# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year 2010 _journal_volume 46 _journal_page_first 1050 _publ_contact_author_name 'Steven Nolan' _publ_contact_author_email SN17@ST-ANDREWS.AC.UK _publ_section_title ; Unusual Reactivities of N-Heterocyclic Carbenes upon Coordination to the Platinum(II)-Dimethyl Moiety ; loop_ _publ_author_name G.C.Fortman N.M.Scott A.Linden 'Edwin D Stevens' 'Reto Dorta' S.P.Nolan # Attachment 'CCDC-741808-Compound3.cif' data_nol233m _database_code_depnum_ccdc_archive 'CCDC 741808' #TrackingRef 'CCDC-741808-Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pt(IGoofy)2(Me2)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H46 N4 Pt' _chemical_formula_weight 585.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.9482(6) _cell_length_b 9.6101(3) _cell_length_c 17.6283(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.6190(10) _cell_angle_gamma 90.00 _cell_volume 2602.01(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 36720 _cell_measurement_theta_min 2.120 _cell_measurement_theta_max 30.529 _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 5.409 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.329447 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41062 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7606 _reflns_number_gt 6919 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+2.2055P] 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 SHELXL _refine_ls_extinction_coef 0.00068(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7606 _refine_ls_number_parameters 281 _refine_ls_number_restraints 234 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0187 _refine_ls_wR_factor_ref 0.0494 _refine_ls_wR_factor_gt 0.0477 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.276746(4) 0.309874(7) 0.334225(4) 0.01605(3) Uani 1 1 d U . . N1 N 0.15076(12) 0.24129(18) 0.43261(10) 0.0221(3) Uani 1 1 d U . . C1 C 0.16981(13) 0.32349(19) 0.37644(11) 0.0183(3) Uani 1 1 d U . . N2 N 0.09964(11) 0.40892(18) 0.35239(10) 0.0228(3) Uani 1 1 d U . . C2 C 0.06974(15) 0.2752(2) 0.44341(14) 0.0293(4) Uani 1 1 d U . . N3 N 0.34775(11) 0.60380(17) 0.32689(9) 0.0184(3) Uani 1 1 d U . . C3 C 0.03726(15) 0.3805(2) 0.39282(14) 0.0289(4) Uani 1 1 d U . . N4 N 0.35058(11) 0.55705(17) 0.44690(9) 0.0199(3) Uani 1 1 d U . . C4 C 0.21146(16) 0.1318(2) 0.47335(13) 0.0295(4) Uani 1 1 d U . . H4 H 0.2646 0.1399 0.4539 0.028(7) Uiso 1 1 calc R . . C5 C 0.1754(2) -0.0145(3) 0.45161(18) 0.0436(6) Uani 1 1 d U . . H5A H 0.1266 -0.0310 0.4743 0.065 Uiso 1 1 calc R . . H5B H 0.2212 -0.0832 0.4724 0.065 Uiso 1 1 calc R . . H5C H 0.1553 -0.0231 0.3942 0.065 Uiso 1 1 calc R . . C6 C 0.2415(2) 0.1526(3) 0.56255(15) 0.0461(7) Uani 1 1 d U . . H6A H 0.2583 0.2501 0.5742 0.069 Uiso 1 1 calc R . . H6B H 0.2916 0.0924 0.5850 0.069 Uiso 1 1 calc R . . H6C H 0.1939 0.1289 0.5856 0.069 Uiso 1 1 calc R . . C7 C 0.09981(16) 0.5196(2) 0.29372(13) 0.0301(5) Uani 1 1 d U . . H7 H 0.1561 0.5084 0.2795 0.041(8) Uiso 1 1 calc R . . C8 C 0.0299(2) 0.5001(5) 0.21829(19) 0.0684(11) Uani 1 1 d U . . H8A H 0.0362 0.4082 0.1963 0.103 Uiso 1 1 calc R . . H8B H 0.0352 0.5723 0.1806 0.103 Uiso 1 1 calc R . . H8C H -0.0273 0.5069 0.2287 0.103 Uiso 1 1 calc R . . C9 C 0.1033(3) 0.6617(3) 0.3292(2) 0.0650(11) Uani 1 1 d U . . H9A H 0.0510 0.6770 0.3473 0.098 Uiso 1 1 calc R . . H9B H 0.1060 0.7319 0.2896 0.098 Uiso 1 1 calc R . . H9C H 0.1551 0.6694 0.3740 0.098 Uiso 1 1 calc R . . C10 C 0.0280(2) 0.2046(3) 0.4992(2) 0.0516(9) Uani 1 1 d U . . H10A H -0.0298 0.2446 0.4938 0.077 Uiso 1 1 calc R . . H10B H 0.0641 0.2178 0.5533 0.077 Uiso 1 1 calc R . . H10C H 0.0223 0.1049 0.4871 0.077 Uiso 1 1 calc R . . C11 C -0.04875(17) 0.4514(3) 0.37875(19) 0.0455(7) Uani 1 1 d U . . H11A H -0.0792 0.4167 0.4164 0.068 Uiso 1 1 calc R . . H11B H -0.0838 0.4320 0.3250 0.068 Uiso 1 1 calc R . . H11C H -0.0398 0.5520 0.3856 0.068 Uiso 1 1 calc R . . C12 C 0.32800(12) 0.50102(19) 0.37328(10) 0.0169(3) Uani 1 1 d U . . C13 C 0.38227(16) 0.7211(2) 0.37128(13) 0.0258(4) Uani 1 1 d U . . C14 C 0.38341(17) 0.6920(2) 0.44654(13) 0.0276(4) Uani 1 1 d U . . C15 C 0.33029(14) 0.5879(2) 0.24075(11) 0.0225(4) Uani 1 1 d U . . H15 H 0.3074 0.4915 0.2277 0.023(6) Uiso 1 1 calc R . . C16 C 0.41326(16) 0.5993(3) 0.21392(13) 0.0328(5) Uani 1 1 d U . . H16A H 0.4309 0.6971 0.2147 0.049 Uiso 1 1 calc R . . H16B H 0.4025 0.5627 0.1603 0.049 Uiso 1 1 calc R . . H16C H 0.4597 0.5454 0.2495 0.049 Uiso 1 1 calc R . . C17 C 0.25928(18) 0.6875(2) 0.19636(15) 0.0338(5) Uani 1 1 d U . . H17A H 0.2074 0.6765 0.2156 0.051 Uiso 1 1 calc R . . H17B H 0.2444 0.6664 0.1399 0.051 Uiso 1 1 calc R . . H17C H 0.2804 0.7835 0.2051 0.051 Uiso 1 1 calc R . . C18 C 0.33481(14) 0.4812(2) 0.51445(11) 0.0226(4) Uani 1 1 d U . . H18 H 0.3184 0.3839 0.4962 0.025(6) Uiso 1 1 calc R . . C19 C 0.25677(18) 0.5430(3) 0.53777(14) 0.0361(5) Uani 1 1 d U . . H19A H 0.2669 0.6423 0.5493 0.054 Uiso 1 1 calc R . . H19B H 0.2494 0.4950 0.5846 0.054 Uiso 1 1 calc R . . H19C H 0.2040 0.5313 0.4943 0.054 Uiso 1 1 calc R . . C20 C 0.41531(18) 0.4707(3) 0.58386(14) 0.0391(6) Uani 1 1 d U . . H20A H 0.4654 0.4438 0.5650 0.059 Uiso 1 1 calc R . . H20B H 0.4057 0.4005 0.6210 0.059 Uiso 1 1 calc R . . H20C H 0.4267 0.5611 0.6104 0.059 Uiso 1 1 calc R . . C21 C 0.4181(2) 0.8467(3) 0.34044(16) 0.0385(6) Uani 1 1 d U . . H21A H 0.4286 0.9206 0.3802 0.058 Uiso 1 1 calc R . . H21B H 0.3761 0.8792 0.2923 0.058 Uiso 1 1 calc R . . H21C H 0.4729 0.8223 0.3287 0.058 Uiso 1 1 calc R . . C22 C 0.4180(2) 0.7806(3) 0.51792(16) 0.0485(8) Uani 1 1 d U . . H22A H 0.4756 0.7465 0.5471 0.073 Uiso 1 1 calc R . . H22B H 0.3783 0.7761 0.5517 0.073 Uiso 1 1 calc R . . H22C H 0.4228 0.8771 0.5017 0.073 Uiso 1 1 calc R . . C23 C 0.38457(14) 0.2653(2) 0.29210(13) 0.0255(4) Uani 1 1 d U . . H23A H 0.4085 0.1745 0.3121 0.038 Uiso 1 1 calc R . . H23B H 0.4291 0.3372 0.3101 0.038 Uiso 1 1 calc R . . H23C H 0.3666 0.2635 0.2344 0.038 Uiso 1 1 calc R . . C24 C 0.22820(18) 0.1207(3) 0.28116(17) 0.0378(6) Uani 1 1 d U . . H24A H 0.2587 0.0434 0.3133 0.057 Uiso 1 1 calc R . . H24B H 0.2374 0.1158 0.2285 0.057 Uiso 1 1 calc R . . H24C H 0.1658 0.1144 0.2769 0.057 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 0.01560(4) 0.01617(4) 0.01675(4) -0.00136(2) 0.00498(3) -0.00145(2) N1 0.0232(8) 0.0209(8) 0.0242(8) 0.0022(6) 0.0097(7) -0.0007(6) C1 0.0178(9) 0.0186(8) 0.0183(8) -0.0011(6) 0.0043(7) -0.0018(6) N2 0.0211(8) 0.0231(8) 0.0236(8) -0.0001(6) 0.0053(6) 0.0021(6) C2 0.0267(11) 0.0297(10) 0.0369(11) -0.0063(9) 0.0179(9) -0.0079(9) N3 0.0202(8) 0.0184(7) 0.0164(7) 0.0011(5) 0.0046(6) -0.0032(6) C3 0.0212(10) 0.0317(11) 0.0361(11) -0.0073(9) 0.0116(9) -0.0012(8) N4 0.0250(8) 0.0197(7) 0.0151(7) -0.0018(6) 0.0054(6) -0.0027(6) C4 0.0322(12) 0.0259(10) 0.0290(10) 0.0084(8) 0.0059(9) -0.0005(9) C5 0.0519(17) 0.0230(11) 0.0536(16) 0.0073(10) 0.0101(13) -0.0018(11) C6 0.0621(19) 0.0442(14) 0.0278(12) 0.0146(11) 0.0050(12) -0.0066(14) C7 0.0331(12) 0.0280(10) 0.0285(10) 0.0055(8) 0.0069(9) 0.0063(9) C8 0.0502(19) 0.108(3) 0.0360(15) 0.0216(17) -0.0074(13) -0.026(2) C9 0.122(4) 0.0305(13) 0.0538(18) 0.0105(13) 0.043(2) 0.0145(17) C10 0.063(2) 0.0386(15) 0.073(2) 0.0026(13) 0.0518(19) -0.0086(13) C11 0.0243(11) 0.0513(16) 0.0631(18) -0.0079(14) 0.0157(12) 0.0069(11) C12 0.0186(8) 0.0178(8) 0.0154(7) 0.0005(6) 0.0065(6) 0.0002(6) C13 0.0325(11) 0.0187(8) 0.0252(9) -0.0013(7) 0.0058(8) -0.0064(8) C14 0.0381(13) 0.0206(9) 0.0231(9) -0.0051(7) 0.0066(9) -0.0074(8) C15 0.0252(9) 0.0269(10) 0.0147(8) 0.0030(7) 0.0046(7) -0.0035(8) C16 0.0332(12) 0.0441(13) 0.0246(10) 0.0023(9) 0.0138(9) -0.0077(10) C17 0.0354(13) 0.0360(13) 0.0269(11) 0.0131(9) 0.0033(10) -0.0002(9) C18 0.0258(10) 0.0275(9) 0.0148(8) 0.0006(7) 0.0059(7) -0.0018(8) C19 0.0428(14) 0.0421(13) 0.0284(11) -0.0045(10) 0.0184(10) 0.0038(11) C20 0.0367(13) 0.0529(15) 0.0225(10) 0.0079(10) -0.0011(9) -0.0069(11) C21 0.0526(16) 0.0241(10) 0.0380(13) 0.0016(9) 0.0106(12) -0.0155(11) C22 0.078(2) 0.0357(13) 0.0294(12) -0.0137(10) 0.0106(13) -0.0217(14) C23 0.0231(10) 0.0270(10) 0.0294(10) -0.0048(8) 0.0121(8) 0.0015(8) C24 0.0365(13) 0.0307(12) 0.0503(15) -0.0176(11) 0.0185(12) -0.0136(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 C1 2.040(2) . ? Pt1 C12 2.0527(19) . ? Pt1 C23 2.093(2) . ? Pt1 C24 2.095(2) . ? N1 C1 1.363(2) . ? N1 C2 1.394(3) . ? N1 C4 1.478(3) . ? C1 N2 1.360(3) . ? N2 C3 1.398(3) . ? N2 C7 1.484(3) . ? C2 C3 1.356(4) . ? C2 C10 1.491(3) . ? N3 C12 1.372(2) . ? N3 C13 1.398(3) . ? N3 C15 1.476(2) . ? C3 C11 1.491(3) . ? N4 C12 1.361(2) . ? N4 C14 1.399(3) . ? N4 C18 1.474(2) . ? C4 C5 1.528(3) . ? C4 C6 1.528(4) . ? C7 C9 1.497(4) . ? C7 C8 1.499(4) . ? C13 C14 1.351(3) . ? C13 C21 1.498(3) . ? C14 C22 1.496(3) . ? C15 C16 1.524(3) . ? C15 C17 1.528(3) . ? C18 C20 1.520(3) . ? C18 C19 1.532(3) . ? 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 C1 Pt1 C12 96.71(7) . . ? C1 Pt1 C23 171.87(8) . . ? C12 Pt1 C23 90.63(8) . . ? C1 Pt1 C24 88.50(9) . . ? C12 Pt1 C24 172.83(9) . . ? C23 Pt1 C24 84.51(9) . . ? C1 N1 C2 111.08(18) . . ? C1 N1 C4 121.36(18) . . ? C2 N1 C4 127.56(18) . . ? N2 C1 N1 104.52(17) . . ? N2 C1 Pt1 128.55(14) . . ? N1 C1 Pt1 126.82(14) . . ? C1 N2 C3 111.19(18) . . ? C1 N2 C7 119.61(18) . . ? C3 N2 C7 129.10(19) . . ? C3 C2 N1 106.77(19) . . ? C3 C2 C10 127.9(2) . . ? N1 C2 C10 125.3(2) . . ? C12 N3 C13 111.48(16) . . ? C12 N3 C15 121.92(16) . . ? C13 N3 C15 126.57(16) . . ? C2 C3 N2 106.44(19) . . ? C2 C3 C11 128.4(2) . . ? N2 C3 C11 125.1(2) . . ? C12 N4 C14 111.44(16) . . ? C12 N4 C18 121.04(16) . . ? C14 N4 C18 127.41(16) . . ? N1 C4 C5 112.3(2) . . ? N1 C4 C6 112.9(2) . . ? C5 C4 C6 111.8(2) . . ? N2 C7 C9 111.7(2) . . ? N2 C7 C8 112.8(2) . . ? C9 C7 C8 114.8(3) . . ? N4 C12 N3 103.85(16) . . ? N4 C12 Pt1 130.77(13) . . ? N3 C12 Pt1 125.38(13) . . ? C14 C13 N3 106.35(18) . . ? C14 C13 C21 128.1(2) . . ? N3 C13 C21 125.3(2) . . ? C13 C14 N4 106.88(18) . . ? C13 C14 C22 127.8(2) . . ? N4 C14 C22 125.3(2) . . ? N3 C15 C16 111.88(17) . . ? N3 C15 C17 111.75(18) . . ? C16 C15 C17 112.44(18) . . ? N4 C18 C20 113.08(18) . . ? N4 C18 C19 110.64(18) . . ? C20 C18 C19 112.38(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 0.0(2) . . . . ? C4 N1 C1 N2 179.40(18) . . . . ? C2 N1 C1 Pt1 -176.44(15) . . . . ? C4 N1 C1 Pt1 3.0(3) . . . . ? C12 Pt1 C1 N2 68.20(18) . . . . ? C23 Pt1 C1 N2 -137.5(5) . . . . ? C24 Pt1 C1 N2 -106.87(19) . . . . ? C12 Pt1 C1 N1 -116.23(17) . . . . ? C23 Pt1 C1 N1 38.1(6) . . . . ? C24 Pt1 C1 N1 68.70(19) . . . . ? N1 C1 N2 C3 -0.1(2) . . . . ? Pt1 C1 N2 C3 176.20(15) . . . . ? N1 C1 N2 C7 176.56(17) . . . . ? Pt1 C1 N2 C7 -7.1(3) . . . . ? C1 N1 C2 C3 0.2(3) . . . . ? C4 N1 C2 C3 -179.2(2) . . . . ? C1 N1 C2 C10 178.9(2) . . . . ? C4 N1 C2 C10 -0.5(4) . . . . ? N1 C2 C3 N2 -0.3(3) . . . . ? C10 C2 C3 N2 -178.9(3) . . . . ? N1 C2 C3 C11 177.6(2) . . . . ? C10 C2 C3 C11 -1.1(4) . . . . ? C1 N2 C3 C2 0.3(2) . . . . ? C7 N2 C3 C2 -176.0(2) . . . . ? C1 N2 C3 C11 -177.7(2) . . . . ? C7 N2 C3 C11 6.0(4) . . . . ? C1 N1 C4 C5 -112.0(2) . . . . ? C2 N1 C4 C5 67.3(3) . . . . ? C1 N1 C4 C6 120.5(2) . . . . ? C2 N1 C4 C6 -60.2(3) . . . . ? C1 N2 C7 C9 -112.0(3) . . . . ? C3 N2 C7 C9 64.0(3) . . . . ? C1 N2 C7 C8 116.8(3) . . . . ? C3 N2 C7 C8 -67.1(3) . . . . ? C14 N4 C12 N3 0.2(2) . . . . ? C18 N4 C12 N3 176.58(17) . . . . ? C14 N4 C12 Pt1 179.98(16) . . . . ? C18 N4 C12 Pt1 -3.7(3) . . . . ? C13 N3 C12 N4 0.2(2) . . . . ? C15 N3 C12 N4 -177.82(17) . . . . ? C13 N3 C12 Pt1 -179.56(15) . . . . ? C15 N3 C12 Pt1 2.4(3) . . . . ? C1 Pt1 C12 N4 56.33(19) . . . . ? C23 Pt1 C12 N4 -120.16(19) . . . . ? C24 Pt1 C12 N4 -167.3(7) . . . . ? C1 Pt1 C12 N3 -123.95(17) . . . . ? C23 Pt1 C12 N3 59.56(17) . . . . ? C24 Pt1 C12 N3 12.5(8) . . . . ? C12 N3 C13 C14 -0.6(3) . . . . ? C15 N3 C13 C14 177.4(2) . . . . ? C12 N3 C13 C21 174.2(2) . . . . ? C15 N3 C13 C21 -7.9(4) . . . . ? N3 C13 C14 N4 0.7(3) . . . . ? C21 C13 C14 N4 -173.9(3) . . . . ? N3 C13 C14 C22 177.0(3) . . . . ? C21 C13 C14 C22 2.4(5) . . . . ? C12 N4 C14 C13 -0.6(3) . . . . ? C18 N4 C14 C13 -176.7(2) . . . . ? C12 N4 C14 C22 -177.0(3) . . . . ? C18 N4 C14 C22 6.9(4) . . . . ? C12 N3 C15 C16 -120.3(2) . . . . ? C13 N3 C15 C16 62.0(3) . . . . ? C12 N3 C15 C17 112.6(2) . . . . ? C13 N3 C15 C17 -65.1(3) . . . . ? C12 N4 C18 C20 128.3(2) . . . . ? C14 N4 C18 C20 -55.9(3) . . . . ? C12 N4 C18 C19 -104.6(2) . . . . ? C14 N4 C18 C19 71.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.011 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.104 # Attachment 'CCDC-741809-Compound1.cif' data_DT0707 _database_code_depnum_ccdc_archive 'CCDC 741809' #TrackingRef 'CCDC-741809-Compound1.cif' _audit_creation_method SHELXL-97 _audit_creation_date 07-03-06 _chemical_name_systematic ; ? ; _chemical_name_common (MeIMe)2Pt(Me)2 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C16 H30 N4 Pt' _chemical_formula_sum 'C16 H30 N4 Pt' _chemical_formula_weight 473.44 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 64 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 120 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 16 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Pt Pt 4 -1.7033 8.3905 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 14 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 14.8926(2) _cell_length_b 8.1788(1) _cell_length_c 16.1119(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.5403(8) _cell_angle_gamma 90.00 _cell_volume 1799.17(4) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 34346 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 7.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.250 _exptl_absorpt_correction_T_max 0.390 _exptl_special_details ; Solvent used: dichloromethane / diethyl ether Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.527(1) Frames collected: 366 Seconds exposure per frame: 18 Degrees rotation per frame: 2.0 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 50417 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 30.03 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 5253 _reflns_number_gt 4641 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2006)' _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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+5.7916P] 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 5253 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.161 _refine_diff_density_min -2.195 _refine_diff_density_rms 0.211 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 0.180706(11) 0.209733(19) 0.436874(10) 0.01729(7) Uani 1 1 d . . . N2 N 0.3746(3) 0.0309(5) 0.5420(2) 0.0207(7) Uani 1 1 d . . . N5 N 0.2766(3) -0.1190(5) 0.4357(3) 0.0228(7) Uani 1 1 d . . . N11 N 0.1280(3) 0.0504(5) 0.5841(2) 0.0193(7) Uani 1 1 d . . . N14 N 0.1635(3) 0.3031(4) 0.6149(3) 0.0189(7) Uani 1 1 d . . . C1 C 0.2826(3) 0.0319(6) 0.4730(3) 0.0198(8) Uani 1 1 d . . . C3 C 0.4226(3) -0.1169(7) 0.5469(3) 0.0256(9) Uani 1 1 d . . . C4 C 0.3601(4) -0.2124(6) 0.4797(4) 0.0269(10) Uani 1 1 d . . . C6 C 0.4153(4) 0.1708(7) 0.5982(4) 0.0284(10) Uani 1 1 d . . . H61 H 0.4743 0.2067 0.5906 0.043 Uiso 1 1 calc R . . H62 H 0.4322 0.1417 0.6617 0.043 Uiso 1 1 calc R . . H63 H 0.3670 0.2596 0.5807 0.043 Uiso 1 1 calc R . . C7 C 0.5240(4) -0.1485(8) 0.6143(4) 0.0374(13) Uani 1 1 d . . . H71 H 0.5402 -0.2641 0.6120 0.056 Uiso 1 1 calc R . . H72 H 0.5284 -0.1218 0.6751 0.056 Uiso 1 1 calc R . . H73 H 0.5702 -0.0805 0.6001 0.056 Uiso 1 1 calc R . . C8 C 0.3679(5) -0.3854(7) 0.4527(4) 0.0386(13) Uani 1 1 d . . . H81 H 0.4301 -0.4324 0.4944 0.058 Uiso 1 1 calc R . . H82 H 0.3652 -0.3873 0.3909 0.058 Uiso 1 1 calc R . . H83 H 0.3135 -0.4497 0.4551 0.058 Uiso 1 1 calc R . . C9 C 0.1913(4) -0.1742(7) 0.3568(4) 0.0306(11) Uani 1 1 d . . . H91 H 0.1433 -0.0855 0.3356 0.046 Uiso 1 1 calc R . . H92 H 0.1617 -0.2686 0.3737 0.046 Uiso 1 1 calc R . . H93 H 0.2119 -0.2057 0.3084 0.046 Uiso 1 1 calc R . . C10 C 0.1574(3) 0.1851(5) 0.5519(3) 0.0179(8) Uani 1 1 d . . . C12 C 0.1158(3) 0.0821(6) 0.6643(3) 0.0212(8) Uani 1 1 d . . . C13 C 0.1380(3) 0.2419(6) 0.6828(3) 0.0204(8) Uani 1 1 d . . . C15 C 0.1108(4) -0.1076(6) 0.5393(3) 0.0257(9) Uani 1 1 d . . . H151 H 0.0973 -0.0924 0.4751 0.039 Uiso 1 1 calc R . . H152 H 0.0546 -0.1605 0.5451 0.039 Uiso 1 1 calc R . . H153 H 0.1690 -0.1764 0.5675 0.039 Uiso 1 1 calc R . . C16 C 0.0796(4) -0.0433(8) 0.7098(4) 0.0344(12) Uani 1 1 d . . . H161 H 0.0788 0.0023 0.7658 0.052 Uiso 1 1 calc R . . H162 H 0.1229 -0.1387 0.7242 0.052 Uiso 1 1 calc R . . H163 H 0.0131 -0.0762 0.6696 0.052 Uiso 1 1 calc R . . C17 C 0.1379(4) 0.3450(8) 0.7592(3) 0.0314(11) Uani 1 1 d . . . H171 H 0.0864 0.4280 0.7359 0.047 Uiso 1 1 calc R . . H172 H 0.2017 0.3989 0.7887 0.047 Uiso 1 1 calc R . . H173 H 0.1256 0.2759 0.8032 0.047 Uiso 1 1 calc R . . C18 C 0.1867(4) 0.4729(6) 0.6070(3) 0.0266(9) Uani 1 1 d . . . H181 H 0.1266 0.5384 0.5874 0.040 Uiso 1 1 calc R . . H182 H 0.2157 0.4827 0.5623 0.040 Uiso 1 1 calc R . . H183 H 0.2333 0.5125 0.6658 0.040 Uiso 1 1 calc R . . C19 C 0.1968(5) 0.2425(8) 0.3149(4) 0.0346(12) Uani 1 1 d . . . H191 H 0.2459 0.1657 0.3118 0.052 Uiso 1 1 calc R . . H192 H 0.2181 0.3547 0.3115 0.052 Uiso 1 1 calc R . . H193 H 0.1339 0.2223 0.2641 0.052 Uiso 1 1 calc R . . C20 C 0.0728(3) 0.3950(6) 0.3892(3) 0.0255(9) Uani 1 1 d . . . H201 H 0.1038 0.4983 0.3845 0.038 Uiso 1 1 calc R . . H202 H 0.0410 0.4080 0.4316 0.038 Uiso 1 1 calc R . . H203 H 0.0238 0.3644 0.3295 0.038 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 0.01460(10) 0.01906(10) 0.01699(10) 0.00259(5) 0.00501(7) 0.00008(5) N2 0.0167(16) 0.0271(19) 0.0195(16) 0.0013(15) 0.0084(14) 0.0008(15) N5 0.0200(17) 0.0254(19) 0.0243(18) -0.0024(16) 0.0104(15) 0.0026(15) N11 0.0174(16) 0.0180(17) 0.0219(17) 0.0016(14) 0.0074(14) -0.0021(14) N14 0.0193(17) 0.0163(16) 0.0228(18) 0.0017(13) 0.0103(15) 0.0022(13) C1 0.0154(18) 0.027(2) 0.0155(18) 0.0005(16) 0.0046(15) 0.0004(16) C3 0.023(2) 0.033(2) 0.024(2) 0.0068(19) 0.0121(18) 0.0081(19) C4 0.029(2) 0.028(2) 0.030(2) 0.0053(19) 0.018(2) 0.0078(18) C6 0.021(2) 0.031(2) 0.026(2) -0.005(2) 0.0026(19) -0.0011(19) C7 0.026(2) 0.052(4) 0.033(3) 0.010(3) 0.010(2) 0.015(2) C8 0.044(3) 0.030(3) 0.049(3) -0.002(2) 0.025(3) 0.010(2) C9 0.031(3) 0.031(2) 0.029(2) -0.011(2) 0.011(2) -0.003(2) C10 0.0131(18) 0.0157(18) 0.024(2) 0.0006(16) 0.0060(16) -0.0001(14) C12 0.0179(19) 0.025(2) 0.022(2) 0.0061(17) 0.0086(16) 0.0019(16) C13 0.021(2) 0.0203(19) 0.019(2) 0.0015(17) 0.0073(17) 0.0028(17) C15 0.027(2) 0.0158(19) 0.032(2) -0.0007(18) 0.0092(19) -0.0030(17) C16 0.027(2) 0.044(3) 0.031(2) 0.019(2) 0.011(2) -0.003(2) C17 0.030(2) 0.042(3) 0.022(2) -0.002(2) 0.011(2) 0.008(2) C18 0.031(2) 0.0149(19) 0.030(2) 0.0001(18) 0.008(2) -0.0016(18) C19 0.038(3) 0.041(3) 0.026(3) 0.002(2) 0.014(2) 0.000(3) C20 0.0178(19) 0.024(2) 0.029(2) 0.0016(18) 0.0031(17) -0.0015(17) _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 C1 2.013(4) . ? Pt1 C10 2.027(5) . ? Pt1 C19 2.090(6) . ? Pt1 C20 2.117(5) . ? N2 C1 1.377(5) . ? N2 C3 1.390(6) . ? N2 C6 1.435(6) . ? N5 C1 1.360(6) . ? N5 C4 1.388(6) . ? N5 C9 1.464(6) . ? N11 C10 1.363(6) . ? N11 C12 1.399(6) . ? N11 C15 1.451(6) . ? N14 C10 1.376(6) . ? N14 C13 1.387(6) . ? N14 C18 1.449(6) . ? C3 C4 1.359(8) . ? C3 C7 1.488(7) . ? C4 C8 1.498(7) . ? C6 H61 0.9800 . ? C6 H62 0.9800 . ? C6 H63 0.9800 . ? C7 H71 0.9800 . ? C7 H72 0.9800 . ? C7 H73 0.9800 . ? C8 H81 0.9800 . ? C8 H82 0.9800 . ? C8 H83 0.9800 . ? C9 H91 0.9800 . ? C9 H92 0.9800 . ? C9 H93 0.9800 . ? C12 C13 1.352(7) . ? C12 C16 1.482(6) . ? C13 C17 1.493(7) . ? C15 H151 0.9800 . ? C15 H152 0.9800 . ? C15 H153 0.9800 . ? C16 H161 0.9800 . ? C16 H162 0.9800 . ? C16 H163 0.9800 . ? C17 H171 0.9800 . ? C17 H172 0.9800 . ? C17 H173 0.9800 . ? C18 H181 0.9800 . ? C18 H182 0.9800 . ? C18 H183 0.9800 . ? C19 H191 0.9800 . ? C19 H192 0.9800 . ? C19 H193 0.9800 . ? C20 H201 0.9800 . ? C20 H202 0.9800 . ? C20 H203 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 C1 Pt1 C10 92.78(17) . . ? C1 Pt1 C19 90.5(2) . . ? C10 Pt1 C19 176.6(2) . . ? C1 Pt1 C20 175.87(18) . . ? C10 Pt1 C20 91.17(18) . . ? C19 Pt1 C20 85.6(2) . . ? C1 N2 C3 112.0(4) . . ? C1 N2 C6 122.5(4) . . ? C3 N2 C6 125.4(4) . . ? C1 N5 C4 112.7(4) . . ? C1 N5 C9 123.0(4) . . ? C4 N5 C9 124.2(4) . . ? C10 N11 C12 112.4(4) . . ? C10 N11 C15 123.4(4) . . ? C12 N11 C15 124.2(4) . . ? C10 N14 C13 111.7(4) . . ? C10 N14 C18 123.7(4) . . ? C13 N14 C18 124.4(4) . . ? N5 C1 N2 102.7(4) . . ? N5 C1 Pt1 128.2(3) . . ? N2 C1 Pt1 129.0(3) . . ? C4 C3 N2 106.3(4) . . ? C4 C3 C7 130.9(5) . . ? N2 C3 C7 122.8(5) . . ? C3 C4 N5 106.2(4) . . ? C3 C4 C8 131.8(5) . . ? N5 C4 C8 122.0(5) . . ? N2 C6 H61 109.5 . . ? N2 C6 H62 109.5 . . ? H61 C6 H62 109.5 . . ? N2 C6 H63 109.5 . . ? H61 C6 H63 109.5 . . ? H62 C6 H63 109.5 . . ? C3 C7 H71 109.5 . . ? C3 C7 H72 109.5 . . ? H71 C7 H72 109.5 . . ? C3 C7 H73 109.5 . . ? H71 C7 H73 109.5 . . ? H72 C7 H73 109.5 . . ? C4 C8 H81 109.5 . . ? C4 C8 H82 109.5 . . ? H81 C8 H82 109.5 . . ? C4 C8 H83 109.5 . . ? H81 C8 H83 109.5 . . ? H82 C8 H83 109.5 . . ? N5 C9 H91 109.5 . . ? N5 C9 H92 109.5 . . ? H91 C9 H92 109.5 . . ? N5 C9 H93 109.5 . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? N11 C10 N14 102.9(4) . . ? N11 C10 Pt1 128.8(3) . . ? N14 C10 Pt1 128.3(3) . . ? C13 C12 N11 105.8(4) . . ? C13 C12 C16 131.7(5) . . ? N11 C12 C16 122.4(5) . . ? C12 C13 N14 107.2(4) . . ? C12 C13 C17 130.3(5) . . ? N14 C13 C17 122.5(4) . . ? N11 C15 H151 109.5 . . ? N11 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? N11 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? C12 C16 H161 109.5 . . ? C12 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? C12 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C13 C17 H171 109.5 . . ? C13 C17 H172 109.5 . . ? H171 C17 H172 109.5 . . ? C13 C17 H173 109.5 . . ? H171 C17 H173 109.5 . . ? H172 C17 H173 109.5 . . ? N14 C18 H181 109.5 . . ? N14 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? N14 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? Pt1 C19 H191 109.5 . . ? Pt1 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? Pt1 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? Pt1 C20 H201 109.5 . . ? Pt1 C20 H202 109.5 . . ? H201 C20 H202 109.5 . . ? Pt1 C20 H203 109.5 . . ? H201 C20 H203 109.5 . . ? H202 C20 H203 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 N5 C1 N2 0.9(5) . . . . ? C9 N5 C1 N2 -178.3(4) . . . . ? C4 N5 C1 Pt1 -178.1(3) . . . . ? C9 N5 C1 Pt1 2.6(6) . . . . ? C3 N2 C1 N5 -0.6(5) . . . . ? C6 N2 C1 N5 176.9(4) . . . . ? C3 N2 C1 Pt1 178.5(3) . . . . ? C6 N2 C1 Pt1 -4.0(6) . . . . ? C10 Pt1 C1 N5 110.8(4) . . . . ? C19 Pt1 C1 N5 -68.1(4) . . . . ? C10 Pt1 C1 N2 -68.0(4) . . . . ? C19 Pt1 C1 N2 113.0(4) . . . . ? C1 N2 C3 C4 0.0(5) . . . . ? C6 N2 C3 C4 -177.4(4) . . . . ? C1 N2 C3 C7 178.6(4) . . . . ? C6 N2 C3 C7 1.2(7) . . . . ? N2 C3 C4 N5 0.5(5) . . . . ? C7 C3 C4 N5 -177.9(5) . . . . ? N2 C3 C4 C8 -177.4(5) . . . . ? C7 C3 C4 C8 4.2(10) . . . . ? C1 N5 C4 C3 -0.9(6) . . . . ? C9 N5 C4 C3 178.3(4) . . . . ? C1 N5 C4 C8 177.2(5) . . . . ? C9 N5 C4 C8 -3.6(8) . . . . ? C12 N11 C10 N14 0.1(5) . . . . ? C15 N11 C10 N14 179.8(4) . . . . ? C12 N11 C10 Pt1 -177.4(3) . . . . ? C15 N11 C10 Pt1 2.2(6) . . . . ? C13 N14 C10 N11 -0.4(5) . . . . ? C18 N14 C10 N11 -176.0(4) . . . . ? C13 N14 C10 Pt1 177.2(3) . . . . ? C18 N14 C10 Pt1 1.5(6) . . . . ? C1 Pt1 C10 N11 -58.7(4) . . . . ? C20 Pt1 C10 N11 120.1(4) . . . . ? C1 Pt1 C10 N14 124.4(4) . . . . ? C20 Pt1 C10 N14 -56.8(4) . . . . ? C10 N11 C12 C13 0.1(5) . . . . ? C15 N11 C12 C13 -179.5(4) . . . . ? C10 N11 C12 C16 177.0(4) . . . . ? C15 N11 C12 C16 -2.6(7) . . . . ? N11 C12 C13 N14 -0.4(5) . . . . ? C16 C12 C13 N14 -176.8(5) . . . . ? N11 C12 C13 C17 179.7(5) . . . . ? C16 C12 C13 C17 3.3(9) . . . . ? C10 N14 C13 C12 0.5(5) . . . . ? C18 N14 C13 C12 176.1(4) . . . . ? C10 N14 C13 C17 -179.6(4) . . . . ? C18 N14 C13 C17 -4.0(7) . . . . ? # End of CIF ============================================================ # Attachment 'CCDC-741810-Compound2.cif' data_nol189a _database_code_depnum_ccdc_archive 'CCDC 741810' #TrackingRef 'CCDC-741810-Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pt(ICy)2Me2).(CH2Cl2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H56 Cl2 N4 Pt' _chemical_formula_weight 774.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 15.5185(7) _cell_length_b 12.9037(6) _cell_length_c 17.4636(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.3540(10) _cell_angle_gamma 90.00 _cell_volume 3372.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19806 _cell_measurement_theta_min 2.222 _cell_measurement_theta_max 30.533 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 4.347 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.720203 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27974 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 30.53 _reflns_number_total 10221 _reflns_number_gt 8950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.1748P] 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 0.021(5) _refine_ls_number_reflns 10221 _refine_ls_number_parameters 363 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0196 _refine_ls_wR_factor_ref 0.0454 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.96832(3) 0.247626(7) 0.91242(2) 0.01112(2) Uani 1 1 d . . . Cl1 Cl 1.08393(5) -0.02126(6) 1.05721(5) 0.03152(16) Uani 1 1 d . . . N1 N 0.79042(14) 0.18101(16) 0.79200(12) 0.0141(4) Uani 1 1 d . . . C1 C 0.8726(2) 0.2246(2) 0.80642(17) 0.0136(5) Uani 1 1 d . . . Cl2 Cl 0.92782(7) -0.12528(8) 0.95691(6) 0.0501(2) Uani 1 1 d . . . N2 N 0.87549(16) 0.26147(15) 0.73287(14) 0.0162(4) Uani 1 1 d . . . C2 C 0.74271(18) 0.1901(2) 0.71269(16) 0.0195(5) Uani 1 1 d . . . H2 H 0.6839 0.1656 0.6893 0.023 Uiso 1 1 calc R . . N3 N 0.82814(13) 0.40117(16) 0.94248(12) 0.0136(4) Uani 1 1 d . . . C3 C 0.7962(2) 0.24035(19) 0.67567(17) 0.0202(5) Uani 1 1 d . . . H3 H 0.7824 0.2580 0.6210 0.024 Uiso 1 1 calc R . . N4 N 0.86226(15) 0.28629(17) 1.03455(13) 0.0146(4) Uani 1 1 d . . . C4 C 0.75327(17) 0.12943(19) 0.85176(15) 0.0151(5) Uani 1 1 d . . . H4 H 0.7984 0.1334 0.9045 0.018 Uiso 1 1 calc R . . C5 C 0.7345(2) 0.0150(2) 0.83010(18) 0.0228(6) Uani 1 1 d . . . H5A H 0.6946 0.0097 0.7757 0.027 Uiso 1 1 calc R . . H5B H 0.7913 -0.0205 0.8309 0.027 Uiso 1 1 calc R . . C6 C 0.6909(2) -0.0381(2) 0.88838(19) 0.0263(6) Uani 1 1 d . . . H6A H 0.6766 -0.1107 0.8713 0.032 Uiso 1 1 calc R . . H6B H 0.7337 -0.0396 0.9416 0.032 Uiso 1 1 calc R . . C7 C 0.6059(2) 0.0165(2) 0.89377(19) 0.0264(6) Uani 1 1 d . . . H7A H 0.5602 0.0106 0.8422 0.032 Uiso 1 1 calc R . . H7B H 0.5822 -0.0177 0.9347 0.032 Uiso 1 1 calc R . . C8 C 0.62352(18) 0.1301(2) 0.91480(17) 0.0218(5) Uani 1 1 d . . . H8A H 0.6623 0.1358 0.9697 0.026 Uiso 1 1 calc R . . H8B H 0.5662 0.1651 0.9130 0.026 Uiso 1 1 calc R . . C9 C 0.66846(18) 0.1848(2) 0.85796(17) 0.0199(5) Uani 1 1 d . . . H9A H 0.6259 0.1884 0.8046 0.024 Uiso 1 1 calc R . . H9B H 0.6836 0.2566 0.8766 0.024 Uiso 1 1 calc R . . C10 C 0.95214(17) 0.31419(19) 0.71496(14) 0.0148(5) Uani 1 1 d . . . H10 H 0.9949 0.3346 0.7664 0.018 Uiso 1 1 calc R . . C11 C 0.92177(18) 0.4134(2) 0.66599(16) 0.0187(5) Uani 1 1 d . . . H11A H 0.8776 0.3951 0.6156 0.022 Uiso 1 1 calc R . . H11B H 0.8924 0.4606 0.6960 0.022 Uiso 1 1 calc R . . C12 C 1.0011(2) 0.4686(2) 0.64772(17) 0.0228(6) Uani 1 1 d . . . H12A H 0.9791 0.5286 0.6126 0.027 Uiso 1 1 calc R . . H12B H 1.0410 0.4954 0.6978 0.027 Uiso 1 1 calc R . . C13 C 1.05392(19) 0.3975(2) 0.60788(17) 0.0234(6) Uani 1 1 d . . . H13A H 1.1078 0.4344 0.6020 0.028 Uiso 1 1 calc R . . H13B H 1.0169 0.3793 0.5541 0.028 Uiso 1 1 calc R . . C14 C 1.08221(19) 0.2984(2) 0.65590(17) 0.0223(6) Uani 1 1 d . . . H14A H 1.1247 0.3159 0.7074 0.027 Uiso 1 1 calc R . . H14B H 1.1130 0.2518 0.6267 0.027 Uiso 1 1 calc R . . C15 C 1.0012(3) 0.2428(2) 0.6707(3) 0.0208(9) Uani 1 1 d . . . H15A H 1.0210 0.1794 0.7025 0.025 Uiso 1 1 calc R . . H15B H 0.9602 0.2218 0.6194 0.025 Uiso 1 1 calc R . . C16 C 0.88167(17) 0.31594(19) 0.96605(15) 0.0129(5) Uani 1 1 d . . . C17 C 0.77862(17) 0.4240(2) 0.99595(15) 0.0171(5) Uani 1 1 d . . . H17 H 0.7379 0.4799 0.9926 0.020 Uiso 1 1 calc R . . C18 C 0.79951(18) 0.3519(2) 1.05315(16) 0.0197(5) Uani 1 1 d . . . H18 H 0.7759 0.3465 1.0979 0.024 Uiso 1 1 calc R . . C19 C 0.82741(16) 0.46569(19) 0.87275(14) 0.0137(5) Uani 1 1 d . . . H19 H 0.8635 0.4297 0.8410 0.016 Uiso 1 1 calc R . . C20 C 0.73208(18) 0.4790(2) 0.82002(16) 0.0209(5) Uani 1 1 d . . . H20A H 0.6934 0.5056 0.8525 0.025 Uiso 1 1 calc R . . H20B H 0.7085 0.4107 0.7984 0.025 Uiso 1 1 calc R . . C21 C 0.72849(18) 0.5541(2) 0.75105(16) 0.0215(6) Uani 1 1 d . . . H21A H 0.7572 0.5211 0.7129 0.026 Uiso 1 1 calc R . . H21B H 0.6653 0.5678 0.7229 0.026 Uiso 1 1 calc R . . C22 C 0.77496(19) 0.6563(2) 0.77875(17) 0.0220(6) Uani 1 1 d . . . H22A H 0.7757 0.6993 0.7320 0.026 Uiso 1 1 calc R . . H22B H 0.7413 0.6943 0.8107 0.026 Uiso 1 1 calc R . . C23 C 0.87009(18) 0.6383(2) 0.82830(16) 0.0207(5) Uani 1 1 d . . . H23A H 0.8985 0.7058 0.8466 0.025 Uiso 1 1 calc R . . H23B H 0.9049 0.6046 0.7953 0.025 Uiso 1 1 calc R . . C24 C 0.87154(18) 0.5700(2) 0.90014(15) 0.0190(5) Uani 1 1 d . . . H24A H 0.8392 0.6051 0.9347 0.023 Uiso 1 1 calc R . . H24B H 0.9341 0.5588 0.9314 0.023 Uiso 1 1 calc R . . C25 C 0.90292(17) 0.19725(18) 1.08533(15) 0.0141(5) Uani 1 1 d . . . H25 H 0.9449 0.1618 1.0592 0.017 Uiso 1 1 calc R . . C26 C 0.83166(19) 0.1194(2) 1.09170(16) 0.0204(5) Uani 1 1 d . . . H26A H 0.8017 0.0927 1.0381 0.024 Uiso 1 1 calc R . . H26B H 0.7860 0.1547 1.1127 0.024 Uiso 1 1 calc R . . C27 C 0.8708(2) 0.0287(2) 1.14593(17) 0.0250(6) Uani 1 1 d . . . H27A H 0.8219 -0.0174 1.1516 0.030 Uiso 1 1 calc R . . H27B H 0.9109 -0.0120 1.1217 0.030 Uiso 1 1 calc R . . C28 C 0.9228(2) 0.0669(2) 1.22721(17) 0.0272(6) Uani 1 1 d . . . H28A H 0.9504 0.0071 1.2603 0.033 Uiso 1 1 calc R . . H28B H 0.8815 0.1013 1.2537 0.033 Uiso 1 1 calc R . . C29 C 0.9955(2) 0.1428(2) 1.22035(17) 0.0255(6) Uani 1 1 d . . . H29A H 1.0401 0.1064 1.1988 0.031 Uiso 1 1 calc R . . H29B H 1.0264 0.1691 1.2738 0.031 Uiso 1 1 calc R . . C30 C 0.9567(3) 0.2341(2) 1.1663(3) 0.0197(8) Uani 1 1 d . . . H30A H 0.9178 0.2756 1.1913 0.024 Uiso 1 1 calc R . . H30B H 1.0059 0.2792 1.1600 0.024 Uiso 1 1 calc R . . C31 C 1.0720(2) 0.2806(3) 1.01403(18) 0.0188(6) Uani 1 1 d . . . H31A H 1.0558 0.3412 1.0411 0.028 Uiso 1 1 calc R . . H31B H 1.1270 0.2952 0.9985 0.028 Uiso 1 1 calc R . . H31C H 1.0815 0.2209 1.0499 0.028 Uiso 1 1 calc R . . C32 C 1.06948(18) 0.1746(2) 0.87195(16) 0.0152(5) Uani 1 1 d . . . H32A H 1.1019 0.2266 0.8496 0.023 Uiso 1 1 calc R . . H32B H 1.0425 0.1236 0.8310 0.023 Uiso 1 1 calc R . . H32C H 1.1111 0.1394 0.9165 0.023 Uiso 1 1 calc R . . C33 C 1.0118(2) -0.0327(3) 0.95991(18) 0.0357(8) Uani 1 1 d . . . H33A H 0.9839 0.0353 0.9426 0.043 Uiso 1 1 calc R . . H33B H 1.0471 -0.0533 0.9227 0.043 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 0.00951(3) 0.01286(3) 0.01126(3) 0.00056(4) 0.00322(2) 0.00093(5) Cl1 0.0271(4) 0.0411(4) 0.0273(4) 0.0017(3) 0.0088(3) 0.0035(3) N1 0.0120(10) 0.0188(10) 0.0111(10) 0.0011(8) 0.0023(8) -0.0007(8) C1 0.0138(14) 0.0143(11) 0.0131(13) 0.0001(10) 0.0044(10) 0.0019(10) Cl2 0.0589(6) 0.0509(5) 0.0318(4) 0.0066(4) -0.0034(4) -0.0159(5) N2 0.0145(11) 0.0214(11) 0.0121(10) -0.0001(8) 0.0023(8) -0.0023(8) C2 0.0149(13) 0.0247(13) 0.0167(12) -0.0021(10) 0.0005(10) -0.0033(10) N3 0.0126(10) 0.0175(10) 0.0127(10) 0.0024(8) 0.0068(8) 0.0037(8) C3 0.0185(13) 0.0261(14) 0.0137(12) -0.0001(10) 0.0003(10) -0.0005(10) N4 0.0156(11) 0.0143(9) 0.0151(11) 0.0013(8) 0.0060(9) 0.0029(8) C4 0.0132(12) 0.0198(12) 0.0129(11) 0.0012(9) 0.0046(9) -0.0015(9) C5 0.0227(14) 0.0202(13) 0.0268(14) -0.0018(11) 0.0090(11) -0.0031(11) C6 0.0262(15) 0.0200(13) 0.0353(17) 0.0007(12) 0.0125(13) -0.0035(11) C7 0.0205(14) 0.0283(14) 0.0322(16) 0.0017(12) 0.0101(12) -0.0071(11) C8 0.0137(13) 0.0302(14) 0.0227(13) -0.0015(11) 0.0068(11) -0.0028(11) C9 0.0159(13) 0.0231(13) 0.0230(14) -0.0015(10) 0.0094(11) 0.0000(10) C10 0.0138(12) 0.0181(11) 0.0130(12) -0.0001(9) 0.0048(9) -0.0005(9) C11 0.0176(13) 0.0196(12) 0.0211(13) 0.0004(10) 0.0093(11) 0.0037(10) C12 0.0255(15) 0.0220(13) 0.0228(14) 0.0070(11) 0.0098(12) 0.0002(11) C13 0.0210(14) 0.0311(15) 0.0233(14) 0.0076(11) 0.0150(12) 0.0036(12) C14 0.0201(14) 0.0296(15) 0.0200(14) 0.0056(11) 0.0106(11) 0.0060(12) C15 0.022(2) 0.0192(16) 0.0234(19) -0.0003(11) 0.0103(15) 0.0052(11) C16 0.0110(12) 0.0136(11) 0.0120(11) -0.0002(9) -0.0006(9) 0.0003(9) C17 0.0167(12) 0.0210(12) 0.0165(12) -0.0004(10) 0.0096(10) 0.0059(10) C18 0.0171(13) 0.0271(14) 0.0183(13) 0.0017(10) 0.0104(11) 0.0040(11) C19 0.0110(11) 0.0183(11) 0.0122(11) 0.0023(9) 0.0038(9) 0.0029(9) C20 0.0156(13) 0.0254(13) 0.0191(13) 0.0034(11) 0.0002(10) -0.0010(11) C21 0.0131(12) 0.0338(15) 0.0158(12) 0.0052(11) 0.0010(10) 0.0067(11) C22 0.0234(14) 0.0241(13) 0.0203(13) 0.0073(11) 0.0088(11) 0.0071(11) C23 0.0205(14) 0.0224(13) 0.0187(13) 0.0048(10) 0.0043(11) 0.0000(11) C24 0.0182(13) 0.0229(13) 0.0158(12) 0.0008(10) 0.0044(10) -0.0029(10) C25 0.0155(12) 0.0148(11) 0.0124(11) 0.0028(9) 0.0045(9) 0.0034(9) C26 0.0218(14) 0.0228(13) 0.0156(13) 0.0025(10) 0.0032(10) -0.0039(11) C27 0.0299(16) 0.0182(13) 0.0257(15) 0.0030(11) 0.0055(12) -0.0047(11) C28 0.0320(17) 0.0285(15) 0.0212(14) 0.0125(12) 0.0070(13) -0.0008(13) C29 0.0231(15) 0.0284(15) 0.0200(14) 0.0073(11) -0.0030(11) -0.0034(12) C30 0.0221(19) 0.0197(14) 0.0176(16) 0.0018(11) 0.0055(14) -0.0018(12) C31 0.0156(15) 0.0238(13) 0.0158(15) -0.0010(12) 0.0023(11) -0.0019(12) C32 0.0123(12) 0.0209(12) 0.0128(12) 0.0023(9) 0.0044(10) 0.0043(9) C33 0.043(2) 0.0403(19) 0.0215(15) 0.0080(13) 0.0038(14) 0.0025(15) _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 C16 2.032(3) . ? Pt1 C1 2.065(3) . ? Pt1 C31 2.099(3) . ? Pt1 C32 2.107(3) . ? Cl1 C33 1.776(3) . ? N1 C1 1.355(4) . ? N1 C2 1.392(3) . ? N1 C4 1.477(3) . ? C1 N2 1.382(4) . ? Cl2 C33 1.758(4) . ? N2 C3 1.391(4) . ? N2 C10 1.474(3) . ? C2 C3 1.346(4) . ? N3 C16 1.374(3) . ? N3 C17 1.389(3) . ? N3 C19 1.473(3) . ? N4 C16 1.363(3) . ? N4 C18 1.392(3) . ? N4 C25 1.486(3) . ? C4 C9 1.526(4) . ? C4 C5 1.532(4) . ? C5 C6 1.527(4) . ? C6 C7 1.520(4) . ? C7 C8 1.519(4) . ? C8 C9 1.528(4) . ? C10 C15 1.529(5) . ? C10 C11 1.542(4) . ? C11 C12 1.528(4) . ? C12 C13 1.516(4) . ? C13 C14 1.529(4) . ? C14 C15 1.528(5) . ? C17 C18 1.341(4) . ? C19 C24 1.529(4) . ? C19 C20 1.531(4) . ? C20 C21 1.535(4) . ? C21 C22 1.519(4) . ? C22 C23 1.518(4) . ? C23 C24 1.529(3) . ? C25 C30 1.516(5) . ? C25 C26 1.519(4) . ? C26 C27 1.528(4) . ? C27 C28 1.518(4) . ? C28 C29 1.522(4) . ? C29 C30 1.530(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 C16 Pt1 C1 93.96(11) . . ? C16 Pt1 C31 88.56(12) . . ? C1 Pt1 C31 174.40(14) . . ? C16 Pt1 C32 172.45(11) . . ? C1 Pt1 C32 93.30(11) . . ? C31 Pt1 C32 84.39(12) . . ? C1 N1 C2 112.1(2) . . ? C1 N1 C4 125.4(2) . . ? C2 N1 C4 122.5(2) . . ? N1 C1 N2 103.3(2) . . ? N1 C1 Pt1 130.1(2) . . ? N2 C1 Pt1 126.2(2) . . ? C1 N2 C3 111.1(2) . . ? C1 N2 C10 125.6(2) . . ? C3 N2 C10 123.2(2) . . ? C3 C2 N1 106.6(2) . . ? C16 N3 C17 111.5(2) . . ? C16 N3 C19 124.9(2) . . ? C17 N3 C19 123.5(2) . . ? C2 C3 N2 106.9(2) . . ? C16 N4 C18 111.4(2) . . ? C16 N4 C25 125.7(2) . . ? C18 N4 C25 122.9(2) . . ? N1 C4 C9 110.1(2) . . ? N1 C4 C5 110.1(2) . . ? C9 C4 C5 110.9(2) . . ? C6 C5 C4 110.9(2) . . ? C7 C6 C5 112.2(2) . . ? C8 C7 C6 111.0(2) . . ? C7 C8 C9 111.9(2) . . ? C4 C9 C8 112.4(2) . . ? N2 C10 C15 111.5(2) . . ? N2 C10 C11 110.8(2) . . ? C15 C10 C11 109.9(2) . . ? C12 C11 C10 111.0(2) . . ? C13 C12 C11 112.1(2) . . ? C12 C13 C14 111.5(2) . . ? C13 C14 C15 110.9(2) . . ? C14 C15 C10 110.1(2) . . ? N4 C16 N3 103.3(2) . . ? N4 C16 Pt1 127.56(18) . . ? N3 C16 Pt1 129.09(19) . . ? C18 C17 N3 106.6(2) . . ? C17 C18 N4 107.1(2) . . ? N3 C19 C24 109.5(2) . . ? N3 C19 C20 110.8(2) . . ? C24 C19 C20 111.8(2) . . ? C19 C20 C21 111.8(2) . . ? C22 C21 C20 112.5(2) . . ? C23 C22 C21 110.9(2) . . ? C22 C23 C24 110.9(2) . . ? C23 C24 C19 110.1(2) . . ? N4 C25 C30 110.9(2) . . ? N4 C25 C26 110.6(2) . . ? C30 C25 C26 111.7(2) . . ? C25 C26 C27 112.0(2) . . ? C28 C27 C26 110.9(2) . . ? C27 C28 C29 110.9(2) . . ? C28 C29 C30 111.4(3) . . ? C25 C30 C29 111.3(2) . . ? Cl2 C33 Cl1 111.06(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.898 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.084 # Attachment 'CCDC-741811-Compound4.cif' data_nol280m _database_code_depnum_ccdc_archive 'CCDC 741811' #TrackingRef 'CCDC-741811-Compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pt(IMes)2(Me2)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H54 N4 Pt' _chemical_formula_weight 834.00 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.7156(10) _cell_length_b 13.1785(8) _cell_length_c 17.6422(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.4110(10) _cell_angle_gamma 90.00 _cell_volume 3834.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49199 _cell_measurement_theta_min 2.195 _cell_measurement_theta_max 30.546 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 3.695 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.601619 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56756 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11107 _reflns_number_gt 9591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+8.9816P] 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 SHELXL _refine_ls_extinction_coef 0.00029(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11107 _refine_ls_number_parameters 457 _refine_ls_number_restraints 438 _refine_ls_R_factor_all 0.0420 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.035 _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 0.287745(6) 0.356718(8) 0.040570(6) 0.01513(4) Uani 1 1 d U . . N1 N 0.25240(15) 0.2059(2) 0.16826(14) 0.0200(5) Uani 1 1 d U . . C1 C 0.30448(17) 0.2467(2) 0.12321(16) 0.0169(5) Uani 1 1 d U . . N2 N 0.37933(15) 0.2235(2) 0.16436(14) 0.0203(5) Uani 1 1 d U . . C2 C 0.29474(19) 0.1625(3) 0.23516(18) 0.0284(7) Uani 1 1 d U . . H2 H 0.2718 0.1314 0.2752 0.034 Uiso 1 1 calc R . . N3 N 0.18066(14) 0.30711(19) -0.10888(13) 0.0189(5) Uani 1 1 d U . . C3 C 0.37383(19) 0.1729(3) 0.23225(18) 0.0279(7) Uani 1 1 d U . . H3 H 0.4177 0.1501 0.2695 0.034 Uiso 1 1 calc R . . N4 N 0.30411(15) 0.2872(2) -0.12517(14) 0.0207(5) Uani 1 1 d U . . C4 C 0.16534(17) 0.1932(2) 0.15436(16) 0.0201(5) Uani 1 1 d U . . C5 C 0.13607(19) 0.0933(2) 0.14530(17) 0.0218(6) Uani 1 1 d U . . C6 C 0.05413(19) 0.0763(2) 0.14760(18) 0.0248(6) Uani 1 1 d U . . H6 H 0.0334 0.0092 0.1409 0.030 Uiso 1 1 calc R . . C7 C 0.00199(18) 0.1549(2) 0.15942(17) 0.0236(6) Uani 1 1 d U . . C8 C 0.03201(18) 0.2529(2) 0.16417(17) 0.0229(6) Uani 1 1 d U . . H8 H -0.0039 0.3073 0.1697 0.028 Uiso 1 1 calc R . . C9 C 0.11351(18) 0.2747(2) 0.16117(16) 0.0202(5) Uani 1 1 d U . . C10 C 0.1427(2) 0.3825(2) 0.1671(2) 0.0272(7) Uani 1 1 d U . . H10A H 0.1932 0.3866 0.2040 0.041 Uiso 1 1 calc R . . H10B H 0.1015 0.4256 0.1845 0.041 Uiso 1 1 calc R . . H10C H 0.1524 0.4058 0.1166 0.041 Uiso 1 1 calc R . . C11 C -0.0842(2) 0.1343(3) 0.1699(2) 0.0331(7) Uani 1 1 d U . . H11A H -0.0848 0.1077 0.2216 0.050 Uiso 1 1 calc R . . H11B H -0.1085 0.0843 0.1318 0.050 Uiso 1 1 calc R . . H11C H -0.1155 0.1975 0.1630 0.050 Uiso 1 1 calc R . . C12 C 0.1903(2) 0.0041(3) 0.1360(2) 0.0312(7) Uani 1 1 d U . . H12A H 0.2174 -0.0184 0.1867 0.047 Uiso 1 1 calc R . . H12B H 0.2311 0.0245 0.1049 0.047 Uiso 1 1 calc R . . H12C H 0.1577 -0.0515 0.1104 0.047 Uiso 1 1 calc R . . C13 C 0.45584(17) 0.2349(2) 0.13772(16) 0.0195(5) Uani 1 1 d U . . C14 C 0.47240(18) 0.1685(2) 0.08046(17) 0.0199(6) Uani 1 1 d U . . C15 C 0.54901(19) 0.1717(2) 0.05925(18) 0.0230(6) Uani 1 1 d U . . H15 H 0.5610 0.1274 0.0201 0.028 Uiso 1 1 calc R . . C16 C 0.60861(18) 0.2385(2) 0.09417(18) 0.0236(6) Uani 1 1 d U . . C17 C 0.58972(18) 0.3033(2) 0.15027(18) 0.0234(6) Uani 1 1 d U . . H17 H 0.6295 0.3503 0.1733 0.028 Uiso 1 1 calc R . . C18 C 0.51399(18) 0.3021(2) 0.17432(17) 0.0216(6) Uani 1 1 d U . . C19 C 0.5001(2) 0.3691(3) 0.2403(2) 0.0339(8) Uani 1 1 d U . . H19A H 0.4417 0.3770 0.2398 0.051 Uiso 1 1 calc R . . H19B H 0.5245 0.4358 0.2351 0.051 Uiso 1 1 calc R . . H19C H 0.5250 0.3381 0.2889 0.051 Uiso 1 1 calc R . . C20 C 0.6919(2) 0.2388(3) 0.0719(2) 0.0331(8) Uani 1 1 d U . . H20A H 0.7283 0.2812 0.1079 0.050 Uiso 1 1 calc R . . H20B H 0.6886 0.2662 0.0198 0.050 Uiso 1 1 calc R . . H20C H 0.7130 0.1693 0.0733 0.050 Uiso 1 1 calc R . . C21 C 0.4092(2) 0.0941(2) 0.0441(2) 0.0270(7) Uani 1 1 d U . . H21A H 0.3905 0.0534 0.0842 0.040 Uiso 1 1 calc R . . H21B H 0.4328 0.0494 0.0091 0.040 Uiso 1 1 calc R . . H21C H 0.3633 0.1312 0.0151 0.040 Uiso 1 1 calc R . . C22 C 0.25778(17) 0.2995(2) -0.06806(16) 0.0168(5) Uani 1 1 d U . . C23 C 0.17979(19) 0.3035(3) -0.18779(17) 0.0266(7) Uani 1 1 d U . . H23 H 0.1336 0.3089 -0.2269 0.032 Uiso 1 1 calc R . . C24 C 0.25654(19) 0.2911(3) -0.19775(18) 0.0280(7) Uani 1 1 d U . . H24 H 0.2754 0.2858 -0.2456 0.034 Uiso 1 1 calc R . . C25 C 0.10551(17) 0.3029(2) -0.07903(15) 0.0193(5) Uani 1 1 d U . . C26 C 0.08296(17) 0.2087(2) -0.05186(16) 0.0202(5) Uani 1 1 d U . . C27 C 0.00546(18) 0.1993(2) -0.03290(17) 0.0231(6) Uani 1 1 d U . . H27 H -0.0108 0.1360 -0.0147 0.028 Uiso 1 1 calc R . . C28 C -0.04862(18) 0.2804(3) -0.03991(18) 0.0250(6) Uani 1 1 d U . . C29 C -0.02399(19) 0.3724(3) -0.06664(18) 0.0264(6) Uani 1 1 d U . . H29 H -0.0602 0.4285 -0.0707 0.032 Uiso 1 1 calc R . . C30 C 0.05266(18) 0.3852(2) -0.08787(18) 0.0237(6) Uani 1 1 d U . . C31 C 0.0729(2) 0.4847(3) -0.1219(2) 0.0338(8) Uani 1 1 d U . . H31A H 0.0491 0.4866 -0.1765 0.051 Uiso 1 1 calc R . . H31B H 0.1319 0.4918 -0.1166 0.051 Uiso 1 1 calc R . . H31C H 0.0509 0.5405 -0.0950 0.051 Uiso 1 1 calc R . . C32 C -0.1329(2) 0.2679(3) -0.0206(2) 0.0367(8) Uani 1 1 d U . . H32A H -0.1422 0.1963 -0.0097 0.055 Uiso 1 1 calc R . . H32B H -0.1730 0.2902 -0.0642 0.055 Uiso 1 1 calc R . . H32C H -0.1381 0.3089 0.0247 0.055 Uiso 1 1 calc R . . C33 C 0.13875(19) 0.1188(2) -0.04695(19) 0.0243(6) Uani 1 1 d U . . H33A H 0.1120 0.0597 -0.0285 0.036 Uiso 1 1 calc R . . H33B H 0.1887 0.1338 -0.0112 0.036 Uiso 1 1 calc R . . H33C H 0.1520 0.1043 -0.0979 0.036 Uiso 1 1 calc R . . C34 C 0.38801(18) 0.2561(3) -0.12056(17) 0.0227(6) Uani 1 1 d U . . C35 C 0.4027(2) 0.1561(3) -0.14112(19) 0.0284(7) Uani 1 1 d U . . C36 C 0.4819(2) 0.1277(3) -0.1473(2) 0.0327(7) Uani 1 1 d U . . H36 H 0.4924 0.0599 -0.1612 0.039 Uiso 1 1 calc R . . C37 C 0.5454(2) 0.1965(3) -0.1336(2) 0.0327(7) Uani 1 1 d U . . C38 C 0.52916(19) 0.2947(3) -0.11363(19) 0.0300(7) Uani 1 1 d U . . H38 H 0.5726 0.3419 -0.1042 0.036 Uiso 1 1 calc R . . C39 C 0.45082(19) 0.3272(3) -0.10682(18) 0.0259(6) Uani 1 1 d U . . C40 C 0.4363(2) 0.4350(3) -0.0868(2) 0.0378(8) Uani 1 1 d U . . H40A H 0.3908 0.4623 -0.1232 0.057 Uiso 1 1 calc R . . H40B H 0.4851 0.4752 -0.0896 0.057 Uiso 1 1 calc R . . H40C H 0.4235 0.4384 -0.0346 0.057 Uiso 1 1 calc R . . C41 C 0.6309(2) 0.1642(3) -0.1398(2) 0.0417(9) Uani 1 1 d U . . H41A H 0.6593 0.2205 -0.1600 0.063 Uiso 1 1 calc R . . H41B H 0.6291 0.1059 -0.1745 0.063 Uiso 1 1 calc R . . H41C H 0.6596 0.1452 -0.0888 0.063 Uiso 1 1 calc R . . C42 C 0.3356(2) 0.0780(3) -0.1573(2) 0.0377(8) Uani 1 1 d U . . H42A H 0.2974 0.0873 -0.1212 0.057 Uiso 1 1 calc R . . H42B H 0.3590 0.0097 -0.1512 0.057 Uiso 1 1 calc R . . H42C H 0.3070 0.0864 -0.2100 0.057 Uiso 1 1 calc R . . C43 C 0.2720(2) 0.4952(2) -0.01784(19) 0.0276(7) Uani 1 1 d U . . H43A H 0.2233 0.5290 -0.0060 0.041 Uiso 1 1 calc R . . H43B H 0.2660 0.4831 -0.0733 0.041 Uiso 1 1 calc R . . H43C H 0.3194 0.5385 -0.0016 0.041 Uiso 1 1 calc R . . C44 C 0.32005(19) 0.4546(2) 0.13394(18) 0.0245(6) Uani 1 1 d U . . H44A H 0.3180 0.4179 0.1819 0.037 Uiso 1 1 calc R . . H44B H 0.2821 0.5118 0.1297 0.037 Uiso 1 1 calc R . . H44C H 0.3752 0.4800 0.1340 0.037 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 0.01510(5) 0.01530(5) 0.01473(5) 0.00070(4) 0.00163(3) 0.00115(4) N1 0.0179(11) 0.0241(12) 0.0186(11) 0.0073(9) 0.0053(9) 0.0056(9) C1 0.0164(12) 0.0190(13) 0.0160(12) 0.0012(10) 0.0049(10) 0.0042(10) N2 0.0177(11) 0.0267(13) 0.0165(11) 0.0045(9) 0.0032(9) 0.0061(10) C2 0.0254(15) 0.040(2) 0.0208(14) 0.0153(13) 0.0075(11) 0.0083(13) N3 0.0173(11) 0.0242(13) 0.0146(10) 0.0030(9) 0.0011(8) -0.0020(9) C3 0.0226(14) 0.0400(18) 0.0213(14) 0.0129(13) 0.0037(11) 0.0100(13) N4 0.0176(11) 0.0262(13) 0.0177(11) 0.0006(10) 0.0015(9) -0.0025(10) C4 0.0190(13) 0.0242(14) 0.0177(13) 0.0046(11) 0.0052(10) 0.0035(11) C5 0.0245(14) 0.0229(14) 0.0199(13) 0.0048(11) 0.0093(11) 0.0059(11) C6 0.0268(15) 0.0222(14) 0.0269(15) 0.0043(12) 0.0087(12) 0.0005(12) C7 0.0209(13) 0.0293(16) 0.0220(13) 0.0031(12) 0.0074(11) 0.0008(12) C8 0.0203(14) 0.0257(15) 0.0236(14) 0.0018(12) 0.0064(11) 0.0063(11) C9 0.0202(13) 0.0230(14) 0.0182(13) 0.0015(11) 0.0051(10) 0.0027(11) C10 0.0235(15) 0.0229(15) 0.0361(17) -0.0010(13) 0.0073(13) 0.0025(12) C11 0.0235(15) 0.0373(19) 0.0413(19) 0.0027(16) 0.0132(14) -0.0023(14) C12 0.0348(18) 0.0226(16) 0.0386(18) 0.0063(14) 0.0135(15) 0.0098(13) C13 0.0163(12) 0.0238(14) 0.0179(12) 0.0046(10) 0.0017(10) 0.0055(11) C14 0.0213(13) 0.0163(13) 0.0225(13) 0.0027(10) 0.0044(11) 0.0041(10) C15 0.0247(14) 0.0216(14) 0.0242(14) 0.0022(11) 0.0083(11) 0.0061(11) C16 0.0198(13) 0.0247(15) 0.0262(15) 0.0101(12) 0.0039(11) 0.0050(11) C17 0.0177(13) 0.0267(16) 0.0246(14) 0.0014(12) -0.0006(11) 0.0035(11) C18 0.0189(13) 0.0262(15) 0.0184(13) -0.0018(11) -0.0007(10) 0.0061(11) C19 0.0251(15) 0.046(2) 0.0288(16) -0.0136(15) -0.0015(12) 0.0048(15) C20 0.0234(16) 0.039(2) 0.0392(19) 0.0076(15) 0.0110(14) 0.0031(14) C21 0.0268(15) 0.0193(15) 0.0362(17) -0.0048(12) 0.0092(13) 0.0004(12) C22 0.0169(12) 0.0154(12) 0.0176(12) 0.0016(10) 0.0015(10) -0.0010(10) C23 0.0245(15) 0.0383(18) 0.0158(13) 0.0009(12) -0.0004(11) -0.0036(13) C24 0.0248(15) 0.0420(19) 0.0170(13) -0.0007(13) 0.0029(11) -0.0039(14) C25 0.0172(12) 0.0277(15) 0.0129(12) 0.0017(10) 0.0022(10) 0.0007(11) C26 0.0190(13) 0.0227(14) 0.0183(13) -0.0014(11) 0.0015(10) 0.0005(11) C27 0.0216(14) 0.0254(15) 0.0229(14) -0.0002(12) 0.0052(11) -0.0026(11) C28 0.0180(13) 0.0337(17) 0.0237(14) -0.0028(12) 0.0047(11) -0.0004(12) C29 0.0217(14) 0.0283(17) 0.0280(15) -0.0006(12) 0.0007(11) 0.0063(12) C30 0.0205(14) 0.0251(15) 0.0233(14) 0.0018(11) -0.0027(11) 0.0009(11) C31 0.0280(17) 0.0277(17) 0.044(2) 0.0105(15) 0.0027(14) 0.0026(14) C32 0.0203(15) 0.044(2) 0.048(2) -0.0020(17) 0.0121(15) 0.0013(14) C33 0.0242(14) 0.0209(15) 0.0287(15) 0.0002(11) 0.0076(12) 0.0003(11) C34 0.0178(13) 0.0320(16) 0.0187(13) 0.0016(12) 0.0045(10) -0.0007(11) C35 0.0266(15) 0.0344(18) 0.0248(15) -0.0030(13) 0.0058(12) -0.0014(13) C36 0.0333(17) 0.038(2) 0.0283(16) -0.0022(14) 0.0095(13) 0.0063(14) C37 0.0228(15) 0.050(2) 0.0269(16) 0.0076(15) 0.0078(12) 0.0056(14) C38 0.0193(14) 0.0433(19) 0.0277(16) 0.0078(14) 0.0048(12) -0.0049(13) C39 0.0227(14) 0.0326(16) 0.0221(14) 0.0036(12) 0.0033(11) -0.0026(12) C40 0.0302(18) 0.0313(18) 0.053(2) -0.0005(17) 0.0099(16) -0.0098(15) C41 0.0277(17) 0.062(3) 0.038(2) 0.0075(18) 0.0114(15) 0.0103(17) C42 0.0326(18) 0.0344(19) 0.046(2) -0.0129(17) 0.0071(16) -0.0030(15) C43 0.0329(17) 0.0219(15) 0.0268(16) 0.0026(12) 0.0010(13) 0.0010(13) C44 0.0252(15) 0.0235(15) 0.0242(14) -0.0061(12) 0.0023(12) -0.0026(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.043(3) . ? Pt1 C22 2.044(3) . ? Pt1 C43 2.091(3) . ? Pt1 C44 2.093(3) . ? N1 C1 1.380(4) . ? N1 C2 1.396(4) . ? N1 C4 1.445(4) . ? C1 N2 1.375(4) . ? N2 C3 1.387(4) . ? N2 C13 1.441(4) . ? C2 C3 1.339(4) . ? N3 C22 1.374(3) . ? N3 C23 1.391(4) . ? N3 C25 1.440(4) . ? N4 C22 1.377(4) . ? N4 C24 1.393(4) . ? N4 C34 1.450(4) . ? C4 C9 1.398(4) . ? C4 C5 1.404(4) . ? C5 C6 1.395(4) . ? C5 C12 1.510(4) . ? C6 C7 1.391(4) . ? C7 C8 1.384(4) . ? C7 C11 1.507(4) . ? C8 C9 1.402(4) . ? C9 C10 1.500(4) . ? C13 C18 1.393(4) . ? C13 C14 1.398(4) . ? C14 C15 1.392(4) . ? C14 C21 1.505(4) . ? C15 C16 1.395(4) . ? C16 C17 1.382(4) . ? C16 C20 1.508(4) . ? C17 C18 1.400(4) . ? C18 C19 1.510(4) . ? C23 C24 1.333(5) . ? C25 C30 1.391(4) . ? C25 C26 1.405(4) . ? C26 C27 1.395(4) . ? C26 C33 1.501(4) . ? C27 C28 1.392(4) . ? C28 C29 1.388(5) . ? C28 C32 1.512(4) . ? C29 C30 1.402(4) . ? C30 C31 1.504(5) . ? C34 C39 1.398(4) . ? C34 C35 1.400(5) . ? C35 C36 1.397(5) . ? C35 C42 1.515(5) . ? C36 C37 1.388(5) . ? C37 C38 1.379(5) . ? C37 C41 1.512(5) . ? C38 C39 1.401(5) . ? C39 C40 1.494(5) . ? 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 C1 Pt1 C22 113.03(11) . . ? C1 Pt1 C43 164.28(12) . . ? C22 Pt1 C43 82.44(12) . . ? C1 Pt1 C44 83.58(12) . . ? C22 Pt1 C44 163.27(12) . . ? C43 Pt1 C44 81.09(13) . . ? C1 N1 C2 111.5(2) . . ? C1 N1 C4 131.3(2) . . ? C2 N1 C4 116.9(2) . . ? N2 C1 N1 102.4(2) . . ? N2 C1 Pt1 122.8(2) . . ? N1 C1 Pt1 131.4(2) . . ? C1 N2 C3 112.3(2) . . ? C1 N2 C13 125.8(2) . . ? C3 N2 C13 121.3(2) . . ? C3 C2 N1 107.0(3) . . ? C22 N3 C23 112.2(2) . . ? C22 N3 C25 127.3(2) . . ? C23 N3 C25 119.9(2) . . ? C2 C3 N2 106.7(3) . . ? C22 N4 C24 111.3(2) . . ? C22 N4 C34 130.3(2) . . ? C24 N4 C34 117.6(3) . . ? C9 C4 C5 121.4(3) . . ? C9 C4 N1 121.1(3) . . ? C5 C4 N1 116.8(3) . . ? C6 C5 C4 118.3(3) . . ? C6 C5 C12 119.2(3) . . ? C4 C5 C12 122.5(3) . . ? C7 C6 C5 121.8(3) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 C11 120.3(3) . . ? C6 C7 C11 121.3(3) . . ? C7 C8 C9 122.3(3) . . ? C4 C9 C8 117.7(3) . . ? C4 C9 C10 122.3(3) . . ? C8 C9 C10 119.9(3) . . ? C18 C13 C14 121.8(3) . . ? C18 C13 N2 120.3(3) . . ? C14 C13 N2 117.5(3) . . ? C15 C14 C13 118.3(3) . . ? C15 C14 C21 121.2(3) . . ? C13 C14 C21 120.5(3) . . ? C14 C15 C16 121.5(3) . . ? C17 C16 C15 118.4(3) . . ? C17 C16 C20 120.9(3) . . ? C15 C16 C20 120.7(3) . . ? C16 C17 C18 122.3(3) . . ? C13 C18 C17 117.7(3) . . ? C13 C18 C19 123.1(3) . . ? C17 C18 C19 119.2(3) . . ? N3 C22 N4 102.5(2) . . ? N3 C22 Pt1 122.0(2) . . ? N4 C22 Pt1 130.4(2) . . ? C24 C23 N3 106.5(3) . . ? C23 C24 N4 107.5(3) . . ? C30 C25 C26 121.8(3) . . ? C30 C25 N3 120.3(3) . . ? C26 C25 N3 117.2(3) . . ? C27 C26 C25 118.1(3) . . ? C27 C26 C33 120.6(3) . . ? C25 C26 C33 121.2(3) . . ? C28 C27 C26 121.7(3) . . ? C29 C28 C27 118.5(3) . . ? C29 C28 C32 120.8(3) . . ? C27 C28 C32 120.8(3) . . ? C28 C29 C30 122.0(3) . . ? C25 C30 C29 117.9(3) . . ? C25 C30 C31 122.9(3) . . ? C29 C30 C31 119.1(3) . . ? C39 C34 C35 121.1(3) . . ? C39 C34 N4 120.8(3) . . ? C35 C34 N4 117.4(3) . . ? C36 C35 C34 118.8(3) . . ? C36 C35 C42 119.0(3) . . ? C34 C35 C42 122.2(3) . . ? C37 C36 C35 121.3(3) . . ? C38 C37 C36 118.7(3) . . ? C38 C37 C41 120.7(3) . . ? C36 C37 C41 120.6(4) . . ? C37 C38 C39 122.3(3) . . ? C34 C39 C38 117.8(3) . . ? C34 C39 C40 122.1(3) . . ? C38 C39 C40 120.1(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.559 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.131 # Attachment 'CCDC-741812-Compound5A.cif' data_nol193 _database_code_depnum_ccdc_archive 'CCDC 741812' #TrackingRef 'CCDC-741812-Compound5A.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Pt(IMes*)(IMes)Me) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H50 N4 Pt' _chemical_formula_weight 817.96 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7787(5) _cell_length_b 20.0707(9) _cell_length_c 17.2875(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.0640(10) _cell_angle_gamma 90.00 _cell_volume 3739.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34334 _cell_measurement_theta_min 2.143 _cell_measurement_theta_max 30.769 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 3.787 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.616063 _exptl_absorpt_correction_T_max 0.925811 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53108 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9017 _reflns_number_gt 7543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+15.6320P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9017 _refine_ls_number_parameters 453 _refine_ls_number_restraints 446 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.007 _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 0.671054(15) 0.239808(8) 0.592926(9) 0.01772(5) Uani 1 1 d U . . N1 N 0.4740(3) 0.2369(2) 0.4578(2) 0.0231(7) Uani 1 1 d U . . C1 C 0.5530(4) 0.2700(2) 0.5073(2) 0.0211(8) Uani 1 1 d U . . N2 N 0.5663(4) 0.33103(19) 0.4733(2) 0.0220(7) Uani 1 1 d U . . C2 C 0.4421(5) 0.2763(2) 0.3943(3) 0.0291(10) Uani 1 1 d U . . H2 H 0.3894 0.2638 0.3521 0.035 Uiso 1 1 calc R . . N3 N 0.5032(3) 0.23399(18) 0.74280(19) 0.0194(7) Uani 1 1 d U . . C3 C 0.4990(4) 0.3345(2) 0.4034(3) 0.0270(10) Uani 1 1 d U . . H3 H 0.4948 0.3714 0.3691 0.032 Uiso 1 1 calc R . . N4 N 0.6590(3) 0.30113(19) 0.7478(2) 0.0226(8) Uani 1 1 d U . . C4 C 0.4100(4) 0.1754(2) 0.4719(3) 0.0246(9) Uani 1 1 d U . . C5 C 0.4561(5) 0.1153(3) 0.4457(3) 0.0309(10) Uani 1 1 d U . . C6 C 0.3839(5) 0.0582(3) 0.4556(3) 0.0376(12) Uani 1 1 d U . . H6 H 0.4164 0.0164 0.4402 0.045 Uiso 1 1 calc R . . C7 C 0.2672(5) 0.0604(3) 0.4869(3) 0.0375(12) Uani 1 1 d U . . C8 C 0.2227(5) 0.1212(3) 0.5118(3) 0.0336(11) Uani 1 1 d U . . H8 H 0.1427 0.1232 0.5339 0.040 Uiso 1 1 calc R . . C9 C 0.2917(5) 0.1795(3) 0.5053(3) 0.0280(10) Uani 1 1 d U . . C10 C 0.2395(5) 0.2448(3) 0.5313(3) 0.0377(12) Uani 1 1 d U . . H10A H 0.1538 0.2385 0.5478 0.057 Uiso 1 1 calc R . . H10B H 0.2409 0.2767 0.4884 0.057 Uiso 1 1 calc R . . H10C H 0.2897 0.2621 0.5747 0.057 Uiso 1 1 calc R . . C11 C 0.1883(7) -0.0021(3) 0.4917(4) 0.0586(18) Uani 1 1 d U . . H11A H 0.1885 -0.0183 0.5452 0.088 Uiso 1 1 calc R . . H11B H 0.2224 -0.0365 0.4580 0.088 Uiso 1 1 calc R . . H11C H 0.1030 0.0082 0.4750 0.088 Uiso 1 1 calc R . . C12 C 0.5770(5) 0.1112(3) 0.4039(4) 0.0500(16) Uani 1 1 d U . . H12A H 0.5699 0.1356 0.3549 0.075 Uiso 1 1 calc R . . H12B H 0.5967 0.0644 0.3935 0.075 Uiso 1 1 calc R . . H12C H 0.6432 0.1309 0.4361 0.075 Uiso 1 1 calc R . . C13 C 0.6302(4) 0.3879(2) 0.5063(3) 0.0222(9) Uani 1 1 d U . . C14 C 0.5676(4) 0.4255(2) 0.5614(3) 0.0255(9) Uani 1 1 d U . . C15 C 0.6262(5) 0.4826(2) 0.5898(3) 0.0296(10) Uani 1 1 d U . . H15 H 0.5854 0.5087 0.6275 0.035 Uiso 1 1 calc R . . C16 C 0.7425(5) 0.5027(2) 0.5649(3) 0.0322(10) Uani 1 1 d U . . C17 C 0.8007(5) 0.4635(2) 0.5105(3) 0.0295(10) Uani 1 1 d U . . H17 H 0.8809 0.4762 0.4939 0.035 Uiso 1 1 calc R . . C18 C 0.7466(5) 0.4064(2) 0.4794(3) 0.0259(9) Uani 1 1 d U . . C19 C 0.8133(5) 0.3676(3) 0.4185(3) 0.0366(12) Uani 1 1 d U . . H19A H 0.8155 0.3937 0.3706 0.055 Uiso 1 1 calc R . . H19B H 0.7696 0.3255 0.4087 0.055 Uiso 1 1 calc R . . H19C H 0.8983 0.3583 0.4364 0.055 Uiso 1 1 calc R . . C20 C 0.4426(5) 0.4055(3) 0.5901(3) 0.0344(11) Uani 1 1 d U . . H20A H 0.3854 0.3991 0.5460 0.052 Uiso 1 1 calc R . . H20B H 0.4106 0.4405 0.6238 0.052 Uiso 1 1 calc R . . H20C H 0.4500 0.3638 0.6193 0.052 Uiso 1 1 calc R . . C21 C 0.8035(6) 0.5655(3) 0.5951(3) 0.0408(13) Uani 1 1 d U . . H21A H 0.8924 0.5575 0.6035 0.061 Uiso 1 1 calc R . . H21B H 0.7659 0.5782 0.6441 0.061 Uiso 1 1 calc R . . H21C H 0.7917 0.6014 0.5573 0.061 Uiso 1 1 calc R . . C22 C 0.5931(4) 0.2618(2) 0.6973(2) 0.0230(8) Uani 1 1 d U . . C23 C 0.5182(5) 0.2551(3) 0.8202(3) 0.0300(10) Uani 1 1 d U . . H23 H 0.4686 0.2423 0.8626 0.036 Uiso 1 1 calc R . . C24 C 0.6152(4) 0.2964(3) 0.8225(3) 0.0285(10) Uani 1 1 d U . . H24 H 0.6481 0.3184 0.8670 0.034 Uiso 1 1 calc R . . C25 C 0.4020(4) 0.1905(2) 0.7220(2) 0.0264(9) Uani 1 1 d U . . C26 C 0.4247(5) 0.1251(3) 0.7009(3) 0.0331(10) Uani 1 1 d U . . C27 C 0.3227(6) 0.0830(3) 0.6935(3) 0.0448(13) Uani 1 1 d U . . H27 H 0.3361 0.0379 0.6792 0.054 Uiso 1 1 calc R . . C28 C 0.2021(6) 0.1041(3) 0.7061(3) 0.0494(14) Uani 1 1 d U . . C29 C 0.1832(5) 0.1697(3) 0.7239(3) 0.0414(12) Uani 1 1 d U . . H29 H 0.1007 0.1853 0.7303 0.050 Uiso 1 1 calc R . . C30 C 0.2818(4) 0.2146(3) 0.7330(3) 0.0309(10) Uani 1 1 d U . . C31 C 0.2566(5) 0.2857(3) 0.7553(3) 0.0381(12) Uani 1 1 d U . . H31A H 0.2724 0.2915 0.8109 0.057 Uiso 1 1 calc R . . H31B H 0.1698 0.2967 0.7431 0.057 Uiso 1 1 calc R . . H31C H 0.3111 0.3154 0.7264 0.057 Uiso 1 1 calc R . . C32 C 0.0941(8) 0.0558(4) 0.7000(4) 0.076(2) Uani 1 1 d U . . H32A H 0.0506 0.0547 0.7492 0.114 Uiso 1 1 calc R . . H32B H 0.1252 0.0111 0.6881 0.114 Uiso 1 1 calc R . . H32C H 0.0367 0.0703 0.6587 0.114 Uiso 1 1 calc R . . C33 C 0.5546(6) 0.1004(3) 0.6874(3) 0.0406(13) Uani 1 1 d U . . H33A H 0.5883 0.1227 0.6419 0.061 Uiso 1 1 calc R . . H33B H 0.5527 0.0521 0.6786 0.061 Uiso 1 1 calc R . . H33C H 0.6071 0.1102 0.7328 0.061 Uiso 1 1 calc R . . C34 C 0.7731(4) 0.3332(2) 0.7275(3) 0.0249(9) Uani 1 1 d U . . C35 C 0.8578(4) 0.2933(2) 0.6875(3) 0.0240(9) Uani 1 1 d U . . C36 C 0.9661(4) 0.3250(3) 0.6628(3) 0.0288(10) Uani 1 1 d U . . H36 H 1.0255 0.2999 0.6352 0.035 Uiso 1 1 calc R . . C37 C 0.9890(5) 0.3915(3) 0.6774(3) 0.0322(10) Uani 1 1 d U . . C38 C 0.9029(5) 0.4285(3) 0.7172(3) 0.0315(10) Uani 1 1 d U . . H38 H 0.9199 0.4740 0.7282 0.038 Uiso 1 1 calc R . . C39 C 0.7912(5) 0.4005(3) 0.7418(3) 0.0288(10) Uani 1 1 d U . . C40 C 0.6942(5) 0.4429(3) 0.7793(3) 0.0377(12) Uani 1 1 d U . . H40A H 0.6122 0.4315 0.7578 0.057 Uiso 1 1 calc R . . H40B H 0.7115 0.4901 0.7693 0.057 Uiso 1 1 calc R . . H40C H 0.6956 0.4349 0.8352 0.057 Uiso 1 1 calc R . . C41 C 1.1069(5) 0.4239(3) 0.6500(4) 0.0487(15) Uani 1 1 d U . . H41A H 1.1761 0.4115 0.6847 0.073 Uiso 1 1 calc R . . H41B H 1.0969 0.4725 0.6503 0.073 Uiso 1 1 calc R . . H41C H 1.1242 0.4089 0.5974 0.073 Uiso 1 1 calc R . . C42 C 0.8241(4) 0.2229(2) 0.6678(3) 0.0251(9) Uani 1 1 d DU . . C43 C 0.7934(4) 0.2115(3) 0.5060(3) 0.0272(10) Uani 1 1 d U . . H43B H 0.7515 0.2154 0.4554 0.041 Uiso 1 1 calc R . . H43A H 0.8194 0.1652 0.5144 0.041 Uiso 1 1 calc R . . H43C H 0.8664 0.2406 0.5076 0.041 Uiso 1 1 calc R . . H42A H 0.893(4) 0.201(2) 0.643(2) 0.014(11) Uiso 1 1 d D . . H42B H 0.808(5) 0.199(3) 0.714(3) 0.041(16) Uiso 1 1 d 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 0.01746(8) 0.02223(8) 0.01345(8) -0.00137(7) -0.00051(5) 0.00133(7) N1 0.0256(18) 0.0294(18) 0.0140(16) -0.0005(14) -0.0048(14) -0.0016(15) C1 0.023(2) 0.027(2) 0.0133(18) -0.0015(16) 0.0029(15) 0.0012(16) N2 0.0236(19) 0.0261(19) 0.0162(18) -0.0006(14) -0.0003(14) -0.0012(14) C2 0.034(3) 0.038(3) 0.015(2) 0.0038(18) -0.0106(18) -0.003(2) N3 0.0269(17) 0.0188(16) 0.0122(15) 0.0114(13) -0.0062(13) 0.0068(13) C3 0.029(2) 0.037(2) 0.015(2) 0.0057(18) -0.0047(18) -0.0004(19) N4 0.0190(17) 0.033(2) 0.0160(17) -0.0034(14) 0.0008(14) 0.0019(14) C4 0.028(2) 0.030(2) 0.016(2) 0.0023(16) -0.0047(17) -0.0054(17) C5 0.035(3) 0.034(2) 0.024(2) -0.0060(19) -0.006(2) -0.0025(19) C6 0.044(3) 0.035(3) 0.033(3) -0.005(2) -0.008(2) -0.003(2) C7 0.047(3) 0.040(3) 0.025(3) 0.006(2) -0.011(2) -0.015(2) C8 0.034(3) 0.048(3) 0.019(2) 0.008(2) -0.002(2) -0.010(2) C9 0.031(2) 0.039(2) 0.014(2) 0.0023(18) -0.0011(18) -0.0029(19) C10 0.037(3) 0.044(3) 0.032(3) 0.002(2) 0.009(2) 0.003(2) C11 0.074(5) 0.052(4) 0.050(4) 0.008(3) -0.007(3) -0.028(3) C12 0.036(3) 0.048(4) 0.067(4) -0.023(3) 0.006(3) 0.002(3) C13 0.023(2) 0.023(2) 0.021(2) 0.0017(16) -0.0036(17) -0.0006(16) C14 0.025(2) 0.029(2) 0.022(2) 0.0027(17) 0.0008(18) 0.0027(17) C15 0.036(2) 0.028(2) 0.025(2) -0.0044(18) -0.003(2) 0.0080(18) C16 0.039(3) 0.028(2) 0.029(3) 0.0023(19) -0.010(2) 0.000(2) C17 0.029(2) 0.030(2) 0.030(3) 0.0059(18) -0.002(2) -0.0043(19) C18 0.031(2) 0.028(2) 0.019(2) 0.0014(17) -0.0010(18) -0.0011(18) C19 0.034(3) 0.040(3) 0.036(3) -0.007(2) 0.017(2) -0.008(2) C20 0.032(3) 0.038(3) 0.034(3) -0.006(2) 0.008(2) 0.003(2) C21 0.045(3) 0.034(3) 0.043(3) -0.006(2) -0.012(3) -0.002(2) C22 0.022(2) 0.028(2) 0.0179(19) 0.0016(17) -0.0029(15) 0.0021(17) C23 0.028(2) 0.046(3) 0.0156(19) 0.0021(19) -0.0002(17) 0.000(2) C24 0.025(2) 0.045(3) 0.015(2) -0.0034(19) -0.0040(17) 0.0035(19) C25 0.029(2) 0.039(2) 0.011(2) 0.0044(17) -0.0010(17) -0.0062(18) C26 0.046(3) 0.038(3) 0.015(2) 0.0061(19) 0.001(2) -0.005(2) C27 0.071(3) 0.040(3) 0.023(3) 0.002(2) 0.004(3) -0.021(3) C28 0.057(3) 0.069(3) 0.022(3) 0.005(3) 0.002(3) -0.033(3) C29 0.030(3) 0.075(3) 0.019(2) 0.006(2) 0.003(2) -0.017(2) C30 0.025(2) 0.052(3) 0.016(2) 0.008(2) 0.0023(18) -0.0053(19) C31 0.030(3) 0.060(3) 0.025(3) 0.001(2) 0.003(2) 0.010(2) C32 0.085(5) 0.096(6) 0.047(4) -0.005(4) 0.007(4) -0.055(5) C33 0.057(3) 0.029(3) 0.036(3) 0.005(2) 0.006(3) 0.005(2) C34 0.021(2) 0.035(2) 0.018(2) -0.0021(18) -0.0029(17) 0.0016(17) C35 0.019(2) 0.036(2) 0.017(2) 0.0008(17) -0.0053(16) 0.0068(17) C36 0.019(2) 0.044(3) 0.023(2) 0.003(2) -0.0016(18) 0.0078(18) C37 0.023(2) 0.045(3) 0.029(3) 0.008(2) -0.0048(19) 0.0000(19) C38 0.030(2) 0.033(3) 0.031(3) 0.002(2) -0.006(2) -0.0004(19) C39 0.027(2) 0.036(2) 0.023(2) -0.0048(19) -0.0058(19) 0.0041(18) C40 0.038(3) 0.040(3) 0.035(3) -0.012(2) -0.003(2) 0.007(2) C41 0.033(3) 0.057(4) 0.056(4) 0.011(3) 0.007(3) -0.005(3) C42 0.020(2) 0.035(2) 0.021(2) -0.0021(18) -0.0065(17) 0.0070(18) C43 0.023(2) 0.037(3) 0.022(2) -0.0039(19) 0.0048(18) -0.0028(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 C1 2.027(4) . ? Pt1 C22 2.052(4) . ? Pt1 C43 2.096(4) . ? Pt1 C42 2.105(4) . ? N1 C1 1.367(6) . ? N1 C2 1.390(6) . ? N1 C4 1.437(6) . ? C1 N2 1.368(6) . ? N2 C3 1.399(6) . ? N2 C13 1.445(6) . ? C2 C3 1.328(7) . ? N3 C22 1.377(6) . ? N3 C23 1.409(6) . ? N3 C25 1.437(6) . ? N4 C22 1.367(6) . ? N4 C24 1.386(6) . ? N4 C34 1.438(6) . ? C4 C5 1.385(7) . ? C4 C9 1.411(7) . ? C5 C6 1.397(7) . ? C5 C12 1.504(8) . ? C6 C7 1.380(8) . ? C7 C8 1.383(8) . ? C7 C11 1.518(8) . ? C8 C9 1.392(7) . ? C9 C10 1.500(7) . ? C13 C14 1.397(6) . ? C13 C18 1.398(6) . ? C14 C15 1.394(7) . ? C14 C20 1.500(7) . ? C15 C16 1.393(7) . ? C16 C17 1.384(7) . ? C16 C21 1.510(7) . ? C17 C18 1.390(7) . ? C18 C19 1.503(7) . ? C23 C24 1.335(7) . ? C25 C26 1.386(7) . ? C25 C30 1.399(7) . ? C26 C27 1.391(8) . ? C26 C33 1.508(8) . ? C27 C28 1.387(10) . ? C28 C29 1.369(9) . ? C28 C32 1.518(8) . ? C29 C30 1.400(7) . ? C30 C31 1.505(8) . ? C34 C39 1.388(7) . ? C34 C35 1.405(6) . ? C35 C36 1.403(7) . ? C35 C42 1.497(7) . ? C36 C37 1.378(7) . ? C37 C38 1.383(7) . ? C37 C41 1.513(7) . ? C38 C39 1.401(7) . ? C39 C40 1.504(7) . ? 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 C1 Pt1 C22 108.44(17) . . ? C1 Pt1 C43 87.25(18) . . ? C22 Pt1 C43 164.11(18) . . ? C1 Pt1 C42 166.28(19) . . ? C22 Pt1 C42 79.80(18) . . ? C43 Pt1 C42 84.33(19) . . ? C1 N1 C2 111.1(4) . . ? C1 N1 C4 127.3(4) . . ? C2 N1 C4 120.7(4) . . ? N1 C1 N2 103.6(4) . . ? N1 C1 Pt1 133.4(3) . . ? N2 C1 Pt1 120.8(3) . . ? C1 N2 C3 111.0(4) . . ? C1 N2 C13 126.2(4) . . ? C3 N2 C13 122.6(4) . . ? C3 C2 N1 107.4(4) . . ? C22 N3 C23 110.6(4) . . ? C22 N3 C25 129.9(4) . . ? C23 N3 C25 119.5(4) . . ? C2 C3 N2 106.8(4) . . ? C22 N4 C24 112.0(4) . . ? C22 N4 C34 122.6(4) . . ? C24 N4 C34 124.5(4) . . ? C5 C4 C9 121.1(4) . . ? C5 C4 N1 121.1(4) . . ? C9 C4 N1 117.4(4) . . ? C4 C5 C6 118.0(5) . . ? C4 C5 C12 121.6(5) . . ? C6 C5 C12 120.3(5) . . ? C7 C6 C5 122.5(5) . . ? C6 C7 C8 118.3(5) . . ? C6 C7 C11 120.8(6) . . ? C8 C7 C11 121.0(6) . . ? C7 C8 C9 121.9(5) . . ? C8 C9 C4 118.2(5) . . ? C8 C9 C10 120.5(5) . . ? C4 C9 C10 121.3(4) . . ? C14 C13 C18 122.1(4) . . ? C14 C13 N2 117.6(4) . . ? C18 C13 N2 120.2(4) . . ? C15 C14 C13 117.6(4) . . ? C15 C14 C20 120.5(4) . . ? C13 C14 C20 122.0(4) . . ? C16 C15 C14 122.2(5) . . ? C17 C16 C15 117.9(5) . . ? C17 C16 C21 120.6(5) . . ? C15 C16 C21 121.5(5) . . ? C16 C17 C18 122.6(5) . . ? C17 C18 C13 117.6(4) . . ? C17 C18 C19 119.8(4) . . ? C13 C18 C19 122.6(4) . . ? N4 C22 N3 103.4(4) . . ? N4 C22 Pt1 118.0(3) . . ? N3 C22 Pt1 136.0(3) . . ? C24 C23 N3 106.9(4) . . ? C23 C24 N4 107.1(4) . . ? C26 C25 C30 122.1(5) . . ? C26 C25 N3 120.2(4) . . ? C30 C25 N3 117.2(4) . . ? C25 C26 C27 117.2(5) . . ? C25 C26 C33 121.5(5) . . ? C27 C26 C33 121.3(5) . . ? C28 C27 C26 122.8(6) . . ? C29 C28 C27 118.2(5) . . ? C29 C28 C32 120.9(7) . . ? C27 C28 C32 120.9(7) . . ? C28 C29 C30 121.9(6) . . ? C25 C30 C29 117.8(5) . . ? C25 C30 C31 122.3(5) . . ? C29 C30 C31 119.9(5) . . ? C39 C34 C35 123.5(4) . . ? C39 C34 N4 120.7(4) . . ? C35 C34 N4 115.6(4) . . ? C36 C35 C34 116.3(4) . . ? C36 C35 C42 124.0(4) . . ? C34 C35 C42 119.5(4) . . ? C37 C36 C35 122.0(5) . . ? C36 C37 C38 119.5(5) . . ? C36 C37 C41 120.6(5) . . ? C38 C37 C41 120.0(5) . . ? C37 C38 C39 121.6(5) . . ? C34 C39 C38 117.0(5) . . ? C34 C39 C40 122.1(5) . . ? C38 C39 C40 120.8(5) . . ? C35 C42 Pt1 99.9(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.021 _refine_diff_density_min -3.836 _refine_diff_density_rms 0.139 # Attachment 'CCDC-741813-Compound6.cif' data_nol305m _database_code_depnum_ccdc_archive 'CCDC 741813' #TrackingRef 'CCDC-741813-Compound6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((IPr)2Pt) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 N4 Pt' _chemical_formula_weight 972.25 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8035(7) _cell_length_b 26.9007(16) _cell_length_c 14.1517(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.1840(10) _cell_angle_gamma 90.00 _cell_volume 4870.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27182 _cell_measurement_theta_min 2.089 _cell_measurement_theta_max 30.525 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 2.919 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.439121 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63794 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10593 _reflns_number_gt 8818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+31.5919P] 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 10593 _refine_ls_number_parameters 548 _refine_ls_number_restraints 531 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1158 _refine_ls_goodness_of_fit_ref 1.296 _refine_ls_restrained_S_all 1.279 _refine_ls_shift/su_max 0.017 _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 0.780639(15) 0.625363(8) 0.751212(14) 0.01768(7) Uani 1 1 d U . . N1 N 0.8876(3) 0.54552(18) 0.8751(3) 0.0222(9) Uani 1 1 d U . . C1 C 0.8001(4) 0.5734(2) 0.8499(4) 0.0194(10) Uani 1 1 d U . . N2 N 0.7273(3) 0.55570(18) 0.9108(3) 0.0216(9) Uani 1 1 d U . . C2 C 0.8677(4) 0.5122(2) 0.9475(4) 0.0263(12) Uani 1 1 d U . . H2 H 0.9157 0.4891 0.9755 0.032 Uiso 1 1 calc R . . N3 N 0.8182(4) 0.71674(18) 0.6311(3) 0.0244(10) Uani 1 1 d U . . C3 C 0.7697(4) 0.5186(2) 0.9697(4) 0.0267(12) Uani 1 1 d U . . H3 H 0.7343 0.5012 1.0173 0.032 Uiso 1 1 calc R . . N4 N 0.6729(4) 0.68213(18) 0.5906(3) 0.0246(10) Uani 1 1 d U . . C4 C 0.9898(4) 0.5500(2) 0.8371(4) 0.0244(11) Uani 1 1 d U . . C5 C 1.0587(4) 0.5854(2) 0.8748(4) 0.0274(11) Uani 1 1 d U . . C6 C 1.1591(5) 0.5867(3) 0.8382(5) 0.0357(14) Uani 1 1 d U . . H6 H 1.2080 0.6108 0.8610 0.043 Uiso 1 1 calc R . . C7 C 1.1876(5) 0.5534(3) 0.7697(5) 0.0396(15) Uani 1 1 d U . . H7 H 1.2555 0.5552 0.7451 0.048 Uiso 1 1 calc R . . C8 C 1.1188(5) 0.5178(3) 0.7368(5) 0.0391(14) Uani 1 1 d U . . H8 H 1.1411 0.4943 0.6916 0.047 Uiso 1 1 calc R . . C9 C 1.0176(5) 0.5153(2) 0.7677(5) 0.0326(13) Uani 1 1 d U . . C10 C 0.9411(6) 0.4766(3) 0.7295(6) 0.0458(16) Uani 1 1 d U . . H10 H 0.8818 0.4757 0.7735 0.055 Uiso 1 1 calc R . . C11 C 0.9870(8) 0.4247(3) 0.7278(9) 0.074(3) Uani 1 1 d U . . H11A H 1.0382 0.4227 0.6782 0.111 Uiso 1 1 calc R . . H11B H 0.9310 0.4005 0.7148 0.111 Uiso 1 1 calc R . . H11C H 1.0215 0.4174 0.7892 0.111 Uiso 1 1 calc R . . C12 C 0.8958(9) 0.4928(4) 0.6333(8) 0.088(3) Uani 1 1 d U . . H12A H 0.8689 0.5268 0.6376 0.132 Uiso 1 1 calc R . . H12B H 0.8388 0.4703 0.6134 0.132 Uiso 1 1 calc R . . H12C H 0.9507 0.4917 0.5868 0.132 Uiso 1 1 calc R . . C13 C 1.0284(5) 0.6206(2) 0.9523(5) 0.0304(12) Uani 1 1 d U . . H13 H 0.9687 0.6053 0.9853 0.037 Uiso 1 1 calc R . . C14 C 0.9916(5) 0.6697(3) 0.9122(5) 0.0374(15) Uani 1 1 d U . . H14A H 1.0501 0.6867 0.8832 0.056 Uiso 1 1 calc R . . H14B H 0.9652 0.6904 0.9631 0.056 Uiso 1 1 calc R . . H14C H 0.9356 0.6640 0.8643 0.056 Uiso 1 1 calc R . . C15 C 1.1173(6) 0.6294(3) 1.0267(5) 0.0428(16) Uani 1 1 d U . . H15A H 1.1723 0.6493 0.9989 0.064 Uiso 1 1 calc R . . H15B H 1.1462 0.5973 1.0477 0.064 Uiso 1 1 calc R . . H15C H 1.0898 0.6471 1.0810 0.064 Uiso 1 1 calc R . . C16 C 0.6247(4) 0.5749(2) 0.9248(4) 0.0233(10) Uani 1 1 d U . . C17 C 0.6158(5) 0.6163(2) 0.9836(4) 0.0278(11) Uani 1 1 d U . . C18 C 0.5156(5) 0.6303(3) 1.0085(5) 0.0355(13) Uani 1 1 d U . . H18 H 0.5069 0.6578 1.0496 0.043 Uiso 1 1 calc R . . C19 C 0.4287(5) 0.6045(3) 0.9741(5) 0.0377(14) Uani 1 1 d U . . H19 H 0.3608 0.6143 0.9918 0.045 Uiso 1 1 calc R . . C20 C 0.4404(5) 0.5645(3) 0.9138(5) 0.0329(13) Uani 1 1 d U . . H20 H 0.3802 0.5476 0.8894 0.039 Uiso 1 1 calc R . . C21 C 0.5384(4) 0.5488(2) 0.8886(4) 0.0260(11) Uani 1 1 d U . . C22 C 0.5521(5) 0.5044(2) 0.8223(4) 0.0300(12) Uani 1 1 d U . . H22 H 0.6155 0.4857 0.8456 0.036 Uiso 1 1 calc R . . C23 C 0.5726(6) 0.5226(3) 0.7230(5) 0.0469(18) Uani 1 1 d U . . H23A H 0.5811 0.4940 0.6811 0.070 Uiso 1 1 calc R . . H23B H 0.6364 0.5427 0.7243 0.070 Uiso 1 1 calc R . . H23C H 0.5135 0.5428 0.6995 0.070 Uiso 1 1 calc R . . C24 C 0.4607(5) 0.4685(3) 0.8208(5) 0.0393(15) Uani 1 1 d U . . H24A H 0.3980 0.4852 0.7946 0.059 Uiso 1 1 calc R . . H24B H 0.4483 0.4573 0.8853 0.059 Uiso 1 1 calc R . . H24C H 0.4767 0.4397 0.7814 0.059 Uiso 1 1 calc R . . C25 C 0.7109(5) 0.6444(3) 1.0229(5) 0.0321(13) Uani 1 1 d U . . H25 H 0.7731 0.6321 0.9892 0.039 Uiso 1 1 calc R . . C26 C 0.6999(7) 0.7000(3) 1.0023(6) 0.055(2) Uani 1 1 d U . . H26A H 0.6373 0.7128 1.0318 0.082 Uiso 1 1 calc R . . H26B H 0.6935 0.7053 0.9338 0.082 Uiso 1 1 calc R . . H26C H 0.7616 0.7176 1.0280 0.082 Uiso 1 1 calc R . . C27 C 0.7302(6) 0.6341(3) 1.1278(5) 0.0448(17) Uani 1 1 d U . . H27A H 0.6681 0.6434 1.1621 0.067 Uiso 1 1 calc R . . H27B H 0.7902 0.6537 1.1516 0.067 Uiso 1 1 calc R . . H27C H 0.7447 0.5986 1.1372 0.067 Uiso 1 1 calc R . . C28 C 0.7570(4) 0.6768(2) 0.6538(4) 0.0224(10) Uani 1 1 d U . . C29 C 0.7723(5) 0.7452(2) 0.5585(5) 0.0332(13) Uani 1 1 d U . . H29 H 0.8003 0.7744 0.5316 0.040 Uiso 1 1 calc R . . C30 C 0.6819(5) 0.7236(2) 0.5339(5) 0.0317(13) Uani 1 1 d U . . H30 H 0.6329 0.7345 0.4864 0.038 Uiso 1 1 calc R . . C31 C 0.9207(4) 0.7278(2) 0.6723(4) 0.0266(11) Uani 1 1 d U . . C32 C 1.0058(5) 0.7016(2) 0.6404(5) 0.0301(12) Uani 1 1 d U . . C33 C 1.1045(5) 0.7140(3) 0.6785(5) 0.0371(14) Uani 1 1 d U . . H33 H 1.1641 0.6960 0.6597 0.044 Uiso 1 1 calc R . . C34 C 1.1168(5) 0.7524(3) 0.7435(5) 0.0379(14) Uani 1 1 d U . . H34 H 1.1844 0.7607 0.7686 0.046 Uiso 1 1 calc R . . C35 C 1.0306(5) 0.7785(3) 0.7718(5) 0.0375(14) Uani 1 1 d U . . H35 H 1.0400 0.8053 0.8150 0.045 Uiso 1 1 calc R . . C36 C 0.9307(5) 0.7666(2) 0.7385(5) 0.0310(12) Uani 1 1 d U . . C37 C 0.8370(6) 0.7953(3) 0.7724(6) 0.0428(15) Uani 1 1 d U . . H37 H 0.7716 0.7773 0.7519 0.051 Uiso 1 1 calc R . . C38 C 0.8415(8) 0.7993(4) 0.8807(6) 0.065(2) Uani 1 1 d U . . H38A H 0.8478 0.7660 0.9084 0.097 Uiso 1 1 calc R . . H38B H 0.7775 0.8152 0.9017 0.097 Uiso 1 1 calc R . . H38C H 0.9022 0.8194 0.9012 0.097 Uiso 1 1 calc R . . C39 C 0.8323(8) 0.8479(4) 0.7335(8) 0.071(3) Uani 1 1 d U . . H39A H 0.8942 0.8664 0.7563 0.106 Uiso 1 1 calc R . . H39B H 0.7692 0.8644 0.7548 0.106 Uiso 1 1 calc R . . H39C H 0.8305 0.8468 0.6642 0.106 Uiso 1 1 calc R . . C40 C 0.9925(6) 0.6626(3) 0.5641(5) 0.0383(14) Uani 1 1 d U . . H40 H 0.9190 0.6501 0.5663 0.046 Uiso 1 1 calc R . . C41 C 1.0626(11) 0.6185(4) 0.5777(9) 0.094(4) Uani 1 1 d U . . H41A H 1.1344 0.6278 0.5641 0.141 Uiso 1 1 calc R . . H41B H 1.0392 0.5918 0.5348 0.141 Uiso 1 1 calc R . . H41C H 1.0601 0.6069 0.6433 0.141 Uiso 1 1 calc R . . C42 C 1.0047(12) 0.6844(4) 0.4678(7) 0.089(3) Uani 1 1 d U . . H42A H 1.0784 0.6925 0.4592 0.133 Uiso 1 1 calc R . . H42B H 0.9625 0.7147 0.4614 0.133 Uiso 1 1 calc R . . H42C H 0.9812 0.6603 0.4196 0.133 Uiso 1 1 calc R . . C43 C 0.5820(4) 0.6505(2) 0.5839(4) 0.0246(11) Uani 1 1 d U . . C44 C 0.5833(5) 0.6090(2) 0.5239(4) 0.0273(11) Uani 1 1 d U . . C45 C 0.4893(5) 0.5835(3) 0.5087(5) 0.0338(13) Uani 1 1 d U . . H45 H 0.4872 0.5554 0.4680 0.041 Uiso 1 1 calc R . . C46 C 0.3996(5) 0.5982(3) 0.5513(5) 0.0363(14) Uani 1 1 d U . . H46 H 0.3358 0.5811 0.5380 0.044 Uiso 1 1 calc R . . C47 C 0.4022(5) 0.6379(3) 0.6136(5) 0.0354(14) Uani 1 1 d U . . H47 H 0.3407 0.6467 0.6452 0.043 Uiso 1 1 calc R . . C48 C 0.4931(5) 0.6650(2) 0.6306(5) 0.0301(12) Uani 1 1 d U . . C49 C 0.4967(5) 0.7076(3) 0.7010(5) 0.0385(14) Uani 1 1 d U . . H49 H 0.5705 0.7198 0.7063 0.046 Uiso 1 1 calc R . . C50 C 0.4665(11) 0.6907(4) 0.7979(6) 0.087(3) Uani 1 1 d U . . H50A H 0.3939 0.6792 0.7950 0.131 Uiso 1 1 calc R . . H50B H 0.4737 0.7186 0.8423 0.131 Uiso 1 1 calc R . . H50C H 0.5125 0.6635 0.8192 0.131 Uiso 1 1 calc R . . C51 C 0.4283(8) 0.7509(3) 0.6702(7) 0.062(2) Uani 1 1 d U . . H51A H 0.3547 0.7417 0.6751 0.094 Uiso 1 1 calc R . . H51B H 0.4419 0.7595 0.6045 0.094 Uiso 1 1 calc R . . H51C H 0.4440 0.7796 0.7110 0.094 Uiso 1 1 calc R . . C52 C 0.6842(5) 0.5919(2) 0.4812(5) 0.0307(12) Uani 1 1 d U . . H52 H 0.7431 0.6013 0.5261 0.037 Uiso 1 1 calc R . . C53 C 0.6875(6) 0.5353(3) 0.4682(5) 0.0419(16) Uani 1 1 d U . . H53A H 0.6733 0.5190 0.5283 0.063 Uiso 1 1 calc R . . H53B H 0.7567 0.5254 0.4478 0.063 Uiso 1 1 calc R . . H53C H 0.6344 0.5253 0.4202 0.063 Uiso 1 1 calc R . . C54 C 0.7029(6) 0.6176(3) 0.3863(5) 0.0469(18) Uani 1 1 d U . . H54A H 0.6475 0.6082 0.3401 0.070 Uiso 1 1 calc R . . H54B H 0.7708 0.6073 0.3632 0.070 Uiso 1 1 calc R . . H54C H 0.7024 0.6537 0.3951 0.070 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 0.01788(10) 0.01642(10) 0.01866(10) 0.00159(8) -0.00026(7) 0.00040(8) N1 0.018(2) 0.022(2) 0.027(2) 0.0044(18) -0.0010(17) -0.0002(17) C1 0.016(2) 0.022(3) 0.021(2) -0.0022(19) 0.0016(18) -0.0010(19) N2 0.016(2) 0.025(2) 0.024(2) 0.0060(18) 0.0009(17) -0.0036(17) C2 0.023(3) 0.024(3) 0.032(3) 0.009(2) -0.004(2) -0.001(2) N3 0.026(2) 0.020(2) 0.028(2) 0.0030(18) -0.0020(18) -0.0035(18) C3 0.018(2) 0.031(3) 0.031(3) 0.012(2) -0.003(2) -0.003(2) N4 0.023(2) 0.023(2) 0.027(2) 0.0049(19) -0.0051(18) -0.0021(18) C4 0.017(2) 0.029(3) 0.028(3) 0.002(2) 0.001(2) 0.004(2) C5 0.018(2) 0.031(3) 0.033(3) 0.006(2) -0.003(2) 0.000(2) C6 0.021(3) 0.044(4) 0.042(3) 0.007(3) -0.001(2) -0.003(2) C7 0.020(3) 0.054(4) 0.045(4) 0.009(3) 0.009(3) 0.006(3) C8 0.033(3) 0.045(4) 0.041(4) -0.002(3) 0.007(3) 0.011(3) C9 0.024(3) 0.033(3) 0.041(3) -0.004(2) 0.000(2) 0.009(2) C10 0.038(4) 0.041(4) 0.058(4) -0.019(3) 0.002(3) 0.003(3) C11 0.064(6) 0.039(4) 0.119(8) -0.018(5) 0.007(5) 0.001(4) C12 0.095(8) 0.083(7) 0.083(7) -0.016(5) -0.046(6) -0.007(6) C13 0.026(3) 0.029(3) 0.036(3) 0.002(2) -0.002(2) -0.002(2) C14 0.033(3) 0.037(3) 0.041(4) -0.004(3) -0.009(3) 0.004(3) C15 0.046(4) 0.034(4) 0.047(4) -0.003(3) -0.017(3) -0.001(3) C16 0.019(2) 0.030(3) 0.021(2) 0.005(2) 0.0036(19) 0.001(2) C17 0.027(3) 0.032(3) 0.024(3) 0.004(2) 0.002(2) 0.003(2) C18 0.033(3) 0.041(4) 0.033(3) 0.000(3) 0.007(2) 0.009(3) C19 0.024(3) 0.053(4) 0.037(3) 0.005(3) 0.009(2) 0.011(3) C20 0.022(3) 0.043(3) 0.034(3) 0.006(3) 0.000(2) 0.000(2) C21 0.020(2) 0.032(3) 0.027(3) 0.007(2) 0.002(2) -0.002(2) C22 0.021(3) 0.036(3) 0.033(3) 0.000(2) -0.002(2) -0.004(2) C23 0.055(5) 0.050(4) 0.035(3) -0.003(3) 0.005(3) -0.021(4) C24 0.036(4) 0.036(4) 0.046(4) 0.006(3) -0.003(3) -0.010(3) C25 0.029(3) 0.035(3) 0.032(3) -0.003(3) 0.004(2) -0.005(2) C26 0.078(6) 0.036(4) 0.050(4) 0.006(3) -0.007(4) -0.015(4) C27 0.047(4) 0.044(4) 0.042(4) 0.002(3) -0.011(3) -0.009(3) C28 0.020(2) 0.020(2) 0.027(3) -0.002(2) 0.001(2) -0.0018(19) C29 0.030(3) 0.030(3) 0.039(3) 0.012(3) -0.004(2) -0.002(2) C30 0.029(3) 0.030(3) 0.036(3) 0.009(2) -0.008(2) 0.001(2) C31 0.022(2) 0.029(3) 0.029(3) 0.003(2) -0.001(2) -0.007(2) C32 0.027(3) 0.030(3) 0.033(3) 0.004(2) 0.001(2) -0.003(2) C33 0.024(3) 0.043(4) 0.044(4) 0.004(3) 0.003(3) -0.003(3) C34 0.025(3) 0.048(4) 0.040(3) 0.004(3) -0.003(3) -0.015(3) C35 0.036(3) 0.038(3) 0.038(3) -0.001(3) -0.003(3) -0.013(3) C36 0.031(3) 0.028(3) 0.035(3) 0.001(2) 0.005(2) -0.008(2) C37 0.037(3) 0.038(3) 0.053(4) -0.013(3) 0.008(3) -0.007(3) C38 0.083(6) 0.059(5) 0.054(4) -0.001(4) 0.028(4) 0.005(5) C39 0.073(6) 0.060(5) 0.081(6) 0.017(5) 0.022(5) 0.026(5) C40 0.040(4) 0.031(3) 0.043(3) -0.003(3) 0.006(3) -0.002(3) C41 0.134(9) 0.056(6) 0.090(7) -0.024(5) -0.031(7) 0.046(6) C42 0.169(11) 0.054(6) 0.043(4) -0.008(4) 0.008(6) -0.008(6) C43 0.018(2) 0.027(3) 0.028(3) 0.004(2) -0.008(2) 0.001(2) C44 0.027(3) 0.030(3) 0.025(3) 0.000(2) -0.005(2) 0.000(2) C45 0.031(3) 0.033(3) 0.036(3) -0.001(3) -0.007(2) -0.005(2) C46 0.022(3) 0.039(3) 0.047(4) 0.000(3) -0.010(2) -0.007(2) C47 0.020(3) 0.040(3) 0.045(4) 0.001(3) -0.002(2) 0.004(2) C48 0.022(3) 0.035(3) 0.034(3) 0.000(2) -0.006(2) 0.006(2) C49 0.029(3) 0.043(4) 0.044(4) -0.009(3) 0.000(3) 0.009(3) C50 0.158(10) 0.067(6) 0.037(4) 0.001(4) -0.001(5) 0.021(7) C51 0.083(6) 0.046(5) 0.058(5) 0.001(4) -0.003(5) 0.022(4) C52 0.025(3) 0.036(3) 0.031(3) -0.005(2) -0.001(2) -0.002(2) C53 0.048(4) 0.038(3) 0.040(4) -0.002(3) 0.008(3) 0.006(3) C54 0.051(4) 0.049(4) 0.042(4) 0.007(3) 0.013(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 C28 1.968(6) . ? Pt1 C1 1.985(6) . ? N1 C1 1.384(7) . ? N1 C2 1.392(7) . ? N1 C4 1.439(7) . ? C1 N2 1.378(7) . ? N2 C3 1.396(7) . ? N2 C16 1.433(7) . ? C2 C3 1.316(8) . ? N3 C28 1.376(7) . ? N3 C29 1.392(8) . ? N3 C31 1.446(7) . ? N4 C28 1.381(7) . ? N4 C30 1.381(8) . ? N4 C43 1.441(7) . ? C4 C5 1.391(8) . ? C4 C9 1.411(9) . ? C5 C6 1.404(9) . ? C5 C13 1.510(9) . ? C6 C7 1.379(10) . ? C7 C8 1.372(10) . ? C8 C9 1.385(9) . ? C9 C10 1.514(10) . ? C10 C11 1.515(11) . ? C10 C12 1.523(13) . ? C13 C14 1.508(9) . ? C13 C15 1.538(9) . ? C16 C21 1.390(8) . ? C16 C17 1.398(9) . ? C17 C18 1.395(8) . ? C17 C25 1.521(9) . ? C18 C19 1.384(10) . ? C19 C20 1.384(10) . ? C20 C21 1.384(8) . ? C21 C22 1.533(9) . ? C22 C24 1.517(9) . ? C22 C23 1.521(9) . ? C25 C27 1.521(10) . ? C25 C26 1.530(10) . ? C29 C30 1.329(9) . ? C31 C32 1.388(9) . ? C31 C36 1.406(9) . ? C32 C33 1.395(9) . ? C32 C40 1.512(9) . ? C33 C34 1.389(10) . ? C34 C35 1.380(10) . ? C35 C36 1.383(9) . ? C36 C37 1.519(10) . ? C37 C39 1.518(12) . ? C37 C38 1.535(11) . ? C40 C41 1.496(11) . ? C40 C42 1.498(12) . ? C43 C48 1.394(9) . ? C43 C44 1.404(9) . ? C44 C45 1.395(9) . ? C44 C52 1.519(9) . ? C45 C46 1.376(10) . ? C46 C47 1.385(10) . ? C47 C48 1.387(9) . ? C48 C49 1.517(9) . ? C49 C50 1.508(12) . ? C49 C51 1.512(10) . ? C52 C53 1.533(9) . ? C52 C54 1.538(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Pt1 C1 178.3(2) . . ? C1 N1 C2 111.7(5) . . ? C1 N1 C4 126.7(5) . . ? C2 N1 C4 121.6(5) . . ? N2 C1 N1 102.2(4) . . ? N2 C1 Pt1 127.9(4) . . ? N1 C1 Pt1 129.9(4) . . ? C1 N2 C3 111.3(5) . . ? C1 N2 C16 127.4(5) . . ? C3 N2 C16 120.9(5) . . ? C3 C2 N1 107.1(5) . . ? C28 N3 C29 111.9(5) . . ? C28 N3 C31 125.6(5) . . ? C29 N3 C31 122.4(5) . . ? C2 C3 N2 107.7(5) . . ? C28 N4 C30 112.3(5) . . ? C28 N4 C43 126.1(5) . . ? C30 N4 C43 121.5(5) . . ? C5 C4 C9 123.2(5) . . ? C5 C4 N1 119.1(5) . . ? C9 C4 N1 117.5(5) . . ? C4 C5 C6 116.8(6) . . ? C4 C5 C13 122.1(5) . . ? C6 C5 C13 121.1(6) . . ? C7 C6 C5 121.0(6) . . ? C8 C7 C6 120.5(6) . . ? C7 C8 C9 121.6(7) . . ? C8 C9 C4 116.8(6) . . ? C8 C9 C10 121.4(6) . . ? C4 C9 C10 121.8(6) . . ? C11 C10 C9 113.1(7) . . ? C11 C10 C12 112.6(8) . . ? C9 C10 C12 109.9(7) . . ? C14 C13 C5 111.2(5) . . ? C14 C13 C15 109.6(5) . . ? C5 C13 C15 112.9(5) . . ? C21 C16 C17 122.7(5) . . ? C21 C16 N2 119.2(5) . . ? C17 C16 N2 117.7(5) . . ? C18 C17 C16 117.5(6) . . ? C18 C17 C25 120.3(6) . . ? C16 C17 C25 122.1(5) . . ? C19 C18 C17 120.7(6) . . ? C20 C19 C18 120.1(6) . . ? C19 C20 C21 121.2(6) . . ? C20 C21 C16 117.8(6) . . ? C20 C21 C22 121.5(6) . . ? C16 C21 C22 120.8(5) . . ? C24 C22 C23 110.6(6) . . ? C24 C22 C21 113.5(5) . . ? C23 C22 C21 110.0(6) . . ? C17 C25 C27 111.4(5) . . ? C17 C25 C26 110.4(6) . . ? C27 C25 C26 112.0(6) . . ? N3 C28 N4 101.8(5) . . ? N3 C28 Pt1 129.7(4) . . ? N4 C28 Pt1 128.5(4) . . ? C30 C29 N3 107.0(5) . . ? C29 C30 N4 107.0(5) . . ? C32 C31 C36 122.8(6) . . ? C32 C31 N3 118.4(5) . . ? C36 C31 N3 118.7(6) . . ? C31 C32 C33 117.7(6) . . ? C31 C32 C40 121.1(6) . . ? C33 C32 C40 121.2(6) . . ? C34 C33 C32 120.7(6) . . ? C35 C34 C33 120.0(6) . . ? C34 C35 C36 121.5(7) . . ? C35 C36 C31 117.2(6) . . ? C35 C36 C37 120.4(6) . . ? C31 C36 C37 122.3(6) . . ? C39 C37 C36 112.3(6) . . ? C39 C37 C38 107.2(7) . . ? C36 C37 C38 110.5(7) . . ? C41 C40 C42 110.2(9) . . ? C41 C40 C32 114.1(7) . . ? C42 C40 C32 111.4(6) . . ? C48 C43 C44 122.5(5) . . ? C48 C43 N4 118.5(5) . . ? C44 C43 N4 118.7(5) . . ? C45 C44 C43 117.0(6) . . ? C45 C44 C52 122.1(6) . . ? C43 C44 C52 120.8(5) . . ? C46 C45 C44 121.5(6) . . ? C45 C46 C47 120.0(6) . . ? C46 C47 C48 121.1(6) . . ? C47 C48 C43 117.8(6) . . ? C47 C48 C49 121.0(6) . . ? C43 C48 C49 121.1(6) . . ? C50 C49 C51 109.1(7) . . ? C50 C49 C48 111.6(7) . . ? C51 C49 C48 112.9(6) . . ? C44 C52 C53 112.1(5) . . ? C44 C52 C54 112.0(5) . . ? C53 C52 C54 109.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 0.6(6) . . . . ? C4 N1 C1 N2 -176.9(5) . . . . ? C2 N1 C1 Pt1 -178.9(4) . . . . ? C4 N1 C1 Pt1 3.7(8) . . . . ? C28 Pt1 C1 N2 -11(8) . . . . ? C28 Pt1 C1 N1 168(7) . . . . ? N1 C1 N2 C3 -0.2(6) . . . . ? Pt1 C1 N2 C3 179.3(4) . . . . ? N1 C1 N2 C16 172.2(5) . . . . ? Pt1 C1 N2 C16 -8.3(8) . . . . ? C1 N1 C2 C3 -0.7(7) . . . . ? C4 N1 C2 C3 176.8(5) . . . . ? N1 C2 C3 N2 0.6(7) . . . . ? C1 N2 C3 C2 -0.3(7) . . . . ? C16 N2 C3 C2 -173.2(5) . . . . ? C1 N1 C4 C5 84.4(7) . . . . ? C2 N1 C4 C5 -92.8(7) . . . . ? C1 N1 C4 C9 -100.2(7) . . . . ? C2 N1 C4 C9 82.6(7) . . . . ? C9 C4 C5 C6 2.1(9) . . . . ? N1 C4 C5 C6 177.2(5) . . . . ? C9 C4 C5 C13 -177.1(6) . . . . ? N1 C4 C5 C13 -2.1(9) . . . . ? C4 C5 C6 C7 -1.4(10) . . . . ? C13 C5 C6 C7 177.8(6) . . . . ? C5 C6 C7 C8 -1.0(11) . . . . ? C6 C7 C8 C9 2.8(11) . . . . ? C7 C8 C9 C4 -2.1(10) . . . . ? C7 C8 C9 C10 178.6(7) . . . . ? C5 C4 C9 C8 -0.4(10) . . . . ? N1 C4 C9 C8 -175.5(6) . . . . ? C5 C4 C9 C10 178.9(6) . . . . ? N1 C4 C9 C10 3.7(9) . . . . ? C8 C9 C10 C11 47.3(11) . . . . ? C4 C9 C10 C11 -131.9(8) . . . . ? C8 C9 C10 C12 -79.5(9) . . . . ? C4 C9 C10 C12 101.3(9) . . . . ? C4 C5 C13 C14 -95.8(7) . . . . ? C6 C5 C13 C14 85.0(7) . . . . ? C4 C5 C13 C15 140.5(6) . . . . ? C6 C5 C13 C15 -38.7(8) . . . . ? C1 N2 C16 C21 106.3(7) . . . . ? C3 N2 C16 C21 -81.9(7) . . . . ? C1 N2 C16 C17 -80.7(7) . . . . ? C3 N2 C16 C17 91.1(7) . . . . ? C21 C16 C17 C18 2.3(9) . . . . ? N2 C16 C17 C18 -170.5(5) . . . . ? C21 C16 C17 C25 179.8(6) . . . . ? N2 C16 C17 C25 7.1(8) . . . . ? C16 C17 C18 C19 -1.5(9) . . . . ? C25 C17 C18 C19 -179.1(6) . . . . ? C17 C18 C19 C20 -0.3(10) . . . . ? C18 C19 C20 C21 1.5(10) . . . . ? C19 C20 C21 C16 -0.8(9) . . . . ? C19 C20 C21 C22 179.7(6) . . . . ? C17 C16 C21 C20 -1.1(9) . . . . ? N2 C16 C21 C20 171.5(5) . . . . ? C17 C16 C21 C22 178.4(5) . . . . ? N2 C16 C21 C22 -8.9(8) . . . . ? C20 C21 C22 C24 -23.6(8) . . . . ? C16 C21 C22 C24 156.9(6) . . . . ? C20 C21 C22 C23 100.9(7) . . . . ? C16 C21 C22 C23 -78.6(7) . . . . ? C18 C17 C25 C27 70.7(8) . . . . ? C16 C17 C25 C27 -106.8(7) . . . . ? C18 C17 C25 C26 -54.4(8) . . . . ? C16 C17 C25 C26 128.1(7) . . . . ? C29 N3 C28 N4 0.9(7) . . . . ? C31 N3 C28 N4 -176.1(5) . . . . ? C29 N3 C28 Pt1 -178.7(5) . . . . ? C31 N3 C28 Pt1 4.3(9) . . . . ? C30 N4 C28 N3 -1.1(7) . . . . ? C43 N4 C28 N3 -178.6(5) . . . . ? C30 N4 C28 Pt1 178.5(5) . . . . ? C43 N4 C28 Pt1 1.0(9) . . . . ? C1 Pt1 C28 N3 147(7) . . . . ? C1 Pt1 C28 N4 -33(8) . . . . ? C28 N3 C29 C30 -0.4(8) . . . . ? C31 N3 C29 C30 176.7(6) . . . . ? N3 C29 C30 N4 -0.3(8) . . . . ? C28 N4 C30 C29 0.9(8) . . . . ? C43 N4 C30 C29 178.6(6) . . . . ? C28 N3 C31 C32 79.0(8) . . . . ? C29 N3 C31 C32 -97.7(7) . . . . ? C28 N3 C31 C36 -104.8(7) . . . . ? C29 N3 C31 C36 78.5(8) . . . . ? C36 C31 C32 C33 1.8(9) . . . . ? N3 C31 C32 C33 177.7(6) . . . . ? C36 C31 C32 C40 -175.6(6) . . . . ? N3 C31 C32 C40 0.3(9) . . . . ? C31 C32 C33 C34 -2.2(10) . . . . ? C40 C32 C33 C34 175.2(6) . . . . ? C32 C33 C34 C35 0.5(11) . . . . ? C33 C34 C35 C36 1.6(11) . . . . ? C34 C35 C36 C31 -2.0(10) . . . . ? C34 C35 C36 C37 178.7(7) . . . . ? C32 C31 C36 C35 0.3(10) . . . . ? N3 C31 C36 C35 -175.7(6) . . . . ? C32 C31 C36 C37 179.6(6) . . . . ? N3 C31 C36 C37 3.6(9) . . . . ? C35 C36 C37 C39 70.9(10) . . . . ? C31 C36 C37 C39 -108.3(8) . . . . ? C35 C36 C37 C38 -48.7(9) . . . . ? C31 C36 C37 C38 132.0(7) . . . . ? C31 C32 C40 C41 -143.1(9) . . . . ? C33 C32 C40 C41 39.6(11) . . . . ? C31 C32 C40 C42 91.3(9) . . . . ? C33 C32 C40 C42 -86.0(10) . . . . ? C28 N4 C43 C48 95.8(7) . . . . ? C30 N4 C43 C48 -81.5(7) . . . . ? C28 N4 C43 C44 -89.9(7) . . . . ? C30 N4 C43 C44 92.8(7) . . . . ? C48 C43 C44 C45 3.0(9) . . . . ? N4 C43 C44 C45 -171.0(5) . . . . ? C48 C43 C44 C52 -174.6(6) . . . . ? N4 C43 C44 C52 11.4(8) . . . . ? C43 C44 C45 C46 -0.6(10) . . . . ? C52 C44 C45 C46 177.0(6) . . . . ? C44 C45 C46 C47 -2.5(11) . . . . ? C45 C46 C47 C48 3.2(11) . . . . ? C46 C47 C48 C43 -0.8(10) . . . . ? C46 C47 C48 C49 -178.2(6) . . . . ? C44 C43 C48 C47 -2.4(9) . . . . ? N4 C43 C48 C47 171.7(6) . . . . ? C44 C43 C48 C49 175.1(6) . . . . ? N4 C43 C48 C49 -10.9(9) . . . . ? C47 C48 C49 C50 57.2(10) . . . . ? C43 C48 C49 C50 -120.1(8) . . . . ? C47 C48 C49 C51 -66.1(9) . . . . ? C43 C48 C49 C51 116.5(8) . . . . ? C45 C44 C52 C53 -30.1(8) . . . . ? C43 C44 C52 C53 147.4(6) . . . . ? C45 C44 C52 C54 93.6(8) . . . . ? C43 C44 C52 C54 -88.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.898 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.133 # Attachment 'CCDC-741814-Compound7.cif' data_nol172m _database_code_depnum_ccdc_archive 'CCDC 756172' #TrackingRef 'CCDC-741814-Compound7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Pt(ItBu)(ItBu*)(Me)2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H46 N4 Pt' _chemical_formula_weight 585.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0260(9) _cell_length_b 14.6685(11) _cell_length_c 14.7642(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.1030(10) _cell_angle_gamma 90.00 _cell_volume 2604.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.164 _cell_measurement_theta_max 28.805 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 5.405 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.576634 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31831 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6239 _reflns_number_gt 4587 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0284P)^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 6239 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.808643(13) 0.704253(11) 0.164604(10) 0.01692(5) Uani 1 1 d . . . N1 N 1.0310(3) 0.6219(2) 0.0978(2) 0.0196(8) Uani 1 1 d . . . C1 C 0.9503(3) 0.6896(3) 0.0900(3) 0.0186(9) Uani 1 1 d . . . N2 N 0.9785(3) 0.7336(2) 0.0108(2) 0.0192(8) Uani 1 1 d . . . C2 C 1.1032(3) 0.6248(3) 0.0257(3) 0.0236(10) Uani 1 1 d . . . H2 H 1.1643 0.5851 0.0163 0.028 Uiso 1 1 calc R . . N3 N 0.9227(3) 0.8159(2) 0.3356(2) 0.0207(8) Uani 1 1 d . . . C3 C 1.0712(3) 0.6933(3) -0.0277(3) 0.0274(11) Uani 1 1 d . . . H3 H 1.1053 0.7114 -0.0823 0.033 Uiso 1 1 calc R . . N4 N 0.8925(3) 0.7201(2) 0.4446(2) 0.0220(8) Uani 1 1 d . . . C4 C 1.0495(3) 0.5592(3) 0.1766(3) 0.0232(10) Uani 1 1 d . . . C5 C 1.0994(4) 0.6141(3) 0.2552(3) 0.0313(11) Uani 1 1 d . . . H5A H 1.1684 0.6432 0.2360 0.047 Uiso 1 1 calc R . . H5B H 1.1154 0.5734 0.3064 0.047 Uiso 1 1 calc R . . H5C H 1.0464 0.6611 0.2736 0.047 Uiso 1 1 calc R . . C6 C 1.1329(4) 0.4848(3) 0.1504(3) 0.0369(12) Uani 1 1 d . . . H6A H 1.1078 0.4554 0.0941 0.055 Uiso 1 1 calc R . . H6B H 1.1381 0.4392 0.1989 0.055 Uiso 1 1 calc R . . H6C H 1.2062 0.5124 0.1417 0.055 Uiso 1 1 calc R . . C7 C 0.9414(4) 0.5116(3) 0.2012(3) 0.0300(11) Uani 1 1 d . . . H7A H 0.8850 0.5575 0.2152 0.045 Uiso 1 1 calc R . . H7B H 0.9544 0.4726 0.2541 0.045 Uiso 1 1 calc R . . H7C H 0.9153 0.4743 0.1499 0.045 Uiso 1 1 calc R . . C8 C 0.9248(3) 0.8130(3) -0.0387(3) 0.0220(10) Uani 1 1 d . . . C9 C 1.0153(4) 0.8851(3) -0.0534(3) 0.0335(11) Uani 1 1 d . . . H9A H 1.0416 0.9085 0.0054 0.050 Uiso 1 1 calc R . . H9B H 0.9845 0.9353 -0.0897 0.050 Uiso 1 1 calc R . . H9C H 1.0776 0.8574 -0.0852 0.050 Uiso 1 1 calc R . . C10 C 0.8814(4) 0.7790(3) -0.1308(3) 0.0333(12) Uani 1 1 d . . . H10A H 0.9420 0.7495 -0.1632 0.050 Uiso 1 1 calc R . . H10B H 0.8532 0.8307 -0.1664 0.050 Uiso 1 1 calc R . . H10C H 0.8213 0.7350 -0.1218 0.050 Uiso 1 1 calc R . . C11 C 0.8327(4) 0.8576(3) 0.0126(3) 0.0356(12) Uani 1 1 d . . . H11A H 0.7758 0.8122 0.0265 0.053 Uiso 1 1 calc R . . H11B H 0.7994 0.9063 -0.0243 0.053 Uiso 1 1 calc R . . H11C H 0.8629 0.8834 0.0692 0.053 Uiso 1 1 calc R . . C12 C 0.9363(4) 0.8002(3) 0.4246(3) 0.0272(10) Uani 1 1 d . . . H12 H 0.9719 0.8403 0.4666 0.033 Uiso 1 1 calc R . . C13 C 0.8667(3) 0.7421(3) 0.2923(3) 0.0186(9) Uani 1 1 d . . . C14 C 0.8500(3) 0.6837(3) 0.3642(3) 0.0215(10) Uani 1 1 d . . . H14 H 0.8140 0.6262 0.3594 0.026 Uiso 1 1 calc R . . C15 C 0.9584(3) 0.9026(3) 0.2907(3) 0.0246(10) Uani 1 1 d . . . C16 C 1.0424(4) 0.8776(3) 0.2194(3) 0.0310(11) Uani 1 1 d . . . H16A H 1.1079 0.8499 0.2488 0.047 Uiso 1 1 calc R . . H16B H 1.0647 0.9327 0.1869 0.047 Uiso 1 1 calc R . . H16C H 1.0089 0.8341 0.1766 0.047 Uiso 1 1 calc R . . C17 C 0.8532(4) 0.9469(3) 0.2514(3) 0.0301(11) Uani 1 1 d . . . H17A H 0.8106 0.9017 0.2164 0.045 Uiso 1 1 calc R . . H17B H 0.8738 0.9975 0.2117 0.045 Uiso 1 1 calc R . . H17C H 0.8079 0.9700 0.3008 0.045 Uiso 1 1 calc R . . C18 C 1.0126(4) 0.9665(3) 0.3605(3) 0.0347(12) Uani 1 1 d . . . H18A H 0.9585 0.9820 0.4069 0.052 Uiso 1 1 calc R . . H18B H 1.0372 1.0222 0.3303 0.052 Uiso 1 1 calc R . . H18C H 1.0767 0.9360 0.3891 0.052 Uiso 1 1 calc R . . C19 C 0.8992(4) 0.6744(3) 0.5356(3) 0.0271(11) Uani 1 1 d . . . C20 C 1.0185(4) 0.6400(4) 0.5487(3) 0.0415(13) Uani 1 1 d . . . H20A H 1.0370 0.5990 0.4988 0.062 Uiso 1 1 calc R . . H20B H 1.0253 0.6071 0.6063 0.062 Uiso 1 1 calc R . . H20C H 1.0698 0.6920 0.5493 0.062 Uiso 1 1 calc R . . C21 C 0.8180(4) 0.5946(4) 0.5368(3) 0.0547(17) Uani 1 1 d . . . H21A H 0.7422 0.6172 0.5257 0.082 Uiso 1 1 calc R . . H21B H 0.8223 0.5645 0.5959 0.082 Uiso 1 1 calc R . . H21C H 0.8372 0.5510 0.4893 0.082 Uiso 1 1 calc R . . C22 C 0.8688(4) 0.7440(4) 0.6079(3) 0.0425(14) Uani 1 1 d . . . H22A H 0.9188 0.7966 0.6044 0.064 Uiso 1 1 calc R . . H22B H 0.8762 0.7160 0.6680 0.064 Uiso 1 1 calc R . . H22C H 0.7918 0.7641 0.5978 0.064 Uiso 1 1 calc R . . C23 C 0.7281(3) 0.6405(3) 0.0541(3) 0.0269(10) Uani 1 1 d . . . H23A H 0.7645 0.6580 -0.0021 0.040 Uiso 1 1 calc R . . H23B H 0.6500 0.6595 0.0513 0.040 Uiso 1 1 calc R . . H23C H 0.7322 0.5742 0.0616 0.040 Uiso 1 1 calc R . . C24 C 0.6532(3) 0.7136(3) 0.2232(3) 0.0269(10) Uani 1 1 d . . . H24A H 0.5965 0.6896 0.1810 0.040 Uiso 1 1 calc R . . H24B H 0.6369 0.7775 0.2367 0.040 Uiso 1 1 calc R . . H24C H 0.6531 0.6780 0.2793 0.040 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 0.01889(8) 0.01993(9) 0.01202(7) 0.00098(8) 0.00207(5) 0.00096(9) N1 0.0232(18) 0.021(2) 0.0151(17) 0.0002(15) 0.0007(14) 0.0022(16) C1 0.020(2) 0.016(3) 0.020(2) -0.0056(18) -0.0026(16) -0.0030(17) N2 0.0234(19) 0.0191(19) 0.0151(17) 0.0016(14) 0.0047(14) 0.0050(15) C2 0.019(2) 0.032(3) 0.020(2) 0.001(2) 0.0020(17) 0.0059(19) N3 0.0193(18) 0.022(2) 0.0209(18) 0.0009(15) 0.0013(14) -0.0001(15) C3 0.026(2) 0.038(3) 0.018(2) -0.006(2) 0.0069(17) 0.002(2) N4 0.0247(19) 0.026(2) 0.0156(17) -0.0001(16) -0.0007(14) 0.0003(16) C4 0.026(2) 0.025(3) 0.019(2) 0.0046(19) 0.0011(18) 0.0085(19) C5 0.032(3) 0.033(3) 0.028(2) 0.001(2) -0.004(2) 0.006(2) C6 0.045(3) 0.031(3) 0.035(3) 0.008(2) 0.001(2) 0.019(2) C7 0.039(3) 0.022(3) 0.028(2) 0.002(2) 0.002(2) 0.002(2) C8 0.028(2) 0.021(3) 0.017(2) 0.0071(18) 0.0048(17) 0.0019(18) C9 0.040(3) 0.024(3) 0.037(3) 0.007(2) 0.012(2) 0.001(2) C10 0.038(3) 0.038(3) 0.024(2) -0.002(2) -0.004(2) 0.007(2) C11 0.042(3) 0.036(3) 0.028(3) 0.014(2) 0.012(2) 0.013(2) C12 0.034(2) 0.029(3) 0.019(2) -0.004(2) -0.0018(17) -0.006(2) C13 0.019(2) 0.020(2) 0.017(2) -0.0036(18) 0.0019(16) -0.0006(18) C14 0.024(2) 0.022(3) 0.018(2) -0.0037(18) -0.0011(17) -0.0055(18) C15 0.031(2) 0.020(2) 0.022(2) 0.0009(19) 0.0028(18) -0.002(2) C16 0.035(3) 0.031(3) 0.028(2) 0.002(2) 0.010(2) -0.006(2) C17 0.036(3) 0.025(3) 0.029(3) 0.001(2) 0.000(2) 0.003(2) C18 0.046(3) 0.023(3) 0.035(3) -0.004(2) -0.001(2) -0.010(2) C19 0.028(2) 0.035(3) 0.018(2) 0.005(2) -0.0052(18) -0.005(2) C20 0.046(3) 0.048(4) 0.030(3) 0.008(2) -0.003(2) 0.011(3) C21 0.063(4) 0.076(5) 0.025(3) 0.029(3) -0.011(2) -0.030(3) C22 0.046(3) 0.060(4) 0.021(3) -0.002(3) 0.001(2) 0.019(3) C23 0.028(2) 0.030(3) 0.022(2) -0.002(2) 0.0049(19) -0.001(2) C24 0.024(2) 0.037(3) 0.019(2) 0.004(2) 0.0015(17) 0.004(2) _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 C1 2.058(4) . ? Pt1 C13 2.074(4) . ? Pt1 C24 2.079(4) . ? Pt1 C23 2.101(4) . ? N1 C2 1.387(5) . ? N1 C1 1.390(5) . ? N1 C4 1.496(5) . ? C1 N2 1.383(5) . ? N2 C3 1.392(5) . ? N2 C8 1.513(5) . ? C2 C3 1.330(6) . ? N3 C12 1.340(5) . ? N3 C13 1.420(5) . ? N3 C15 1.501(5) . ? N4 C12 1.324(5) . ? N4 C14 1.389(5) . ? N4 C19 1.503(5) . ? C4 C7 1.525(6) . ? C4 C5 1.527(6) . ? C4 C6 1.537(6) . ? C8 C11 1.504(6) . ? C8 C10 1.530(6) . ? C8 C9 1.536(6) . ? C13 C14 1.383(6) . ? C15 C16 1.518(6) . ? C15 C17 1.527(6) . ? C15 C18 1.530(6) . ? C19 C21 1.525(7) . ? C19 C22 1.527(7) . ? C19 C20 1.529(6) . ? 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 C1 Pt1 C13 104.29(15) . . ? C1 Pt1 C24 171.78(15) . . ? C13 Pt1 C24 83.93(16) . . ? C1 Pt1 C23 84.93(15) . . ? C13 Pt1 C23 165.35(16) . . ? C24 Pt1 C23 86.99(16) . . ? C2 N1 C1 111.1(3) . . ? C2 N1 C4 121.9(3) . . ? C1 N1 C4 126.7(3) . . ? N2 C1 N1 102.8(3) . . ? N2 C1 Pt1 128.5(3) . . ? N1 C1 Pt1 127.8(3) . . ? C1 N2 C3 110.9(3) . . ? C1 N2 C8 131.1(3) . . ? C3 N2 C8 117.9(3) . . ? C3 C2 N1 107.4(4) . . ? C12 N3 C13 111.1(4) . . ? C12 N3 C15 123.2(4) . . ? C13 N3 C15 125.7(3) . . ? C2 C3 N2 107.7(4) . . ? C12 N4 C14 107.0(3) . . ? C12 N4 C19 125.5(4) . . ? C14 N4 C19 127.2(4) . . ? N1 C4 C7 110.6(3) . . ? N1 C4 C5 108.4(4) . . ? C7 C4 C5 112.6(3) . . ? N1 C4 C6 109.3(3) . . ? C7 C4 C6 107.4(4) . . ? C5 C4 C6 108.4(4) . . ? C11 C8 N2 113.8(3) . . ? C11 C8 C10 110.4(4) . . ? N2 C8 C10 108.2(3) . . ? C11 C8 C9 107.6(4) . . ? N2 C8 C9 107.5(3) . . ? C10 C8 C9 109.2(3) . . ? N4 C12 N3 109.2(4) . . ? C14 C13 N3 101.6(3) . . ? C14 C13 Pt1 118.7(3) . . ? N3 C13 Pt1 139.7(3) . . ? C13 C14 N4 111.2(4) . . ? N3 C15 C16 107.6(3) . . ? N3 C15 C17 106.7(3) . . ? C16 C15 C17 113.4(4) . . ? N3 C15 C18 110.1(3) . . ? C16 C15 C18 109.5(4) . . ? C17 C15 C18 109.5(4) . . ? N4 C19 C21 109.2(3) . . ? N4 C19 C22 108.5(4) . . ? C21 C19 C22 110.1(4) . . ? N4 C19 C20 107.1(4) . . ? C21 C19 C20 110.2(4) . . ? C22 C19 C20 111.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 -0.8(4) . . . . ? C4 N1 C1 N2 172.9(4) . . . . ? C2 N1 C1 Pt1 169.1(3) . . . . ? C4 N1 C1 Pt1 -17.2(6) . . . . ? C13 Pt1 C1 N2 -122.3(4) . . . . ? C24 Pt1 C1 N2 58.5(13) . . . . ? C23 Pt1 C1 N2 69.2(4) . . . . ? C13 Pt1 C1 N1 70.3(4) . . . . ? C24 Pt1 C1 N1 -108.9(12) . . . . ? C23 Pt1 C1 N1 -98.2(4) . . . . ? N1 C1 N2 C3 0.8(4) . . . . ? Pt1 C1 N2 C3 -169.1(3) . . . . ? N1 C1 N2 C8 179.0(4) . . . . ? Pt1 C1 N2 C8 9.2(6) . . . . ? C1 N1 C2 C3 0.5(5) . . . . ? C4 N1 C2 C3 -173.5(4) . . . . ? N1 C2 C3 N2 0.0(5) . . . . ? C1 N2 C3 C2 -0.5(5) . . . . ? C8 N2 C3 C2 -179.0(4) . . . . ? C2 N1 C4 C7 -134.8(4) . . . . ? C1 N1 C4 C7 52.2(5) . . . . ? C2 N1 C4 C5 101.3(4) . . . . ? C1 N1 C4 C5 -71.8(5) . . . . ? C2 N1 C4 C6 -16.8(5) . . . . ? C1 N1 C4 C6 170.2(4) . . . . ? C1 N2 C8 C11 7.6(6) . . . . ? C3 N2 C8 C11 -174.3(4) . . . . ? C1 N2 C8 C10 -115.5(4) . . . . ? C3 N2 C8 C10 62.6(5) . . . . ? C1 N2 C8 C9 126.6(4) . . . . ? C3 N2 C8 C9 -55.2(5) . . . . ? C14 N4 C12 N3 0.4(5) . . . . ? C19 N4 C12 N3 174.6(4) . . . . ? C13 N3 C12 N4 -0.3(5) . . . . ? C15 N3 C12 N4 177.3(4) . . . . ? C12 N3 C13 C14 0.1(4) . . . . ? C15 N3 C13 C14 -177.4(4) . . . . ? C12 N3 C13 Pt1 179.1(4) . . . . ? C15 N3 C13 Pt1 1.6(7) . . . . ? C1 Pt1 C13 C14 -115.3(3) . . . . ? C24 Pt1 C13 C14 64.6(3) . . . . ? C23 Pt1 C13 C14 12.6(8) . . . . ? C1 Pt1 C13 N3 65.8(5) . . . . ? C24 Pt1 C13 N3 -114.3(5) . . . . ? C23 Pt1 C13 N3 -166.3(5) . . . . ? N3 C13 C14 N4 0.2(4) . . . . ? Pt1 C13 C14 N4 -179.1(3) . . . . ? C12 N4 C14 C13 -0.3(5) . . . . ? C19 N4 C14 C13 -174.4(4) . . . . ? C12 N3 C15 C16 120.2(4) . . . . ? C13 N3 C15 C16 -62.6(5) . . . . ? C12 N3 C15 C17 -117.8(4) . . . . ? C13 N3 C15 C17 59.4(5) . . . . ? C12 N3 C15 C18 1.0(6) . . . . ? C13 N3 C15 C18 178.2(4) . . . . ? C12 N4 C19 C21 167.6(4) . . . . ? C14 N4 C19 C21 -19.3(6) . . . . ? C12 N4 C19 C22 47.6(6) . . . . ? C14 N4 C19 C22 -139.3(4) . . . . ? C12 N4 C19 C20 -73.1(5) . . . . ? C14 N4 C19 C20 100.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.795 _refine_diff_density_min -1.710 _refine_diff_density_rms 0.137 # Attachment 'UnusualPt.cif' #------------------------ # # Complex 1 CCDC-741809 # #