# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_3 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C22 H21 N3 O2 Pt' _chemical_formula_sum 'C22 H21 N3 O2 Pt' _chemical_formula_weight 554.51 _chemical_compound_source 'see text' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 25.953(5) _cell_length_b 11.773(2) _cell_length_c 14.429(3) _cell_angle_alpha 90 _cell_angle_beta 103.65(3) _cell_angle_gamma 90 _cell_volume 4284.2(15) _cell_formula_units_Z 8 _cell_measurement_temperature 198 _cell_measurement_reflns_used 971 _cell_measurement_theta_min 4.09 _cell_measurement_theta_max 27.02 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.390 _exptl_crystal_size_min 0.340 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 6.571 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.186 _exptl_absorpt_correction_T_max 0.212 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Tronnier ; _diffrn_ambient_temperature 198 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Bruker KappaCCD' _diffrn_measurement_method 'phi- and omega-rotation' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 # number of measured reflections (redundant set) _diffrn_reflns_number 84091 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_unetI/netI 0.0110 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.83 _diffrn_reflns_theta_max 25.40 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3917 # number of observed reflections (> n sig(I)) _reflns_number_gt 3478 _reflns_threshold_expression I>2\s(I) _audit_creation_method 'PLATON option' _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+31.1323P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3917 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0257 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0539 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.881 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.117 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt Uani 0.26445(1) 0.14399(1) 0.43779(1) 1.000 0.0192(1) d . . . O1 O Uani 0.30075(12) 0.0343(3) 0.5474(2) 1.000 0.0312(10) d . . . O2 O Uani 0.19357(12) 0.0615(3) 0.4297(2) 1.000 0.0284(9) d . . . N1 N Uani 0.31811(13) 0.3124(3) 0.3569(2) 1.000 0.0216(10) d . . . N2 N Uani 0.37824(13) 0.2352(3) 0.4699(2) 1.000 0.0245(10) d . . . N3 N Uani 0.06744(17) 0.2865(4) 0.0918(3) 1.000 0.0485(16) d . . . C1 C Uani 0.32597(16) 0.2320(4) 0.4270(3) 1.000 0.0220(12) d . . . C2 C Uani 0.40394(17) 0.3159(4) 0.4256(3) 1.000 0.0252(12) d . . . C3 C Uani 0.36553(16) 0.3665(4) 0.3538(3) 1.000 0.0235(12) d . . . C4 C Uani 0.37829(18) 0.4522(4) 0.2973(3) 1.000 0.0334(16) d . . . C5 C Uani 0.4312(2) 0.4846(5) 0.3150(4) 1.000 0.0418(17) d . . . C6 C Uani 0.46920(18) 0.4339(5) 0.3854(4) 1.000 0.0398(16) d . . . C7 C Uani 0.45711(18) 0.3477(4) 0.4417(3) 1.000 0.0325(14) d . . . C8 C Uani 0.26527(16) 0.3186(4) 0.2991(3) 1.000 0.0231(12) d . . . C9 C Uani 0.23180(16) 0.2402(3) 0.3280(3) 1.000 0.0214(12) d . . . C10 C Uani 0.18015(16) 0.2360(4) 0.2745(3) 1.000 0.0239(12) d . . . C11 C Uani 0.16302(17) 0.3070(4) 0.1951(3) 1.000 0.0274(9) d . . . C12 C Uani 0.19702(17) 0.3855(4) 0.1691(3) 1.000 0.0274(9) d . . . C13 C Uani 0.24900(18) 0.3934(4) 0.2228(3) 1.000 0.0321(14) d . . . C14 C Uani 0.10930(18) 0.2967(4) 0.1374(3) 1.000 0.0315(14) d . . . C15 C Uani 0.4036(2) 0.1636(5) 0.5531(4) 1.000 0.0481(12) d . . . C16 C Uani 0.4361(2) 0.2334(6) 0.6345(3) 1.000 0.049(2) d . . . C17 C Uani 0.4354(2) 0.0699(5) 0.5204(4) 1.000 0.0481(12) d . . . C18 C Uani 0.3143(2) -0.1173(5) 0.6549(5) 1.000 0.058(2) d . . . C19 C Uani 0.27886(19) -0.0477(4) 0.5793(4) 1.000 0.0353(17) d . . . C20 C Uani 0.2256(2) -0.0760(4) 0.5515(4) 1.000 0.0375(16) d . . . C21 C Uani 0.18646(18) -0.0237(4) 0.4810(3) 1.000 0.0289(12) d . . . C22 C Uani 0.1306(2) -0.0689(5) 0.4583(4) 1.000 0.0413(17) d . . . H4A H Uiso 0.35200 0.48720 0.24860 1.000 0.0400 c R . . H5A H Uiso 0.44130 0.54320 0.27760 1.000 0.0500 c R . . H6A H Uiso 0.50490 0.45900 0.39570 1.000 0.0480 c R . . H7A H Uiso 0.48380 0.31180 0.48920 1.000 0.0390 c R . . H10A H Uiso 0.15590 0.18430 0.29170 1.000 0.0290 c R . . H12A H Uiso 0.18490 0.43330 0.11530 1.000 0.0330 c R . . H13A H Uiso 0.27270 0.44810 0.20790 1.000 0.0390 c R . . H15A H Uiso 0.37450 0.12650 0.57690 1.000 0.0580 c R . . H16A H Uiso 0.41680 0.30320 0.64180 1.000 0.0730 c R . . H16B H Uiso 0.47020 0.25300 0.62050 1.000 0.0730 c R . . H16C H Uiso 0.44230 0.18930 0.69360 1.000 0.0730 c R . . H17A H Uiso 0.41260 0.02850 0.46720 1.000 0.0720 c R . . H17B H Uiso 0.44860 0.01730 0.57340 1.000 0.0720 c R . . H17C H Uiso 0.46530 0.10320 0.49960 1.000 0.0720 c R . . H18A H Uiso 0.35120 -0.10760 0.65070 1.000 0.0870 c R . . H18B H Uiso 0.30440 -0.19760 0.64580 1.000 0.0870 c R . . H18C H Uiso 0.31060 -0.09240 0.71780 1.000 0.0870 c R . . H20A H Uiso 0.21430 -0.13790 0.58410 1.000 0.0450 c R . . H22A H Uiso 0.10560 -0.00520 0.44760 1.000 0.0620 c R . . H22B H Uiso 0.12520 -0.11480 0.51190 1.000 0.0620 c R . . H22C H Uiso 0.12470 -0.11600 0.40080 1.000 0.0620 c 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 0.0200(1) 0.0179(1) 0.0208(1) 0.0006(1) 0.0071(1) 0.0000(1) O1 0.0309(17) 0.0300(18) 0.0331(17) 0.0099(14) 0.0081(14) 0.0023(14) O2 0.0291(16) 0.0277(16) 0.0299(16) 0.0014(13) 0.0101(13) -0.0055(13) N2 0.0205(17) 0.0268(19) 0.0259(18) 0.0020(15) 0.0047(14) 0.0003(15) N1 0.0175(17) 0.0220(17) 0.0241(18) 0.0042(14) 0.0023(14) -0.0005(14) N3 0.030(2) 0.054(3) 0.053(3) 0.002(2) -0.007(2) -0.002(2) C1 0.023(2) 0.021(2) 0.022(2) -0.0022(17) 0.0056(16) 0.0035(17) C2 0.026(2) 0.024(2) 0.026(2) -0.0020(18) 0.0069(18) -0.0022(18) C3 0.020(2) 0.026(2) 0.025(2) -0.0030(17) 0.0062(16) -0.0035(17) C4 0.026(2) 0.035(3) 0.037(3) 0.010(2) 0.0029(19) -0.006(2) C5 0.035(3) 0.043(3) 0.048(3) 0.014(2) 0.011(2) -0.011(2) C6 0.020(2) 0.050(3) 0.047(3) 0.006(2) 0.003(2) -0.012(2) C7 0.021(2) 0.040(3) 0.034(2) 0.001(2) 0.0014(19) -0.003(2) C8 0.020(2) 0.024(2) 0.025(2) -0.0002(17) 0.0049(17) 0.0017(17) C9 0.022(2) 0.019(2) 0.024(2) -0.0038(16) 0.0071(16) 0.0011(16) C10 0.023(2) 0.021(2) 0.028(2) -0.0030(17) 0.0067(17) 0.0001(17) C11 0.0233(15) 0.0241(16) 0.0329(17) 0.0014(13) 0.0030(13) 0.0005(12) C12 0.0233(15) 0.0241(16) 0.0329(17) 0.0014(13) 0.0030(13) 0.0005(12) C13 0.028(2) 0.031(2) 0.038(3) 0.009(2) 0.009(2) -0.004(2) C14 0.027(2) 0.034(3) 0.033(2) 0.001(2) 0.006(2) 0.001(2) C15 0.043(2) 0.038(2) 0.057(2) 0.0156(19) -0.0010(18) 0.0076(17) C16 0.030(3) 0.088(5) 0.026(2) 0.004(3) 0.002(2) -0.003(3) C17 0.043(2) 0.038(2) 0.057(2) 0.0156(19) -0.0010(18) 0.0076(17) C18 0.048(3) 0.058(4) 0.064(4) 0.042(3) 0.006(3) 0.005(3) C19 0.032(3) 0.036(3) 0.040(3) 0.013(2) 0.013(2) 0.001(2) C20 0.047(3) 0.027(2) 0.045(3) 0.012(2) 0.024(2) 0.000(2) C21 0.032(2) 0.029(2) 0.029(2) -0.0032(19) 0.0138(19) -0.0069(19) C22 0.038(3) 0.038(3) 0.051(3) 0.002(2) 0.017(2) -0.011(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.086(3) . . yes Pt1 O2 2.059(3) . . yes Pt1 C1 1.940(4) . . yes Pt1 C9 1.969(4) . . yes O1 C19 1.261(6) . . yes O2 C21 1.286(6) . . yes N2 C1 1.352(5) . . yes N2 C2 1.399(6) . . yes N2 C15 1.487(6) . . yes N1 C1 1.365(5) . . yes N1 C3 1.396(6) . . yes N1 C8 1.429(5) . . yes N3 C14 1.136(6) . . yes C2 C3 1.391(6) . . no C2 C7 1.395(7) . . no C3 C4 1.386(6) . . no C4 C5 1.390(7) . . no C5 C6 1.374(8) . . no C6 C7 1.382(7) . . no C8 C9 1.397(6) . . no C8 C13 1.395(6) . . no C9 C10 1.381(6) . . no C10 C11 1.403(6) . . no C11 C12 1.389(6) . . no C11 C14 1.450(6) . . no C12 C13 1.391(6) . . no C15 C16 1.516(8) . . no C15 C17 1.518(8) . . no C18 C19 1.495(8) . . no C19 C20 1.386(7) . . no C20 C21 1.399(7) . . no C21 C22 1.506(7) . . no C4 H4A 0.9500 . . no C5 H5A 0.9500 . . no C6 H6A 0.9500 . . no C7 H7A 0.9500 . . no C10 H10A 0.9500 . . no C12 H12A 0.9500 . . no C13 H13A 0.9500 . . no C15 H15A 1.0000 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C17 H17C 0.9800 . . no C18 H18A 0.9800 . . no C18 H18B 0.9800 . . no C18 H18C 0.9800 . . no C20 H20A 0.9500 . . no C22 H22A 0.9800 . . no C22 H22B 0.9800 . . no C22 H22C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 89.35(13) . . . yes O1 Pt1 C1 99.12(16) . . . yes O1 Pt1 C9 175.96(15) . . . yes O2 Pt1 C1 171.29(15) . . . yes O2 Pt1 C9 90.95(15) . . . yes C1 Pt1 C9 80.46(18) . . . yes Pt1 O1 C19 126.1(3) . . . yes Pt1 O2 C21 125.7(3) . . . yes C1 N2 C2 110.2(3) . . . yes C1 N2 C15 124.0(4) . . . yes C2 N2 C15 125.9(4) . . . yes C1 N1 C3 111.2(3) . . . yes C1 N1 C8 115.0(4) . . . yes C3 N1 C8 133.6(3) . . . yes Pt1 C1 N2 137.2(3) . . . yes Pt1 C1 N1 116.6(3) . . . yes N2 C1 N1 106.2(4) . . . yes N2 C2 C3 107.2(4) . . . yes N2 C2 C7 131.7(4) . . . yes C3 C2 C7 121.1(4) . . . no N1 C3 C2 105.3(4) . . . yes N1 C3 C4 133.3(4) . . . yes C2 C3 C4 121.4(4) . . . no C3 C4 C5 117.1(4) . . . no C4 C5 C6 121.5(5) . . . no C5 C6 C7 122.1(5) . . . no C2 C7 C6 116.9(4) . . . no N1 C8 C9 111.8(4) . . . yes N1 C8 C13 124.3(4) . . . yes C9 C8 C13 124.0(4) . . . no Pt1 C9 C8 116.1(3) . . . yes Pt1 C9 C10 127.3(3) . . . yes C8 C9 C10 116.5(4) . . . no C9 C10 C11 120.9(4) . . . no C10 C11 C12 121.2(4) . . . no C10 C11 C14 119.7(4) . . . no C12 C11 C14 119.1(4) . . . no C11 C12 C13 119.2(4) . . . no C8 C13 C12 118.1(4) . . . no N3 C14 C11 178.7(5) . . . yes N2 C15 C16 112.2(5) . . . yes N2 C15 C17 109.3(4) . . . yes C16 C15 C17 113.0(5) . . . no O1 C19 C18 115.7(4) . . . yes O1 C19 C20 125.7(5) . . . yes C18 C19 C20 118.7(5) . . . no C19 C20 C21 127.4(5) . . . no O2 C21 C20 125.7(4) . . . yes O2 C21 C22 114.3(4) . . . yes C20 C21 C22 119.9(4) . . . no C3 C4 H4A 121.00 . . . no C5 C4 H4A 122.00 . . . no C4 C5 H5A 119.00 . . . no C6 C5 H5A 119.00 . . . no C5 C6 H6A 119.00 . . . no C7 C6 H6A 119.00 . . . no C2 C7 H7A 122.00 . . . no C6 C7 H7A 121.00 . . . no C9 C10 H10A 120.00 . . . no C11 C10 H10A 120.00 . . . no C11 C12 H12A 120.00 . . . no C13 C12 H12A 120.00 . . . no C8 C13 H13A 121.00 . . . no C12 C13 H13A 121.00 . . . no N2 C15 H15A 107.00 . . . no C16 C15 H15A 107.00 . . . no C17 C15 H15A 107.00 . . . no C15 C16 H16A 109.00 . . . no C15 C16 H16B 109.00 . . . no C15 C16 H16C 110.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 110.00 . . . no H16B C16 H16C 109.00 . . . no C15 C17 H17A 109.00 . . . no C15 C17 H17B 109.00 . . . no C15 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H17A C17 H17C 110.00 . . . no H17B C17 H17C 110.00 . . . no C19 C18 H18A 109.00 . . . no C19 C18 H18B 110.00 . . . no C19 C18 H18C 110.00 . . . no H18A C18 H18B 109.00 . . . no H18A C18 H18C 109.00 . . . no H18B C18 H18C 109.00 . . . no C19 C20 H20A 116.00 . . . no C21 C20 H20A 116.00 . . . no C21 C22 H22A 109.00 . . . no C21 C22 H22B 109.00 . . . no C21 C22 H22C 110.00 . . . no H22A C22 H22B 109.00 . . . no H22A C22 H22C 110.00 . . . no H22B C22 H22C 109.00 . . . no 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 O2 Pt1 O1 C19 2.9(4) . . . . no C1 Pt1 O1 C19 -175.0(4) . . . . no O1 Pt1 O2 C21 -0.8(4) . . . . no C9 Pt1 O2 C21 175.2(4) . . . . no O1 Pt1 C1 N2 -0.5(5) . . . . no O1 Pt1 C1 N1 177.1(3) . . . . no C9 Pt1 C1 N2 -176.4(5) . . . . no C9 Pt1 C1 N1 1.2(3) . . . . no O2 Pt1 C9 C8 -179.3(3) . . . . no O2 Pt1 C9 C10 -1.8(4) . . . . no C1 Pt1 C9 C8 -0.8(3) . . . . no C1 Pt1 C9 C10 176.8(4) . . . . no Pt1 O1 C19 C18 177.0(4) . . . . no Pt1 O1 C19 C20 -4.3(7) . . . . no Pt1 O2 C21 C20 -0.1(7) . . . . no Pt1 O2 C21 C22 -178.7(3) . . . . no C2 N2 C1 Pt1 176.4(4) . . . . no C2 N2 C1 N1 -1.4(5) . . . . no C15 N2 C1 Pt1 -4.5(7) . . . . no C15 N2 C1 N1 177.7(4) . . . . no C1 N2 C2 C3 1.5(5) . . . . no C1 N2 C2 C7 -177.8(5) . . . . no C15 N2 C2 C3 -177.6(4) . . . . no C15 N2 C2 C7 3.1(8) . . . . no C1 N2 C15 C16 -128.1(5) . . . . no C1 N2 C15 C17 105.8(5) . . . . no C2 N2 C15 C16 50.9(6) . . . . no C2 N2 C15 C17 -75.2(6) . . . . no C3 N1 C1 Pt1 -177.5(3) . . . . no C3 N1 C1 N2 0.8(5) . . . . no C8 N1 C1 Pt1 -1.5(5) . . . . no C8 N1 C1 N2 176.8(3) . . . . no C1 N1 C3 C2 0.1(5) . . . . no C1 N1 C3 C4 -179.7(5) . . . . no C8 N1 C3 C2 -174.9(4) . . . . no C8 N1 C3 C4 5.3(8) . . . . no C1 N1 C8 C9 0.8(5) . . . . no C1 N1 C8 C13 -178.9(4) . . . . no C3 N1 C8 C9 175.7(4) . . . . no C3 N1 C8 C13 -4.0(7) . . . . no N2 C2 C3 N1 -1.0(5) . . . . no N2 C2 C3 C4 178.9(4) . . . . no C7 C2 C3 N1 178.5(4) . . . . no C7 C2 C3 C4 -1.7(7) . . . . no N2 C2 C7 C6 -178.6(5) . . . . no C3 C2 C7 C6 2.2(7) . . . . no N1 C3 C4 C5 -179.7(5) . . . . no C2 C3 C4 C5 0.6(7) . . . . no C3 C4 C5 C6 0.0(8) . . . . no C4 C5 C6 C7 0.6(9) . . . . no C5 C6 C7 C2 -1.6(8) . . . . no N1 C8 C9 Pt1 0.2(5) . . . . no N1 C8 C9 C10 -177.6(4) . . . . no C13 C8 C9 Pt1 179.9(4) . . . . no C13 C8 C9 C10 2.2(6) . . . . no N1 C8 C13 C12 176.2(4) . . . . no C9 C8 C13 C12 -3.5(7) . . . . no Pt1 C9 C10 C11 -177.1(3) . . . . no C8 C9 C10 C11 0.4(6) . . . . no C9 C10 C11 C12 -1.5(7) . . . . no C9 C10 C11 C14 176.9(4) . . . . no C10 C11 C12 C13 0.2(7) . . . . no C14 C11 C12 C13 -178.3(4) . . . . no C11 C12 C13 C8 2.2(7) . . . . no O1 C19 C20 C21 3.0(9) . . . . no C18 C19 C20 C21 -178.4(5) . . . . no C19 C20 C21 O2 -0.5(9) . . . . no C19 C20 C21 C22 178.0(5) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C7 H7A N3 0.9500 2.5900 3.530(6) 168.00 8_555 yes C10 H10A O2 0.9500 2.4700 2.998(5) 115.00 . yes C15 H15A O1 1.0000 2.1500 3.057(6) 149.00 . yes # Loop Mechanism for Extra Tables(s) 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 _platon_squeeze_void_content 1 0.500 0.138 0.250 126 18 ' ' 2 0.500 -0.138 0.750 125 18 ' ' 3 1.000 0.362 0.750 125 18 ' ' 4 0.000 0.638 0.250 126 18 ' ' _platon_squeeze_details ; The unit cell contains one dcm molecule which has been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _iucr_refine_instructions_details ; TITL AT 151 CELL 0.71073 25.9530 11.7730 14.4290 90.000 103.654 90.000 ZERR 8 0.0050 0.0020 0.0030 0.000 0.030 0.000 LATT 7 SYMM - X , Y , 0.50000 - Z SFAC H C N O Pt UNIT 168 176 24 16 8 L.S. 28 ACTA BOND $H FMAP -2 PLAN 1 CONF EADP C15 C17 EADP C11 C12 OMIT -31 1 2 OMIT 31 -1 -2 SIZE 0.343 0.385 0.386 TEMP -75 WGHT 0.022800 31.132299 FVAR 1.01807 PT1 5 0.264453 0.143989 0.437791 11.00000 0.02000 0.01789 = 0.02077 0.00055 0.00713 0.00000 O1 4 0.300754 0.034305 0.547436 11.00000 0.03090 0.03002 = 0.03307 0.00993 0.00814 0.00227 O2 4 0.193566 0.061477 0.429694 11.00000 0.02906 0.02773 = 0.02988 0.00136 0.01006 -0.00548 N1 3 0.378240 0.235183 0.469931 11.00000 0.02046 0.02677 = 0.02593 0.00199 0.00470 0.00034 N2 3 0.318111 0.312423 0.356872 11.00000 0.01751 0.02204 = 0.02410 0.00418 0.00232 -0.00046 N3 3 0.067439 0.286502 0.091808 11.00000 0.03036 0.05419 = 0.05310 0.00222 -0.00657 -0.00184 C1 2 0.325974 0.232018 0.426955 11.00000 0.02333 0.02089 = 0.02216 -0.00221 0.00562 0.00345 C2 2 0.403944 0.315873 0.425589 11.00000 0.02586 0.02385 = 0.02649 -0.00203 0.00695 -0.00222 C3 2 0.365526 0.366522 0.353799 11.00000 0.01981 0.02645 = 0.02488 -0.00305 0.00622 -0.00353 C4 2 0.378290 0.452172 0.297313 11.00000 0.02589 0.03545 = 0.03686 0.00952 0.00293 -0.00574 AFIX 43 H4A 1 0.352022 0.487194 0.248605 11.00000 -1.20000 AFIX 0 C5 2 0.431182 0.484641 0.314989 11.00000 0.03464 0.04275 = 0.04818 0.01443 0.01131 -0.01087 AFIX 43 H5A 1 0.441298 0.543179 0.277560 11.00000 -1.20000 AFIX 0 C6 2 0.469196 0.433947 0.385425 11.00000 0.01982 0.04951 = 0.04728 0.00583 0.00340 -0.01158 AFIX 43 H6A 1 0.504899 0.458977 0.395725 11.00000 -1.20000 AFIX 0 C7 2 0.457113 0.347739 0.441710 11.00000 0.02148 0.04014 = 0.03380 0.00106 0.00140 -0.00331 AFIX 43 H7A 1 0.483756 0.311820 0.489180 11.00000 -1.20000 AFIX 0 C8 2 0.265272 0.318631 0.299088 11.00000 0.01952 0.02368 = 0.02461 -0.00019 0.00488 0.00168 C9 2 0.231798 0.240199 0.327980 11.00000 0.02203 0.01946 = 0.02398 -0.00381 0.00714 0.00113 C10 2 0.180153 0.235963 0.274519 11.00000 0.02278 0.02147 = 0.02762 -0.00305 0.00673 0.00010 AFIX 43 H10A 1 0.155881 0.184281 0.291726 11.00000 -1.20000 AFIX 0 C11 2 0.163022 0.307010 0.195064 11.00000 0.02331 0.02405 = 0.03285 0.00139 0.00295 0.00049 C12 2 0.197020 0.385526 0.169126 11.00000 0.02331 0.02405 = 0.03285 0.00139 0.00295 0.00049 AFIX 43 H12A 1 0.184903 0.433319 0.115343 11.00000 -1.20000 AFIX 0 C13 2 0.249002 0.393416 0.222752 11.00000 0.02796 0.03131 = 0.03783 0.00915 0.00918 -0.00410 AFIX 43 H13A 1 0.272729 0.448106 0.207850 11.00000 -1.20000 AFIX 0 C14 2 0.109303 0.296725 0.137369 11.00000 0.02724 0.03404 = 0.03315 0.00135 0.00599 0.00070 C15 2 0.403579 0.163564 0.553120 11.00000 0.04313 0.03757 = 0.05685 0.01557 -0.00103 0.00760 AFIX 13 H15A 1 0.374500 0.126474 0.576886 11.00000 -1.20000 AFIX 0 C16 2 0.436090 0.233440 0.634458 11.00000 0.02985 0.08845 = 0.02626 0.00432 0.00181 -0.00306 AFIX 137 H16A 1 0.416829 0.303197 0.641779 11.00000 -1.50000 H16B 1 0.470186 0.253007 0.620537 11.00000 -1.50000 H16C 1 0.442268 0.189283 0.693635 11.00000 -1.50000 AFIX 0 C17 2 0.435353 0.069854 0.520418 11.00000 0.04313 0.03757 = 0.05685 0.01557 -0.00103 0.00760 AFIX 137 H17A 1 0.412609 0.028534 0.467218 11.00000 -1.50000 H17B 1 0.448637 0.017329 0.573357 11.00000 -1.50000 H17C 1 0.465330 0.103192 0.499563 11.00000 -1.50000 AFIX 0 C18 2 0.314346 -0.117306 0.654905 11.00000 0.04806 0.05848 = 0.06419 0.04239 0.00602 0.00492 AFIX 137 H18A 1 0.351224 -0.107567 0.650685 11.00000 -1.50000 H18B 1 0.304446 -0.197572 0.645763 11.00000 -1.50000 H18C 1 0.310641 -0.092391 0.717812 11.00000 -1.50000 AFIX 0 C19 2 0.278857 -0.047748 0.579349 11.00000 0.03216 0.03562 = 0.04018 0.01290 0.01293 0.00081 C20 2 0.225556 -0.075965 0.551491 11.00000 0.04720 0.02699 = 0.04501 0.01193 0.02397 -0.00004 AFIX 43 H20A 1 0.214304 -0.137892 0.584063 11.00000 -1.20000 AFIX 0 C21 2 0.186462 -0.023731 0.480957 11.00000 0.03198 0.02895 = 0.02896 -0.00320 0.01384 -0.00694 C22 2 0.130613 -0.068868 0.458313 11.00000 0.03831 0.03824 = 0.05089 0.00163 0.01701 -0.01139 AFIX 137 H22A 1 0.105560 -0.005237 0.447552 11.00000 -1.50000 H22B 1 0.125204 -0.114776 0.511878 11.00000 -1.50000 H22C 1 0.124720 -0.115975 0.400769 11.00000 -1.50000 HKLF 4 REM AT 151 REM R1 = 0.0207 for 3478 Fo > 4sig(Fo) and 0.0257 for all 3917 data REM 245 parameters refined using 0 restraints END ; _database_code_depnum_ccdc_archive 'CCDC 972158' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_4 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point 566 _chemical_formula_moiety 'C20 H23 N3 O2 Pt' _chemical_formula_sum 'C20 H23 N3 O2 Pt' _chemical_formula_weight 532.50 _chemical_compound_source 'see text' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 12.4720(19) _cell_length_b 9.6470(9) _cell_length_c 16.8840(18) _cell_angle_alpha 90 _cell_angle_beta 110.760(7) _cell_angle_gamma 90 _cell_volume 1899.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 198 _cell_measurement_reflns_used 957 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.40 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.840 _exptl_crystal_size_mid 0.480 _exptl_crystal_size_min 0.370 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.862 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 7.406 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.062 _exptl_absorpt_correction_T_max 0.168 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Tronnier scanspeed 29 s per frame dx 40 mm ; _diffrn_ambient_temperature 198 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Bruker KappaCCD' _diffrn_measurement_method 'phi- and omega-rotation' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 # number of measured reflections (redundant set) _diffrn_reflns_number 36075 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_unetI/netI 0.0342 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 3814 # number of observed reflections (> n sig(I)) _reflns_number_gt 2967 _reflns_threshold_expression I>2\s(I) _audit_creation_method 'PLATON
option' _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.3376P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 3814 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0456 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.672 _refine_diff_density_min -1.496 _refine_diff_density_rms 0.179 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt Uani 1.00600(1) 0.10523(1) 0.42544(1) 1.000 0.0166(1) d . . . O1 O Uani 0.8989(2) 0.2253(3) 0.46839(17) 1.000 0.0257(9) d . . . O2 O Uani 1.1467(2) 0.1999(3) 0.51049(16) 1.000 0.0247(9) d . . . N1 N Uani 0.9243(3) -0.0654(3) 0.28029(19) 1.000 0.0180(10) d . . . N2 N Uani 0.7722(2) 0.0024(3) 0.30037(18) 1.000 0.0178(10) d . . . N3 N Uani 1.4983(3) -0.0881(4) 0.4084(2) 1.000 0.0411(16) d . . . C1 C Uani 0.8875(3) 0.0108(4) 0.3329(2) 1.000 0.0187(12) d . . . C2 C Uani 0.7362(3) -0.0781(4) 0.2257(2) 1.000 0.0201(12) d . . . C3 C Uani 0.6143(3) -0.0946(4) 0.1646(3) 1.000 0.0254(12) d . . . C4 C Uani 0.6155(4) -0.1877(5) 0.0920(3) 1.000 0.0433(17) d . . . C5 C Uani 0.5330(4) -0.1615(6) 0.2031(3) 1.000 0.0483(19) d . . . C6 C Uani 0.5677(4) 0.0482(5) 0.1282(3) 1.000 0.0348(16) d . . . C7 C Uani 0.8334(3) -0.1220(4) 0.2150(2) 1.000 0.0209(12) d . . . C8 C Uani 1.0451(3) -0.0730(4) 0.3024(2) 1.000 0.0210(12) d . . . C9 C Uani 1.1042(3) 0.0002(4) 0.3761(2) 1.000 0.0183(12) d . . . C10 C Uani 1.2224(3) -0.0059(4) 0.4036(2) 1.000 0.0206(12) d . . . C11 C Uani 1.2773(3) -0.0782(4) 0.3574(2) 1.000 0.0206(12) d . . . C12 C Uani 1.4008(4) -0.0821(4) 0.3864(3) 1.000 0.0273(16) d . . . C13 C Uani 1.2147(4) -0.1466(4) 0.2827(3) 1.000 0.0272(16) d . . . C14 C Uani 1.0968(4) -0.1454(4) 0.2544(3) 1.000 0.0246(12) d . . . C15 C Uani 0.7002(3) 0.0605(5) 0.3439(3) 1.000 0.0301(16) d . . . C16 C Uani 0.8404(4) 0.3792(5) 0.5531(3) 1.000 0.0406(17) d . . . C17 C Uani 0.9322(4) 0.3091(4) 0.5296(2) 1.000 0.0266(14) d . . . C18 C Uani 1.0487(4) 0.3425(5) 0.5778(3) 1.000 0.0316(16) d . . . C19 C Uani 1.1438(3) 0.2904(4) 0.5649(2) 1.000 0.0257(14) d . . . C20 C Uani 1.2604(4) 0.3451(5) 0.6184(3) 1.000 0.0388(17) d . . . H4A H Uiso 0.66450 -0.14640 0.06400 1.000 0.0650 c R . . H4B H Uiso 0.53730 -0.19760 0.05110 1.000 0.0650 c R . . H4C H Uiso 0.64560 -0.27920 0.11440 1.000 0.0650 c R . . H5A H Uiso 0.55670 -0.25750 0.21880 1.000 0.0720 c R . . H5B H Uiso 0.45470 -0.16030 0.16150 1.000 0.0720 c R . . H5C H Uiso 0.53550 -0.10950 0.25360 1.000 0.0720 c R . . H6A H Uiso 0.56180 0.10750 0.17360 1.000 0.0530 c R . . H6B H Uiso 0.49170 0.03720 0.08430 1.000 0.0530 c R . . H6C H Uiso 0.61980 0.09090 0.10340 1.000 0.0530 c R . . H7 H Uiso 0.83810 -0.18050 0.17110 1.000 0.0250 c R . . H10 H Uiso 1.26680 0.03970 0.45460 1.000 0.0250 c R . . H13 H Uiso 1.25340 -0.19410 0.25140 1.000 0.0330 c R . . H14 H Uiso 1.05240 -0.19220 0.20400 1.000 0.0300 c R . . H15A H Uiso 0.66600 -0.01490 0.36580 1.000 0.0450 c R . . H15B H Uiso 0.63930 0.11660 0.30410 1.000 0.0450 c R . . H15C H Uiso 0.74710 0.11880 0.39100 1.000 0.0450 c R . . H16A H Uiso 0.76490 0.35040 0.51380 1.000 0.0610 c R . . H16B H Uiso 0.84810 0.47990 0.54990 1.000 0.0610 c R . . H16C H Uiso 0.84810 0.35300 0.61100 1.000 0.0610 c R . . H18 H Uiso 1.06170 0.40680 0.62280 1.000 0.0380 c R . . H20A H Uiso 1.31980 0.28260 0.61370 1.000 0.0580 c R . . H20B H Uiso 1.26600 0.35040 0.67770 1.000 0.0580 c R . . H20C H Uiso 1.27120 0.43760 0.59840 1.000 0.0580 c 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 0.0182(1) 0.0173(1) 0.0148(1) -0.0007(1) 0.0065(1) 0.0007(1) O1 0.0271(16) 0.0268(17) 0.0250(15) -0.0034(13) 0.0116(13) 0.0045(13) O2 0.0243(15) 0.0277(17) 0.0197(14) -0.0055(13) 0.0049(12) -0.0024(13) N1 0.0171(18) 0.0185(18) 0.0176(17) -0.0002(14) 0.0052(14) 0.0008(13) N2 0.0174(18) 0.0195(18) 0.0174(17) 0.0020(14) 0.0072(14) 0.0008(14) N3 0.027(2) 0.050(3) 0.049(3) -0.006(2) 0.017(2) -0.0059(19) C1 0.023(2) 0.017(2) 0.018(2) 0.0051(17) 0.0098(18) 0.0019(17) C2 0.020(2) 0.020(2) 0.018(2) 0.0044(17) 0.0038(17) -0.0007(17) C3 0.023(2) 0.025(2) 0.025(2) 0.0015(19) 0.0047(18) -0.0021(19) C4 0.035(3) 0.043(3) 0.036(3) -0.011(3) -0.007(2) 0.006(2) C5 0.030(3) 0.069(4) 0.035(3) 0.012(3) -0.002(2) -0.023(3) C6 0.026(2) 0.030(3) 0.039(3) 0.006(2) 0.000(2) 0.006(2) C7 0.023(2) 0.017(2) 0.018(2) 0.0000(17) 0.0016(18) -0.0024(17) C8 0.023(2) 0.021(2) 0.019(2) 0.0022(17) 0.0074(18) 0.0003(17) C9 0.022(2) 0.017(2) 0.017(2) 0.0019(17) 0.0083(17) -0.0014(17) C10 0.023(2) 0.018(2) 0.021(2) -0.0004(17) 0.0081(18) -0.0045(17) C11 0.022(2) 0.018(2) 0.026(2) 0.0011(17) 0.0137(18) -0.0005(17) C12 0.029(3) 0.026(3) 0.032(2) -0.0041(19) 0.017(2) -0.003(2) C13 0.030(3) 0.028(3) 0.031(2) -0.0022(19) 0.020(2) 0.0059(19) C14 0.028(2) 0.025(2) 0.021(2) -0.0080(17) 0.0090(19) -0.0003(18) C15 0.023(2) 0.036(3) 0.033(3) -0.006(2) 0.012(2) -0.001(2) C16 0.053(3) 0.035(3) 0.040(3) -0.002(2) 0.024(3) 0.014(2) C17 0.042(3) 0.017(2) 0.022(2) 0.007(2) 0.013(2) 0.010(2) C18 0.039(3) 0.027(3) 0.026(2) -0.009(2) 0.008(2) -0.002(2) C19 0.035(3) 0.022(2) 0.016(2) 0.0036(18) 0.0039(19) -0.0029(19) C20 0.044(3) 0.033(3) 0.031(3) -0.004(2) 0.003(2) -0.007(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.083(3) . . yes Pt1 O2 2.047(3) . . yes Pt1 C1 1.954(4) . . yes Pt1 C9 1.986(4) . . yes O1 C17 1.261(4) . . yes O2 C19 1.277(4) . . yes N1 C1 1.352(5) . . yes N1 C7 1.383(5) . . yes N1 C8 1.420(5) . . yes N2 C1 1.348(5) . . yes N2 C2 1.412(4) . . yes N2 C15 1.459(5) . . yes N3 C12 1.140(7) . . yes C2 C3 1.513(6) . . no C2 C7 1.355(6) . . no C3 C4 1.524(7) . . no C3 C5 1.528(7) . . no C3 C6 1.536(6) . . no C8 C9 1.393(5) . . no C8 C14 1.390(6) . . no C9 C10 1.381(5) . . no C10 C11 1.394(5) . . no C11 C12 1.442(7) . . no C11 C13 1.392(6) . . no C13 C14 1.376(7) . . no C16 C17 1.499(7) . . no C17 C18 1.428(7) . . no C18 C19 1.375(7) . . no C19 C20 1.509(6) . . no C4 H4A 0.9800 . . no C4 H4B 0.9800 . . no C4 H4C 0.9800 . . no C5 H5A 0.9800 . . no C5 H5B 0.9800 . . no C5 H5C 0.9800 . . no C6 H6A 0.9800 . . no C6 H6B 0.9800 . . no C6 H6C 0.9800 . . no C7 H7 0.9500 . . no C10 H10 0.9500 . . no C13 H13 0.9500 . . no C14 H14 0.9500 . . no C15 H15A 0.9800 . . no C15 H15B 0.9800 . . no C15 H15C 0.9800 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C18 H18 0.9500 . . no C20 H20A 0.9800 . . no C20 H20B 0.9800 . . no C20 H20C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 90.22(11) . . . yes O1 Pt1 C1 98.11(14) . . . yes O1 Pt1 C9 175.36(12) . . . yes O2 Pt1 C1 170.54(13) . . . yes O2 Pt1 C9 91.10(13) . . . yes C1 Pt1 C9 80.26(15) . . . yes Pt1 O1 C17 125.2(3) . . . yes Pt1 O2 C19 125.0(2) . . . yes C1 N1 C7 111.4(3) . . . yes C1 N1 C8 115.5(3) . . . yes C7 N1 C8 133.1(3) . . . yes C1 N2 C2 110.7(3) . . . yes C1 N2 C15 122.0(3) . . . yes C2 N2 C15 127.1(3) . . . yes Pt1 C1 N1 116.2(3) . . . yes Pt1 C1 N2 138.5(3) . . . yes N1 C1 N2 105.1(3) . . . yes N2 C2 C3 126.3(3) . . . yes N2 C2 C7 105.9(3) . . . yes C3 C2 C7 127.3(3) . . . no C2 C3 C4 108.5(3) . . . no C2 C3 C5 114.4(4) . . . no C2 C3 C6 109.0(3) . . . no C4 C3 C5 106.9(4) . . . no C4 C3 C6 108.5(4) . . . no C5 C3 C6 109.6(4) . . . no N1 C7 C2 106.8(3) . . . yes N1 C8 C9 112.6(3) . . . yes N1 C8 C14 122.8(3) . . . yes C9 C8 C14 124.6(4) . . . no Pt1 C9 C8 115.1(3) . . . yes Pt1 C9 C10 128.6(3) . . . yes C8 C9 C10 116.3(3) . . . no C9 C10 C11 120.7(3) . . . no C10 C11 C12 120.0(3) . . . no C10 C11 C13 121.0(4) . . . no C12 C11 C13 118.9(4) . . . no N3 C12 C11 178.4(5) . . . yes C11 C13 C14 119.9(4) . . . no C8 C14 C13 117.5(4) . . . no O1 C17 C16 116.5(4) . . . yes O1 C17 C18 125.8(4) . . . yes C16 C17 C18 117.8(4) . . . no C17 C18 C19 126.0(4) . . . no O2 C19 C18 127.6(4) . . . yes O2 C19 C20 113.7(4) . . . yes C18 C19 C20 118.7(4) . . . no C3 C4 H4A 110.00 . . . no C3 C4 H4B 109.00 . . . no C3 C4 H4C 109.00 . . . no H4A C4 H4B 110.00 . . . no H4A C4 H4C 109.00 . . . no H4B C4 H4C 109.00 . . . no C3 C5 H5A 109.00 . . . no C3 C5 H5B 109.00 . . . no C3 C5 H5C 109.00 . . . no H5A C5 H5B 109.00 . . . no H5A C5 H5C 110.00 . . . no H5B C5 H5C 109.00 . . . no C3 C6 H6A 109.00 . . . no C3 C6 H6B 109.00 . . . no C3 C6 H6C 109.00 . . . no H6A C6 H6B 110.00 . . . no H6A C6 H6C 110.00 . . . no H6B C6 H6C 109.00 . . . no N1 C7 H7 127.00 . . . no C2 C7 H7 127.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C11 C13 H13 120.00 . . . no C14 C13 H13 120.00 . . . no C8 C14 H14 121.00 . . . no C13 C14 H14 121.00 . . . no N2 C15 H15A 109.00 . . . no N2 C15 H15B 109.00 . . . no N2 C15 H15C 109.00 . . . no H15A C15 H15B 109.00 . . . no H15A C15 H15C 110.00 . . . no H15B C15 H15C 110.00 . . . no C17 C16 H16A 109.00 . . . no C17 C16 H16B 109.00 . . . no C17 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 109.00 . . . no C17 C18 H18 117.00 . . . no C19 C18 H18 117.00 . . . no C19 C20 H20A 109.00 . . . no C19 C20 H20B 110.00 . . . no C19 C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no H20A C20 H20C 109.00 . . . no H20B C20 H20C 110.00 . . . no 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 O2 Pt1 O1 C17 -4.5(3) . . . . no C1 Pt1 O1 C17 -180.0(3) . . . . no O1 Pt1 O2 C19 2.9(3) . . . . no C9 Pt1 O2 C19 178.4(3) . . . . no O1 Pt1 C1 N1 171.1(3) . . . . no C9 Pt1 C1 N1 -4.5(3) . . . . no O1 Pt1 C1 N2 -4.5(4) . . . . no C9 Pt1 C1 N2 179.9(4) . . . . no O2 Pt1 C9 C10 6.3(3) . . . . no O2 Pt1 C9 C8 -171.4(3) . . . . no C1 Pt1 C9 C8 4.7(3) . . . . no C1 Pt1 C9 C10 -177.6(4) . . . . no Pt1 O1 C17 C18 3.4(6) . . . . no Pt1 O1 C17 C16 -176.6(3) . . . . no Pt1 O2 C19 C20 -178.8(3) . . . . no Pt1 O2 C19 C18 -0.1(6) . . . . no C1 N1 C8 C9 0.5(5) . . . . no C7 N1 C1 Pt1 -177.1(2) . . . . no C7 N1 C8 C14 1.7(6) . . . . no C7 N1 C8 C9 -178.7(4) . . . . no C1 N1 C8 C14 -179.1(4) . . . . no C8 N1 C7 C2 -179.6(4) . . . . no C8 N1 C1 Pt1 3.5(4) . . . . no C1 N1 C7 C2 1.2(4) . . . . no C8 N1 C1 N2 -179.5(3) . . . . no C7 N1 C1 N2 -0.1(4) . . . . no C15 N2 C1 N1 174.0(3) . . . . no C15 N2 C2 C7 -172.9(4) . . . . no C1 N2 C2 C3 -170.8(4) . . . . no C2 N2 C1 Pt1 174.9(3) . . . . no C1 N2 C2 C7 1.7(4) . . . . no C2 N2 C1 N1 -1.0(4) . . . . no C15 N2 C2 C3 14.6(6) . . . . no C15 N2 C1 Pt1 -10.1(6) . . . . no C7 C2 C3 C4 7.7(6) . . . . no C7 C2 C3 C5 126.9(5) . . . . no N2 C2 C3 C6 60.8(5) . . . . no N2 C2 C3 C5 -62.2(5) . . . . no C3 C2 C7 N1 170.7(4) . . . . no C7 C2 C3 C6 -110.2(5) . . . . no N2 C2 C7 N1 -1.7(4) . . . . no N2 C2 C3 C4 178.6(4) . . . . no C9 C8 C14 C13 1.2(6) . . . . no N1 C8 C9 C10 177.9(3) . . . . no N1 C8 C14 C13 -179.3(4) . . . . no C14 C8 C9 C10 -2.6(6) . . . . no N1 C8 C9 Pt1 -4.2(4) . . . . no C14 C8 C9 Pt1 175.4(3) . . . . no C8 C9 C10 C11 2.1(5) . . . . no Pt1 C9 C10 C11 -175.6(3) . . . . no C9 C10 C11 C13 -0.3(6) . . . . no C9 C10 C11 C12 179.2(4) . . . . no C10 C11 C13 C14 -1.2(6) . . . . no C12 C11 C13 C14 179.3(4) . . . . no C11 C13 C14 C8 0.7(6) . . . . no O1 C17 C18 C19 0.9(7) . . . . no C16 C17 C18 C19 -179.1(4) . . . . no C17 C18 C19 C20 175.8(4) . . . . no C17 C18 C19 O2 -2.8(7) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C10 H10 O2 0.9500 2.5500 3.049(5) 113.00 . yes C15 H15A N3 0.9800 2.5400 3.395(6) 146.00 1_455 yes C15 H15C O1 0.9800 2.1400 3.065(5) 156.00 . yes # Loop Mechanism for Extra Tables(s) _iucr_refine_instructions_details ; TITL AT157A CELL 0.71073 12.4720 9.6470 16.8840 90.0000 110.7600 90.0000 ZERR 4 0.0019 0.0009 0.0018 0.00 0.0074 0.00 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O Pt UNIT 80 92 12 8 4 L.S. 18 ACTA BOND $H FMAP -2 PLAN 10 LIST 4 SIZE 0.374 0.484 0.842 WGHT 0.023300 1.338000 FVAR 0.247540 TEMP -75 C1 1 0.887527 0.010806 0.332892 11.000000 0.022910 0.016990 = 0.018200 0.005060 0.009790 0.001850 C2 1 0.736249 -0.078057 0.225744 11.000000 0.020350 0.019840 = 0.017690 0.004350 0.003800 -0.000740 C3 1 0.614302 -0.094572 0.164591 11.000000 0.022520 0.024700 = 0.025350 0.001460 0.004660 -0.002070 C4 1 0.615533 -0.187735 0.092044 11.000000 0.034740 0.042860 = 0.036210 -0.011410 -0.007020 0.005810 AFIX 137 H4A 2 0.664470 -0.146360 0.064021 11.000000 -1.500000 H4B 2 0.537328 -0.197596 0.051092 11.000000 -1.500000 H4C 2 0.645593 -0.279169 0.114358 11.000000 -1.500000 AFIX 0 C5 1 0.533002 -0.161451 0.203065 11.000000 0.030400 0.068760 = 0.034520 0.011960 -0.001530 -0.023100 AFIX 137 H5A 2 0.556672 -0.257473 0.218835 11.000000 -1.500000 H5B 2 0.454719 -0.160268 0.161479 11.000000 -1.500000 H5C 2 0.535456 -0.109519 0.253564 11.000000 -1.500000 AFIX 0 C6 1 0.567692 0.048175 0.128198 11.000000 0.026310 0.030500 = 0.039400 0.006060 -0.000210 0.006200 AFIX 137 H6A 2 0.561818 0.107502 0.173602 11.000000 -1.500000 H6B 2 0.491683 0.037237 0.084348 11.000000 -1.500000 H6C 2 0.619833 0.090874 0.103422 11.000000 -1.500000 AFIX 0 C7 1 0.833361 -0.122041 0.214977 11.000000 0.023250 0.017290 = 0.018030 0.000000 0.001620 -0.002450 AFIX 43 H7 2 0.838090 -0.180497 0.171052 11.000000 -1.200000 AFIX 0 C8 1 1.045063 -0.073049 0.302406 11.000000 0.023090 0.020760 = 0.018890 0.002240 0.007450 0.000320 C9 1 1.104187 0.000218 0.376080 11.000000 0.021750 0.016510 = 0.016990 0.001900 0.008270 -0.001400 C10 1 1.222415 -0.005890 0.403621 11.000000 0.022960 0.017970 = 0.020780 -0.000440 0.008110 -0.004460 AFIX 43 H10 2 1.266797 0.039658 0.454597 11.000000 -1.200000 AFIX 0 C11 1 1.277277 -0.078226 0.357367 11.000000 0.022180 0.018110 = 0.025980 0.001100 0.013720 -0.000520 C12 1 1.400759 -0.082053 0.386399 11.000000 0.029400 0.025910 = 0.031660 -0.004140 0.017480 -0.003270 C13 1 1.214747 -0.146646 0.282715 11.000000 0.029920 0.027870 = 0.031150 -0.002200 0.019630 0.005880 AFIX 43 H13 2 1.253353 -0.194108 0.251358 11.000000 -1.200000 AFIX 0 C14 1 1.096824 -0.145368 0.254434 11.000000 0.028190 0.025110 = 0.020760 -0.008040 0.009050 -0.000300 AFIX 43 H14 2 1.052434 -0.192215 0.203961 11.000000 -1.200000 AFIX 0 C15 1 0.700232 0.060493 0.343908 11.000000 0.023030 0.036480 = 0.033150 -0.006380 0.012410 -0.001070 AFIX 137 H15A 2 0.666009 -0.014906 0.365838 11.000000 -1.500000 H15B 2 0.639288 0.116647 0.304128 11.000000 -1.500000 H15C 2 0.747058 0.118778 0.391008 11.000000 -1.500000 AFIX 0 C16 1 0.840376 0.379166 0.553104 11.000000 0.053140 0.035290 = 0.040420 -0.002000 0.024460 0.014430 AFIX 137 H16A 2 0.764927 0.350372 0.513794 11.000000 -1.500000 H16B 2 0.848104 0.479908 0.549904 11.000000 -1.500000 H16C 2 0.848067 0.353027 0.610954 11.000000 -1.500000 AFIX 0 C17 1 0.932189 0.309105 0.529642 11.000000 0.042130 0.016720 = 0.022470 0.006900 0.012750 0.009720 C18 1 1.048717 0.342520 0.577760 11.000000 0.038580 0.026920 = 0.026350 -0.009130 0.008380 -0.001990 AFIX 43 H18 2 1.061721 0.406792 0.622838 11.000000 -1.200000 AFIX 0 C19 1 1.143758 0.290383 0.564936 11.000000 0.034860 0.021890 = 0.016330 0.003600 0.003890 -0.002880 C20 1 1.260417 0.345051 0.618365 11.000000 0.044150 0.032620 = 0.031300 -0.004160 0.003290 -0.007160 AFIX 137 H20A 2 1.319848 0.282583 0.613681 11.000000 -1.500000 H20B 2 1.265985 0.350448 0.677656 11.000000 -1.500000 H20C 2 1.271158 0.437617 0.598446 11.000000 -1.500000 AFIX 0 N1 3 0.924305 -0.065401 0.280290 11.000000 0.017060 0.018500 = 0.017630 -0.000150 0.005220 0.000790 N2 3 0.772190 0.002383 0.300367 11.000000 0.017410 0.019480 = 0.017420 0.002000 0.007160 0.000770 N3 3 1.498349 -0.088129 0.408410 11.000000 0.026710 0.050040 = 0.049480 -0.005640 0.017190 -0.005940 O1 4 0.898921 0.225302 0.468392 11.000000 0.027070 0.026750 = 0.024990 -0.003450 0.011600 0.004460 O2 4 1.146695 0.199928 0.510489 11.000000 0.024300 0.027700 = 0.019750 -0.005480 0.004910 -0.002410 Pt1 5 1.006001 0.105230 0.425441 11.000000 0.018230 0.017290 = 0.014750 -0.000680 0.006480 0.000650 HKLF 4 END ; _database_code_depnum_ccdc_archive 'CCDC 972159' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_5 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C38 H37 N3 O2 Pt' _chemical_formula_sum 'C38 H37 N3 O2 Pt' _chemical_formula_weight 762.80 _chemical_compound_source 'see text' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,-y,1/2+z 3 1/2+x,1/2-y,-z 4 -x,1/2+y,1/2-z _cell_length_a 10.251(2) _cell_length_b 13.9000(6) _cell_length_c 22.872(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3259.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 198 _cell_measurement_reflns_used 989 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.40 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.310 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.343 _exptl_crystal_density_meas_temp ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2.10.(Sheldrick,Bruker AXS Inc.,2002)' _exptl_absorpt_correction_T_min 0.318 _exptl_absorpt_correction_T_max 0.359 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Tronnier scanspeed 30 s per frame dx 35 mm ; _diffrn_ambient_temperature 198 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Bruker KappaCCD' _diffrn_measurement_method 'phi- and omega-rotation' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 # number of measured reflections (redundant set) _diffrn_reflns_number 70606 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_unetI/netI 0.0462 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.40 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 6671 # number of observed reflections (> n sig(I)) _reflns_number_gt 5633 _reflns_threshold_expression I>2\s(I) _audit_creation_method 'PLATON
option' _computing_data_collection 'Collect (Nonius BV, 1999)' _computing_cell_refinement 'Dirax/lsq (Duisenberg, 1992)' _computing_data_reduction 'EvalCCD (Duisenberg et al., 2003)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011), ORTEP (Farrugia, L. J. 1997), MERCURY (van de Streek, J. 2006)' _computing_publication_material 'PLATON (Spek, 2011)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.2947P] 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_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.018(9) _refine_ls_number_reflns 6671 _refine_ls_number_parameters 405 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.042 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.205 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt Uani 0.46996(3) 0.10956(2) 0.90071(1) 1.000 0.0252(1) d . . . O1 O Uani 0.6124(5) 0.0091(3) 0.8787(2) 1.000 0.0323(17) d . . . O2 O Uani 0.5647(4) 0.2090(3) 0.8515(2) 1.000 0.0290(17) d . . . N1 N Uani 0.2745(6) 0.0850(4) 0.9869(3) 1.000 0.0290(19) d . . . N2 N Uani 0.3727(6) -0.0537(4) 0.9787(2) 1.000 0.0287(17) d . . . N3 N Uani 0.2604(9) 0.5448(5) 0.8942(4) 1.000 0.063(3) d . . . C1 C Uani 0.3683(7) 0.0344(5) 0.9569(3) 1.000 0.028(3) d . . . C2 C Uani 0.2895(8) -0.0609(6) 1.0273(3) 1.000 0.033(2) d . . . C3 C Uani 0.2692(8) -0.1328(6) 1.0690(3) 1.000 0.039(3) d . . . C4 C Uani 0.1820(9) -0.1151(7) 1.1146(3) 1.000 0.049(3) d . . . C5 C Uani 0.1165(9) -0.0258(7) 1.1174(4) 1.000 0.048(3) d . . . C6 C Uani 0.1369(8) 0.0455(6) 1.0776(3) 1.000 0.036(3) d . . . C7 C Uani 0.2256(7) 0.0292(5) 1.0329(3) 1.000 0.032(2) d . . . C8 C Uani 0.2574(7) 0.1838(5) 0.9703(3) 1.000 0.029(2) d . . . C9 C Uani 0.3424(7) 0.2100(5) 0.9261(3) 1.000 0.026(2) d . . . C10 C Uani 0.3377(7) 0.3030(5) 0.9064(3) 1.000 0.028(2) d . . . C11 C Uani 0.2505(7) 0.3686(5) 0.9307(3) 1.000 0.032(3) d . . . C12 C Uani 0.2529(8) 0.4658(7) 0.9103(4) 1.000 0.045(3) d . . . C13 C Uani 0.1661(8) 0.3395(6) 0.9728(3) 1.000 0.043(3) d . . . C14 C Uani 0.1680(8) 0.2456(6) 0.9935(4) 1.000 0.042(3) d . . . C15 C Uani 0.4536(8) -0.1328(4) 0.9553(3) 1.000 0.032(2) d . . . C16 C Uani 0.3722(9) -0.2235(6) 0.9417(4) 1.000 0.047(3) d . . . C17 C Uani 0.5704(8) -0.1530(7) 0.9946(4) 1.000 0.053(3) d . . . C18 C Uani 1.0582(9) -0.3014(5) 0.8267(4) 1.000 0.052(3) d . . . C19 C Uani 0.9722(9) -0.2144(5) 0.8321(3) 1.000 0.036(2) d . . . C20 C Uani 0.8846(8) -0.1909(5) 0.7886(4) 1.000 0.039(3) d . . . C21 C Uani 0.8041(7) -0.1115(6) 0.7927(3) 1.000 0.037(3) d . . . C22 C Uani 0.7153(11) -0.0837(7) 0.7419(4) 1.000 0.062(4) d . . . C23 C Uani 0.8073(7) -0.0561(5) 0.8434(3) 1.000 0.028(2) d . . . C24 C Uani 0.8971(7) -0.0773(5) 0.8879(3) 1.000 0.032(2) d . . . C25 C Uani 0.9065(10) -0.0161(6) 0.9424(4) 1.000 0.053(3) d . . . C26 C Uani 0.9753(8) -0.1560(5) 0.8809(3) 1.000 0.036(2) d . . . C27 C Uani 0.7164(7) 0.0276(5) 0.8503(3) 1.000 0.028(3) d . . . C28 C Uani 0.7506(7) 0.1157(6) 0.8251(3) 1.000 0.035(2) d . . . C29 C Uani 0.6757(7) 0.1992(5) 0.8251(3) 1.000 0.028(2) d . . . C30 C Uani 0.7220(7) 0.2870(5) 0.7928(3) 1.000 0.030(2) d . . . C31 C Uani 0.8282(8) 0.3391(6) 0.8134(3) 1.000 0.034(3) d . . . C32 C Uani 0.9085(10) 0.3108(6) 0.8656(4) 1.000 0.054(3) d . . . C33 C Uani 0.8600(9) 0.4235(5) 0.7832(4) 1.000 0.040(3) d . . . C34 C Uani 0.7921(9) 0.4543(6) 0.7345(3) 1.000 0.039(3) d . . . C35 C Uani 0.8315(10) 0.5467(6) 0.7029(4) 1.000 0.063(4) d . . . C36 C Uani 0.6894(7) 0.3991(6) 0.7149(3) 1.000 0.038(3) d . . . C37 C Uani 0.6515(8) 0.3142(5) 0.7425(3) 1.000 0.036(3) d . . . C38 C Uani 0.5461(9) 0.2541(6) 0.7181(3) 1.000 0.049(3) d . . . H3 H Uiso 0.31400 -0.19250 1.06640 1.000 0.0470 c R . . H4 H Uiso 0.16660 -0.16280 1.14350 1.000 0.0590 c R . . H5 H Uiso 0.05610 -0.01510 1.14820 1.000 0.0580 c R . . H6 H Uiso 0.09160 0.10490 1.08040 1.000 0.0440 c R . . H10 H Uiso 0.39440 0.32290 0.87580 1.000 0.0340 c R . . H13 H Uiso 0.10480 0.38390 0.98840 1.000 0.0520 c R . . H14 H Uiso 0.10880 0.22510 1.02290 1.000 0.0500 c R . . H15 H Uiso 0.48950 -0.10980 0.91720 1.000 0.0390 c R . . H16A H Uiso 0.34280 -0.25280 0.97840 1.000 0.0700 c R . . H16B H Uiso 0.42590 -0.26970 0.92010 1.000 0.0700 c R . . H16C H Uiso 0.29630 -0.20560 0.91810 1.000 0.0700 c R . . H17A H Uiso 0.62770 -0.09660 0.99520 1.000 0.0800 c R . . H17B H Uiso 0.61860 -0.20860 0.97950 1.000 0.0800 c R . . H17C H Uiso 0.54000 -0.16680 1.03430 1.000 0.0800 c R . . H18A H Uiso 1.01130 -0.35820 0.84100 1.000 0.0780 c R . . H18B H Uiso 1.13740 -0.29190 0.85000 1.000 0.0780 c R . . H18C H Uiso 1.08180 -0.31100 0.78560 1.000 0.0780 c R . . H20 H Uiso 0.87940 -0.23060 0.75490 1.000 0.0470 c R . . H22A H Uiso 0.62590 -0.07520 0.75620 1.000 0.0930 c R . . H22B H Uiso 0.71680 -0.13460 0.71230 1.000 0.0930 c R . . H22C H Uiso 0.74600 -0.02330 0.72450 1.000 0.0930 c R . . H25A H Uiso 0.81920 -0.00660 0.95880 1.000 0.0800 c R . . H25B H Uiso 0.94450 0.04650 0.93240 1.000 0.0800 c R . . H25C H Uiso 0.96200 -0.04840 0.97120 1.000 0.0800 c R . . H26 H Uiso 1.03510 -0.17140 0.91130 1.000 0.0430 c R . . H28 H Uiso 0.83290 0.11880 0.80610 1.000 0.0420 c R . . H32A H Uiso 0.85320 0.27720 0.89390 1.000 0.0810 c R . . H32B H Uiso 0.94540 0.36860 0.88370 1.000 0.0810 c R . . H32C H Uiso 0.97940 0.26820 0.85310 1.000 0.0810 c R . . H33 H Uiso 0.93120 0.46110 0.79670 1.000 0.0480 c R . . H35A H Uiso 0.92600 0.54670 0.69640 1.000 0.0950 c R . . H35B H Uiso 0.80740 0.60240 0.72680 1.000 0.0950 c R . . H35C H Uiso 0.78630 0.55020 0.66520 1.000 0.0950 c R . . H36 H Uiso 0.64280 0.41960 0.68120 1.000 0.0460 c R . . H38A H Uiso 0.48020 0.24220 0.74830 1.000 0.0740 c R . . H38B H Uiso 0.58230 0.19270 0.70480 1.000 0.0740 c R . . H38C H Uiso 0.50560 0.28760 0.68510 1.000 0.0740 c 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 0.0243(1) 0.0270(1) 0.0243(1) -0.0019(1) 0.0013(1) 0.0036(1) O1 0.032(3) 0.032(3) 0.033(3) 0.000(2) 0.006(2) 0.003(2) O2 0.027(3) 0.028(3) 0.032(3) 0.004(2) 0.009(2) 0.005(2) N1 0.026(3) 0.031(4) 0.030(3) -0.003(2) 0.004(3) 0.002(3) N2 0.028(3) 0.029(3) 0.029(3) -0.003(3) 0.003(3) 0.001(3) N3 0.090(6) 0.035(4) 0.063(5) 0.005(4) 0.001(5) 0.025(4) C1 0.020(4) 0.043(5) 0.020(4) -0.005(3) -0.003(3) 0.001(3) C2 0.030(4) 0.036(4) 0.034(4) 0.002(3) -0.003(4) -0.007(4) C3 0.042(5) 0.038(5) 0.036(4) 0.002(3) 0.001(4) -0.009(4) C4 0.057(6) 0.054(5) 0.036(4) -0.003(4) 0.011(4) -0.023(5) C5 0.037(5) 0.065(6) 0.043(5) -0.005(4) 0.016(4) -0.003(5) C6 0.035(5) 0.044(5) 0.030(4) 0.001(3) 0.004(3) 0.000(4) C7 0.027(4) 0.039(4) 0.031(4) -0.005(3) 0.002(3) -0.004(3) C8 0.035(4) 0.029(4) 0.023(4) -0.007(3) -0.003(3) 0.005(3) C9 0.028(4) 0.026(4) 0.025(4) -0.012(3) -0.007(3) 0.010(3) C10 0.028(4) 0.035(4) 0.022(4) -0.008(3) -0.007(3) 0.007(3) C11 0.037(5) 0.035(5) 0.023(4) -0.001(3) -0.005(3) 0.010(3) C12 0.044(5) 0.053(6) 0.037(5) -0.009(4) -0.006(4) 0.019(4) C13 0.034(5) 0.053(5) 0.042(5) -0.015(4) 0.000(4) 0.018(4) C14 0.039(5) 0.050(5) 0.036(4) -0.005(4) 0.009(4) 0.005(4) C15 0.034(4) 0.027(4) 0.036(4) 0.002(3) 0.005(3) -0.002(3) C16 0.050(6) 0.035(5) 0.056(5) -0.010(4) 0.016(5) -0.009(4) C17 0.047(6) 0.059(5) 0.053(5) 0.000(4) -0.004(4) 0.014(4) C18 0.062(7) 0.031(5) 0.063(5) 0.006(4) 0.020(5) 0.015(4) C19 0.037(4) 0.033(4) 0.039(4) 0.010(3) 0.011(4) 0.003(4) C20 0.048(5) 0.028(4) 0.042(5) -0.004(3) 0.016(4) 0.005(4) C21 0.040(5) 0.040(4) 0.031(4) -0.005(4) -0.001(3) -0.005(4) C22 0.079(8) 0.066(7) 0.041(5) -0.011(4) -0.018(5) 0.023(5) C23 0.032(4) 0.022(4) 0.031(4) 0.006(3) 0.010(3) 0.005(3) C24 0.029(4) 0.037(4) 0.029(4) 0.003(3) 0.002(3) -0.002(3) C25 0.063(6) 0.052(5) 0.044(5) -0.015(4) -0.013(5) 0.017(5) C26 0.030(4) 0.035(4) 0.042(4) 0.009(3) 0.002(4) 0.006(4) C27 0.029(5) 0.032(4) 0.024(4) 0.000(3) -0.001(3) 0.002(3) C28 0.030(4) 0.036(4) 0.038(4) 0.007(4) 0.009(3) 0.009(4) C29 0.032(4) 0.029(4) 0.023(4) 0.002(3) 0.001(3) 0.004(3) C30 0.030(4) 0.028(4) 0.031(4) -0.002(3) 0.006(4) 0.009(3) C31 0.041(5) 0.033(4) 0.028(4) -0.003(3) 0.003(3) 0.002(4) C32 0.055(6) 0.058(6) 0.049(5) 0.002(4) -0.009(5) -0.007(5) C33 0.038(5) 0.039(5) 0.044(5) -0.008(4) 0.001(4) -0.003(4) C34 0.051(6) 0.035(5) 0.032(4) 0.001(3) 0.005(4) 0.007(4) C35 0.070(7) 0.046(6) 0.074(7) 0.013(5) -0.005(6) -0.013(5) C36 0.036(5) 0.041(5) 0.038(4) 0.002(4) -0.006(3) 0.001(4) C37 0.038(5) 0.036(4) 0.034(4) 0.000(3) -0.002(4) -0.001(4) C38 0.053(6) 0.049(5) 0.046(5) 0.008(4) -0.021(5) -0.011(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 O1 2.082(5) . . yes Pt1 O2 2.030(4) . . yes Pt1 C1 1.957(7) . . yes Pt1 C9 1.999(7) . . yes O1 C27 1.275(9) . . yes O2 C29 1.295(8) . . yes N1 C1 1.375(9) . . yes N1 C7 1.400(9) . . yes N1 C8 1.436(9) . . yes N2 C1 1.323(9) . . yes N2 C2 1.405(9) . . yes N2 C15 1.478(9) . . yes N3 C12 1.161(12) . . yes C2 C3 1.397(11) . . no C2 C7 1.419(11) . . no C3 C4 1.396(11) . . no C4 C5 1.413(14) . . no C5 C6 1.362(12) . . no C6 C7 1.387(10) . . no C8 C9 1.383(10) . . no C8 C14 1.364(11) . . no C9 C10 1.370(10) . . no C10 C11 1.393(10) . . no C11 C12 1.430(12) . . no C11 C13 1.356(10) . . no C13 C14 1.389(12) . . no C15 C16 1.544(11) . . no C15 C17 1.523(12) . . no C18 C19 1.502(11) . . no C19 C20 1.380(12) . . no C19 C26 1.381(10) . . no C20 C21 1.381(11) . . no C21 C22 1.526(12) . . no C21 C23 1.392(10) . . no C23 C24 1.404(10) . . no C23 C27 1.499(10) . . no C24 C25 1.512(11) . . no C24 C26 1.366(10) . . no C27 C28 1.398(11) . . no C28 C29 1.392(11) . . no C29 C30 1.504(10) . . no C30 C31 1.390(11) . . no C30 C37 1.410(10) . . no C31 C32 1.503(12) . . no C31 C33 1.400(11) . . no C33 C34 1.382(12) . . no C34 C35 1.528(12) . . no C34 C36 1.378(12) . . no C36 C37 1.394(11) . . no C37 C38 1.475(12) . . no C3 H3 0.9500 . . no C4 H4 0.9500 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C10 H10 0.9500 . . no C13 H13 0.9500 . . no C14 H14 0.9500 . . no C15 H15 1.0000 . . no C16 H16A 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C17 H17A 0.9800 . . no C17 H17B 0.9800 . . no C17 H17C 0.9800 . . no C18 H18A 0.9800 . . no C18 H18B 0.9800 . . no C18 H18C 0.9800 . . no C20 H20 0.9500 . . no C22 H22A 0.9800 . . no C22 H22B 0.9800 . . no C22 H22C 0.9800 . . no C25 H25A 0.9800 . . no C25 H25B 0.9800 . . no C25 H25C 0.9800 . . no C26 H26 0.9500 . . no C28 H28 0.9500 . . no C32 H32A 0.9800 . . no C32 H32B 0.9800 . . no C32 H32C 0.9800 . . no C33 H33 0.9500 . . no C35 H35A 0.9800 . . no C35 H35B 0.9800 . . no C35 H35C 0.9800 . . no C36 H36 0.9500 . . no C38 H38A 0.9800 . . no C38 H38B 0.9800 . . no C38 H38C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pt1 O2 89.26(17) . . . yes O1 Pt1 C1 100.0(2) . . . yes O1 Pt1 C9 175.8(2) . . . yes O2 Pt1 C1 169.3(2) . . . yes O2 Pt1 C9 89.9(2) . . . yes C1 Pt1 C9 80.4(3) . . . yes Pt1 O1 C27 125.1(4) . . . yes Pt1 O2 C29 127.4(4) . . . yes C1 N1 C7 110.0(6) . . . yes C1 N1 C8 116.3(6) . . . yes C7 N1 C8 133.2(6) . . . yes C1 N2 C2 110.1(6) . . . yes C1 N2 C15 124.9(5) . . . yes C2 N2 C15 125.1(6) . . . yes Pt1 C1 N1 115.3(5) . . . yes Pt1 C1 N2 136.4(5) . . . yes N1 C1 N2 108.0(6) . . . yes N2 C2 C3 133.0(7) . . . yes N2 C2 C7 106.8(6) . . . yes C3 C2 C7 120.1(7) . . . no C2 C3 C4 118.7(8) . . . no C3 C4 C5 119.6(8) . . . no C4 C5 C6 122.4(8) . . . no C5 C6 C7 118.3(8) . . . no N1 C7 C2 104.8(6) . . . yes N1 C7 C6 134.3(7) . . . yes C2 C7 C6 120.9(7) . . . no N1 C8 C9 111.6(6) . . . yes N1 C8 C14 125.6(7) . . . yes C9 C8 C14 122.8(7) . . . no Pt1 C9 C8 116.1(5) . . . yes Pt1 C9 C10 125.9(5) . . . yes C8 C9 C10 117.8(6) . . . no C9 C10 C11 120.6(6) . . . no C10 C11 C12 118.5(7) . . . no C10 C11 C13 119.8(7) . . . no C12 C11 C13 121.6(7) . . . no N3 C12 C11 177.1(9) . . . yes C11 C13 C14 120.9(7) . . . no C8 C14 C13 118.0(8) . . . no N2 C15 C16 112.2(7) . . . yes N2 C15 C17 111.4(6) . . . yes C16 C15 C17 113.2(6) . . . no C18 C19 C20 120.9(7) . . . no C18 C19 C26 121.8(7) . . . no C20 C19 C26 117.3(7) . . . no C19 C20 C21 122.0(7) . . . no C20 C21 C22 120.5(7) . . . no C20 C21 C23 119.0(7) . . . no C22 C21 C23 120.5(7) . . . no C21 C23 C24 120.2(7) . . . no C21 C23 C27 120.2(6) . . . no C24 C23 C27 119.6(6) . . . no C23 C24 C25 121.4(7) . . . no C23 C24 C26 117.9(6) . . . no C25 C24 C26 120.7(7) . . . no C19 C26 C24 123.5(7) . . . no O1 C27 C23 114.7(6) . . . yes O1 C27 C28 126.6(6) . . . yes C23 C27 C28 118.7(6) . . . no C27 C28 C29 126.3(7) . . . no O2 C29 C28 124.9(6) . . . yes O2 C29 C30 114.9(6) . . . yes C28 C29 C30 120.2(6) . . . no C29 C30 C31 120.2(6) . . . no C29 C30 C37 117.2(6) . . . no C31 C30 C37 122.6(7) . . . no C30 C31 C32 124.2(7) . . . no C30 C31 C33 116.9(7) . . . no C32 C31 C33 118.9(8) . . . no C31 C33 C34 122.7(8) . . . no C33 C34 C35 120.6(8) . . . no C33 C34 C36 118.4(7) . . . no C35 C34 C36 121.1(7) . . . no C34 C36 C37 122.5(7) . . . no C30 C37 C36 117.0(7) . . . no C30 C37 C38 122.2(6) . . . no C36 C37 C38 120.8(6) . . . no C2 C3 H3 121.00 . . . no C4 C3 H3 121.00 . . . no C3 C4 H4 120.00 . . . no C5 C4 H4 120.00 . . . no C4 C5 H5 119.00 . . . no C6 C5 H5 119.00 . . . no C5 C6 H6 121.00 . . . no C7 C6 H6 121.00 . . . no C9 C10 H10 120.00 . . . no C11 C10 H10 120.00 . . . no C11 C13 H13 120.00 . . . no C14 C13 H13 119.00 . . . no C8 C14 H14 121.00 . . . no C13 C14 H14 121.00 . . . no N2 C15 H15 107.00 . . . no C16 C15 H15 107.00 . . . no C17 C15 H15 107.00 . . . no C15 C16 H16A 109.00 . . . no C15 C16 H16B 109.00 . . . no C15 C16 H16C 109.00 . . . no H16A C16 H16B 109.00 . . . no H16A C16 H16C 109.00 . . . no H16B C16 H16C 110.00 . . . no C15 C17 H17A 109.00 . . . no C15 C17 H17B 109.00 . . . no C15 C17 H17C 109.00 . . . no H17A C17 H17B 109.00 . . . no H17A C17 H17C 110.00 . . . no H17B C17 H17C 109.00 . . . no C19 C18 H18A 109.00 . . . no C19 C18 H18B 109.00 . . . no C19 C18 H18C 109.00 . . . no H18A C18 H18B 109.00 . . . no H18A C18 H18C 109.00 . . . no H18B C18 H18C 110.00 . . . no C19 C20 H20 119.00 . . . no C21 C20 H20 119.00 . . . no C21 C22 H22A 110.00 . . . no C21 C22 H22B 110.00 . . . no C21 C22 H22C 110.00 . . . no H22A C22 H22B 109.00 . . . no H22A C22 H22C 109.00 . . . no H22B C22 H22C 109.00 . . . no C24 C25 H25A 109.00 . . . no C24 C25 H25B 109.00 . . . no C24 C25 H25C 109.00 . . . no H25A C25 H25B 109.00 . . . no H25A C25 H25C 110.00 . . . no H25B C25 H25C 109.00 . . . no C19 C26 H26 118.00 . . . no C24 C26 H26 118.00 . . . no C27 C28 H28 117.00 . . . no C29 C28 H28 117.00 . . . no C31 C32 H32A 109.00 . . . no C31 C32 H32B 109.00 . . . no C31 C32 H32C 109.00 . . . no H32A C32 H32B 110.00 . . . no H32A C32 H32C 110.00 . . . no H32B C32 H32C 109.00 . . . no C31 C33 H33 119.00 . . . no C34 C33 H33 119.00 . . . no C34 C35 H35A 109.00 . . . no C34 C35 H35B 109.00 . . . no C34 C35 H35C 109.00 . . . no H35A C35 H35B 110.00 . . . no H35A C35 H35C 110.00 . . . no H35B C35 H35C 109.00 . . . no C34 C36 H36 119.00 . . . no C37 C36 H36 119.00 . . . no C37 C38 H38A 109.00 . . . no C37 C38 H38B 109.00 . . . no C37 C38 H38C 109.00 . . . no H38A C38 H38B 109.00 . . . no H38A C38 H38C 109.00 . . . no H38B C38 H38C 110.00 . . . no 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 O2 Pt1 O1 C27 6.8(5) . . . . no C1 Pt1 O1 C27 -167.8(5) . . . . no O1 Pt1 O2 C29 -5.1(5) . . . . no C9 Pt1 O2 C29 170.8(6) . . . . no O1 Pt1 C1 N1 171.2(5) . . . . no C9 Pt1 C1 N1 -4.6(5) . . . . no O1 Pt1 C1 N2 -1.0(8) . . . . no C9 Pt1 C1 N2 -176.8(8) . . . . no C1 Pt1 C9 C8 4.4(5) . . . . no O2 Pt1 C9 C10 4.7(6) . . . . no C1 Pt1 C9 C10 180.0(7) . . . . no O2 Pt1 C9 C8 -170.9(5) . . . . no Pt1 O1 C27 C23 176.3(4) . . . . no Pt1 O1 C27 C28 -4.9(10) . . . . no Pt1 O2 C29 C30 -178.9(4) . . . . no Pt1 O2 C29 C28 1.1(10) . . . . no C1 N1 C8 C9 -0.5(9) . . . . no C7 N1 C1 N2 5.4(8) . . . . no C8 N1 C1 N2 178.5(6) . . . . no C8 N1 C7 C6 4.7(14) . . . . no C1 N1 C7 C6 176.3(8) . . . . no C7 N1 C8 C9 170.7(7) . . . . no C1 N1 C8 C14 178.4(7) . . . . no C7 N1 C1 Pt1 -169.0(5) . . . . no C8 N1 C1 Pt1 4.2(8) . . . . no C8 N1 C7 C2 -174.9(7) . . . . no C7 N1 C8 C14 -10.5(13) . . . . no C1 N1 C7 C2 -3.3(8) . . . . no C15 N2 C1 Pt1 -12.5(11) . . . . no C2 N2 C1 Pt1 167.4(6) . . . . no C2 N2 C1 N1 -5.2(8) . . . . no C2 N2 C15 C17 -73.8(9) . . . . no C1 N2 C15 C16 -125.9(7) . . . . no C2 N2 C15 C16 54.2(9) . . . . no C1 N2 C15 C17 106.1(8) . . . . no C1 N2 C2 C7 3.1(8) . . . . no C15 N2 C1 N1 174.9(6) . . . . no C1 N2 C2 C3 -171.9(8) . . . . no C15 N2 C2 C7 -177.0(6) . . . . no C15 N2 C2 C3 8.0(13) . . . . no N2 C2 C7 N1 0.2(8) . . . . no C7 C2 C3 C4 2.2(12) . . . . no N2 C2 C3 C4 176.7(8) . . . . no C3 C2 C7 N1 176.0(7) . . . . no N2 C2 C7 C6 -179.5(7) . . . . no C3 C2 C7 C6 -3.7(11) . . . . no C2 C3 C4 C5 0.2(12) . . . . no C3 C4 C5 C6 -1.3(13) . . . . no C4 C5 C6 C7 -0.1(13) . . . . no C5 C6 C7 N1 -176.9(8) . . . . no C5 C6 C7 C2 2.6(11) . . . . no N1 C8 C9 Pt1 -3.3(8) . . . . no C9 C8 C14 C13 -2.1(12) . . . . no C14 C8 C9 Pt1 177.8(6) . . . . no N1 C8 C14 C13 179.1(7) . . . . no N1 C8 C9 C10 -179.3(6) . . . . no C14 C8 C9 C10 1.8(11) . . . . no C8 C9 C10 C11 0.5(10) . . . . no Pt1 C9 C10 C11 -175.0(5) . . . . no C9 C10 C11 C13 -2.4(11) . . . . no C9 C10 C11 C12 177.5(7) . . . . no C10 C11 C13 C14 2.1(11) . . . . no C12 C11 C13 C14 -177.8(8) . . . . no C11 C13 C14 C8 0.1(12) . . . . no C26 C19 C20 C21 1.0(12) . . . . no C18 C19 C26 C24 -178.8(7) . . . . no C18 C19 C20 C21 179.7(8) . . . . no C20 C19 C26 C24 -0.1(12) . . . . no C19 C20 C21 C23 -3.0(12) . . . . no C19 C20 C21 C22 175.7(8) . . . . no C20 C21 C23 C27 -177.0(7) . . . . no C22 C21 C23 C24 -174.6(7) . . . . no C22 C21 C23 C27 4.4(11) . . . . no C20 C21 C23 C24 4.1(11) . . . . no C21 C23 C24 C25 177.6(7) . . . . no C21 C23 C27 C28 -82.9(9) . . . . no C24 C23 C27 O1 -85.0(8) . . . . no C24 C23 C27 C28 96.1(8) . . . . no C21 C23 C27 O1 96.1(8) . . . . no C21 C23 C24 C26 -3.2(11) . . . . no C27 C23 C24 C26 177.9(7) . . . . no C27 C23 C24 C25 -1.4(11) . . . . no C25 C24 C26 C19 -179.6(8) . . . . no C23 C24 C26 C19 1.2(11) . . . . no O1 C27 C28 C29 -1.7(12) . . . . no C23 C27 C28 C29 177.1(7) . . . . no C27 C28 C29 C30 -176.1(7) . . . . no C27 C28 C29 O2 3.9(12) . . . . no O2 C29 C30 C31 109.6(8) . . . . no O2 C29 C30 C37 -68.9(8) . . . . no C28 C29 C30 C31 -70.4(9) . . . . no C28 C29 C30 C37 111.1(8) . . . . no C29 C30 C31 C32 3.6(11) . . . . no C29 C30 C31 C33 -175.8(7) . . . . no C37 C30 C31 C32 -177.9(7) . . . . no C37 C30 C31 C33 2.6(11) . . . . no C29 C30 C37 C36 175.9(6) . . . . no C29 C30 C37 C38 -6.8(10) . . . . no C31 C30 C37 C36 -2.6(11) . . . . no C31 C30 C37 C38 174.7(7) . . . . no C30 C31 C33 C34 -1.1(12) . . . . no C32 C31 C33 C34 179.4(8) . . . . no C31 C33 C34 C35 -179.6(8) . . . . no C31 C33 C34 C36 -0.3(13) . . . . no C33 C34 C36 C37 0.4(12) . . . . no C35 C34 C36 C37 179.6(7) . . . . no C34 C36 C37 C30 1.0(11) . . . . no C34 C36 C37 C38 -176.3(7) . . . . no 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 _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C10 H10 O2 0.9500 2.4200 2.949(8) 115.00 . yes C15 H15 O1 1.0000 2.2600 3.100(8) 141.00 . yes C38 H38A O2 0.9800 2.5600 3.121(8) 117.00 . yes # Loop Mechanism for Extra Tables(s) _iucr_refine_instructions_details ; TITL AT202A2 CELL 0.71073 10.2510 13.9000 22.8720 90.0000 90.0000 90.0000 ZERR 4 0.0021 0.0006 0.0029 0.00 0.00 0.00 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O Pt UNIT 152 148 12 8 4 MERG 2 L.S. 18 ACTA BOND $H FMAP -2 PLAN 10 LIST 4 SIZE 0.297 0.307 0.342 CONF WGHT 0.048700 0.312000 FVAR 0.285980 TEMP -75 C1 1 0.368333 0.034430 0.956890 11.000000 0.019990 0.042640 = 0.019660 -0.005030 -0.003120 0.001020 C2 1 0.289519 -0.060852 1.027296 11.000000 0.030410 0.036210 = 0.034270 0.002330 -0.003260 -0.006510 C3 1 0.269241 -0.132792 1.069010 11.000000 0.042170 0.038360 = 0.035920 0.002010 0.000520 -0.009210 AFIX 43 H3 2 0.313962 -0.192498 1.066394 11.000000 -1.200000 AFIX 0 C4 1 0.181958 -0.115116 1.114578 11.000000 0.057200 0.054440 = 0.035630 -0.003160 0.010900 -0.022640 AFIX 43 H4 2 0.166643 -0.162844 1.143505 11.000000 -1.200000 AFIX 0 C5 1 0.116531 -0.025820 1.117423 11.000000 0.037420 0.065350 = 0.042700 -0.005300 0.015690 -0.003240 AFIX 43 H5 2 0.056089 -0.015109 1.148229 11.000000 -1.200000 AFIX 0 C6 1 0.136909 0.045514 1.077618 11.000000 0.034920 0.044030 = 0.030140 0.000540 0.004080 0.000260 AFIX 43 H6 2 0.091563 0.104940 1.080422 11.000000 -1.200000 AFIX 0 C7 1 0.225600 0.029164 1.032865 11.000000 0.026650 0.038620 = 0.031290 -0.005060 0.002360 -0.003850 C8 1 0.257445 0.183797 0.970320 11.000000 0.035010 0.028650 = 0.022780 -0.007160 -0.002910 0.004850 C9 1 0.342452 0.209956 0.926149 11.000000 0.027510 0.025710 = 0.024720 -0.012230 -0.006530 0.010070 C10 1 0.337662 0.302966 0.906394 11.000000 0.027780 0.035260 = 0.022320 -0.007880 -0.007380 0.007330 AFIX 43 H10 2 0.394366 0.322862 0.875847 11.000000 -1.200000 AFIX 0 C11 1 0.250474 0.368598 0.930667 11.000000 0.037270 0.034770 = 0.022850 -0.000650 -0.005230 0.010470 C12 1 0.252859 0.465801 0.910274 11.000000 0.043720 0.052500 = 0.037310 -0.009270 -0.005900 0.019390 C13 1 0.166072 0.339459 0.972821 11.000000 0.033940 0.053220 = 0.042370 -0.014720 -0.000230 0.018480 AFIX 43 H13 2 0.104845 0.383906 0.988395 11.000000 -1.200000 AFIX 0 C14 1 0.168041 0.245629 0.993461 11.000000 0.038590 0.049820 = 0.035930 -0.004900 0.008810 0.004620 AFIX 43 H14 2 0.108822 0.225056 1.022863 11.000000 -1.200000 AFIX 0 C15 1 0.453644 -0.132832 0.955325 11.000000 0.033700 0.027050 = 0.035580 0.001980 0.004710 -0.001730 AFIX 13 H15 2 0.489542 -0.109802 0.917156 11.000000 -1.200000 AFIX 0 C16 1 0.372249 -0.223515 0.941734 11.000000 0.049560 0.034900 = 0.056270 -0.010230 0.016040 -0.009060 AFIX 137 H16A 2 0.342785 -0.252787 0.978409 11.000000 -1.500000 H16B 2 0.425942 -0.269719 0.920093 11.000000 -1.500000 H16C 2 0.296333 -0.205626 0.918070 11.000000 -1.500000 AFIX 0 C17 1 0.570364 -0.152971 0.994579 11.000000 0.046880 0.059220 = 0.053460 0.000430 -0.004440 0.013880 AFIX 137 H17A 2 0.627722 -0.096577 0.995215 11.000000 -1.500000 H17B 2 0.618560 -0.208552 0.979470 11.000000 -1.500000 H17C 2 0.539970 -0.166752 1.034330 11.000000 -1.500000 AFIX 0 C18 1 1.058157 -0.301409 0.826706 11.000000 0.061870 0.031220 = 0.062840 0.005860 0.019620 0.015020 AFIX 137 H18A 2 1.011344 -0.358159 0.841065 11.000000 -1.500000 H18B 2 1.137447 -0.291873 0.849931 11.000000 -1.500000 H18C 2 1.081795 -0.310979 0.785598 11.000000 -1.500000 AFIX 0 C19 1 0.972203 -0.214428 0.832101 11.000000 0.036510 0.032520 = 0.038590 0.010470 0.010850 0.002790 C20 1 0.884573 -0.190948 0.788611 11.000000 0.047690 0.027870 = 0.042460 -0.004290 0.016390 0.004870 AFIX 43 H20 2 0.879399 -0.230581 0.754852 11.000000 -1.200000 AFIX 0 C21 1 0.804085 -0.111471 0.792703 11.000000 0.039500 0.040320 = 0.030830 -0.005070 -0.001290 -0.004950 C22 1 0.715259 -0.083661 0.741872 11.000000 0.079230 0.065800 = 0.040950 -0.011020 -0.018110 0.023190 AFIX 137 H22A 2 0.625903 -0.075166 0.756202 11.000000 -1.500000 H22B 2 0.716814 -0.134628 0.712275 11.000000 -1.500000 H22C 2 0.746034 -0.023336 0.724507 11.000000 -1.500000 AFIX 0 C23 1 0.807294 -0.056086 0.843426 11.000000 0.032290 0.022270 = 0.031300 0.005510 0.009810 0.005420 C24 1 0.897087 -0.077314 0.887950 11.000000 0.028710 0.037010 = 0.028890 0.003370 0.002280 -0.001650 C25 1 0.906527 -0.016084 0.942404 11.000000 0.062760 0.052510 = 0.044360 -0.015240 -0.012630 0.016670 AFIX 137 H25A 2 0.819182 -0.006594 0.958839 11.000000 -1.500000 H25B 2 0.944561 0.046484 0.932430 11.000000 -1.500000 H25C 2 0.961959 -0.048444 0.971247 11.000000 -1.500000 AFIX 0 C26 1 0.975347 -0.155991 0.880945 11.000000 0.030040 0.035070 = 0.042070 0.008740 0.002360 0.005680 AFIX 43 H26 2 1.035136 -0.171357 0.911276 11.000000 -1.200000 AFIX 0 C27 1 0.716431 0.027609 0.850348 11.000000 0.028720 0.032430 = 0.024430 0.000380 -0.001440 0.001810 C28 1 0.750560 0.115658 0.825108 11.000000 0.030160 0.036160 = 0.038120 0.007250 0.008840 0.008530 AFIX 43 H28 2 0.832867 0.118794 0.806115 11.000000 -1.200000 AFIX 0 C29 1 0.675655 0.199230 0.825095 11.000000 0.032480 0.028710 = 0.023010 0.001820 0.000570 0.003980 C30 1 0.722026 0.286995 0.792792 11.000000 0.030340 0.028040 = 0.031020 -0.001600 0.005870 0.009030 C31 1 0.828235 0.339063 0.813404 11.000000 0.040590 0.032870 = 0.027770 -0.002990 0.003440 0.001830 C32 1 0.908529 0.310783 0.865561 11.000000 0.054700 0.057740 = 0.048770 0.002160 -0.009060 -0.007440 AFIX 137 H32A 2 0.853210 0.277179 0.893918 11.000000 -1.500000 H32B 2 0.945383 0.368572 0.883716 11.000000 -1.500000 H32C 2 0.979394 0.268142 0.853087 11.000000 -1.500000 AFIX 0 C33 1 0.859972 0.423486 0.783204 11.000000 0.038290 0.038920 = 0.043900 -0.007950 0.001120 -0.002800 AFIX 43 H33 2 0.931167 0.461138 0.796748 11.000000 -1.200000 AFIX 0 C34 1 0.792059 0.454275 0.734548 11.000000 0.050580 0.035300 = 0.032250 0.000830 0.005320 0.007200 C35 1 0.831481 0.546678 0.702919 11.000000 0.070380 0.046020 = 0.073950 0.013410 -0.005440 -0.012880 AFIX 137 H35A 2 0.925980 0.546707 0.696432 11.000000 -1.500000 H35B 2 0.807387 0.602406 0.726841 11.000000 -1.500000 H35C 2 0.786353 0.550166 0.665206 11.000000 -1.500000 AFIX 0 C36 1 0.689440 0.399080 0.714866 11.000000 0.036010 0.040510 = 0.037580 0.002250 -0.006220 0.001290 AFIX 43 H36 2 0.642832 0.419603 0.681202 11.000000 -1.200000 AFIX 0 C37 1 0.651470 0.314194 0.742543 11.000000 0.037630 0.035530 = 0.033580 0.000200 -0.002070 -0.000810 C38 1 0.546053 0.254120 0.718125 11.000000 0.053190 0.048790 = 0.046320 0.008230 -0.021360 -0.010530 AFIX 137 H38A 2 0.480238 0.242156 0.748339 11.000000 -1.500000 H38B 2 0.582312 0.192705 0.704754 11.000000 -1.500000 H38C 2 0.505592 0.287596 0.685062 11.000000 -1.500000 AFIX 0 N1 3 0.274540 0.084987 0.986855 11.000000 0.026090 0.030800 = 0.030110 -0.002740 0.003800 0.002450 N2 3 0.372720 -0.053720 0.978730 11.000000 0.028130 0.028620 = 0.028740 -0.003220 0.002930 0.001420 N3 3 0.260407 0.544795 0.894225 11.000000 0.090140 0.035320 = 0.062730 0.005060 0.001110 0.024640 O1 4 0.612436 0.009072 0.878719 11.000000 0.031700 0.032360 = 0.033190 0.000470 0.005820 0.002770 O2 4 0.564741 0.208970 0.851488 11.000000 0.027270 0.028370 = 0.031740 0.003850 0.008570 0.004810 Pt1 5 0.469963 0.109564 0.900707 11.000000 0.024300 0.026990 = 0.024340 -0.001860 0.001280 0.003590 HKLF 4 END ; #===END _database_code_depnum_ccdc_archive 'CCDC 972160'