# Electronic Supplementary Material (ESI) for Chemical Communications # 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_ar73 _database_code_depnum_ccdc_archive 'CCDC 922512' #TrackingRef 'ar73.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H35 F N P Pt' _chemical_formula_sum 'C30 H35 F N P Pt' _chemical_formula_weight 654.65 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.0365(3) _cell_length_b 15.9084(3) _cell_length_c 19.5224(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5291.03(16) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5752 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.35 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 5.390 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3460 _exptl_absorpt_correction_T_max 0.7041 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f & \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38403 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4787 _reflns_number_gt 2919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4787 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0850 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.077926(14) 0.017856(15) 0.253230(10) 0.02038(9) Uani 1 1 d . . . P2 P 0.14196(12) 0.07071(12) 0.34972(8) 0.0232(4) Uani 1 1 d . . . C3 C 0.2298(5) 0.1214(4) 0.3119(3) 0.0269(17) Uani 1 1 d . . . C4 C 0.2957(5) 0.1551(5) 0.3431(3) 0.0290(17) Uani 1 1 d . . . C5 C 0.3519(5) 0.1971(5) 0.3031(3) 0.036(2) Uani 1 1 d . . . H5 H 0.3971 0.2192 0.3252 0.043 Uiso 1 1 calc R . . C6 C 0.3448(4) 0.2076(5) 0.2347(3) 0.0325(18) Uani 1 1 d . . . H6 H 0.3838 0.2379 0.2100 0.039 Uiso 1 1 calc R . . C7 C 0.2794(4) 0.1736(5) 0.1999(3) 0.0287(18) Uani 1 1 d . . . C8 C 0.2220(4) 0.1277(4) 0.2378(3) 0.0218(15) Uani 1 1 d . . . C9 C 0.1584(4) 0.0867(4) 0.2032(3) 0.0259(17) Uani 1 1 d . . . C10 C 0.1508(4) 0.1017(4) 0.1330(3) 0.0264(18) Uani 1 1 d . . . H10 H 0.1074 0.0785 0.1089 0.032 Uiso 1 1 calc R . . C11 C 0.2064(5) 0.1510(4) 0.0970(3) 0.0273(17) Uani 1 1 d . . . H11 H 0.1989 0.1611 0.0495 0.033 Uiso 1 1 calc R . . C12 C 0.2701(5) 0.1840(4) 0.1287(3) 0.0289(18) Uani 1 1 d . . . H12 H 0.3083 0.2141 0.1031 0.035 Uiso 1 1 calc R . . C13 C 0.3148(5) 0.1509(5) 0.4188(3) 0.040(2) Uani 1 1 d . . . H13A H 0.2683 0.1323 0.4442 0.060 Uiso 1 1 calc R . . H13B H 0.3307 0.2066 0.4349 0.060 Uiso 1 1 calc R . . H13C H 0.3578 0.1109 0.4262 0.060 Uiso 1 1 calc R . . C14 C 0.0462(4) -0.0393(4) 0.1624(3) 0.0231(16) Uani 1 1 d . . . C15 C 0.0987(4) -0.0941(4) 0.1321(3) 0.0272(18) Uani 1 1 d . . . H15 H 0.1470 -0.1055 0.1545 0.033 Uiso 1 1 calc R . . C16 C 0.0830(5) -0.1335(5) 0.0694(3) 0.0289(18) Uani 1 1 d . . . H16 H 0.1197 -0.1712 0.0495 0.035 Uiso 1 1 calc R . . C17 C 0.0138(5) -0.1163(4) 0.0377(3) 0.0268(17) Uani 1 1 d . . . C18 C -0.0413(4) -0.0641(5) 0.0651(3) 0.0274(17) Uani 1 1 d . . . H18 H -0.0892 -0.0533 0.0417 0.033 Uiso 1 1 calc R . . C19 C -0.0254(4) -0.0265(4) 0.1288(3) 0.0247(16) Uani 1 1 d . . . H19 H -0.0641 0.0082 0.1495 0.030 Uiso 1 1 calc R . . F20 F -0.0023(2) -0.1538(3) -0.02445(15) 0.0339(10) Uani 1 1 d . . . N21 N -0.0232(3) -0.0472(4) 0.2935(2) 0.0233(13) Uani 1 1 d . . . C22 C -0.0891(4) -0.0040(5) 0.3056(3) 0.0305(19) Uani 1 1 d . . . H22 H -0.0880 0.0553 0.2999 0.037 Uiso 1 1 calc R . . C23 C -0.1581(5) -0.0408(5) 0.3259(3) 0.037(2) Uani 1 1 d . . . H23 H -0.2035 -0.0074 0.3337 0.045 Uiso 1 1 calc R . . C24 C -0.1608(5) -0.1265(5) 0.3347(4) 0.038(2) Uani 1 1 d . . . H24 H -0.2072 -0.1532 0.3507 0.046 Uiso 1 1 calc R . . C25 C -0.0938(5) -0.1731(5) 0.3197(3) 0.039(2) Uani 1 1 d . . . H25 H -0.0938 -0.2326 0.3242 0.047 Uiso 1 1 calc R . . C26 C -0.0281(5) -0.1312(5) 0.2984(3) 0.0348(19) Uani 1 1 d . . . H26 H 0.0168 -0.1634 0.2864 0.042 Uiso 1 1 calc R . . C27 C 0.1731(5) -0.0165(5) 0.4104(3) 0.0316(19) Uani 1 1 d . . . C28 C 0.1835(5) 0.0040(5) 0.4872(3) 0.050(3) Uani 1 1 d . . . H28A H 0.1351 0.0292 0.5049 0.075 Uiso 1 1 calc R . . H28B H 0.2271 0.0436 0.4929 0.075 Uiso 1 1 calc R . . H28C H 0.1949 -0.0479 0.5125 0.075 Uiso 1 1 calc R . . C29 C 0.1098(5) -0.0829(5) 0.4081(4) 0.042(2) Uani 1 1 d . . . H29A H 0.1078 -0.1076 0.3622 0.063 Uiso 1 1 calc R . . H29B H 0.0590 -0.0572 0.4189 0.063 Uiso 1 1 calc R . . H29C H 0.1216 -0.1268 0.4417 0.063 Uiso 1 1 calc R . . C30 C 0.2484(5) -0.0556(5) 0.3818(4) 0.045(2) Uani 1 1 d . . . H30A H 0.2608 -0.1069 0.4074 0.068 Uiso 1 1 calc R . . H30B H 0.2918 -0.0155 0.3865 0.068 Uiso 1 1 calc R . . H30C H 0.2409 -0.0693 0.3333 0.068 Uiso 1 1 calc R . . C31 C 0.0883(4) 0.1587(5) 0.3938(3) 0.0295(18) Uani 1 1 d . . . C32 C 0.1338(5) 0.2107(5) 0.4470(3) 0.041(2) Uani 1 1 d . . . H32A H 0.1817 0.2331 0.4260 0.061 Uiso 1 1 calc R . . H32B H 0.1478 0.1748 0.4859 0.061 Uiso 1 1 calc R . . H32C H 0.1009 0.2573 0.4630 0.061 Uiso 1 1 calc R . . C33 C 0.0632(5) 0.2188(5) 0.3364(3) 0.036(2) Uani 1 1 d . . . H33A H 0.0309 0.2640 0.3557 0.054 Uiso 1 1 calc R . . H33B H 0.0327 0.1878 0.3022 0.054 Uiso 1 1 calc R . . H33C H 0.1099 0.2429 0.3147 0.054 Uiso 1 1 calc R . . C34 C 0.0145(5) 0.1223(5) 0.4284(3) 0.042(2) Uani 1 1 d . . . H34A H 0.0301 0.0851 0.4660 0.063 Uiso 1 1 calc R . . H34B H -0.0159 0.0902 0.3947 0.063 Uiso 1 1 calc R . . H34C H -0.0177 0.1682 0.4464 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02022(15) 0.02173(15) 0.01918(13) 0.00113(11) 0.00037(13) -0.00021(12) P2 0.0257(11) 0.0262(12) 0.0175(8) 0.0012(7) -0.0008(7) 0.0009(9) C3 0.030(5) 0.024(4) 0.027(3) 0.001(3) 0.001(3) 0.000(4) C4 0.028(5) 0.022(5) 0.037(4) -0.001(3) 0.001(3) 0.001(4) C5 0.025(5) 0.040(5) 0.043(4) -0.002(4) -0.010(4) -0.016(4) C6 0.030(5) 0.023(4) 0.045(5) 0.001(3) 0.004(3) 0.000(3) C7 0.029(5) 0.030(5) 0.027(3) 0.000(3) 0.005(3) 0.004(4) C8 0.022(4) 0.019(4) 0.025(3) -0.004(3) 0.002(3) 0.002(3) C9 0.031(5) 0.019(4) 0.027(3) -0.007(3) -0.001(3) 0.009(3) C10 0.025(5) 0.027(5) 0.027(3) -0.007(3) 0.002(3) 0.007(4) C11 0.035(5) 0.023(4) 0.023(3) 0.004(3) 0.006(3) 0.008(4) C12 0.033(5) 0.023(4) 0.031(4) 0.009(3) 0.012(3) 0.000(4) C13 0.033(5) 0.046(6) 0.041(4) -0.011(4) -0.008(3) -0.006(4) C14 0.023(4) 0.022(4) 0.025(3) -0.001(3) 0.006(3) 0.001(3) C15 0.034(5) 0.023(4) 0.025(3) 0.006(3) -0.002(3) 0.004(3) C16 0.033(5) 0.034(5) 0.021(3) 0.000(3) -0.001(3) 0.002(4) C17 0.031(5) 0.030(4) 0.019(3) 0.003(3) 0.003(3) -0.009(4) C18 0.020(4) 0.039(5) 0.024(3) 0.006(3) -0.003(3) -0.004(4) C19 0.013(4) 0.034(5) 0.027(3) 0.005(3) 0.001(3) -0.006(3) F20 0.038(3) 0.044(3) 0.0196(17) -0.0035(17) -0.0036(18) -0.003(2) N21 0.021(4) 0.026(4) 0.023(3) 0.000(2) -0.002(2) -0.001(3) C22 0.023(5) 0.044(5) 0.025(3) 0.002(3) 0.009(3) -0.007(4) C23 0.027(5) 0.053(7) 0.032(4) 0.005(4) 0.000(3) 0.006(4) C24 0.034(6) 0.038(6) 0.043(4) 0.002(4) 0.005(4) -0.014(4) C25 0.057(7) 0.021(5) 0.039(4) -0.003(3) 0.007(4) -0.008(4) C26 0.040(5) 0.030(5) 0.034(4) -0.002(3) 0.010(3) 0.002(4) C27 0.042(5) 0.025(4) 0.028(4) 0.006(3) -0.009(3) 0.005(4) C28 0.066(7) 0.048(6) 0.036(4) 0.012(4) -0.015(4) 0.004(5) C29 0.041(6) 0.044(6) 0.041(4) 0.017(4) 0.002(4) -0.007(4) C30 0.039(6) 0.037(5) 0.059(5) 0.014(4) 0.000(4) 0.009(4) C31 0.027(5) 0.034(5) 0.027(3) -0.007(3) -0.002(3) 0.002(4) C32 0.042(6) 0.041(6) 0.039(4) -0.017(4) -0.004(4) 0.008(4) C33 0.038(6) 0.036(5) 0.034(4) 0.001(3) -0.005(3) 0.009(4) C34 0.038(5) 0.046(6) 0.042(4) -0.002(4) 0.007(4) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C9 2.008(7) . ? Pt1 C14 2.064(6) . ? Pt1 N21 2.157(6) . ? Pt1 P2 2.3336(17) . ? P2 C3 1.854(7) . ? P2 C31 1.881(7) . ? P2 C27 1.900(7) . ? C3 C4 1.386(10) . ? C3 C8 1.455(8) . ? C4 C5 1.405(10) . ? C4 C13 1.513(9) . ? C5 C6 1.351(9) . ? C5 H5 0.9500 . ? C6 C7 1.414(9) . ? C6 H6 0.9500 . ? C7 C12 1.409(8) . ? C7 C8 1.427(9) . ? C8 C9 1.434(9) . ? C9 C10 1.398(8) . ? C10 C11 1.416(10) . ? C10 H10 0.9500 . ? C11 C12 1.355(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.383(9) . ? C14 C19 1.399(9) . ? C15 C16 1.401(8) . ? C15 H15 0.9500 . ? C16 C17 1.358(10) . ? C16 H16 0.9500 . ? C17 C18 1.363(10) . ? C17 F20 1.380(7) . ? C18 C19 1.407(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? N21 C22 1.337(9) . ? N21 C26 1.342(9) . ? C22 C23 1.371(10) . ? C22 H22 0.9500 . ? C23 C24 1.376(11) . ? C23 H23 0.9500 . ? C24 C25 1.392(11) . ? C24 H24 0.9500 . ? C25 C26 1.369(10) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C29 1.510(10) . ? C27 C30 1.530(10) . ? C27 C28 1.545(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.534(9) . ? C31 C32 1.537(9) . ? C31 C34 1.540(10) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C9 Pt1 C14 90.1(3) . . ? C9 Pt1 N21 169.6(2) . . ? C14 Pt1 N21 83.8(2) . . ? C9 Pt1 P2 82.94(18) . . ? C14 Pt1 P2 167.0(2) . . ? N21 Pt1 P2 104.61(13) . . ? C3 P2 C31 104.5(3) . . ? C3 P2 C27 109.9(3) . . ? C31 P2 C27 113.2(3) . . ? C3 P2 Pt1 102.3(2) . . ? C31 P2 Pt1 114.2(2) . . ? C27 P2 Pt1 111.8(2) . . ? C4 C3 C8 119.1(6) . . ? C4 C3 P2 130.3(5) . . ? C8 C3 P2 110.6(5) . . ? C3 C4 C5 119.4(6) . . ? C3 C4 C13 125.9(7) . . ? C5 C4 C13 114.7(7) . . ? C6 C5 C4 123.3(7) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C5 C6 C7 119.8(7) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C12 C7 C6 121.1(7) . . ? C12 C7 C8 119.7(7) . . ? C6 C7 C8 119.2(6) . . ? C7 C8 C9 120.4(5) . . ? C7 C8 C3 119.2(6) . . ? C9 C8 C3 120.4(6) . . ? C10 C9 C8 117.0(6) . . ? C10 C9 Pt1 120.5(5) . . ? C8 C9 Pt1 122.3(4) . . ? C9 C10 C11 121.3(7) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C12 C11 C10 121.6(6) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C7 119.6(7) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C4 C13 H13A 109.5 . . ? C4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 117.0(6) . . ? C15 C14 Pt1 118.4(5) . . ? C19 C14 Pt1 124.5(5) . . ? C14 C15 C16 122.2(7) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C17 C16 C15 118.2(7) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C18 122.8(6) . . ? C16 C17 F20 119.0(6) . . ? C18 C17 F20 118.1(6) . . ? C17 C18 C19 118.2(7) . . ? C17 C18 H18 120.9 . . ? C19 C18 H18 120.9 . . ? C14 C19 C18 121.4(6) . . ? C14 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C22 N21 C26 116.4(7) . . ? C22 N21 Pt1 119.3(5) . . ? C26 N21 Pt1 123.6(5) . . ? N21 C22 C23 123.6(7) . . ? N21 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? C22 C23 C24 119.2(8) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C25 118.3(7) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C26 C25 C24 118.4(7) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? N21 C26 C25 123.9(7) . . ? N21 C26 H26 118.0 . . ? C25 C26 H26 118.0 . . ? C29 C27 C30 107.7(7) . . ? C29 C27 C28 104.9(6) . . ? C30 C27 C28 110.1(6) . . ? C29 C27 P2 107.0(5) . . ? C30 C27 P2 107.7(5) . . ? C28 C27 P2 118.9(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 107.4(6) . . ? C33 C31 C34 109.1(6) . . ? C32 C31 C34 108.6(6) . . ? C33 C31 P2 105.3(4) . . ? C32 C31 P2 117.7(5) . . ? C34 C31 P2 108.5(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.704 _refine_diff_density_min -1.379 _refine_diff_density_rms 0.142 data_ar76 _database_code_depnum_ccdc_archive 'CCDC 922513' #TrackingRef 'ar76.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 F5 N P Pt' _chemical_formula_sum 'C30 H31 F5 N P Pt' _chemical_formula_weight 726.62 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.6094(2) _cell_length_b 16.0440(2) _cell_length_c 19.7637(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5583.74(11) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7063 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 5.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3079 _exptl_absorpt_correction_T_max 0.3600 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34676 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6643 _reflns_number_gt 4355 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+1.4150P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6643 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.071215(7) 0.004252(7) 0.248972(5) 0.01784(6) Uani 1 1 d . . . P2 P 0.12951(5) 0.05422(6) 0.15231(4) 0.02272(19) Uani 1 1 d . . . C3 C 0.1614(2) -0.0339(2) 0.09433(17) 0.0280(8) Uani 1 1 d . . . C4 C 0.1023(2) -0.1037(2) 0.10033(18) 0.0347(9) Uani 1 1 d . . . H4A H 0.0522 -0.0821 0.0877 0.052 Uiso 1 1 calc R . . H4B H 0.1007 -0.1240 0.1471 0.052 Uiso 1 1 calc R . . H4C H 0.1161 -0.1497 0.0701 0.052 Uiso 1 1 calc R . . C5 C 0.1710(2) -0.0160(3) 0.01842(19) 0.0406(10) Uani 1 1 d . . . H5A H 0.2155 0.0197 0.0115 0.061 Uiso 1 1 calc R . . H5B H 0.1256 0.0122 0.0013 0.061 Uiso 1 1 calc R . . H5C H 0.1781 -0.0686 -0.0060 0.061 Uiso 1 1 calc R . . C6 C 0.2361(2) -0.0671(2) 0.12442(19) 0.0394(10) Uani 1 1 d . . . H6A H 0.2506 -0.1186 0.1011 0.059 Uiso 1 1 calc R . . H6B H 0.2290 -0.0786 0.1727 0.059 Uiso 1 1 calc R . . H6C H 0.2761 -0.0253 0.1186 0.059 Uiso 1 1 calc R . . C7 C 0.0701(2) 0.1352(2) 0.10804(17) 0.0299(9) Uani 1 1 d . . . C8 C 0.1106(2) 0.1906(2) 0.05482(18) 0.0402(10) Uani 1 1 d . . . H8A H 0.0740 0.2297 0.0351 0.060 Uiso 1 1 calc R . . H8B H 0.1318 0.1553 0.0190 0.060 Uiso 1 1 calc R . . H8C H 0.1517 0.2219 0.0767 0.060 Uiso 1 1 calc R . . C9 C 0.0429(2) 0.1934(2) 0.16504(17) 0.0362(9) Uani 1 1 d . . . H9A H 0.0087 0.2357 0.1462 0.054 Uiso 1 1 calc R . . H9B H 0.0868 0.2208 0.1859 0.054 Uiso 1 1 calc R . . H9C H 0.0158 0.1608 0.1993 0.054 Uiso 1 1 calc R . . C10 C 0.0016(2) 0.0934(2) 0.07440(18) 0.0388(10) Uani 1 1 d . . . H10A H -0.0234 0.0565 0.1070 0.058 Uiso 1 1 calc R . . H10B H 0.0188 0.0607 0.0354 0.058 Uiso 1 1 calc R . . H10C H -0.0343 0.1362 0.0593 0.058 Uiso 1 1 calc R . . C11 C 0.15155(18) 0.07230(19) 0.29561(16) 0.0219(7) Uani 1 1 d . . . C12 C 0.15046(19) 0.0859(2) 0.36517(16) 0.0252(8) Uani 1 1 d . . . H12 H 0.1109 0.0612 0.3909 0.030 Uiso 1 1 calc R . . C13 C 0.2049(2) 0.1346(2) 0.39932(17) 0.0297(8) Uani 1 1 d . . . H13 H 0.2010 0.1426 0.4468 0.036 Uiso 1 1 calc R . . C14 C 0.2635(2) 0.1702(2) 0.36425(17) 0.0292(8) Uani 1 1 d . . . H14 H 0.3013 0.2012 0.3876 0.035 Uiso 1 1 calc R . . C15 C 0.26773(18) 0.1609(2) 0.29360(17) 0.0247(8) Uani 1 1 d . . . C16 C 0.3278(2) 0.1963(2) 0.25553(19) 0.0316(9) Uani 1 1 d . . . H16 H 0.3669 0.2260 0.2782 0.038 Uiso 1 1 calc R . . C17 C 0.3303(2) 0.1887(2) 0.1877(2) 0.0358(9) Uani 1 1 d . . . H17 H 0.3716 0.2129 0.1638 0.043 Uiso 1 1 calc R . . C18 C 0.27352(19) 0.1457(2) 0.15088(18) 0.0292(8) Uani 1 1 d . . . C19 C 0.21339(19) 0.1092(2) 0.18579(16) 0.0247(7) Uani 1 1 d . . . C20 C 0.21097(19) 0.1139(2) 0.25821(15) 0.0225(7) Uani 1 1 d . . . C21 C 0.2866(2) 0.1434(2) 0.07568(18) 0.0394(9) Uani 1 1 d . . . H21A H 0.3314 0.1092 0.0658 0.059 Uiso 1 1 calc R . . H21B H 0.2948 0.2001 0.0589 0.059 Uiso 1 1 calc R . . H21C H 0.2421 0.1192 0.0533 0.059 Uiso 1 1 calc R . . N22 N -0.02859(15) -0.05957(17) 0.21161(13) 0.0240(6) Uani 1 1 d . . . C23 C -0.0338(2) -0.1425(2) 0.20553(16) 0.0286(8) Uani 1 1 d . . . H23 H 0.0100 -0.1751 0.2148 0.034 Uiso 1 1 calc R . . C24 C -0.0997(2) -0.1833(2) 0.18652(18) 0.0359(9) Uani 1 1 d . . . H24 H -0.1003 -0.2422 0.1816 0.043 Uiso 1 1 calc R . . C25 C -0.1648(2) -0.1367(3) 0.17468(19) 0.0383(10) Uani 1 1 d . . . H25 H -0.2108 -0.1626 0.1608 0.046 Uiso 1 1 calc R . . C26 C -0.1608(2) -0.0521(2) 0.18362(18) 0.0333(9) Uani 1 1 d . . . H26 H -0.2048 -0.0188 0.1773 0.040 Uiso 1 1 calc R . . C27 C -0.0930(2) -0.0151(2) 0.20178(18) 0.0291(8) Uani 1 1 d . . . H27 H -0.0915 0.0437 0.2076 0.035 Uiso 1 1 calc R . . C28 C 0.03852(18) -0.0477(2) 0.34059(16) 0.0244(7) Uani 1 1 d . . . C29 C 0.08253(19) -0.1085(2) 0.37127(17) 0.0244(8) Uani 1 1 d . . . C30 C 0.0660(2) -0.1444(2) 0.43287(17) 0.0286(8) Uani 1 1 d . . . C31 C 0.0028(2) -0.1184(2) 0.46776(16) 0.0288(8) Uani 1 1 d . . . C32 C -0.04370(19) -0.0593(2) 0.43936(16) 0.0265(8) Uani 1 1 d . . . C33 C -0.02523(19) -0.0266(2) 0.37722(17) 0.0256(7) Uani 1 1 d . . . F34 F -0.07303(11) 0.03362(14) 0.35271(10) 0.0357(5) Uani 1 1 d . . . F35 F -0.10629(11) -0.03431(14) 0.47383(9) 0.0365(5) Uani 1 1 d . . . F36 F -0.01319(12) -0.15185(13) 0.52905(9) 0.0372(5) Uani 1 1 d . . . F37 F 0.11027(12) -0.20572(12) 0.45897(9) 0.0375(5) Uani 1 1 d . . . F38 F 0.14756(11) -0.13505(12) 0.34060(9) 0.0327(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01665(9) 0.01980(9) 0.01708(9) -0.00138(5) -0.00060(5) -0.00025(5) P2 0.0253(5) 0.0240(5) 0.0189(4) -0.0004(4) -0.0003(4) 0.0029(4) C3 0.0292(19) 0.030(2) 0.0248(18) -0.0036(15) 0.0031(16) 0.0051(16) C4 0.043(2) 0.033(2) 0.0284(19) -0.0093(16) 0.0000(18) -0.0013(19) C5 0.051(3) 0.041(2) 0.031(2) -0.0056(18) 0.0097(18) 0.000(2) C6 0.035(2) 0.032(2) 0.051(2) -0.0064(18) 0.0037(19) 0.0114(18) C7 0.037(2) 0.032(2) 0.0210(18) 0.0016(15) 0.0013(15) 0.0086(17) C8 0.049(3) 0.039(2) 0.033(2) 0.0088(18) 0.0009(18) 0.012(2) C9 0.040(2) 0.037(2) 0.031(2) 0.0004(16) -0.0027(17) 0.0190(18) C10 0.038(2) 0.049(3) 0.030(2) -0.0010(17) -0.0096(18) 0.011(2) C11 0.0238(17) 0.0192(17) 0.0227(16) 0.0022(13) -0.0021(14) 0.0018(14) C12 0.0235(18) 0.029(2) 0.0232(17) 0.0044(14) 0.0004(15) 0.0027(15) C13 0.036(2) 0.031(2) 0.0220(18) -0.0025(15) -0.0083(16) 0.0003(17) C14 0.031(2) 0.0239(19) 0.0321(19) 0.0004(14) -0.0099(16) -0.0012(15) C15 0.0224(18) 0.0159(17) 0.036(2) 0.0018(14) -0.0033(15) -0.0012(14) C16 0.025(2) 0.0226(19) 0.047(3) -0.0007(17) -0.0018(17) -0.0042(14) C17 0.033(2) 0.027(2) 0.048(2) 0.0038(18) 0.0106(18) -0.0047(17) C18 0.028(2) 0.0232(19) 0.037(2) 0.0004(15) 0.0046(16) 0.0007(16) C19 0.0275(19) 0.0198(18) 0.0268(18) 0.0024(14) -0.0001(15) 0.0013(15) C20 0.0219(17) 0.0199(16) 0.0258(18) 0.0022(13) 0.0006(14) 0.0022(14) C21 0.046(2) 0.037(2) 0.035(2) 0.0063(17) 0.0119(19) -0.002(2) N22 0.0225(15) 0.0264(16) 0.0230(15) -0.0025(12) -0.0025(12) -0.0026(13) C23 0.028(2) 0.028(2) 0.0289(19) 0.0012(15) -0.0005(16) 0.0022(16) C24 0.041(2) 0.028(2) 0.039(2) 0.0007(16) -0.0022(18) -0.0071(18) C25 0.029(2) 0.041(2) 0.045(2) -0.0022(19) -0.0084(18) -0.0046(18) C26 0.0209(18) 0.035(2) 0.044(2) -0.0051(18) -0.0065(16) 0.0020(16) C27 0.026(2) 0.0285(19) 0.033(2) -0.0004(16) -0.0048(16) -0.0005(16) C28 0.0253(18) 0.0247(18) 0.0233(17) -0.0014(14) -0.0007(15) -0.0064(15) C29 0.0238(18) 0.0224(19) 0.0271(18) -0.0092(14) -0.0017(15) 0.0000(15) C30 0.041(2) 0.0210(19) 0.0243(18) 0.0000(15) -0.0091(16) 0.0007(17) C31 0.042(2) 0.028(2) 0.0172(17) -0.0019(14) -0.0003(16) -0.0086(17) C32 0.0232(18) 0.034(2) 0.0218(17) -0.0052(15) 0.0000(15) -0.0066(16) C33 0.0231(19) 0.0265(18) 0.0273(18) -0.0015(15) -0.0008(15) -0.0012(15) F34 0.0280(12) 0.0479(14) 0.0312(11) 0.0058(10) 0.0027(9) 0.0116(10) F35 0.0320(12) 0.0511(14) 0.0263(10) -0.0014(9) 0.0070(9) 0.0013(11) F36 0.0553(14) 0.0365(13) 0.0197(10) 0.0021(9) 0.0021(10) -0.0063(11) F37 0.0552(14) 0.0292(12) 0.0280(11) -0.0025(9) -0.0104(10) 0.0116(10) F38 0.0334(12) 0.0352(12) 0.0294(11) 0.0003(9) 0.0030(9) 0.0094(10) _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 C11 2.011(3) . ? Pt1 C28 2.074(3) . ? Pt1 N22 2.164(3) . ? Pt1 P2 2.3122(9) . ? P2 C19 1.843(3) . ? P2 C7 1.884(4) . ? P2 C3 1.905(3) . ? C3 C4 1.534(5) . ? C3 C5 1.537(5) . ? C3 C6 1.538(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C10 1.531(5) . ? C7 C9 1.540(5) . ? C7 C8 1.551(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.392(4) . ? C11 C20 1.444(4) . ? C12 C13 1.409(5) . ? C12 H12 0.9500 . ? C13 C14 1.368(5) . ? C13 H13 0.9500 . ? C14 C15 1.406(5) . ? C14 H14 0.9500 . ? C15 C16 1.417(5) . ? C15 C20 1.434(4) . ? C16 C17 1.347(5) . ? C16 H16 0.9500 . ? C17 C18 1.417(5) . ? C17 H17 0.9500 . ? C18 C19 1.393(5) . ? C18 C21 1.505(5) . ? C19 C20 1.434(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N22 C23 1.340(4) . ? N22 C27 1.353(4) . ? C23 C24 1.383(5) . ? C23 H23 0.9500 . ? C24 C25 1.390(5) . ? C24 H24 0.9500 . ? C25 C26 1.370(5) . ? C25 H25 0.9500 . ? C26 C27 1.381(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.378(4) . ? C28 C29 1.386(5) . ? C29 F38 1.364(4) . ? C29 C30 1.378(5) . ? C30 F37 1.357(4) . ? C30 C31 1.373(5) . ? C31 F36 1.354(4) . ? C31 C32 1.373(5) . ? C32 F35 1.357(4) . ? C32 C33 1.375(5) . ? C33 F34 1.370(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pt1 C28 90.75(12) . . ? C11 Pt1 N22 170.00(11) . . ? C28 Pt1 N22 83.25(11) . . ? C11 Pt1 P2 83.00(9) . . ? C28 Pt1 P2 169.60(9) . . ? N22 Pt1 P2 104.05(7) . . ? C19 P2 C7 106.37(16) . . ? C19 P2 C3 109.54(15) . . ? C7 P2 C3 113.38(16) . . ? C19 P2 Pt1 103.01(11) . . ? C7 P2 Pt1 112.10(11) . . ? C3 P2 Pt1 111.75(11) . . ? C4 C3 C5 106.6(3) . . ? C4 C3 C6 107.4(3) . . ? C5 C3 C6 110.4(3) . . ? C4 C3 P2 107.1(2) . . ? C5 C3 P2 118.7(3) . . ? C6 C3 P2 106.1(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 C7 C9 109.8(3) . . ? C10 C7 C8 108.6(3) . . ? C9 C7 C8 107.0(3) . . ? C10 C7 P2 109.7(3) . . ? C9 C7 P2 104.6(2) . . ? C8 C7 P2 117.0(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C20 116.3(3) . . ? C12 C11 Pt1 121.9(2) . . ? C20 C11 Pt1 121.7(2) . . ? C11 C12 C13 123.4(3) . . ? C11 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 121.6(3) . . ? C14 C15 C20 120.2(3) . . ? C16 C15 C20 118.2(3) . . ? C17 C16 C15 121.1(3) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 122.2(3) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C19 C18 C17 119.1(3) . . ? C19 C18 C21 126.6(3) . . ? C17 C18 C21 114.3(3) . . ? C18 C19 C20 119.7(3) . . ? C18 C19 P2 129.2(3) . . ? C20 C19 P2 111.1(2) . . ? C19 C20 C15 119.6(3) . . ? C19 C20 C11 120.5(3) . . ? C15 C20 C11 119.9(3) . . ? 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 . . ? C23 N22 C27 117.0(3) . . ? C23 N22 Pt1 123.8(2) . . ? C27 N22 Pt1 118.7(2) . . ? N22 C23 C24 123.5(3) . . ? N22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 118.9(4) . . ? C23 C24 H24 120.6 . . ? C25 C24 H24 120.6 . . ? C26 C25 C24 117.9(4) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 C27 120.3(4) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? N22 C27 C26 122.3(3) . . ? N22 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C33 C28 C29 113.5(3) . . ? C33 C28 Pt1 125.9(3) . . ? C29 C28 Pt1 120.6(2) . . ? F38 C29 C30 116.1(3) . . ? F38 C29 C28 119.7(3) . . ? C30 C29 C28 124.3(3) . . ? F37 C30 C31 119.7(3) . . ? F37 C30 C29 121.2(3) . . ? C31 C30 C29 119.2(3) . . ? F36 C31 C30 119.8(3) . . ? F36 C31 C32 121.0(3) . . ? C30 C31 C32 119.2(3) . . ? F35 C32 C31 118.9(3) . . ? F35 C32 C33 121.8(3) . . ? C31 C32 C33 119.2(3) . . ? F34 C33 C32 116.1(3) . . ? F34 C33 C28 119.2(3) . . ? C32 C33 C28 124.6(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.219 _refine_diff_density_min -2.103 _refine_diff_density_rms 0.118 data_ar77sq _database_code_depnum_ccdc_archive 'CCDC 922514' #TrackingRef 'ar77sq.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H31 F N P Pt' _chemical_formula_sum 'C27 H31 F N P Pt' _chemical_formula_weight 614.59 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.1768(3) _cell_length_b 7.44570(10) _cell_length_c 21.2471(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.0982(8) _cell_angle_gamma 90.00 _cell_volume 2610.81(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5767 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 5.456 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2511 _exptl_absorpt_correction_T_max 0.4950 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19492 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.87 _reflns_number_total 6196 _reflns_number_gt 4079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The structure contains unidentified disordered solvent, which could not be modeled by dicrete atoms. Its contribution to the diffraction pattern was thus subtracted by the Squeeze technique, using the PLATON software (Spek, 2009). ; _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^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6196 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1080 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.374715(10) 0.25354(2) 0.379711(8) 0.02279(8) Uani 1 1 d . . . P2 P 0.24419(8) 0.13718(16) 0.35887(7) 0.0262(3) Uani 1 1 d . . . C3 C 0.1886(3) 0.1871(7) 0.4222(3) 0.0344(12) Uani 1 1 d . . . C4 C 0.1520(4) 0.3803(7) 0.4074(3) 0.0438(15) Uani 1 1 d . . . H4A H 0.1358 0.4246 0.4454 0.066 Uiso 1 1 calc R . . H4B H 0.1046 0.3763 0.3691 0.066 Uiso 1 1 calc R . . H4C H 0.1928 0.4611 0.3986 0.066 Uiso 1 1 calc R . . C5 C 0.2509(4) 0.1958(8) 0.4891(3) 0.0394(13) Uani 1 1 d . . . H5A H 0.2914 0.2881 0.4884 0.059 Uiso 1 1 calc R . . H5B H 0.2777 0.0790 0.4992 0.059 Uiso 1 1 calc R . . H5C H 0.2237 0.2259 0.5226 0.059 Uiso 1 1 calc R . . C6 C 0.1208(4) 0.0576(8) 0.4286(3) 0.0453(15) Uani 1 1 d . . . H6A H 0.1427 -0.0644 0.4369 0.068 Uiso 1 1 calc R . . H6B H 0.0766 0.0592 0.3880 0.068 Uiso 1 1 calc R . . H6C H 0.1003 0.0960 0.4652 0.068 Uiso 1 1 calc R . . C7 C 0.2479(3) -0.1115(6) 0.3421(2) 0.0263(11) Uani 1 1 d . . . C8 C 0.1679(3) -0.2093(6) 0.3131(3) 0.0309(12) Uani 1 1 d . . . H8A H 0.1372 -0.1475 0.2732 0.046 Uiso 1 1 calc R . . H8B H 0.1363 -0.2101 0.3450 0.046 Uiso 1 1 calc R . . H8C H 0.1789 -0.3331 0.3024 0.046 Uiso 1 1 calc R . . C9 C 0.2957(3) -0.2043(7) 0.4061(3) 0.0318(12) Uani 1 1 d . . . H9A H 0.2628 -0.2057 0.4372 0.048 Uiso 1 1 calc R . . H9B H 0.3460 -0.1383 0.4253 0.048 Uiso 1 1 calc R . . H9C H 0.3085 -0.3279 0.3966 0.048 Uiso 1 1 calc R . . C10 C 0.2963(3) -0.1283(6) 0.2912(2) 0.0318(11) Uani 1 1 d . . . H10A H 0.3083 -0.2551 0.2857 0.048 Uiso 1 1 calc R . . H10B H 0.3471 -0.0611 0.3063 0.048 Uiso 1 1 calc R . . H10C H 0.2643 -0.0795 0.2491 0.048 Uiso 1 1 calc R . . C11 C 0.1937(3) 0.2408(5) 0.2782(3) 0.0264(10) Uani 1 1 d . . . C12 C 0.1132(4) 0.2385(6) 0.2414(3) 0.0340(12) Uani 1 1 d . . . C13 C 0.0904(3) 0.3257(7) 0.1791(3) 0.0394(13) Uani 1 1 d . . . H13 H 0.0349 0.3258 0.1547 0.047 Uiso 1 1 calc R . . C14 C 0.1451(3) 0.4086(7) 0.1532(3) 0.0390(13) Uani 1 1 d . . . H14 H 0.1277 0.4611 0.1108 0.047 Uiso 1 1 calc R . . C15 C 0.2277(3) 0.4167(6) 0.1891(3) 0.0317(12) Uani 1 1 d . . . C16 C 0.2858(4) 0.5081(6) 0.1648(3) 0.0362(13) Uani 1 1 d . . . H16 H 0.2695 0.5636 0.1229 0.043 Uiso 1 1 calc R . . C17 C 0.3656(4) 0.5174(7) 0.2011(3) 0.0365(13) Uani 1 1 d . . . H17 H 0.4040 0.5789 0.1843 0.044 Uiso 1 1 calc R . . C18 C 0.3906(3) 0.4340(6) 0.2643(2) 0.0273(11) Uani 1 1 d . . . C19 C 0.3341(3) 0.3455(6) 0.2893(2) 0.0266(11) Uani 1 1 d . . . C20 C 0.2524(3) 0.3345(6) 0.2519(2) 0.0307(12) Uani 1 1 d . . . C21 C 0.0450(3) 0.1486(8) 0.2618(3) 0.0444(14) Uani 1 1 d . . . H21A H 0.0677 0.0661 0.2982 0.067 Uiso 1 1 calc R . . H21B H 0.0109 0.0812 0.2247 0.067 Uiso 1 1 calc R . . H21C H 0.0123 0.2401 0.2757 0.067 Uiso 1 1 calc R . . C22 C 0.4740(3) 0.4391(6) 0.3074(2) 0.0290(11) Uani 1 1 d . . . C23 C 0.5410(3) 0.5112(6) 0.2916(3) 0.0318(12) Uani 1 1 d . . . H23 H 0.5347 0.5639 0.2498 0.038 Uiso 1 1 calc R . . C24 C 0.6173(4) 0.5065(7) 0.3369(3) 0.0377(14) Uani 1 1 d . . . H24 H 0.6629 0.5590 0.3270 0.045 Uiso 1 1 calc R . . C25 C 0.6250(3) 0.4236(7) 0.3965(3) 0.0375(13) Uani 1 1 d . . . C26 C 0.5584(3) 0.3513(7) 0.4134(3) 0.0327(12) Uani 1 1 d . . . H26 H 0.5655 0.2966 0.4550 0.039 Uiso 1 1 calc R . . C27 C 0.4817(3) 0.3596(6) 0.3693(2) 0.0288(11) Uani 1 1 d . . . F28 F 0.69989(18) 0.4104(4) 0.44016(16) 0.0461(8) Uani 1 1 d . . . N29 N 0.4279(3) 0.1857(6) 0.4759(2) 0.0312(10) Uani 1 1 d . . . C30 C 0.4557(3) 0.1724(7) 0.5312(3) 0.0297(11) Uani 1 1 d . . . C31 C 0.4893(3) 0.1552(7) 0.6024(2) 0.0336(12) Uani 1 1 d . . . H31A H 0.4452 0.1592 0.6233 0.050 Uiso 1 1 calc R . . H31B H 0.5270 0.2543 0.6188 0.050 Uiso 1 1 calc R . . H31C H 0.5181 0.0406 0.6125 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02693(12) 0.02070(12) 0.02130(12) 0.00015(8) 0.00764(8) -0.00107(8) P2 0.0261(7) 0.0217(6) 0.0317(7) -0.0001(5) 0.0095(6) 0.0010(5) C3 0.042(3) 0.029(2) 0.040(3) -0.004(2) 0.023(3) -0.001(3) C4 0.044(4) 0.031(3) 0.062(4) -0.003(3) 0.024(3) 0.004(3) C5 0.043(3) 0.043(3) 0.037(3) -0.003(3) 0.019(3) 0.002(3) C6 0.046(4) 0.045(3) 0.053(4) -0.003(3) 0.029(3) -0.007(3) C7 0.030(3) 0.016(2) 0.032(3) -0.0034(19) 0.008(2) -0.001(2) C8 0.025(3) 0.029(2) 0.037(3) -0.002(2) 0.006(2) 0.000(2) C9 0.029(3) 0.028(2) 0.035(3) 0.003(2) 0.004(2) 0.000(2) C10 0.039(3) 0.026(2) 0.031(3) -0.004(2) 0.009(2) 0.000(2) C11 0.033(3) 0.020(2) 0.026(3) -0.0002(19) 0.008(2) 0.006(2) C12 0.031(3) 0.027(3) 0.040(3) -0.005(2) 0.003(2) 0.004(2) C13 0.032(3) 0.035(3) 0.041(4) -0.002(3) -0.005(3) 0.007(3) C14 0.048(4) 0.031(3) 0.034(3) 0.000(2) 0.005(3) 0.013(3) C15 0.043(3) 0.023(2) 0.030(3) -0.001(2) 0.010(2) 0.010(2) C16 0.064(4) 0.025(2) 0.021(3) 0.006(2) 0.015(3) 0.014(3) C17 0.052(4) 0.025(2) 0.037(3) 0.003(2) 0.020(3) 0.005(3) C18 0.033(3) 0.020(2) 0.030(3) -0.0016(19) 0.010(2) 0.005(2) C19 0.031(3) 0.018(2) 0.031(3) -0.003(2) 0.010(2) 0.001(2) C20 0.045(3) 0.022(2) 0.027(3) 0.000(2) 0.012(2) 0.000(2) C21 0.029(3) 0.041(3) 0.056(4) 0.002(3) 0.001(3) 0.007(3) C22 0.041(3) 0.022(2) 0.028(3) -0.006(2) 0.016(2) -0.004(2) C23 0.045(3) 0.025(2) 0.030(3) -0.006(2) 0.018(2) -0.007(2) C24 0.047(3) 0.030(3) 0.044(4) -0.015(2) 0.025(3) -0.013(3) C25 0.040(3) 0.034(3) 0.037(3) -0.012(2) 0.010(3) -0.010(3) C26 0.035(3) 0.031(3) 0.034(3) 0.000(2) 0.013(2) -0.004(2) C27 0.043(3) 0.019(2) 0.025(3) 0.0002(19) 0.010(2) 0.000(2) F28 0.0341(18) 0.054(2) 0.048(2) -0.0057(16) 0.0076(16) -0.0114(15) N29 0.030(2) 0.030(2) 0.036(3) -0.001(2) 0.015(2) 0.004(2) C30 0.032(3) 0.029(3) 0.030(3) -0.007(2) 0.010(2) 0.000(2) C31 0.040(3) 0.035(3) 0.024(3) -0.002(2) 0.005(2) 0.005(3) _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 C19 1.975(5) . ? Pt1 N29 2.057(5) . ? Pt1 C27 2.067(5) . ? Pt1 P2 2.3287(13) . ? P2 C11 1.861(5) . ? P2 C3 1.890(5) . ? P2 C7 1.890(4) . ? C3 C5 1.524(8) . ? C3 C6 1.547(7) . ? C3 C4 1.566(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.526(7) . ? C7 C10 1.541(7) . ? C7 C9 1.544(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.387(8) . ? C11 C20 1.457(7) . ? C12 C13 1.429(8) . ? C12 C21 1.513(8) . ? C13 C14 1.361(8) . ? C13 H13 0.9500 . ? C14 C15 1.414(7) . ? C14 H14 0.9500 . ? C15 C16 1.419(7) . ? C15 C20 1.423(7) . ? C16 C17 1.375(8) . ? C16 H16 0.9500 . ? C17 C18 1.433(7) . ? C17 H17 0.9500 . ? C18 C19 1.396(6) . ? C18 C22 1.471(7) . ? C19 C20 1.411(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.391(7) . ? C22 C27 1.416(7) . ? C23 C24 1.395(8) . ? C23 H23 0.9500 . ? C24 C25 1.383(8) . ? C24 H24 0.9500 . ? C25 F28 1.365(6) . ? C25 C26 1.398(7) . ? C26 C27 1.391(7) . ? C26 H26 0.9500 . ? N29 C30 1.143(6) . ? C30 C31 1.467(7) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 C19 Pt1 N29 172.35(18) . . ? C19 Pt1 C27 81.3(2) . . ? N29 Pt1 C27 92.13(18) . . ? C19 Pt1 P2 83.23(14) . . ? N29 Pt1 P2 103.67(12) . . ? C27 Pt1 P2 163.57(15) . . ? C11 P2 C3 112.1(2) . . ? C11 P2 C7 105.3(2) . . ? C3 P2 C7 112.2(2) . . ? C11 P2 Pt1 101.47(17) . . ? C3 P2 Pt1 116.17(19) . . ? C7 P2 Pt1 108.62(16) . . ? C5 C3 C6 107.2(5) . . ? C5 C3 C4 106.7(5) . . ? C6 C3 C4 108.7(5) . . ? C5 C3 P2 108.0(4) . . ? C6 C3 P2 118.8(4) . . ? C4 C3 P2 107.0(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C10 106.2(4) . . ? C8 C7 C9 109.9(4) . . ? C10 C7 C9 108.9(4) . . ? C8 C7 P2 118.1(3) . . ? C10 C7 P2 105.4(3) . . ? C9 C7 P2 108.0(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C20 118.5(5) . . ? C12 C11 P2 130.6(4) . . ? C20 C11 P2 110.9(4) . . ? C11 C12 C13 119.4(5) . . ? C11 C12 C21 125.1(5) . . ? C13 C12 C21 115.5(5) . . ? C14 C13 C12 122.6(5) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 120.2(5) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 121.7(5) . . ? C14 C15 C20 118.8(5) . . ? C16 C15 C20 119.5(5) . . ? C17 C16 C15 120.8(5) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 120.2(5) . . ? C19 C18 C22 115.8(4) . . ? C17 C18 C22 124.0(5) . . ? C18 C19 C20 120.1(5) . . ? C18 C19 Pt1 116.0(4) . . ? C20 C19 Pt1 123.8(4) . . ? C19 C20 C15 119.6(5) . . ? C19 C20 C11 119.8(4) . . ? C15 C20 C11 120.5(5) . . ? C12 C21 H21A 109.5 . . ? C12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 121.0(5) . . ? C23 C22 C18 126.0(5) . . ? C27 C22 C18 113.0(4) . . ? C22 C23 C24 120.4(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 118.4(5) . . ? C25 C24 H24 120.8 . . ? C23 C24 H24 120.8 . . ? F28 C25 C24 119.1(5) . . ? F28 C25 C26 118.8(5) . . ? C24 C25 C26 122.1(6) . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 118.1(5) . . ? C26 C27 Pt1 127.9(4) . . ? C22 C27 Pt1 113.8(4) . . ? C30 N29 Pt1 170.5(4) . . ? N29 C30 C31 178.6(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.000 0.000 0.000 191 84 ' ' 2 1.000 0.500 0.500 191 84 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.247 _refine_diff_density_min -2.095 _refine_diff_density_rms 0.164 data_ar80 _database_code_depnum_ccdc_archive 'CCDC 922515' #TrackingRef 'ar80.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H34 F4 N P Pt, 1.7(C2 H3 N), 0.79(C H3 O)' _chemical_formula_sum 'C34.19 H41.46 F4 N2.70 O0.79 P Pt' _chemical_formula_weight 804.86 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1311(3) _cell_length_b 11.4959(4) _cell_length_c 15.7724(5) _cell_angle_alpha 75.0835(16) _cell_angle_beta 79.7841(18) _cell_angle_gamma 86.3353(11) _cell_volume 1746.59(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6408 _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 27.91 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 801.9 _exptl_absorpt_coefficient_mu 4.112 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4262 _exptl_absorpt_correction_T_max 0.4935 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19408 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.91 _reflns_number_total 8240 _reflns_number_gt 6508 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. In the asymmetric unit there is one well-ordered molecule of acetonitrile, another partly disaordered molecule of acetonitrile refined with 0.7 occupancy, and another partly disordered molecule of methanol with refine occupancy of about 79%. The disordered species were assigned an isotropic ADPs. ; _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^)+(0.0678P)^2^+4.0376P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8240 _refine_ls_number_parameters 393 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1301 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.66671(3) 0.70507(2) 0.282991(15) 0.02609(10) Uani 1 1 d . . . P2 P 0.70009(16) 0.67448(14) 0.14084(10) 0.0238(3) Uani 1 1 d . . . F3 F 0.4792(4) 0.6312(3) 0.3336(2) 0.0323(8) Uani 1 1 d . . . F4 F 0.7350(4) 0.5391(3) 0.3444(2) 0.0358(9) Uani 1 1 d . . . C5 C 0.7642(7) 0.5164(6) 0.1427(4) 0.0299(14) Uani 1 1 d . . . C6 C 0.8019(7) 0.4890(7) 0.0503(5) 0.0349(15) Uani 1 1 d . . . H6A H 0.8401 0.4073 0.0572 0.052 Uiso 1 1 calc R . . H6B H 0.8680 0.5469 0.0124 0.052 Uiso 1 1 calc R . . H6C H 0.7214 0.4954 0.0228 0.052 Uiso 1 1 calc R . . C7 C 0.8959(7) 0.4962(6) 0.1822(5) 0.0339(15) Uani 1 1 d . . . H7A H 0.8810 0.5184 0.2392 0.051 Uiso 1 1 calc R . . H7B H 0.9664 0.5461 0.1408 0.051 Uiso 1 1 calc R . . H7C H 0.9235 0.4112 0.1916 0.051 Uiso 1 1 calc R . . C8 C 0.6582(7) 0.4280(6) 0.2018(4) 0.0342(15) Uani 1 1 d . . . H8A H 0.6927 0.3454 0.2068 0.051 Uiso 1 1 calc R . . H8B H 0.5764 0.4389 0.1752 0.051 Uiso 1 1 calc R . . H8C H 0.6378 0.4434 0.2611 0.051 Uiso 1 1 calc R . . C9 C 0.5453(7) 0.7131(6) 0.0840(4) 0.0305(14) Uani 1 1 d . . . C10 C 0.4194(7) 0.6850(7) 0.1560(5) 0.0344(15) Uani 1 1 d . . . H10A H 0.3392 0.6985 0.1277 0.052 Uiso 1 1 calc R . . H10B H 0.4153 0.7377 0.1964 0.052 Uiso 1 1 calc R . . H10C H 0.4236 0.6007 0.1898 0.052 Uiso 1 1 calc R . . C11 C 0.5317(7) 0.6417(6) 0.0162(4) 0.0328(15) Uani 1 1 d . . . H11A H 0.5208 0.5562 0.0466 0.049 Uiso 1 1 calc R . . H11B H 0.6125 0.6516 -0.0294 0.049 Uiso 1 1 calc R . . H11C H 0.4532 0.6716 -0.0120 0.049 Uiso 1 1 calc R . . C12 C 0.5443(7) 0.8492(6) 0.0383(4) 0.0319(15) Uani 1 1 d . . . H12A H 0.6268 0.8692 -0.0051 0.048 Uiso 1 1 calc R . . H12B H 0.5389 0.8953 0.0831 0.048 Uiso 1 1 calc R . . H12C H 0.4665 0.8694 0.0077 0.048 Uiso 1 1 calc R . . N13 N 0.6391(5) 0.7355(5) 0.4136(3) 0.0267(11) Uani 1 1 d . . . C14 C 0.6040(7) 0.6399(7) 0.4809(4) 0.0346(15) Uani 1 1 d . . . H14 H 0.5978 0.5638 0.4688 0.042 Uiso 1 1 calc R . . C15 C 0.5762(8) 0.6492(7) 0.5689(4) 0.0376(16) Uani 1 1 d . . . H15 H 0.5503 0.5806 0.6163 0.045 Uiso 1 1 calc R . . C16 C 0.5869(9) 0.7599(7) 0.5858(5) 0.047(2) Uani 1 1 d . . . H16 H 0.5679 0.7686 0.6450 0.056 Uiso 1 1 calc R . . C17 C 0.6252(9) 0.8570(7) 0.5164(5) 0.0416(18) Uani 1 1 d . . . H17 H 0.6328 0.9336 0.5273 0.050 Uiso 1 1 calc R . . C18 C 0.6529(8) 0.8433(6) 0.4300(4) 0.0341(15) Uani 1 1 d . . . H18 H 0.6818 0.9104 0.3820 0.041 Uiso 1 1 calc R . . C19 C 0.5890(6) 0.8735(5) 0.2431(4) 0.0235(12) Uani 1 1 d . . . C20 C 0.4559(6) 0.8916(6) 0.2820(4) 0.0278(13) Uani 1 1 d . . . H20 H 0.4048 0.8259 0.3198 0.033 Uiso 1 1 calc R . . C21 C 0.4003(6) 1.0072(6) 0.2641(4) 0.0290(14) Uani 1 1 d . . . C22 C 0.4675(7) 1.1075(6) 0.2116(4) 0.0288(14) Uani 1 1 d . . . H22 H 0.4273 1.1857 0.2003 0.035 Uiso 1 1 calc R . . C23 C 0.5974(7) 1.0847(6) 0.1770(4) 0.0267(13) Uani 1 1 d . . . C24 C 0.6604(7) 0.9742(6) 0.1901(4) 0.0260(13) Uani 1 1 d . . . H24 H 0.7513 0.9660 0.1637 0.031 Uiso 1 1 calc R . . F25 F 0.2714(4) 1.0221(4) 0.3037(3) 0.0439(10) Uani 1 1 d . . . F26 F 0.6708(4) 1.1817(3) 0.1244(2) 0.0344(9) Uani 1 1 d . . . C27 C 0.8549(6) 0.7653(6) 0.2444(4) 0.0254(13) Uani 1 1 d . . . C28 C 0.9292(7) 0.7821(6) 0.3059(4) 0.0327(15) Uani 1 1 d . . . H28 H 0.8920 0.7606 0.3674 0.039 Uiso 1 1 calc R . . C29 C 1.0567(7) 0.8298(6) 0.2795(5) 0.0374(16) Uani 1 1 d . . . H29 H 1.1050 0.8401 0.3234 0.045 Uiso 1 1 calc R . . C30 C 1.1142(7) 0.8621(6) 0.1921(5) 0.0348(15) Uani 1 1 d . . . H30 H 1.2010 0.8959 0.1751 0.042 Uiso 1 1 calc R . . C31 C 1.0436(7) 0.8446(6) 0.1276(5) 0.0387(18) Uani 1 1 d . . . C32 C 1.1030(7) 0.8699(6) 0.0353(5) 0.0369(16) Uani 1 1 d . . . H32 H 1.1913 0.9003 0.0172 0.044 Uiso 1 1 calc R . . C33 C 1.0343(7) 0.8509(6) -0.0268(5) 0.0365(16) Uani 1 1 d . . . H33 H 1.0739 0.8733 -0.0879 0.044 Uiso 1 1 calc R . . C34 C 0.9062(7) 0.7988(6) -0.0031(4) 0.0304(14) Uani 1 1 d . . . C35 C 0.8477(6) 0.7683(5) 0.0863(4) 0.0256(13) Uani 1 1 d . . . C36 C 0.9150(6) 0.7930(5) 0.1525(4) 0.0246(13) Uani 1 1 d . . . C37 C 0.8471(8) 0.7805(7) -0.0790(4) 0.0368(16) Uani 1 1 d . . . H37A H 0.7638 0.7358 -0.0560 0.055 Uiso 1 1 calc R . . H37B H 0.9110 0.7347 -0.1130 0.055 Uiso 1 1 calc R . . H37C H 0.8281 0.8589 -0.1178 0.055 Uiso 1 1 calc R . . N38 N 0.2615(8) 0.3707(7) 0.2146(5) 0.0530(18) Uani 1 1 d . . . C39 C 0.2161(8) 0.4302(8) 0.2594(6) 0.0458(19) Uani 1 1 d . . . C40 C 0.1628(10) 0.5087(10) 0.3161(7) 0.070(3) Uani 1 1 d . . . H40A H 0.2370 0.5451 0.3319 0.105 Uiso 1 1 calc R . . H40B H 0.1083 0.4619 0.3704 0.105 Uiso 1 1 calc R . . H40C H 0.1071 0.5722 0.2846 0.105 Uiso 1 1 calc R . . N41 N 0.750(2) 0.1306(19) 0.3488(13) 0.130(7) Uiso 0.701(15) 1 d P . . C42 C 0.8604(18) 0.1290(15) 0.3424(11) 0.074(5) Uiso 0.701(15) 1 d P . . C43 C 0.9910(18) 0.1288(16) 0.3394(11) 0.083(5) Uiso 0.701(15) 1 d P . . H43A H 1.0299 0.1962 0.2914 0.124 Uiso 0.701(15) 1 calc PR . . H43B H 1.0303 0.0528 0.3284 0.124 Uiso 0.701(15) 1 calc PR . . H43C H 1.0102 0.1372 0.3963 0.124 Uiso 0.701(15) 1 calc PR . . O44 O 0.2521(13) 0.6761(11) 0.4951(8) 0.105(5) Uiso 0.786(19) 1 d P . . C45 C 0.103(3) 0.689(2) 0.5025(16) 0.150(10) Uiso 0.786(19) 1 d P . . H45A H 0.0717 0.7578 0.5273 0.225 Uiso 0.786(19) 1 calc PR . . H45B H 0.0610 0.6155 0.5417 0.225 Uiso 0.786(19) 1 calc PR . . H45C H 0.0782 0.7023 0.4434 0.225 Uiso 0.786(19) 1 calc PR . . 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 0.03111(15) 0.02178(14) 0.02518(14) -0.00488(9) -0.00460(9) -0.00350(9) P2 0.0256(8) 0.0203(8) 0.0264(8) -0.0070(6) -0.0039(6) -0.0030(6) F3 0.034(2) 0.032(2) 0.0279(19) -0.0038(16) -0.0003(15) -0.0103(17) F4 0.050(2) 0.0217(19) 0.034(2) -0.0041(16) -0.0086(18) 0.0003(17) C5 0.031(4) 0.025(3) 0.035(3) -0.009(3) -0.007(3) 0.000(3) C6 0.035(4) 0.033(4) 0.040(4) -0.017(3) -0.006(3) 0.001(3) C7 0.036(4) 0.025(3) 0.041(4) -0.009(3) -0.008(3) 0.004(3) C8 0.044(4) 0.021(3) 0.038(4) -0.008(3) -0.005(3) -0.003(3) C9 0.030(4) 0.030(4) 0.035(3) -0.014(3) -0.009(3) 0.003(3) C10 0.026(3) 0.039(4) 0.042(4) -0.016(3) -0.009(3) 0.000(3) C11 0.034(4) 0.031(4) 0.039(4) -0.016(3) -0.010(3) -0.001(3) C12 0.041(4) 0.026(3) 0.033(3) -0.007(3) -0.016(3) 0.001(3) N13 0.030(3) 0.021(3) 0.027(3) -0.002(2) -0.003(2) -0.006(2) C14 0.039(4) 0.033(4) 0.030(3) -0.005(3) -0.003(3) -0.004(3) C15 0.048(4) 0.032(4) 0.028(3) 0.002(3) -0.003(3) -0.009(3) C16 0.067(6) 0.044(5) 0.030(4) -0.006(3) -0.013(4) -0.003(4) C17 0.065(5) 0.029(4) 0.036(4) -0.014(3) -0.012(3) -0.005(4) C18 0.047(4) 0.024(3) 0.032(3) -0.008(3) -0.007(3) -0.005(3) C19 0.027(3) 0.018(3) 0.028(3) -0.008(2) -0.005(2) -0.008(2) C20 0.031(3) 0.023(3) 0.031(3) -0.011(3) 0.000(3) -0.003(3) C21 0.023(3) 0.032(4) 0.035(3) -0.015(3) -0.005(3) 0.001(3) C22 0.036(4) 0.025(3) 0.029(3) -0.009(3) -0.011(3) -0.002(3) C23 0.032(3) 0.026(3) 0.021(3) -0.003(2) -0.005(2) -0.006(3) C24 0.028(3) 0.028(3) 0.022(3) -0.007(2) -0.003(2) -0.001(3) F25 0.030(2) 0.041(2) 0.061(3) -0.021(2) 0.0049(19) 0.0009(18) F26 0.039(2) 0.0240(19) 0.035(2) -0.0031(16) 0.0006(17) -0.0002(16) C27 0.029(3) 0.024(3) 0.025(3) -0.007(2) -0.008(2) 0.002(3) C28 0.034(4) 0.033(4) 0.032(3) -0.005(3) -0.011(3) -0.002(3) C29 0.038(4) 0.033(4) 0.045(4) -0.009(3) -0.019(3) 0.000(3) C30 0.031(4) 0.033(4) 0.044(4) -0.010(3) -0.014(3) 0.001(3) C31 0.034(4) 0.032(4) 0.045(4) 0.011(3) -0.018(3) -0.022(3) C32 0.028(4) 0.032(4) 0.049(4) -0.012(3) 0.001(3) -0.003(3) C33 0.037(4) 0.032(4) 0.035(4) -0.004(3) 0.003(3) -0.002(3) C34 0.035(4) 0.023(3) 0.032(3) -0.008(3) -0.003(3) -0.003(3) C35 0.028(3) 0.017(3) 0.033(3) -0.008(2) -0.005(3) -0.002(2) C36 0.025(3) 0.017(3) 0.031(3) -0.007(2) -0.004(2) 0.003(2) C37 0.042(4) 0.037(4) 0.031(3) -0.010(3) -0.001(3) -0.005(3) N38 0.062(5) 0.043(4) 0.062(4) -0.020(4) -0.024(4) 0.008(4) C39 0.044(5) 0.041(4) 0.058(5) -0.017(4) -0.019(4) 0.005(4) C40 0.060(6) 0.078(7) 0.092(7) -0.055(6) -0.023(5) 0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C27 2.006(6) . ? Pt1 C19 2.029(6) . ? Pt1 F4 2.043(4) . ? Pt1 F3 2.071(4) . ? Pt1 N13 2.144(5) . ? Pt1 P2 2.3209(16) . ? P2 C35 1.847(6) . ? P2 C5 1.885(7) . ? P2 C9 1.914(7) . ? C5 C8 1.533(9) . ? C5 C6 1.547(9) . ? C5 C7 1.550(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C11 1.535(9) . ? C9 C10 1.539(9) . ? C9 C12 1.545(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N13 C14 1.333(8) . ? N13 C18 1.350(8) . ? C14 C15 1.397(10) . ? C14 H14 0.9500 . ? C15 C16 1.380(11) . ? C15 H15 0.9500 . ? C16 C17 1.367(10) . ? C16 H16 0.9500 . ? C17 C18 1.390(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.399(8) . ? C19 C20 1.405(9) . ? C20 C21 1.390(9) . ? C20 H20 0.9500 . ? C21 F25 1.365(7) . ? C21 C22 1.373(9) . ? C22 C23 1.369(9) . ? C22 H22 0.9500 . ? C23 C24 1.368(9) . ? C23 F26 1.377(7) . ? C24 H24 0.9500 . ? C27 C28 1.386(9) . ? C27 C36 1.432(8) . ? C28 C29 1.387(10) . ? C28 H28 0.9500 . ? C29 C30 1.363(10) . ? C29 H29 0.9500 . ? C30 C31 1.404(10) . ? C30 H30 0.9500 . ? C31 C36 1.415(9) . ? C31 C32 1.435(10) . ? C32 C33 1.366(11) . ? C32 H32 0.9500 . ? C33 C34 1.413(10) . ? C33 H33 0.9500 . ? C34 C35 1.392(9) . ? C34 C37 1.496(9) . ? C35 C36 1.436(9) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? N38 C39 1.127(10) . ? C39 C40 1.445(12) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? N41 C42 1.10(2) . ? C42 C43 1.32(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O44 C45 1.50(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 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 C27 Pt1 C19 91.7(2) . . ? C27 Pt1 F4 91.0(2) . . ? C19 Pt1 F4 170.35(19) . . ? C27 Pt1 F3 174.3(2) . . ? C19 Pt1 F3 92.8(2) . . ? F4 Pt1 F3 84.00(16) . . ? C27 Pt1 N13 96.3(2) . . ? C19 Pt1 N13 86.6(2) . . ? F4 Pt1 N13 83.93(18) . . ? F3 Pt1 N13 80.42(17) . . ? C27 Pt1 P2 82.61(18) . . ? C19 Pt1 P2 93.18(17) . . ? F4 Pt1 P2 96.36(11) . . ? F3 Pt1 P2 100.64(11) . . ? N13 Pt1 P2 178.91(15) . . ? C35 P2 C5 103.7(3) . . ? C35 P2 C9 115.2(3) . . ? C5 P2 C9 111.8(3) . . ? C35 P2 Pt1 101.5(2) . . ? C5 P2 Pt1 110.4(2) . . ? C9 P2 Pt1 113.4(2) . . ? C8 C5 C6 109.8(5) . . ? C8 C5 C7 109.8(6) . . ? C6 C5 C7 105.1(5) . . ? C8 C5 P2 108.5(5) . . ? C6 C5 P2 115.0(5) . . ? C7 C5 P2 108.5(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C11 C9 C10 105.7(6) . . ? C11 C9 C12 109.3(5) . . ? C10 C9 C12 108.7(6) . . ? C11 C9 P2 115.7(5) . . ? C10 C9 P2 108.3(4) . . ? C12 C9 P2 108.9(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 N13 C18 120.0(6) . . ? C14 N13 Pt1 115.8(4) . . ? C18 N13 Pt1 124.2(4) . . ? N13 C14 C15 121.4(7) . . ? N13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 118.8(6) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 119.4(7) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 119.9(7) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? N13 C18 C17 120.5(6) . . ? N13 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C24 C19 C20 118.0(6) . . ? C24 C19 Pt1 125.8(5) . . ? C20 C19 Pt1 115.7(4) . . ? C21 C20 C19 118.8(6) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? F25 C21 C22 118.1(6) . . ? F25 C21 C20 117.4(6) . . ? C22 C21 C20 124.5(6) . . ? C23 C22 C21 114.1(6) . . ? C23 C22 H22 123.0 . . ? C21 C22 H22 123.0 . . ? C24 C23 C22 125.7(6) . . ? C24 C23 F26 117.3(6) . . ? C22 C23 F26 117.0(6) . . ? C23 C24 C19 118.9(6) . . ? C23 C24 H24 120.5 . . ? C19 C24 H24 120.5 . . ? C28 C27 C36 118.5(6) . . ? C28 C27 Pt1 120.8(5) . . ? C36 C27 Pt1 120.7(5) . . ? C27 C28 C29 121.3(6) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 121.5(7) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C29 C30 C31 119.1(7) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C30 C31 C36 120.8(7) . . ? C30 C31 C32 121.3(6) . . ? C36 C31 C32 117.7(6) . . ? C33 C32 C31 120.9(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C34 122.0(6) . . ? C32 C33 H33 119.0 . . ? C34 C33 H33 119.0 . . ? C35 C34 C33 118.7(6) . . ? C35 C34 C37 126.3(6) . . ? C33 C34 C37 115.0(6) . . ? C34 C35 C36 120.4(6) . . ? C34 C35 P2 129.0(5) . . ? C36 C35 P2 109.9(4) . . ? C31 C36 C27 118.6(6) . . ? C31 C36 C35 120.2(6) . . ? C27 C36 C35 121.2(6) . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N38 C39 C40 177.8(10) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N41 C42 C43 177(2) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O44 C45 H45A 109.5 . . ? O44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.603 _refine_diff_density_min -1.817 _refine_diff_density_rms 0.186 data_ar83 _database_code_depnum_ccdc_archive 'CCDC 922516' #TrackingRef 'ar83.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 F2 N P Pt' _chemical_formula_sum 'C27 H30 F2 N P Pt' _chemical_formula_weight 632.58 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.4339(2) _cell_length_b 8.35340(10) _cell_length_c 17.3846(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.5476(6) _cell_angle_gamma 90.00 _cell_volume 2365.86(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5157 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 6.029 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2267 _exptl_absorpt_correction_T_max 0.3784 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17473 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5598 _reflns_number_gt 4744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution DIRDIF-96 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+2.6280P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5598 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.039231(8) 0.199826(16) 0.152762(8) 0.01726(6) Uani 1 1 d . . . P2 P -0.01979(6) 0.27689(11) 0.26083(6) 0.0173(2) Uani 1 1 d . . . C3 C -0.0191(2) 0.5029(5) 0.2768(2) 0.0234(8) Uani 1 1 d . . . C4 C -0.0857(3) 0.5729(5) 0.3202(3) 0.0281(9) Uani 1 1 d . . . H4A H -0.0807 0.5276 0.3727 0.042 Uiso 1 1 calc R . . H4B H -0.1399 0.5466 0.2924 0.042 Uiso 1 1 calc R . . H4C H -0.0795 0.6894 0.3235 0.042 Uiso 1 1 calc R . . C5 C 0.0660(3) 0.5457(5) 0.3173(3) 0.0311(10) Uani 1 1 d . . . H5A H 0.0718 0.6624 0.3201 0.047 Uiso 1 1 calc R . . H5B H 0.1077 0.5013 0.2879 0.047 Uiso 1 1 calc R . . H5C H 0.0733 0.5010 0.3699 0.047 Uiso 1 1 calc R . . C6 C -0.0298(3) 0.5802(5) 0.1959(2) 0.0322(10) Uani 1 1 d . . . H6A H -0.0237 0.6966 0.2012 0.048 Uiso 1 1 calc R . . H6B H -0.0846 0.5552 0.1691 0.048 Uiso 1 1 calc R . . H6C H 0.0120 0.5383 0.1659 0.048 Uiso 1 1 calc R . . C7 C -0.1247(2) 0.1851(4) 0.2600(2) 0.0203(8) Uani 1 1 d . . . C8 C -0.1659(3) 0.1979(5) 0.3338(3) 0.0297(10) Uani 1 1 d . . . H8A H -0.1747 0.3109 0.3454 0.045 Uiso 1 1 calc R . . H8B H -0.1305 0.1489 0.3772 0.045 Uiso 1 1 calc R . . H8C H -0.2188 0.1421 0.3261 0.045 Uiso 1 1 calc R . . C9 C -0.1126(3) 0.0070(5) 0.2437(3) 0.0283(9) Uani 1 1 d . . . H9A H -0.1661 -0.0469 0.2368 0.042 Uiso 1 1 calc R . . H9B H -0.0775 -0.0413 0.2875 0.042 Uiso 1 1 calc R . . H9C H -0.0866 -0.0047 0.1964 0.042 Uiso 1 1 calc R . . C10 C -0.1817(2) 0.2579(6) 0.1912(3) 0.0272(9) Uani 1 1 d . . . H10A H -0.1581 0.2398 0.1430 0.041 Uiso 1 1 calc R . . H10B H -0.1874 0.3731 0.1995 0.041 Uiso 1 1 calc R . . H10C H -0.2358 0.2069 0.1875 0.041 Uiso 1 1 calc R . . C11 C 0.1120(2) 0.0721(4) 0.2286(2) 0.0191(8) Uani 1 1 d . . . C12 C 0.1713(2) -0.0231(4) 0.2000(2) 0.0193(8) Uani 1 1 d . . . C13 C 0.2219(2) -0.1255(5) 0.2501(2) 0.0238(8) Uani 1 1 d . . . H13 H 0.2610 -0.1915 0.2296 0.029 Uiso 1 1 calc R . . C14 C 0.2155(2) -0.1309(5) 0.3274(2) 0.0236(8) Uani 1 1 d . . . H14 H 0.2498 -0.2011 0.3603 0.028 Uiso 1 1 calc R . . C15 C 0.1579(2) -0.0322(4) 0.3591(2) 0.0208(8) Uani 1 1 d . . . C16 C 0.1513(2) -0.0285(5) 0.4393(2) 0.0246(8) Uani 1 1 d . . . H16 H 0.1838 -0.0992 0.4734 0.030 Uiso 1 1 calc R . . C17 C 0.0990(2) 0.0752(5) 0.4683(2) 0.0258(9) Uani 1 1 d . . . H17 H 0.0978 0.0781 0.5228 0.031 Uiso 1 1 calc R . . C18 C 0.0462(2) 0.1794(4) 0.4200(2) 0.0201(8) Uani 1 1 d . . . C19 C 0.0472(2) 0.1733(5) 0.3401(2) 0.0204(8) Uani 1 1 d . . . C20 C 0.1048(2) 0.0701(4) 0.3089(2) 0.0181(7) Uani 1 1 d . . . C21 C -0.0030(3) 0.2927(5) 0.4631(2) 0.0253(9) Uani 1 1 d . . . H21A H 0.0318 0.3824 0.4834 0.038 Uiso 1 1 calc R . . H21B H -0.0232 0.2360 0.5062 0.038 Uiso 1 1 calc R . . H21C H -0.0498 0.3335 0.4277 0.038 Uiso 1 1 calc R . . C22 C 0.1766(2) 0.0000(5) 0.1170(2) 0.0206(8) Uani 1 1 d . . . C23 C 0.2390(2) -0.0674(5) 0.0794(2) 0.0250(9) Uani 1 1 d . . . H23 H 0.2775 -0.1408 0.1053 0.030 Uiso 1 1 calc R . . C24 C 0.2425(3) -0.0232(5) 0.0034(3) 0.0289(9) Uani 1 1 d . . . C25 C 0.1878(3) 0.0818(6) -0.0364(2) 0.0299(9) Uani 1 1 d . . . H25 H 0.1921 0.1122 -0.0884 0.036 Uiso 1 1 calc R . . C26 C 0.1259(2) 0.1416(5) 0.0031(2) 0.0246(8) Uani 1 1 d . . . C27 C 0.1171(2) 0.1074(5) 0.0797(2) 0.0206(8) Uani 1 1 d . . . F28 F 0.30399(15) -0.0841(4) -0.03388(16) 0.0410(7) Uani 1 1 d . . . F29 F 0.07392(17) 0.2465(4) -0.03861(15) 0.0353(6) Uani 1 1 d . . . N30 N -0.0387(2) 0.3089(4) 0.0643(2) 0.0236(7) Uani 1 1 d . . . C31 C -0.0797(2) 0.3567(5) 0.0120(2) 0.0229(8) Uani 1 1 d . . . C32 C -0.1321(3) 0.4167(6) -0.0563(3) 0.0317(10) Uani 1 1 d . . . H32A H -0.1150 0.5254 -0.0681 0.047 Uiso 1 1 calc R . . H32B H -0.1893 0.4184 -0.0459 0.047 Uiso 1 1 calc R . . H32C H -0.1272 0.3466 -0.1006 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01655(9) 0.01734(9) 0.01777(9) 0.00102(5) 0.00179(6) 0.00196(5) P2 0.0157(4) 0.0174(5) 0.0188(5) 0.0014(4) 0.0027(4) 0.0012(4) C3 0.0269(19) 0.0207(19) 0.0233(19) -0.0011(16) 0.0060(16) 0.0019(17) C4 0.034(2) 0.0188(19) 0.033(2) 0.0001(17) 0.0101(18) 0.0046(17) C5 0.030(2) 0.020(2) 0.043(3) -0.0007(18) 0.0040(19) -0.0053(17) C6 0.049(3) 0.020(2) 0.029(2) 0.0041(18) 0.012(2) 0.007(2) C7 0.0167(18) 0.0216(19) 0.023(2) 0.0012(15) 0.0048(15) -0.0006(15) C8 0.025(2) 0.037(2) 0.029(2) -0.0042(18) 0.0074(18) -0.0057(18) C9 0.029(2) 0.0216(19) 0.035(2) -0.0019(18) 0.0057(18) -0.0066(18) C10 0.0177(19) 0.033(2) 0.030(2) -0.0008(19) 0.0002(17) -0.0016(18) C11 0.0169(17) 0.0147(17) 0.0252(19) 0.0000(15) 0.0008(15) -0.0020(14) C12 0.0172(17) 0.0172(18) 0.0236(19) -0.0024(15) 0.0027(15) -0.0016(15) C13 0.0173(17) 0.022(2) 0.032(2) -0.0015(17) 0.0032(16) 0.0024(16) C14 0.0193(18) 0.0204(19) 0.029(2) 0.0046(16) -0.0032(16) 0.0016(16) C15 0.0179(17) 0.0172(18) 0.026(2) 0.0018(15) -0.0021(15) -0.0049(15) C16 0.0238(19) 0.025(2) 0.023(2) 0.0051(16) -0.0011(16) 0.0018(17) C17 0.029(2) 0.031(2) 0.0180(19) 0.0034(17) 0.0036(16) -0.0021(18) C18 0.0211(19) 0.0178(18) 0.0218(19) 0.0001(15) 0.0045(15) -0.0038(15) C19 0.0201(19) 0.0184(18) 0.0223(19) 0.0014(15) 0.0010(15) -0.0011(15) C20 0.0170(16) 0.0158(17) 0.0211(18) 0.0000(14) 0.0008(14) -0.0012(14) C21 0.033(2) 0.025(2) 0.0189(19) -0.0011(16) 0.0081(17) 0.0001(17) C22 0.0180(17) 0.0176(18) 0.026(2) -0.0042(16) 0.0023(15) -0.0026(15) C23 0.0195(18) 0.025(2) 0.031(2) -0.0026(17) 0.0054(16) 0.0041(16) C24 0.023(2) 0.034(2) 0.030(2) -0.0074(19) 0.0087(17) 0.0008(18) C25 0.030(2) 0.040(2) 0.021(2) -0.0036(19) 0.0082(17) -0.002(2) C26 0.0229(19) 0.031(2) 0.0200(19) -0.0023(17) 0.0024(16) -0.0004(17) C27 0.0202(17) 0.0204(18) 0.0210(18) -0.0047(16) 0.0016(14) -0.0008(16) F28 0.0308(13) 0.0585(18) 0.0369(15) -0.0032(14) 0.0165(11) 0.0112(13) F29 0.0385(15) 0.0457(14) 0.0223(13) 0.0090(12) 0.0069(11) 0.0122(13) N30 0.0202(16) 0.0278(18) 0.0229(18) 0.0006(14) 0.0034(14) 0.0041(14) C31 0.0215(19) 0.0230(19) 0.025(2) 0.0030(16) 0.0042(16) 0.0003(16) C32 0.026(2) 0.033(2) 0.034(2) 0.010(2) -0.0055(18) -0.0011(19) _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 C11 1.973(4) . ? Pt1 C27 2.067(4) . ? Pt1 N30 2.078(3) . ? Pt1 P2 2.3159(10) . ? P2 C19 1.860(4) . ? P2 C7 1.885(4) . ? P2 C3 1.908(4) . ? C3 C5 1.524(6) . ? C3 C4 1.525(6) . ? C3 C6 1.537(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.532(5) . ? C7 C8 1.531(6) . ? C7 C10 1.543(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.398(5) . ? C11 C20 1.418(5) . ? C12 C13 1.412(5) . ? C12 C22 1.470(5) . ? C13 C14 1.363(6) . ? C13 H13 0.9500 . ? C14 C15 1.420(6) . ? C14 H14 0.9500 . ? C15 C16 1.413(6) . ? C15 C20 1.432(5) . ? C16 C17 1.363(6) . ? C16 H16 0.9500 . ? C17 C18 1.423(6) . ? C17 H17 0.9500 . ? C18 C19 1.393(6) . ? C18 C21 1.507(6) . ? C19 C20 1.438(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.404(5) . ? C22 C27 1.419(5) . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 F28 1.369(5) . ? C24 C25 1.376(6) . ? C25 C26 1.394(6) . ? C25 H25 0.9500 . ? C26 F29 1.364(5) . ? C26 C27 1.387(6) . ? N30 C31 1.131(5) . ? C31 C32 1.461(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 C11 Pt1 C27 80.70(16) . . ? C11 Pt1 N30 172.85(14) . . ? C27 Pt1 N30 94.60(14) . . ? C11 Pt1 P2 83.70(12) . . ? C27 Pt1 P2 163.98(11) . . ? N30 Pt1 P2 101.27(10) . . ? C19 P2 C7 105.55(18) . . ? C19 P2 C3 111.15(18) . . ? C7 P2 C3 113.03(18) . . ? C19 P2 Pt1 101.62(13) . . ? C7 P2 Pt1 111.14(13) . . ? C3 P2 Pt1 113.47(13) . . ? C5 C3 C4 110.9(3) . . ? C5 C3 C6 108.1(4) . . ? C4 C3 C6 106.8(3) . . ? C5 C3 P2 106.7(3) . . ? C4 C3 P2 117.4(3) . . ? C6 C3 P2 106.6(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 107.7(3) . . ? C9 C7 C10 108.6(3) . . ? C8 C7 C10 109.4(3) . . ? C9 C7 P2 104.8(3) . . ? C8 C7 P2 118.0(3) . . ? C10 C7 P2 107.9(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C20 119.8(3) . . ? C12 C11 Pt1 117.4(3) . . ? C20 C11 Pt1 122.9(3) . . ? C11 C12 C13 120.5(4) . . ? C11 C12 C22 114.1(3) . . ? C13 C12 C22 125.3(3) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 122.4(4) . . ? C16 C15 C20 117.9(4) . . ? C14 C15 C20 119.7(4) . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 122.4(4) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 C21 126.6(4) . . ? C17 C18 C21 114.6(4) . . ? C18 C19 C20 119.5(3) . . ? C18 C19 P2 129.7(3) . . ? C20 C19 P2 110.8(3) . . ? C11 C20 C15 118.9(3) . . ? C11 C20 C19 120.6(3) . . ? C15 C20 C19 120.5(3) . . ? 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 . . ? C23 C22 C27 122.9(4) . . ? C23 C22 C12 123.1(4) . . ? C27 C22 C12 113.9(3) . . ? C24 C23 C22 117.5(4) . . ? C24 C23 H23 121.2 . . ? C22 C23 H23 121.2 . . ? F28 C24 C23 118.7(4) . . ? F28 C24 C25 118.2(4) . . ? C23 C24 C25 123.2(4) . . ? C24 C25 C26 116.8(4) . . ? C24 C25 H25 121.6 . . ? C26 C25 H25 121.6 . . ? F29 C26 C27 120.4(4) . . ? F29 C26 C25 114.5(4) . . ? C27 C26 C25 125.1(4) . . ? C26 C27 C22 114.6(4) . . ? C26 C27 Pt1 131.6(3) . . ? C22 C27 Pt1 113.6(3) . . ? C31 N30 Pt1 173.7(3) . . ? N30 C31 C32 179.1(5) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.160 _refine_diff_density_min -1.465 _refine_diff_density_rms 0.152 data_ar84 _database_code_depnum_ccdc_archive 'CCDC 922517' #TrackingRef 'ar84.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N O P Pt' _chemical_formula_sum 'C28 H34 N O P Pt' _chemical_formula_weight 626.62 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.0579(4) _cell_length_b 7.3176(2) _cell_length_c 19.7918(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.2537(9) _cell_angle_gamma 90.00 _cell_volume 2420.50(10) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5570 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.89 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 5.884 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3209 _exptl_absorpt_correction_T_max 0.5907 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19408 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.89 _reflns_number_total 5742 _reflns_number_gt 4087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5742 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.171996(12) 0.27382(3) 0.519353(12) 0.02477(9) Uani 1 1 d . . . P2 P 0.22499(9) 0.4026(2) 0.43945(8) 0.0244(3) Uani 1 1 d . . . C3 C 0.2386(3) 0.6553(8) 0.4586(3) 0.0279(13) Uani 1 1 d . . . C4 C 0.2913(4) 0.7581(8) 0.4253(4) 0.0347(15) Uani 1 1 d . . . H4A H 0.2649 0.7585 0.3720 0.052 Uiso 1 1 calc R . . H4B H 0.3433 0.6969 0.4395 0.052 Uiso 1 1 calc R . . H4C H 0.2993 0.8842 0.4433 0.052 Uiso 1 1 calc R . . C5 C 0.1567(4) 0.7460(9) 0.4373(4) 0.0365(16) Uani 1 1 d . . . H5A H 0.1635 0.8717 0.4557 0.055 Uiso 1 1 calc R . . H5B H 0.1242 0.6772 0.4585 0.055 Uiso 1 1 calc R . . H5C H 0.1298 0.7473 0.3840 0.055 Uiso 1 1 calc R . . C6 C 0.2813(4) 0.6719(9) 0.5425(3) 0.0362(15) Uani 1 1 d . . . H6A H 0.2858 0.8011 0.5565 0.054 Uiso 1 1 calc R . . H6B H 0.3348 0.6180 0.5579 0.054 Uiso 1 1 calc R . . H6C H 0.2502 0.6070 0.5662 0.054 Uiso 1 1 calc R . . C7 C 0.1706(3) 0.3537(9) 0.3377(3) 0.0283(13) Uani 1 1 d . . . C8 C 0.0818(3) 0.3259(9) 0.3258(3) 0.0346(15) Uani 1 1 d . . . H8A H 0.0507 0.3021 0.2740 0.052 Uiso 1 1 calc R . . H8B H 0.0614 0.4363 0.3409 0.052 Uiso 1 1 calc R . . H8C H 0.0769 0.2217 0.3550 0.052 Uiso 1 1 calc R . . C9 C 0.1730(4) 0.4963(10) 0.2822(3) 0.0392(16) Uani 1 1 d . . . H9A H 0.2288 0.5195 0.2887 0.059 Uiso 1 1 calc R . . H9B H 0.1485 0.6100 0.2897 0.059 Uiso 1 1 calc R . . H9C H 0.1435 0.4507 0.2327 0.059 Uiso 1 1 calc R . . C10 C 0.1997(4) 0.1697(10) 0.3228(4) 0.0374(15) Uani 1 1 d . . . H10A H 0.1676 0.1315 0.2728 0.056 Uiso 1 1 calc R . . H10B H 0.1945 0.0791 0.3572 0.056 Uiso 1 1 calc R . . H10C H 0.2560 0.1794 0.3289 0.056 Uiso 1 1 calc R . . C11 C 0.3283(3) 0.3078(8) 0.4754(3) 0.0241(12) Uani 1 1 d . . . C12 C 0.3890(3) 0.3243(9) 0.4480(3) 0.0305(14) Uani 1 1 d . . . C13 C 0.4648(4) 0.2519(8) 0.4900(4) 0.0337(15) Uani 1 1 d . . . H13 H 0.5063 0.2650 0.4719 0.040 Uiso 1 1 calc R . . C14 C 0.4821(4) 0.1650(9) 0.5544(4) 0.0336(15) Uani 1 1 d . . . H14 H 0.5348 0.1213 0.5806 0.040 Uiso 1 1 calc R . . C15 C 0.4222(3) 0.1391(8) 0.5830(3) 0.0293(14) Uani 1 1 d . . . C16 C 0.4360(3) 0.0442(8) 0.6491(3) 0.0303(14) Uani 1 1 d . . . H16 H 0.4868 -0.0093 0.6747 0.036 Uiso 1 1 calc R . . C17 C 0.3770(3) 0.0284(8) 0.6767(3) 0.0276(13) Uani 1 1 d . . . H17 H 0.3880 -0.0325 0.7218 0.033 Uiso 1 1 calc R . . C18 C 0.3004(3) 0.1018(8) 0.6384(3) 0.0250(13) Uani 1 1 d . . . C19 C 0.2839(3) 0.1936(8) 0.5724(3) 0.0257(13) Uani 1 1 d . . . C20 C 0.3447(3) 0.2147(7) 0.5441(3) 0.0245(12) Uani 1 1 d . . . C21 C 0.3808(4) 0.4109(9) 0.3766(4) 0.0360(15) Uani 1 1 d . . . H21A H 0.3288 0.4721 0.3552 0.054 Uiso 1 1 calc R . . H21B H 0.3847 0.3164 0.3430 0.054 Uiso 1 1 calc R . . H21C H 0.4237 0.5007 0.3849 0.054 Uiso 1 1 calc R . . C22 C 0.2320(3) 0.0902(8) 0.6614(3) 0.0249(13) Uani 1 1 d . . . C23 C 0.2342(3) 0.0158(8) 0.7266(3) 0.0312(14) Uani 1 1 d . . . H23 H 0.2821 -0.0404 0.7585 0.037 Uiso 1 1 calc R . . C24 C 0.1675(4) 0.0214(8) 0.7465(3) 0.0320(14) Uani 1 1 d . . . H24 H 0.1701 -0.0271 0.7919 0.038 Uiso 1 1 calc R . . C25 C 0.0975(4) 0.1000(9) 0.6979(3) 0.0320(14) Uani 1 1 d . . . C26 C 0.0931(4) 0.1709(9) 0.6304(3) 0.0311(14) Uani 1 1 d . . . H26 H 0.0440 0.2205 0.5976 0.037 Uiso 1 1 calc R . . C27 C 0.1598(3) 0.1695(8) 0.6108(3) 0.0292(13) Uani 1 1 d . . . O28 O 0.0274(2) 0.1171(6) 0.7104(2) 0.0381(11) Uani 1 1 d . . . C29 C 0.0297(4) 0.0588(9) 0.7791(3) 0.0348(15) Uani 1 1 d . . . H29A H 0.0455 -0.0701 0.7863 0.052 Uiso 1 1 calc R . . H29B H -0.0234 0.0732 0.7811 0.052 Uiso 1 1 calc R . . H29C H 0.0686 0.1326 0.8176 0.052 Uiso 1 1 calc R . . N30 N 0.0496(3) 0.3210(7) 0.4689(3) 0.0310(12) Uani 1 1 d . . . C31 C -0.0168(4) 0.3207(9) 0.4387(4) 0.0325(14) Uani 1 1 d . . . C32 C -0.1034(4) 0.3195(10) 0.3951(4) 0.0393(16) Uani 1 1 d . . . H32A H -0.1276 0.4315 0.4048 0.059 Uiso 1 1 calc R . . H32B H -0.1279 0.2130 0.4085 0.059 Uiso 1 1 calc R . . H32C H -0.1126 0.3134 0.3431 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02315(14) 0.02989(14) 0.02043(13) 0.00206(10) 0.00730(9) 0.00207(9) P2 0.0264(8) 0.0244(8) 0.0222(8) -0.0008(6) 0.0090(6) -0.0005(6) C3 0.026(3) 0.024(3) 0.031(3) -0.001(3) 0.007(3) 0.003(2) C4 0.031(3) 0.031(4) 0.039(4) 0.000(3) 0.010(3) -0.006(3) C5 0.039(4) 0.041(4) 0.019(3) 0.001(3) 0.000(3) 0.004(3) C6 0.045(4) 0.027(3) 0.031(4) -0.007(3) 0.008(3) -0.003(3) C7 0.031(3) 0.034(3) 0.021(3) -0.001(3) 0.010(3) -0.004(3) C8 0.036(4) 0.042(4) 0.022(3) 0.000(3) 0.006(3) -0.006(3) C9 0.034(4) 0.054(5) 0.027(4) 0.005(3) 0.008(3) -0.007(3) C10 0.045(4) 0.040(4) 0.027(4) -0.011(3) 0.014(3) -0.006(3) C11 0.028(3) 0.021(3) 0.023(3) -0.002(2) 0.010(2) 0.006(2) C12 0.030(3) 0.029(3) 0.031(4) -0.004(3) 0.011(3) -0.001(3) C13 0.029(3) 0.047(4) 0.032(4) -0.005(3) 0.019(3) -0.004(3) C14 0.027(3) 0.033(4) 0.037(4) -0.007(3) 0.008(3) 0.006(3) C15 0.026(3) 0.025(3) 0.032(4) -0.001(3) 0.005(3) -0.002(2) C16 0.021(3) 0.029(3) 0.032(4) -0.004(3) 0.000(3) 0.003(2) C17 0.031(3) 0.025(3) 0.024(3) 0.000(2) 0.007(3) 0.002(2) C18 0.023(3) 0.026(3) 0.025(3) -0.002(2) 0.008(2) 0.002(2) C19 0.029(3) 0.023(3) 0.025(3) -0.001(2) 0.010(2) 0.000(2) C20 0.027(3) 0.019(3) 0.026(3) -0.005(2) 0.007(2) 0.000(2) C21 0.031(3) 0.039(4) 0.039(4) 0.002(3) 0.014(3) -0.003(3) C22 0.029(3) 0.022(3) 0.021(3) 0.002(2) 0.007(2) 0.000(2) C23 0.033(3) 0.028(3) 0.027(3) 0.004(3) 0.005(3) 0.004(3) C24 0.040(4) 0.028(3) 0.025(3) 0.005(3) 0.009(3) -0.001(3) C25 0.034(3) 0.035(4) 0.030(4) -0.004(3) 0.016(3) -0.004(3) C26 0.029(3) 0.039(4) 0.025(3) 0.007(3) 0.010(3) 0.001(3) C27 0.030(3) 0.025(3) 0.032(3) 0.000(3) 0.010(3) 0.000(2) O28 0.037(3) 0.049(3) 0.032(3) 0.011(2) 0.017(2) -0.001(2) C29 0.042(4) 0.038(4) 0.029(4) 0.001(3) 0.018(3) -0.008(3) N30 0.031(3) 0.036(3) 0.027(3) 0.006(2) 0.012(2) 0.003(2) C31 0.032(4) 0.040(4) 0.028(3) -0.007(3) 0.015(3) 0.000(3) C32 0.032(4) 0.048(4) 0.035(4) -0.005(3) 0.009(3) 0.010(3) _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 C19 1.981(6) . ? Pt1 C27 2.051(6) . ? Pt1 N30 2.080(5) . ? Pt1 P2 2.3348(16) . ? P2 C11 1.861(5) . ? P2 C3 1.885(6) . ? P2 C7 1.910(6) . ? C3 C5 1.528(8) . ? C3 C4 1.542(9) . ? C3 C6 1.549(8) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C10 1.515(9) . ? C7 C9 1.528(9) . ? C7 C8 1.543(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.399(8) . ? C11 C20 1.448(8) . ? C12 C13 1.408(9) . ? C12 C21 1.505(9) . ? C13 C14 1.352(9) . ? C13 H13 0.9500 . ? C14 C15 1.411(9) . ? C14 H14 0.9500 . ? C15 C16 1.416(9) . ? C15 C20 1.429(8) . ? C16 C17 1.373(8) . ? C16 H16 0.9500 . ? C17 C18 1.408(8) . ? C17 H17 0.9500 . ? C18 C19 1.397(8) . ? C18 C22 1.472(8) . ? C19 C20 1.416(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.388(8) . ? C22 C27 1.432(8) . ? C23 C24 1.403(8) . ? C23 H23 0.9500 . ? C24 C25 1.390(8) . ? C24 H24 0.9500 . ? C25 O28 1.385(7) . ? C25 C26 1.407(9) . ? C26 C27 1.398(8) . ? C26 H26 0.9500 . ? O28 C29 1.410(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? N30 C31 1.119(7) . ? C31 C32 1.473(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 C19 Pt1 C27 81.5(2) . . ? C19 Pt1 N30 171.3(2) . . ? C27 Pt1 N30 92.1(2) . . ? C19 Pt1 P2 83.14(18) . . ? C27 Pt1 P2 162.99(17) . . ? N30 Pt1 P2 103.95(15) . . ? C11 P2 C3 104.7(3) . . ? C11 P2 C7 112.0(3) . . ? C3 P2 C7 111.8(3) . . ? C11 P2 Pt1 101.51(19) . . ? C3 P2 Pt1 108.4(2) . . ? C7 P2 Pt1 117.30(19) . . ? C5 C3 C4 111.1(5) . . ? C5 C3 C6 107.3(5) . . ? C4 C3 C6 106.4(5) . . ? C5 C3 P2 109.4(4) . . ? C4 C3 P2 116.6(4) . . ? C6 C3 P2 105.4(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 C7 C9 111.1(5) . . ? C10 C7 C8 105.7(5) . . ? C9 C7 C8 107.0(5) . . ? C10 C7 P2 107.1(4) . . ? C9 C7 P2 119.1(4) . . ? C8 C7 P2 106.0(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C20 119.5(5) . . ? C12 C11 P2 129.7(5) . . ? C20 C11 P2 110.7(4) . . ? C11 C12 C13 117.9(6) . . ? C11 C12 C21 126.0(5) . . ? C13 C12 C21 116.1(5) . . ? C14 C13 C12 124.0(6) . . ? C14 C13 H13 118.0 . . ? C12 C13 H13 118.0 . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 122.9(5) . . ? C14 C15 C20 118.4(6) . . ? C16 C15 C20 118.7(6) . . ? C17 C16 C15 121.2(5) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C16 C17 C18 120.3(6) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 120.3(5) . . ? C19 C18 C22 114.2(5) . . ? C17 C18 C22 125.4(5) . . ? C18 C19 C20 119.9(5) . . ? C18 C19 Pt1 116.8(4) . . ? C20 C19 Pt1 123.1(4) . . ? C19 C20 C15 119.5(6) . . ? C19 C20 C11 120.6(5) . . ? C15 C20 C11 119.9(5) . . ? C12 C21 H21A 109.5 . . ? C12 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C12 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 120.4(5) . . ? C23 C22 C18 125.4(5) . . ? C27 C22 C18 114.2(5) . . ? C22 C23 C24 121.7(6) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 118.0(6) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C24 C25 O28 124.5(6) . . ? C24 C25 C26 121.3(6) . . ? O28 C25 C26 114.1(5) . . ? C27 C26 C25 121.0(6) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C22 117.4(6) . . ? C26 C27 Pt1 129.3(4) . . ? C22 C27 Pt1 113.2(4) . . ? C25 O28 C29 116.7(5) . . ? O28 C29 H29A 109.5 . . ? O28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 N30 Pt1 169.9(5) . . ? N30 C31 C32 176.9(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.489 _refine_diff_density_min -2.210 _refine_diff_density_rms 0.189 data_ar87 _database_code_depnum_ccdc_archive 'CCDC 922518' #TrackingRef 'ar87.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H36 N P Pt' _chemical_formula_sum 'C31 H36 N P Pt' _chemical_formula_weight 648.67 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 212121' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0997(8) _cell_length_b 12.1213(7) _cell_length_c 19.4130(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2611.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5979 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 5.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3155 _exptl_absorpt_correction_T_max 0.6633 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ApexDuo diffractometerd' _diffrn_measurement_method '0.5 deg. \f and \w scans' _diffrn_detector_area_resol_mean 1.75 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13059 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0622 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5979 _reflns_number_gt 5614 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2, Bruker-AXS, Inc.' _computing_cell_refinement 'SAINT, Bruker-AXS, Inc.' _computing_data_reduction 'SAINT, Bruker-AXS, Inc.' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(8) _refine_ls_number_reflns 5979 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.849527(16) 0.956599(15) 0.939132(9) 0.01438(6) Uani 1 1 d . . . P P 0.74386(12) 0.85536(11) 0.85705(7) 0.0148(3) Uani 1 1 d . . . C1 C 0.9779(5) 1.0404(5) 0.9937(2) 0.0191(10) Uani 1 1 d . . . C2 C 0.9617(5) 1.1031(4) 1.0535(3) 0.0247(11) Uani 1 1 d . . . H2 H 0.8834 1.1089 1.0730 0.030 Uiso 1 1 calc R . . C3 C 1.0575(7) 1.1570(5) 1.0850(3) 0.0322(15) Uani 1 1 d . . . H3 H 1.0445 1.1983 1.1259 0.039 Uiso 1 1 calc R . . C4 C 1.1718(5) 1.1504(4) 1.0568(3) 0.0303(13) Uani 1 1 d . . . H4 H 1.2365 1.1878 1.0788 0.036 Uiso 1 1 calc R . . C5 C 1.1945(6) 1.0900(5) 0.9968(3) 0.0274(13) Uani 1 1 d . . . C6 C 1.0979(5) 1.0321(5) 0.9656(3) 0.0203(11) Uani 1 1 d . . . C7 C 1.3235(5) 1.0931(6) 0.9701(3) 0.0327(15) Uani 1 1 d . . . H7A H 1.3228 1.1045 0.9201 0.049 Uiso 1 1 calc R . . H7B H 1.3636 1.0231 0.9807 0.049 Uiso 1 1 calc R . . H7C H 1.3672 1.1538 0.9922 0.049 Uiso 1 1 calc R . . C8 C 1.1050(4) 0.9583(5) 0.9042(3) 0.0190(10) Uani 1 1 d . . . C9 C 0.9912(5) 0.9195(4) 0.8823(3) 0.0170(10) Uani 1 1 d . . . C10 C 0.9828(4) 0.8473(4) 0.8248(3) 0.0147(10) Uani 1 1 d . . . C11 C 1.0920(5) 0.8139(5) 0.7903(3) 0.0220(12) Uani 1 1 d . . . C12 C 1.2027(5) 0.8513(5) 0.8151(3) 0.0284(13) Uani 1 1 d . . . H12 H 1.2746 0.8283 0.7928 0.034 Uiso 1 1 calc R . . C13 C 1.2104(5) 0.9204(5) 0.8708(3) 0.0260(13) Uani 1 1 d . . . H13 H 1.2872 0.9430 0.8871 0.031 Uiso 1 1 calc R . . C14 C 0.8685(5) 0.8079(4) 0.8003(3) 0.0189(11) Uani 1 1 d . . . C15 C 0.8638(5) 0.7412(4) 0.7420(3) 0.0209(11) Uani 1 1 d . . . C16 C 0.9723(5) 0.7066(5) 0.7102(3) 0.0235(12) Uani 1 1 d . . . H16 H 0.9683 0.6577 0.6720 0.028 Uiso 1 1 calc R . . C17 C 1.0820(5) 0.7412(5) 0.7328(3) 0.0230(12) Uani 1 1 d . . . H17 H 1.1528 0.7167 0.7100 0.028 Uiso 1 1 calc R . . C18 C 0.7505(6) 0.7067(5) 0.7053(3) 0.0290(13) Uani 1 1 d . . . H18A H 0.7470 0.7426 0.6601 0.044 Uiso 1 1 calc R . . H18B H 0.6802 0.7286 0.7326 0.044 Uiso 1 1 calc R . . H18C H 0.7504 0.6264 0.6992 0.044 Uiso 1 1 calc R . . C19 C 0.6725(5) 0.7286(5) 0.8958(3) 0.0223(12) Uani 1 1 d . . . C20 C 0.6339(6) 0.6334(5) 0.8485(3) 0.0341(14) Uani 1 1 d . . . H20A H 0.5685 0.6582 0.8184 0.051 Uiso 1 1 calc R . . H20B H 0.6059 0.5713 0.8766 0.051 Uiso 1 1 calc R . . H20C H 0.7027 0.6099 0.8205 0.051 Uiso 1 1 calc R . . C21 C 0.7738(5) 0.6819(4) 0.9436(3) 0.0276(12) Uani 1 1 d . . . H21A H 0.8419 0.6574 0.9154 0.041 Uiso 1 1 calc R . . H21B H 0.7423 0.6194 0.9700 0.041 Uiso 1 1 calc R . . H21C H 0.8008 0.7398 0.9753 0.041 Uiso 1 1 calc R . . C22 C 0.5637(5) 0.7629(5) 0.9399(3) 0.0281(12) Uani 1 1 d . . . H22A H 0.4925 0.7703 0.9104 0.042 Uiso 1 1 calc R . . H22B H 0.5806 0.8337 0.9623 0.042 Uiso 1 1 calc R . . H22C H 0.5486 0.7066 0.9751 0.042 Uiso 1 1 calc R . . C23 C 0.6357(5) 0.9415(4) 0.8037(3) 0.0211(11) Uani 1 1 d . . . C24 C 0.7062(6) 0.9903(5) 0.7436(3) 0.0285(13) Uani 1 1 d . . . H24A H 0.7255 0.9319 0.7105 0.043 Uiso 1 1 calc R . . H24B H 0.7810 1.0233 0.7608 0.043 Uiso 1 1 calc R . . H24C H 0.6575 1.0471 0.7209 0.043 Uiso 1 1 calc R . . C25 C 0.5945(5) 1.0376(6) 0.8507(3) 0.0319(13) Uani 1 1 d . . . H25A H 0.6647 1.0814 0.8645 0.048 Uiso 1 1 calc R . . H25B H 0.5550 1.0077 0.8918 0.048 Uiso 1 1 calc R . . H25C H 0.5377 1.0846 0.8256 0.048 Uiso 1 1 calc R . . C26 C 0.5215(5) 0.8869(6) 0.7775(3) 0.0337(15) Uani 1 1 d . . . H26A H 0.4675 0.9431 0.7585 0.051 Uiso 1 1 calc R . . H26B H 0.4812 0.8487 0.8156 0.051 Uiso 1 1 calc R . . H26C H 0.5420 0.8335 0.7414 0.051 Uiso 1 1 calc R . . N27 N 0.7144(4) 0.9948(4) 1.0151(2) 0.0213(10) Uani 1 1 d . . . C28 C 0.6848(5) 0.9221(5) 1.0641(3) 0.0242(11) Uani 1 1 d . . . H28 H 0.7223 0.8516 1.0638 0.029 Uiso 1 1 calc R . . C29 C 0.6008(5) 0.9459(6) 1.1158(3) 0.0261(12) Uani 1 1 d . . . H29 H 0.5791 0.8918 1.1490 0.031 Uiso 1 1 calc R . . C30 C 0.5498(5) 1.0509(6) 1.1175(3) 0.0301(13) Uani 1 1 d . . . H30 H 0.4924 1.0701 1.1518 0.036 Uiso 1 1 calc R . . C31 C 0.5846(5) 1.1259(5) 1.0684(3) 0.0274(12) Uani 1 1 d . . . H31 H 0.5537 1.1990 1.0695 0.033 Uiso 1 1 calc R . . C32 C 0.6643(6) 1.0951(5) 1.0175(3) 0.0247(12) Uani 1 1 d . . . H32 H 0.6845 1.1472 0.9828 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt 0.01472(8) 0.01278(9) 0.01562(8) 0.00052(8) -0.00122(8) -0.00064(8) P 0.0140(6) 0.0146(6) 0.0157(6) 0.0025(5) 0.0005(5) -0.0027(5) C1 0.029(3) 0.009(2) 0.020(2) 0.007(2) -0.006(2) 0.002(2) C2 0.031(3) 0.017(3) 0.026(3) 0.003(2) -0.009(3) 0.004(2) C3 0.051(4) 0.019(3) 0.026(3) -0.004(2) -0.012(3) -0.008(3) C4 0.037(3) 0.021(3) 0.033(3) 0.002(3) -0.018(3) -0.010(2) C5 0.030(3) 0.025(3) 0.027(3) 0.011(2) -0.009(2) -0.008(2) C6 0.022(2) 0.017(3) 0.022(2) 0.012(2) -0.009(2) -0.004(2) C7 0.025(3) 0.038(3) 0.035(3) 0.011(3) -0.018(3) -0.014(3) C8 0.019(2) 0.017(2) 0.020(2) 0.011(2) 0.0007(19) -0.006(2) C9 0.020(2) 0.012(2) 0.019(2) 0.0023(19) 0.004(2) 0.0017(19) C10 0.019(2) 0.012(2) 0.012(2) 0.0078(19) 0.0014(19) 0.0040(19) C11 0.019(3) 0.020(3) 0.027(3) 0.007(2) 0.002(2) 0.005(2) C12 0.017(2) 0.036(3) 0.032(3) 0.004(3) 0.007(2) 0.004(2) C13 0.018(3) 0.033(3) 0.028(3) 0.005(2) -0.001(2) -0.007(2) C14 0.023(3) 0.016(2) 0.018(2) 0.0049(19) -0.004(2) 0.001(2) C15 0.027(3) 0.015(2) 0.020(2) 0.0015(19) 0.001(2) -0.001(2) C16 0.037(3) 0.014(3) 0.019(3) -0.001(2) 0.003(2) 0.004(2) C17 0.025(3) 0.022(3) 0.022(3) -0.001(2) 0.009(2) 0.009(2) C18 0.037(3) 0.028(3) 0.022(3) -0.007(2) 0.000(3) -0.001(3) C19 0.022(3) 0.020(3) 0.025(3) 0.002(2) 0.003(2) -0.006(2) C20 0.045(4) 0.025(3) 0.033(3) -0.003(3) 0.004(3) -0.014(3) C21 0.036(3) 0.017(3) 0.030(3) 0.014(3) 0.000(3) -0.003(2) C22 0.025(3) 0.033(3) 0.027(3) -0.001(3) 0.005(3) -0.008(2) C23 0.021(3) 0.022(3) 0.021(2) 0.005(2) -0.005(2) -0.002(2) C24 0.031(3) 0.021(3) 0.033(3) 0.008(2) 0.002(3) 0.006(2) C25 0.030(3) 0.037(3) 0.029(3) 0.000(3) -0.004(2) 0.015(3) C26 0.021(3) 0.050(4) 0.030(3) 0.003(3) -0.009(2) 0.000(3) N27 0.022(2) 0.020(2) 0.021(2) -0.0008(18) -0.003(2) 0.0024(18) C28 0.028(3) 0.021(3) 0.024(3) 0.000(2) -0.004(2) -0.001(2) C29 0.029(3) 0.029(3) 0.021(3) 0.001(3) 0.001(2) -0.007(3) C30 0.026(3) 0.035(3) 0.030(3) -0.011(3) 0.002(2) -0.002(3) C31 0.028(3) 0.026(3) 0.028(3) -0.008(3) -0.005(3) 0.006(2) C32 0.030(3) 0.021(3) 0.023(3) -0.004(2) -0.003(3) 0.004(3) _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 Pt C9 1.974(5) . ? Pt C1 2.045(5) . ? Pt N27 2.154(5) . ? Pt P 2.3282(13) . ? P C14 1.859(5) . ? P C19 1.886(5) . ? P C23 1.898(5) . ? C1 C2 1.399(8) . ? C1 C6 1.444(7) . ? C2 C3 1.390(8) . ? C3 C4 1.384(9) . ? C4 C5 1.398(9) . ? C5 C6 1.418(8) . ? C5 C7 1.524(9) . ? C6 C8 1.492(8) . ? C8 C13 1.415(8) . ? C8 C9 1.413(7) . ? C9 C10 1.422(7) . ? C10 C11 1.442(7) . ? C10 C14 1.437(7) . ? C11 C12 1.396(8) . ? C11 C17 1.427(8) . ? C12 C13 1.370(9) . ? C14 C15 1.393(7) . ? C15 C16 1.417(8) . ? C15 C18 1.505(8) . ? C16 C17 1.361(8) . ? C19 C20 1.536(8) . ? C19 C22 1.538(8) . ? C19 C21 1.563(8) . ? C23 C26 1.518(8) . ? C23 C24 1.524(8) . ? C23 C25 1.549(8) . ? N27 C32 1.338(7) . ? N27 C28 1.338(8) . ? C28 C29 1.400(8) . ? C29 C30 1.393(9) . ? C30 C31 1.373(9) . ? C31 C32 1.378(8) . ? 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 C9 Pt C1 81.2(2) . . ? C9 Pt N27 170.8(2) . . ? C1 Pt N27 91.35(19) . . ? C9 Pt P 84.17(16) . . ? C1 Pt P 165.26(15) . . ? N27 Pt P 103.37(13) . . ? C14 P C19 107.3(2) . . ? C14 P C23 108.5(2) . . ? C19 P C23 113.6(2) . . ? C14 P Pt 101.16(17) . . ? C19 P Pt 111.59(18) . . ? C23 P Pt 113.70(18) . . ? C2 C1 C6 118.1(5) . . ? C2 C1 Pt 127.6(4) . . ? C6 C1 Pt 114.4(4) . . ? C3 C2 C1 121.5(6) . . ? C4 C3 C2 120.1(6) . . ? C3 C4 C5 121.6(5) . . ? C4 C5 C6 118.7(6) . . ? C4 C5 C7 116.1(5) . . ? C6 C5 C7 125.2(6) . . ? C5 C6 C1 120.1(5) . . ? C5 C6 C8 126.8(5) . . ? C1 C6 C8 113.1(4) . . ? C13 C8 C9 119.5(5) . . ? C13 C8 C6 127.2(5) . . ? C9 C8 C6 113.2(4) . . ? C8 C9 C10 120.0(5) . . ? C8 C9 Pt 117.9(4) . . ? C10 C9 Pt 121.8(4) . . ? C9 C10 C11 118.8(5) . . ? C9 C10 C14 121.4(5) . . ? C11 C10 C14 119.8(5) . . ? C12 C11 C17 122.6(5) . . ? C12 C11 C10 119.3(5) . . ? C17 C11 C10 118.1(5) . . ? C13 C12 C11 121.7(5) . . ? C12 C13 C8 120.5(5) . . ? C15 C14 C10 119.6(5) . . ? C15 C14 P 129.3(4) . . ? C10 C14 P 111.1(4) . . ? C14 C15 C16 119.7(5) . . ? C14 C15 C18 125.3(5) . . ? C16 C15 C18 114.9(5) . . ? C17 C16 C15 121.9(5) . . ? C16 C17 C11 120.8(5) . . ? C20 C19 C22 108.5(5) . . ? C20 C19 C21 106.5(5) . . ? C22 C19 C21 109.4(5) . . ? C20 C19 P 119.4(4) . . ? C22 C19 P 109.4(4) . . ? C21 C19 P 103.2(3) . . ? C26 C23 C24 110.0(5) . . ? C26 C23 C25 106.2(5) . . ? C24 C23 C25 108.1(5) . . ? C26 C23 P 118.1(4) . . ? C24 C23 P 107.8(4) . . ? C25 C23 P 106.2(3) . . ? C32 N27 C28 118.1(5) . . ? C32 N27 Pt 120.6(4) . . ? C28 N27 Pt 121.1(4) . . ? N27 C28 C29 122.5(6) . . ? C30 C29 C28 118.4(6) . . ? C31 C30 C29 118.3(5) . . ? C30 C31 C32 119.9(6) . . ? N27 C32 C31 122.6(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.082 _refine_diff_density_min -1.257 _refine_diff_density_rms 0.112 data_ar90x _database_code_depnum_ccdc_archive 'CCDC 922519' #TrackingRef 'ar90x.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 F5 N P Pt' _chemical_formula_sum 'C30 H29 F5 N P Pt' _chemical_formula_weight 724.60 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F dd2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 21.6091(9) _cell_length_b 42.7935(14) _cell_length_c 11.5194(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10652.3(6) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6678 _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 28.61 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5664 _exptl_absorpt_coefficient_mu 5.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3462 _exptl_absorpt_correction_T_max 0.6150 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ApexDuo, Bruker-AXS' _diffrn_measurement_method '0.5 deg. \f and \w scans' _diffrn_detector_area_resol_mean 1.75 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36427 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -53 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.61 _reflns_number_total 6678 _reflns_number_gt 6399 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(5) _refine_ls_number_reflns 6678 _refine_ls_number_parameters 348 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.604095(6) 0.282704(3) 0.37694(2) 0.01219(5) Uani 1 1 d . . . P1 P 0.57535(5) 0.32449(2) 0.26806(9) 0.01168(19) Uani 1 1 d . . . F1 F 0.64836(15) 0.20999(7) 0.3213(3) 0.0233(6) Uani 1 1 d . . . F2 F 0.69745(15) 0.16610(6) 0.4557(3) 0.0264(6) Uani 1 1 d . . . F3 F 0.72065(15) 0.17760(7) 0.6850(3) 0.0284(7) Uani 1 1 d . . . F4 F 0.69203(16) 0.23437(8) 0.7766(3) 0.0356(8) Uani 1 1 d . . . F5 F 0.64752(15) 0.27993(7) 0.6411(3) 0.0307(7) Uani 1 1 d . . . C1 C 0.64476(18) 0.24774(11) 0.4741(4) 0.0151(8) Uani 1 1 d . . . C2 C 0.6594(2) 0.21794(10) 0.4344(4) 0.0156(9) Uani 1 1 d . . . C3 C 0.6850(2) 0.19449(10) 0.5008(4) 0.0177(8) Uani 1 1 d . . . C4 C 0.6967(2) 0.20019(10) 0.6170(5) 0.0198(9) Uani 1 1 d . . . C5 C 0.6827(2) 0.22909(12) 0.6620(4) 0.0207(9) Uani 1 1 d . . . C6 C 0.6586(2) 0.25179(11) 0.5907(4) 0.0190(9) Uani 1 1 d . . . C7 C 0.6221(2) 0.31937(9) 0.1396(4) 0.0152(8) Uani 1 1 d . . . C8 C 0.6062(2) 0.33081(10) 0.0280(4) 0.0157(9) Uani 1 1 d . . . C9 C 0.6478(2) 0.32449(11) -0.0664(4) 0.0193(10) Uani 1 1 d . . . C10 C 0.7028(2) 0.30706(10) -0.0431(4) 0.0215(9) Uani 1 1 d . . . H2 H 0.7319 0.3038 -0.1038 0.026 Uiso 1 1 calc R . . C11 C 0.7144(2) 0.29508(11) 0.0644(4) 0.0220(9) Uani 1 1 d . . . H1 H 0.7505 0.2828 0.0767 0.026 Uiso 1 1 calc R . . C12 C 0.6733(2) 0.30071(9) 0.1581(4) 0.0156(8) Uani 1 1 d . . . C13 C 0.6330(3) 0.33454(11) -0.1801(4) 0.0251(11) Uani 1 1 d . . . H3 H 0.6613 0.3311 -0.2418 0.030 Uiso 1 1 calc R . . C14 C 0.5775(3) 0.34940(11) -0.2012(4) 0.0285(12) Uani 1 1 d . . . H10 H 0.5675 0.3563 -0.2773 0.034 Uiso 1 1 calc R . . C15 C 0.5359(2) 0.35423(10) -0.1095(4) 0.0235(10) Uani 1 1 d . . . H9 H 0.4973 0.3639 -0.1260 0.028 Uiso 1 1 calc R . . C16 C 0.5483(2) 0.34568(10) 0.0031(4) 0.0188(9) Uani 1 1 d . . . C17 C 0.5008(2) 0.35229(10) 0.0960(4) 0.0189(9) Uani 1 1 d . . . H4 H 0.4595 0.3527 0.0586 0.023 Uiso 1 1 calc R . . H5 H 0.5087 0.3735 0.1269 0.023 Uiso 1 1 calc R . . C18 C 0.4977(2) 0.32944(10) 0.2000(3) 0.0138(8) Uani 1 1 d . . . C19 C 0.4484(2) 0.34069(11) 0.2860(4) 0.0213(9) Uani 1 1 d . . . H8 H 0.4577 0.3622 0.3097 0.032 Uiso 1 1 calc R . . H7 H 0.4485 0.3271 0.3545 0.032 Uiso 1 1 calc R . . H6 H 0.4076 0.3400 0.2490 0.032 Uiso 1 1 calc R . . C20 C 0.4794(2) 0.29701(10) 0.1528(4) 0.0178(9) Uani 1 1 d . . . H20A H 0.4745 0.2824 0.2176 0.027 Uiso 1 1 calc R . . H20B H 0.5118 0.2894 0.1004 0.027 Uiso 1 1 calc R . . H20C H 0.4402 0.2986 0.1103 0.027 Uiso 1 1 calc R . . C21 C 0.6017(2) 0.36183(10) 0.3405(4) 0.0161(8) Uani 1 1 d . . . C22 C 0.6721(2) 0.36017(12) 0.3530(5) 0.0264(11) Uani 1 1 d . . . H22A H 0.6911 0.3594 0.2758 0.040 Uiso 1 1 calc R . . H22B H 0.6834 0.3413 0.3965 0.040 Uiso 1 1 calc R . . H22C H 0.6869 0.3787 0.3947 0.040 Uiso 1 1 calc R . . C23 C 0.5748(3) 0.36262(12) 0.4636(4) 0.0260(10) Uani 1 1 d . . . H23A H 0.5896 0.3445 0.5073 0.039 Uiso 1 1 calc R . . H23B H 0.5295 0.3621 0.4594 0.039 Uiso 1 1 calc R . . H23C H 0.5880 0.3818 0.5027 0.039 Uiso 1 1 calc R . . C24 C 0.5853(3) 0.39206(11) 0.2771(5) 0.0285(10) Uani 1 1 d . . . H24A H 0.6072 0.4096 0.3132 0.043 Uiso 1 1 calc R . . H24B H 0.5406 0.3956 0.2819 0.043 Uiso 1 1 calc R . . H24C H 0.5976 0.3904 0.1954 0.043 Uiso 1 1 calc R . . C25 C 0.5092(2) 0.29068(11) 0.5752(4) 0.0182(9) Uani 1 1 d . . . H25 H 0.5407 0.3033 0.6087 0.022 Uiso 1 1 calc R . . C26 C 0.4536(2) 0.28780(10) 0.6330(5) 0.0231(9) Uani 1 1 d . . . H26 H 0.4470 0.2984 0.7045 0.028 Uiso 1 1 calc R . . C27 C 0.4076(2) 0.26937(12) 0.5858(5) 0.0235(10) Uani 1 1 d . . . H27 H 0.3688 0.2672 0.6237 0.028 Uiso 1 1 calc R . . C28 C 0.4193(2) 0.25411(11) 0.4814(4) 0.0208(9) Uani 1 1 d . . . H28 H 0.3886 0.2412 0.4467 0.025 Uiso 1 1 calc R . . C29 C 0.4764(2) 0.25800(10) 0.4292(4) 0.0189(8) Uani 1 1 d . . . H29 H 0.4845 0.2471 0.3589 0.023 Uiso 1 1 calc R . . N30 N 0.52085(18) 0.27637(8) 0.4732(3) 0.0145(7) Uani 1 1 d . . . C31 C 0.6825(2) 0.28507(10) 0.2760(4) 0.0158(8) Uani 1 1 d . . . H31A H 0.7147 0.2967 0.3193 0.019 Uiso 1 1 calc R . . H31B H 0.6981 0.2636 0.2633 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01030(7) 0.01033(7) 0.01594(8) 0.00119(6) 0.00055(6) 0.00134(5) P1 0.0111(5) 0.0102(4) 0.0137(4) 0.0006(4) 0.0037(4) 0.0016(4) F1 0.0290(17) 0.0220(14) 0.0188(14) -0.0014(11) -0.0027(12) 0.0049(13) F2 0.0340(17) 0.0153(12) 0.0301(14) -0.0019(11) -0.0025(12) 0.0121(12) F3 0.0321(17) 0.0246(14) 0.0285(15) 0.0077(12) -0.0110(13) 0.0089(12) F4 0.049(2) 0.0349(17) 0.0234(15) -0.0051(13) -0.0202(15) 0.0109(15) F5 0.041(2) 0.0213(13) 0.0300(17) -0.0065(14) -0.0127(15) 0.0100(11) C1 0.009(2) 0.015(2) 0.021(2) 0.0008(16) -0.0038(15) 0.0020(14) C2 0.015(2) 0.014(2) 0.017(2) 0.0013(15) -0.0010(17) 0.0005(15) C3 0.017(2) 0.0124(18) 0.024(2) 0.0009(16) -0.0017(17) 0.0014(15) C4 0.0144(19) 0.0186(19) 0.026(2) 0.0069(19) -0.0045(19) 0.0012(15) C5 0.018(2) 0.026(2) 0.019(2) -0.0016(17) -0.0083(16) 0.0024(18) C6 0.019(2) 0.0143(19) 0.024(2) -0.0040(16) -0.0044(17) 0.0009(17) C7 0.0147(18) 0.0117(16) 0.019(2) -0.0001(17) 0.0049(18) -0.0017(15) C8 0.022(2) 0.0101(18) 0.015(2) -0.0006(15) 0.0066(16) -0.0021(15) C9 0.027(3) 0.0110(19) 0.020(2) -0.0023(16) 0.0099(18) -0.0093(16) C10 0.023(2) 0.017(2) 0.025(2) -0.0079(17) 0.0140(18) -0.0067(17) C11 0.014(2) 0.016(2) 0.036(3) -0.0058(19) 0.0106(19) -0.0010(16) C12 0.0129(19) 0.0101(17) 0.024(2) -0.0033(14) 0.0029(15) -0.0017(14) C13 0.040(3) 0.016(2) 0.019(2) -0.0022(18) 0.013(2) -0.007(2) C14 0.052(4) 0.016(2) 0.017(2) 0.0008(18) 0.005(2) -0.001(2) C15 0.037(3) 0.0150(18) 0.018(2) -0.0013(17) 0.001(2) 0.0027(17) C16 0.030(3) 0.0115(18) 0.015(2) 0.0010(15) 0.0033(18) -0.0005(17) C17 0.022(2) 0.0175(19) 0.017(2) 0.0027(15) 0.0008(16) 0.0053(17) C18 0.0117(19) 0.0158(19) 0.0139(19) 0.0008(14) 0.0023(14) 0.0040(15) C19 0.016(2) 0.026(2) 0.022(2) 0.0001(17) 0.0061(17) 0.0086(17) C20 0.016(2) 0.0172(19) 0.021(2) -0.0002(15) -0.0013(16) 0.0000(16) C21 0.016(2) 0.0109(18) 0.022(2) -0.0017(15) 0.0034(15) -0.0007(15) C22 0.016(2) 0.023(2) 0.040(3) -0.008(2) 0.0010(19) -0.0031(17) C23 0.029(3) 0.026(2) 0.022(2) -0.006(2) 0.0071(19) -0.003(2) C24 0.037(3) 0.014(2) 0.035(3) 0.0017(19) 0.000(2) -0.001(2) C25 0.019(2) 0.017(2) 0.018(2) 0.0016(16) 0.0020(17) 0.0015(17) C26 0.027(2) 0.0212(18) 0.022(2) 0.002(2) 0.007(2) 0.0030(17) C27 0.019(2) 0.022(2) 0.030(2) 0.0082(19) 0.0077(19) 0.0016(19) C28 0.020(2) 0.018(2) 0.025(2) 0.0066(17) 0.0007(18) -0.0042(17) C29 0.024(2) 0.0132(19) 0.020(2) 0.0036(16) 0.0028(18) -0.0002(16) N30 0.0142(17) 0.0134(15) 0.0158(17) 0.0042(13) 0.0024(14) 0.0013(14) C31 0.0062(18) 0.018(2) 0.023(2) -0.0009(15) 0.0062(16) 0.0025(14) _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 C31 2.057(4) . ? Pt1 C1 2.065(4) . ? Pt1 N30 2.130(4) . ? Pt1 P1 2.2710(10) . ? P1 C7 1.806(5) . ? P1 C18 1.865(4) . ? P1 C21 1.890(5) . ? F1 C2 1.367(5) . ? F2 C3 1.348(5) . ? F3 C4 1.347(5) . ? F4 C5 1.355(5) . ? F5 C6 1.358(5) . ? C1 C2 1.391(6) . ? C1 C6 1.387(7) . ? C2 C3 1.377(6) . ? C3 C4 1.384(7) . ? C4 C5 1.375(7) . ? C5 C6 1.374(7) . ? C7 C12 1.381(6) . ? C7 C8 1.418(6) . ? C8 C16 1.431(7) . ? C8 C9 1.436(6) . ? C9 C13 1.415(7) . ? C9 C10 1.429(7) . ? C10 C11 1.364(7) . ? C10 H2 0.9500 . ? C11 C12 1.418(6) . ? C11 H1 0.9500 . ? C12 C31 1.528(6) . ? C13 C14 1.379(9) . ? C13 H3 0.9500 . ? C14 C15 1.402(7) . ? C14 H10 0.9500 . ? C15 C16 1.374(7) . ? C15 H9 0.9500 . ? C16 C17 1.510(6) . ? C17 C18 1.548(6) . ? C17 H4 0.9900 . ? C17 H5 0.9900 . ? C18 C19 1.532(6) . ? C18 C20 1.542(6) . ? C19 H8 0.9800 . ? C19 H7 0.9800 . ? C19 H6 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.530(6) . ? C21 C24 1.527(7) . ? C21 C23 1.533(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N30 1.349(6) . ? C25 C26 1.380(7) . ? C25 H25 0.9500 . ? C26 C27 1.380(8) . ? C26 H26 0.9500 . ? C27 C28 1.391(7) . ? C27 H27 0.9500 . ? C28 C29 1.382(7) . ? C28 H28 0.9500 . ? C29 N30 1.341(6) . ? C29 H29 0.9500 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? 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 C31 Pt1 C1 89.52(17) . . ? C31 Pt1 N30 174.71(16) . . ? C1 Pt1 N30 89.15(15) . . ? C31 Pt1 P1 82.78(12) . . ? C1 Pt1 P1 170.54(12) . . ? N30 Pt1 P1 99.02(10) . . ? C7 P1 C18 100.0(2) . . ? C7 P1 C21 107.2(2) . . ? C18 P1 C21 111.14(19) . . ? C7 P1 Pt1 101.78(14) . . ? C18 P1 Pt1 124.59(13) . . ? C21 P1 Pt1 109.85(16) . . ? C2 C1 C6 112.6(4) . . ? C2 C1 Pt1 125.7(4) . . ? C6 C1 Pt1 121.7(3) . . ? F1 C2 C3 114.7(4) . . ? F1 C2 C1 120.1(4) . . ? C3 C2 C1 125.2(5) . . ? F2 C3 C2 121.5(4) . . ? F2 C3 C4 119.6(4) . . ? C2 C3 C4 118.8(4) . . ? F3 C4 C5 120.7(5) . . ? F3 C4 C3 120.4(4) . . ? C5 C4 C3 118.8(4) . . ? F4 C5 C6 121.4(5) . . ? F4 C5 C4 119.0(4) . . ? C6 C5 C4 119.6(4) . . ? F5 C6 C5 116.0(4) . . ? F5 C6 C1 119.1(4) . . ? C5 C6 C1 124.9(4) . . ? C12 C7 C8 122.3(4) . . ? C12 C7 P1 113.1(3) . . ? C8 C7 P1 124.4(3) . . ? C7 C8 C16 123.2(4) . . ? C7 C8 C9 117.9(4) . . ? C16 C8 C9 118.6(4) . . ? C13 C9 C10 121.3(4) . . ? C13 C9 C8 120.2(5) . . ? C10 C9 C8 118.5(4) . . ? C11 C10 C9 121.3(4) . . ? C11 C10 H2 119.4 . . ? C9 C10 H2 119.4 . . ? C10 C11 C12 120.8(4) . . ? C10 C11 H1 119.6 . . ? C12 C11 H1 119.6 . . ? C7 C12 C11 118.8(4) . . ? C7 C12 C31 119.7(4) . . ? C11 C12 C31 121.4(4) . . ? C14 C13 C9 119.9(5) . . ? C14 C13 H3 120.0 . . ? C9 C13 H3 120.0 . . ? C13 C14 C15 119.5(5) . . ? C13 C14 H10 120.3 . . ? C15 C14 H10 120.3 . . ? C16 C15 C14 123.2(5) . . ? C16 C15 H9 118.4 . . ? C14 C15 H9 118.4 . . ? C15 C16 C8 118.5(4) . . ? C15 C16 C17 119.1(4) . . ? C8 C16 C17 122.4(4) . . ? C16 C17 C18 117.3(4) . . ? C16 C17 H4 108.0 . . ? C18 C17 H4 108.0 . . ? C16 C17 H5 108.0 . . ? C18 C17 H5 108.0 . . ? H4 C17 H5 107.2 . . ? C19 C18 C17 109.4(3) . . ? C19 C18 C20 109.4(4) . . ? C17 C18 C20 107.9(3) . . ? C19 C18 P1 112.9(3) . . ? C17 C18 P1 111.0(3) . . ? C20 C18 P1 106.1(3) . . ? C18 C19 H8 109.5 . . ? C18 C19 H7 109.5 . . ? H8 C19 H7 109.5 . . ? C18 C19 H6 109.5 . . ? H8 C19 H6 109.5 . . ? H7 C19 H6 109.5 . . ? 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 . . ? C22 C21 C24 108.3(4) . . ? C22 C21 C23 106.9(4) . . ? C24 C21 C23 109.6(4) . . ? C22 C21 P1 107.6(3) . . ? C24 C21 P1 115.8(4) . . ? C23 C21 P1 108.2(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N30 C25 C26 122.9(5) . . ? N30 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C27 119.2(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C26 C27 C28 118.6(5) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 118.8(4) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? N30 C29 C28 123.1(4) . . ? N30 C29 H29 118.5 . . ? C28 C29 H29 118.5 . . ? C29 N30 C25 117.5(4) . . ? C29 N30 Pt1 118.9(3) . . ? C25 N30 Pt1 123.6(3) . . ? C12 C31 Pt1 114.7(3) . . ? C12 C31 H31A 108.6 . . ? Pt1 C31 H31A 108.6 . . ? C12 C31 H31B 108.6 . . ? Pt1 C31 H31B 108.6 . . ? H31A C31 H31B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.61 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.829 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.115 data_ar94sq _database_code_depnum_ccdc_archive 'CCDC 922520' #TrackingRef 'ar94sq.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H33 F3 N P Pt' _chemical_formula_sum 'C30 H33 F3 N P Pt' _chemical_formula_weight 690.63 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.5182(11) _cell_length_b 7.8685(6) _cell_length_c 26.5569(9) _cell_angle_alpha 90.00 _cell_angle_beta 116.11(4) _cell_angle_gamma 90.00 _cell_volume 6477(2) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5719 _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 25.10 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 4.416 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3071 _exptl_absorpt_correction_T_max 0.6665 _exptl_absorpt_process_details 'Apex2, Bruker-AXS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ApexKappa, Bruker-AXS' _diffrn_measurement_method '0.5 deg. \f scans' _diffrn_detector_area_resol_mean 1.75 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14734 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5496 _reflns_number_gt 4321 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2, Bruker-AXS' _computing_cell_refinement 'Saint, Bruker-AXS' _computing_data_reduction 'Saint, Bruker-AXS' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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. The crystal contains disordered molecules of the THF solvent, which could not be modeled precisely by discrete atoms. Correspondingly, the solvent contribution to the diffraction pattern was subtracted by the Squeeze procedure using the PLATON software (Spek, 2009). ; _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^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5496 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.121013(8) 0.43881(3) 0.104923(10) 0.02170(10) Uani 1 1 d . . . P1 P 0.10871(6) 0.4070(2) 0.18306(7) 0.0232(4) Uani 1 1 d . . . F1 F 0.06928(13) 0.6048(5) 0.06303(16) 0.0316(10) Uani 1 1 d . . . F2 F 0.10790(15) 0.6414(9) -0.09433(16) 0.0779(19) Uani 1 1 d . . . F3 F 0.24129(14) 0.7385(7) 0.05820(16) 0.0586(15) Uani 1 1 d . . . N1 N 0.08180(17) 0.2458(7) 0.0451(2) 0.0227(13) Uani 1 1 d . . . C1 C 0.1289(2) 0.6253(9) 0.2019(3) 0.0292(17) Uani 1 1 d . . . C2 C 0.0939(3) 0.7600(10) 0.1795(3) 0.045(2) Uani 1 1 d . . . H2A H 0.0764 0.7551 0.2002 0.067 Uiso 1 1 calc R . . H2B H 0.0754 0.7392 0.1396 0.067 Uiso 1 1 calc R . . H2C H 0.1071 0.8726 0.1842 0.067 Uiso 1 1 calc R . . C3 C 0.1579(2) 0.6624(10) 0.2636(3) 0.041(2) Uani 1 1 d . . . H3A H 0.1733 0.7695 0.2668 0.061 Uiso 1 1 calc R . . H3B H 0.1788 0.5699 0.2796 0.061 Uiso 1 1 calc R . . H3C H 0.1402 0.6719 0.2839 0.061 Uiso 1 1 calc R . . C4 C 0.1530(2) 0.2692(8) 0.2261(2) 0.0210(15) Uani 1 1 d . . . C5 C 0.17653(19) 0.2073(9) 0.1975(2) 0.0208(15) Uani 1 1 d . . . C6 C 0.2097(2) 0.0883(8) 0.2232(3) 0.0214(15) Uani 1 1 d . . . C7 C 0.2200(2) 0.0356(9) 0.2787(3) 0.0300(17) Uani 1 1 d . . . H7 H 0.2418 -0.0471 0.2965 0.036 Uiso 1 1 calc R . . C8 C 0.1990(2) 0.1024(10) 0.3059(3) 0.0334(19) Uani 1 1 d . . . H8 H 0.2074 0.0687 0.3437 0.040 Uiso 1 1 calc R . . C9 C 0.1654(2) 0.2189(9) 0.2817(3) 0.0285(17) Uani 1 1 d . . . C10 C 0.1447(3) 0.2869(12) 0.3169(3) 0.045(2) Uani 1 1 d . . . H10A H 0.1251 0.2013 0.3196 0.067 Uiso 1 1 calc R . . H10B H 0.1285 0.3903 0.2996 0.067 Uiso 1 1 calc R . . H10C H 0.1671 0.3135 0.3546 0.067 Uiso 1 1 calc R . . C11 C 0.2314(2) 0.0184(10) 0.1936(3) 0.0329(18) Uani 1 1 d . . . H11 H 0.2522 -0.0689 0.2101 0.039 Uiso 1 1 calc R . . C12 C 0.2224(2) 0.0764(10) 0.1419(3) 0.0325(18) Uani 1 1 d . . . H12 H 0.2369 0.0291 0.1219 0.039 Uiso 1 1 calc R . . C13 C 0.1922(2) 0.2048(10) 0.1173(3) 0.0280(16) Uani 1 1 d . . . H13 H 0.1878 0.2470 0.0817 0.034 Uiso 1 1 calc R . . C14 C 0.1683(2) 0.2734(8) 0.1426(2) 0.0192(14) Uani 1 1 d . . . C15 C 0.0553(2) 0.3479(9) 0.1808(3) 0.0302(17) Uani 1 1 d . . . C16 C 0.0208(2) 0.4165(11) 0.1242(3) 0.042(2) Uani 1 1 d . . . H16A H -0.0077 0.3759 0.1182 0.063 Uiso 1 1 calc R . . H16B H 0.0272 0.3761 0.0937 0.063 Uiso 1 1 calc R . . H16C H 0.0212 0.5410 0.1249 0.063 Uiso 1 1 calc R . . C17 C 0.0461(3) 0.4205(11) 0.2286(3) 0.047(2) Uani 1 1 d . . . H17A H 0.0150 0.4184 0.2173 0.071 Uiso 1 1 calc R . . H17B H 0.0566 0.5378 0.2365 0.071 Uiso 1 1 calc R . . H17C H 0.0610 0.3512 0.2624 0.071 Uiso 1 1 calc R . . C18 C 0.0530(2) 0.1565(10) 0.1800(3) 0.038(2) Uani 1 1 d . . . H18A H 0.0767 0.1113 0.2140 0.056 Uiso 1 1 calc R . . H18B H 0.0556 0.1135 0.1469 0.056 Uiso 1 1 calc R . . H18C H 0.0254 0.1205 0.1785 0.056 Uiso 1 1 calc R . . C19 C 0.1458(2) 0.5316(9) 0.0520(3) 0.0251(16) Uani 1 1 d . . . C20 C 0.1190(2) 0.5492(10) -0.0058(3) 0.0355(19) Uani 1 1 d . . . H20 H 0.0901 0.5084 -0.0216 0.043 Uiso 1 1 calc R . . C21 C 0.1347(3) 0.6245(12) -0.0384(3) 0.045(2) Uani 1 1 d . . . C22 C 0.1759(2) 0.6893(12) -0.0190(3) 0.043(2) Uani 1 1 d . . . H22 H 0.1861 0.7398 -0.0433 0.052 Uiso 1 1 calc R . . C23 C 0.2008(2) 0.6761(11) 0.0372(3) 0.039(2) Uani 1 1 d . . . C24 C 0.1873(2) 0.5978(10) 0.0725(3) 0.0325(18) Uani 1 1 d . . . H24 H 0.2064 0.5883 0.1113 0.039 Uiso 1 1 calc R . . C25 C 0.0443(2) 0.2909(11) 0.0025(3) 0.042(2) Uani 1 1 d . . . H25 H 0.0355 0.4065 -0.0008 0.050 Uiso 1 1 calc R . . C26 C 0.0182(3) 0.1763(13) -0.0363(3) 0.068(3) Uani 1 1 d . . . H26 H -0.0082 0.2125 -0.0660 0.082 Uiso 1 1 calc R . . C27 C 0.0302(3) 0.0120(14) -0.0325(4) 0.074(4) Uani 1 1 d . . . H27 H 0.0126 -0.0675 -0.0599 0.089 Uiso 1 1 calc R . . C28 C 0.0684(3) -0.0405(10) 0.0115(3) 0.047(2) Uani 1 1 d . . . H28 H 0.0775 -0.1558 0.0156 0.057 Uiso 1 1 calc R . . C29 C 0.0928(2) 0.0834(9) 0.0494(3) 0.0291(17) Uani 1 1 d . . . H29 H 0.1189 0.0496 0.0802 0.035 Uiso 1 1 calc R . . C30 C 0.1535(2) 0.6210(9) 0.1650(3) 0.0277(17) Uani 1 1 d . . . H30A H 0.1841 0.5885 0.1875 0.033 Uiso 1 1 calc R . . H30B H 0.1524 0.7331 0.1474 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02453(15) 0.02044(18) 0.02434(14) 0.00450(12) 0.01459(11) 0.00228(13) P1 0.0281(10) 0.0236(12) 0.0252(8) 0.0021(7) 0.0184(8) 0.0015(8) F1 0.039(2) 0.022(3) 0.043(2) 0.0144(18) 0.025(2) 0.0095(18) F2 0.056(3) 0.151(6) 0.023(2) 0.014(3) 0.014(2) -0.036(4) F3 0.042(3) 0.101(5) 0.039(2) 0.014(3) 0.022(2) -0.024(3) N1 0.029(3) 0.017(4) 0.023(3) 0.007(2) 0.013(2) 0.003(2) C1 0.038(4) 0.010(4) 0.048(4) -0.003(3) 0.027(4) -0.001(3) C2 0.058(6) 0.018(5) 0.074(6) -0.002(4) 0.043(5) 0.010(4) C3 0.061(5) 0.029(5) 0.048(4) -0.019(4) 0.038(4) -0.020(4) C4 0.027(4) 0.015(4) 0.024(3) 0.000(3) 0.014(3) -0.003(3) C5 0.021(3) 0.020(4) 0.018(3) 0.003(3) 0.006(3) 0.002(3) C6 0.020(3) 0.018(4) 0.024(3) 0.004(3) 0.008(3) -0.005(3) C7 0.028(4) 0.026(5) 0.028(3) 0.006(3) 0.005(3) 0.002(3) C8 0.033(4) 0.040(5) 0.023(3) 0.007(3) 0.010(3) -0.002(3) C9 0.035(4) 0.027(5) 0.025(3) 0.003(3) 0.015(3) -0.008(3) C10 0.058(5) 0.056(6) 0.030(4) 0.000(4) 0.028(4) -0.003(4) C11 0.025(4) 0.028(5) 0.041(4) 0.002(3) 0.011(3) 0.010(3) C12 0.035(4) 0.035(5) 0.034(4) -0.006(3) 0.021(3) 0.005(4) C13 0.030(4) 0.035(5) 0.022(3) 0.001(3) 0.014(3) 0.003(3) C14 0.029(4) 0.017(4) 0.016(3) 0.001(3) 0.014(3) 0.002(3) C15 0.037(4) 0.023(5) 0.043(4) 0.008(3) 0.028(3) 0.004(3) C16 0.031(4) 0.049(6) 0.056(5) 0.021(4) 0.030(4) 0.010(4) C17 0.047(5) 0.056(6) 0.061(5) 0.000(4) 0.044(4) 0.006(4) C18 0.029(4) 0.052(6) 0.038(4) 0.007(4) 0.021(3) -0.003(4) C19 0.034(4) 0.014(4) 0.031(3) 0.009(3) 0.018(3) 0.011(3) C20 0.031(4) 0.053(6) 0.024(3) 0.003(4) 0.014(3) -0.004(4) C21 0.045(5) 0.070(7) 0.024(4) 0.006(4) 0.018(4) -0.003(4) C22 0.039(5) 0.068(7) 0.030(4) 0.004(4) 0.022(3) -0.018(4) C23 0.034(4) 0.055(6) 0.031(4) 0.008(4) 0.016(3) -0.013(4) C24 0.031(4) 0.043(5) 0.027(3) 0.008(3) 0.016(3) -0.004(3) C25 0.036(5) 0.039(6) 0.038(4) 0.015(4) 0.005(3) -0.008(4) C26 0.060(6) 0.043(7) 0.053(5) 0.028(5) -0.020(4) -0.034(5) C27 0.084(8) 0.052(7) 0.039(5) 0.009(5) -0.015(5) -0.037(6) C28 0.070(6) 0.019(5) 0.041(4) -0.005(4) 0.013(4) -0.008(4) C29 0.033(4) 0.026(5) 0.026(3) 0.007(3) 0.011(3) 0.003(3) C30 0.039(4) 0.020(4) 0.034(4) 0.000(3) 0.025(3) -0.006(3) _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 C14 1.981(8) . ? Pt1 C19 2.073(8) . ? Pt1 C30 2.070(9) . ? Pt1 F1 2.094(7) . ? Pt1 N1 2.184(8) . ? Pt1 P1 2.308(2) . ? P1 C4 1.811(8) . ? P1 C1 1.838(10) . ? P1 C15 1.877(10) . ? F2 C21 1.367(9) . ? F3 C23 1.349(9) . ? N1 C29 1.324(10) . ? N1 C25 1.339(9) . ? C1 C2 1.520(11) . ? C1 C3 1.525(11) . ? C1 C30 1.554(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C9 1.402(10) . ? C4 C5 1.421(9) . ? C5 C6 1.401(10) . ? C5 C14 1.455(10) . ? C6 C11 1.415(10) . ? C6 C7 1.417(10) . ? C7 C8 1.337(10) . ? C7 H7 0.9500 . ? C8 C9 1.393(10) . ? C8 H8 0.9500 . ? C9 C10 1.503(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.348(11) . ? C11 H11 0.9500 . ? C12 C13 1.391(10) . ? C12 H12 0.9500 . ? C13 C14 1.381(9) . ? C13 H13 0.9500 . ? C15 C18 1.507(12) . ? C15 C17 1.547(10) . ? C15 C16 1.546(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.393(11) . ? C19 C20 1.407(10) . ? C20 C21 1.346(10) . ? C20 H20 0.9500 . ? C21 C22 1.378(11) . ? C22 C23 1.362(10) . ? C22 H22 0.9500 . ? C23 C24 1.363(9) . ? C24 H24 0.9500 . ? C25 C26 1.367(12) . ? C25 H25 0.9500 . ? C26 C27 1.348(15) . ? C26 H26 0.9500 . ? C27 C28 1.385(13) . ? C27 H27 0.9500 . ? C28 C29 1.388(11) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? 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 C14 Pt1 C19 94.5(3) . . ? C14 Pt1 C30 91.1(4) . . ? C19 Pt1 C30 91.9(4) . . ? C14 Pt1 F1 177.5(2) . . ? C19 Pt1 F1 86.0(3) . . ? C30 Pt1 F1 91.4(3) . . ? C14 Pt1 N1 91.1(3) . . ? C19 Pt1 N1 93.5(4) . . ? C30 Pt1 N1 174.0(2) . . ? F1 Pt1 N1 86.4(3) . . ? C14 Pt1 P1 85.0(2) . . ? C19 Pt1 P1 160.4(2) . . ? C30 Pt1 P1 68.5(3) . . ? F1 Pt1 P1 95.4(2) . . ? N1 Pt1 P1 106.1(3) . . ? C4 P1 C1 105.9(4) . . ? C4 P1 C15 114.6(4) . . ? C1 P1 C15 119.4(3) . . ? C4 P1 Pt1 101.2(3) . . ? C1 P1 Pt1 86.9(2) . . ? C15 P1 Pt1 124.4(2) . . ? C29 N1 C25 117.6(6) . . ? C29 N1 Pt1 123.1(5) . . ? C25 N1 Pt1 119.3(6) . . ? C2 C1 C3 108.6(6) . . ? C2 C1 C30 109.3(6) . . ? C3 C1 C30 113.5(7) . . ? C2 C1 P1 113.8(6) . . ? C3 C1 P1 117.6(5) . . ? C30 C1 P1 93.2(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C9 C4 C5 118.9(6) . . ? C9 C4 P1 128.1(5) . . ? C5 C4 P1 113.0(5) . . ? C6 C5 C4 120.4(6) . . ? C6 C5 C14 118.9(5) . . ? C4 C5 C14 120.6(6) . . ? C5 C6 C11 120.5(6) . . ? C5 C6 C7 118.7(6) . . ? C11 C6 C7 120.8(7) . . ? C8 C7 C6 120.0(7) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 123.2(7) . . ? C7 C8 H8 118.4 . . ? C9 C8 H8 118.4 . . ? C8 C9 C4 118.7(6) . . ? C8 C9 C10 118.3(6) . . ? C4 C9 C10 123.1(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C6 119.6(7) . . ? C12 C11 H11 120.2 . . ? C6 C11 H11 120.2 . . ? C11 C12 C13 120.8(6) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 122.7(6) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C5 117.0(6) . . ? C13 C14 Pt1 123.2(5) . . ? C5 C14 Pt1 119.6(4) . . ? C18 C15 C17 110.6(6) . . ? C18 C15 C16 108.8(6) . . ? C17 C15 C16 108.7(7) . . ? C18 C15 P1 107.0(5) . . ? C17 C15 P1 115.8(5) . . ? C16 C15 P1 105.7(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 117.4(6) . . ? C24 C19 Pt1 121.8(5) . . ? C20 C19 Pt1 120.3(6) . . ? C21 C20 C19 119.2(7) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 F2 118.0(7) . . ? C20 C21 C22 124.3(7) . . ? F2 C21 C22 117.7(6) . . ? C23 C22 C21 115.6(6) . . ? C23 C22 H22 122.2 . . ? C21 C22 H22 122.2 . . ? F3 C23 C22 117.7(6) . . ? F3 C23 C24 119.1(6) . . ? C22 C23 C24 123.2(7) . . ? C23 C24 C19 120.2(7) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? N1 C25 C26 122.2(9) . . ? N1 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C27 C26 C25 119.9(8) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C28 119.8(8) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 116.8(8) . . ? C27 C28 H28 121.6 . . ? C29 C28 H28 121.6 . . ? N1 C29 C28 123.8(7) . . ? N1 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? C1 C30 Pt1 103.9(5) . . ? C1 C30 H30A 111.0 . . ? Pt1 C30 H30A 111.0 . . ? C1 C30 H30B 111.0 . . ? Pt1 C30 H30B 111.0 . . ? H30A C30 H30B 109.0 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.164 0.250 -0.086 831 256 ' ' 2 0.664 0.750 -0.086 831 256 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.799 _refine_diff_density_min -1.755 _refine_diff_density_rms 0.162