data_global _audit_creation_method SHELXL-97 #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Okada, K.' _publ_contact_author_address ; Department of Chemistry, Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558-8585, Japan ; _publ_contact_author_email 'okadak@sci.osaka-cu.ac.jp' _publ_contact_author_fax '+81-666902709' _publ_contact_author_phone '+81-66052568' _publ_contact_letter 'August06 in 2012' _publ_requested_journal ; Journal of the American Chemical Society ; #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; NCN Pincer-Pt Complexes Coordinated by (Nitronyl Nitroxide)-2-ide Radical Anion ; _publ_section_title_footnote ; New pincer-Pt complexes coordinated by (nitronyl nitroxide)-2-ide radical anion were prepared in high yield as stable compounds. The structures of these Pt-complexes and the oxidized complexes were unequivocally determined by spectral and crystal structure analyses. The oxidation potential of the nitronyl nitroxide moiety in these complexes shifted to the negative direction (by about 0.6 V) by coordination to a Pt(II) atom. ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Xun Zhang' ; FIRST AUTHORS FOOTNOTES ; ; Department of Chemistry, Graduate School of Science, Osaka City University, ; # TEXT _audit_creation_date '2010-11-18' _audit_author_name 'Tanaka, R.' #========================================================= data_1(NN-Pt(NCN)-1)-EtOH # CHEMICAL DATA _chemical_formula_moiety 'C23 H23 N4 O2 Pt, 2(C2 H6 O)' _chemical_formula_sum 'C27 H35 N4 O4 Pt' _chemical_formula_weight 674.68 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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8562(13) _cell_length_b 10.4837(19) _cell_length_c 16.091(3) _cell_angle_alpha 81.251(17) _cell_angle_beta 75.385(17) _cell_angle_gamma 66.316(13) _cell_volume 1321.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5751 _cell_measurement_theta_min 4.0033 _cell_measurement_theta_max 27.4835 _exptl_crystal_preparation 'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 120(2) K' _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Red' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 670 _exptl_absorpt_coefficient_mu 5.348 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.1287 _exptl_absorpt_correction_T_max 0.8560 _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_special_details ; The diameter of collimator is 1.0 mm ; # EXPERIMENTAL DATA _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector 'CCD' _diffrn_measurement_method '\w or \f' _diffrn_measurement_device 'Mercury CCD (2x2 bin mode)' _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_device_details 'AFC7: Eulerian 3-circle' _diffrn_detector_area_resol_mean 7.32 _diffrn_ambient_temperature 120(2) _diffrn_source_power 16.8000 _diffrn_source_voltage 60.0000 _diffrn_source_current 280.0000 _diffrn_reflns_number 12972 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measurement_details ; scan: Number of images: 360 Slice: -80.0000 - 100.0000 Image width: 0.5000 Exp time: 2.0000 Rotation axis: Phi Omega: 0.0000 Chi: 0.0000 Phi: 0.0000 XTD: 35.1993 2theta: 9.8495 scan: Number of images: 100 Slice: -30.0000 - 20.0000 Image width: 0.5000 Exp time: 2.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 0.0000 XTD: 35.1993 2theta: 9.8495 scan: Number of images: 100 Slice: -30.0000 - 20.0000 Image width: 0.5000 Exp time: 2.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 90.0000 XTD: 35.1993 2theta: 9.8495 scan: Number of images: 100 Slice: -30.0000 - 20.0000 Image width: 0.5000 Exp time: 2.0000 Rotation axis: Omega Omega: 0.0000 Chi: 90.0000 Phi: 180.0000 XTD: 35.1993 2theta: 9.8495 ; # REFINEMENT DATA _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. ; _reflns_number_total 5919 _reflns_number_gt 5316 _reflns_threshold_expression >2sigma(I) _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^)+(0.0140P)^2^+23.5520P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5919 _refine_ls_number_parameters 323 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.795 _refine_diff_density_min -2.335 _refine_diff_density_rms 0.233 _computing_data_collection 'CrystalClear (Rigaku, 2001)' _computing_cell_refinement 'CrystalClear' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL97' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 0.69457(4) 0.55031(4) 0.57045(2) 0.01681(10) Uani 1 1 d . . . N1 N 0.6090(9) 0.3909(7) 0.5955(5) 0.0188(14) Uani 1 1 d . . . N2 N 0.8115(8) 0.6797(7) 0.5027(5) 0.0171(14) Uani 1 1 d . . . C1 C 0.6475(10) 0.3118(8) 0.5277(6) 0.0167(16) Uani 1 1 d . . . C2 C 0.5928(11) 0.2027(9) 0.5348(6) 0.0217(18) Uani 1 1 d . . . H2A H 0.6185 0.1499 0.4865 0.026 Uiso 1 1 calc R . . C3 C 0.5006(11) 0.1717(9) 0.6126(6) 0.0234(19) Uani 1 1 d . . . H3A H 0.4621 0.0977 0.6181 0.028 Uiso 1 1 calc R . . C4 C 0.4647(11) 0.2499(10) 0.6826(6) 0.0231(18) Uani 1 1 d . . . H4A H 0.4039 0.2289 0.7370 0.028 Uiso 1 1 calc R . . C5 C 0.5203(11) 0.3609(9) 0.6713(6) 0.0214(17) Uani 1 1 d . . . H5A H 0.4945 0.4160 0.7185 0.026 Uiso 1 1 calc R . . C6 C 0.7826(10) 0.4684(8) 0.4597(5) 0.0130(10) Uani 1 1 d . . . C7 C 0.7517(10) 0.3519(9) 0.4492(5) 0.0174(16) Uani 1 1 d . . . C8 C 0.8152(11) 0.2914(9) 0.3688(6) 0.0238(18) Uani 1 1 d . . . H8A H 0.7923 0.2137 0.3604 0.029 Uiso 1 1 calc R . . C9 C 0.9135(9) 0.3462(8) 0.3002(5) 0.0121(14) Uani 1 1 d . . . H9A H 0.9572 0.3054 0.2461 0.015 Uiso 1 1 calc R . . C10 C 0.9450(11) 0.4631(9) 0.3143(6) 0.0223(18) Uani 1 1 d . . . H10A H 1.0113 0.5006 0.2696 0.027 Uiso 1 1 calc R . . C11 C 0.8774(10) 0.5231(8) 0.3947(5) 0.0130(10) Uani 1 1 d . . . C12 C 0.8913(10) 0.6471(8) 0.4203(5) 0.0169(16) Uani 1 1 d . . . C13 C 0.9745(11) 0.7271(9) 0.3664(6) 0.0206(17) Uani 1 1 d . . . H13A H 1.0294 0.7037 0.3088 0.025 Uiso 1 1 calc R . . C14 C 0.9744(11) 0.8427(9) 0.3998(6) 0.026(2) Uani 1 1 d . . . H14A H 1.0316 0.8980 0.3648 0.031 Uiso 1 1 calc R . . C15 C 0.8928(10) 0.8769(9) 0.4826(6) 0.0202(17) Uani 1 1 d . . . H15A H 0.8909 0.9563 0.5051 0.024 Uiso 1 1 calc R . . C16 C 0.8117(10) 0.7917(8) 0.5336(6) 0.0195(17) Uani 1 1 d . . . H16A H 0.7558 0.8139 0.5913 0.023 Uiso 1 1 calc R . . C17 C 0.5996(10) 0.6385(8) 0.6884(5) 0.0133(15) Uani 1 1 d . . . N3 N 0.6220(9) 0.5773(7) 0.7670(5) 0.0199(14) Uani 1 1 d . . . O1 O 0.7172(8) 0.4482(6) 0.7810(4) 0.0245(13) Uani 1 1 d . . . N4 N 0.4936(8) 0.7740(7) 0.7049(4) 0.0166(14) Uani 1 1 d . . . O2 O 0.4389(8) 0.8707(6) 0.6474(4) 0.0213(13) Uani 1 1 d . . . C18 C 0.5114(12) 0.6658(10) 0.8412(6) 0.0251(19) Uani 1 1 d . . . C19 C 0.4633(12) 0.8130(9) 0.7957(5) 0.0231(18) Uani 1 1 d . . . C20 C 0.3619(14) 0.6195(13) 0.8755(7) 0.039(3) Uani 1 1 d . . . H20A H 0.2986 0.6365 0.8303 0.059 Uiso 1 1 calc R . . H20B H 0.2877 0.6728 0.9253 0.059 Uiso 1 1 calc R . . H20C H 0.4040 0.5198 0.8928 0.059 Uiso 1 1 calc R . . C21 C 0.6095(14) 0.6404(11) 0.9110(6) 0.036(2) Uani 1 1 d . . . H21A H 0.6363 0.5440 0.9350 0.054 Uiso 1 1 calc R . . H21B H 0.5413 0.7048 0.9566 0.054 Uiso 1 1 calc R . . H21C H 0.7144 0.6558 0.8864 0.054 Uiso 1 1 calc R . . C22 C 0.2839(15) 0.9108(12) 0.8239(7) 0.042(3) Uani 1 1 d . . . H22A H 0.2616 0.9960 0.7861 0.063 Uiso 1 1 calc R . . H22B H 0.2651 0.9346 0.8832 0.063 Uiso 1 1 calc R . . H22C H 0.2078 0.8657 0.8208 0.063 Uiso 1 1 calc R . . C23 C 0.5855(15) 0.8816(11) 0.7949(7) 0.035(2) Uani 1 1 d . . . H23A H 0.5639 0.9641 0.7548 0.053 Uiso 1 1 calc R . . H23B H 0.7015 0.8154 0.7766 0.053 Uiso 1 1 calc R . . H23C H 0.5700 0.9096 0.8529 0.053 Uiso 1 1 calc R . . O3 O 0.6468(9) 0.2484(7) 0.8875(5) 0.059(3) Uani 1 1 d . A 1 H3O H 0.6789 0.3147 0.8692 0.088 Uiso 1 1 calc R A 1 C24 C 0.7717(9) 0.1200(7) 0.8474(5) 0.043(3) Uani 1 1 d R . . H24A H 0.8765 0.1342 0.8173 0.052 Uiso 1 1 calc R A 1 H24B H 0.7268 0.0940 0.8050 0.052 Uiso 1 1 calc R A 1 C25 C 0.8072(17) 0.0088(15) 0.9164(9) 0.056(3) Uani 1 1 d . A 1 H25A H 0.7006 0.0065 0.9520 0.084 Uiso 1 1 calc R A 1 H25B H 0.8700 0.0273 0.9522 0.084 Uiso 1 1 calc R A 1 H25C H 0.8745 -0.0814 0.8908 0.084 Uiso 1 1 calc R A 1 O4 O 0.3412(12) 0.2093(10) 0.9041(7) 0.063(3) Uani 1 1 d . B 1 H4O H 0.4223 0.2317 0.9039 0.094 Uiso 1 1 calc R B 1 C26 C 0.1882(16) 0.3323(15) 0.9103(10) 0.059(4) Uani 1 1 d . . . H26A H 0.1613 0.3738 0.9661 0.071 Uiso 1 1 calc R B 1 H26B H 0.2035 0.4022 0.8637 0.071 Uiso 1 1 calc R B 1 C27 C 0.0523(18) 0.2955(16) 0.9033(10) 0.063(4) Uani 1 1 d . B 1 H27A H 0.0393 0.2248 0.9488 0.095 Uiso 1 1 calc R B 1 H27B H 0.0774 0.2581 0.8470 0.095 Uiso 1 1 calc R B 1 H27C H -0.0525 0.3786 0.9093 0.095 Uiso 1 1 calc R B 1 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 0.01894(15) 0.01498(15) 0.01853(16) -0.00053(11) -0.00602(11) -0.00742(12) N1 0.016(3) 0.011(3) 0.028(4) -0.004(3) -0.007(3) -0.001(3) N2 0.015(3) 0.012(3) 0.023(4) 0.004(3) -0.002(3) -0.008(3) C1 0.017(4) 0.009(3) 0.026(4) -0.003(3) -0.011(3) -0.003(3) C2 0.026(4) 0.018(4) 0.025(5) -0.001(3) -0.014(4) -0.008(4) C3 0.020(4) 0.013(4) 0.043(6) 0.001(4) -0.016(4) -0.008(3) C4 0.024(4) 0.027(5) 0.019(4) 0.003(3) -0.004(3) -0.013(4) C5 0.020(4) 0.025(4) 0.019(4) -0.003(3) -0.008(3) -0.005(4) C6 0.015(2) 0.009(2) 0.016(3) 0.004(2) -0.007(2) -0.005(2) C7 0.016(4) 0.020(4) 0.016(4) -0.002(3) -0.006(3) -0.004(3) C8 0.028(4) 0.016(4) 0.032(5) -0.004(4) -0.011(4) -0.008(4) C9 0.010(3) 0.015(4) 0.009(4) -0.004(3) -0.002(3) -0.001(3) C10 0.017(4) 0.025(4) 0.020(4) 0.002(3) 0.001(3) -0.007(4) C11 0.015(2) 0.009(2) 0.016(3) 0.004(2) -0.007(2) -0.005(2) C12 0.015(4) 0.017(4) 0.017(4) 0.004(3) -0.007(3) -0.003(3) C13 0.019(4) 0.020(4) 0.017(4) 0.002(3) -0.004(3) -0.003(3) C14 0.023(4) 0.018(4) 0.038(5) 0.009(4) -0.008(4) -0.012(4) C15 0.018(4) 0.016(4) 0.027(5) 0.001(3) -0.008(3) -0.006(3) C16 0.020(4) 0.012(4) 0.026(5) -0.001(3) -0.009(3) -0.003(3) C17 0.016(4) 0.016(4) 0.014(4) 0.002(3) -0.003(3) -0.013(3) N3 0.022(3) 0.018(3) 0.018(4) 0.004(3) -0.006(3) -0.007(3) O1 0.025(3) 0.018(3) 0.028(3) 0.003(3) -0.006(3) -0.008(3) N4 0.018(3) 0.017(3) 0.018(4) -0.001(3) -0.004(3) -0.008(3) O2 0.030(3) 0.020(3) 0.019(3) 0.005(2) -0.011(3) -0.013(3) C18 0.027(4) 0.026(5) 0.019(4) -0.009(4) 0.001(4) -0.007(4) C19 0.035(5) 0.025(4) 0.012(4) -0.004(3) -0.007(4) -0.011(4) C20 0.034(6) 0.050(7) 0.034(6) 0.000(5) 0.001(5) -0.022(5) C21 0.049(6) 0.031(5) 0.021(5) -0.001(4) -0.010(4) -0.007(5) C22 0.047(7) 0.036(6) 0.030(6) -0.006(5) 0.000(5) -0.005(5) C23 0.054(7) 0.036(6) 0.032(6) -0.001(4) -0.015(5) -0.030(5) O3 0.055(5) 0.034(5) 0.068(6) 0.000(4) 0.013(5) -0.013(4) C24 0.047(7) 0.039(6) 0.052(7) 0.008(5) -0.020(6) -0.023(6) C25 0.046(7) 0.053(8) 0.061(9) 0.007(7) -0.013(6) -0.013(6) O4 0.056(6) 0.056(6) 0.069(7) -0.007(5) -0.004(5) -0.019(5) C26 0.045(7) 0.061(9) 0.066(9) -0.031(7) 0.005(6) -0.017(7) C27 0.057(8) 0.056(9) 0.075(11) 0.011(7) -0.014(8) -0.023(7) # MOLECULAR GEOMETRY _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 C6 1.935(8) . ? Pt1 N1 2.047(7) . ? Pt1 N2 2.051(6) . ? Pt1 C17 2.065(8) . ? N1 C5 1.342(11) . ? N1 C1 1.362(10) . ? N2 C16 1.345(10) . ? N2 C12 1.357(11) . ? C1 C2 1.390(11) . ? C1 C7 1.478(12) . ? C2 C3 1.383(13) . ? C2 H2A 0.9500 . ? C3 C4 1.391(13) . ? C3 H3A 0.9500 . ? C4 C5 1.407(12) . ? C4 H4A 0.9500 . ? C5 H5A 0.9500 . ? C6 C11 1.374(10) . ? C6 C7 1.396(11) . ? C7 C8 1.410(12) . ? C8 C9 1.425(12) . ? C8 H8A 0.9500 . ? C9 C10 1.422(12) . ? C9 H9A 0.9500 . ? C10 C11 1.409(12) . ? C10 H10A 0.9500 . ? C11 C12 1.480(11) . ? C12 C13 1.397(11) . ? C13 C14 1.398(12) . ? C13 H13A 0.9500 . ? C14 C15 1.371(13) . ? C14 H14A 0.9500 . ? C15 C16 1.407(12) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 N3 1.353(10) . ? C17 N4 1.373(10) . ? N3 O1 1.295(9) . ? N3 C18 1.504(11) . ? N4 O2 1.291(9) . ? N4 C19 1.507(10) . ? C18 C21 1.518(13) . ? C18 C20 1.536(13) . ? C18 C19 1.543(13) . ? C19 C22 1.501(14) . ? C19 C23 1.518(13) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 . ? O3 C24 1.4694 . ? O3 H3O 0.8400 . ? C24 C25 1.476(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O4 C26 1.441(16) . ? O4 H4O 0.8400 . ? C26 C27 1.437(18) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? 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 C6 Pt1 N1 80.0(3) . . ? C6 Pt1 N2 79.2(3) . . ? N1 Pt1 N2 159.2(3) . . ? C6 Pt1 C17 179.7(4) . . ? N1 Pt1 C17 100.0(3) . . ? N2 Pt1 C17 100.8(3) . . ? C5 N1 C1 119.5(7) . . ? C5 N1 Pt1 125.5(6) . . ? C1 N1 Pt1 115.1(6) . . ? C16 N2 C12 119.6(7) . . ? C16 N2 Pt1 124.9(6) . . ? C12 N2 Pt1 115.5(5) . . ? N1 C1 C2 121.2(8) . . ? N1 C1 C7 114.1(7) . . ? C2 C1 C7 124.7(8) . . ? C3 C2 C1 119.6(8) . . ? C3 C2 H2A 120.2 . . ? C1 C2 H2A 120.2 . . ? C2 C3 C4 119.4(8) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C3 C4 C5 118.6(8) . . ? C3 C4 H4A 120.7 . . ? C5 C4 H4A 120.7 . . ? N1 C5 C4 121.7(8) . . ? N1 C5 H5A 119.1 . . ? C4 C5 H5A 119.1 . . ? C11 C6 C7 121.8(7) . . ? C11 C6 Pt1 119.6(5) . . ? C7 C6 Pt1 118.6(6) . . ? C6 C7 C8 119.0(8) . . ? C6 C7 C1 112.2(7) . . ? C8 C7 C1 128.8(7) . . ? C7 C8 C9 120.3(7) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C10 C9 C8 118.8(7) . . ? C10 C9 H9A 120.6 . . ? C8 C9 H9A 120.6 . . ? C11 C10 C9 119.6(7) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C6 C11 C10 120.3(7) . . ? C6 C11 C12 112.2(7) . . ? C10 C11 C12 127.4(7) . . ? N2 C12 C13 121.7(8) . . ? N2 C12 C11 113.5(7) . . ? C13 C12 C11 124.8(8) . . ? C12 C13 C14 118.0(8) . . ? C12 C13 H13A 121.0 . . ? C14 C13 H13A 121.0 . . ? C15 C14 C13 120.6(8) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C16 118.5(8) . . ? C14 C15 H15A 120.8 . . ? C16 C15 H15A 120.8 . . ? N2 C16 C15 121.6(8) . . ? N2 C16 H16A 119.2 . . ? C15 C16 H16A 119.2 . . ? N3 C17 N4 103.8(7) . . ? N3 C17 Pt1 128.8(6) . . ? N4 C17 Pt1 127.4(6) . . ? O1 N3 C17 124.5(7) . . ? O1 N3 C18 120.3(7) . . ? C17 N3 C18 114.8(7) . . ? O2 N4 C17 125.0(7) . . ? O2 N4 C19 119.1(7) . . ? C17 N4 C19 115.2(7) . . ? N3 C18 C21 109.6(8) . . ? N3 C18 C20 106.5(7) . . ? C21 C18 C20 109.7(8) . . ? N3 C18 C19 100.9(7) . . ? C21 C18 C19 115.5(8) . . ? C20 C18 C19 113.8(8) . . ? C22 C19 N4 110.1(8) . . ? C22 C19 C23 111.2(9) . . ? N4 C19 C23 106.4(7) . . ? C22 C19 C18 115.7(8) . . ? N4 C19 C18 99.2(7) . . ? C23 C19 C18 113.2(8) . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 O3 H3O 109.5 . . ? O3 C24 C25 107.7(7) . . ? O3 C24 H24A 110.2 . . ? C25 C24 H24A 110.2 . . ? O3 C24 H24B 110.2 . . ? C25 C24 H24B 110.2 . . ? H24A C24 H24B 108.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? C26 O4 H4O 109.5 . . ? C27 C26 O4 109.4(12) . . ? C27 C26 H26A 109.8 . . ? O4 C26 H26A 109.8 . . ? C27 C26 H26B 109.8 . . ? O4 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Pt1 N1 C5 178.8(7) . . . . ? N2 Pt1 N1 C5 -179.5(7) . . . . ? C17 Pt1 N1 C5 -1.5(7) . . . . ? C6 Pt1 N1 C1 -1.5(6) . . . . ? N2 Pt1 N1 C1 0.2(11) . . . . ? C17 Pt1 N1 C1 178.2(6) . . . . ? C6 Pt1 N2 C16 177.7(7) . . . . ? N1 Pt1 N2 C16 176.1(7) . . . . ? C17 Pt1 N2 C16 -2.0(7) . . . . ? C6 Pt1 N2 C12 -1.4(6) . . . . ? N1 Pt1 N2 C12 -3.1(11) . . . . ? C17 Pt1 N2 C12 178.9(6) . . . . ? C5 N1 C1 C2 1.8(11) . . . . ? Pt1 N1 C1 C2 -177.9(6) . . . . ? C5 N1 C1 C7 -177.5(7) . . . . ? Pt1 N1 C1 C7 2.8(8) . . . . ? N1 C1 C2 C3 -1.4(12) . . . . ? C7 C1 C2 C3 177.8(8) . . . . ? C1 C2 C3 C4 -0.2(12) . . . . ? C2 C3 C4 C5 1.5(13) . . . . ? C1 N1 C5 C4 -0.4(12) . . . . ? Pt1 N1 C5 C4 179.3(6) . . . . ? C3 C4 C5 N1 -1.2(13) . . . . ? N1 Pt1 C6 C11 -178.3(6) . . . . ? N2 Pt1 C6 C11 2.3(6) . . . . ? C17 Pt1 C6 C11 87(64) . . . . ? N1 Pt1 C6 C7 -0.3(6) . . . . ? N2 Pt1 C6 C7 -179.7(6) . . . . ? C17 Pt1 C6 C7 -95(64) . . . . ? C11 C6 C7 C8 -2.0(12) . . . . ? Pt1 C6 C7 C8 180.0(6) . . . . ? C11 C6 C7 C1 179.8(7) . . . . ? Pt1 C6 C7 C1 1.8(9) . . . . ? N1 C1 C7 C6 -2.9(10) . . . . ? C2 C1 C7 C6 177.8(7) . . . . ? N1 C1 C7 C8 179.1(8) . . . . ? C2 C1 C7 C8 -0.2(14) . . . . ? C6 C7 C8 C9 1.8(12) . . . . ? C1 C7 C8 C9 179.7(8) . . . . ? C7 C8 C9 C10 -0.4(12) . . . . ? C8 C9 C10 C11 -0.7(12) . . . . ? C7 C6 C11 C10 0.8(12) . . . . ? Pt1 C6 C11 C10 178.8(6) . . . . ? C7 C6 C11 C12 179.3(7) . . . . ? Pt1 C6 C11 C12 -2.7(9) . . . . ? C9 C10 C11 C6 0.6(12) . . . . ? C9 C10 C11 C12 -177.7(7) . . . . ? C16 N2 C12 C13 0.1(11) . . . . ? Pt1 N2 C12 C13 179.2(6) . . . . ? C16 N2 C12 C11 -178.8(7) . . . . ? Pt1 N2 C12 C11 0.4(8) . . . . ? C6 C11 C12 N2 1.3(9) . . . . ? C10 C11 C12 N2 179.7(8) . . . . ? C6 C11 C12 C13 -177.5(7) . . . . ? C10 C11 C12 C13 0.9(13) . . . . ? N2 C12 C13 C14 0.4(12) . . . . ? C11 C12 C13 C14 179.1(7) . . . . ? C12 C13 C14 C15 -1.0(13) . . . . ? C13 C14 C15 C16 1.1(13) . . . . ? C12 N2 C16 C15 0.1(12) . . . . ? Pt1 N2 C16 C15 -179.0(6) . . . . ? C14 C15 C16 N2 -0.7(12) . . . . ? C6 Pt1 C17 N3 150(64) . . . . ? N1 Pt1 C17 N3 55.2(7) . . . . ? N2 Pt1 C17 N3 -125.5(7) . . . . ? C6 Pt1 C17 N4 -28(65) . . . . ? N1 Pt1 C17 N4 -122.7(6) . . . . ? N2 Pt1 C17 N4 56.6(7) . . . . ? N4 C17 N3 O1 -178.6(7) . . . . ? Pt1 C17 N3 O1 3.1(11) . . . . ? N4 C17 N3 C18 8.2(9) . . . . ? Pt1 C17 N3 C18 -170.1(6) . . . . ? N3 C17 N4 O2 179.8(7) . . . . ? Pt1 C17 N4 O2 -1.9(11) . . . . ? N3 C17 N4 C19 9.2(9) . . . . ? Pt1 C17 N4 C19 -172.4(5) . . . . ? O1 N3 C18 C21 43.3(10) . . . . ? C17 N3 C18 C21 -143.1(8) . . . . ? O1 N3 C18 C20 -75.3(10) . . . . ? C17 N3 C18 C20 98.2(9) . . . . ? O1 N3 C18 C19 165.6(7) . . . . ? C17 N3 C18 C19 -20.9(9) . . . . ? O2 N4 C19 C22 45.8(10) . . . . ? C17 N4 C19 C22 -143.0(8) . . . . ? O2 N4 C19 C23 -74.8(9) . . . . ? C17 N4 C19 C23 96.4(8) . . . . ? O2 N4 C19 C18 167.6(7) . . . . ? C17 N4 C19 C18 -21.3(9) . . . . ? N3 C18 C19 C22 139.9(8) . . . . ? C21 C18 C19 C22 -102.0(10) . . . . ? C20 C18 C19 C22 26.2(11) . . . . ? N3 C18 C19 N4 22.3(8) . . . . ? C21 C18 C19 N4 140.3(8) . . . . ? C20 C18 C19 N4 -91.4(9) . . . . ? N3 C18 C19 C23 -90.0(9) . . . . ? C21 C18 C19 C23 28.0(11) . . . . ? C20 C18 C19 C23 156.3(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3O O1 0.84 1.90 2.671(9) 151.3 . O4 H4O O3 0.84 2.01 2.838(12) 167.2 .