.0257(11) 0.0193(12) -0.0031(10) 0.0047(9) 0.0035(9) C23 0.0233(11) 0.0166(10) 0.0274(13) -0.0008(10) 0.0063(10) 0.0024(9) C24 0.0109(9) 0.0342(13) 0.0227(13) -0.0045(11) 0.0024(9) -0.0002(10) C25 0.0322(14) 0.0440(15) 0.0244(15) -0.0031(13) 0.0001(12) -0.0090(12) C26 0.0281(13) 0.0268(12) 0.0433(18) -0.0092(13) 0.0000(12) -0.0082(11) C27 0.0142(11) 0.0565(17) 0.060(2) -0.0287(15) 0.0073(12) -0.0037(12) C28 0.0263(13) 0.0393(15) 0.0441(18) 0.0026(14) 0.0078(12) -0.0005(12) _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 N2 1.922(2) . ? Pt1 N1 2.0142(18) . ? Pt1 N3 2.0195(18) . ? Pt1 Cl1 2.3035(6) . ? Cl3 C28 1.758(3) . ? Cl4 C28 1.767(3) . ? N1 C1 1.325(3) . ? N1 C5 1.413(3) . ? N2 C6 1.350(3) . ? N2 C10 1.353(3) . ? N3 C15 1.344(3) . ? N3 C11 1.361(3) . ? C1 C2 1.362(3) . ? C2 C3 1.387(4) . ? C3 C4 1.397(3) . ? C3 C16 1.532(3) . ? C4 C5 1.399(3) . ? C5 C6 1.436(3) . ? C6 C7 1.404(3) . ? C7 C8 1.407(3) . ? C8 C9 1.419(3) . ? C8 C20 1.541(3) . ? C9 C10 1.379(3) . ? C10 C11 1.484(3) . ? C11 C12 1.375(3) . ? C12 C13 1.399(3) . ? C13 C14 1.381(4) . ? C13 C24 1.530(3) . ? C14 C15 1.373(3) . ? C16 C19 1.521(4) . ? C16 C17 1.541(4) . ? C16 C18 1.555(4) . ? C20 C22 1.515(4) . ? C20 C21 1.537(3) . ? C20 C23 1.539(3) . ? C24 C26 1.529(4) . ? C24 C25 1.537(4) . ? C24 C27 1.537(4) . ? 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 N2 Pt1 N1 81.12(8) . . ? N2 Pt1 N3 81.12(8) . . ? N1 Pt1 N3 161.99(8) . . ? N2 Pt1 Cl1 179.40(6) . . ? N1 Pt1 Cl1 98.71(6) . . ? N3 Pt1 Cl1 99.09(6) . . ? C1 N1 C5 119.38(19) . . ? C1 N1 Pt1 128.74(17) . . ? C5 N1 Pt1 111.88(15) . . ? C6 N2 C10 122.7(2) . . ? C6 N2 Pt1 119.02(15) . . ? C10 N2 Pt1 118.26(14) . . ? C15 N3 C11 118.43(19) . . ? C15 N3 Pt1 127.64(17) . . ? C11 N3 Pt1 113.59(14) . . ? N1 C1 C2 122.9(2) . . ? C1 C2 C3 120.6(2) . . ? C2 C3 C4 117.0(2) . . ? C2 C3 C16 122.8(2) . . ? C4 C3 C16 120.1(2) . . ? C3 C4 C5 121.7(2) . . ? C4 C5 N1 117.5(2) . . ? C4 C5 C6 126.4(2) . . ? N1 C5 C6 115.26(18) . . ? N2 C6 C7 119.9(2) . . ? N2 C6 C5 112.7(2) . . ? C7 C6 C5 127.35(19) . . ? C6 C7 C8 118.87(19) . . ? C7 C8 C9 118.8(2) . . ? C7 C8 C20 122.88(19) . . ? C9 C8 C20 118.3(2) . . ? C10 C9 C8 119.8(2) . . ? N2 C10 C9 119.81(19) . . ? N2 C10 C11 112.4(2) . . ? C9 C10 C11 127.7(2) . . ? N3 C11 C12 121.7(2) . . ? N3 C11 C10 114.33(19) . . ? C12 C11 C10 123.9(2) . . ? C11 C12 C13 120.2(2) . . ? C14 C13 C12 116.5(2) . . ? C14 C13 C24 123.2(2) . . ? C12 C13 C24 120.3(2) . . ? C15 C14 C13 121.5(2) . . ? N3 C15 C14 121.5(2) . . ? C19 C16 C3 110.7(2) . . ? C19 C16 C17 109.2(2) . . ? C3 C16 C17 111.9(2) . . ? C19 C16 C18 109.5(2) . . ? C3 C16 C18 107.1(2) . . ? C17 C16 C18 108.4(2) . . ? C22 C20 C21 109.9(2) . . ? C22 C20 C23 109.7(2) . . ? C21 C20 C23 108.68(18) . . ? C22 C20 C8 108.33(18) . . ? C21 C20 C8 111.66(19) . . ? C23 C20 C8 108.6(2) . . ? C26 C24 C13 109.8(2) . . ? C26 C24 C25 108.8(2) . . ? C13 C24 C25 108.5(2) . . ? C26 C24 C27 108.5(2) . . ? C13 C24 C27 111.3(2) . . ? C25 C24 C27 109.9(2) . . ? Cl3 C28 Cl4 111.30(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.730 _refine_diff_density_min -3.740 _refine_diff_density_rms 0.233 #===END data_Compound-2 _database_code_depnum_ccdc_archive 'CCDC 768819' #TrackingRef 'Baddour-Doerrer-et-al---five-CIFs-and-CheckCIF-report.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H39 Au Cl9 N3 Pt' _chemical_formula_weight 1140.74 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' 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 21.7744(18) _cell_length_b 12.4046(10) _cell_length_c 28.889(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7802.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9321 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.68 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.942 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352 _exptl_absorpt_coefficient_mu 7.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5026 _exptl_absorpt_correction_T_max 0.7408 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52082 _diffrn_reflns_av_R_equivalents 0.1452 _diffrn_reflns_av_sigmaI/netI 0.1152 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.90 _reflns_number_total 9219 _reflns_number_gt 5175 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0556P)^2^+33.9355P] 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 9219 _refine_ls_number_parameters 386 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.1406 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _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 Au1 Au 0.55061(2) 0.28623(6) 0.91878(3) 0.0751(3) Uani 1 1 d . . . Pt1 Pt 0.740522(17) 0.63052(3) 0.239518(16) 0.02817(13) Uani 1 1 d . . . Cl1 Cl 0.83344(12) 0.5401(2) 0.24168(12) 0.0432(7) Uani 1 1 d . . . Cl2 Cl 0.69306(13) 0.4965(2) 0.28262(11) 0.0405(7) Uani 1 1 d . . . Cl3 Cl 0.78350(13) 0.7651(2) 0.19483(12) 0.0433(8) Uani 1 1 d . . . Cl4 Cl 0.54775(19) 0.1479(5) 0.96968(19) 0.0962(16) Uani 1 1 d . . . Cl5 Cl 0.55525(16) 0.4207(4) 0.86595(16) 0.0803(13) Uani 1 1 d . . . Cl6 Cl 0.9480(3) 0.1529(7) 0.3668(3) 0.152(3) Uani 1 1 d . . . Cl7 Cl 0.9064(2) 0.2269(5) 0.4533(3) 0.125(2) Uani 1 1 d . . . Cl8 Cl 0.8862(4) 0.5369(11) 0.1022(4) 0.260(6) Uani 1 1 d . . . Cl9 Cl 0.8547(4) 0.3227(6) 0.0830(4) 0.204(5) Uani 1 1 d . . . N1 N 0.7501(3) 0.7192(7) 0.2977(3) 0.031(2) Uani 1 1 d . . . N2 N 0.6613(4) 0.7050(6) 0.2388(3) 0.0251(19) Uani 1 1 d . . . N3 N 0.7064(4) 0.5657(7) 0.1807(3) 0.032(2) Uani 1 1 d . . . C1 C 0.7987(4) 0.7211(9) 0.3267(4) 0.036(3) Uani 1 1 d . . . H1 H 0.8335 0.6771 0.3205 0.043 Uiso 1 1 calc R . . C1S C 0.9552(8) 0.1355(15) 0.4265(7) 0.084(6) Uani 1 1 d . . . H28A H 0.9439 0.0609 0.4352 0.101 Uiso 1 1 calc R . . H28B H 0.9982 0.1487 0.4361 0.101 Uiso 1 1 calc R . . C2 C 0.7980(5) 0.7867(10) 0.3653(4) 0.040(3) Uani 1 1 d . . . H2 H 0.8332 0.7887 0.3846 0.048 Uiso 1 1 calc R . . C2S C 0.8918(12) 0.447(2) 0.0602(10) 0.189(15) Uani 1 1 d . . . H2S1 H 0.9354 0.4335 0.0525 0.227 Uiso 1 1 calc R . . H2S2 H 0.8704 0.4729 0.0320 0.227 Uiso 1 1 calc R . . C3 C 0.7481(5) 0.8494(9) 0.3767(5) 0.038(3) Uani 1 1 d . . . C4 C 0.6978(5) 0.8462(9) 0.3459(4) 0.034(3) Uani 1 1 d . . . H4 H 0.6624 0.8889 0.3517 0.041 Uiso 1 1 calc R . . C5 C 0.7001(5) 0.7800(9) 0.3067(4) 0.034(3) Uani 1 1 d . . . C6 C 0.7498(5) 0.9237(11) 0.4182(5) 0.042(3) Uani 1 1 d . . . C7 C 0.8065(7) 0.9980(12) 0.4142(6) 0.067(5) Uani 1 1 d . . . H7A H 0.8437 0.9539 0.4116 0.101 Uiso 1 1 calc R . . H7B H 0.8093 1.0435 0.4419 0.101 Uiso 1 1 calc R . . H7C H 0.8025 1.0436 0.3867 0.101 Uiso 1 1 calc R . . C8 C 0.7586(7) 0.8517(13) 0.4611(5) 0.067(4) Uani 1 1 d . . . H8A H 0.7962 0.8089 0.4576 0.100 Uiso 1 1 calc R . . H8B H 0.7233 0.8034 0.4644 0.100 Uiso 1 1 calc R . . H8C H 0.7620 0.8971 0.4888 0.100 Uiso 1 1 calc R . . C9 C 0.6920(6) 0.9940(13) 0.4222(5) 0.061(4) Uani 1 1 d . . . H9A H 0.6879 1.0387 0.3944 0.092 Uiso 1 1 calc R . . H9B H 0.6955 1.0405 0.4495 0.092 Uiso 1 1 calc R . . H9C H 0.6558 0.9477 0.4253 0.092 Uiso 1 1 calc R . . C10 C 0.6490(4) 0.7717(9) 0.2721(4) 0.031(3) Uani 1 1 d . . . C11 C 0.5929(4) 0.8222(9) 0.2739(4) 0.029(3) Uani 1 1 d . . . H11 H 0.5833 0.8700 0.2986 0.035 Uiso 1 1 calc R . . C12 C 0.5500(4) 0.8018(9) 0.2387(4) 0.032(3) Uani 1 1 d . A . C13 C 0.5649(4) 0.7295(9) 0.2039(4) 0.030(3) Uani 1 1 d . . . H13 H 0.5360 0.7138 0.1802 0.037 Uiso 1 1 calc R . . C14 C 0.6221(5) 0.6800(8) 0.2037(4) 0.030(3) Uani 1 1 d . . . C15 C 0.4882(4) 0.8603(9) 0.2385(4) 0.040(3) Uani 1 1 d D . . C16 C 0.4526(10) 0.8355(18) 0.2820(6) 0.056(7) Uiso 0.60(2) 1 d PDU A 1 H16A H 0.4779 0.8527 0.3091 0.084 Uiso 0.60(2) 1 calc PR A 1 H16B H 0.4418 0.7588 0.2826 0.084 Uiso 0.60(2) 1 calc PR A 1 H16C H 0.4150 0.8790 0.2827 0.084 Uiso 0.60(2) 1 calc PR A 1 C16A C 0.4399(14) 0.777(2) 0.2476(12) 0.063(11) Uiso 0.40(2) 1 d PDU A 2 H16D H 0.4456 0.7163 0.2265 0.094 Uiso 0.40(2) 1 calc PR A 2 H16E H 0.3992 0.8092 0.2426 0.094 Uiso 0.40(2) 1 calc PR A 2 H16F H 0.4431 0.7524 0.2797 0.094 Uiso 0.40(2) 1 calc PR A 2 C17 C 0.4985(9) 0.9804(12) 0.2380(8) 0.045(6) Uiso 0.60(2) 1 d PDU A 1 H17A H 0.5255 1.0003 0.2638 0.067 Uiso 0.60(2) 1 calc PR A 1 H17B H 0.4591 1.0176 0.2413 0.067 Uiso 0.60(2) 1 calc PR A 1 H17C H 0.5178 1.0013 0.2087 0.067 Uiso 0.60(2) 1 calc PR A 1 C17A C 0.4822(15) 0.954(2) 0.2701(10) 0.054(10) Uiso 0.40(2) 1 d PDU A 2 H17D H 0.5140 1.0073 0.2627 0.080 Uiso 0.40(2) 1 calc PR A 2 H17E H 0.4873 0.9298 0.3021 0.080 Uiso 0.40(2) 1 calc PR A 2 H17F H 0.4416 0.9866 0.2662 0.080 Uiso 0.40(2) 1 calc PR A 2 C18 C 0.4475(10) 0.8323(18) 0.1986(6) 0.056(7) Uiso 0.60(2) 1 d PDU A 1 H18A H 0.4689 0.8481 0.1695 0.085 Uiso 0.60(2) 1 calc PR A 1 H18B H 0.4097 0.8750 0.2003 0.085 Uiso 0.60(2) 1 calc PR A 1 H18C H 0.4373 0.7554 0.1998 0.085 Uiso 0.60(2) 1 calc PR A 1 C18A C 0.4756(17) 0.902(3) 0.1899(7) 0.068(12) Uiso 0.40(2) 1 d PDU A 2 H18D H 0.4788 0.8419 0.1678 0.101 Uiso 0.40(2) 1 calc PR A 2 H18E H 0.5057 0.9574 0.1820 0.101 Uiso 0.40(2) 1 calc PR A 2 H18F H 0.4341 0.9322 0.1886 0.101 Uiso 0.40(2) 1 calc PR A 2 C19 C 0.6473(5) 0.5995(8) 0.1712(4) 0.030(3) Uani 1 1 d . . . C20 C 0.6170(5) 0.5578(9) 0.1332(4) 0.032(3) Uani 1 1 d . . . H20 H 0.5760 0.5796 0.1272 0.038 Uiso 1 1 calc R . . C21 C 0.6455(5) 0.4840(9) 0.1034(4) 0.032(3) Uani 1 1 d . . . C22 C 0.7051(5) 0.4555(9) 0.1134(4) 0.034(3) Uani 1 1 d . . . H22 H 0.7267 0.4077 0.0935 0.041 Uiso 1 1 calc R . . C23 C 0.7341(5) 0.4970(9) 0.1530(4) 0.037(3) Uani 1 1 d . . . H23 H 0.7749 0.4749 0.1600 0.044 Uiso 1 1 calc R . . C24 C 0.6109(5) 0.4351(10) 0.0626(4) 0.041(3) Uani 1 1 d . . . C25 C 0.5544(6) 0.3724(12) 0.0810(5) 0.065(4) Uani 1 1 d . . . H25A H 0.5282 0.4212 0.0989 0.098 Uiso 1 1 calc R . . H25B H 0.5683 0.3130 0.1008 0.098 Uiso 1 1 calc R . . H25C H 0.5310 0.3432 0.0548 0.098 Uiso 1 1 calc R . . C26 C 0.5900(6) 0.5276(12) 0.0313(4) 0.055(4) Uani 1 1 d . . . H26A H 0.5645 0.5778 0.0491 0.083 Uiso 1 1 calc R . . H26B H 0.5660 0.4986 0.0054 0.083 Uiso 1 1 calc R . . H26C H 0.6260 0.5658 0.0192 0.083 Uiso 1 1 calc R . . C27 C 0.6511(6) 0.3572(11) 0.0356(5) 0.059(4) Uani 1 1 d . . . H27A H 0.6647 0.2989 0.0561 0.088 Uiso 1 1 calc R . . H27B H 0.6870 0.3956 0.0235 0.088 Uiso 1 1 calc R . . H27C H 0.6275 0.3269 0.0098 0.088 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 Au1 0.0312(3) 0.1109(6) 0.0832(5) -0.0537(4) -0.0016(3) 0.0020(3) Pt1 0.01943(19) 0.0253(2) 0.0397(3) 0.0006(2) -0.00003(18) 0.00222(17) Cl1 0.0235(13) 0.0439(17) 0.062(2) -0.0051(16) -0.0026(13) 0.0084(12) Cl2 0.0341(14) 0.0363(16) 0.051(2) 0.0063(14) 0.0018(13) -0.0026(12) Cl3 0.0355(15) 0.0390(17) 0.055(2) 0.0077(15) 0.0044(13) -0.0062(13) Cl4 0.062(3) 0.125(4) 0.102(4) -0.040(3) 0.006(2) -0.013(3) Cl5 0.0412(19) 0.111(4) 0.089(3) -0.033(3) -0.0111(19) 0.007(2) Cl6 0.139(6) 0.217(8) 0.101(5) -0.003(5) -0.006(4) -0.012(5) Cl7 0.080(3) 0.104(4) 0.192(7) -0.044(4) 0.006(4) 0.010(3) Cl8 0.151(7) 0.335(15) 0.294(13) -0.089(12) 0.114(8) -0.104(9) Cl9 0.164(7) 0.106(5) 0.342(13) 0.032(7) 0.123(8) 0.047(5) N1 0.017(4) 0.039(5) 0.036(6) 0.003(5) 0.002(3) -0.006(4) N2 0.025(4) 0.014(4) 0.036(6) -0.002(4) 0.002(4) 0.003(3) N3 0.028(5) 0.030(5) 0.038(6) 0.001(5) 0.003(4) -0.006(4) C1 0.012(5) 0.044(7) 0.051(8) 0.006(6) -0.008(5) -0.008(5) C1S 0.067(11) 0.084(13) 0.101(16) 0.010(11) -0.002(9) 0.020(10) C2 0.033(6) 0.052(8) 0.034(8) 0.000(6) -0.019(5) -0.004(6) C2S 0.16(2) 0.23(3) 0.17(3) -0.07(3) 0.14(2) -0.09(2) C3 0.032(6) 0.033(6) 0.050(8) -0.005(6) 0.000(5) -0.009(5) C4 0.022(5) 0.030(6) 0.051(8) 0.007(6) 0.001(5) 0.002(5) C5 0.026(6) 0.032(6) 0.044(8) -0.005(6) 0.001(5) 0.001(5) C6 0.040(7) 0.048(7) 0.039(8) -0.012(6) -0.006(5) 0.010(6) C7 0.070(10) 0.051(9) 0.081(12) -0.010(8) -0.016(8) -0.028(8) C8 0.075(10) 0.076(11) 0.050(10) -0.003(8) -0.004(8) -0.012(9) C9 0.046(8) 0.091(12) 0.047(10) -0.024(8) -0.011(6) 0.012(8) C10 0.016(5) 0.037(6) 0.038(8) -0.004(6) -0.002(4) -0.005(4) C11 0.012(4) 0.034(6) 0.042(8) -0.009(5) 0.002(4) 0.004(4) C12 0.015(5) 0.038(6) 0.045(7) 0.001(6) -0.005(5) -0.004(4) C13 0.021(5) 0.031(6) 0.039(7) -0.003(5) -0.005(4) 0.000(4) C14 0.023(5) 0.028(6) 0.040(8) -0.010(5) 0.001(5) -0.008(4) C15 0.023(5) 0.044(7) 0.053(8) -0.014(7) -0.008(5) 0.010(5) C19 0.028(6) 0.024(6) 0.039(7) -0.002(5) 0.002(5) 0.004(4) C20 0.031(6) 0.033(6) 0.031(7) -0.004(5) -0.009(5) 0.002(5) C21 0.037(6) 0.032(6) 0.029(7) 0.002(5) 0.002(5) -0.003(5) C22 0.034(6) 0.036(7) 0.034(7) 0.002(6) 0.004(5) 0.003(5) C23 0.025(5) 0.038(7) 0.047(8) -0.002(6) 0.008(5) 0.011(5) C24 0.034(6) 0.046(8) 0.045(8) -0.003(6) 0.000(5) -0.006(6) C25 0.061(9) 0.061(9) 0.074(12) -0.028(9) 0.014(8) -0.025(8) C26 0.067(9) 0.069(10) 0.031(8) -0.012(7) 0.005(6) 0.005(8) C27 0.046(8) 0.058(9) 0.071(11) -0.016(8) 0.009(7) 0.006(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 Au1 Cl4 2.261(6) . ? Au1 Cl5 2.263(5) . ? Pt1 N2 1.957(8) . ? Pt1 N1 2.018(9) . ? Pt1 N3 2.022(9) . ? Pt1 Cl3 2.308(3) . ? Pt1 Cl1 2.314(3) . ? Pt1 Cl2 2.320(3) . ? Cl6 C1S 1.745(19) . ? Cl7 C1S 1.737(17) . ? Cl8 C2S 1.65(3) . ? Cl9 C2S 1.86(3) . ? N1 C5 1.350(13) . ? N1 C1 1.351(13) . ? N2 C10 1.297(13) . ? N2 C14 1.359(13) . ? N3 C23 1.315(13) . ? N3 C19 1.382(13) . ? C1 C2 1.380(16) . ? C1 H1 0.9500 . ? C1S H28A 0.9900 . ? C1S H28B 0.9900 . ? C2 C3 1.377(16) . ? C2 H2 0.9500 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3 C4 1.412(16) . ? C3 C6 1.512(17) . ? C4 C5 1.398(16) . ? C4 H4 0.9500 . ? C5 C10 1.500(15) . ? C6 C9 1.536(17) . ? C6 C8 1.54(2) . ? C6 C7 1.544(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.374(13) . ? C11 C12 1.405(14) . ? C11 H11 0.9500 . ? C12 C13 1.386(16) . ? C12 C15 1.529(14) . ? C13 C14 1.389(14) . ? C13 H13 0.9500 . ? C14 C19 1.477(14) . ? C15 C17A 1.483(16) . ? C15 C18 1.494(15) . ? C15 C16A 1.494(16) . ? C15 C17 1.507(14) . ? C15 C16 1.509(15) . ? C15 C18A 1.519(17) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19 C20 1.381(15) . ? C20 C21 1.401(15) . ? C20 H20 0.9500 . ? C21 C22 1.377(15) . ? C21 C24 1.525(16) . ? C22 C23 1.404(16) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C27 1.518(17) . ? C24 C26 1.531(18) . ? C24 C25 1.549(17) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 Cl4 Au1 Cl5 177.89(17) . . ? N2 Pt1 N1 81.0(3) . . ? N2 Pt1 N3 81.6(4) . . ? N1 Pt1 N3 162.6(3) . . ? N2 Pt1 Cl3 90.6(3) . . ? N1 Pt1 Cl3 91.7(3) . . ? N3 Pt1 Cl3 88.1(3) . . ? N2 Pt1 Cl1 178.8(3) . . ? N1 Pt1 Cl1 98.7(2) . . ? N3 Pt1 Cl1 98.7(3) . . ? Cl3 Pt1 Cl1 90.64(11) . . ? N2 Pt1 Cl2 87.2(3) . . ? N1 Pt1 Cl2 89.4(3) . . ? N3 Pt1 Cl2 90.1(3) . . ? Cl3 Pt1 Cl2 177.34(11) . . ? Cl1 Pt1 Cl2 91.57(11) . . ? C5 N1 C1 120.1(10) . . ? C5 N1 Pt1 112.5(7) . . ? C1 N1 Pt1 127.4(8) . . ? C10 N2 C14 124.7(9) . . ? C10 N2 Pt1 118.3(7) . . ? C14 N2 Pt1 117.0(7) . . ? C23 N3 C19 120.3(10) . . ? C23 N3 Pt1 126.9(8) . . ? C19 N3 Pt1 112.8(7) . . ? N1 C1 C2 120.2(10) . . ? N1 C1 H1 119.9 . . ? C2 C1 H1 119.9 . . ? Cl7 C1S Cl6 107.8(10) . . ? Cl7 C1S H28A 110.1 . . ? Cl6 C1S H28A 110.1 . . ? Cl7 C1S H28B 110.1 . . ? Cl6 C1S H28B 110.1 . . ? H28A C1S H28B 108.5 . . ? C3 C2 C1 122.4(10) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? Cl8 C2S Cl9 105.5(13) . . ? Cl8 C2S H2S1 110.7 . . ? Cl9 C2S H2S1 110.7 . . ? Cl8 C2S H2S2 110.7 . . ? Cl9 C2S H2S2 110.7 . . ? H2S1 C2S H2S2 108.8 . . ? C2 C3 C4 116.4(11) . . ? C2 C3 C6 121.0(10) . . ? C4 C3 C6 122.5(10) . . ? C5 C4 C3 119.9(10) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 121.0(10) . . ? N1 C5 C10 115.5(10) . . ? C4 C5 C10 123.6(10) . . ? C3 C6 C9 112.7(10) . . ? C3 C6 C8 106.8(11) . . ? C9 C6 C8 111.7(12) . . ? C3 C6 C7 109.0(11) . . ? C9 C6 C7 108.8(12) . . ? C8 C6 C7 107.8(11) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 120.2(10) . . ? N2 C10 C5 112.7(9) . . ? C11 C10 C5 127.0(10) . . ? C10 C11 C12 118.8(10) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? C13 C12 C11 119.1(9) . . ? C13 C12 C15 120.7(9) . . ? C11 C12 C15 120.2(10) . . ? C12 C13 C14 119.9(10) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? N2 C14 C13 117.3(10) . . ? N2 C14 C19 113.3(9) . . ? C13 C14 C19 129.3(10) . . ? C17A C15 C18 127.3(16) . . ? C17A C15 C16A 111.7(16) . . ? C18 C15 C16A 63.8(14) . . ? C17A C15 C17 40.9(13) . . ? C18 C15 C17 108.2(12) . . ? C16A C15 C17 141.9(17) . . ? C17A C15 C16 66.5(14) . . ? C18 C15 C16 107.0(12) . . ? C16A C15 C16 49.6(14) . . ? C17 C15 C16 106.5(12) . . ? C17A C15 C18A 106.7(16) . . ? C18 C15 C18A 42.2(14) . . ? C16A C15 C18A 105.6(16) . . ? C17 C15 C18A 71.7(15) . . ? C16 C15 C18A 138.3(18) . . ? C17A C15 C12 116.5(15) . . ? C18 C15 C12 114.5(12) . . ? C16A C15 C12 107.0(16) . . ? C17 C15 C12 109.7(11) . . ? C16 C15 C12 110.6(12) . . ? C18A C15 C12 108.8(16) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C16A H16D 109.5 . . ? C15 C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C15 C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C17A H17D 109.5 . . ? C15 C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C15 C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C18A H18D 109.5 . . ? C15 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C15 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C20 C19 N3 119.2(10) . . ? C20 C19 C14 125.6(9) . . ? N3 C19 C14 115.2(10) . . ? C19 C20 C21 121.5(10) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 117.1(11) . . ? C22 C21 C24 121.7(10) . . ? C20 C21 C24 121.2(10) . . ? C21 C22 C23 120.1(11) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? N3 C23 C22 121.7(10) . . ? N3 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C27 C24 C21 111.5(10) . . ? C27 C24 C26 110.2(11) . . ? C21 C24 C26 107.8(10) . . ? C27 C24 C25 108.3(11) . . ? C21 C24 C25 109.0(11) . . ? C26 C24 C25 110.0(11) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.052 _refine_diff_density_min -2.883 _refine_diff_density_rms 0.226 #===END data_Compound3_from_DMF _database_code_depnum_ccdc_archive 'CCDC 768820' #TrackingRef 'Baddour-Doerrer-et-al---five-CIFs-and-CheckCIF-report.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H35 Cl3 N3 Pt, C3 H7 N O, Cl' _chemical_formula_sum 'C30 H42 Cl4 N4 O Pt' _chemical_formula_weight 811.57 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' 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' O O 0.0106 0.0060 '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 26.211(2) _cell_length_b 18.7055(16) _cell_length_c 17.6380(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.510(3) _cell_angle_gamma 90.00 _cell_volume 8200.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 445 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 24.5 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 3.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3928 _exptl_absorpt_correction_T_max 0.5243 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'double-curved silicon crystal' _diffrn_measurement_device_type 'Bruker SMART X2S' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26324 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7175 _reflns_number_gt 5696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0774P)^2^+29.6905P] 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 7175 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.115911(9) 0.207253(12) 0.402719(15) 0.03000(11) Uani 1 1 d . . . Cl1 Cl 0.17648(8) 0.29286(9) 0.39347(12) 0.0462(4) Uani 1 1 d . . . Cl2 Cl 0.04655(7) 0.28990(9) 0.36576(12) 0.0451(4) Uani 1 1 d . . . Cl3 Cl 0.05657(8) 0.11846(10) 0.41086(13) 0.0536(5) Uani 1 1 d . . . Cl4 Cl 0.23669(8) 0.47240(10) 0.25797(10) 0.0441(4) Uani 1 1 d . . . N1 N 0.1392(2) 0.2234(3) 0.5226(3) 0.0355(13) Uani 1 1 d . . . N2 N 0.1747(2) 0.1375(3) 0.4354(3) 0.0307(12) Uani 1 1 d . . . N3 N 0.1125(2) 0.1710(3) 0.2931(3) 0.0337(12) Uani 1 1 d . . . C1 C 0.1212(3) 0.2724(4) 0.5615(4) 0.0457(18) Uani 1 1 d . . . H1A H 0.0925 0.3028 0.5328 0.055 Uiso 1 1 calc R . . C2 C 0.1436(4) 0.2803(4) 0.6438(5) 0.056(2) Uani 1 1 d . . . H2A H 0.1302 0.3162 0.6705 0.067 Uiso 1 1 calc R . . C3 C 0.1849(3) 0.2371(4) 0.6868(4) 0.0446(18) Uani 1 1 d . . . C4 C 0.2027(3) 0.1844(3) 0.6446(4) 0.0344(15) Uani 1 1 d . . . H4A H 0.2302 0.1522 0.6728 0.041 Uiso 1 1 calc R . . C5 C 0.1809(3) 0.1788(3) 0.5633(4) 0.0330(15) Uani 1 1 d . . . C6 C 0.2004(2) 0.1305(3) 0.5136(4) 0.0281(13) Uani 1 1 d . . . C7 C 0.2427(3) 0.0815(3) 0.5379(4) 0.0295(14) Uani 1 1 d . . . H7A H 0.2604 0.0729 0.5932 0.035 Uiso 1 1 calc R . . C8 C 0.2585(3) 0.0456(3) 0.4805(4) 0.0315(14) Uani 1 1 d . . . C9 C 0.2296(3) 0.0554(3) 0.3986(4) 0.0338(15) Uani 1 1 d . . . H9A H 0.2395 0.0303 0.3587 0.041 Uiso 1 1 calc R . . C10 C 0.1867(3) 0.1022(3) 0.3778(4) 0.0333(15) Uani 1 1 d . . . C11 C 0.1505(3) 0.1200(4) 0.2958(4) 0.0370(15) Uani 1 1 d . . . C12 C 0.1527(3) 0.0883(4) 0.2269(4) 0.0458(18) Uani 1 1 d . . . H12A H 0.1797 0.0537 0.2291 0.055 Uiso 1 1 calc R . . C13 C 0.1155(3) 0.1066(5) 0.1538(5) 0.053(2) Uani 1 1 d . . . C14 C 0.0783(3) 0.1592(5) 0.1534(5) 0.054(2) Uani 1 1 d . . . H14A H 0.0530 0.1737 0.1041 0.065 Uiso 1 1 calc R . . C15 C 0.0775(3) 0.1905(4) 0.2229(4) 0.0415(18) Uani 1 1 d . . . H15A H 0.0517 0.2266 0.2213 0.050 Uiso 1 1 calc R . . C16 C 0.2097(4) 0.2448(5) 0.7766(5) 0.063(3) Uani 1 1 d . . . C17 C 0.1986(6) 0.3184(6) 0.8059(6) 0.101(5) Uani 1 1 d . . . H17A H 0.1603 0.3224 0.8005 0.151 Uiso 1 1 calc R . . H17B H 0.2082 0.3557 0.7739 0.151 Uiso 1 1 calc R . . H17C H 0.2201 0.3243 0.8622 0.151 Uiso 1 1 calc R . . C18 C 0.1824(5) 0.1863(6) 0.8138(6) 0.082(3) Uani 1 1 d . . . H18A H 0.1435 0.1944 0.7967 0.123 Uiso 1 1 calc R . . H18B H 0.1969 0.1887 0.8722 0.123 Uiso 1 1 calc R . . H18C H 0.1898 0.1390 0.7958 0.123 Uiso 1 1 calc R . . C19 C 0.2726(4) 0.2305(5) 0.8039(5) 0.067(3) Uani 1 1 d . . . H19A H 0.2901 0.2671 0.7808 0.100 Uiso 1 1 calc R . . H19B H 0.2795 0.1832 0.7853 0.100 Uiso 1 1 calc R . . H19C H 0.2872 0.2324 0.8623 0.100 Uiso 1 1 calc R . . C20 C 0.3080(3) -0.0041(4) 0.5041(4) 0.0380(16) Uani 1 1 d . . . C21 C 0.3348(3) -0.0096(4) 0.5927(4) 0.051(2) Uani 1 1 d . . . H21A H 0.3468 0.0380 0.6145 0.077 Uiso 1 1 calc R . . H21B H 0.3660 -0.0415 0.6038 0.077 Uiso 1 1 calc R . . H21C H 0.3092 -0.0287 0.6177 0.077 Uiso 1 1 calc R . . C22 C 0.3489(3) 0.0249(5) 0.4649(5) 0.062(2) Uani 1 1 d . . . H22A H 0.3614 0.0722 0.4868 0.093 Uiso 1 1 calc R . . H22B H 0.3315 0.0286 0.4070 0.093 Uiso 1 1 calc R . . H22C H 0.3796 -0.0077 0.4761 0.093 Uiso 1 1 calc R . . C23 C 0.2897(4) -0.0796(4) 0.4689(5) 0.062(2) Uani 1 1 d . . . H23A H 0.3208 -0.1116 0.4817 0.093 Uiso 1 1 calc R . . H23B H 0.2735 -0.0761 0.4107 0.093 Uiso 1 1 calc R . . H23C H 0.2631 -0.0986 0.4921 0.093 Uiso 1 1 calc R . . C24 C 0.1151(4) 0.0669(6) 0.0771(5) 0.082(4) Uani 1 1 d . . . C25 C 0.0657(5) 0.0792(7) 0.0094(6) 0.101(4) Uani 1 1 d . . . H25A H 0.0637 0.1297 -0.0062 0.151 Uiso 1 1 calc R . . H25B H 0.0343 0.0669 0.0254 0.151 Uiso 1 1 calc R . . H25C H 0.0663 0.0493 -0.0359 0.151 Uiso 1 1 calc R . . C26 C 0.1651(5) 0.0811(8) 0.0598(6) 0.105(5) Uani 1 1 d . . . H26A H 0.1673 0.1322 0.0487 0.158 Uiso 1 1 calc R . . H26B H 0.1658 0.0532 0.0132 0.158 Uiso 1 1 calc R . . H26C H 0.1959 0.0676 0.1061 0.158 Uiso 1 1 calc R . . C27 C 0.1143(6) -0.0166(7) 0.0966(7) 0.119(5) Uani 1 1 d . . . H27A H 0.1052 -0.0440 0.0467 0.179 Uiso 1 1 calc R . . H27B H 0.0873 -0.0257 0.1232 0.179 Uiso 1 1 calc R . . H27C H 0.1498 -0.0313 0.1318 0.179 Uiso 1 1 calc R . . C28 C 0.0055(7) 0.5253(10) 0.6290(16) 0.245(14) Uani 1 1 d . . . H28A H -0.0130 0.4938 0.6563 0.367 Uiso 1 1 calc R . . H28B H 0.0006 0.5070 0.5751 0.367 Uiso 1 1 calc R . . H28C H -0.0097 0.5736 0.6254 0.367 Uiso 1 1 calc R . . C29 C 0.0903(5) 0.5970(6) 0.6951(9) 0.104(4) Uani 1 1 d . . . H29A H 0.1286 0.5897 0.7240 0.156 Uiso 1 1 calc R . . H29B H 0.0737 0.6238 0.7290 0.156 Uiso 1 1 calc R . . H29C H 0.0864 0.6241 0.6460 0.156 Uiso 1 1 calc R . . C30 C 0.0899(4) 0.4688(6) 0.6902(7) 0.073(3) Uani 1 1 d . . . H30 H 0.1274 0.4724 0.7175 0.050 Uiso 1 1 calc . . . O1 O 0.0725(3) 0.4102(4) 0.6740(7) 0.131(4) Uani 1 1 d . . . N4 N 0.0637(4) 0.5277(5) 0.6748(7) 0.107(4) 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 Pt1 0.02488(16) 0.02789(16) 0.03746(17) -0.00136(10) 0.01024(11) 0.00218(10) Cl1 0.0404(10) 0.0396(9) 0.0576(11) 0.0009(8) 0.0141(9) -0.0103(7) Cl2 0.0358(10) 0.0417(9) 0.0539(11) -0.0026(8) 0.0089(8) 0.0136(7) Cl3 0.0387(10) 0.0460(10) 0.0786(13) 0.0071(10) 0.0222(10) -0.0081(8) Cl4 0.0478(10) 0.0460(9) 0.0388(9) 0.0055(7) 0.0144(8) -0.0072(8) N1 0.034(3) 0.036(3) 0.039(3) -0.001(2) 0.014(3) 0.002(2) N2 0.025(3) 0.029(3) 0.037(3) 0.001(2) 0.008(2) 0.002(2) N3 0.026(3) 0.035(3) 0.039(3) -0.007(2) 0.010(3) 0.002(2) C1 0.058(5) 0.041(4) 0.045(4) -0.002(3) 0.027(4) 0.017(4) C2 0.079(6) 0.045(4) 0.050(5) -0.003(4) 0.028(5) 0.018(4) C3 0.054(5) 0.041(4) 0.045(4) 0.000(3) 0.024(4) 0.007(4) C4 0.037(4) 0.029(3) 0.039(4) -0.001(3) 0.016(3) 0.001(3) C5 0.031(4) 0.028(3) 0.044(4) 0.002(3) 0.017(3) 0.003(3) C6 0.026(3) 0.029(3) 0.030(3) -0.001(3) 0.009(3) -0.005(3) C7 0.031(3) 0.026(3) 0.032(3) 0.002(3) 0.010(3) -0.004(3) C8 0.027(3) 0.029(3) 0.040(4) -0.004(3) 0.013(3) 0.002(3) C9 0.036(4) 0.028(3) 0.039(4) -0.004(3) 0.014(3) 0.005(3) C10 0.033(4) 0.030(3) 0.037(4) -0.003(3) 0.012(3) 0.000(3) C11 0.030(3) 0.038(3) 0.040(4) -0.001(3) 0.006(3) 0.002(3) C12 0.037(4) 0.057(4) 0.038(4) -0.013(3) 0.004(3) 0.011(3) C13 0.033(4) 0.075(6) 0.044(4) -0.018(4) 0.004(4) 0.013(4) C14 0.042(5) 0.066(5) 0.042(4) 0.001(4) -0.002(4) 0.015(4) C15 0.031(4) 0.050(4) 0.037(4) -0.009(3) 0.002(3) 0.010(3) C16 0.099(7) 0.052(5) 0.042(4) -0.011(4) 0.029(5) 0.023(5) C17 0.159(12) 0.075(7) 0.055(6) -0.021(5) 0.016(7) 0.049(8) C18 0.089(8) 0.106(8) 0.061(6) 0.025(6) 0.038(6) 0.018(7) C19 0.074(7) 0.076(6) 0.041(5) -0.008(4) 0.007(5) 0.005(5) C20 0.034(4) 0.037(4) 0.042(4) -0.002(3) 0.011(3) 0.010(3) C21 0.050(5) 0.054(5) 0.043(4) 0.004(3) 0.005(4) 0.020(4) C22 0.042(5) 0.089(7) 0.059(5) 0.016(5) 0.021(4) 0.020(4) C23 0.070(6) 0.036(4) 0.066(5) -0.009(4) 0.003(5) 0.019(4) C24 0.055(6) 0.122(9) 0.051(5) -0.037(5) -0.006(5) 0.036(6) C25 0.095(9) 0.124(9) 0.052(6) -0.036(6) -0.019(6) 0.047(7) C26 0.090(9) 0.174(13) 0.057(6) -0.019(7) 0.030(6) 0.039(9) C27 0.125(11) 0.106(10) 0.094(9) -0.053(8) -0.011(8) 0.029(8) C28 0.111(14) 0.144(16) 0.38(3) -0.106(19) -0.063(17) 0.058(12) C29 0.098(9) 0.074(8) 0.133(11) -0.016(7) 0.026(8) 0.014(7) C30 0.061(6) 0.066(6) 0.097(7) -0.018(5) 0.030(6) 0.014(5) O1 0.082(6) 0.069(5) 0.249(12) -0.038(6) 0.065(7) 0.007(4) N4 0.065(6) 0.067(6) 0.166(10) -0.033(6) 0.005(6) 0.023(5) _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 N2 1.961(5) . ? Pt1 N3 2.024(5) . ? Pt1 N1 2.028(6) . ? Pt1 Cl1 2.2968(18) . ? Pt1 Cl3 2.3108(18) . ? Pt1 Cl2 2.3168(16) . ? N1 C1 1.319(9) . ? N1 C5 1.380(8) . ? N2 C10 1.330(8) . ? N2 C6 1.336(8) . ? N3 C15 1.337(9) . ? N3 C11 1.369(8) . ? C1 C2 1.390(11) . ? C1 H1A 0.9500 . ? C2 C3 1.370(11) . ? C2 H2A 0.9500 . ? C3 C4 1.402(10) . ? C3 C16 1.515(11) . ? C4 C5 1.368(9) . ? C4 H4A 0.9500 . ? C5 C6 1.460(9) . ? C6 C7 1.396(9) . ? C7 C8 1.384(9) . ? C7 H7A 0.9500 . ? C8 C9 1.413(9) . ? C8 C20 1.543(9) . ? C9 C10 1.378(9) . ? C9 H9A 0.9500 . ? C10 C11 1.493(9) . ? C11 C12 1.370(10) . ? C12 C13 1.391(10) . ? C12 H12A 0.9500 . ? C13 C14 1.384(11) . ? C13 C24 1.541(11) . ? C14 C15 1.364(11) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.531(12) . ? C16 C18 1.561(14) . ? C16 C19 1.589(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.500(10) . ? C20 C22 1.545(11) . ? C20 C23 1.556(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.461(16) . ? C24 C25 1.475(12) . ? C24 C27 1.602(17) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N4 1.483(17) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N4 1.463(14) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 O1 1.186(12) . ? C30 N4 1.281(12) . ? C30 H30 0.9500 . ? 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 N2 Pt1 N3 81.4(2) . . ? N2 Pt1 N1 81.0(2) . . ? N3 Pt1 N1 162.3(2) . . ? N2 Pt1 Cl1 89.30(16) . . ? N3 Pt1 Cl1 89.26(17) . . ? N1 Pt1 Cl1 89.09(17) . . ? N2 Pt1 Cl3 89.18(16) . . ? N3 Pt1 Cl3 89.57(17) . . ? N1 Pt1 Cl3 91.61(17) . . ? Cl1 Pt1 Cl3 178.21(7) . . ? N2 Pt1 Cl2 179.28(16) . . ? N3 Pt1 Cl2 99.33(16) . . ? N1 Pt1 Cl2 98.29(16) . . ? Cl1 Pt1 Cl2 90.75(7) . . ? Cl3 Pt1 Cl2 90.78(7) . . ? C1 N1 C5 120.2(6) . . ? C1 N1 Pt1 127.3(5) . . ? C5 N1 Pt1 112.3(4) . . ? C10 N2 C6 125.2(5) . . ? C10 N2 Pt1 117.4(4) . . ? C6 N2 Pt1 117.4(4) . . ? C15 N3 C11 120.0(6) . . ? C15 N3 Pt1 127.1(5) . . ? C11 N3 Pt1 112.9(4) . . ? N1 C1 C2 121.0(7) . . ? N1 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 C2 C1 120.9(7) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 117.2(7) . . ? C2 C3 C16 121.6(7) . . ? C4 C3 C16 121.2(7) . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 N1 119.8(6) . . ? C4 C5 C6 124.6(6) . . ? N1 C5 C6 115.5(6) . . ? N2 C6 C7 118.2(6) . . ? N2 C6 C5 113.7(5) . . ? C7 C6 C5 128.1(6) . . ? C8 C7 C6 119.1(6) . . ? C8 C7 H7A 120.5 . . ? C6 C7 H7A 120.5 . . ? C7 C8 C9 119.8(6) . . ? C7 C8 C20 121.1(6) . . ? C9 C8 C20 119.1(6) . . ? C10 C9 C8 118.8(6) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? N2 C10 C9 118.8(6) . . ? N2 C10 C11 113.4(6) . . ? C9 C10 C11 127.8(6) . . ? N3 C11 C12 120.4(6) . . ? N3 C11 C10 114.9(6) . . ? C12 C11 C10 124.7(6) . . ? C11 C12 C13 120.1(7) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 117.8(7) . . ? C14 C13 C24 122.0(7) . . ? C12 C13 C24 120.1(7) . . ? C15 C14 C13 120.8(7) . . ? C15 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? N3 C15 C14 121.0(7) . . ? N3 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C3 C16 C17 112.0(7) . . ? C3 C16 C18 105.7(8) . . ? C17 C16 C18 109.1(9) . . ? C3 C16 C19 111.1(7) . . ? C17 C16 C19 109.9(9) . . ? C18 C16 C19 108.9(8) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C8 113.4(6) . . ? C21 C20 C22 109.2(6) . . ? C8 C20 C22 108.1(6) . . ? C21 C20 C23 109.7(6) . . ? C8 C20 C23 108.2(6) . . ? C22 C20 C23 108.1(7) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C25 114.7(10) . . ? C26 C24 C13 109.9(9) . . ? C25 C24 C13 113.2(7) . . ? C26 C24 C27 107.3(10) . . ? C25 C24 C27 104.9(10) . . ? C13 C24 C27 106.2(9) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O1 C30 N4 127.2(11) . . ? O1 C30 H30 116.4 . . ? N4 C30 H30 116.4 . . ? C30 N4 C29 122.0(10) . . ? C30 N4 C28 118.6(11) . . ? C29 N4 C28 119.2(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.073 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.163 #===END data_Compound-3-with-Et2O _database_code_depnum_ccdc_archive 'CCDC 768821' #TrackingRef 'Baddour-Doerrer-et-al---five-CIFs-and-CheckCIF-report.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H35 Cl3 N3 Pt, 2(C4 H10 O), Cl' _chemical_formula_sum 'C35 H55 Cl4 N3 O2 Pt' _chemical_formula_weight 886.71 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 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 15.362(4) _cell_length_b 10.441(3) _cell_length_c 24.357(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.297(5) _cell_angle_gamma 90.00 _cell_volume 3768.3(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3556 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 28.23 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 4.041 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4315 _exptl_absorpt_correction_T_max 0.4987 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58242 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8900 _reflns_number_gt 7111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0493P)^2^+21.9744P] 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 8900 _refine_ls_number_parameters 389 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.006 _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 0.110348(13) 0.71779(2) 0.311215(10) 0.02510(8) Uani 1 1 d . . . Cl1 Cl 0.16255(10) 0.56097(17) 0.26072(7) 0.0393(4) Uani 1 1 d . . . Cl2 Cl 0.25564(9) 0.79375(16) 0.34884(7) 0.0359(4) Uani 1 1 d . . . Cl3 Cl 0.05224(10) 0.87181(15) 0.35984(7) 0.0334(3) Uani 1 1 d . . . N1 N 0.0761(3) 0.8302(5) 0.2407(2) 0.0296(11) Uani 1 1 d . . . N2 N -0.0121(3) 0.6540(5) 0.2787(2) 0.0230(10) Uani 1 1 d . . . N3 N 0.1056(3) 0.5857(5) 0.3717(2) 0.0267(10) Uani 1 1 d . . . C1 C 0.1252(4) 0.9204(7) 0.2250(3) 0.0372(15) Uani 1 1 d . . . H1 H 0.1860 0.9318 0.2465 0.045 Uiso 1 1 calc R . . C2 C 0.0916(4) 0.9979(8) 0.1789(3) 0.0475(19) Uani 1 1 d . . . H2 H 0.1290 1.0611 0.1687 0.057 Uiso 1 1 calc R . . C3 C 0.0020(4) 0.9840(7) 0.1469(3) 0.0411(17) Uani 1 1 d . . . C4 C -0.0488(4) 0.8867(7) 0.1629(3) 0.0334(14) Uani 1 1 d . . . H4 H -0.1095 0.8729 0.1417 0.040 Uiso 1 1 calc R . . C5 C -0.0112(4) 0.8106(6) 0.2094(3) 0.0271(12) Uani 1 1 d . . . C6 C -0.0593(4) 0.7063(6) 0.2295(2) 0.0250(12) Uani 1 1 d . . . C7 C -0.1443(4) 0.6571(6) 0.2036(2) 0.0253(12) Uani 1 1 d . . . H7 H -0.1789 0.6914 0.1685 0.030 Uiso 1 1 calc R . . C8 C -0.1784(4) 0.5566(5) 0.2297(2) 0.0240(11) Uani 1 1 d . . . C9 C -0.1263(4) 0.5083(6) 0.2820(3) 0.0254(12) Uani 1 1 d . . . H9 H -0.1494 0.4420 0.3008 0.030 Uiso 1 1 calc R . . C10 C -0.0408(3) 0.5580(5) 0.3060(2) 0.0237(11) Uani 1 1 d . . . C11 C 0.0260(3) 0.5190(6) 0.3592(2) 0.0252(12) Uani 1 1 d . . . C12 C 0.0134(4) 0.4200(6) 0.3942(2) 0.0256(12) Uani 1 1 d . . . H12 H -0.0415 0.3732 0.3847 0.031 Uiso 1 1 calc R . . C13 C 0.0814(4) 0.3877(6) 0.4439(3) 0.0292(13) Uani 1 1 d . . . C14 C 0.1587(4) 0.4637(6) 0.4560(3) 0.0314(13) Uani 1 1 d . . . H14 H 0.2050 0.4485 0.4899 0.038 Uiso 1 1 calc R . . C15 C 0.1691(4) 0.5611(6) 0.4195(3) 0.0316(13) Uani 1 1 d . . . H15 H 0.2226 0.6112 0.4288 0.038 Uiso 1 1 calc R . . C16 C -0.0414(4) 1.0730(9) 0.0971(3) 0.055(2) Uani 1 1 d . . . C17 C 0.0285(5) 1.1591(11) 0.0808(4) 0.074(3) Uani 1 1 d . . . H17A H -0.0017 1.2141 0.0488 0.111 Uiso 1 1 calc R . . H17B H 0.0735 1.1058 0.0697 0.111 Uiso 1 1 calc R . . H17C H 0.0583 1.2125 0.1134 0.111 Uiso 1 1 calc R . . C18 C -0.0890(5) 0.9898(11) 0.0455(3) 0.072(3) Uani 1 1 d . . . H18A H -0.1333 0.9340 0.0560 0.108 Uiso 1 1 calc R . . H18B H -0.0442 0.9372 0.0338 0.108 Uiso 1 1 calc R . . H18C H -0.1198 1.0453 0.0139 0.108 Uiso 1 1 calc R . . C19 C -0.1112(5) 1.1572(9) 0.1156(4) 0.066(3) Uani 1 1 d . . . H19A H -0.1559 1.1024 0.1262 0.099 Uiso 1 1 calc R . . H19B H -0.1415 1.2131 0.0840 0.099 Uiso 1 1 calc R . . H19C H -0.0804 1.2097 0.1483 0.099 Uiso 1 1 calc R . . C20 C -0.2717(4) 0.4992(6) 0.2026(3) 0.0296(13) Uani 1 1 d . . . C21 C -0.3075(5) 0.5386(8) 0.1403(3) 0.059(2) Uani 1 1 d . . . H21A H -0.3669 0.4999 0.1245 0.088 Uiso 1 1 calc R . . H21B H -0.2657 0.5092 0.1187 0.088 Uiso 1 1 calc R . . H21C H -0.3128 0.6321 0.1378 0.088 Uiso 1 1 calc R . . C22 C -0.3346(5) 0.5379(10) 0.2386(4) 0.067(3) Uani 1 1 d . . . H22A H -0.3948 0.5026 0.2218 0.101 Uiso 1 1 calc R . . H22B H -0.3381 0.6315 0.2399 0.101 Uiso 1 1 calc R . . H22C H -0.3113 0.5044 0.2773 0.101 Uiso 1 1 calc R . . C23 C -0.2654(5) 0.3525(7) 0.2037(3) 0.0468(18) Uani 1 1 d . . . H23A H -0.3250 0.3160 0.1859 0.070 Uiso 1 1 calc R . . H23B H -0.2449 0.3229 0.2432 0.070 Uiso 1 1 calc R . . H23C H -0.2224 0.3249 0.1827 0.070 Uiso 1 1 calc R . . C24 C 0.0688(4) 0.2766(6) 0.4807(3) 0.0318(13) Uani 1 1 d . . . C25 C -0.0116(6) 0.3039(8) 0.5057(4) 0.056(2) Uani 1 1 d . . . H25A H 0.0012 0.3805 0.5298 0.085 Uiso 1 1 calc R . . H25B H -0.0209 0.2306 0.5286 0.085 Uiso 1 1 calc R . . H25C H -0.0661 0.3181 0.4747 0.085 Uiso 1 1 calc R . . C26 C 0.0487(7) 0.1572(8) 0.4447(3) 0.060(2) Uani 1 1 d . . . H26A H 0.0409 0.0846 0.4685 0.090 Uiso 1 1 calc R . . H26B H 0.0990 0.1396 0.4280 0.090 Uiso 1 1 calc R . . H26C H -0.0067 0.1697 0.4142 0.090 Uiso 1 1 calc R . . C27 C 0.1521(6) 0.2556(9) 0.5315(4) 0.059(2) Uani 1 1 d . . . H27A H 0.1640 0.3336 0.5547 0.088 Uiso 1 1 calc R . . H27B H 0.2047 0.2358 0.5174 0.088 Uiso 1 1 calc R . . H27C H 0.1406 0.1842 0.5548 0.088 Uiso 1 1 calc R . . Cl4 Cl 0.21691(9) 0.60909(16) 0.61214(7) 0.0346(3) Uani 1 1 d . . . O1 O 0.3901(14) -0.121(2) 0.5657(8) 0.111(8) Uiso 0.464(16) 1 d PD A 1 C28 C 0.2416(16) -0.053(3) 0.4975(14) 0.113(10) Uiso 0.464(16) 1 d PD A 1 H28A H 0.2106 -0.0386 0.4574 0.169 Uiso 0.464(16) 1 calc PR A 1 H28B H 0.2424 0.0273 0.5187 0.169 Uiso 0.464(16) 1 calc PR A 1 H28C H 0.2098 -0.1189 0.5132 0.169 Uiso 0.464(16) 1 calc PR A 1 C29 C 0.3300(11) -0.092(2) 0.5022(7) 0.056(5) Uiso 0.464(16) 1 d PD A 1 H29A H 0.3605 -0.0254 0.4853 0.068 Uiso 0.464(16) 1 calc PR A 1 H29B H 0.3279 -0.1711 0.4793 0.068 Uiso 0.464(16) 1 calc PR A 1 C30 C 0.4535(11) -0.0178(17) 0.5624(7) 0.049(5) Uiso 0.464(16) 1 d PD A 1 H30A H 0.4210 0.0602 0.5450 0.059 Uiso 0.464(16) 1 calc PR A 1 H30B H 0.4954 -0.0449 0.5400 0.059 Uiso 0.464(16) 1 calc PR A 1 C31 C 0.504(2) 0.006(3) 0.6249(9) 0.078(4) Uiso 0.464(16) 1 d PD A 1 H31A H 0.5471 0.0762 0.6271 0.117 Uiso 0.464(16) 1 calc PR A 1 H31B H 0.5368 -0.0720 0.6409 0.117 Uiso 0.464(16) 1 calc PR A 1 H31C H 0.4609 0.0284 0.6466 0.117 Uiso 0.464(16) 1 calc PR A 1 O1A O 0.3740(10) -0.0613(17) 0.5589(7) 0.086(5) Uiso 0.536(16) 1 d PD A 2 C28A C 0.2315(11) -0.1349(18) 0.5010(8) 0.059(4) Uiso 0.536(16) 1 d PD A 2 H28D H 0.1988 -0.2011 0.4751 0.088 Uiso 0.536(16) 1 calc PR A 2 H28E H 0.2258 -0.0527 0.4810 0.088 Uiso 0.536(16) 1 calc PR A 2 H28F H 0.2059 -0.1275 0.5337 0.088 Uiso 0.536(16) 1 calc PR A 2 C29A C 0.3211(14) -0.168(3) 0.5196(12) 0.117(9) Uiso 0.536(16) 1 d PD A 2 H29C H 0.3464 -0.1796 0.4865 0.141 Uiso 0.536(16) 1 calc PR A 2 H29D H 0.3272 -0.2498 0.5407 0.141 Uiso 0.536(16) 1 calc PR A 2 C30A C 0.4656(16) -0.105(4) 0.5603(13) 0.163(14) Uiso 0.536(16) 1 d PD A 2 H30C H 0.4850 -0.0779 0.5265 0.196 Uiso 0.536(16) 1 calc PR A 2 H30D H 0.4732 -0.1988 0.5658 0.196 Uiso 0.536(16) 1 calc PR A 2 C31A C 0.5115(18) -0.029(2) 0.6139(10) 0.078(4) Uiso 0.536(16) 1 d PD A 2 H31D H 0.5771 -0.0390 0.6222 0.117 Uiso 0.536(16) 1 calc PR A 2 H31E H 0.4907 -0.0601 0.6462 0.117 Uiso 0.536(16) 1 calc PR A 2 H31F H 0.4961 0.0623 0.6077 0.117 Uiso 0.536(16) 1 calc PR A 2 O2 O 0.8088(5) -0.2597(7) 0.6603(3) 0.081(2) Uiso 1 1 d D . . C32 C 0.6690(9) -0.2281(16) 0.5778(6) 0.021(3) Uiso 0.464(16) 1 d PD A 3 H32A H 0.6235 -0.1664 0.5580 0.031 Uiso 0.464(16) 1 calc PR A 3 H32B H 0.6393 -0.3002 0.5912 0.031 Uiso 0.464(16) 1 calc PR A 3 H32C H 0.7028 -0.2597 0.5516 0.031 Uiso 0.464(16) 1 calc PR A 3 C33 C 0.7343(16) -0.162(2) 0.6289(11) 0.091(5) Uiso 0.464(16) 1 d PD A 3 H33A H 0.7004 -0.1310 0.6556 0.109 Uiso 0.464(16) 1 calc PR A 3 H33B H 0.7630 -0.0880 0.6156 0.109 Uiso 0.464(16) 1 calc PR A 3 C34 C 0.8699(15) -0.180(2) 0.6979(11) 0.079(4) Uiso 0.464(16) 1 d PD A 3 H34A H 0.8404 -0.1449 0.7261 0.095 Uiso 0.464(16) 1 calc PR A 3 H34B H 0.8856 -0.1073 0.6763 0.095 Uiso 0.464(16) 1 calc PR A 3 C35 C 0.9578(15) -0.250(2) 0.7297(11) 0.061(3) Uiso 0.464(16) 1 d PD A 3 H35A H 1.0028 -0.1864 0.7486 0.092 Uiso 0.464(16) 1 calc PR A 3 H35B H 0.9811 -0.2990 0.7025 0.092 Uiso 0.464(16) 1 calc PR A 3 H35C H 0.9449 -0.3077 0.7582 0.092 Uiso 0.464(16) 1 calc PR A 3 C32A C 0.6676(9) -0.2637(16) 0.5817(6) 0.029(3) Uiso 0.536(16) 1 d PD A 4 H32D H 0.6115 -0.2152 0.5676 0.043 Uiso 0.536(16) 1 calc PR A 4 H32E H 0.6532 -0.3527 0.5887 0.043 Uiso 0.536(16) 1 calc PR A 4 H32F H 0.7024 -0.2615 0.5534 0.043 Uiso 0.536(16) 1 calc PR A 4 C33A C 0.7203(12) -0.207(2) 0.6345(9) 0.091(5) Uiso 0.536(16) 1 d PD A 4 H33C H 0.7280 -0.1146 0.6274 0.109 Uiso 0.536(16) 1 calc PR A 4 H33D H 0.6845 -0.2126 0.6628 0.109 Uiso 0.536(16) 1 calc PR A 4 C34A C 0.8456(12) -0.202(2) 0.6989(9) 0.079(4) Uiso 0.536(16) 1 d PD A 4 H34C H 0.8217 -0.2265 0.7315 0.095 Uiso 0.536(16) 1 calc PR A 4 H34D H 0.8329 -0.1103 0.6911 0.095 Uiso 0.536(16) 1 calc PR A 4 C35A C 0.9474(12) -0.223(2) 0.7154(10) 0.061(3) Uiso 0.536(16) 1 d PD A 4 H35D H 0.9760 -0.1635 0.7459 0.092 Uiso 0.536(16) 1 calc PR A 4 H35E H 0.9708 -0.2080 0.6822 0.092 Uiso 0.536(16) 1 calc PR A 4 H35F H 0.9609 -0.3114 0.7287 0.092 Uiso 0.536(16) 1 calc PR A 4 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 0.01270(11) 0.03025(13) 0.03111(13) 0.00366(10) 0.00361(8) 0.00103(8) Cl1 0.0274(7) 0.0448(9) 0.0484(9) -0.0009(8) 0.0149(7) 0.0087(6) Cl2 0.0160(6) 0.0418(9) 0.0454(9) 0.0080(7) 0.0002(6) -0.0036(6) Cl3 0.0287(7) 0.0323(8) 0.0375(8) 0.0016(6) 0.0058(6) 0.0019(6) N1 0.017(2) 0.042(3) 0.030(3) 0.006(2) 0.0065(19) 0.002(2) N2 0.0138(19) 0.029(2) 0.026(2) 0.000(2) 0.0036(17) 0.0039(18) N3 0.016(2) 0.030(3) 0.032(3) 0.006(2) 0.0037(19) 0.0032(19) C1 0.015(2) 0.053(4) 0.040(4) 0.012(3) 0.001(2) -0.002(3) C2 0.022(3) 0.065(5) 0.055(5) 0.023(4) 0.009(3) -0.011(3) C3 0.022(3) 0.057(4) 0.042(4) 0.021(3) 0.003(3) -0.004(3) C4 0.016(2) 0.051(4) 0.031(3) 0.006(3) 0.004(2) -0.004(3) C5 0.014(2) 0.037(3) 0.029(3) 0.001(2) 0.005(2) -0.001(2) C6 0.020(2) 0.030(3) 0.026(3) 0.001(2) 0.008(2) 0.003(2) C7 0.019(2) 0.030(3) 0.026(3) -0.004(2) 0.004(2) 0.003(2) C8 0.021(2) 0.023(3) 0.029(3) -0.003(2) 0.007(2) -0.002(2) C9 0.020(2) 0.025(3) 0.032(3) -0.001(2) 0.008(2) 0.000(2) C10 0.016(2) 0.023(3) 0.030(3) -0.001(2) 0.003(2) 0.004(2) C11 0.016(2) 0.033(3) 0.026(3) 0.000(2) 0.004(2) 0.008(2) C12 0.019(2) 0.030(3) 0.028(3) 0.002(2) 0.006(2) 0.004(2) C13 0.024(3) 0.031(3) 0.030(3) 0.000(3) 0.004(2) 0.003(2) C14 0.022(3) 0.033(3) 0.035(3) 0.008(3) 0.000(2) 0.003(2) C15 0.017(2) 0.033(3) 0.041(4) 0.003(3) -0.001(2) 0.001(2) C16 0.023(3) 0.085(6) 0.053(5) 0.039(4) 0.001(3) -0.010(3) C17 0.030(4) 0.111(8) 0.071(6) 0.058(6) -0.004(4) -0.017(4) C18 0.034(4) 0.129(9) 0.045(5) 0.041(5) -0.005(3) -0.023(5) C19 0.030(4) 0.073(6) 0.087(6) 0.047(5) 0.001(4) -0.003(4) C20 0.020(3) 0.030(3) 0.036(3) -0.005(3) 0.002(2) -0.004(2) C21 0.051(4) 0.049(4) 0.053(5) 0.018(4) -0.027(4) -0.026(4) C22 0.020(3) 0.101(7) 0.079(6) -0.051(6) 0.010(4) -0.012(4) C23 0.039(4) 0.036(4) 0.055(4) 0.005(3) -0.006(3) -0.012(3) C24 0.026(3) 0.034(3) 0.032(3) 0.008(3) 0.002(2) -0.001(3) C25 0.064(5) 0.055(5) 0.058(5) 0.012(4) 0.030(4) 0.009(4) C26 0.090(7) 0.038(4) 0.044(4) 0.004(4) 0.004(4) -0.015(4) C27 0.046(4) 0.064(5) 0.057(5) 0.023(4) -0.003(4) -0.006(4) Cl4 0.0206(6) 0.0411(8) 0.0414(9) -0.0059(7) 0.0066(6) -0.0001(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 N2 1.955(4) . ? Pt1 N1 2.032(5) . ? Pt1 N3 2.033(5) . ? Pt1 Cl3 2.3116(16) . ? Pt1 Cl1 2.3146(17) . ? Pt1 Cl2 2.3176(15) . ? N1 C1 1.325(8) . ? N1 C5 1.372(7) . ? N2 C10 1.341(7) . ? N2 C6 1.341(7) . ? N3 C15 1.332(7) . ? N3 C11 1.370(7) . ? C1 C2 1.370(9) . ? C1 H1 0.9500 . ? C2 C3 1.399(9) . ? C2 H2 0.9500 . ? C3 C4 1.399(9) . ? C3 C16 1.533(9) . ? C4 C5 1.379(9) . ? C4 H4 0.9500 . ? C5 C6 1.471(8) . ? C6 C7 1.390(8) . ? C7 C8 1.398(8) . ? C7 H7 0.9500 . ? C8 C9 1.407(8) . ? C8 C20 1.533(7) . ? C9 C10 1.389(7) . ? C9 H9 0.9500 . ? C10 C11 1.482(7) . ? C11 C12 1.385(8) . ? C12 C13 1.416(8) . ? C12 H12 0.9500 . ? C13 C14 1.392(8) . ? C13 C24 1.510(9) . ? C14 C15 1.388(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.532(10) . ? C16 C19 1.542(13) . ? C16 C18 1.544(13) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C22 1.520(10) . ? C20 C21 1.528(9) . ? C20 C23 1.535(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.509(10) . ? C24 C25 1.540(10) . ? C24 C27 1.544(10) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? O1 C30 1.465(17) . ? O1 C29 1.605(17) . ? C28 C29 1.394(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.536(18) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? O1A C30A 1.470(19) . ? O1A C29A 1.551(18) . ? C28A C29A 1.375(17) . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C30A C31A 1.535(19) . ? C30A H30C 0.9900 . ? C30A H30D 0.9900 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? O2 C34A 1.132(15) . ? O2 C34 1.399(17) . ? O2 C33A 1.447(15) . ? O2 C33 1.570(17) . ? C32 C33 1.538(17) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.548(18) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C32A C33A 1.454(16) . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33C 0.9900 . ? C33A H33D 0.9900 . ? C34A C35A 1.524(17) . ? C34A H34C 0.9900 . ? C34A H34D 0.9900 . ? C35A H35D 0.9800 . ? C35A H35E 0.9800 . ? C35A H35F 0.9800 . ? 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 N2 Pt1 N1 81.21(19) . . ? N2 Pt1 N3 81.27(19) . . ? N1 Pt1 N3 162.48(19) . . ? N2 Pt1 Cl3 89.13(14) . . ? N1 Pt1 Cl3 89.00(16) . . ? N3 Pt1 Cl3 90.48(15) . . ? N2 Pt1 Cl1 88.53(14) . . ? N1 Pt1 Cl1 90.46(16) . . ? N3 Pt1 Cl1 89.34(15) . . ? Cl3 Pt1 Cl1 177.65(5) . . ? N2 Pt1 Cl2 179.39(14) . . ? N1 Pt1 Cl2 98.28(14) . . ? N3 Pt1 Cl2 99.24(13) . . ? Cl3 Pt1 Cl2 91.21(6) . . ? Cl1 Pt1 Cl2 91.13(6) . . ? C1 N1 C5 119.6(5) . . ? C1 N1 Pt1 127.9(4) . . ? C5 N1 Pt1 112.4(4) . . ? C10 N2 C6 125.2(5) . . ? C10 N2 Pt1 117.4(4) . . ? C6 N2 Pt1 117.3(4) . . ? C15 N3 C11 120.0(5) . . ? C15 N3 Pt1 127.4(4) . . ? C11 N3 Pt1 112.6(4) . . ? N1 C1 C2 122.4(6) . . ? N1 C1 H1 118.8 . . ? C2 C1 H1 118.8 . . ? C1 C2 C3 119.9(6) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 117.3(6) . . ? C2 C3 C16 122.5(6) . . ? C4 C3 C16 120.2(5) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N1 C5 C4 120.5(5) . . ? N1 C5 C6 115.4(5) . . ? C4 C5 C6 124.1(5) . . ? N2 C6 C7 118.5(5) . . ? N2 C6 C5 113.4(5) . . ? C7 C6 C5 128.1(5) . . ? C6 C7 C8 119.3(5) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 119.3(5) . . ? C7 C8 C20 121.1(5) . . ? C9 C8 C20 119.6(5) . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? N2 C10 C9 117.9(5) . . ? N2 C10 C11 113.4(5) . . ? C9 C10 C11 128.7(5) . . ? N3 C11 C12 120.3(5) . . ? N3 C11 C10 115.2(5) . . ? C12 C11 C10 124.5(5) . . ? C11 C12 C13 120.9(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 116.1(6) . . ? C14 C13 C24 123.2(5) . . ? C12 C13 C24 120.6(5) . . ? C15 C14 C13 121.2(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? N3 C15 C14 121.3(5) . . ? N3 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C3 111.8(5) . . ? C17 C16 C19 109.2(8) . . ? C3 C16 C19 107.8(6) . . ? C17 C16 C18 109.4(7) . . ? C3 C16 C18 108.5(7) . . ? C19 C16 C18 110.0(7) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C21 112.6(7) . . ? C22 C20 C8 108.2(5) . . ? C21 C20 C8 111.9(5) . . ? C22 C20 C23 107.6(7) . . ? C21 C20 C23 106.8(6) . . ? C8 C20 C23 109.6(5) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C26 C24 C13 109.2(6) . . ? C26 C24 C25 108.7(7) . . ? C13 C24 C25 109.6(5) . . ? C26 C24 C27 110.4(6) . . ? C13 C24 C27 112.1(5) . . ? C25 C24 C27 106.9(6) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 O1 C29 92.0(14) . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C28 C29 O1 116(2) . . ? C28 C29 H29A 108.4 . . ? O1 C29 H29A 108.4 . . ? C28 C29 H29B 108.4 . . ? O1 C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? O1 C30 C31 103.6(17) . . ? O1 C30 H30A 111.0 . . ? C31 C30 H30A 111.0 . . ? O1 C30 H30B 111.0 . . ? C31 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30A O1A C29A 97.7(17) . . ? C29A C28A H28D 109.5 . . ? C29A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C29A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C28A C29A O1A 109.9(18) . . ? C28A C29A H29C 109.7 . . ? O1A C29A H29C 109.7 . . ? C28A C29A H29D 109.7 . . ? O1A C29A H29D 109.7 . . ? H29C C29A H29D 108.2 . . ? O1A C30A C31A 94.6(19) . . ? O1A C30A H30C 112.8 . . ? C31A C30A H30C 112.8 . . ? O1A C30A H30D 112.8 . . ? C31A C30A H30D 112.8 . . ? H30C C30A H30D 110.3 . . ? C30A C31A H31D 109.5 . . ? C30A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C30A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C34A O2 C34 16(2) . . ? C34A O2 C33A 111.4(13) . . ? C34 O2 C33A 116.6(14) . . ? C34A O2 C33 101.7(15) . . ? C34 O2 C33 102.2(13) . . ? C33A O2 C33 20.2(16) . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C32 C33 O2 109.9(14) . . ? C32 C33 H33A 109.7 . . ? O2 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? O2 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? O2 C34 C35 113.3(19) . . ? O2 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? O2 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33A C32A H32D 109.5 . . ? C33A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C33A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? O2 C33A C32A 117.9(16) . . ? O2 C33A H33C 107.8 . . ? C32A C33A H33C 107.8 . . ? O2 C33A H33D 107.8 . . ? C32A C33A H33D 107.8 . . ? H33C C33A H33D 107.2 . . ? O2 C34A C35A 113.4(18) . . ? O2 C34A H34C 108.9 . . ? C35A C34A H34C 108.9 . . ? O2 C34A H34D 108.9 . . ? C35A C34A H34D 108.9 . . ? H34C C34A H34D 107.7 . . ? C34A C35A H35D 109.5 . . ? C34A C35A H35E 109.5 . . ? H35D C35A H35E 109.5 . . ? C34A C35A H35F 109.5 . . ? H35D C35A H35F 109.5 . . ? H35E C35A H35F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.708 _refine_diff_density_min -1.680 _refine_diff_density_rms 0.156 #===END data_Compound-4 _database_code_depnum_ccdc_archive 'CCDC 768822' #TrackingRef 'Baddour-Doerrer-et-al---five-CIFs-and-CheckCIF-report.pdf' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H35 Au Cl3 N3 Pt' _chemical_formula_weight 899.99 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' 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' Au Au -2.0133 8.8022 '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 10.3656(5) _cell_length_b 29.6013(14) _cell_length_c 19.1978(9) _cell_angle_alpha 90.00 _cell_angle_beta 101.8690(10) _cell_angle_gamma 90.00 _cell_volume 5764.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9717 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.89 _exptl_crystal_description BLOCK _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.074 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 10.231 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1841 _exptl_absorpt_correction_T_max 0.4949 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62815 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.00 _reflns_number_total 13140 _reflns_number_gt 11239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0157P)^2^+0.8982P] 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 13140 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0472 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _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 Au1 Au 0.809196(14) 0.313570(6) 0.205756(8) 0.01788(4) Uani 1 1 d . . . Au2 Au -0.168242(16) 0.048282(5) 0.198199(8) 0.02011(4) Uani 1 1 d . . . Pt1 Pt 0.442243(13) 0.282002(5) 0.319721(7) 0.00990(4) Uani 1 1 d . . . Pt2 Pt 0.690332(13) 0.230671(5) 0.590362(7) 0.01050(4) Uani 1 1 d . . . Cl1 Cl 0.38178(9) 0.31817(3) 0.41426(5) 0.0167(2) Uani 1 1 d . . . Cl2 Cl 0.75698(9) 0.19033(3) 0.50117(5) 0.0164(2) Uani 1 1 d . . . Cl3 Cl 0.80398(10) 0.33227(5) 0.09055(6) 0.0374(3) Uani 1 1 d . . . Cl4 Cl 0.81028(9) 0.29421(4) 0.32025(5) 0.0223(2) Uani 1 1 d . . . Cl5 Cl -0.37834(11) 0.05982(4) 0.21065(6) 0.0289(3) Uani 1 1 d . . . Cl6 Cl 0.04319(10) 0.03587(4) 0.18796(5) 0.0246(2) Uani 1 1 d . . . N1 N 0.4594(3) 0.33638(10) 0.25896(15) 0.0122(7) Uani 1 1 d . . . N2 N 0.4900(3) 0.25149(10) 0.23960(15) 0.0114(7) Uani 1 1 d . . . N3 N 0.4453(3) 0.21789(10) 0.35553(15) 0.0109(7) Uani 1 1 d . . . N4 N 0.6961(3) 0.29307(10) 0.55066(15) 0.0113(7) Uani 1 1 d . . . N5 N 0.6416(3) 0.26466(10) 0.66687(15) 0.0103(6) Uani 1 1 d . . . N6 N 0.6604(3) 0.17867(10) 0.65301(16) 0.0117(7) Uani 1 1 d . . . C1 C 0.4510(3) 0.38025(13) 0.2755(2) 0.0141(8) Uani 1 1 d . . . H1A H 0.4329 0.3881 0.3205 0.017 Uiso 1 1 calc R . . C2 C 0.4680(3) 0.41434(13) 0.22890(19) 0.0149(8) Uani 1 1 d . . . H2A H 0.4644 0.4450 0.2429 0.018 Uiso 1 1 calc R . . C3 C 0.4905(3) 0.40398(13) 0.16153(19) 0.0140(8) Uani 1 1 d . . . C4 C 0.5012(3) 0.35849(13) 0.14549(19) 0.0127(8) Uani 1 1 d . . . H4A H 0.5176 0.3500 0.1004 0.015 Uiso 1 1 calc R . . C5 C 0.4882(3) 0.32538(12) 0.19459(19) 0.0112(8) Uani 1 1 d . . . C6 C 0.5079(3) 0.27672(12) 0.18396(19) 0.0114(8) Uani 1 1 d . . . C7 C 0.5475(3) 0.25577(13) 0.12720(18) 0.0125(8) Uani 1 1 d . . . H7A H 0.5576 0.2730 0.0869 0.015 Uiso 1 1 calc R . . C8 C 0.5726(3) 0.20939(13) 0.12936(19) 0.0127(8) Uani 1 1 d . . . C9 C 0.5511(3) 0.18456(13) 0.18825(19) 0.0128(8) Uani 1 1 d . . . H9A H 0.5654 0.1528 0.1905 0.015 Uiso 1 1 calc R . . C10 C 0.5087(3) 0.20690(13) 0.24318(19) 0.0110(8) Uani 1 1 d . . . C11 C 0.4818(3) 0.18677(12) 0.30959(19) 0.0117(8) Uani 1 1 d . . . C12 C 0.4923(3) 0.14186(13) 0.32655(19) 0.0143(8) Uani 1 1 d . . . H12A H 0.5192 0.1211 0.2945 0.017 Uiso 1 1 calc R . . C13 C 0.4640(3) 0.12608(13) 0.39046(19) 0.0133(8) Uani 1 1 d . . . C14 C 0.4273(3) 0.15809(13) 0.43552(19) 0.0130(8) Uani 1 1 d . . . H14A H 0.4068 0.1488 0.4794 0.016 Uiso 1 1 calc R . . C15 C 0.4202(3) 0.20318(13) 0.41724(19) 0.0142(8) Uani 1 1 d . . . H15A H 0.3968 0.2245 0.4495 0.017 Uiso 1 1 calc R . . C16 C 0.5018(4) 0.44177(13) 0.10827(19) 0.0154(8) Uani 1 1 d . . . C17 C 0.3845(4) 0.47468(14) 0.1039(2) 0.0249(10) Uani 1 1 d . . . H17A H 0.3897 0.4983 0.0689 0.037 Uiso 1 1 calc R . . H17B H 0.3880 0.4885 0.1506 0.037 Uiso 1 1 calc R . . H17C H 0.3015 0.4580 0.0895 0.037 Uiso 1 1 calc R . . C18 C 0.6313(4) 0.46689(14) 0.1351(2) 0.0265(10) Uani 1 1 d . . . H18A H 0.7054 0.4461 0.1367 0.040 Uiso 1 1 calc R . . H18B H 0.6328 0.4787 0.1829 0.040 Uiso 1 1 calc R . . H18C H 0.6387 0.4920 0.1028 0.040 Uiso 1 1 calc R . . C19 C 0.5006(4) 0.42301(13) 0.0342(2) 0.0218(9) Uani 1 1 d . . . H19A H 0.5799 0.4048 0.0353 0.033 Uiso 1 1 calc R . . H19B H 0.4988 0.4481 0.0006 0.033 Uiso 1 1 calc R . . H19C H 0.4221 0.4041 0.0190 0.033 Uiso 1 1 calc R . . C20 C 0.6317(4) 0.18655(13) 0.0712(2) 0.0161(9) Uani 1 1 d . . . C21 C 0.5770(4) 0.13841(14) 0.0558(2) 0.0298(11) Uani 1 1 d . . . H21A H 0.4805 0.1394 0.0440 0.045 Uiso 1 1 calc R . . H21B H 0.6059 0.1194 0.0980 0.045 Uiso 1 1 calc R . . H21C H 0.6099 0.1257 0.0157 0.045 Uiso 1 1 calc R . . C22 C 0.7806(4) 0.18356(16) 0.1002(2) 0.0321(12) Uani 1 1 d . . . H22A H 0.8166 0.2140 0.1106 0.048 Uiso 1 1 calc R . . H22B H 0.8228 0.1693 0.0645 0.048 Uiso 1 1 calc R . . H22C H 0.7978 0.1655 0.1438 0.048 Uiso 1 1 calc R . . C23 C 0.6037(4) 0.21332(14) 0.0022(2) 0.0215(9) Uani 1 1 d . . . H23A H 0.5083 0.2172 -0.0138 0.032 Uiso 1 1 calc R . . H23B H 0.6389 0.1970 -0.0342 0.032 Uiso 1 1 calc R . . H23C H 0.6459 0.2430 0.0101 0.032 Uiso 1 1 calc R . . C24 C 0.4785(4) 0.07577(13) 0.4094(2) 0.0167(8) Uani 1 1 d . . . C25 C 0.4251(4) 0.06499(14) 0.4769(2) 0.0253(10) Uani 1 1 d . . . H25A H 0.4330 0.0325 0.4866 0.038 Uiso 1 1 calc R . . H25B H 0.3323 0.0739 0.4695 0.038 Uiso 1 1 calc R . . H25C H 0.4762 0.0817 0.5174 0.038 Uiso 1 1 calc R . . C26 C 0.6269(4) 0.06445(15) 0.4236(2) 0.0259(10) Uani 1 1 d . . . H26A H 0.6604 0.0691 0.3800 0.039 Uiso 1 1 calc R . . H26B H 0.6401 0.0328 0.4386 0.039 Uiso 1 1 calc R . . H26C H 0.6745 0.0842 0.4613 0.039 Uiso 1 1 calc R . . C27 C 0.4056(4) 0.04652(13) 0.3485(2) 0.0218(9) Uani 1 1 d . . . H27A H 0.4408 0.0523 0.3057 0.033 Uiso 1 1 calc R . . H27B H 0.3115 0.0539 0.3390 0.033 Uiso 1 1 calc R . . H27C H 0.4178 0.0146 0.3616 0.033 Uiso 1 1 calc R . . C28 C 0.7228(3) 0.30445(13) 0.48799(19) 0.0146(8) Uani 1 1 d . . . H28A H 0.7457 0.2814 0.4584 0.017 Uiso 1 1 calc R . . C29 C 0.7182(4) 0.34896(13) 0.4645(2) 0.0163(8) Uani 1 1 d . . . H29A H 0.7384 0.3558 0.4196 0.020 Uiso 1 1 calc R . . C30 C 0.6841(3) 0.38360(13) 0.50639(19) 0.0143(8) Uani 1 1 d . . . C31 C 0.6557(3) 0.37094(13) 0.57248(19) 0.0135(8) Uani 1 1 d . . . H31A H 0.6316 0.3934 0.6027 0.016 Uiso 1 1 calc R . . C32 C 0.6623(3) 0.32680(13) 0.59358(19) 0.0124(8) Uani 1 1 d . . . C33 C 0.6322(3) 0.31001(12) 0.66190(19) 0.0108(8) Uani 1 1 d . . . C34 C 0.5945(3) 0.33467(13) 0.71585(19) 0.0133(8) Uani 1 1 d . . . H34A H 0.5865 0.3666 0.7125 0.016 Uiso 1 1 calc R . . C35 C 0.5681(3) 0.31173(13) 0.77582(19) 0.0124(8) Uani 1 1 d . . . C36 C 0.5828(3) 0.26509(12) 0.77924(19) 0.0123(8) Uani 1 1 d . . . H36A H 0.5680 0.2492 0.8199 0.015 Uiso 1 1 calc R . . C37 C 0.6188(3) 0.24142(13) 0.72387(19) 0.0116(8) Uani 1 1 d . . . C38 C 0.6307(3) 0.19235(12) 0.71610(19) 0.0099(8) Uani 1 1 d . . . C39 C 0.6060(3) 0.16054(12) 0.76501(19) 0.0126(8) Uani 1 1 d . . . H39A H 0.5884 0.1704 0.8092 0.015 Uiso 1 1 calc R . . C40 C 0.6067(3) 0.11468(13) 0.75054(19) 0.0122(8) Uani 1 1 d . . . C41 C 0.6335(4) 0.10240(13) 0.6849(2) 0.0162(8) Uani 1 1 d . . . H41A H 0.6327 0.0714 0.6721 0.019 Uiso 1 1 calc R . . C42 C 0.6613(3) 0.13461(13) 0.63806(19) 0.0150(8) Uani 1 1 d . . . H42A H 0.6815 0.1252 0.5942 0.018 Uiso 1 1 calc R . . C43 C 0.6698(4) 0.43272(13) 0.48190(19) 0.0161(8) Uani 1 1 d . . . C44 C 0.7224(4) 0.43966(14) 0.4132(2) 0.0235(10) Uani 1 1 d . . . H44A H 0.6724 0.4207 0.3753 0.035 Uiso 1 1 calc R . . H44B H 0.8158 0.4313 0.4218 0.035 Uiso 1 1 calc R . . H44C H 0.7125 0.4715 0.3989 0.035 Uiso 1 1 calc R . . C45 C 0.5221(4) 0.44379(14) 0.4675(2) 0.0209(9) Uani 1 1 d . . . H45A H 0.4732 0.4208 0.4359 0.031 Uiso 1 1 calc R . . H45B H 0.5070 0.4735 0.4448 0.031 Uiso 1 1 calc R . . H45C H 0.4916 0.4441 0.5126 0.031 Uiso 1 1 calc R . . C46 C 0.7470(4) 0.46356(14) 0.5398(2) 0.0228(9) Uani 1 1 d . . . H46A H 0.7382 0.4950 0.5234 0.034 Uiso 1 1 calc R . . H46B H 0.8402 0.4549 0.5498 0.034 Uiso 1 1 calc R . . H46C H 0.7119 0.4605 0.5832 0.034 Uiso 1 1 calc R . . C47 C 0.5159(3) 0.33768(13) 0.83369(19) 0.0122(8) Uani 1 1 d . . . C48 C 0.5418(4) 0.31157(13) 0.90433(19) 0.0181(9) Uani 1 1 d . . . H48A H 0.4902 0.2836 0.8986 0.027 Uiso 1 1 calc R . . H48B H 0.5159 0.3302 0.9414 0.027 Uiso 1 1 calc R . . H48C H 0.6358 0.3043 0.9181 0.027 Uiso 1 1 calc R . . C49 C 0.3651(3) 0.34260(14) 0.8079(2) 0.0189(9) Uani 1 1 d . . . H49A H 0.3255 0.3126 0.7975 0.028 Uiso 1 1 calc R . . H49B H 0.3466 0.3611 0.7646 0.028 Uiso 1 1 calc R . . H49C H 0.3276 0.3572 0.8450 0.028 Uiso 1 1 calc R . . C50 C 0.5793(4) 0.38464(13) 0.8472(2) 0.0181(9) Uani 1 1 d . . . H50A H 0.6750 0.3814 0.8625 0.027 Uiso 1 1 calc R . . H50B H 0.5441 0.4000 0.8845 0.027 Uiso 1 1 calc R . . H50C H 0.5592 0.4024 0.8032 0.027 Uiso 1 1 calc R . . C51 C 0.5704(4) 0.07921(13) 0.80025(19) 0.0141(8) Uani 1 1 d . . . C52 C 0.6674(4) 0.03919(14) 0.8084(2) 0.0221(9) Uani 1 1 d . . . H52A H 0.7556 0.0496 0.8314 0.033 Uiso 1 1 calc R . . H52B H 0.6699 0.0268 0.7614 0.033 Uiso 1 1 calc R . . H52C H 0.6383 0.0157 0.8377 0.033 Uiso 1 1 calc R . . C53 C 0.4305(4) 0.06240(14) 0.7671(2) 0.0217(9) Uani 1 1 d . . . H53A H 0.3689 0.0879 0.7614 0.033 Uiso 1 1 calc R . . H53B H 0.4033 0.0397 0.7983 0.033 Uiso 1 1 calc R . . H53C H 0.4303 0.0490 0.7204 0.033 Uiso 1 1 calc R . . C54 C 0.5721(4) 0.09828(13) 0.8744(2) 0.0219(9) Uani 1 1 d . . . H54A H 0.6570 0.1130 0.8926 0.033 Uiso 1 1 calc R . . H54B H 0.5595 0.0737 0.9065 0.033 Uiso 1 1 calc R . . H54C H 0.5009 0.1204 0.8717 0.033 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 Au1 0.01406(8) 0.02548(10) 0.01445(8) -0.00063(6) 0.00376(6) -0.00153(6) Au2 0.03297(9) 0.01125(9) 0.01833(9) -0.00196(6) 0.01039(7) -0.00091(7) Pt1 0.01247(7) 0.00896(8) 0.00914(7) 0.00038(6) 0.00424(5) 0.00035(5) Pt2 0.01282(7) 0.00959(8) 0.00976(7) -0.00031(6) 0.00391(5) 0.00132(6) Cl1 0.0240(5) 0.0149(5) 0.0136(5) -0.0006(4) 0.0095(4) 0.0024(4) Cl2 0.0227(5) 0.0143(5) 0.0137(5) -0.0027(4) 0.0074(4) 0.0034(4) Cl3 0.0247(6) 0.0699(10) 0.0185(6) 0.0123(6) 0.0069(4) -0.0061(6) Cl4 0.0228(5) 0.0314(7) 0.0139(5) -0.0005(4) 0.0069(4) 0.0024(4) Cl5 0.0375(6) 0.0149(6) 0.0391(7) 0.0005(5) 0.0193(5) 0.0023(5) Cl6 0.0330(6) 0.0180(6) 0.0255(6) -0.0029(4) 0.0121(5) -0.0012(4) N1 0.0127(15) 0.0125(18) 0.0119(16) 0.0001(13) 0.0035(12) -0.0002(13) N2 0.0108(15) 0.0130(18) 0.0103(16) 0.0020(13) 0.0025(12) -0.0006(13) N3 0.0127(15) 0.0112(18) 0.0099(16) 0.0011(13) 0.0047(12) 0.0000(13) N4 0.0131(15) 0.0118(18) 0.0105(16) -0.0001(13) 0.0056(12) 0.0014(13) N5 0.0106(15) 0.0101(18) 0.0101(16) 0.0007(13) 0.0020(12) -0.0002(12) N6 0.0112(15) 0.0104(18) 0.0135(17) -0.0010(13) 0.0023(13) 0.0009(12) C1 0.0158(19) 0.013(2) 0.015(2) 0.0006(16) 0.0062(15) 0.0014(16) C2 0.019(2) 0.011(2) 0.014(2) -0.0053(16) 0.0012(15) -0.0010(16) C3 0.0129(18) 0.014(2) 0.014(2) 0.0004(16) 0.0016(15) 0.0005(15) C4 0.0154(18) 0.015(2) 0.0078(19) -0.0017(15) 0.0032(15) -0.0018(16) C5 0.0112(18) 0.012(2) 0.0117(19) -0.0003(15) 0.0043(14) -0.0015(15) C6 0.0106(17) 0.012(2) 0.0116(19) 0.0016(15) 0.0027(14) -0.0010(15) C7 0.0102(17) 0.019(2) 0.0080(18) 0.0001(15) 0.0017(14) -0.0036(15) C8 0.0103(18) 0.016(2) 0.0109(19) -0.0013(16) 0.0005(14) 0.0012(15) C9 0.0159(19) 0.009(2) 0.012(2) -0.0003(15) -0.0005(15) 0.0019(15) C10 0.0120(18) 0.010(2) 0.0093(19) 0.0000(15) -0.0022(14) 0.0004(15) C11 0.0143(18) 0.013(2) 0.0082(19) 0.0013(15) 0.0033(15) 0.0017(15) C12 0.0156(19) 0.013(2) 0.015(2) -0.0026(16) 0.0034(15) -0.0014(16) C13 0.0163(19) 0.016(2) 0.0088(19) 0.0023(15) 0.0040(15) -0.0013(16) C14 0.0161(19) 0.011(2) 0.013(2) 0.0002(15) 0.0058(15) -0.0013(15) C15 0.0170(19) 0.015(2) 0.012(2) 0.0010(16) 0.0060(15) 0.0008(16) C16 0.022(2) 0.012(2) 0.013(2) 0.0070(16) 0.0051(16) 0.0009(16) C17 0.033(2) 0.020(3) 0.023(2) 0.0111(19) 0.0097(19) 0.0098(19) C18 0.032(2) 0.022(3) 0.025(2) 0.006(2) 0.0057(19) -0.007(2) C19 0.032(2) 0.017(2) 0.018(2) 0.0056(18) 0.0066(18) -0.0010(18) C20 0.024(2) 0.016(2) 0.010(2) 0.0008(16) 0.0072(16) 0.0067(17) C21 0.052(3) 0.020(3) 0.020(2) -0.0052(19) 0.014(2) 0.003(2) C22 0.023(2) 0.056(4) 0.019(2) 0.002(2) 0.0091(19) 0.017(2) C23 0.030(2) 0.024(3) 0.012(2) 0.0048(17) 0.0075(17) 0.0106(19) C24 0.025(2) 0.008(2) 0.016(2) 0.0042(16) 0.0034(17) 0.0009(16) C25 0.041(3) 0.014(2) 0.024(2) 0.0086(18) 0.013(2) 0.0036(19) C26 0.025(2) 0.020(3) 0.031(3) 0.009(2) 0.0029(19) 0.0045(19) C27 0.034(2) 0.009(2) 0.025(2) 0.0030(18) 0.0130(19) -0.0011(18) C28 0.0153(19) 0.020(2) 0.0092(19) -0.0005(16) 0.0042(15) 0.0034(16) C29 0.021(2) 0.017(2) 0.012(2) 0.0011(16) 0.0062(16) 0.0010(17) C30 0.0140(18) 0.014(2) 0.014(2) 0.0008(16) 0.0026(15) 0.0014(16) C31 0.0160(19) 0.014(2) 0.0117(19) -0.0039(16) 0.0058(15) -0.0003(16) C32 0.0137(18) 0.014(2) 0.0111(19) -0.0001(15) 0.0063(15) 0.0021(15) C33 0.0110(18) 0.011(2) 0.0107(19) 0.0002(15) 0.0018(14) 0.0010(14) C34 0.0193(19) 0.007(2) 0.014(2) -0.0014(15) 0.0049(15) 0.0005(15) C35 0.0121(18) 0.015(2) 0.0106(19) 0.0000(15) 0.0027(15) 0.0010(15) C36 0.0159(19) 0.011(2) 0.0103(19) 0.0028(15) 0.0041(15) -0.0002(15) C37 0.0100(17) 0.014(2) 0.0098(19) -0.0002(15) -0.0011(14) -0.0022(15) C38 0.0078(17) 0.011(2) 0.0108(19) -0.0037(15) 0.0011(14) -0.0017(14) C39 0.0132(18) 0.013(2) 0.0122(19) 0.0004(16) 0.0046(15) 0.0039(15) C40 0.0102(18) 0.011(2) 0.014(2) 0.0007(15) -0.0001(15) 0.0004(15) C41 0.020(2) 0.010(2) 0.019(2) -0.0004(16) 0.0032(16) 0.0023(16) C42 0.020(2) 0.015(2) 0.0102(19) -0.0051(16) 0.0030(15) 0.0031(16) C43 0.027(2) 0.009(2) 0.012(2) 0.0006(16) 0.0054(17) 0.0029(17) C44 0.038(3) 0.017(2) 0.019(2) 0.0021(18) 0.0150(19) 0.0026(19) C45 0.029(2) 0.014(2) 0.020(2) 0.0022(17) 0.0063(18) 0.0100(18) C46 0.028(2) 0.020(3) 0.021(2) -0.0004(18) 0.0070(18) -0.0049(18) C47 0.0180(19) 0.010(2) 0.0092(19) -0.0003(15) 0.0037(15) 0.0008(15) C48 0.026(2) 0.020(2) 0.010(2) 0.0016(16) 0.0068(16) 0.0034(17) C49 0.018(2) 0.019(2) 0.019(2) -0.0010(17) 0.0030(16) 0.0045(17) C50 0.028(2) 0.013(2) 0.013(2) -0.0018(16) 0.0045(17) -0.0010(17) C51 0.022(2) 0.008(2) 0.012(2) 0.0010(15) 0.0029(16) -0.0025(16) C52 0.028(2) 0.015(2) 0.023(2) 0.0048(18) 0.0068(18) 0.0032(18) C53 0.021(2) 0.017(2) 0.027(2) 0.0020(18) 0.0055(18) -0.0042(17) C54 0.037(2) 0.014(2) 0.017(2) 0.0008(17) 0.0106(19) -0.0055(18) _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 Au1 Cl4 2.2693(9) . ? Au1 Cl3 2.2698(10) . ? Au2 Cl5 2.2651(10) . ? Au2 Cl6 2.2702(10) . ? Pt1 N2 1.934(3) . ? Pt1 N3 2.016(3) . ? Pt1 N1 2.017(3) . ? Pt1 Cl1 2.3024(9) . ? Pt2 N5 1.931(3) . ? Pt2 N4 2.004(3) . ? Pt2 N6 2.016(3) . ? Pt2 Cl2 2.3069(9) . ? N1 C1 1.344(5) . ? N1 C5 1.369(4) . ? N2 C10 1.334(4) . ? N2 C6 1.347(4) . ? N3 C15 1.337(4) . ? N3 C11 1.381(4) . ? N4 C28 1.332(4) . ? N4 C32 1.385(4) . ? N5 C33 1.348(4) . ? N5 C37 1.354(4) . ? N6 C42 1.336(4) . ? N6 C38 1.371(4) . ? C1 C2 1.384(5) . ? C1 H1A 0.9500 . ? C2 C3 1.395(5) . ? C2 H2A 0.9500 . ? C3 C4 1.391(5) . ? C3 C16 1.536(5) . ? C4 C5 1.385(5) . ? C4 H4A 0.9500 . ? C5 C6 1.475(5) . ? C6 C7 1.387(5) . ? C7 C8 1.397(5) . ? C7 H7A 0.9500 . ? C8 C9 1.404(5) . ? C8 C20 1.536(5) . ? C9 C10 1.391(5) . ? C9 H9A 0.9500 . ? C10 C11 1.485(5) . ? C11 C12 1.368(5) . ? C12 C13 1.399(5) . ? C12 H12A 0.9500 . ? C13 C14 1.388(5) . ? C13 C24 1.533(5) . ? C14 C15 1.378(5) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C19 1.524(5) . ? C16 C18 1.528(5) . ? C16 C17 1.547(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C23 1.521(5) . ? C20 C22 1.532(5) . ? C20 C21 1.540(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C27 1.525(5) . ? C24 C26 1.543(5) . ? C24 C25 1.544(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.390(5) . ? C28 H28A 0.9500 . ? C29 C30 1.393(5) . ? C29 H29A 0.9500 . ? C30 C31 1.411(5) . ? C30 C43 1.526(5) . ? C31 C32 1.365(5) . ? C31 H31A 0.9500 . ? C32 C33 1.494(5) . ? C33 C34 1.387(5) . ? C34 C35 1.411(5) . ? C34 H34A 0.9500 . ? C35 C36 1.389(5) . ? C35 C47 1.538(5) . ? C36 C37 1.387(5) . ? C36 H36A 0.9500 . ? C37 C38 1.468(5) . ? C38 C39 1.390(5) . ? C39 C40 1.386(5) . ? C39 H39A 0.9500 . ? C40 C41 1.394(5) . ? C40 C51 1.517(5) . ? C41 C42 1.380(5) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C46 1.531(5) . ? C43 C45 1.535(5) . ? C43 C44 1.540(5) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.536(5) . ? C47 C50 1.537(5) . ? C47 C49 1.547(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C54 1.528(5) . ? C51 C52 1.541(5) . ? C51 C53 1.541(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? 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 Cl4 Au1 Cl3 178.83(4) . . ? Cl5 Au2 Cl6 178.76(4) . . ? N2 Pt1 N3 80.97(12) . . ? N2 Pt1 N1 81.09(12) . . ? N3 Pt1 N1 162.01(11) . . ? N2 Pt1 Cl1 179.05(9) . . ? N3 Pt1 Cl1 99.01(8) . . ? N1 Pt1 Cl1 98.95(9) . . ? N5 Pt2 N4 80.91(12) . . ? N5 Pt2 N6 81.24(12) . . ? N4 Pt2 N6 161.98(11) . . ? N5 Pt2 Cl2 177.79(9) . . ? N4 Pt2 Cl2 99.08(8) . . ? N6 Pt2 Cl2 98.85(8) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Pt1 128.1(2) . . ? C5 N1 Pt1 113.2(2) . . ? C10 N2 C6 123.2(3) . . ? C10 N2 Pt1 118.6(2) . . ? C6 N2 Pt1 118.1(2) . . ? C15 N3 C11 118.5(3) . . ? C15 N3 Pt1 128.1(2) . . ? C11 N3 Pt1 113.4(2) . . ? C28 N4 C32 118.7(3) . . ? C28 N4 Pt2 127.2(3) . . ? C32 N4 Pt2 114.0(2) . . ? C33 N5 C37 122.8(3) . . ? C33 N5 Pt2 119.4(2) . . ? C37 N5 Pt2 117.8(2) . . ? C42 N6 C38 119.4(3) . . ? C42 N6 Pt2 127.5(2) . . ? C38 N6 Pt2 113.0(2) . . ? N1 C1 C2 121.9(3) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C1 C2 C3 120.5(4) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C4 C3 C2 117.0(3) . . ? C4 C3 C16 122.5(3) . . ? C2 C3 C16 120.5(3) . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 124.1(3) . . ? N2 C6 C7 119.1(3) . . ? N2 C6 C5 112.7(3) . . ? C7 C6 C5 128.1(3) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C8 C9 118.6(3) . . ? C7 C8 C20 120.7(3) . . ? C9 C8 C20 120.5(3) . . ? C10 C9 C8 119.3(3) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? N2 C10 C9 119.8(3) . . ? N2 C10 C11 113.0(3) . . ? C9 C10 C11 127.2(3) . . ? C12 C11 N3 121.0(3) . . ? C12 C11 C10 125.1(3) . . ? N3 C11 C10 113.9(3) . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C14 C13 C12 116.9(3) . . ? C14 C13 C24 122.8(3) . . ? C12 C13 C24 120.3(3) . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? N3 C15 C14 122.1(3) . . ? N3 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? C19 C16 C18 109.3(3) . . ? C19 C16 C3 111.6(3) . . ? C18 C16 C3 108.2(3) . . ? C19 C16 C17 108.9(3) . . ? C18 C16 C17 109.8(3) . . ? C3 C16 C17 109.1(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C23 C20 C22 110.1(3) . . ? C23 C20 C8 111.8(3) . . ? C22 C20 C8 106.6(3) . . ? C23 C20 C21 108.5(3) . . ? C22 C20 C21 108.7(3) . . ? C8 C20 C21 111.2(3) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C24 C13 111.1(3) . . ? C27 C24 C26 109.3(3) . . ? C13 C24 C26 107.4(3) . . ? C27 C24 C25 108.7(3) . . ? C13 C24 C25 111.4(3) . . ? C26 C24 C25 108.8(3) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 122.2(3) . . ? N4 C28 H28A 118.9 . . ? C29 C28 H28A 118.9 . . ? C28 C29 C30 120.4(3) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C29 C30 C31 116.6(4) . . ? C29 C30 C43 122.9(3) . . ? C31 C30 C43 120.3(3) . . ? C32 C31 C30 120.9(3) . . ? C32 C31 H31A 119.5 . . ? C30 C31 H31A 119.5 . . ? C31 C32 N4 121.1(3) . . ? C31 C32 C33 124.9(3) . . ? N4 C32 C33 114.0(3) . . ? N5 C33 C34 119.9(3) . . ? N5 C33 C32 111.6(3) . . ? C34 C33 C32 128.5(3) . . ? C33 C34 C35 119.2(3) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C36 C35 C34 118.6(3) . . ? C36 C35 C47 120.9(3) . . ? C34 C35 C47 120.3(3) . . ? C37 C36 C35 120.7(3) . . ? C37 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? N5 C37 C36 118.8(3) . . ? N5 C37 C38 112.9(3) . . ? C36 C37 C38 128.3(3) . . ? N6 C38 C39 120.2(3) . . ? N6 C38 C37 114.9(3) . . ? C39 C38 C37 124.8(3) . . ? C40 C39 C38 121.3(3) . . ? C40 C39 H39A 119.4 . . ? C38 C39 H39A 119.4 . . ? C39 C40 C41 116.5(3) . . ? C39 C40 C51 122.7(3) . . ? C41 C40 C51 120.7(3) . . ? C42 C41 C40 121.1(4) . . ? C42 C41 H41A 119.5 . . ? C40 C41 H41A 119.5 . . ? N6 C42 C41 121.5(3) . . ? N6 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C30 C43 C46 110.0(3) . . ? C30 C43 C45 106.8(3) . . ? C46 C43 C45 110.9(3) . . ? C30 C43 C44 111.2(3) . . ? C46 C43 C44 108.5(3) . . ? C45 C43 C44 109.4(3) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C50 108.4(3) . . ? C48 C47 C35 111.3(3) . . ? C50 C47 C35 111.8(3) . . ? C48 C47 C49 108.2(3) . . ? C50 C47 C49 109.8(3) . . ? C35 C47 C49 107.3(3) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C40 C51 C54 111.9(3) . . ? C40 C51 C52 110.8(3) . . ? C54 C51 C52 107.9(3) . . ? C40 C51 C53 107.3(3) . . ? C54 C51 C53 109.5(3) . . ? C52 C51 C53 109.4(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.668 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.152 #===END