data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Sreebrata Goswami' _publ_contact_author_address ; Department of Inorganic Chemistry Indian Association for the Cultivation of Science 2A &2B Raja S. C. Mullick Road Jadavpur Kolkata West Bengal 700 032 INDIA ; _publ_contact_author_email ICSG@IACS.RES.IN _publ_section_title ; Platinum Complexes of Diazo Ligands. Studies of Regioselective Aromatic Ring Amination, Oxidative Halogen Addition and Reductive Halogen Elimination Reactions ; loop_ _publ_author_name 'Sreebrata Goswami' 'Alfonso Castineiras' 'Srijit Das' 'Golam Mostafa' 'Manashi Panda' data_compound_1c _database_code_depnum_ccdc_archive 'CCDC 258038' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PtCl2(L1c)]' _chemical_formula_sum 'C11 H8 Cl3 N3 Pt' _chemical_formula_weight 483.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _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 7.3352(3) _cell_length_b 19.9225(12) _cell_length_c 9.3996(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.766(9) _cell_angle_gamma 90.00 _cell_volume 1364.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.646 _cell_measurement_theta_max 12.405 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 10.857 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.7386 _exptl_absorpt_correction_T_max 0.9770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf Nonius CAD4' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 3866 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 27.98 _reflns_number_total 3289 _reflns_number_gt 2745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4-Express Software (Nonius, 1994)' _computing_cell_refinement 'CAD4-Express Software (Nonius, 1994)' _computing_data_reduction 'GENHKL (Kretschmar, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2002)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0332P)^2^+0.1568P] 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 3289 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.21557(2) 0.045809(7) 0.556992(15) 0.02744(6) Uani 1 1 d . . . Cl1 Cl 0.28559(17) -0.05227(5) 0.67803(12) 0.0394(2) Uani 1 1 d . . . Cl2 Cl 0.1714(2) 0.09857(6) 0.76538(11) 0.0469(3) Uani 1 1 d . . . N1 N 0.1517(5) 0.11908(17) 0.2996(4) 0.0328(8) Uani 1 1 d . . . N2 N 0.1593(5) 0.12452(17) 0.4348(4) 0.0303(7) Uani 1 1 d . . . N6 N 0.2436(5) 0.00934(18) 0.3635(3) 0.0298(7) Uani 1 1 d . . . C1 C 0.1991(6) 0.0548(2) 0.2585(5) 0.0341(9) Uani 1 1 d . . . C2 C 0.2061(7) 0.0405(3) 0.1140(5) 0.0443(11) Uani 1 1 d . . . H2 H 0.1712 0.0724 0.0439 0.053 Uiso 1 1 d R . . C3 C 0.2654(7) -0.0214(3) 0.0780(5) 0.0489(13) Uani 1 1 d . . . H3 H 0.2713 -0.0326 -0.0174 0.059 Uiso 1 1 d R . . C4 C 0.3169(7) -0.0678(3) 0.1867(6) 0.0467(12) Uani 1 1 d . . . H4 H 0.3609 -0.1098 0.1639 0.056 Uiso 1 1 d R . . C5 C 0.3027(7) -0.0516(2) 0.3285(5) 0.0408(11) Uani 1 1 d . . . H5 H 0.3345 -0.0832 0.4000 0.049 Uiso 1 1 d R . . C11 C 0.1189(6) 0.1911(2) 0.4833(4) 0.0314(9) Uani 1 1 d . . . C12 C 0.2551(6) 0.2318(3) 0.5440(6) 0.0468(12) Uani 1 1 d . . . C13 C 0.2169(7) 0.2947(2) 0.5943(6) 0.0501(13) Uani 1 1 d . . . H13 H 0.3115 0.3226 0.6336 0.060 Uiso 1 1 d R . . C14 C 0.0382(7) 0.3157(2) 0.5858(6) 0.0506(13) Uani 1 1 d . . . H14 H 0.0106 0.3573 0.6230 0.061 Uiso 1 1 d R . . C15 C -0.0983(8) 0.2762(3) 0.5235(8) 0.0689(18) Uani 1 1 d . . . H15 H -0.2189 0.2915 0.5152 0.083 Uiso 1 1 d R . . C16 C -0.0606(7) 0.2130(3) 0.4718(7) 0.0567(15) Uani 1 1 d . . . H16 H -0.1552 0.1858 0.4300 0.068 Uiso 1 1 d R . . Cl3A Cl 0.4831(16) 0.2062(6) 0.542(7) 0.088(10) Uani 0.57(7) 1 d P . . Cl3B Cl 0.457(9) 0.217(3) 0.437(12) 0.072(19) Uani 0.10(3) 1 d P . . Cl3C Cl 0.476(3) 0.2047(9) 0.588(3) 0.044(4) Uani 0.33(8) 1 d P . . 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 0.03374(9) 0.02679(9) 0.02209(8) 0.00162(6) 0.00453(6) 0.00019(7) Cl1 0.0529(7) 0.0312(5) 0.0328(5) 0.0073(4) -0.0003(5) -0.0006(5) Cl2 0.0706(8) 0.0447(6) 0.0266(5) -0.0022(5) 0.0116(5) 0.0028(6) N1 0.040(2) 0.0325(19) 0.0266(17) 0.0030(14) 0.0059(15) -0.0004(15) N2 0.0327(18) 0.0278(18) 0.0305(17) 0.0040(14) 0.0038(14) -0.0011(14) N6 0.0314(18) 0.0346(19) 0.0233(16) -0.0027(14) 0.0037(13) -0.0012(15) C1 0.038(2) 0.036(2) 0.029(2) 0.0004(17) 0.0075(17) -0.0028(18) C2 0.057(3) 0.051(3) 0.026(2) 0.000(2) 0.011(2) -0.006(2) C3 0.053(3) 0.066(3) 0.029(2) -0.014(2) 0.008(2) -0.007(3) C4 0.050(3) 0.043(3) 0.049(3) -0.015(2) 0.010(2) 0.003(2) C5 0.048(3) 0.039(3) 0.036(2) -0.0024(19) 0.006(2) 0.003(2) C11 0.040(2) 0.026(2) 0.0277(19) 0.0023(16) 0.0040(17) 0.0007(17) C12 0.031(2) 0.035(2) 0.074(4) 0.005(2) 0.003(2) 0.004(2) C13 0.048(3) 0.029(2) 0.070(3) -0.003(2) -0.006(3) -0.007(2) C14 0.052(3) 0.031(2) 0.070(3) -0.009(2) 0.013(3) 0.000(2) C15 0.037(3) 0.042(3) 0.129(6) -0.015(3) 0.015(3) 0.004(2) C16 0.039(3) 0.040(3) 0.087(4) -0.009(3) -0.007(3) -0.003(2) Cl3A 0.034(3) 0.051(3) 0.18(3) -0.003(8) 0.027(8) -0.003(2) Cl3B 0.059(15) 0.055(17) 0.11(4) -0.026(19) 0.06(2) -0.023(12) Cl3C 0.030(4) 0.033(4) 0.068(10) -0.002(2) 0.000(4) 0.003(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 N2 1.959(3) . y Pt1 N6 1.992(3) . y Pt1 Cl2 2.2796(11) . y Pt1 Cl1 2.2888(10) . y N1 N2 1.271(4) . ? N1 C1 1.394(5) . ? N2 C11 1.445(5) . ? N6 C5 1.343(5) . ? N6 C1 1.350(5) . ? C1 C2 1.395(6) . ? C2 C3 1.364(7) . ? C2 H2 0.9300 . ? C3 C4 1.396(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C11 C12 1.360(6) . ? C11 C16 1.379(7) . ? C12 C13 1.379(7) . ? C12 Cl3C 1.715(19) . ? C12 Cl3A 1.751(15) . ? C12 Cl3B 1.91(2) . ? C13 C14 1.369(7) . ? C13 H13 0.9300 . ? C14 C15 1.352(7) . ? C14 H14 0.9300 . ? C15 C16 1.389(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? Cl3A Cl3B 1.00(9) . ? Cl3B Cl3C 1.42(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 N2 Pt1 N6 78.11(14) . . y N2 Pt1 Cl2 95.34(10) . . y N6 Pt1 Cl2 173.41(10) . . y N2 Pt1 Cl1 173.92(10) . . y N6 Pt1 Cl1 95.81(11) . . y Cl2 Pt1 Cl1 90.74(4) . . y N2 N1 C1 111.9(3) . . ? N1 N2 C11 114.1(3) . . ? N1 N2 Pt1 120.0(3) . . ? C11 N2 Pt1 125.9(3) . . ? C5 N6 C1 119.0(4) . . ? C5 N6 Pt1 128.6(3) . . ? C1 N6 Pt1 112.4(3) . . ? N6 C1 N1 117.4(4) . . ? N6 C1 C2 122.8(4) . . ? N1 C1 C2 119.7(4) . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C2 C3 C4 118.9(4) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? N6 C5 C4 120.6(4) . . ? N6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C12 C11 C16 119.4(4) . . ? C12 C11 N2 120.8(4) . . ? C16 C11 N2 119.7(4) . . ? C11 C12 C13 121.1(4) . . ? C11 C12 Cl3C 122.7(7) . . ? C13 C12 Cl3C 115.5(7) . . ? C11 C12 Cl3A 118.5(11) . . ? C13 C12 Cl3A 120.1(9) . . ? Cl3C C12 Cl3A 14.6(17) . . ? C11 C12 Cl3B 105.4(16) . . ? C13 C12 Cl3B 121.5(13) . . ? Cl3C C12 Cl3B 46(3) . . ? Cl3A C12 Cl3B 31(3) . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.8(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 119.2(5) . . ? C11 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? Cl3B Cl3A C12 83(2) . . ? Cl3A Cl3B Cl3C 5.9(14) . . ? Cl3A Cl3B C12 65.7(13) . . ? Cl3C Cl3B C12 59.9(17) . . ? Cl3B Cl3C C12 74(2) . . ? 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 C1 N1 N2 C11 177.5(4) . . . . ? C1 N1 N2 Pt1 -4.0(5) . . . . ? N6 Pt1 N2 N1 4.6(3) . . . . ? Cl2 Pt1 N2 N1 -174.6(3) . . . . ? Cl1 Pt1 N2 N1 4.0(12) . . . . ? N6 Pt1 N2 C11 -177.1(4) . . . . ? Cl2 Pt1 N2 C11 3.6(3) . . . . ? Cl1 Pt1 N2 C11 -177.7(8) . . . . ? N2 Pt1 N6 C5 174.4(4) . . . . ? Cl2 Pt1 N6 C5 -179.1(7) . . . . ? Cl1 Pt1 N6 C5 -5.6(4) . . . . ? N2 Pt1 N6 C1 -4.0(3) . . . . ? Cl2 Pt1 N6 C1 2.5(11) . . . . ? Cl1 Pt1 N6 C1 175.9(3) . . . . ? C5 N6 C1 N1 -175.2(4) . . . . ? Pt1 N6 C1 N1 3.4(5) . . . . ? C5 N6 C1 C2 2.1(7) . . . . ? Pt1 N6 C1 C2 -179.3(4) . . . . ? N2 N1 C1 N6 0.2(6) . . . . ? N2 N1 C1 C2 -177.2(4) . . . . ? N6 C1 C2 C3 -1.8(8) . . . . ? N1 C1 C2 C3 175.4(5) . . . . ? C1 C2 C3 C4 -0.2(8) . . . . ? C2 C3 C4 C5 1.9(8) . . . . ? C1 N6 C5 C4 -0.3(7) . . . . ? Pt1 N6 C5 C4 -178.7(4) . . . . ? C3 C4 C5 N6 -1.6(8) . . . . ? N1 N2 C11 C12 -105.2(5) . . . . ? Pt1 N2 C11 C12 76.5(5) . . . . ? N1 N2 C11 C16 76.7(6) . . . . ? Pt1 N2 C11 C16 -101.7(5) . . . . ? C16 C11 C12 C13 0.0(8) . . . . ? N2 C11 C12 C13 -178.1(5) . . . . ? C16 C11 C12 Cl3C 169.9(12) . . . . ? N2 C11 C12 Cl3C -8.2(13) . . . . ? C16 C11 C12 Cl3A -174(2) . . . . ? N2 C11 C12 Cl3A 8(2) . . . . ? C16 C11 C12 Cl3B -143(4) . . . . ? N2 C11 C12 Cl3B 39(4) . . . . ? C11 C12 C13 C14 1.5(9) . . . . ? Cl3C C12 C13 C14 -169.1(12) . . . . ? Cl3A C12 C13 C14 175(2) . . . . ? Cl3B C12 C13 C14 139(4) . . . . ? C12 C13 C14 C15 -2.6(9) . . . . ? C13 C14 C15 C16 2.2(10) . . . . ? C12 C11 C16 C15 -0.4(8) . . . . ? N2 C11 C16 C15 177.7(5) . . . . ? C14 C15 C16 C11 -0.7(10) . . . . ? C11 C12 Cl3A Cl3B 72.0(16) . . . . ? C13 C12 Cl3A Cl3B -102(3) . . . . ? Cl3C C12 Cl3A Cl3B -177(5) . . . . ? C12 Cl3A Cl3B Cl3C 8(15) . . . . ? C11 C12 Cl3B Cl3A -119.9(13) . . . . ? C13 C12 Cl3B Cl3A 97(4) . . . . ? Cl3C C12 Cl3B Cl3A 1.0(18) . . . . ? C11 C12 Cl3B Cl3C -120.9(15) . . . . ? C13 C12 Cl3B Cl3C 96(3) . . . . ? Cl3A C12 Cl3B Cl3C -1.0(18) . . . . ? Cl3A Cl3B Cl3C C12 -171(15) . . . . ? C11 C12 Cl3C Cl3B 79.5(15) . . . . ? C13 C12 Cl3C Cl3B -110.1(18) . . . . ? Cl3A C12 Cl3C Cl3B 2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.969 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.134 #END data_compound_2b _database_code_depnum_ccdc_archive 'CCDC 258039' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PtCl(L2b)]' _chemical_formula_sum 'C18 H15 Cl N4 Pt' _chemical_formula_weight 517.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _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 6.7696(3) _cell_length_b 16.4559(8) _cell_length_c 14.7526(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.1020(10) _cell_angle_gamma 90.00 _cell_volume 1643.13(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description brown _exptl_crystal_colour prism _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 8.708 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.1323 _exptl_absorpt_correction_T_max 0.5426 _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 'Bruker, SMART CCD-1000' _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_% 0 _diffrn_reflns_number 10140 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3858 _reflns_number_gt 3008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Software (Bruker, 1997)' _computing_cell_refinement 'SMART Software (Bruker, 1997)' _computing_data_reduction 'SAINT Software (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0068P)^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 3858 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0376 _refine_ls_wR_factor_gt 0.0355 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.68328(2) 0.380436(8) 0.451581(11) 0.02135(5) Uani 1 1 d . . . Cl1 Cl 0.63414(16) 0.26284(6) 0.36879(8) 0.0386(3) Uani 1 1 d . . . N11 N 0.6575(4) 0.33175(18) 0.5763(2) 0.0219(7) Uani 1 1 d . . . N12 N 0.7361(4) 0.46835(18) 0.6147(2) 0.0247(8) Uani 1 1 d . . . N13 N 0.7348(4) 0.47429(18) 0.5266(2) 0.0213(7) Uani 1 1 d . . . N14 N 0.7261(4) 0.46228(17) 0.3508(2) 0.0229(7) Uani 1 1 d . . . C11 C 0.6125(5) 0.2556(2) 0.6021(3) 0.0287(10) Uani 1 1 d . . . H11 H 0.5866 0.2156 0.5569 0.034 Uiso 1 1 d R . . C12 C 0.6030(6) 0.2341(2) 0.6925(3) 0.0348(11) Uani 1 1 d . . . H12 H 0.5722 0.1798 0.7091 0.042 Uiso 1 1 d R . . C13 C 0.6382(6) 0.2914(2) 0.7578(3) 0.0347(11) Uani 1 1 d . . . H13 H 0.6324 0.2773 0.8202 0.042 Uiso 1 1 d R . . C14 C 0.6827(5) 0.3707(2) 0.7321(3) 0.0283(9) Uani 1 1 d . . . H14 H 0.7069 0.4114 0.7767 0.034 Uiso 1 1 d R . . C15 C 0.6910(5) 0.3893(2) 0.6420(3) 0.0245(9) Uani 1 1 d . . . C16 C 0.7758(5) 0.5447(2) 0.4819(3) 0.0212(9) Uani 1 1 d . . . C17 C 0.8198(5) 0.6192(2) 0.5253(3) 0.0263(9) Uani 1 1 d . . . H17 H 0.8255 0.6228 0.5896 0.032 Uiso 1 1 d R . . C18 C 0.8539(5) 0.6860(2) 0.4731(3) 0.0291(10) Uani 1 1 d . . . H18 H 0.8853 0.7365 0.5010 0.035 Uiso 1 1 d R . . C19 C 0.8425(5) 0.6801(2) 0.3774(3) 0.0296(10) Uani 1 1 d . . . H19 H 0.8645 0.7275 0.3421 0.036 Uiso 1 1 d R . . C20 C 0.8009(5) 0.6086(2) 0.3343(3) 0.0268(9) Uani 1 1 d . . . H20 H 0.7937 0.6070 0.2699 0.032 Uiso 1 1 d R . . C21 C 0.7683(5) 0.5362(2) 0.3850(3) 0.0217(9) Uani 1 1 d . . . C22 C 0.7175(6) 0.4483(2) 0.2571(3) 0.0266(10) Uani 1 1 d . . . C23 C 0.8790(6) 0.4643(2) 0.2025(3) 0.0318(10) Uani 1 1 d . . . H23 H 0.9980 0.4848 0.2289 0.038 Uiso 1 1 d R . . C24 C 0.8666(7) 0.4506(2) 0.1097(3) 0.0392(12) Uani 1 1 d . . . H24 H 0.9774 0.4629 0.0736 0.047 Uiso 1 1 d R . . C25 C 0.6997(7) 0.4199(2) 0.0687(3) 0.0377(11) Uani 1 1 d . . . C26 C 0.5411(7) 0.4018(2) 0.1240(3) 0.0387(11) Uani 1 1 d . . . H26 H 0.4241 0.3798 0.0972 0.046 Uiso 1 1 d R . . C27 C 0.5486(6) 0.4149(2) 0.2168(3) 0.0316(10) Uani 1 1 d . . . H27 H 0.4388 0.4010 0.2529 0.038 Uiso 1 1 d R . . C28 C 0.6848(8) 0.4064(3) -0.0334(3) 0.0560(14) Uani 1 1 d . . . H28A H 0.6940 0.4588 -0.0647 0.084 Uiso 1 1 d R . . H28B H 0.5580 0.3807 -0.0488 0.084 Uiso 1 1 d R . . H28C H 0.7929 0.3710 -0.0523 0.084 Uiso 1 1 d 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 0.02355(7) 0.02101(8) 0.01949(8) -0.00210(8) 0.00085(6) 0.00053(7) Cl1 0.0608(7) 0.0259(6) 0.0292(6) -0.0072(5) 0.0022(6) -0.0040(5) N11 0.0220(16) 0.0218(18) 0.0218(19) 0.0004(15) -0.0009(15) 0.0013(13) N12 0.0219(17) 0.0301(19) 0.022(2) -0.0019(16) -0.0010(16) -0.0009(14) N13 0.0168(16) 0.0249(18) 0.0220(19) -0.0026(15) -0.0006(15) -0.0001(13) N14 0.0293(18) 0.0209(18) 0.0184(19) -0.0023(15) 0.0003(16) -0.0009(14) C11 0.031(2) 0.022(2) 0.033(3) -0.0003(19) -0.001(2) 0.0025(17) C12 0.044(3) 0.025(2) 0.035(3) 0.007(2) -0.005(2) -0.0004(19) C13 0.044(3) 0.038(3) 0.023(3) 0.006(2) 0.001(2) -0.002(2) C14 0.032(2) 0.032(2) 0.021(2) -0.003(2) -0.0020(19) -0.0043(19) C15 0.0189(18) 0.026(2) 0.028(2) -0.003(2) 0.0008(18) 0.0002(17) C16 0.0157(18) 0.019(2) 0.029(2) 0.0015(18) -0.0003(18) 0.0028(15) C17 0.0212(18) 0.028(2) 0.029(2) -0.008(2) -0.0001(18) 0.0023(19) C18 0.024(2) 0.025(2) 0.039(3) -0.006(2) -0.002(2) -0.0008(17) C19 0.026(2) 0.022(2) 0.042(3) 0.000(2) 0.007(2) 0.0018(17) C20 0.024(2) 0.031(2) 0.026(2) -0.0020(19) 0.0012(18) 0.0014(17) C21 0.0143(19) 0.024(2) 0.027(2) 0.0005(18) 0.0005(18) 0.0046(15) C22 0.033(2) 0.021(2) 0.026(3) 0.0021(18) -0.001(2) 0.0066(17) C23 0.039(2) 0.027(2) 0.030(3) 0.002(2) 0.007(2) -0.0013(19) C24 0.059(3) 0.028(2) 0.031(3) 0.006(2) 0.018(3) 0.006(2) C25 0.076(3) 0.014(2) 0.023(3) 0.0018(18) -0.003(3) 0.006(2) C26 0.057(3) 0.024(2) 0.035(3) -0.002(2) -0.015(3) 0.000(2) C27 0.042(3) 0.028(2) 0.025(3) -0.0034(19) -0.002(2) -0.0031(19) C28 0.109(4) 0.039(3) 0.021(3) 0.006(2) 0.002(3) 0.001(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 N13 1.928(3) . y Pt1 N11 2.018(3) . y Pt1 N14 2.031(3) . y Pt1 Cl1 2.3090(10) . y N11 C11 1.346(4) . ? N11 C15 1.370(4) . ? N12 N13 1.303(4) . ? N12 C15 1.398(4) . ? N13 C16 1.363(4) . ? N14 C21 1.345(4) . ? N14 C22 1.402(5) . ? C11 C12 1.383(6) . ? C11 H11 0.9500 . ? C12 C13 1.366(5) . ? C12 H12 0.9500 . ? C13 C14 1.394(5) . ? C13 H13 0.9500 . ? C14 C15 1.366(5) . ? C14 H14 0.9500 . ? C16 C17 1.413(5) . ? C16 C21 1.438(5) . ? C17 C18 1.364(5) . ? C17 H17 0.9500 . ? C18 C19 1.415(6) . ? C18 H18 0.9500 . ? C19 C20 1.365(5) . ? C19 H19 0.9500 . ? C20 C21 1.426(5) . ? C20 H20 0.9500 . ? C22 C27 1.391(5) . ? C22 C23 1.396(5) . ? C23 C24 1.388(6) . ? C23 H23 0.9500 . ? C24 C25 1.368(6) . ? C24 H24 0.9500 . ? C25 C26 1.394(6) . ? C25 C28 1.523(6) . ? C26 C27 1.387(6) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 N13 Pt1 N11 79.19(13) . . y N13 Pt1 N14 82.06(13) . . y N11 Pt1 N14 161.25(12) . . y N13 Pt1 Cl1 176.08(9) . . y N11 Pt1 Cl1 97.79(9) . . y N14 Pt1 Cl1 100.95(9) . . y C11 N11 C15 118.6(3) . . ? C11 N11 Pt1 130.6(3) . . ? C15 N11 Pt1 110.8(2) . . ? N13 N12 C15 111.1(3) . . ? N12 N13 C16 123.2(3) . . ? N12 N13 Pt1 120.7(2) . . ? C16 N13 Pt1 116.1(3) . . ? C21 N14 C22 121.5(3) . . ? C21 N14 Pt1 111.0(3) . . ? C22 N14 Pt1 127.5(2) . . ? N11 C11 C12 121.7(4) . . ? N11 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 119.5(4) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 119.4(4) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.1(4) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 N11 121.6(4) . . ? C14 C15 N12 120.1(4) . . ? N11 C15 N12 118.2(3) . . ? N13 C16 C17 124.2(4) . . ? N13 C16 C21 113.2(3) . . ? C17 C16 C21 122.6(3) . . ? C18 C17 C16 118.7(4) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 122.0(4) . . ? C20 C19 H19 119.0 . . ? C18 C19 H19 119.0 . . ? C19 C20 C21 120.6(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? N14 C21 C20 126.4(4) . . ? N14 C21 C16 117.6(3) . . ? C20 C21 C16 115.9(3) . . ? C27 C22 C23 118.4(4) . . ? C27 C22 N14 120.3(4) . . ? C23 C22 N14 121.3(4) . . ? C24 C23 C22 120.3(4) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 122.0(4) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 117.3(4) . . ? C24 C25 C28 122.0(5) . . ? C26 C25 C28 120.7(4) . . ? C27 C26 C25 122.1(4) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C22 119.8(4) . . ? C26 C27 H27 120.1 . . ? C22 C27 H27 120.1 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 N13 Pt1 N11 C11 178.6(3) . . . . ? N14 Pt1 N11 C11 178.0(3) . . . . ? Cl1 Pt1 N11 C11 -3.9(3) . . . . ? N13 Pt1 N11 C15 -0.6(2) . . . . ? N14 Pt1 N11 C15 -1.2(5) . . . . ? Cl1 Pt1 N11 C15 176.9(2) . . . . ? C15 N12 N13 C16 -179.3(3) . . . . ? C15 N12 N13 Pt1 -1.8(4) . . . . ? N11 Pt1 N13 N12 1.4(3) . . . . ? N14 Pt1 N13 N12 -178.8(3) . . . . ? Cl1 Pt1 N13 N12 -38.5(15) . . . . ? N11 Pt1 N13 C16 179.1(3) . . . . ? N14 Pt1 N13 C16 -1.1(2) . . . . ? Cl1 Pt1 N13 C16 139.2(13) . . . . ? N13 Pt1 N14 C21 0.6(2) . . . . ? N11 Pt1 N14 C21 1.2(5) . . . . ? Cl1 Pt1 N14 C21 -176.9(2) . . . . ? N13 Pt1 N14 C22 180.0(3) . . . . ? N11 Pt1 N14 C22 -179.4(3) . . . . ? Cl1 Pt1 N14 C22 2.5(3) . . . . ? C15 N11 C11 C12 -1.2(5) . . . . ? Pt1 N11 C11 C12 179.7(3) . . . . ? N11 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C14 0.1(6) . . . . ? C12 C13 C14 C15 -0.3(6) . . . . ? C13 C14 C15 N11 -0.2(6) . . . . ? C13 C14 C15 N12 -179.8(3) . . . . ? C11 N11 C15 C14 1.0(5) . . . . ? Pt1 N11 C15 C14 -179.7(3) . . . . ? C11 N11 C15 N12 -179.5(3) . . . . ? Pt1 N11 C15 N12 -0.2(4) . . . . ? N13 N12 C15 C14 -179.3(3) . . . . ? N13 N12 C15 N11 1.2(4) . . . . ? N12 N13 C16 C17 -1.5(5) . . . . ? Pt1 N13 C16 C17 -179.1(3) . . . . ? N12 N13 C16 C21 179.1(3) . . . . ? Pt1 N13 C16 C21 1.4(4) . . . . ? N13 C16 C17 C18 -178.5(3) . . . . ? C21 C16 C17 C18 0.9(5) . . . . ? C16 C17 C18 C19 0.8(5) . . . . ? C17 C18 C19 C20 -1.1(6) . . . . ? C18 C19 C20 C21 -0.4(6) . . . . ? C22 N14 C21 C20 2.7(6) . . . . ? Pt1 N14 C21 C20 -177.9(3) . . . . ? C22 N14 C21 C16 -179.4(3) . . . . ? Pt1 N14 C21 C16 0.0(4) . . . . ? C19 C20 C21 N14 179.9(3) . . . . ? C19 C20 C21 C16 2.0(5) . . . . ? N13 C16 C21 N14 -0.9(5) . . . . ? C17 C16 C21 N14 179.6(3) . . . . ? N13 C16 C21 C20 177.2(3) . . . . ? C17 C16 C21 C20 -2.2(5) . . . . ? C21 N14 C22 C27 -124.8(4) . . . . ? Pt1 N14 C22 C27 55.9(5) . . . . ? C21 N14 C22 C23 57.6(5) . . . . ? Pt1 N14 C22 C23 -121.7(3) . . . . ? C27 C22 C23 C24 2.9(6) . . . . ? N14 C22 C23 C24 -179.5(4) . . . . ? C22 C23 C24 C25 -1.2(6) . . . . ? C23 C24 C25 C26 -0.7(6) . . . . ? C23 C24 C25 C28 178.8(4) . . . . ? C24 C25 C26 C27 0.7(6) . . . . ? C28 C25 C26 C27 -178.8(4) . . . . ? C25 C26 C27 C22 1.1(6) . . . . ? C23 C22 C27 C26 -2.8(6) . . . . ? N14 C22 C27 C26 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.006 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.122 #END data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 258040' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PtBr3(L2a)]' _chemical_formula_sum 'C17 H13 Br3 N4 Pt' _chemical_formula_weight 708.13 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' Br Br -0.2901 2.4595 '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_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 12.1865(9) _cell_length_b 8.5286(6) _cell_length_c 18.5423(13) _cell_angle_alpha 90.00 _cell_angle_beta 105.1650(10) _cell_angle_gamma 90.00 _cell_volume 1860.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4737 _cell_measurement_theta_min 2.473 _cell_measurement_theta_max 28.254 _exptl_crystal_description Parallelopiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 13.996 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1202 _exptl_absorpt_correction_T_max 0.1705 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% 0 _diffrn_reflns_number 12039 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4579 _reflns_number_gt 4038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.0472P)^2^+3.4995P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4579 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.786854(18) 0.36152(2) 0.127239(11) 0.00860(8) Uani 1 1 d . . . Br1 Br 0.96941(5) 0.22218(7) 0.16792(3) 0.01422(13) Uani 1 1 d . . . Br2 Br 0.80269(6) 0.45307(7) 0.25514(3) 0.02075(15) Uani 1 1 d . . . Br3 Br 0.60291(5) 0.49301(7) 0.08194(3) 0.01453(13) Uani 1 1 d . . . N1 N 0.8635(4) 0.5482(6) 0.0904(3) 0.0118(9) Uani 1 1 d . . . N2 N 0.8096(5) 0.3939(6) -0.0204(3) 0.0141(10) Uani 1 1 d . . . N3 N 0.7743(4) 0.2982(5) 0.0231(2) 0.0093(9) Uani 1 1 d . . . N4 N 0.7072(4) 0.1523(5) 0.1286(3) 0.0117(10) Uani 1 1 d . . . C1 C 0.9106(5) 0.6759(7) 0.1267(3) 0.0151(12) Uani 1 1 d . . . H1 H 0.9155 0.6862 0.1774 0.018 Uiso 1 1 calc R . . C2 C 0.9529(5) 0.7944(7) 0.0899(3) 0.0171(12) Uani 1 1 d . . . H2 H 0.9861 0.8834 0.1156 0.021 Uiso 1 1 calc R . . C3 C 0.9446(6) 0.7773(7) 0.0137(3) 0.0174(12) Uani 1 1 d . . . H3 H 0.9717 0.8559 -0.0118 0.021 Uiso 1 1 calc R . . C4 C 0.8967(6) 0.6454(7) -0.0235(4) 0.0167(13) Uani 1 1 d . . . H4 H 0.8916 0.6335 -0.0741 0.020 Uiso 1 1 calc R . . C5 C 0.8560(5) 0.5297(7) 0.0153(3) 0.0138(11) Uani 1 1 d . . . C6 C 0.7251(5) 0.1572(7) 0.0041(3) 0.0132(12) Uani 1 1 d . . . C7 C 0.7056(6) 0.0920(7) -0.0690(3) 0.0163(12) Uani 1 1 d . . . H7 H 0.7275 0.1462 -0.1064 0.020 Uiso 1 1 calc R . . C8 C 0.6548(6) -0.0496(7) -0.0830(3) 0.0191(13) Uani 1 1 d . . . H8 H 0.6411 -0.0939 -0.1304 0.023 Uiso 1 1 calc R . . C9 C 0.6219(6) -0.1315(6) -0.0237(4) 0.0182(13) Uani 1 1 d . . . H9 H 0.5875 -0.2293 -0.0339 0.022 Uiso 1 1 calc R . . C10 C 0.6391(5) -0.0719(7) 0.0459(3) 0.0152(12) Uani 1 1 d . . . H10 H 0.6173 -0.1288 0.0827 0.018 Uiso 1 1 calc R . . C11 C 0.6911(5) 0.0793(6) 0.0631(3) 0.0116(11) Uani 1 1 d . . . C12 C 0.6821(5) 0.0839(7) 0.1927(3) 0.0125(11) Uani 1 1 d . . . C13 C 0.7346(5) -0.0533(7) 0.2236(3) 0.0148(12) Uani 1 1 d . . . H13 H 0.7869 -0.1022 0.2025 0.018 Uiso 1 1 calc R . . C14 C 0.7093(6) -0.1181(7) 0.2859(3) 0.0190(13) Uani 1 1 d . . . H14 H 0.7444 -0.2105 0.3065 0.023 Uiso 1 1 calc R . . C15 C 0.6323(5) -0.0452(7) 0.3172(3) 0.0182(13) Uani 1 1 d . . . H15 H 0.6157 -0.0886 0.3591 0.022 Uiso 1 1 calc R . . C16 C 0.5791(6) 0.0921(8) 0.2870(4) 0.0211(13) Uani 1 1 d . . . H16 H 0.5272 0.1403 0.3087 0.025 Uiso 1 1 calc R . . C17 C 0.6032(5) 0.1584(7) 0.2240(3) 0.0142(12) Uani 1 1 d . . . H17 H 0.5675 0.2504 0.2033 0.017 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 0.00815(12) 0.00909(12) 0.00770(12) 0.00011(7) 0.00053(8) -0.00063(8) Br1 0.0107(3) 0.0177(3) 0.0129(3) 0.0020(2) 0.0008(2) 0.0027(2) Br2 0.0228(3) 0.0231(3) 0.0164(3) -0.0029(2) 0.0051(3) -0.0044(3) Br3 0.0103(3) 0.0144(3) 0.0178(3) 0.0025(2) 0.0017(2) 0.0019(2) N1 0.008(2) 0.017(2) 0.010(2) 0.0015(18) 0.0024(19) -0.003(2) N2 0.017(3) 0.017(2) 0.007(2) 0.0011(18) 0.000(2) -0.004(2) N3 0.010(2) 0.010(2) 0.009(2) 0.0008(17) 0.0043(19) 0.0023(19) N4 0.013(3) 0.011(2) 0.011(2) 0.0029(17) 0.003(2) -0.0010(19) C1 0.015(3) 0.015(3) 0.014(3) -0.001(2) 0.001(2) 0.000(2) C2 0.015(3) 0.016(3) 0.021(3) -0.004(2) 0.006(3) -0.004(2) C3 0.020(3) 0.012(3) 0.021(3) 0.002(2) 0.007(3) -0.003(2) C4 0.017(3) 0.016(3) 0.020(3) 0.004(2) 0.009(3) -0.001(2) C5 0.014(3) 0.018(3) 0.007(3) 0.000(2) -0.001(2) 0.005(2) C6 0.012(3) 0.018(3) 0.009(3) -0.002(2) 0.000(2) -0.003(2) C7 0.022(3) 0.017(3) 0.012(3) 0.000(2) 0.006(2) 0.003(3) C8 0.028(4) 0.014(3) 0.016(3) -0.005(2) 0.005(3) 0.000(3) C9 0.017(3) 0.009(3) 0.030(4) -0.005(2) 0.009(3) -0.003(2) C10 0.014(3) 0.010(3) 0.021(3) 0.001(2) 0.003(2) -0.003(2) C11 0.011(3) 0.010(3) 0.014(3) 0.003(2) 0.004(2) 0.000(2) C12 0.012(3) 0.015(3) 0.010(3) 0.002(2) 0.000(2) -0.001(2) C13 0.012(3) 0.014(3) 0.019(3) 0.000(2) 0.007(2) 0.000(2) C14 0.024(4) 0.017(3) 0.014(3) 0.007(2) 0.002(3) 0.003(3) C15 0.020(3) 0.021(3) 0.013(3) 0.003(2) 0.005(3) -0.007(3) C16 0.020(3) 0.025(3) 0.022(3) -0.005(3) 0.013(3) -0.004(3) C17 0.012(3) 0.015(3) 0.015(3) 0.001(2) 0.003(2) -0.002(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 N3 1.971(4) . ? Pt1 N4 2.035(5) . ? Pt1 N1 2.050(5) . ? Pt1 Br3 2.4501(6) . ? Pt1 Br2 2.4560(6) . ? Pt1 Br1 2.4602(6) . ? N1 C1 1.329(8) . ? N1 C5 1.381(7) . ? N2 N3 1.298(6) . ? N2 C5 1.380(8) . ? N3 C6 1.349(7) . ? N4 C11 1.333(7) . ? N4 C12 1.428(7) . ? C1 C2 1.391(8) . ? C1 H1 0.9300 . ? C2 C3 1.398(8) . ? C2 H2 0.9300 . ? C3 C4 1.367(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(8) . ? C4 H4 0.9300 . ? C6 C7 1.425(8) . ? C6 C11 1.431(7) . ? C7 C8 1.351(9) . ? C7 H7 0.9300 . ? C8 C9 1.445(8) . ? C8 H8 0.9300 . ? C9 C10 1.352(8) . ? C9 H9 0.9300 . ? C10 C11 1.435(8) . ? C10 H10 0.9300 . ? C12 C13 1.384(8) . ? C12 C17 1.399(8) . ? C13 C14 1.386(8) . ? C13 H13 0.9300 . ? C14 C15 1.375(9) . ? C14 H14 0.9300 . ? C15 C16 1.383(9) . ? C15 H15 0.9300 . ? C16 C17 1.396(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? 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 N3 Pt1 N4 81.77(19) . . ? N3 Pt1 N1 79.17(18) . . ? N4 Pt1 N1 160.93(19) . . ? N3 Pt1 Br3 87.72(14) . . ? N4 Pt1 Br3 90.53(14) . . ? N1 Pt1 Br3 89.20(14) . . ? N3 Pt1 Br2 177.35(13) . . ? N4 Pt1 Br2 100.62(13) . . ? N1 Pt1 Br2 98.45(13) . . ? Br3 Pt1 Br2 91.10(2) . . ? N3 Pt1 Br1 90.00(14) . . ? N4 Pt1 Br1 88.19(14) . . ? N1 Pt1 Br1 91.32(14) . . ? Br3 Pt1 Br1 177.52(2) . . ? Br2 Pt1 Br1 91.22(2) . . ? C1 N1 C5 120.6(5) . . ? C1 N1 Pt1 130.0(4) . . ? C5 N1 Pt1 109.4(4) . . ? N3 N2 C5 112.9(4) . . ? N2 N3 C6 126.4(5) . . ? N2 N3 Pt1 118.9(4) . . ? C6 N3 Pt1 114.6(3) . . ? C11 N4 C12 123.8(5) . . ? C11 N4 Pt1 110.8(4) . . ? C12 N4 Pt1 125.1(4) . . ? N1 C1 C2 120.9(5) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 118.8(5) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 120.3(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.2(6) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N2 C5 N1 119.4(5) . . ? N2 C5 C4 120.4(5) . . ? N1 C5 C4 120.2(5) . . ? N3 C6 C7 123.3(5) . . ? N3 C6 C11 114.3(5) . . ? C7 C6 C11 122.4(5) . . ? C8 C7 C6 119.1(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.3(5) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 122.7(5) . . ? C10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C9 C10 C11 119.9(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N4 C11 C6 118.5(5) . . ? N4 C11 C10 124.9(5) . . ? C6 C11 C10 116.6(5) . . ? C13 C12 C17 120.4(5) . . ? C13 C12 N4 120.9(5) . . ? C17 C12 N4 118.7(5) . . ? C12 C13 C14 120.1(5) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 119.8(6) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(5) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C17 120.2(6) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 118.7(6) . . ? C16 C17 H17 120.6 . . ? C12 C17 H17 120.6 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.222 _refine_diff_density_min -2.135 _refine_diff_density_rms 0.265 #END data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 258041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PtClI2(L2a)]' _chemical_formula_sum 'C17 H13 Cl I2 N4 Pt' _chemical_formula_weight 757.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' I I -0.4742 1.8119 '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_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _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 9.6500(7) _cell_length_b 14.2218(10) _cell_length_c 14.8154(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.4540(10) _cell_angle_gamma 90.00 _cell_volume 1928.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8079 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.29 _exptl_crystal_description Parallelopiped _exptl_crystal_colour Green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 10.623 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1751 _exptl_absorpt_correction_T_max 0.3783 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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_% 0 _diffrn_reflns_number 12549 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 28.29 _reflns_number_total 4729 _reflns_number_gt 4517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.0359P)^2^+7.8912P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4729 _refine_ls_number_parameters 226 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.01347(2) 0.114355(13) 0.223164(13) 0.00640(7) Uani 1 1 d . . . I1 I -0.23086(4) 0.14047(3) 0.07931(2) 0.01227(9) Uani 1 1 d . . . I2 I 0.26021(4) 0.09373(3) 0.36615(3) 0.01482(9) Uani 1 1 d . . . Cl1 Cl -0.10838(14) 0.15409(9) 0.33246(9) 0.0108(2) Uani 1 1 d . . . N1 N -0.0184(5) -0.0281(3) 0.2218(3) 0.0098(9) Uani 1 1 d . . . N2 N 0.1190(5) -0.0143(3) 0.1142(3) 0.0123(9) Uani 1 1 d . . . N3 N 0.1150(5) 0.0741(3) 0.1349(3) 0.0096(9) Uani 1 1 d . . . N4 N 0.0785(5) 0.2437(3) 0.1932(3) 0.0095(9) Uani 1 1 d U . . C1 C -0.0881(6) -0.0805(4) 0.2692(4) 0.0134(11) Uani 1 1 d . . . H1 H -0.1311 -0.0513 0.3099 0.016 Uiso 1 1 calc R . . C2 C -0.0972(6) -0.1779(4) 0.2585(4) 0.0159(11) Uani 1 1 d . . . H2 H -0.1473 -0.2137 0.2906 0.019 Uiso 1 1 calc R . . C3 C -0.0305(6) -0.2203(4) 0.1993(4) 0.0154(11) Uani 1 1 d . . . H3 H -0.0352 -0.2853 0.1918 0.018 Uiso 1 1 calc R . . C4 C 0.0435(6) -0.1670(4) 0.1508(4) 0.0131(11) Uani 1 1 d . . . H4 H 0.0893 -0.1956 0.1115 0.016 Uiso 1 1 calc R . . C5 C 0.0478(6) -0.0696(4) 0.1625(4) 0.0102(10) Uani 1 1 d . . . C6 C 0.1804(6) 0.1441(4) 0.0997(4) 0.0083(10) Uani 1 1 d . . . C7 C 0.2625(6) 0.1296(4) 0.0381(4) 0.0117(10) Uani 1 1 d . . . H7 H 0.2754 0.0691 0.0183 0.014 Uiso 1 1 calc R . . C8 C 0.3228(6) 0.2038(4) 0.0075(4) 0.0148(11) Uani 1 1 d . . . H8 H 0.3792 0.1949 -0.0323 0.018 Uiso 1 1 calc R . . C9 C 0.2987(6) 0.2966(4) 0.0373(4) 0.0134(11) Uani 1 1 d . . . H9 H 0.3398 0.3475 0.0156 0.016 Uiso 1 1 calc R . . C10 C 0.2177(6) 0.3133(4) 0.0964(4) 0.0118(10) Uani 1 1 d . . . H10 H 0.2034 0.3746 0.1136 0.014 Uiso 1 1 calc R . . C11 C 0.1549(6) 0.2361(4) 0.1317(4) 0.0093(10) Uani 1 1 d . . . C12 C 0.0282(6) 0.3314(4) 0.2163(4) 0.0102(10) Uani 1 1 d . . . C13 C -0.0537(6) 0.3904(4) 0.1432(4) 0.0117(11) Uani 1 1 d . . . H13 H -0.0762 0.3720 0.0800 0.014 Uiso 1 1 calc R . . C14 C -0.1007(6) 0.4761(4) 0.1660(4) 0.0160(11) Uani 1 1 d . . . H14 H -0.1531 0.5163 0.1177 0.019 Uiso 1 1 calc R . . C15 C -0.0702(6) 0.5027(4) 0.2602(5) 0.0162(12) Uani 1 1 d . . . H15 H -0.1020 0.5608 0.2750 0.019 Uiso 1 1 calc R . . C16 C 0.0072(6) 0.4432(4) 0.3324(4) 0.0153(11) Uani 1 1 d . . . H16 H 0.0264 0.4607 0.3957 0.018 Uiso 1 1 calc R . . C17 C 0.0564(6) 0.3568(4) 0.3100(4) 0.0130(11) Uani 1 1 d . . . H17 H 0.1083 0.3165 0.3583 0.016 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 0.01280(11) 0.00206(11) 0.00301(11) -0.00057(6) 0.00059(8) 0.00025(7) I1 0.01643(18) 0.01028(18) 0.00686(17) -0.00159(12) -0.00090(13) 0.00087(13) I2 0.01863(19) 0.00835(17) 0.01121(18) 0.00181(13) -0.00421(14) -0.00111(13) Cl1 0.0183(6) 0.0056(6) 0.0115(6) -0.0027(4) 0.0089(5) -0.0001(5) N1 0.015(2) 0.004(2) 0.008(2) -0.0029(16) 0.0000(17) -0.0005(17) N2 0.019(2) 0.007(2) 0.010(2) -0.0013(17) 0.0035(18) 0.0001(18) N3 0.018(2) 0.007(2) 0.002(2) -0.0001(16) 0.0002(17) 0.0014(18) N4 0.0111(11) 0.0078(12) 0.0089(12) -0.0006(9) 0.0021(9) -0.0003(9) C1 0.015(3) 0.011(3) 0.014(3) 0.000(2) 0.004(2) -0.002(2) C2 0.018(3) 0.009(3) 0.018(3) 0.004(2) 0.002(2) -0.006(2) C3 0.019(3) 0.006(2) 0.018(3) 0.000(2) 0.000(2) -0.003(2) C4 0.020(3) 0.004(2) 0.014(3) 0.000(2) 0.004(2) 0.002(2) C5 0.012(2) 0.011(3) 0.005(2) -0.0010(19) -0.0004(19) 0.000(2) C6 0.012(2) 0.006(2) 0.005(2) 0.0017(18) -0.0001(19) 0.0015(19) C7 0.014(3) 0.012(3) 0.010(3) 0.000(2) 0.004(2) 0.007(2) C8 0.015(3) 0.017(3) 0.011(3) 0.001(2) 0.002(2) 0.003(2) C9 0.014(3) 0.010(3) 0.014(3) 0.004(2) 0.003(2) -0.001(2) C10 0.016(3) 0.006(2) 0.012(3) 0.0028(19) 0.004(2) -0.002(2) C11 0.013(2) 0.007(2) 0.005(2) 0.0027(18) -0.0018(19) 0.0004(19) C12 0.015(3) 0.004(2) 0.009(3) 0.0010(19) 0.000(2) 0.0019(19) C13 0.019(3) 0.010(3) 0.005(3) 0.0015(19) 0.003(2) 0.001(2) C14 0.016(3) 0.012(3) 0.020(3) 0.008(2) 0.006(2) 0.005(2) C15 0.017(3) 0.004(2) 0.028(3) -0.001(2) 0.008(2) 0.000(2) C16 0.023(3) 0.010(3) 0.012(3) -0.005(2) 0.003(2) 0.000(2) C17 0.017(3) 0.006(2) 0.011(3) -0.002(2) -0.002(2) 0.002(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 N3 1.952(4) . ? Pt1 N4 2.037(5) . ? Pt1 N1 2.048(4) . ? Pt1 Cl1 2.3515(12) . ? Pt1 I2 2.6552(4) . ? Pt1 I1 2.6567(4) . ? N1 C1 1.343(7) . ? N1 C5 1.373(7) . ? N2 N3 1.297(6) . ? N2 C5 1.384(7) . ? N3 C6 1.368(7) . ? N4 C11 1.345(7) . ? N4 C12 1.420(7) . ? C1 C2 1.395(8) . ? C1 H1 0.9300 . ? C2 C3 1.380(8) . ? C2 H2 0.9300 . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.394(8) . ? C4 H4 0.9300 . ? C6 C7 1.400(7) . ? C6 C11 1.440(7) . ? C7 C8 1.351(8) . ? C7 H7 0.9300 . ? C8 C9 1.434(8) . ? C8 H8 0.9300 . ? C9 C10 1.366(8) . ? C9 H9 0.9300 . ? C10 C11 1.430(7) . ? C10 H10 0.9300 . ? C12 C17 1.375(8) . ? C12 C13 1.400(7) . ? C13 C14 1.379(8) . ? C13 H13 0.9300 . ? C14 C15 1.386(9) . ? C14 H14 0.9300 . ? C15 C16 1.383(8) . ? C15 H15 0.9300 . ? C16 C17 1.394(7) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? 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 N3 Pt1 N4 82.21(18) . . ? N3 Pt1 N1 78.95(19) . . ? N4 Pt1 N1 161.16(18) . . ? N3 Pt1 Cl1 176.78(14) . . ? N4 Pt1 Cl1 100.88(13) . . ? N1 Pt1 Cl1 97.96(13) . . ? N3 Pt1 I2 89.35(13) . . ? N4 Pt1 I2 90.76(13) . . ? N1 Pt1 I2 89.58(13) . . ? Cl1 Pt1 I2 89.70(4) . . ? N3 Pt1 I1 90.55(13) . . ? N4 Pt1 I1 87.44(13) . . ? N1 Pt1 I1 92.17(13) . . ? Cl1 Pt1 I1 90.49(3) . . ? I2 Pt1 I1 178.198(13) . . ? C1 N1 C5 120.5(5) . . ? C1 N1 Pt1 130.0(4) . . ? C5 N1 Pt1 109.5(4) . . ? N3 N2 C5 111.8(4) . . ? N2 N3 C6 124.3(5) . . ? N2 N3 Pt1 120.1(4) . . ? C6 N3 Pt1 115.6(3) . . ? C11 N4 C12 122.4(5) . . ? C11 N4 Pt1 110.4(4) . . ? C12 N4 Pt1 126.0(3) . . ? N1 C1 C2 121.0(5) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 118.8(5) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.7(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 118.6(5) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 N2 119.6(5) . . ? N1 C5 C4 120.3(5) . . ? N2 C5 C4 120.1(5) . . ? N3 C6 C7 124.5(5) . . ? N3 C6 C11 112.9(5) . . ? C7 C6 C11 122.7(5) . . ? C8 C7 C6 119.7(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.1(5) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C10 C9 C8 122.6(5) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C11 119.7(5) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N4 C11 C10 124.9(5) . . ? N4 C11 C6 118.9(5) . . ? C10 C11 C6 116.2(5) . . ? C17 C12 C13 120.4(5) . . ? C17 C12 N4 120.1(5) . . ? C13 C12 N4 119.5(5) . . ? C14 C13 C12 119.3(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.4(5) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.1(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.8(5) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C12 C17 C16 119.9(5) . . ? C12 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.448 _refine_diff_density_min -2.994 _refine_diff_density_rms 0.299 #END