# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 893216' #TrackingRef 'c1CC_Mercier.cif' _audit_creation_date 2012-07-06T18:24:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H8 Cl2 N2 O Pb' _chemical_formula_weight 450.29 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 16.459(1) _cell_length_b 4.1097(5) _cell_length_c 18.072(1) _cell_angle_alpha 90 _cell_angle_beta 93.72(1) _cell_angle_gamma 90 _cell_volume 1219.84(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.305 _exptl_absorpt_correction_T_max 0.475 _exptl_absorpt_process_details '(SADABS (Sheldrick, Bruker, 2000))' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_unetI/netI 0.0714 _diffrn_reflns_number 6612 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 29.53 _diffrn_reflns_theta_full 29.53 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 3161 _reflns_number_gt 2537 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0000P)^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_number_reflns 3161 _refine_ls_number_parameters 147 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.052(15) _refine_diff_density_max 1.067 _refine_diff_density_min -1.002 _refine_diff_density_rms 0.172 #----------------------------------------------------------------------------# # 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 0.003 0.002 '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' Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.394 10.111 '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 Cl1 Cl 0.03899(18) 0.7565(9) 0.60896(14) 0.0577(7) Uani 1 1 d . . . Cl2 Cl -0.58221(16) 0.9554(8) 0.91164(13) 0.0509(6) Uani 1 1 d . . . C6 C -0.2914(5) 0.786(3) 0.7890(5) 0.036(2) Uani 1 1 d . . . O1 O -0.1389(3) 1.282(2) 0.5465(4) 0.0517(18) Uani 1 1 d . . . C3 C -0.2471(5) 0.900(2) 0.7253(5) 0.033(2) Uani 1 1 d . . . C1 C -0.2398(5) 0.968(3) 0.5931(5) 0.042(2) Uani 1 1 d . . . H1 H -0.2621 0.9306 0.5453 0.05 Uiso 1 1 calc R . . C10 C -0.2669(6) 0.865(3) 0.8620(5) 0.043(2) Uani 1 1 d . . . H10 H -0.219 0.9797 0.8736 0.052 Uiso 1 1 calc R . . C4 C -0.1748(6) 1.068(3) 0.7342(5) 0.046(3) Uani 1 1 d . . . H4 H -0.1507 1.1007 0.7816 0.055 Uiso 1 1 calc R . . C9 C -0.3170(6) 0.766(3) 0.9172(5) 0.047(2) Uani 1 1 d . . . H9 H -0.3002 0.8185 0.9659 0.057 Uiso 1 1 calc R . . N1 N -0.1710(5) 1.141(2) 0.6044(4) 0.0382(19) Uani 1 1 d . . . C2 C -0.2771(6) 0.845(3) 0.6536(5) 0.043(2) Uani 1 1 d . . . H2 H -0.3242 0.7215 0.6454 0.052 Uiso 1 1 calc R . . C8 C -0.4069(7) 0.525(4) 0.8367(5) 0.057(3) Uani 1 1 d . . . H8 H -0.4543 0.4045 0.8273 0.068 Uiso 1 1 calc R . . C7 C -0.3633(7) 0.610(3) 0.7779(6) 0.051(3) Uani 1 1 d . . . H7 H -0.3817 0.5485 0.7302 0.061 Uiso 1 1 calc R . . C5 C -0.1379(6) 1.187(3) 0.6739(6) 0.050(3) Uani 1 1 d . . . H5 H -0.0893 1.3018 0.6811 0.06 Uiso 1 1 calc R . . N2 N -0.3856(5) 0.606(2) 0.9068(5) 0.055(2) Uani 1 1 d . . . Pb1 Pb -0.5 0.49756(12) 1 0.03327(16) Uani 1 2 d S . . Pb2 Pb 0 1.24349(9) 0.5 0.03322(16) Uani 1 2 d S . . 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 Cl1 0.0772(17) 0.0369(14) 0.0557(14) 0.0003(14) -0.0201(13) -0.0045(19) Cl2 0.0564(14) 0.0415(17) 0.0525(14) 0.0026(12) -0.0149(12) 0.0044(15) C6 0.023(4) 0.045(6) 0.040(5) -0.006(5) 0.000(4) 0.007(5) O1 0.031(3) 0.074(5) 0.051(4) 0.011(4) 0.008(3) 0.003(4) C3 0.027(4) 0.029(5) 0.044(5) -0.001(4) 0.003(5) 0.007(4) C1 0.045(5) 0.052(6) 0.028(4) 0.001(5) 0.001(4) 0.010(6) C10 0.036(5) 0.051(7) 0.043(6) 0.001(4) 0.003(4) 0.003(5) C4 0.034(5) 0.070(10) 0.034(5) 0.000(5) 0.002(4) 0.000(5) C9 0.047(6) 0.052(7) 0.043(5) 0.002(6) -0.002(4) 0.008(7) N1 0.031(4) 0.046(5) 0.037(4) 0.000(4) -0.001(3) 0.005(4) C2 0.038(5) 0.047(6) 0.046(5) -0.002(4) 0.005(4) -0.009(5) C8 0.058(7) 0.066(8) 0.046(5) -0.008(6) 0.004(5) -0.020(8) C7 0.065(7) 0.055(7) 0.032(6) -0.010(5) 0.003(5) -0.007(6) C5 0.032(5) 0.071(9) 0.048(6) -0.007(6) 0.005(4) -0.008(6) N2 0.050(5) 0.058(6) 0.060(6) 0.001(4) 0.020(5) -0.003(5) Pb1 0.0373(3) 0.0252(4) 0.0374(3) 0 0.0029(3) 0 Pb2 0.0342(3) 0.0267(4) 0.0390(4) 0 0.0043(3) 0 #----------------------------------------------------------------------------# # 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 Cl1 Pb2 2.851(3) . ? Cl1 Pb2 2.928(3) 1_545 ? Cl2 Pb1 2.764(3) . ? Cl2 Pb1 3.011(3) 1_565 ? C6 C7 1.391(14) . ? C6 C10 1.394(12) . ? C6 C3 1.478(14) . ? O1 N1 1.333(10) . ? O1 Pb2 2.492(6) . ? C3 C2 1.375(11) . ? C3 C4 1.376(13) . ? C1 N1 1.343(12) . ? C1 C2 1.382(12) . ? C10 C9 1.396(13) . ? C4 C5 1.372(13) . ? C9 N2 1.310(13) . ? N1 C5 1.349(11) . ? C8 N2 1.334(12) . ? C8 C7 1.365(14) . ? N2 Pb1 2.643(8) . ? Pb1 N2 2.643(8) 2_457 ? Pb1 Cl2 2.764(3) 2_457 ? Pb1 Cl2 3.011(3) 1_545 ? Pb1 Cl2 3.011(3) 2_447 ? Pb2 O1 2.492(6) 2_556 ? Pb2 Cl1 2.851(3) 2_556 ? Pb2 Cl1 2.928(3) 1_565 ? Pb2 Cl1 2.928(3) 2_566 ? 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 Pb2 Cl1 Pb2 90.65(7) . 1_545 ? Pb1 Cl2 Pb1 90.63(6) . 1_565 ? C7 C6 C10 116.7(9) . . ? C7 C6 C3 120.7(9) . . ? C10 C6 C3 122.5(10) . . ? N1 O1 Pb2 131.0(6) . . ? C2 C3 C4 116.6(9) . . ? C2 C3 C6 121.1(9) . . ? C4 C3 C6 122.3(8) . . ? N1 C1 C2 119.2(8) . . ? C6 C10 C9 117.4(10) . . ? C5 C4 C3 120.7(9) . . ? N2 C9 C10 126.0(10) . . ? O1 N1 C1 118.9(8) . . ? O1 N1 C5 120.9(9) . . ? C1 N1 C5 120.1(9) . . ? C3 C2 C1 122.2(9) . . ? N2 C8 C7 123.9(11) . . ? C8 C7 C6 120.4(9) . . ? N1 C5 C4 121.0(10) . . ? C9 N2 C8 115.6(10) . . ? C9 N2 Pb1 129.5(7) . . ? C8 N2 Pb1 114.2(7) . . ? N2 Pb1 N2 160.6(4) 2_457 . ? N2 Pb1 Cl2 81.9(2) 2_457 2_457 ? N2 Pb1 Cl2 84.9(2) . 2_457 ? N2 Pb1 Cl2 84.9(2) 2_457 . ? N2 Pb1 Cl2 81.9(2) . . ? Cl2 Pb1 Cl2 94.21(12) 2_457 . ? N2 Pb1 Cl2 98.5(2) 2_457 1_545 ? N2 Pb1 Cl2 95.8(2) . 1_545 ? Cl2 Pb1 Cl2 175.16(9) 2_457 1_545 ? Cl2 Pb1 Cl2 90.63(6) . 1_545 ? N2 Pb1 Cl2 95.8(2) 2_457 2_447 ? N2 Pb1 Cl2 98.5(2) . 2_447 ? Cl2 Pb1 Cl2 90.63(6) 2_457 2_447 ? Cl2 Pb1 Cl2 175.16(10) . 2_447 ? Cl2 Pb1 Cl2 84.53(10) 1_545 2_447 ? O1 Pb2 O1 172.8(4) 2_556 . ? O1 Pb2 Cl1 88.94(19) 2_556 2_556 ? O1 Pb2 Cl1 96.1(2) . 2_556 ? O1 Pb2 Cl1 96.1(2) 2_556 . ? O1 Pb2 Cl1 88.94(19) . . ? Cl1 Pb2 Cl1 90.85(12) 2_556 . ? O1 Pb2 Cl1 90.90(19) 2_556 1_565 ? O1 Pb2 Cl1 83.9(2) . 1_565 ? Cl1 Pb2 Cl1 178.50(10) 2_556 1_565 ? Cl1 Pb2 Cl1 90.65(7) . 1_565 ? O1 Pb2 Cl1 83.9(2) 2_556 2_566 ? O1 Pb2 Cl1 90.90(19) . 2_566 ? Cl1 Pb2 Cl1 90.65(7) 2_556 2_566 ? Cl1 Pb2 Cl1 178.50(10) . 2_566 ? Cl1 Pb2 Cl1 87.86(12) 1_565 2_566 ? data_2 _database_code_depnum_ccdc_archive 'CCDC 893217' #TrackingRef 'c2CC_Mercier.cif' _audit_creation_date 2012-07-06T18:24:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C20 H18 Cl2 N6 O8 Pb' _chemical_formula_weight 748.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.847(1) _cell_length_b 4.0866(5) _cell_length_c 35.249(3) _cell_angle_alpha 90 _cell_angle_beta 97.55(1) _cell_angle_gamma 90 _cell_volume 2406.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 0.528 _exptl_absorpt_process_details '(SADABS (Sheldrick, Bruker, 2000))' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_av_unetI/netI 0.091 _diffrn_reflns_number 13502 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 30.06 _diffrn_reflns_theta_full 30.06 _diffrn_measured_fraction_theta_full 0.958 _diffrn_measured_fraction_theta_max 0.958 _reflns_number_total 3392 _reflns_number_gt 2294 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0232P)^2^+2.7105P] 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_number_reflns 3392 _refine_ls_number_parameters 168 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0856 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.283 _refine_diff_density_min -1.883 _refine_diff_density_rms 0.17 #----------------------------------------------------------------------------# # 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 0.003 0.002 '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' Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.394 10.111 '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 Pb1 Pb 0 0.35781(6) 0.25 0.03215(10) Uani 1 2 d S . . Cl1 Cl -0.02418(9) -0.1474(3) 0.30482(4) 0.0544(3) Uani 1 1 d . . . N1 N 0.1879(2) 0.2480(9) 0.30250(10) 0.0363(9) Uani 1 1 d . . . O1 O 0.14759(19) 0.4107(9) 0.27371(9) 0.0501(9) Uani 1 1 d . . . C6 C 0.3238(3) -0.2429(12) 0.39568(13) 0.0392(12) Uani 1 1 d . . . C5 C 0.2554(3) 0.0885(13) 0.29745(13) 0.0432(13) Uani 1 1 d . . . H5 H 0.2718 0.0829 0.2733 0.052 Uiso 1 1 calc R . . C2 C 0.2050(3) 0.0847(11) 0.36728(12) 0.0352(11) Uani 1 1 d . . . H2 H 0.1858 0.0807 0.3909 0.042 Uiso 1 1 calc R . . C1 C 0.1624(3) 0.2465(12) 0.33725(13) 0.0397(12) Uani 1 1 d . . . H1 H 0.1156 0.3562 0.3408 0.048 Uiso 1 1 calc R . . C3 C 0.2764(3) -0.0738(11) 0.36314(12) 0.0324(11) Uani 1 1 d . . . C4 C 0.3000(3) -0.0640(12) 0.32694(13) 0.0411(12) Uani 1 1 d . . . H4 H 0.3477 -0.1647 0.3228 0.049 Uiso 1 1 calc R . . C10 C 0.3990(3) -0.3713(15) 0.39303(16) 0.0596(15) Uani 1 1 d . . . H10 H 0.422 -0.3435 0.3707 0.072 Uiso 1 1 calc R . . N2 N 0.4073(4) -0.5774(12) 0.45529(17) 0.0728(16) Uani 1 1 d . . . H2A H 0.4329 -0.6847 0.474 0.087 Uiso 1 1 calc R . . C9 C 0.4402(4) -0.5421(16) 0.4238(2) 0.0736(19) Uani 1 1 d . . . H9 H 0.4905 -0.6301 0.422 0.088 Uiso 1 1 calc R . . C7 C 0.2942(3) -0.2877(15) 0.43032(15) 0.0575(16) Uani 1 1 d . . . H7 H 0.2445 -0.2016 0.4337 0.069 Uiso 1 1 calc R . . C8 C 0.3369(4) -0.4553(17) 0.45928(18) 0.0722(19) Uani 1 1 d . . . H8 H 0.3161 -0.4839 0.4822 0.087 Uiso 1 1 calc R . . N3 N 0.3962(3) 0.0962(12) 0.54878(12) 0.0507(11) Uani 1 1 d . . . O2 O 0.4092(2) -0.0137(12) 0.58154(11) 0.0770(14) Uani 1 1 d . . . O3 O 0.4448(2) 0.0455(11) 0.52520(10) 0.0634(11) Uani 1 1 d . . . O4 O 0.3360(3) 0.2594(13) 0.53909(13) 0.0928(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 Pb1 0.03234(15) 0.02868(15) 0.03515(14) 0 0.00342(10) 0 Cl1 0.0737(9) 0.0450(8) 0.0491(7) -0.0046(7) 0.0258(6) -0.0039(7) N1 0.030(2) 0.042(2) 0.037(2) 0.0006(17) 0.0042(18) -0.0068(17) O1 0.040(2) 0.070(3) 0.0381(17) 0.0183(18) -0.0004(15) -0.0002(19) C6 0.036(3) 0.034(3) 0.045(3) -0.002(2) -0.003(2) -0.003(2) C5 0.042(3) 0.054(3) 0.038(3) -0.005(3) 0.019(2) 0.004(3) C2 0.033(3) 0.040(3) 0.034(2) -0.001(2) 0.009(2) 0.004(2) C1 0.033(3) 0.050(3) 0.038(3) -0.002(2) 0.011(2) 0.002(2) C3 0.030(2) 0.029(3) 0.038(2) -0.0048(19) 0.005(2) -0.0041(19) C4 0.036(3) 0.044(3) 0.046(3) -0.003(2) 0.015(2) 0.001(2) C10 0.049(3) 0.065(4) 0.062(3) -0.016(3) -0.003(3) 0.016(3) N2 0.079(4) 0.052(3) 0.075(4) 0.006(3) -0.034(3) -0.002(3) C9 0.056(4) 0.061(4) 0.093(5) -0.019(4) -0.031(4) 0.019(3) C7 0.047(3) 0.070(4) 0.055(3) 0.023(3) 0.002(3) 0.004(3) C8 0.066(4) 0.074(5) 0.070(4) 0.029(4) -0.015(3) -0.007(4) N3 0.041(3) 0.062(3) 0.050(3) 0.007(2) 0.010(2) 0.013(2) O2 0.070(3) 0.117(4) 0.049(2) 0.022(2) 0.022(2) 0.046(3) O3 0.052(2) 0.096(3) 0.046(2) 0.009(2) 0.0214(18) 0.027(2) O4 0.068(3) 0.139(4) 0.077(3) 0.051(3) 0.032(2) 0.060(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 Pb1 O1 2.526(3) . ? Pb1 O1 2.526(3) 2 ? Pb1 Cl1 2.8628(13) 1_565 ? Pb1 Cl1 2.8628(13) 2_565 ? Pb1 Cl1 2.8930(13) 2 ? Pb1 Cl1 2.8930(13) . ? Cl1 Pb1 2.8628(13) 1_545 ? N1 O1 1.324(5) . ? N1 C5 1.344(6) . ? N1 C1 1.350(6) . ? C6 C10 1.386(7) . ? C6 C7 1.391(7) . ? C6 C3 1.480(6) . ? C5 C4 1.352(7) . ? C2 C1 1.369(7) . ? C2 C3 1.391(6) . ? C3 C4 1.386(6) . ? C10 C9 1.395(8) . ? N2 C8 1.311(8) . ? N2 C9 1.314(8) . ? C7 C8 1.355(8) . ? N3 O4 1.224(5) . ? N3 O2 1.232(5) . ? N3 O3 1.258(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O1 170.18(17) . 2 ? O1 Pb1 Cl1 86.41(9) . 1_565 ? O1 Pb1 Cl1 86.65(8) 2 1_565 ? O1 Pb1 Cl1 86.65(8) . 2_565 ? O1 Pb1 Cl1 86.41(9) 2 2_565 ? Cl1 Pb1 Cl1 90.13(5) 1_565 2_565 ? O1 Pb1 Cl1 93.62(9) . 2 ? O1 Pb1 Cl1 93.38(8) 2 2 ? Cl1 Pb1 Cl1 179.40(4) 1_565 2 ? Cl1 Pb1 Cl1 90.47(3) 2_565 2 ? O1 Pb1 Cl1 93.38(8) . . ? O1 Pb1 Cl1 93.62(9) 2 . ? Cl1 Pb1 Cl1 90.47(3) 1_565 . ? Cl1 Pb1 Cl1 179.40(4) 2_565 . ? Cl1 Pb1 Cl1 88.93(5) 2 . ? Pb1 Cl1 Pb1 90.47(3) 1_545 . ? O1 N1 C5 120.0(4) . . ? O1 N1 C1 120.4(4) . . ? C5 N1 C1 119.6(4) . . ? N1 O1 Pb1 126.4(3) . . ? C10 C6 C7 116.5(5) . . ? C10 C6 C3 122.0(5) . . ? C7 C6 C3 121.5(4) . . ? N1 C5 C4 121.1(4) . . ? C1 C2 C3 121.1(4) . . ? N1 C1 C2 120.5(4) . . ? C4 C3 C2 116.1(4) . . ? C4 C3 C6 122.4(4) . . ? C2 C3 C6 121.5(4) . . ? C5 C4 C3 121.5(4) . . ? C6 C10 C9 120.3(6) . . ? C8 N2 C9 122.5(6) . . ? N2 C9 C10 119.3(6) . . ? C8 C7 C6 120.8(6) . . ? N2 C8 C7 120.7(6) . . ? O4 N3 O2 120.0(4) . . ? O4 N3 O3 119.5(4) . . ? O2 N3 O3 120.5(4) . . ?