# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_name 'Elena Lalinde' _publ_contact_author_email elena.lalinde@dq.unirioja.es _publ_author_name E.Lalinde data_2 _database_code_depnum_ccdc_archive 'CCDC 874676' #TrackingRef '- CC-COM-04-2012-032390.cif' _audit_creation_date 2012-04-25T19:33:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_sum 'C22 H20 N2 O2 Pt Tl2' _chemical_formula_weight 948.23 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2450(3) _cell_length_b 7.3320(3) _cell_length_c 13.4130(6) _cell_angle_alpha 87.875(3) _cell_angle_beta 86.713(3) _cell_angle_gamma 70.242(2) _cell_volume 576.95(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 867 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 19.996 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Linear fit to sin(theta)/lambda - 12 parameters ; _exptl_absorpt_correction_T_min 0.0037 _exptl_absorpt_correction_T_max 0.0099 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.1649446 _diffrn_orient_matrix_ub_12 0.0708348 _diffrn_orient_matrix_ub_13 0.0164296 _diffrn_orient_matrix_ub_21 0.0293223 _diffrn_orient_matrix_ub_22 -0.0169665 _diffrn_orient_matrix_ub_23 0.0728548 _diffrn_orient_matrix_ub_31 0.0308603 _diffrn_orient_matrix_ub_32 0.1253175 _diffrn_orient_matrix_ub_33 -0.0010504 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0392 _diffrn_reflns_number 1999 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 1999 _reflns_number_gt 1852 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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^)+(0.1072P)^2^+0.2554P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1999 _refine_ls_number_parameters 135 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1365 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.156 _refine_diff_density_min -4.078 _refine_diff_density_rms 0.524 #----------------------------------------------------------------------------# # 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' Tl Tl -2.8358 9.6688 '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' N N 0.0061 0.0033 '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' O O 0.0106 0.006 '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 0 0 0.0118(2) Uani 1 2 d S . . Tl1 Tl -0.30324(6) 0.72235(5) 0.03264(3) 0.0164(2) Uani 1 1 d . . . N1 N -0.3405(14) 0.3705(12) 0.1049(6) 0.0210(19) Uani 1 1 d . . . C1 C -0.2147(16) 0.2328(14) 0.0680(8) 0.018(2) Uani 1 1 d . . . C2 C -0.1814(16) 0.0714(13) -0.1238(8) 0.016(2) Uani 1 1 d . . . C3 C -0.3018(17) 0.1121(13) -0.1941(7) 0.017(2) Uani 1 1 d . . . C4 C -0.4497(16) 0.1447(14) -0.2752(7) 0.017(2) Uani 1 1 d . . . C5 C -0.6138(17) 0.0516(14) -0.2766(7) 0.017(2) Uani 1 1 d . . . H5 H -0.6276 -0.0314 -0.2224 0.021 Uiso 1 1 calc R . . C6 C -0.7571(17) 0.0801(15) -0.3570(8) 0.021(2) Uani 1 1 d . . . H6 H -0.868 0.0176 -0.3556 0.025 Uiso 1 1 calc R . . C7 C -0.7404(17) 0.1963(14) -0.4376(7) 0.017(2) Uani 1 1 d . . . C8 C -0.887(2) 0.2221(16) -0.5262(8) 0.025(2) Uani 1 1 d . . . H8A H -0.7968 0.1444 -0.5816 0.037 Uiso 1 1 calc R . . H8B H -0.9422 0.3591 -0.5467 0.037 Uiso 1 1 calc R . . H8C H -1.0169 0.1795 -0.5078 0.037 Uiso 1 1 calc R . . C9 C -0.5748(18) 0.2881(14) -0.4367(8) 0.022(2) Uani 1 1 d . . . H9 H -0.5587 0.3677 -0.4921 0.026 Uiso 1 1 calc R . . C10 C -0.4378(17) 0.2656(14) -0.3587(7) 0.018(2) Uani 1 1 d . . . H10 H -0.3314 0.3327 -0.3602 0.022 Uiso 1 1 calc R . . O1 O -0.1025(12) 0.4722(9) -0.1280(5) 0.0197(15) Uani 1 1 d . . . C11 C -0.1104(18) 0.5643(15) -0.2231(7) 0.021(2) Uani 1 1 d . . . H11A H -0.2672 0.6088 -0.2449 0.032 Uiso 1 1 calc R . . H11B H -0.0112 0.4723 -0.2712 0.032 Uiso 1 1 calc R . . H11C H -0.0583 0.6756 -0.2189 0.032 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 0.0141(4) 0.0128(4) 0.0092(4) 0.0010(2) -0.0043(3) -0.0048(3) Tl1 0.0155(3) 0.0158(3) 0.0174(3) 0.0000(2) -0.0012(2) -0.0046(2) N1 0.025(5) 0.017(4) 0.020(5) -0.002(4) 0.002(4) -0.006(4) C1 0.015(5) 0.025(5) 0.015(5) 0.002(4) 0.001(4) -0.011(4) C2 0.019(5) 0.010(4) 0.019(6) 0.004(4) -0.003(4) -0.004(4) C3 0.029(5) 0.014(5) 0.008(5) -0.004(4) 0.005(4) -0.009(4) C4 0.017(5) 0.019(5) 0.009(5) 0.001(4) -0.007(4) 0.000(4) C5 0.026(5) 0.020(5) 0.007(5) -0.005(4) 0.002(4) -0.009(4) C6 0.022(5) 0.027(6) 0.018(6) -0.012(4) 0.004(4) -0.014(5) C7 0.021(5) 0.020(5) 0.008(5) 0.002(4) -0.009(4) -0.004(4) C8 0.040(6) 0.031(6) 0.006(5) 0.000(4) -0.005(5) -0.014(5) C9 0.031(6) 0.020(5) 0.018(6) 0.006(4) -0.007(4) -0.014(5) C10 0.025(5) 0.016(5) 0.013(5) 0.009(4) -0.005(4) -0.007(4) O1 0.027(4) 0.019(4) 0.016(4) 0.005(3) -0.004(3) -0.012(3) C11 0.031(6) 0.024(5) 0.010(5) 0.000(4) -0.002(4) -0.011(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.993(10) 2 ? Pt1 C1 1.993(10) . ? Pt1 C2 2.016(10) 2 ? Pt1 C2 2.016(10) . ? Pt1 Tl1 3.2198(3) 1_545 ? Pt1 Tl1 3.2198(3) 2_565 ? Tl1 N1 2.800(8) . ? Tl1 Pt1 3.2198(3) 1_565 ? N1 C1 1.156(13) . ? C2 C3 1.205(14) . ? C3 C4 1.429(14) . ? C4 C5 1.412(13) . ? C4 C10 1.416(13) . ? C5 C6 1.406(14) . ? C5 H5 0.95 . ? C6 C7 1.373(14) . ? C6 H6 0.95 . ? C7 C9 1.412(13) . ? C7 C8 1.508(14) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.360(14) . ? C9 H9 0.95 . ? C10 H10 0.95 . ? O1 C11 1.417(11) . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? 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 C1 180.0 . . ? C1 Pt1 C2 90.2(4) 2 2 ? C1 Pt1 C2 89.8(4) . 2 ? C1 Pt1 C2 89.8(4) 2 . ? C1 Pt1 C2 90.2(4) . . ? C2 Pt1 C2 180.0 . . ? C1 Pt1 Tl1 82.1(2) 2 1_545 ? C1 Pt1 Tl1 97.9(2) . 1_545 ? C2 Pt1 Tl1 99.6(2) 2 1_545 ? C2 Pt1 Tl1 80.4(2) . 1_545 ? C1 Pt1 Tl1 97.9(2) 2 2_565 ? C1 Pt1 Tl1 82.1(2) . 2_565 ? C2 Pt1 Tl1 80.4(2) 2 2_565 ? C2 Pt1 Tl1 99.6(2) . 2_565 ? Tl1 Pt1 Tl1 180.0 . . ? N1 Tl1 Pt1 148.67(17) . 1_565 ? C1 N1 Tl1 115.6(7) . . ? N1 C1 Pt1 178.1(9) . . ? C3 C2 Pt1 175.6(8) . . ? C2 C3 C4 174.7(10) . . ? C5 C4 C10 116.5(9) . . ? C5 C4 C3 120.6(8) . . ? C10 C4 C3 122.9(9) . . ? C6 C5 C4 120.9(9) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C7 C6 C5 121.5(9) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C9 117.6(9) . . ? C6 C7 C8 122.0(9) . . ? C9 C7 C8 120.3(9) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C7 121.8(9) . . ? C10 C9 H9 119.1 . . ? C7 C9 H9 119.1 . . ? C9 C10 C4 121.6(9) . . ? C9 C10 H10 119.2 . . ? C4 C10 H10 119.2 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 874677' #TrackingRef '- CC-COM-04-2012-032390.cif' _audit_creation_date 2012-04-27T17:16:51-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_formula_sum 'C44 H48 B2 N14 O3 Pb2 Pt' _chemical_formula_weight 1452.05 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7464(6) _cell_length_b 11.2992(7) _cell_length_c 15.3002(12) _cell_angle_alpha 71.013(4) _cell_angle_beta 89.708(3) _cell_angle_gamma 79.895(4) _cell_volume 1244.75(16) _cell_formula_units_Z 1 _cell_measurement_temperature 173.0(10) _cell_measurement_reflns_used 2645 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.934 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3319 _exptl_absorpt_correction_T_max 0.4175 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173.0(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.0386583 _diffrn_orient_matrix_ub_12 -0.0569052 _diffrn_orient_matrix_ub_13 0.0645188 _diffrn_orient_matrix_ub_21 0.1249031 _diffrn_orient_matrix_ub_22 -0.008297 _diffrn_orient_matrix_ub_23 -0.0176668 _diffrn_orient_matrix_ub_31 0.0123569 _diffrn_orient_matrix_ub_32 0.0758885 _diffrn_orient_matrix_ub_33 0.0178218 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.0501 _diffrn_reflns_number 16185 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 4373 _reflns_number_gt 3409 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # 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^ > 2\s(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. Three restrains have been used in order to modelize the acetone molecule: The restrains are as follow: DFIX 1.500 0.020 C21 C20 DFIX 1.500 0.020 C21 C22 FLAT 0.100 C20 C21 C22 O1 ; _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^)+(0.0469P)^2^+2.5664P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4373 _refine_ls_number_parameters 309 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0575 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0959 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.184 _refine_diff_density_min -1.682 _refine_diff_density_rms 0.155 #----------------------------------------------------------------------------# # 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 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' B B 0.0013 0.0007 '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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 C1 C 0.7540(12) 0.0900(8) 0.4565(6) 0.046(2) Uani 1 1 d . . . C2 C 0.9429(10) -0.0150(8) 0.6302(5) 0.038(2) Uani 1 1 d . . . C3 C 0.9102(10) -0.0286(7) 0.7087(6) 0.038(2) Uani 1 1 d . . . C4 C 0.8793(10) -0.0480(7) 0.8060(5) 0.0330(18) Uani 1 1 d . . . C5 C 0.9848(11) -0.1492(8) 0.8752(5) 0.0395(19) Uani 1 1 d . . . H5 H 1.0755 -0.2042 0.8579 0.047 Uiso 1 1 calc R . . C6 C 0.9580(11) -0.1691(8) 0.9670(6) 0.043(2) Uani 1 1 d . . . H6 H 1.0303 -0.2385 1.0121 0.051 Uiso 1 1 calc R . . C7 C 0.8283(11) -0.0910(8) 0.9961(5) 0.0375(19) Uani 1 1 d . . . C8 C 0.7248(12) 0.0103(8) 0.9285(6) 0.044(2) Uani 1 1 d . . . H8 H 0.6362 0.0663 0.9463 0.052 Uiso 1 1 calc R . . C9 C 0.7499(12) 0.0300(8) 0.8361(6) 0.044(2) Uani 1 1 d . . . H9 H 0.6766 0.0992 0.7914 0.053 Uiso 1 1 calc R . . C10 C 0.7980(13) -0.1134(9) 1.0977(6) 0.053(2) Uani 1 1 d . . . H10A H 0.703 -0.0472 1.1038 0.08 Uiso 1 1 calc R . . H10B H 0.9059 -0.1101 1.1294 0.08 Uiso 1 1 calc R . . H10C H 0.7657 -0.1971 1.1257 0.08 Uiso 1 1 calc R . . C11 C -0.1438(10) 0.3531(8) 0.2647(6) 0.041(2) Uani 1 1 d . . . H11 H -0.1989 0.2969 0.312 0.049 Uiso 1 1 calc R . . C12 C -0.2294(10) 0.4447(8) 0.1869(6) 0.042(2) Uani 1 1 d . . . H12 H -0.3518 0.4636 0.1705 0.051 Uiso 1 1 calc R . . C13 C -0.1024(9) 0.5024(7) 0.1382(5) 0.039(2) Uani 1 1 d . . . H13 H -0.1202 0.5689 0.0802 0.047 Uiso 1 1 calc R . . C14 C 0.4334(12) 0.4841(9) 0.3745(7) 0.051(2) Uani 1 1 d . . . H14 H 0.4744 0.4459 0.4375 0.061 Uiso 1 1 calc R . . C15 C 0.4439(13) 0.6044(10) 0.3231(8) 0.064(3) Uani 1 1 d . . . H15 H 0.4904 0.6655 0.3417 0.077 Uiso 1 1 calc R . . C16 C 0.3715(11) 0.6185(8) 0.2375(8) 0.055(3) Uani 1 1 d . . . H16 H 0.3596 0.6935 0.1849 0.066 Uiso 1 1 calc R . . C17 C 0.5139(12) 0.1736(9) 0.1831(7) 0.053(2) Uani 1 1 d . . . H17 H 0.5716 0.0898 0.2174 0.064 Uiso 1 1 calc R . . C18 C 0.5304(13) 0.2321(10) 0.0908(7) 0.058(3) Uani 1 1 d . . . H18 H 0.5983 0.1982 0.0497 0.07 Uiso 1 1 calc R . . C19 C 0.4272(11) 0.3507(9) 0.0706(6) 0.046(2) Uani 1 1 d . . . H19 H 0.4104 0.4146 0.0113 0.055 Uiso 1 1 calc R . . B1 B 0.2372(11) 0.4776(9) 0.1612(7) 0.036(2) Uani 1 1 d . . . N1 N 0.6132(9) 0.1440(8) 0.4322(6) 0.063(2) Uani 1 1 d . . . N2 N 0.0298(8) 0.3549(6) 0.2640(4) 0.0392(17) Uani 1 1 d . . . N3 N 0.0529(7) 0.4492(6) 0.1861(4) 0.0343(15) Uani 1 1 d . . . N4 N 0.3587(8) 0.4249(6) 0.3265(5) 0.0409(17) Uani 1 1 d . . . N5 N 0.3207(8) 0.5107(6) 0.2395(5) 0.0374(16) Uani 1 1 d . . . N6 N 0.4058(8) 0.2499(6) 0.2186(5) 0.0390(16) Uani 1 1 d . . . N7 N 0.3543(8) 0.3618(6) 0.1472(4) 0.0332(15) Uani 1 1 d . . . Pb1 Pb 0.28423(4) 0.21073(3) 0.37117(2) 0.04115(14) Uani 1 1 d . . . Pt1 Pt 1 0 0.5 0.03198(13) Uani 1 2 d S . . O1 O 0.2086(13) 0.2975(11) 0.5230(7) 0.116(4) Uani 1 1 d D . . C21 C 0.095(2) 0.3029(11) 0.5671(9) 0.101(5) Uani 1 1 d D . . C20 C 0.067(2) 0.3009(19) 0.6619(9) 0.144(7) Uani 1 1 d D . . H20A H 0.1797 0.2718 0.6981 0.216 Uiso 1 1 calc R . . H20B H -0.0133 0.2427 0.6897 0.216 Uiso 1 1 calc R . . H20C H 0.0163 0.3868 0.6616 0.216 Uiso 1 1 calc R . . C22 C -0.0850(18) 0.3466(13) 0.5107(10) 0.107(5) Uani 1 1 d D . . H22A H -0.0677 0.3449 0.4476 0.16 Uiso 1 1 calc R . . H22B H -0.1357 0.4334 0.5085 0.16 Uiso 1 1 calc R . . H22C H -0.1648 0.289 0.5406 0.16 Uiso 1 1 calc R . . O2 O 0.484(3) -0.073(2) 0.3509(14) 0.136(8) Uani 0.5 1 d P . . H1 H 0.231(10) 0.571(8) 0.096(6) 0.05(2) Uiso 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 C1 0.051(6) 0.046(5) 0.030(5) 0.004(4) 0.000(4) -0.011(4) C2 0.036(5) 0.046(5) 0.025(4) -0.002(4) -0.003(3) -0.008(4) C3 0.037(5) 0.026(4) 0.040(5) -0.002(4) -0.005(4) 0.001(4) C4 0.035(4) 0.033(4) 0.033(4) -0.011(4) 0.004(3) -0.010(4) C5 0.040(5) 0.037(5) 0.038(5) -0.011(4) 0.001(4) 0.000(4) C6 0.045(5) 0.037(5) 0.041(5) -0.006(4) -0.004(4) -0.008(4) C7 0.046(5) 0.034(5) 0.036(4) -0.014(4) -0.005(4) -0.012(4) C8 0.051(5) 0.042(5) 0.046(5) -0.026(4) 0.008(4) -0.006(4) C9 0.049(5) 0.035(5) 0.040(5) -0.008(4) -0.008(4) 0.002(4) C10 0.069(6) 0.061(6) 0.031(5) -0.020(4) 0.002(4) -0.006(5) C11 0.028(4) 0.051(5) 0.043(5) -0.008(4) 0.002(4) -0.015(4) C12 0.014(4) 0.056(5) 0.050(5) -0.010(4) -0.005(3) -0.005(4) C13 0.026(4) 0.036(4) 0.040(5) 0.007(4) -0.013(3) -0.002(3) C14 0.042(5) 0.062(6) 0.053(6) -0.022(5) -0.003(4) -0.012(5) C15 0.054(6) 0.058(7) 0.098(9) -0.044(6) 0.003(6) -0.021(5) C16 0.038(5) 0.033(5) 0.095(8) -0.025(5) 0.004(5) -0.004(4) C17 0.046(6) 0.043(5) 0.069(7) -0.018(5) 0.000(5) -0.004(4) C18 0.049(6) 0.072(7) 0.069(7) -0.041(6) 0.013(5) -0.016(5) C19 0.038(5) 0.058(6) 0.045(5) -0.018(4) -0.002(4) -0.016(5) B1 0.016(4) 0.032(5) 0.048(6) 0.001(4) -0.007(4) -0.003(4) N1 0.028(4) 0.068(5) 0.066(6) 0.009(4) -0.009(4) 0.005(4) N2 0.028(4) 0.048(4) 0.031(4) 0.002(3) -0.002(3) -0.009(3) N3 0.018(3) 0.034(4) 0.039(4) 0.003(3) -0.006(3) -0.002(3) N4 0.031(4) 0.039(4) 0.047(4) -0.008(3) -0.005(3) -0.005(3) N5 0.026(3) 0.032(4) 0.052(4) -0.009(3) 0.002(3) -0.010(3) N6 0.032(4) 0.036(4) 0.044(4) -0.005(3) -0.003(3) -0.006(3) N7 0.027(3) 0.033(4) 0.038(4) -0.006(3) -0.001(3) -0.009(3) Pb1 0.03001(19) 0.0433(2) 0.0379(2) 0.00608(15) -0.01037(13) -0.01202(14) Pt1 0.0263(2) 0.0310(2) 0.0288(2) 0.00144(18) -0.00431(17) -0.00126(18) O1 0.091(7) 0.190(11) 0.085(7) -0.054(7) 0.043(6) -0.055(7) C21 0.122(13) 0.096(10) 0.092(11) -0.024(8) 0.029(10) -0.056(10) C20 0.105(11) 0.28(2) 0.064(9) -0.058(12) 0.035(8) -0.080(14) C22 0.115(12) 0.100(10) 0.099(11) -0.037(9) -0.025(9) 0.005(9) O2 0.140(19) 0.17(2) 0.100(15) -0.040(14) 0.009(13) -0.056(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 N1 1.150(11) . ? C1 Pt1 2.001(9) . ? C2 C3 1.191(11) . ? C2 Pt1 1.998(8) . ? C3 C4 1.458(11) . ? C4 C9 1.395(12) . ? C4 C5 1.410(11) . ? C5 C6 1.369(11) . ? C5 H5 0.95 . ? C6 C7 1.388(12) . ? C6 H6 0.95 . ? C7 C8 1.393(11) . ? C7 C10 1.516(12) . ? C8 C9 1.375(11) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 N2 1.348(10) . ? C11 C12 1.377(11) . ? C11 H11 0.95 . ? C12 C13 1.360(11) . ? C12 H12 0.95 . ? C13 N3 1.347(9) . ? C13 H13 0.95 . ? C14 N4 1.335(11) . ? C14 C15 1.347(13) . ? C14 H14 0.95 . ? C15 C16 1.377(14) . ? C15 H15 0.95 . ? C16 N5 1.336(10) . ? C16 H16 0.95 . ? C17 N6 1.337(11) . ? C17 C18 1.366(13) . ? C17 H17 0.95 . ? C18 C19 1.374(13) . ? C18 H18 0.95 . ? C19 N7 1.331(10) . ? C19 H19 0.95 . ? B1 N7 1.532(11) . ? B1 N3 1.536(10) . ? B1 N5 1.541(12) . ? B1 H1 1.19(8) . ? N1 Pb1 2.613(7) . ? N2 N3 1.352(8) . ? N2 Pb1 2.529(6) . ? N4 N5 1.364(9) . ? N4 Pb1 2.462(6) . ? N6 N7 1.371(8) . ? N6 Pb1 2.446(7) . ? Pt1 C2 1.998(8) 2_756 ? Pt1 C1 2.001(10) 2_756 ? O1 C21 1.109(15) . ? C21 C20 1.460(14) . ? C21 C22 1.559(14) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? 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 N1 C1 Pt1 178.4(9) . . ? C3 C2 Pt1 177.6(8) . . ? C2 C3 C4 177.1(8) . . ? C9 C4 C5 116.7(7) . . ? C9 C4 C3 123.5(7) . . ? C5 C4 C3 119.9(7) . . ? C6 C5 C4 120.8(8) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 122.0(8) . . ? C5 C6 H6 119 . . ? C7 C6 H6 119 . . ? C6 C7 C8 117.8(8) . . ? C6 C7 C10 122.0(7) . . ? C8 C7 C10 120.2(8) . . ? C9 C8 C7 120.5(8) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C4 122.2(8) . . ? C8 C9 H9 118.9 . . ? C4 C9 H9 118.9 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 110.0(7) . . ? N2 C11 H11 125 . . ? C12 C11 H11 125 . . ? C13 C12 C11 105.6(7) . . ? C13 C12 H12 127.2 . . ? C11 C12 H12 127.2 . . ? N3 C13 C12 108.5(7) . . ? N3 C13 H13 125.8 . . ? C12 C13 H13 125.8 . . ? N4 C14 C15 112.2(9) . . ? N4 C14 H14 123.9 . . ? C15 C14 H14 123.9 . . ? C14 C15 C16 104.1(8) . . ? C14 C15 H15 128 . . ? C16 C15 H15 128 . . ? N5 C16 C15 109.6(9) . . ? N5 C16 H16 125.2 . . ? C15 C16 H16 125.2 . . ? N6 C17 C18 111.0(8) . . ? N6 C17 H17 124.5 . . ? C18 C17 H17 124.5 . . ? C17 C18 C19 104.9(9) . . ? C17 C18 H18 127.6 . . ? C19 C18 H18 127.6 . . ? N7 C19 C18 109.2(8) . . ? N7 C19 H19 125.4 . . ? C18 C19 H19 125.4 . . ? N7 B1 N3 110.3(7) . . ? N7 B1 N5 109.3(6) . . ? N3 B1 N5 109.9(7) . . ? N7 B1 H1 112(4) . . ? N3 B1 H1 111(4) . . ? N5 B1 H1 104(4) . . ? C1 N1 Pb1 165.0(8) . . ? C11 N2 N3 106.2(6) . . ? C11 N2 Pb1 131.3(5) . . ? N3 N2 Pb1 122.4(4) . . ? C13 N3 N2 109.6(6) . . ? C13 N3 B1 129.5(6) . . ? N2 N3 B1 120.8(6) . . ? C14 N4 N5 105.9(7) . . ? C14 N4 Pb1 131.9(6) . . ? N5 N4 Pb1 122.3(5) . . ? C16 N5 N4 108.3(7) . . ? C16 N5 B1 129.5(8) . . ? N4 N5 B1 122.2(6) . . ? C17 N6 N7 105.9(7) . . ? C17 N6 Pb1 131.4(6) . . ? N7 N6 Pb1 122.4(5) . . ? C19 N7 N6 109.0(7) . . ? C19 N7 B1 128.9(7) . . ? N6 N7 B1 122.1(7) . . ? N6 Pb1 N4 73.5(2) . . ? N6 Pb1 N2 77.4(2) . . ? N4 Pb1 N2 75.1(2) . . ? N6 Pb1 N1 84.2(2) . . ? N4 Pb1 N1 81.9(2) . . ? N2 Pb1 N1 153.8(2) . . ? C2 Pt1 C2 180 . . ? C2 Pt1 C1 90.0(3) . . ? C2 Pt1 C1 90.0(3) 2_756 . ? C2 Pt1 C1 90.0(3) . 2_756 ? C2 Pt1 C1 90.0(3) 2_756 2_756 ? C1 Pt1 C1 180 . . ? O1 C21 C20 137.1(15) . . ? O1 C21 C22 112.9(13) . . ? C20 C21 C22 109.0(13) . . ? C21 C20 H20A 109.5 . . ? C21 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C21 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? #===END