Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 #------------------------------------------------------------------------- #2 Person making the deposition # _publ_contact_author 'Prof Chi-Ming Che' _publ_contact_author_address ; Prof Chi-Ming Che Department of Chemistry The University of Hong Kong Pokfulam Road HONG KONG ; _publ_contact_author_email CMCHE@HKU.HK #------------------------------------------------------------------------- #3 Publication details # loop_ _publ_author_name 'Wei Lu' 'Bao-Xiu Mi' 'Michael C. W. Chan' 'Zheng Hui' 'Nian-Yong Zhu' 'Shuit-Tong Lee' 'Chi-Ming Che' _journal_name_full 'Chemical communication' _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _publ_section_title ; [(C^N^N)Pt(C?C)nR] (HC^N^N = 6-aryl-2,2'-bipyridine, n = 1?4, R = aryl, SiMe3) as New Class of Light-Emitting Materials and their Applications in Electrophosphorescent Devices? ; #------------------------------------------------------------------------- #4 Chemical and physical data # #------------------------------------------------------------------------- #5 Other data relating to the structure determination and refinement # #------------------------------------------------------------------------- data_mar120b _database_code_CSD 172097 _audit_creation_date 2001-09-26T16:54:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #--------------------------------------------------------------------------- # CHEMICAL INFORMATION # #--------------------------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H14 N2 Pt1' _chemical_formula_structural 'PT1 N2 C27 H14' _chemical_formula_sum 'C26 H16 N2 Pt' _chemical_formula_weight 551.5 _chemical_compound_source 'synthesis as described' #--------------------------------------------------------------------------- # UNIT CELL INFORMATION # #--------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _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 15.268(3) _cell_length_b 12.626(3) _cell_length_c 10.929(2) _cell_angle_alpha 90 _cell_angle_beta 107.33(3) _cell_angle_gamma 90 _cell_volume 2011.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 301(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #--------------------------------------------------------------------------- # CRYSTAL INFORMATION # #--------------------------------------------------------------------------- _exptl_crystal_description prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.821 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- # ABSORPTION CORRECTION # #--------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 6.991 _exptl_absorpt_correction_type none #--------------------------------------------------------------------------- # DATA COLLECTION # #--------------------------------------------------------------------------- _diffrn_ambient_temperature 301(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_unetI/netI 0.0746 _diffrn_reflns_number 9846 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 25.55 _diffrn_reflns_theta_full 25.55 _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _reflns_number_total 3584 _reflns_number_gt 2521 _reflns_threshold_expression >2sigma(I) #--------------------------------------------------------------------------- # COMPUTER PROGRAMS USED # #--------------------------------------------------------------------------- _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #--------------------------------------------------------------------------- # REFINEMENT INFORMATION # #--------------------------------------------------------------------------- _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^)+(0.0520P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3584 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.83 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.251 #--------------------------------------------------------------------------- -# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #--------------------------------------------------------------------------- -# 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' 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.60771(2) 0.45213(2) 0.21725(2) 0.05364(14) Uani 1 1 d . . . N1 N 0.5239(4) 0.3713(4) 0.0721(5) 0.0543(15) Uani 1 1 d . . . N2 N 0.4819(5) 0.4889(5) 0.2435(6) 0.0698(18) Uani 1 1 d . . . C1 C 0.6905(6) 0.5352(6) 0.3549(8) 0.065(2) Uani 1 1 d . . . C2 C 0.7427(6) 0.5918(7) 0.4337(8) 0.065(2) Uani 1 1 d . . . C3 C 0.8016(6) 0.6596(6) 0.5149(7) 0.061(2) Uani 1 1 d . . . C4 C 0.8530(5) 0.7220(6) 0.5823(7) 0.0629(19) Uani 1 1 d . . . C5 C 0.9163(5) 0.7992(6) 0.6569(7) 0.0643(19) Uani 1 1 d . . . C6 C 0.9157(6) 0.8231(7) 0.7792(7) 0.079(3) Uani 1 1 d . . . H6 H 0.8737 0.79 0.8131 0.095 Uiso 1 1 calc R . . C7 C 0.9757(8) 0.8946(9) 0.8511(10) 0.103(3) Uani 1 1 d . . . H7 H 0.9756 0.9082 0.9346 0.124 Uiso 1 1 calc R . . C8 C 1.0356(9) 0.9460(8) 0.8031(13) 0.120(4) Uani 1 1 d . . . H8 H 1.0758 0.9955 0.8529 0.144 Uiso 1 1 calc R . . C9 C 1.0369(9) 0.9248(10) 0.6791(13) 0.124(4) Uani 1 1 d . . . H9 H 1.0783 0.9594 0.6454 0.149 Uiso 1 1 calc R . . C10 C 0.9760(7) 0.8514(8) 0.6062(9) 0.102(3) Uani 1 1 d . . . H10 H 0.9756 0.8376 0.5225 0.122 Uiso 1 1 calc R . . C11 C 0.4643(7) 0.5471(6) 0.3387(9) 0.072(2) Uani 1 1 d . . . H11 H 0.5126 0.5805 0.3988 0.086 Uiso 1 1 calc R . . C12 C 0.3776(8) 0.5577(6) 0.3477(10) 0.085(3) Uani 1 1 d . . . H12 H 0.3679 0.5947 0.4161 0.102 Uiso 1 1 calc R . . C13 C 0.3045(8) 0.5137(8) 0.2564(11) 0.090(3) Uani 1 1 d . . . H13 H 0.2451 0.5229 0.2608 0.108 Uiso 1 1 calc R . . C14 C 0.3205(7) 0.4554(6) 0.1573(9) 0.075(2) Uani 1 1 d . . . H14 H 0.2716 0.4246 0.0953 0.09 Uiso 1 1 calc R . . C15 C 0.4091(6) 0.4430(5) 0.1508(7) 0.0581(19) Uani 1 1 d . . . C16 C 0.4338(6) 0.3772(5) 0.0540(7) 0.0583(19) Uani 1 1 d . . . C17 C 0.3745(6) 0.3242(6) -0.0478(8) 0.074(2) Uani 1 1 d . . . H17 H 0.3115 0.3265 -0.0608 0.089 Uiso 1 1 calc R . . C18 C 0.4099(8) 0.2683(7) -0.1289(8) 0.087(3) Uani 1 1 d . . . H18 H 0.3704 0.2339 -0.199 0.105 Uiso 1 1 calc R . . C19 C 0.5035(7) 0.2620(6) -0.1084(8) 0.078(2) Uani 1 1 d . . . H19 H 0.5271 0.2221 -0.1629 0.094 Uiso 1 1 calc R . . C20 C 0.5622(6) 0.3163(5) -0.0047(7) 0.0585(19) Uani 1 1 d . . . C21 C 0.6632(6) 0.3232(5) 0.0347(8) 0.064(2) Uani 1 1 d . . . C22 C 0.7159(8) 0.2713(7) -0.0294(9) 0.085(3) Uani 1 1 d . . . H22 H 0.688 0.2308 -0.1016 0.102 Uiso 1 1 calc R . . C23 C 0.8107(9) 0.2798(9) 0.0145(12) 0.108(4) Uani 1 1 d . . . H23 H 0.8471 0.2437 -0.0263 0.13 Uiso 1 1 calc R . . C24 C 0.8496(7) 0.3421(9) 0.1187(11) 0.107(3) Uani 1 1 d . . . H24 H 0.913 0.3499 0.149 0.128 Uiso 1 1 calc R . . C25 C 0.7937(7) 0.3935(7) 0.1786(9) 0.088(3) Uani 1 1 d . . . H25 H 0.8209 0.4358 0.2494 0.106 Uiso 1 1 calc R . . C26 C 0.7027(5) 0.3851(5) 0.1397(7) 0.0545(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0598(2) 0.04993(19) 0.05221(19) -0.00045(12) 0.01834(14) -0.00419(13) N1 0.067(5) 0.046(3) 0.049(3) 0.006(3) 0.016(3) -0.003(3) N2 0.087(6) 0.059(4) 0.066(4) 0.001(3) 0.028(4) 0.002(4) C1 0.064(6) 0.073(5) 0.061(5) 0.008(4) 0.024(4) -0.001(4) C2 0.054(5) 0.075(5) 0.063(5) -0.011(4) 0.014(4) -0.005(4) C3 0.052(5) 0.073(5) 0.061(4) -0.002(4) 0.021(4) 0.007(4) C4 0.049(5) 0.077(5) 0.063(4) -0.004(4) 0.017(4) 0.002(4) C5 0.047(5) 0.074(5) 0.070(5) -0.012(4) 0.014(4) 0.000(4) C6 0.078(7) 0.090(6) 0.072(5) -0.023(5) 0.029(5) -0.014(5) C7 0.106(9) 0.114(8) 0.088(6) -0.040(6) 0.027(6) -0.020(7) C8 0.116(11) 0.117(9) 0.117(9) -0.056(7) 0.021(8) -0.034(7) C9 0.098(10) 0.150(10) 0.136(11) -0.018(9) 0.051(8) -0.054(8) C10 0.094(8) 0.127(8) 0.091(6) -0.029(6) 0.040(6) -0.049(7) C11 0.081(7) 0.070(5) 0.072(5) -0.010(4) 0.034(5) 0.002(4) C12 0.095(8) 0.078(6) 0.093(7) -0.009(5) 0.044(6) 0.011(5) C13 0.078(8) 0.084(6) 0.116(8) 0.006(6) 0.042(7) 0.017(6) C14 0.065(6) 0.069(5) 0.089(6) 0.004(4) 0.022(5) 0.002(4) C15 0.067(6) 0.048(4) 0.058(4) 0.008(3) 0.018(4) 0.000(4) C16 0.065(6) 0.049(4) 0.059(4) 0.012(3) 0.015(4) -0.001(4) C17 0.071(6) 0.066(5) 0.079(5) -0.010(4) 0.014(5) -0.021(4) C18 0.104(9) 0.073(6) 0.074(6) -0.027(5) 0.008(5) -0.023(5) C19 0.107(8) 0.054(5) 0.073(5) -0.015(4) 0.025(5) -0.016(5) C20 0.081(6) 0.039(3) 0.062(4) 0.001(3) 0.030(4) -0.001(4) C21 0.072(6) 0.051(4) 0.078(5) 0.008(4) 0.036(5) -0.002(4) C22 0.105(9) 0.074(5) 0.089(6) -0.011(5) 0.049(6) -0.007(5) C23 0.096(9) 0.109(8) 0.140(10) -0.015(8) 0.067(8) 0.005(7) C24 0.067(7) 0.127(9) 0.135(9) -0.021(8) 0.041(7) 0.004(6) C25 0.095(8) 0.079(6) 0.097(7) -0.008(5) 0.039(6) -0.006(5) C26 0.047(5) 0.054(4) 0.062(4) 0.002(4) 0.014(4) -0.009(3) #--------------------------------------------------------------------------- # MOLECULAR GEOMETRY # #--------------------------------------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 1.957(9) . ? Pt1 N1 1.996(6) . ? Pt1 C26 2.066(7) . ? Pt1 N2 2.078(7) . ? N1 C16 1.332(9) . ? N1 C20 1.350(9) . ? N2 C11 1.364(10) . ? N2 C15 1.387(10) . ? C1 C2 1.216(11) . ? C2 C3 1.362(12) . ? C3 C4 1.197(10) . ? C4 C5 1.442(11) . ? C5 C10 1.369(11) . ? C5 C6 1.372(10) . ? C6 C7 1.357(12) . ? C7 C8 1.348(15) . ? C8 C9 1.387(16) . ? C9 C10 1.384(14) . ? C11 C12 1.362(14) . ? C12 C13 1.373(14) . ? C13 C14 1.390(13) . ? C14 C15 1.386(12) . ? C15 C16 1.479(10) . ? C16 C17 1.381(10) . ? C17 C18 1.364(12) . ? C18 C19 1.382(12) . ? C19 C20 1.398(11) . ? C20 C21 1.474(11) . ? C21 C26 1.371(10) . ? C21 C22 1.381(11) . ? C22 C23 1.387(14) . ? C23 C24 1.366(14) . ? C24 C25 1.383(13) . ? C25 C26 1.330(11) . ? 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 N1 177.9(3) . . ? C1 Pt1 C26 99.4(3) . . ? N1 Pt1 C26 80.0(3) . . ? C1 Pt1 N2 100.7(3) . . ? N1 Pt1 N2 79.9(3) . . ? C26 Pt1 N2 159.9(3) . . ? C16 N1 C20 123.8(6) . . ? C16 N1 Pt1 118.6(5) . . ? C20 N1 Pt1 117.6(5) . . ? C11 N2 C15 119.0(8) . . ? C11 N2 Pt1 128.8(6) . . ? C15 N2 Pt1 112.2(5) . . ? C2 C1 Pt1 175.3(7) . . ? C1 C2 C3 175.9(9) . . ? C4 C3 C2 177.4(9) . . ? C3 C4 C5 176.7(8) . . ? C10 C5 C6 119.1(8) . . ? C10 C5 C4 120.8(7) . . ? C6 C5 C4 120.1(7) . . ? C7 C6 C5 120.7(9) . . ? C8 C7 C6 120.9(10) . . ? C7 C8 C9 119.7(10) . . ? C10 C9 C8 119.2(11) . . ? C5 C10 C9 120.2(9) . . ? C12 C11 N2 121.6(9) . . ? C11 C12 C13 120.3(9) . . ? C12 C13 C14 119.2(10) . . ? C15 C14 C13 120.0(9) . . ? C14 C15 N2 119.8(7) . . ? C14 C15 C16 124.1(8) . . ? N2 C15 C16 116.0(7) . . ? N1 C16 C17 119.5(7) . . ? N1 C16 C15 113.4(7) . . ? C17 C16 C15 127.1(8) . . ? C18 C17 C16 118.9(9) . . ? C17 C18 C19 121.0(8) . . ? C18 C19 C20 119.1(8) . . ? N1 C20 C19 117.7(8) . . ? N1 C20 C21 113.4(6) . . ? C19 C20 C21 128.9(8) . . ? C26 C21 C22 121.2(8) . . ? C26 C21 C20 116.1(7) . . ? C22 C21 C20 122.7(8) . . ? C21 C22 C23 119.6(9) . . ? C24 C23 C22 118.9(10) . . ? C23 C24 C25 119.2(10) . . ? C26 C25 C24 123.0(9) . . ? C25 C26 C21 118.1(8) . . ? C25 C26 Pt1 129.1(6) . . ? C21 C26 Pt1 112.8(6) . . ? #===END #------------------------------------------------------------------------- data_mar20 _database_code_CSD 161089 _audit_creation_date 2001-09-26T16:55:07-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #--------------------------------------------------------------------------- -# # CHEMICAL INFORMATION # #--------------------------------------------------------------------------- -# _chemical_name_systematic ; ? ; _chemical_name_common Platinum-compound _chemical_formula_moiety 'C25 H18 N2 Pt' _chemical_formula_structural 'PT1 C30 N2 H30' _chemical_formula_sum 'C25 H18 N2 Pt' _chemical_formula_weight 541.5 _chemical_compound_source 'synthesis as described' #--------------------------------------------------------------------------- -# # UNIT CELL INFORMATION # #--------------------------------------------------------------------------- -# _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 34.132(3) _cell_length_b 34.132(3) _cell_length_c 8.6940(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 8771.6(15) _cell_formula_units_Z 18 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_wavelength 0.71073 #--------------------------------------------------------------------------- -# # CRYSTAL INFORMATION # #--------------------------------------------------------------------------- -# _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4680 _exptl_special_details ; ? ; #--------------------------------------------------------------------------- -# # ABSORPTION CORRECTION # #--------------------------------------------------------------------------- -# _exptl_absorpt_coefficient_mu 7.211 _exptl_absorpt_correction_type None #--------------------------------------------------------------------------- -# # DATA COLLECTION # #--------------------------------------------------------------------------- -# _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type MarResearch-IP300 _diffrn_measurement_method Imaging _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_number 11467 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.51 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.896 _diffrn_measured_fraction_theta_max 0.896 _reflns_number_total 3260 _reflns_number_gt 2469 _reflns_threshold_expression >2sigma(I) #--------------------------------------------------------------------------- # COMPUTER PROGRAMS USED # #--------------------------------------------------------------------------- _computing_data_collection MarControl _computing_cell_refinement Scalepack _computing_data_reduction Denzo _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 'WinGX publication routines (Farrugia, 1999)' #--------------------------------------------------------------------------- # REFINEMENT INFORMATION # #--------------------------------------------------------------------------- _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^)+(0.0637P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3260 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.095 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.382 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.212 #--------------------------------------------------------------------------- -# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #--------------------------------------------------------------------------- -# 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' 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.114616(10) 0.310353(11) 0.94675(3) 0.05647(16) Uani 1 1 d . . . N1 N 0.1277(2) 0.3733(2) 0.9048(7) 0.0573(16) Uani 1 1 d . . . N2 N 0.1716(2) 0.3478(3) 1.0870(7) 0.0651(18) Uani 1 1 d . . . C25 C 0.0650(3) 0.2955(3) 0.7954(8) 0.059(2) Uani 1 1 d . . . C1 C 0.0326(3) 0.2543(3) 0.7376(9) 0.067(2) Uani 1 1 d . . . H1 H 0.0316 0.228 0.7714 0.081 Uiso 1 1 calc R . . C2 C 0.0015(3) 0.2519(3) 0.6291(9) 0.076(2) Uani 1 1 d . . . H2 H -0.0201 0.2238 0.5911 0.091 Uiso 1 1 calc R . . C3 C 0.0022(3) 0.2904(4) 0.5770(11) 0.079(3) Uani 1 1 d . . . H3 H -0.0191 0.2882 0.5054 0.095 Uiso 1 1 calc R . . C4 C 0.0339(3) 0.3314(3) 0.6305(9) 0.068(2) Uani 1 1 d . . . H4 H 0.0349 0.3575 0.5937 0.082 Uiso 1 1 calc R . . C5 C 0.0650(3) 0.3347(3) 0.7403(8) 0.0576(19) Uani 1 1 d . . . C6 C 0.1002(3) 0.3783(3) 0.8034(8) 0.0570(19) Uani 1 1 d . . . C7 C 0.1084(3) 0.4220(3) 0.7760(10) 0.070(2) Uani 1 1 d . . . H7 H 0.0896 0.4268 0.7108 0.084 Uiso 1 1 calc R . . C8 C 0.1443(3) 0.4577(3) 0.8452(12) 0.083(3) Uani 1 1 d . . . H8 H 0.1506 0.4869 0.8219 0.1 Uiso 1 1 calc R . . C9 C 0.1715(3) 0.4516(4) 0.9493(11) 0.079(3) Uani 1 1 d . . . H9 H 0.1952 0.4761 0.9991 0.095 Uiso 1 1 calc R . . C10 C 0.1620(3) 0.4073(3) 0.9769(9) 0.066(2) Uani 1 1 d . . . C11 C 0.1873(3) 0.3938(3) 1.0836(9) 0.066(2) Uani 1 1 d . . . C12 C 0.2233(3) 0.4233(4) 1.1710(11) 0.089(3) Uani 1 1 d . . . H12 H 0.2333 0.4541 1.1681 0.106 Uiso 1 1 calc R . . C13 C 0.2447(4) 0.4065(5) 1.2647(12) 0.098(4) Uani 1 1 d . . . H13 H 0.269 0.4261 1.3262 0.118 Uiso 1 1 calc R . . C14 C 0.2298(4) 0.3612(5) 1.2657(12) 0.096(4) Uani 1 1 d . . . H14 H 0.2443 0.3497 1.3262 0.116 Uiso 1 1 calc R . . C15 C 0.1934(3) 0.3327(4) 1.1769(9) 0.075(2) Uani 1 1 d . . . H15 H 0.1835 0.3019 1.1786 0.09 Uiso 1 1 calc R . . C16 C 0.1015(3) 0.2486(3) 1.0002(9) 0.064(2) Uani 1 1 d . . . C17 C 0.0974(3) 0.2141(3) 1.0466(10) 0.071(2) Uani 1 1 d . . . C18 C 0.0947(3) 0.1750(3) 1.1178(10) 0.067(2) Uani 1 1 d . . . C19 C 0.0586(4) 0.1319(3) 1.0988(12) 0.090(3) Uani 1 1 d . . . H19 H 0.0345 0.1271 1.0362 0.108 Uiso 1 1 calc R . . C20 C 0.0581(4) 0.0951(4) 1.1736(15) 0.104(4) Uani 1 1 d . . . H20 H 0.0338 0.0662 1.1575 0.125 Uiso 1 1 calc R . . C21 C 0.0919(5) 0.1003(4) 1.2685(15) 0.103(4) Uani 1 1 d . . . C22 C 0.1270(4) 0.1426(4) 1.2872(12) 0.093(3) Uani 1 1 d . . . H22 H 0.1503 0.1473 1.3538 0.112 Uiso 1 1 calc R . . C23 C 0.1294(3) 0.1792(3) 1.2109(11) 0.081(3) Uani 1 1 d . . . H23 H 0.1552 0.2075 1.2223 0.098 Uiso 1 1 calc R . . C24 C 0.0905(5) 0.0600(4) 1.3467(17) 0.147(6) Uani 1 1 d . . . H24A H 0.063 0.033 1.3195 0.22 Uiso 1 1 calc R . . H24B H 0.0917 0.064 1.4562 0.22 Uiso 1 1 calc R . . H24C H 0.1159 0.0573 1.314 0.22 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 0.0611(2) 0.0728(3) 0.0454(2) 0.00822(12) 0.00785(12) 0.04085(19) N1 0.050(4) 0.077(5) 0.050(4) 0.005(3) 0.009(3) 0.036(4) N2 0.059(4) 0.099(6) 0.043(4) 0.011(3) 0.015(3) 0.044(4) C25 0.063(5) 0.069(5) 0.051(4) 0.003(4) 0.014(3) 0.037(4) C1 0.071(6) 0.072(6) 0.059(5) 0.006(4) 0.007(4) 0.036(5) C2 0.075(6) 0.079(6) 0.061(5) 0.001(4) 0.006(4) 0.029(5) C3 0.066(6) 0.105(8) 0.065(6) 0.010(5) -0.003(4) 0.041(6) C4 0.061(5) 0.091(7) 0.056(5) 0.020(4) 0.004(4) 0.041(5) C5 0.064(5) 0.069(5) 0.051(4) 0.014(4) 0.015(3) 0.042(4) C6 0.055(5) 0.070(6) 0.050(4) 0.012(4) 0.012(3) 0.035(4) C7 0.077(6) 0.071(6) 0.072(6) 0.019(4) 0.013(4) 0.044(5) C8 0.082(7) 0.068(6) 0.099(7) 0.019(5) 0.030(6) 0.037(6) C9 0.067(6) 0.080(7) 0.081(6) -0.005(5) 0.013(5) 0.030(5) C10 0.056(5) 0.079(6) 0.060(5) -0.001(4) 0.015(4) 0.031(5) C11 0.055(5) 0.093(7) 0.047(5) -0.001(4) 0.011(4) 0.036(5) C12 0.069(6) 0.111(9) 0.074(6) -0.017(6) -0.004(5) 0.037(6) C13 0.061(7) 0.138(11) 0.074(7) -0.021(7) -0.004(5) 0.034(7) C14 0.059(6) 0.182(14) 0.055(6) 0.005(7) 0.010(4) 0.066(8) C15 0.063(6) 0.117(8) 0.051(5) 0.017(5) 0.014(4) 0.050(6) C16 0.057(5) 0.093(7) 0.054(5) 0.004(4) 0.001(3) 0.047(5) C17 0.081(6) 0.083(7) 0.069(5) 0.007(5) 0.003(4) 0.057(6) C18 0.065(6) 0.068(6) 0.078(6) 0.001(4) 0.007(4) 0.042(5) C19 0.087(7) 0.070(7) 0.116(8) -0.007(6) -0.013(6) 0.041(6) C20 0.097(8) 0.058(7) 0.147(11) -0.006(6) 0.010(8) 0.031(6) C21 0.120(10) 0.088(9) 0.123(10) 0.035(7) 0.028(8) 0.067(8) C22 0.094(8) 0.106(9) 0.095(7) 0.019(6) 0.011(6) 0.062(8) C23 0.074(6) 0.070(6) 0.103(7) 0.017(5) 0.002(5) 0.039(5) C24 0.176(14) 0.097(10) 0.197(16) 0.055(10) 0.048(12) 0.091(10) #--------------------------------------------------------------------------- # MOLECULAR GEOMETRY # #--------------------------------------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C16 1.978(10) . ? Pt1 N1 1.997(7) . ? Pt1 C25 2.000(8) . ? Pt1 N2 2.101(7) . ? N1 C10 1.324(11) . ? N1 C6 1.361(10) . ? N2 C15 1.349(10) . ? N2 C11 1.383(11) . ? C25 C1 1.377(12) . ? C25 C5 1.419(11) . ? C1 C2 1.392(12) . ? C2 C3 1.380(14) . ? C3 C4 1.354(13) . ? C4 C5 1.390(11) . ? C5 C6 1.474(12) . ? C6 C7 1.393(11) . ? C7 C8 1.361(13) . ? C8 C9 1.385(13) . ? C9 C10 1.401(13) . ? C10 C11 1.489(12) . ? C11 C12 1.364(13) . ? C12 C13 1.395(15) . ? C13 C14 1.367(16) . ? C14 C15 1.370(17) . ? C16 C17 1.185(12) . ? C17 C18 1.431(12) . ? C18 C19 1.377(13) . ? C18 C23 1.384(12) . ? C19 C20 1.407(15) . ? C20 C21 1.355(16) . ? C21 C22 1.348(16) . ? C21 C24 1.515(14) . ? C22 C23 1.378(13) . ? 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 N1 176.9(3) . . ? C16 Pt1 C25 100.0(3) . . ? N1 Pt1 C25 81.8(3) . . ? C16 Pt1 N2 99.2(3) . . ? N1 Pt1 N2 79.1(3) . . ? C25 Pt1 N2 160.8(3) . . ? C10 N1 C6 124.1(8) . . ? C10 N1 Pt1 118.7(6) . . ? C6 N1 Pt1 117.2(6) . . ? C15 N2 C11 118.1(8) . . ? C15 N2 Pt1 128.6(7) . . ? C11 N2 Pt1 113.3(5) . . ? C1 C25 C5 117.5(8) . . ? C1 C25 Pt1 130.0(6) . . ? C5 C25 Pt1 112.5(6) . . ? C25 C1 C2 120.5(9) . . ? C3 C2 C1 121.1(9) . . ? C4 C3 C2 119.8(9) . . ? C3 C4 C5 120.2(9) . . ? C4 C5 C25 121.0(8) . . ? C4 C5 C6 122.7(7) . . ? C25 C5 C6 116.3(7) . . ? N1 C6 C7 117.6(8) . . ? N1 C6 C5 112.2(7) . . ? C7 C6 C5 130.2(8) . . ? C8 C7 C6 119.5(9) . . ? C7 C8 C9 121.7(10) . . ? C8 C9 C10 117.6(9) . . ? N1 C10 C9 119.4(9) . . ? N1 C10 C11 114.8(8) . . ? C9 C10 C11 125.7(9) . . ? C12 C11 N2 121.4(9) . . ? C12 C11 C10 124.5(10) . . ? N2 C11 C10 114.1(8) . . ? C11 C12 C13 119.1(12) . . ? C14 C13 C12 119.5(11) . . ? C13 C14 C15 119.5(11) . . ? N2 C15 C14 122.3(11) . . ? C17 C16 Pt1 171.9(8) . . ? C16 C17 C18 173.7(10) . . ? C19 C18 C23 116.2(9) . . ? C19 C18 C17 123.5(9) . . ? C23 C18 C17 120.3(9) . . ? C18 C19 C20 120.3(10) . . ? C21 C20 C19 122.4(10) . . ? C22 C21 C20 117.1(10) . . ? C22 C21 C24 121.9(13) . . ? C20 C21 C24 121.1(13) . . ? C21 C22 C23 122.1(11) . . ? C22 C23 C18 121.9(10) . . ? #===END