Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'David Billing' _publ_contact_author_address ; School of Chemistry University of the Witwatersrand Molecular Sciences Institute Johannesburg 2050 SOUTH AFRICA ; _publ_contact_author_email DAVE@CHEM.WITS.AC.ZA _publ_section_title ; Synthesis and crystal structures of inorganic-organic hybrids incorporating an aromatic amine with a chiral functional group ; _publ_requested_category FM loop_ _publ_author_name 'David Billing' 'Andreas Lemmerer' data_1 _database_code_depnum_ccdc_archive 'CCDC 607734' _audit_creation_date 2006-04-04T08:39:11-00:00 _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 ; (S-(\b)-phenethylammonium)trichloroplumbate(II) ; _chemical_formula_sum 'C8 H12 Cl3 N Pb' _chemical_formula_moiety 'C8 H12 N, Cl3 Pb' _chemical_formula_weight 435.73 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.6917(15) _cell_length_b 7.7273(15) _cell_length_c 20.524(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1219.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 901 _cell_measurement_theta_min 2.998 _cell_measurement_theta_max 28.279 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 2.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.075 0 0 1 0.075 4 0 1 0.16 0 1 -1 0.2 -4 0 1 0.16 -1 -5 8 0.2 -3 3 -4 0.19 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.446 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.015 _exptl_absorpt_correction_T_max 0.1541 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0755 _diffrn_reflns_av_unetI/netI 0.0574 _diffrn_reflns_number 8272 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2922 _reflns_number_gt 2753 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0236P)^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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0253(6) _refine_ls_number_reflns 2922 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0619 _refine_ls_wR_factor_gt 0.0609 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1208 Friedel pairs' _refine_ls_abs_structure_Flack -0.011(7) _refine_diff_density_max 1.977 _refine_diff_density_min -0.41 _refine_diff_density_rms 0.242 #----------------------------------------------------------------------------# # 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' 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' Pb Pb -3.3944 10.1111 '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 0.9563(8) 0.5687(7) 0.4516(3) 0.0360(11) Uani 1 1 d . . . C2 C 1.0897(10) 0.5883(10) 0.4958(4) 0.0578(19) Uani 1 1 d . . . H2 H 1.1757 0.6702 0.4879 0.069 Uiso 1 1 calc R . . C3 C 1.0982(12) 0.4889(12) 0.5517(4) 0.070(2) Uani 1 1 d . . . H3 H 1.192 0.5003 0.5799 0.084 Uiso 1 1 calc R . . C4 C 0.9670(11) 0.3725(9) 0.5655(3) 0.0526(18) Uani 1 1 d . . . H4 H 0.9704 0.3062 0.6033 0.063 Uiso 1 1 calc R . . C5 C 0.8317(11) 0.3563(11) 0.5225(4) 0.061(2) Uani 1 1 d . . . H5 H 0.7421 0.2793 0.5318 0.073 Uiso 1 1 calc R . . C6 C 0.8255(10) 0.4523(9) 0.4654(4) 0.0536(17) Uani 1 1 d . . . H6 H 0.7333 0.4382 0.4366 0.064 Uiso 1 1 calc R . . C7 C 0.9486(8) 0.6710(7) 0.3882(3) 0.0379(12) Uani 1 1 d . . . H7 H 0.8263 0.6916 0.3773 0.045 Uiso 1 1 calc R . . C8 C 1.0415(11) 0.8413(7) 0.3886(4) 0.0529(17) Uani 1 1 d . . . H8A H 1.0268 0.897 0.3472 0.079 Uiso 1 1 calc R . . H8B H 1.1631 0.8226 0.3966 0.079 Uiso 1 1 calc R . . H8C H 0.9942 0.9134 0.4223 0.079 Uiso 1 1 calc R . . N1 N 1.0279(7) 0.5598(5) 0.3354(2) 0.0371(10) Uani 1 1 d . . . H1A H 0.973 0.4585 0.334 0.056 Uiso 1 1 calc R . . H1B H 1.1399 0.5425 0.3441 0.056 Uiso 1 1 calc R . . H1C H 1.0173 0.613 0.2972 0.056 Uiso 1 1 calc R . . Cl1 Cl 0.4572(2) 0.59145(17) 0.35095(6) 0.0376(3) Uani 1 1 d . . . Cl3 Cl 0.75396(19) 0.23658(17) 0.29542(7) 0.0356(3) Uani 1 1 d . . . Cl2 Cl 0.76506(18) 0.72196(17) 0.22471(8) 0.0389(3) Uani 1 1 d . . . Pb1 Pb 0.51006(3) 0.43844(2) 0.234956(10) 0.03286(9) 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 C1 0.032(3) 0.042(3) 0.034(2) -0.007(2) 0.003(2) 0.008(3) C2 0.048(4) 0.071(5) 0.054(4) 0.005(4) -0.004(3) -0.019(4) C3 0.063(5) 0.102(6) 0.045(4) 0.000(4) -0.018(4) -0.005(5) C4 0.068(5) 0.059(4) 0.031(3) 0.004(3) 0.003(3) -0.003(4) C5 0.058(5) 0.070(5) 0.054(4) 0.011(4) 0.003(3) -0.021(4) C6 0.051(4) 0.062(4) 0.047(3) 0.006(3) -0.011(3) -0.013(4) C7 0.027(3) 0.041(3) 0.046(3) -0.006(3) -0.001(2) 0.004(3) C8 0.063(5) 0.030(3) 0.066(4) 0.000(3) 0.009(3) -0.004(3) N1 0.038(3) 0.036(2) 0.037(2) 0.0017(18) 0.0033(19) -0.007(3) Cl1 0.0350(7) 0.0395(6) 0.0383(6) -0.0016(5) -0.0021(5) 0.0009(6) Cl3 0.0293(7) 0.0361(6) 0.0414(6) -0.0023(6) -0.0032(5) 0.0022(6) Cl2 0.0273(7) 0.0343(6) 0.0550(9) 0.0077(6) 0.0023(6) 0.0011(6) Pb1 0.02937(13) 0.02897(11) 0.04023(12) 0.00042(8) -0.00036(10) 0.00028(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 C1 C2 1.378(9) . ? C1 C6 1.379(9) . ? C1 C7 1.522(8) . ? C2 C3 1.382(11) . ? C2 H2 0.93 . ? C3 C4 1.381(11) . ? C3 H3 0.93 . ? C4 C5 1.370(11) . ? C4 H4 0.93 . ? C5 C6 1.388(11) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.498(9) . ? C7 N1 1.511(7) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? Cl1 Pb1 2.6891(14) . ? Cl1 Pb1 3.2189(14) 4_655 ? Cl3 Pb1 2.7372(14) . ? Cl3 Pb1 3.1338(15) 4_645 ? Cl2 Pb1 2.8216(14) 4_655 ? Cl2 Pb1 2.9480(14) . ? Pb1 Cl2 2.8216(15) 4_645 ? Pb1 Cl3 3.1338(15) 4_655 ? Pb1 Cl1 3.2189(14) 4_645 ? 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 C2 C1 C6 118.6(6) . . ? C2 C1 C7 122.3(6) . . ? C6 C1 C7 119.1(5) . . ? C1 C2 C3 121.4(7) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 119.8(7) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 118.9(6) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.4(7) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C1 C6 C5 119.8(7) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C8 C7 N1 108.1(5) . . ? C8 C7 C1 115.7(5) . . ? N1 C7 C1 107.5(4) . . ? C8 C7 H7 108.4 . . ? N1 C7 H7 108.4 . . ? C1 C7 H7 108.4 . . ? 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 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 Cl1 Pb1 82.50(4) . 4_655 ? Pb1 Cl3 Pb1 83.37(4) . 4_645 ? Pb1 Cl2 Pb1 85.45(4) 4_655 . ? Cl1 Pb1 Cl3 87.30(4) . . ? Cl1 Pb1 Cl2 83.54(4) . 4_645 ? Cl3 Pb1 Cl2 92.47(5) . 4_645 ? Cl1 Pb1 Cl2 80.62(4) . . ? Cl3 Pb1 Cl2 89.99(4) . . ? Cl2 Pb1 Cl2 163.84(3) 4_645 . ? Cl1 Pb1 Cl3 75.81(4) . 4_655 ? Cl3 Pb1 Cl3 162.42(3) . 4_655 ? Cl2 Pb1 Cl3 90.47(4) 4_645 4_655 ? Cl2 Pb1 Cl3 82.57(4) . 4_655 ? Cl1 Pb1 Cl1 149.66(4) . 4_645 ? Cl3 Pb1 Cl1 73.74(4) . 4_645 ? Cl2 Pb1 Cl1 74.07(4) 4_645 4_645 ? Cl2 Pb1 Cl1 121.86(4) . 4_645 ? Cl3 Pb1 Cl1 123.65(4) 4_655 4_645 ? 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 C6 C1 C2 C3 2.9(11) . . . . ? C7 C1 C2 C3 -177.2(7) . . . . ? C1 C2 C3 C4 -3.0(13) . . . . ? C2 C3 C4 C5 1.0(13) . . . . ? C3 C4 C5 C6 0.9(13) . . . . ? C2 C1 C6 C5 -1.0(11) . . . . ? C7 C1 C6 C5 179.1(7) . . . . ? C4 C5 C6 C1 -0.9(13) . . . . ? C2 C1 C7 C8 -25.7(9) . . . . ? C6 C1 C7 C8 154.3(6) . . . . ? C2 C1 C7 N1 95.3(7) . . . . ? C6 C1 C7 N1 -84.8(7) . . . . ? Pb1 Cl1 Pb1 Cl3 132.04(4) 4_655 . . . ? Pb1 Cl1 Pb1 Cl2 -135.16(4) 4_655 . . 4_645 ? Pb1 Cl1 Pb1 Cl2 41.60(3) 4_655 . . . ? Pb1 Cl1 Pb1 Cl3 -43.03(3) 4_655 . . 4_655 ? Pb1 Cl1 Pb1 Cl1 -177.41(3) 4_655 . . 4_645 ? Pb1 Cl3 Pb1 Cl1 113.52(4) 4_645 . . . ? Pb1 Cl3 Pb1 Cl2 30.11(5) 4_645 . . 4_645 ? Pb1 Cl3 Pb1 Cl2 -165.87(4) 4_645 . . . ? Pb1 Cl3 Pb1 Cl3 129.52(10) 4_645 . . 4_655 ? Pb1 Cl3 Pb1 Cl1 -42.51(3) 4_645 . . 4_645 ? Pb1 Cl2 Pb1 Cl1 -48.88(4) 4_655 . . . ? Pb1 Cl2 Pb1 Cl3 -136.14(5) 4_655 . . . ? Pb1 Cl2 Pb1 Cl2 -37.26(10) 4_655 . . 4_645 ? Pb1 Cl2 Pb1 Cl3 27.88(4) 4_655 . . 4_655 ? Pb1 Cl2 Pb1 Cl1 153.11(3) 4_655 . . 4_645 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Cl3 0.89 2.53 3.369(5) 157.2 . N1 H1B Cl1 0.89 2.47 3.327(5) 160.7 1_655 N1 H1C Cl2 0.89 2.59 3.289(5) 136.6 . N1 H1C Cl3 0.89 2.76 3.449(5) 135.1 4_755 _chemical_name_common (S-(beta)-phenethylammonium)trichloroplumbate(ii) ###END data_2 _database_code_depnum_ccdc_archive 'CCDC 607735' _audit_creation_date 2006-06-21T16:05:48-00:00 _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 ; (S-(\b)-phenethylammonium)tribromoplumbate(II) ; _chemical_formula_moiety 'C8 H12 N, Br3 Pb' _chemical_formula_sum 'C8 H12 Br3 N Pb' _chemical_formula_weight 569.11 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.9199(11) _cell_length_b 8.1392(11) _cell_length_c 20.555(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1325.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 3.724 _cell_measurement_theta_max 28.211 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.13 -1 0 0 0.13 0 -1 0 0.22 0 0 1 0.035 0 0 -1 0.035 3 4 1 0.15 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 21.741 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_absorpt_correction_T_min 0.0064 _exptl_absorpt_correction_T_max 0.2226 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_number 9027 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 3157 _reflns_number_gt 2683 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0231P)^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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0056(2) _refine_ls_number_reflns 3157 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0648 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1306 Friedel pairs' _refine_ls_abs_structure_Flack -0.010(11) _refine_diff_density_max 0.991 _refine_diff_density_min -0.866 _refine_diff_density_rms 0.158 #----------------------------------------------------------------------------# # 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' 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' Pb Pb -3.3944 10.1111 '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 0.8251(6) 0.2924(6) 0.7038(2) 0.0392(18) Uani 1 1 d G . . C2 C 0.7234(8) 0.4252(5) 0.7202(3) 0.055(2) Uani 1 1 d G . . H2 H 0.7259 0.5203 0.6951 0.066 Uiso 1 1 calc R . . C3 C 0.6179(7) 0.4161(6) 0.7741(3) 0.063(3) Uani 1 1 d G . . H3 H 0.5498 0.505 0.7851 0.076 Uiso 1 1 calc R . . C4 C 0.6141(8) 0.2740(7) 0.8116(3) 0.060(2) Uani 1 1 d G . . H4 H 0.5435 0.2679 0.8477 0.072 Uiso 1 1 calc R . . C5 C 0.7158(8) 0.1412(6) 0.7952(3) 0.061(3) Uani 1 1 d G . . H5 H 0.7132 0.0461 0.8203 0.073 Uiso 1 1 calc R . . C6 C 0.8213(7) 0.1503(5) 0.7413(3) 0.053(2) Uani 1 1 d G . . H6 H 0.8894 0.0614 0.7304 0.064 Uiso 1 1 calc R . . C7 C 0.9314(10) 0.3043(9) 0.6432(4) 0.0406(18) Uani 1 1 d . . . H7 H 0.9449 0.4206 0.6321 0.049 Uiso 1 1 calc R . . C8 C 1.1042(11) 0.2273(12) 0.6472(6) 0.072(3) Uani 1 1 d . . . H8A H 1.1635 0.2455 0.6071 0.108 Uiso 1 1 calc R . . H8B H 1.093 0.1114 0.6546 0.108 Uiso 1 1 calc R . . H8C H 1.1661 0.2761 0.6824 0.108 Uiso 1 1 calc R . . N1 N 0.8355(8) 0.2200(7) 0.5877(3) 0.0427(15) Uani 1 1 d . . . H1A H 0.8973 0.2235 0.5516 0.064 Uiso 1 1 calc R . . H1B H 0.738 0.2718 0.5811 0.064 Uiso 1 1 calc R . . H1C H 0.8154 0.1158 0.5984 0.064 Uiso 1 1 calc R . . Br1 Br -0.12360(10) 0.79235(8) 0.60923(4) 0.0410(2) Uani 1 1 d . . . Br2 Br 0.48589(9) 1.01752(8) 0.53062(4) 0.0405(2) Uani 1 1 d . . . Br3 Br 0.50366(9) 0.49321(9) 0.54897(4) 0.03804(19) Uani 1 1 d . . . Pb1 Pb 0.20981(3) 0.75675(4) 0.512285(15) 0.03671(10) 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 C1 0.044(4) 0.040(4) 0.034(4) -0.004(3) 0.002(3) -0.001(3) C2 0.063(6) 0.048(5) 0.054(5) 0.003(4) 0.010(5) -0.002(5) C3 0.070(6) 0.057(5) 0.062(6) -0.001(5) 0.008(6) 0.023(5) C4 0.059(5) 0.079(6) 0.043(4) -0.018(5) 0.002(4) -0.018(6) C5 0.086(7) 0.052(5) 0.045(5) 0.013(4) 0.016(6) 0.007(5) C6 0.058(5) 0.043(4) 0.058(5) 0.001(4) 0.021(5) 0.001(4) C7 0.045(4) 0.035(4) 0.042(4) 0.001(3) 0.004(4) -0.010(3) C8 0.037(4) 0.082(7) 0.096(8) 0.012(7) -0.006(5) -0.007(6) N1 0.040(3) 0.046(4) 0.043(3) 0.003(3) -0.007(3) 0.002(3) Br1 0.0414(4) 0.0384(4) 0.0432(4) 0.0021(3) -0.0009(3) -0.0006(3) Br2 0.0345(4) 0.0297(3) 0.0572(5) -0.0028(4) -0.0081(4) 0.0002(3) Br3 0.0342(4) 0.0330(3) 0.0470(4) 0.0021(3) -0.0022(3) -0.0013(3) Pb1 0.02768(12) 0.03345(15) 0.04900(16) 0.00018(15) 0.00001(12) 0.00016(13) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.507(9) . ? C2 C3 1.39 . ? C2 H2 0.93 . ? C3 C4 1.39 . ? C3 H3 0.93 . ? C4 C5 1.39 . ? C4 H4 0.93 . ? C5 C6 1.39 . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.508(11) . ? C7 N1 1.531(10) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? Br1 Pb1 2.8530(9) 4_466 ? Br1 Pb1 3.3208(9) . ? Br2 Pb1 2.9843(8) 4_566 ? Br2 Pb1 3.0705(8) . ? Br3 Pb1 2.8971(8) 4_566 ? Br3 Pb1 3.2536(8) . ? Pb1 Br1 2.8530(9) 4_566 ? Pb1 Br3 2.8971(8) 4_466 ? Pb1 Br2 2.9843(8) 4_466 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 118.3(4) . . ? C6 C1 C7 121.6(4) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C1 C7 C8 115.8(7) . . ? C1 C7 N1 108.0(6) . . ? C8 C7 N1 107.8(7) . . ? C1 C7 H7 108.4 . . ? C8 C7 H7 108.4 . . ? N1 C7 H7 108.4 . . ? 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 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 Br1 Pb1 80.22(2) 4_466 . ? Pb1 Br2 Pb1 82.52(2) 4_566 . ? Pb1 Br3 Pb1 80.75(2) 4_566 . ? Br1 Pb1 Br3 88.77(2) 4_566 4_466 ? Br1 Pb1 Br2 84.91(2) 4_566 4_466 ? Br3 Pb1 Br2 93.56(2) 4_466 4_466 ? Br1 Pb1 Br2 82.82(2) 4_566 . ? Br3 Pb1 Br2 88.23(2) 4_466 . ? Br2 Pb1 Br2 167.559(18) 4_466 . ? Br1 Pb1 Br3 77.28(2) 4_566 . ? Br3 Pb1 Br3 165.236(19) 4_466 . ? Br2 Pb1 Br3 90.02(2) 4_466 . ? Br2 Pb1 Br3 85.29(2) . . ? Br1 Pb1 Br1 154.87(2) 4_566 . ? Br3 Pb1 Br1 75.61(2) 4_466 . ? Br2 Pb1 Br1 76.71(2) 4_466 . ? Br2 Pb1 Br1 115.61(2) . . ? Br3 Pb1 Br1 119.16(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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 177.1(6) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 -177.0(6) . . . . ? C2 C1 C7 C8 142.6(6) . . . . ? C6 C1 C7 C8 -40.4(9) . . . . ? C2 C1 C7 N1 -96.5(6) . . . . ? C6 C1 C7 N1 80.6(7) . . . . ? Pb1 Br2 Pb1 Br1 -48.28(2) 4_566 . . 4_566 ? Pb1 Br2 Pb1 Br3 -137.26(3) 4_566 . . 4_466 ? Pb1 Br2 Pb1 Br2 -38.74(8) 4_566 . . 4_466 ? Pb1 Br2 Pb1 Br3 29.46(2) 4_566 . . . ? Pb1 Br2 Pb1 Br1 149.63(2) 4_566 . . . ? Pb1 Br3 Pb1 Br1 53.09(2) 4_566 . . 4_566 ? Pb1 Br3 Pb1 Br3 33.67(6) 4_566 . . 4_466 ? Pb1 Br3 Pb1 Br2 137.87(3) 4_566 . . 4_466 ? Pb1 Br3 Pb1 Br2 -30.59(2) 4_566 . . . ? Pb1 Br3 Pb1 Br1 -147.38(2) 4_566 . . . ? Pb1 Br1 Pb1 Br1 -0.970(18) 4_466 . . 4_566 ? Pb1 Br1 Pb1 Br3 52.20(2) 4_466 . . 4_466 ? Pb1 Br1 Pb1 Br2 -45.065(19) 4_466 . . 4_466 ? Pb1 Br1 Pb1 Br2 133.09(2) 4_466 . . . ? Pb1 Br1 Pb1 Br3 -127.52(2) 4_466 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Br2 0.89 2.79 3.450(7) 131.9 4_566 N1 H1A Br3 0.89 2.85 3.562(7) 138.5 4_556 N1 H1B Br3 0.89 2.67 3.533(6) 163.8 . N1 H1B Br2 0.89 3.06 3.430(6) 107.4 1_545 N1 H1C Br1 0.89 2.69 3.524(6) 157.2 1_645 _chemical_name_common (S-(beta)-phenethylammonium)tribromoplumbate(ii) ###END data_3 _database_code_depnum_ccdc_archive 'CCDC 607736' _audit_creation_date 2006-04-04T09:36:49-00:00 _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 ; ((R)-\b-phenethylammonium)triiodoplumbate(II) ; _chemical_formula_sum 'C8 H12 I3 N Pb' _chemical_formula_moiety 'C8 H12 N, I3 Pb' _chemical_formula_weight 710.08 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.0814(12) _cell_length_b 8.6983(13) _cell_length_c 21.337(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1499.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 962 _cell_measurement_theta_min 2.695 _cell_measurement_theta_max 28.007 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 3.145 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.085 0 0 1 0.085 0 2 3 0.24 0 -2 1 0.21 -1 0 -2 0.085 1 0 -1 0.125 -2 -1 3 0.14 -1 0 1 0.135 1 0 1 0.115 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 17.391 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0322 _exptl_absorpt_correction_T_max 0.1071 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1 K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_av_unetI/netI 0.0386 _diffrn_reflns_number 10282 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 3626 _reflns_number_gt 3276 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0263P)^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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0095(2) _refine_ls_number_reflns 3626 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0608 _refine_ls_wR_factor_gt 0.0592 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1526 Friedel Pairs' _refine_ls_abs_structure_Flack -0.009(5) _refine_diff_density_max 1.529 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.329 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' Pb Pb -3.3944 10.1111 '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 0.8219(9) 0.2966(8) 0.6994(3) 0.0408(17) Uani 1 1 d . . . C2 C 0.7480(12) 0.4258(10) 0.7235(4) 0.062(2) Uani 1 1 d . . . H2 H 0.7679 0.5211 0.7052 0.075 Uiso 1 1 calc R . . C3 C 0.6454(12) 0.4147(11) 0.7739(5) 0.066(3) Uani 1 1 d . . . H3 H 0.597 0.5031 0.7902 0.08 Uiso 1 1 calc R . . C4 C 0.6128(11) 0.2765(12) 0.8008(4) 0.070(3) Uani 1 1 d . . . H4 H 0.5383 0.2701 0.8339 0.084 Uiso 1 1 calc R . . C5 C 0.6897(12) 0.1465(11) 0.7792(5) 0.067(3) Uani 1 1 d . . . H5 H 0.6734 0.0527 0.7991 0.081 Uiso 1 1 calc R . . C6 C 0.7902(11) 0.1563(9) 0.7282(4) 0.057(2) Uani 1 1 d . . . H6 H 0.8385 0.0675 0.7122 0.068 Uiso 1 1 calc R . . C7 C 0.9335(10) 0.3110(8) 0.6432(4) 0.0503(19) Uani 1 1 d . . . H7 H 0.9403 0.4196 0.6313 0.06 Uiso 1 1 calc R . . C8 C 1.1072(10) 0.2501(14) 0.6532(5) 0.081(3) Uani 1 1 d . . . H8A H 1.1709 0.2645 0.6157 0.122 Uiso 1 1 calc R . . H8B H 1.1023 0.1425 0.6631 0.122 Uiso 1 1 calc R . . H8C H 1.1584 0.3046 0.6872 0.122 Uiso 1 1 calc R . . N1 N 0.8599(8) 0.2226(8) 0.5902(3) 0.0512(16) Uani 1 1 d . . . H1A H 0.9252 0.2302 0.5568 0.077 Uiso 1 1 calc R . . H1B H 0.7605 0.2607 0.5812 0.077 Uiso 1 1 calc R . . H1C H 0.8501 0.1243 0.6011 0.077 Uiso 1 1 calc R . . I1 I -0.07562(7) 0.79160(5) 0.61663(2) 0.04640(14) Uani 1 1 d . . . I2 I 0.48238(6) 1.02085(5) 0.54018(3) 0.04432(13) Uani 1 1 d . . . I3 I 0.49900(6) 0.49471(5) 0.55739(2) 0.04305(13) Uani 1 1 d . . . Pb1 Pb 0.21656(3) 0.75238(4) 0.505229(13) 0.04041(9) 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 C1 0.046(4) 0.041(4) 0.035(4) -0.003(3) 0.003(3) 0.000(3) C2 0.087(7) 0.044(5) 0.055(6) 0.003(4) 0.004(5) 0.010(4) C3 0.081(6) 0.058(5) 0.060(6) -0.001(5) 0.010(5) 0.020(5) C4 0.066(6) 0.088(7) 0.056(6) -0.001(5) 0.006(4) -0.018(6) C5 0.090(8) 0.054(5) 0.058(6) 0.002(5) 0.006(6) -0.015(5) C6 0.071(6) 0.040(4) 0.060(6) -0.002(4) 0.017(5) 0.002(4) C7 0.059(5) 0.042(4) 0.050(5) 0.002(3) 0.002(4) -0.009(4) C8 0.056(5) 0.108(8) 0.080(7) -0.010(7) 0.001(5) -0.021(7) N1 0.058(4) 0.057(4) 0.038(3) 0.004(3) -0.001(3) -0.001(3) I1 0.0550(3) 0.0411(3) 0.0431(3) 0.0004(2) -0.0010(2) -0.0006(2) I2 0.0428(2) 0.0313(2) 0.0589(3) -0.0048(2) -0.0054(2) 0.00123(19) I3 0.0441(3) 0.0348(2) 0.0502(3) 0.0050(2) -0.0010(2) -0.0018(2) Pb1 0.03221(12) 0.03410(14) 0.05493(18) -0.00069(13) 0.00046(12) -0.00041(12) #----------------------------------------------------------------------------# # 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 C1 C2 1.372(11) . ? C1 C6 1.389(11) . ? C1 C7 1.506(11) . ? C2 C3 1.363(13) . ? C2 H2 0.93 . ? C3 C4 1.357(13) . ? C3 H3 0.93 . ? C4 C5 1.370(13) . ? C4 H4 0.93 . ? C5 C6 1.361(12) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 N1 1.491(10) . ? C7 C8 1.515(13) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1190(7) 4_466 ? I1 Pb1 3.3678(7) . ? I2 Pb1 3.1889(6) 4_566 ? I2 Pb1 3.2595(6) . ? I3 Pb1 3.1170(6) 4_566 ? I3 Pb1 3.3870(6) . ? Pb1 I3 3.1170(6) 4_466 ? Pb1 I1 3.1190(7) 4_566 ? Pb1 I2 3.1889(6) 4_466 ? 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 C2 C1 C6 118.3(7) . . ? C2 C1 C7 119.4(7) . . ? C6 C1 C7 122.3(7) . . ? C3 C2 C1 120.2(9) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.9(9) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 120.1(9) . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? C6 C5 C4 119.2(9) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? C5 C6 C1 121.2(8) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? N1 C7 C1 108.8(6) . . ? N1 C7 C8 107.2(7) . . ? C1 C7 C8 114.4(7) . . ? N1 C7 H7 108.8 . . ? C1 C7 H7 108.8 . . ? C8 C7 H7 108.8 . . ? 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 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I1 Pb1 77.097(16) 4_466 . ? Pb1 I2 Pb1 77.739(15) 4_566 . ? Pb1 I3 Pb1 76.836(14) 4_566 . ? I3 Pb1 I1 91.889(17) 4_466 4_566 ? I3 Pb1 I2 93.497(17) 4_466 4_466 ? I1 Pb1 I2 88.559(16) 4_566 4_466 ? I3 Pb1 I2 87.948(18) 4_466 . ? I1 Pb1 I2 85.627(16) 4_566 . ? I2 Pb1 I2 174.054(14) 4_466 . ? I3 Pb1 I1 80.536(16) 4_466 . ? I1 Pb1 I1 168.062(17) 4_566 . ? I2 Pb1 I1 82.753(16) 4_466 . ? I2 Pb1 I1 103.179(16) . . ? I3 Pb1 I3 171.113(15) 4_466 . ? I1 Pb1 I3 80.206(16) 4_566 . ? I2 Pb1 I3 90.378(17) 4_466 . ? I2 Pb1 I3 87.408(17) . . ? I1 Pb1 I3 107.914(16) . . ? 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 C6 C1 C2 C3 -0.5(14) . . . . ? C7 C1 C2 C3 179.4(8) . . . . ? C1 C2 C3 C4 -0.9(16) . . . . ? C2 C3 C4 C5 3.2(16) . . . . ? C3 C4 C5 C6 -4.2(14) . . . . ? C4 C5 C6 C1 2.9(14) . . . . ? C2 C1 C6 C5 -0.6(13) . . . . ? C7 C1 C6 C5 179.6(8) . . . . ? C2 C1 C7 N1 -116.9(8) . . . . ? C6 C1 C7 N1 62.9(10) . . . . ? C2 C1 C7 C8 123.2(9) . . . . ? C6 C1 C7 C8 -57.0(11) . . . . ? Pb1 I2 Pb1 I3 -137.754(18) 4_566 . . 4_466 ? Pb1 I2 Pb1 I1 -45.701(13) 4_566 . . 4_566 ? Pb1 I2 Pb1 I1 142.464(16) 4_566 . . . ? Pb1 I2 Pb1 I3 34.667(13) 4_566 . . . ? Pb1 I1 Pb1 I3 50.527(13) 4_466 . . 4_466 ? Pb1 I1 Pb1 I1 -0.65(5) 4_466 . . 4_566 ? Pb1 I1 Pb1 I2 -44.265(12) 4_466 . . 4_466 ? Pb1 I1 Pb1 I2 136.149(17) 4_466 . . . ? Pb1 I1 Pb1 I3 -132.310(17) 4_466 . . . ? Pb1 I3 Pb1 I1 50.274(13) 4_566 . . 4_566 ? Pb1 I3 Pb1 I2 138.746(17) 4_566 . . 4_466 ? Pb1 I3 Pb1 I2 -35.732(13) 4_566 . . . ? Pb1 I3 Pb1 I1 -138.749(16) 4_566 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.03 3.702(6) 133.7 4_566 N1 H1A I3 0.89 3.18 3.842(6) 132.8 4_556 N1 H1B I3 0.89 2.98 3.821(7) 158.7 . N1 H1B I2 0.89 3.19 3.678(7) 116.9 1_545 N1 H1C I1 0.89 2.97 3.827(7) 161.1 1_645 _chemical_name_common ((R)-beta-phenethylammonium)triiodoplumbate(ii) ###END data_4 _database_code_depnum_ccdc_archive 'CCDC 607737' _audit_creation_date 2006-04-04T09:46:19-00:00 _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 ; ((R)-\b-phenethylammonium)triiodoplumbate(II) ; _chemical_formula_sum 'C8 H12 I3 N Pb' _chemical_formula_moiety 'C8 H12 N, I3 Pb' _chemical_formula_weight 710.08 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall ' P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.0950(12) _cell_length_b 8.7141(13) _cell_length_c 21.368(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1507.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 945 _cell_measurement_theta_min 2.524 _cell_measurement_theta_max 28.144 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 3.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.03 0 0 1 0.03 0 8 -5 0.11 0 -5 4 0.11 1 0 0 0.1 -1 0 0 0.1 -3 7 -7 0.1 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 17.305 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0609 _exptl_absorpt_correction_T_max 0.3746 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_unetI/netI 0.0465 _diffrn_reflns_number 10283 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 3645 _reflns_number_gt 3085 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0179P)^2^+0.1435P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00402(10) _refine_ls_number_reflns 3645 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), 1538 Friedel Pairs' _refine_ls_abs_structure_Flack -0.008(6) _refine_diff_density_max 0.754 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.138 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' Pb Pb -3.3944 10.1111 '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 0.1766(6) 0.7020(5) 0.3008(2) 0.0417(19) Uani 1 1 d G . . C2 C 0.2497(7) 0.5696(4) 0.2773(3) 0.060(3) Uani 1 1 d G . . H2 H 0.2286 0.4753 0.2961 0.072 Uiso 1 1 calc R . . C3 C 0.3542(7) 0.5780(5) 0.2258(3) 0.062(3) Uani 1 1 d G . . H3 H 0.4031 0.4894 0.2102 0.074 Uiso 1 1 calc R . . C4 C 0.3856(6) 0.7189(7) 0.1978(2) 0.066(3) Uani 1 1 d G . . H4 H 0.4555 0.7246 0.1633 0.079 Uiso 1 1 calc R . . C5 C 0.3125(7) 0.8514(5) 0.2212(3) 0.069(3) Uani 1 1 d G . . H5 H 0.3336 0.9456 0.2024 0.083 Uiso 1 1 calc R . . C6 C 0.2080(7) 0.8429(4) 0.2727(3) 0.054(2) Uani 1 1 d G . . H6 H 0.1591 0.9315 0.2884 0.064 Uiso 1 1 calc R . . C7 C 0.0657(10) 0.6883(8) 0.3568(4) 0.050(2) Uani 1 1 d . . . H7 H 0.0564 0.5801 0.3688 0.06 Uiso 1 1 calc R . . C8 C -0.1093(10) 0.7547(13) 0.3452(5) 0.084(3) Uani 1 1 d . . . H8A H -0.1756 0.7413 0.382 0.126 Uiso 1 1 calc R . . H8B H -0.1598 0.7018 0.3107 0.126 Uiso 1 1 calc R . . H8C H -0.101 0.862 0.3356 0.126 Uiso 1 1 calc R . . N1 N 0.1376(8) 0.7765(8) 0.4096(3) 0.0534(18) Uani 1 1 d . . . H1A H 0.072 0.7687 0.4429 0.08 Uiso 1 1 calc R . . H1B H 0.147 0.8748 0.3988 0.08 Uiso 1 1 calc R . . H1C H 0.2369 0.7391 0.4189 0.08 Uiso 1 1 calc R . . I1 I 1.07548(7) 0.20827(5) 0.38333(3) 0.04607(15) Uani 1 1 d . . . I2 I 0.51751(6) -0.02093(5) 0.45981(3) 0.04417(14) Uani 1 1 d . . . I3 I 0.50077(6) 0.50523(5) 0.44257(3) 0.04291(13) Uani 1 1 d . . . Pb1 Pb 0.78322(3) 0.24760(4) 0.494755(15) 0.04023(9) 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 C1 0.050(5) 0.039(4) 0.036(5) -0.002(3) -0.002(4) -0.007(3) C2 0.085(7) 0.048(5) 0.048(6) 0.000(5) -0.002(5) 0.020(4) C3 0.075(6) 0.052(5) 0.059(7) -0.003(5) 0.007(5) 0.021(4) C4 0.067(6) 0.086(7) 0.045(5) -0.005(5) 0.006(5) 0.001(5) C5 0.104(8) 0.062(6) 0.041(6) 0.010(5) 0.003(6) -0.018(6) C6 0.076(6) 0.045(5) 0.039(5) 0.001(4) 0.011(5) -0.005(4) C7 0.063(5) 0.033(4) 0.053(5) -0.003(4) 0.012(5) -0.016(4) C8 0.048(5) 0.120(8) 0.084(8) 0.000(9) 0.004(5) -0.019(6) N1 0.058(4) 0.054(4) 0.048(4) 0.001(4) 0.003(4) 0.001(3) I1 0.0546(3) 0.0396(3) 0.0440(3) 0.0004(2) -0.0008(3) -0.0007(2) I2 0.0425(3) 0.0306(2) 0.0595(3) -0.0051(2) -0.0059(3) 0.0013(2) I3 0.0434(3) 0.0343(2) 0.0510(3) 0.0048(2) -0.0003(2) -0.0015(2) Pb1 0.03221(12) 0.03331(13) 0.0552(2) -0.00052(16) 0.00011(14) -0.00022(12) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.501(9) . ? C2 C3 1.39 . ? C2 H2 0.93 . ? C3 C4 1.39 . ? C3 H3 0.93 . ? C4 C5 1.39 . ? C4 H4 0.93 . ? C5 C6 1.39 . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 N1 1.484(10) . ? C7 C8 1.550(12) . ? C7 H7 0.98 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1244(7) 4_556 ? I1 Pb1 3.3740(7) . ? I2 Pb1 3.1958(6) 4_456 ? I2 Pb1 3.2649(6) . ? I3 Pb1 3.1223(6) 4_456 ? I3 Pb1 3.3928(6) . ? Pb1 I3 3.1223(6) 4_556 ? Pb1 I1 3.1244(7) 4_456 ? Pb1 I2 3.1958(6) 4_556 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 118.4(4) . . ? C6 C1 C7 121.6(4) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C3 C4 C5 120 . . ? C3 C4 H4 120 . . ? C5 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? N1 C7 C1 109.3(6) . . ? N1 C7 C8 106.7(7) . . ? C1 C7 C8 112.9(7) . . ? N1 C7 H7 109.3 . . ? C1 C7 H7 109.3 . . ? C8 C7 H7 109.3 . . ? 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 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I1 Pb1 77.088(17) 4_556 . ? Pb1 I2 Pb1 77.720(15) 4_456 . ? Pb1 I3 Pb1 76.833(14) 4_456 . ? I3 Pb1 I1 91.880(17) 4_556 4_456 ? I3 Pb1 I2 93.490(17) 4_556 4_556 ? I1 Pb1 I2 88.531(17) 4_456 4_556 ? I3 Pb1 I2 87.934(18) 4_556 . ? I1 Pb1 I2 85.661(16) 4_456 . ? I2 Pb1 I2 174.064(15) 4_556 . ? I3 Pb1 I1 80.531(16) 4_556 . ? I1 Pb1 I1 168.036(18) 4_456 . ? I2 Pb1 I1 82.758(16) 4_556 . ? I2 Pb1 I1 103.165(17) . . ? I3 Pb1 I3 171.106(15) 4_556 . ? I1 Pb1 I3 80.205(16) 4_456 . ? I2 Pb1 I3 90.378(18) 4_556 . ? I2 Pb1 I3 87.428(17) . . ? I1 Pb1 I3 107.929(17) . . ? 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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 -179.4(6) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 179.4(6) . . . . ? C2 C1 C7 N1 117.2(6) . . . . ? C6 C1 C7 N1 -62.2(8) . . . . ? C2 C1 C7 C8 -124.2(6) . . . . ? C6 C1 C7 C8 56.4(8) . . . . ? Pb1 I2 Pb1 I3 137.738(19) 4_456 . . 4_556 ? Pb1 I2 Pb1 I1 45.694(13) 4_456 . . 4_456 ? Pb1 I2 Pb1 I1 -142.487(17) 4_456 . . . ? Pb1 I2 Pb1 I3 -34.670(14) 4_456 . . . ? Pb1 I1 Pb1 I3 -50.535(13) 4_556 . . 4_556 ? Pb1 I1 Pb1 I1 0.66(5) 4_556 . . 4_456 ? Pb1 I1 Pb1 I2 44.249(12) 4_556 . . 4_556 ? Pb1 I1 Pb1 I2 -136.145(17) 4_556 . . . ? Pb1 I1 Pb1 I3 132.293(17) 4_556 . . . ? Pb1 I3 Pb1 I1 -50.287(13) 4_456 . . 4_456 ? Pb1 I3 Pb1 I2 -138.731(19) 4_456 . . 4_556 ? Pb1 I3 Pb1 I2 35.751(14) 4_456 . . . ? Pb1 I3 Pb1 I1 138.760(17) 4_456 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.03 3.700(7) 133.6 4_456 N1 H1A I3 0.89 3.19 3.850(7) 132.2 4_466 N1 H1B I1 0.89 2.98 3.837(7) 161.7 1_465 N1 H1C I3 0.89 3 3.838(7) 158.6 . N1 H1C I2 0.89 3.21 3.705(7) 117.5 1_565 _chemical_name_common ((R)-beta-phenethylammonium)triiodoplumbate(ii) ###END data_5 _database_code_depnum_ccdc_archive 'CCDC 607738' _audit_creation_date 2006-04-04T10:06:59-00:00 _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 ; tris((racemic)-\b-phenethylammonium)pentachloroplumbate(II) ; _chemical_formula_moiety '3(C8 H12 N), Cl5 Pb, H2 O' _chemical_formula_sum 'C24 H38 Cl5 N3 O Pb' _chemical_formula_weight 769.01 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 28.826(5) _cell_length_b 7.8120(13) _cell_length_c 27.055(5) _cell_angle_alpha 90 _cell_angle_beta 92.684(4) _cell_angle_gamma 90 _cell_volume 6086.0(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 966 _cell_measurement_theta_min 2.261 _cell_measurement_theta_max 28.136 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.025 1 0 0 0.025 0 0 -1 0.155 0 0 1 0.155 1 -2 0 0.19 -1 2 1 0.19 -5 6 7 0.18 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.005 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1802 _exptl_absorpt_correction_T_max 0.7339 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0499 _diffrn_reflns_number 20019 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7326 _reflns_number_gt 5436 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0146P)^2^+16.8143P] 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 7326 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0655 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.995 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.119 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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' 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 0.37838(9) 0.8078(3) 0.00867(10) 0.0235(9) Uani 1 1 d G . . C2 C 0.41193(10) 0.8260(3) 0.04691(8) 0.0286(10) Uani 1 1 d G . . H2 H 0.4152 0.7409 0.0719 0.034 Uiso 1 1 calc R . . C3 C 0.44069(9) 0.9689(4) 0.04859(9) 0.0341(11) Uani 1 1 d G . . H3 H 0.4636 0.9815 0.0747 0.041 Uiso 1 1 calc R . . C4 C 0.43590(9) 1.0936(3) 0.01204(11) 0.0361(11) Uani 1 1 d G . . H4 H 0.4556 1.1912 0.0132 0.043 Uiso 1 1 calc R . . C5 C 0.40236(10) 1.0753(3) -0.02620(9) 0.0319(10) Uani 1 1 d G . . H5 H 0.3991 1.1604 -0.0512 0.038 Uiso 1 1 calc R . . C6 C 0.37360(9) 0.9324(4) -0.02789(9) 0.0276(9) Uani 1 1 d G . . H6 H 0.3507 0.9199 -0.054 0.033 Uiso 1 1 calc R . . C7 C 0.34625(15) 0.6567(6) 0.00395(16) 0.0283(10) Uani 1 1 d . . . H7 H 0.3328 0.6553 -0.0308 0.034 Uiso 1 1 calc R . . C8 C 0.36813(18) 0.4850(6) 0.01390(19) 0.0405(11) Uani 1 1 d . . . H8A H 0.3445 0.3953 0.0095 0.061 Uiso 1 1 calc R . . H8B H 0.3813 0.4817 0.0479 0.061 Uiso 1 1 calc R . . H8C H 0.3928 0.4658 -0.0092 0.061 Uiso 1 1 calc R . . C9 C 0.08892(8) 0.9673(4) 0.13801(9) 0.0271(10) Uani 1 1 d G . . C10 C 0.06336(10) 1.1167(3) 0.13048(10) 0.0345(11) Uani 1 1 d G . . H10 H 0.071 1.2162 0.1493 0.041 Uiso 1 1 calc R . . C11 C 0.02657(10) 1.1204(3) 0.09541(11) 0.0390(12) Uani 1 1 d G . . H11 H 0.0091 1.2225 0.0903 0.047 Uiso 1 1 calc R . . C12 C 0.01534(9) 0.9748(4) 0.06786(10) 0.0360(12) Uani 1 1 d G . . H12 H -0.0098 0.9773 0.0439 0.043 Uiso 1 1 calc R . . C13 C 0.04089(10) 0.8254(3) 0.07539(10) 0.0339(11) Uani 1 1 d G . . H13 H 0.0332 0.7259 0.0566 0.041 Uiso 1 1 calc R . . C14 C 0.07769(9) 0.8216(3) 0.11046(10) 0.0312(10) Uani 1 1 d G . . H14 H 0.0952 0.7195 0.1156 0.037 Uiso 1 1 calc R . . C15 C 0.12700(17) 0.9517(7) 0.17796(17) 0.0388(12) Uani 1 1 d . . . H15 H 0.1398 0.833 0.1762 0.047 Uiso 1 1 calc R . . C16 C 0.1112(2) 0.9763(8) 0.22799(17) 0.0604(19) Uani 1 1 d . . . H16A H 0.1376 0.9648 0.2519 0.091 Uiso 1 1 calc R . . H16B H 0.0877 0.8899 0.2349 0.091 Uiso 1 1 calc R . . H16C H 0.0977 1.0908 0.2308 0.091 Uiso 1 1 calc R . . C17 C 0.09486(7) 0.5629(3) 0.32100(10) 0.0222(9) Uani 1 1 d G . . C18 C 0.07339(9) 0.4049(3) 0.31394(10) 0.0296(10) Uani 1 1 d G . . H18 H 0.0916 0.3045 0.311 0.036 Uiso 1 1 calc R . . C19 C 0.02522(10) 0.3938(3) 0.31115(11) 0.0386(12) Uani 1 1 d G . . H19 H 0.0105 0.2859 0.3063 0.046 Uiso 1 1 calc R . . C20 C -0.00149(7) 0.5408(4) 0.31541(11) 0.0408(13) Uani 1 1 d G . . H20 H -0.0344 0.5332 0.3135 0.049 Uiso 1 1 calc R . . C21 C 0.01998(9) 0.6988(3) 0.32247(11) 0.0400(12) Uani 1 1 d G . . H21 H 0.0017 0.7992 0.3254 0.048 Uiso 1 1 calc R . . C22 C 0.06816(10) 0.7099(3) 0.32526(10) 0.0301(10) Uani 1 1 d G . . H22 H 0.0828 0.8179 0.3301 0.036 Uiso 1 1 calc R . . C23 C 0.14684(14) 0.5851(5) 0.32596(14) 0.0233(9) Uani 1 1 d . . . H23 H 0.1549 0.6962 0.3101 0.028 Uiso 1 1 calc R . . C24 C 0.16518(16) 0.5890(6) 0.37903(15) 0.0328(11) Uani 1 1 d . . . H24A H 0.199 0.6028 0.3801 0.049 Uiso 1 1 calc R . . H24B H 0.1573 0.4816 0.3953 0.049 Uiso 1 1 calc R . . H24C H 0.1512 0.6852 0.3962 0.049 Uiso 1 1 calc R . . N1 N 0.30672(11) 0.6818(4) 0.03758(12) 0.0225(7) Uani 1 1 d . . . H1A H 0.2869 0.5914 0.0345 0.034 Uiso 1 1 calc R . . H1B H 0.2913 0.7799 0.0291 0.034 Uiso 1 1 calc R . . H1C H 0.3181 0.6894 0.0695 0.034 Uiso 1 1 calc R . . N2 N 0.16515(12) 1.0722(5) 0.16722(12) 0.0258(8) Uani 1 1 d . . . H2A H 0.1743 1.054 0.1359 0.039 Uiso 1 1 calc R . . H2B H 0.1896 1.0545 0.1892 0.039 Uiso 1 1 calc R . . H2C H 0.1549 1.1817 0.17 0.039 Uiso 1 1 calc R . . N3 N 0.17129(12) 0.4433(4) 0.29970(12) 0.0229(7) Uani 1 1 d . . . H3A H 0.2025 0.4592 0.3032 0.034 Uiso 1 1 calc R . . H3B H 0.1623 0.4444 0.267 0.034 Uiso 1 1 calc R . . H3C H 0.1637 0.3407 0.3131 0.034 Uiso 1 1 calc R . . O1 O 0.23465(10) 0.4922(4) -0.01261(9) 0.0263(6) Uani 1 1 d . . . H1D H 0.2283 0.4177 0.0129 0.032 Uiso 1 1 d R . . H1E H 0.2473 0.4305 -0.038 0.032 Uiso 1 1 d R . . Cl1 Cl 0.33660(4) 0.57086(14) 0.14872(3) 0.0254(2) Uani 1 1 d . . . Cl2 Cl 0.14258(4) 0.47054(13) 0.18511(4) 0.0268(2) Uani 1 1 d . . . Cl3 Cl 0.25036(4) 0.69756(13) 0.25835(3) 0.0252(2) Uani 1 1 d . . . Cl4 Cl 0.22548(4) 0.78870(13) 0.11347(4) 0.0275(2) Uani 1 1 d . . . Cl5 Cl 0.21850(4) 0.28183(14) 0.08319(3) 0.0272(2) Uani 1 1 d . . . Pb1 Pb 0.239400(5) 0.50301(2) 0.166474(5) 0.01835(5) 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 C1 0.020(2) 0.026(2) 0.025(2) -0.0058(17) 0.0066(16) 0.0053(18) C2 0.030(2) 0.032(3) 0.025(2) -0.0008(18) 0.0034(18) 0.006(2) C3 0.033(2) 0.031(3) 0.037(2) -0.0087(19) -0.0059(19) 0.003(2) C4 0.028(2) 0.025(3) 0.056(3) -0.005(2) 0.002(2) -0.003(2) C5 0.030(3) 0.027(2) 0.039(3) 0.006(2) 0.002(2) 0.003(2) C6 0.022(2) 0.029(2) 0.032(2) -0.0052(19) -0.0020(18) 0.0067(19) C7 0.028(2) 0.026(2) 0.030(2) -0.0032(18) 0.0072(18) 0.0011(19) C8 0.040(3) 0.026(3) 0.056(3) -0.005(2) 0.013(2) 0.005(2) C9 0.021(2) 0.039(3) 0.0221(19) 0.0077(17) 0.0052(16) -0.0062(18) C10 0.035(3) 0.032(3) 0.036(3) -0.005(2) -0.001(2) -0.007(2) C11 0.034(3) 0.037(3) 0.045(3) 0.006(2) -0.006(2) 0.003(2) C12 0.027(2) 0.054(3) 0.026(2) 0.000(2) -0.0057(17) -0.004(2) C13 0.028(3) 0.044(3) 0.031(2) -0.010(2) 0.0046(19) -0.006(2) C14 0.027(2) 0.034(3) 0.033(2) 0.003(2) 0.0063(19) 0.002(2) C15 0.034(3) 0.045(3) 0.037(3) 0.006(2) -0.007(2) -0.011(2) C16 0.049(3) 0.107(6) 0.024(2) 0.008(3) -0.004(2) -0.028(4) C17 0.023(2) 0.025(2) 0.0185(19) 0.0039(16) 0.0015(16) 0.0024(18) C18 0.024(2) 0.036(3) 0.029(2) -0.007(2) 0.0039(18) -0.005(2) C19 0.027(3) 0.057(4) 0.031(2) -0.002(2) 0.000(2) -0.011(2) C20 0.022(2) 0.072(4) 0.028(2) 0.004(2) -0.0018(18) 0.002(2) C21 0.032(3) 0.054(3) 0.035(2) 0.007(2) 0.010(2) 0.018(2) C22 0.032(2) 0.031(3) 0.028(2) 0.0067(19) 0.0100(18) 0.006(2) C23 0.024(2) 0.019(2) 0.027(2) 0.0026(17) 0.0052(17) 0.0005(18) C24 0.030(3) 0.037(3) 0.031(2) -0.004(2) -0.0053(19) -0.001(2) N1 0.0214(18) 0.0191(18) 0.0270(17) -0.0003(14) 0.0003(14) 0.0005(14) N2 0.0206(18) 0.0251(18) 0.0315(19) -0.0038(16) -0.0014(15) -0.0025(15) N3 0.0190(17) 0.0238(18) 0.0264(17) 0.0019(14) 0.0054(14) -0.0003(14) O1 0.0299(15) 0.0259(15) 0.0234(13) -0.0013(14) 0.0053(11) 0.0025(15) Cl1 0.0245(5) 0.0279(5) 0.0237(5) 0.0004(4) -0.0001(4) 0.0031(4) Cl2 0.0259(5) 0.0230(6) 0.0313(5) -0.0001(4) 0.0000(4) 0.0027(4) Cl3 0.0275(5) 0.0256(5) 0.0226(5) -0.0030(4) 0.0015(4) -0.0063(4) Cl4 0.0308(6) 0.0239(5) 0.0284(5) 0.0092(4) 0.0074(4) 0.0061(4) Cl5 0.0361(6) 0.0254(5) 0.0202(5) -0.0008(4) 0.0028(4) 0.0051(5) Pb1 0.02007(7) 0.01817(7) 0.01677(7) 0.00085(7) 0.00053(5) -0.00114(7) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.502(5) . ? C2 C3 1.39 . ? C2 H2 0.95 . ? C3 C4 1.39 . ? C3 H3 0.95 . ? C4 C5 1.39 . ? C4 H4 0.95 . ? C5 C6 1.39 . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.502(6) . ? C7 N1 1.504(5) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C9 C15 1.509(5) . ? C10 C11 1.39 . ? C10 H10 0.95 . ? C11 C12 1.39 . ? C11 H11 0.95 . ? C12 C13 1.39 . ? C12 H12 0.95 . ? C13 C14 1.39 . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.461(7) . ? C15 N2 1.486(6) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.39 . ? C17 C22 1.39 . ? C17 C23 1.508(4) . ? C18 C19 1.39 . ? C18 H18 0.95 . ? C19 C20 1.39 . ? C19 H19 0.95 . ? C20 C21 1.39 . ? C20 H20 0.95 . ? C21 C22 1.39 . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 C24 1.507(5) . ? C23 N3 1.508(5) . ? C23 H23 1 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N2 H2C 0.91 . ? N3 H3A 0.91 . ? N3 H3B 0.91 . ? N3 H3C 0.91 . ? O1 H1D 0.9281 . ? O1 H1E 0.9267 . ? Cl1 Pb1 2.9135(11) . ? Cl2 Pb1 2.8704(12) . ? Cl3 Pb1 2.9180(10) . ? Cl3 Pb1 3.1404(10) 4 ? Cl4 Pb1 2.6730(10) . ? Cl5 Pb1 2.8807(10) . ? Pb1 Cl3 3.1404(10) 4_545 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 123.3(2) . . ? C6 C1 C7 116.7(2) . . ? C1 C2 C3 120 . . ? C1 C2 H2 120 . . ? C3 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C1 C7 C8 115.8(4) . . ? C1 C7 N1 109.1(3) . . ? C8 C7 N1 109.4(4) . . ? C1 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? N1 C7 H7 107.4 . . ? 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 C14 120 . . ? C10 C9 C15 122.4(3) . . ? C14 C9 C15 117.5(3) . . ? C11 C10 C9 120 . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C10 C11 C12 120 . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C13 C12 C11 120 . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C12 C13 C14 120 . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C13 C14 C9 120 . . ? C13 C14 H14 120 . . ? C9 C14 H14 120 . . ? C16 C15 N2 111.3(4) . . ? C16 C15 C9 113.9(4) . . ? N2 C15 C9 109.2(3) . . ? C16 C15 H15 107.4 . . ? N2 C15 H15 107.4 . . ? C9 C15 H15 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120 . . ? C18 C17 C23 123.3(2) . . ? C22 C17 C23 116.7(2) . . ? C19 C18 C17 120 . . ? C19 C18 H18 120 . . ? C17 C18 H18 120 . . ? C20 C19 C18 120 . . ? C20 C19 H19 120 . . ? C18 C19 H19 120 . . ? C19 C20 C21 120 . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C22 C21 C20 120 . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C21 C22 C17 120 . . ? C21 C22 H22 120 . . ? C17 C22 H22 120 . . ? C24 C23 C17 112.9(3) . . ? C24 C23 N3 108.2(3) . . ? C17 C23 N3 111.0(3) . . ? C24 C23 H23 108.2 . . ? C17 C23 H23 108.2 . . ? N3 C23 H23 108.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C15 N2 H2A 109.5 . . ? C15 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C15 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C23 N3 H3A 109.5 . . ? C23 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C23 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? H1D O1 H1E 108.8 . . ? Pb1 Cl3 Pb1 161.92(4) . 4 ? Cl4 Pb1 Cl2 92.60(3) . . ? Cl4 Pb1 Cl5 93.47(3) . . ? Cl2 Pb1 Cl5 85.12(3) . . ? Cl4 Pb1 Cl1 83.17(3) . . ? Cl2 Pb1 Cl1 174.57(3) . . ? Cl5 Pb1 Cl1 98.49(3) . . ? Cl4 Pb1 Cl3 91.70(3) . . ? Cl2 Pb1 Cl3 87.92(3) . . ? Cl5 Pb1 Cl3 171.51(3) . . ? Cl1 Pb1 Cl3 88.80(3) . . ? Cl4 Pb1 Cl3 171.55(3) . 4_545 ? Cl2 Pb1 Cl3 83.21(3) . 4_545 ? Cl5 Pb1 Cl3 93.48(3) . 4_545 ? Cl1 Pb1 Cl3 100.55(3) . 4_545 ? Cl3 Pb1 Cl3 80.844(14) . 4_545 ? 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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 179.5(3) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 -179.5(3) . . . . ? C2 C1 C7 C8 -42.8(5) . . . . ? C6 C1 C7 C8 136.6(3) . . . . ? C2 C1 C7 N1 81.0(4) . . . . ? C6 C1 C7 N1 -99.5(3) . . . . ? C14 C9 C10 C11 0 . . . . ? C15 C9 C10 C11 -175.6(3) . . . . ? C9 C10 C11 C12 0 . . . . ? C10 C11 C12 C13 0 . . . . ? C11 C12 C13 C14 0 . . . . ? C12 C13 C14 C9 0 . . . . ? C10 C9 C14 C13 0 . . . . ? C15 C9 C14 C13 175.8(3) . . . . ? C10 C9 C15 C16 60.7(5) . . . . ? C14 C9 C15 C16 -115.0(4) . . . . ? C10 C9 C15 N2 -64.4(5) . . . . ? C14 C9 C15 N2 119.9(3) . . . . ? C22 C17 C18 C19 0 . . . . ? C23 C17 C18 C19 178.1(3) . . . . ? C17 C18 C19 C20 0 . . . . ? C18 C19 C20 C21 0 . . . . ? C19 C20 C21 C22 0 . . . . ? C20 C21 C22 C17 0 . . . . ? C18 C17 C22 C21 0 . . . . ? C23 C17 C22 C21 -178.2(3) . . . . ? C18 C17 C23 C24 -95.1(4) . . . . ? C22 C17 C23 C24 83.0(4) . . . . ? C18 C17 C23 N3 26.6(4) . . . . ? C22 C17 C23 N3 -155.3(2) . . . . ? Pb1 Cl3 Pb1 Cl4 -6.83(13) 4 . . . ? Pb1 Cl3 Pb1 Cl2 -99.37(13) 4 . . . ? Pb1 Cl3 Pb1 Cl1 76.29(13) 4 . . . ? Pb1 Cl3 Pb1 Cl3 177.18(15) 4 . . 4_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.91 2.08 2.844(4) 141.3 . N1 H1B O1 0.91 1.97 2.879(4) 172.7 7_565 N1 H1C Cl1 0.91 2.37 3.208(3) 152.5 . N2 H2A Cl4 0.91 2.63 3.206(4) 121.9 . N2 H2A Cl5 0.91 2.64 3.247(4) 124.4 1_565 N2 H2B Cl3 0.91 2.46 3.238(3) 144.2 4 N2 H2C Cl2 0.91 2.32 3.221(4) 168.9 1_565 N3 H3A Cl3 0.91 2.64 3.260(4) 125.7 . N3 H3B Cl2 0.91 2.27 3.178(3) 175 . N3 H3C Cl1 0.91 2.35 3.239(4) 166.4 4_545 O1 H1D Cl5 0.93 2.21 3.123(3) 168.6 . O1 H1E Cl5 0.93 2.31 3.209(3) 163.3 7 _chemical_name_common tris((racemic)-beta-phenethylammonium)pentachloroplumbate(ii) ###END data_3apb13la _database_code_depnum_ccdc_archive 'CCDC 607739' _audit_creation_date 2006-06-21T12:29:39-00:00 _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 ; tris((racemic)-\b-phenethylammonium)pentachloroplumbate(II) ; _chemical_formula_moiety '3(C8 H12 N), Br5 Pb, H2 O' _chemical_formula_sum 'C24 H38 Br5 N3 O Pb' _chemical_formula_weight 991.31 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 29.171(4) _cell_length_b 8.1095(12) _cell_length_c 27.656(4) _cell_angle_alpha 90 _cell_angle_beta 92.234(3) _cell_angle_gamma 90 _cell_volume 6537.5(17) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 980 _cell_measurement_theta_min 3.272 _cell_measurement_theta_max 28.294 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.015 1 0 0 0.015 0 0 -1 0.075 0 0 1 0.075 0 -1 0 0.16 -1 4 4 0.18 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.294 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.147 _exptl_absorpt_correction_T_max 0.7065 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_unetI/netI 0.0703 _diffrn_reflns_number 21393 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 7843 _reflns_number_gt 5659 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0337P)^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 7843 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.914 _refine_diff_density_min -1.816 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 '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' 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 0.38199(13) 0.8064(4) 0.00752(14) 0.0222(13) Uani 1 1 d G . . C2 C 0.41456(14) 0.8205(4) 0.04533(12) 0.0259(14) Uani 1 1 d G . . H2 H 0.418 0.7348 0.0686 0.031 Uiso 1 1 calc R . . C3 C 0.44217(13) 0.9600(5) 0.04907(14) 0.0364(18) Uani 1 1 d G . . H3 H 0.4644 0.9696 0.0749 0.044 Uiso 1 1 calc R . . C4 C 0.43720(14) 1.0853(4) 0.01499(17) 0.0413(19) Uani 1 1 d G . . H4 H 0.4561 1.1807 0.0176 0.05 Uiso 1 1 calc R . . C5 C 0.40463(15) 1.0712(4) -0.02282(14) 0.0376(17) Uani 1 1 d G . . H5 H 0.4012 1.1569 -0.0461 0.045 Uiso 1 1 calc R . . C6 C 0.37702(13) 0.9318(5) -0.02656(12) 0.0257(14) Uani 1 1 d G . . H6 H 0.3548 0.9221 -0.0524 0.031 Uiso 1 1 calc R . . C7 C 0.3513(2) 0.6585(8) 0.0016(2) 0.0255(14) Uani 1 1 d . . . H7 H 0.3397 0.6568 -0.0329 0.031 Uiso 1 1 calc R . . C8 C 0.3723(3) 0.4921(8) 0.0122(3) 0.0371(17) Uani 1 1 d . . . H8A H 0.3487 0.4065 0.0077 0.056 Uiso 1 1 calc R . . H8B H 0.3845 0.4896 0.0457 0.056 Uiso 1 1 calc R . . H8C H 0.3971 0.4717 -0.0098 0.056 Uiso 1 1 calc R . . C9 C 0.08627(12) 0.9604(5) 0.13817(13) 0.0292(16) Uani 1 1 d G . . C10 C 0.06208(15) 1.1061(4) 0.13006(15) 0.0384(18) Uani 1 1 d G . . H10 H 0.0697 1.2017 0.1486 0.046 Uiso 1 1 calc R . . C11 C 0.02677(15) 1.1121(5) 0.09487(16) 0.045(2) Uani 1 1 d G . . H11 H 0.0102 1.2116 0.0893 0.053 Uiso 1 1 calc R . . C12 C 0.01566(13) 0.9723(6) 0.06778(14) 0.0395(19) Uani 1 1 d G . . H12 H -0.0085 0.9763 0.0437 0.047 Uiso 1 1 calc R . . C13 C 0.03985(15) 0.8266(5) 0.07589(14) 0.0348(17) Uani 1 1 d G . . H13 H 0.0323 0.731 0.0574 0.042 Uiso 1 1 calc R . . C14 C 0.07516(13) 0.8206(4) 0.11108(15) 0.0308(16) Uani 1 1 d G . . H14 H 0.0917 0.7211 0.1166 0.037 Uiso 1 1 calc R . . C15 C 0.1234(2) 0.9433(9) 0.1785(2) 0.0331(16) Uani 1 1 d . . . H15 H 0.1368 0.8304 0.1759 0.04 Uiso 1 1 calc R . . C16 C 0.1055(3) 0.9586(11) 0.2276(2) 0.053(2) Uani 1 1 d . . . H16A H 0.1309 0.9476 0.2517 0.08 Uiso 1 1 calc R . . H16B H 0.0829 0.8716 0.2326 0.08 Uiso 1 1 calc R . . H16C H 0.091 1.0667 0.2311 0.08 Uiso 1 1 calc R . . C17 C 0.09464(10) 0.5505(5) 0.32369(15) 0.0231(14) Uani 1 1 d G . . C18 C 0.07339(14) 0.3986(4) 0.31650(15) 0.0303(16) Uani 1 1 d G . . H18 H 0.0914 0.3013 0.3146 0.036 Uiso 1 1 calc R . . C19 C 0.02583(15) 0.3891(5) 0.31210(16) 0.042(2) Uani 1 1 d G . . H19 H 0.0113 0.2852 0.3072 0.051 Uiso 1 1 calc R . . C20 C -0.00047(10) 0.5314(7) 0.31488(17) 0.046(2) Uani 1 1 d G . . H20 H -0.033 0.5249 0.3119 0.055 Uiso 1 1 calc R . . C21 C 0.02078(14) 0.6833(5) 0.32207(16) 0.044(2) Uani 1 1 d G . . H21 H 0.0028 0.7806 0.324 0.053 Uiso 1 1 calc R . . C22 C 0.06834(15) 0.6929(4) 0.32648(15) 0.0312(16) Uani 1 1 d G . . H22 H 0.0829 0.7967 0.3314 0.037 Uiso 1 1 calc R . . C23 C 0.1459(2) 0.5729(8) 0.3303(2) 0.0243(14) Uani 1 1 d . . . H23 H 0.1542 0.6802 0.3152 0.029 Uiso 1 1 calc R . . C24 C 0.1625(2) 0.5770(9) 0.3819(2) 0.0320(16) Uani 1 1 d . . . H24A H 0.1959 0.5906 0.3836 0.048 Uiso 1 1 calc R . . H24B H 0.1543 0.4735 0.3977 0.048 Uiso 1 1 calc R . . H24C H 0.1481 0.6696 0.3983 0.048 Uiso 1 1 calc R . . N1 N 0.30988(16) 0.6830(6) 0.03293(17) 0.0234(11) Uani 1 1 d . . . H1A H 0.2909 0.5944 0.0296 0.035 Uiso 1 1 calc R . . H1B H 0.2945 0.7759 0.0233 0.035 Uiso 1 1 calc R . . H1C H 0.3196 0.6934 0.0645 0.035 Uiso 1 1 calc R . . N2 N 0.16101(18) 1.0642(7) 0.17021(18) 0.0289(13) Uani 1 1 d . . . H2A H 0.1712 1.0511 0.1398 0.043 Uiso 1 1 calc R . . H2B H 0.1846 1.0465 0.1921 0.043 Uiso 1 1 calc R . . H2C H 0.1502 1.1686 0.1737 0.043 Uiso 1 1 calc R . . N3 N 0.17133(17) 0.4367(7) 0.30483(18) 0.0266(12) Uani 1 1 d . . . H3A H 0.2021 0.4538 0.3085 0.04 Uiso 1 1 calc R . . H3B H 0.163 0.4371 0.2728 0.04 Uiso 1 1 calc R . . H3C H 0.1641 0.3375 0.3179 0.04 Uiso 1 1 calc R . . O1 O 0.23424(15) 0.5076(5) -0.01090(14) 0.0259(10) Uani 1 1 d . . . H1D H 0.2279 0.433 0.0146 0.031 Uiso 1 1 d R . . H1E H 0.2468 0.4458 -0.0363 0.031 Uiso 1 1 d R . . Br1 Br 0.33891(2) 0.55174(8) 0.14702(2) 0.02462(14) Uani 1 1 d . . . Br2 Br 0.13757(2) 0.46650(8) 0.18768(2) 0.02622(15) Uani 1 1 d . . . Br3 Br 0.24903(2) 0.69847(8) 0.25874(2) 0.02468(15) Uani 1 1 d . . . Br4 Br 0.22512(2) 0.79005(8) 0.11136(2) 0.02488(15) Uani 1 1 d . . . Br5 Br 0.21499(2) 0.26971(8) 0.08206(2) 0.02525(15) Uani 1 1 d . . . Pb1 Pb 0.237704(8) 0.49550(3) 0.165766(7) 0.01719(7) 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 C1 0.025(3) 0.017(3) 0.024(3) -0.007(2) -0.001(2) 0.006(3) C2 0.024(4) 0.030(4) 0.025(3) -0.002(3) 0.002(3) 0.004(3) C3 0.028(4) 0.042(5) 0.039(4) -0.006(3) -0.007(3) 0.005(3) C4 0.023(4) 0.038(5) 0.061(5) -0.016(4) -0.006(3) -0.006(3) C5 0.030(4) 0.030(4) 0.052(5) 0.008(3) 0.001(3) -0.002(3) C6 0.022(4) 0.024(3) 0.031(4) 0.001(3) -0.003(3) 0.005(3) C7 0.028(4) 0.031(4) 0.018(3) -0.001(3) 0.000(3) 0.001(3) C8 0.036(4) 0.035(4) 0.041(4) -0.003(3) 0.005(3) 0.005(4) C9 0.022(4) 0.043(5) 0.022(3) 0.005(3) 0.003(3) -0.007(3) C10 0.033(4) 0.036(4) 0.046(4) -0.013(3) -0.001(3) -0.008(3) C11 0.041(5) 0.040(5) 0.051(5) 0.002(4) -0.011(4) 0.010(4) C12 0.030(4) 0.064(6) 0.023(3) 0.004(3) -0.009(3) 0.002(4) C13 0.033(4) 0.039(4) 0.032(4) -0.013(3) 0.000(3) -0.005(3) C14 0.024(4) 0.041(4) 0.028(4) 0.004(3) 0.002(3) -0.001(3) C15 0.031(4) 0.038(4) 0.030(4) 0.005(3) -0.005(3) -0.006(3) C16 0.044(5) 0.089(7) 0.027(4) 0.003(4) -0.001(3) -0.026(5) C17 0.012(3) 0.037(4) 0.020(3) 0.001(3) -0.001(2) -0.001(3) C18 0.021(4) 0.039(4) 0.030(4) -0.002(3) -0.002(3) -0.001(3) C19 0.032(4) 0.061(6) 0.034(4) -0.004(4) -0.003(3) -0.023(4) C20 0.018(4) 0.082(7) 0.038(4) 0.005(4) 0.000(3) 0.006(4) C21 0.030(4) 0.069(6) 0.033(4) 0.004(4) 0.003(3) 0.019(4) C22 0.023(4) 0.037(4) 0.034(4) 0.009(3) 0.005(3) 0.006(3) C23 0.023(4) 0.017(3) 0.033(4) 0.003(3) 0.004(3) 0.000(3) C24 0.023(4) 0.039(4) 0.035(4) -0.008(3) 0.000(3) -0.002(3) N1 0.019(3) 0.026(3) 0.026(3) 0.002(2) -0.004(2) 0.002(2) N2 0.027(3) 0.028(3) 0.031(3) -0.007(2) -0.005(2) -0.001(3) N3 0.017(3) 0.035(3) 0.028(3) 0.004(2) 0.003(2) 0.000(2) O1 0.034(3) 0.021(2) 0.024(2) 0.0026(18) 0.0051(18) 0.002(2) Br1 0.0235(3) 0.0265(4) 0.0237(3) 0.0017(2) -0.0014(2) 0.0027(3) Br2 0.0213(3) 0.0253(4) 0.0320(3) 0.0001(3) -0.0015(3) 0.0025(3) Br3 0.0271(3) 0.0258(4) 0.0211(3) -0.0055(2) 0.0014(2) -0.0090(3) Br4 0.0267(3) 0.0231(3) 0.0250(3) 0.0085(2) 0.0027(2) 0.0051(3) Br5 0.0351(4) 0.0223(3) 0.0183(3) -0.0007(2) -0.0001(2) 0.0034(3) Pb1 0.01938(11) 0.01686(12) 0.01517(10) 0.00106(9) -0.00132(7) -0.00076(9) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.501(7) . ? C2 C3 1.39 . ? C2 H2 0.95 . ? C3 C4 1.39 . ? C3 H3 0.95 . ? C4 C5 1.39 . ? C4 H4 0.95 . ? C5 C6 1.39 . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.506(9) . ? C7 N1 1.528(7) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C9 C15 1.531(7) . ? C10 C11 1.39 . ? C10 H10 0.95 . ? C11 C12 1.39 . ? C11 H11 0.95 . ? C12 C13 1.39 . ? C12 H12 0.95 . ? C13 C14 1.39 . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.478(9) . ? C15 N2 1.497(8) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.39 . ? C17 C22 1.39 . ? C17 C23 1.511(7) . ? C18 C19 1.39 . ? C18 H18 0.95 . ? C19 C20 1.39 . ? C19 H19 0.95 . ? C20 C21 1.39 . ? C20 H20 0.95 . ? C21 C22 1.39 . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 C24 1.487(8) . ? C23 N3 1.519(8) . ? C23 H23 1 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N2 H2C 0.91 . ? N3 H3A 0.91 . ? N3 H3B 0.91 . ? N3 H3C 0.91 . ? O1 H1D 0.953 . ? O1 H1E 0.9476 . ? Br1 Pb1 3.0515(8) . ? Br2 Pb1 3.0156(8) . ? Br3 Pb1 3.0600(7) . ? Br3 Pb1 3.2014(7) 4 ? Br4 Pb1 2.8393(7) . ? Br5 Pb1 3.0052(7) . ? Pb1 Br3 3.2014(7) 4_545 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 122.3(3) . . ? C6 C1 C7 117.7(3) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120 . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C1 C7 C8 117.4(5) . . ? C1 C7 N1 108.3(5) . . ? C8 C7 N1 109.2(5) . . ? C1 C7 H7 107.1 . . ? C8 C7 H7 107.1 . . ? N1 C7 H7 107.1 . . ? 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 C14 120 . . ? C10 C9 C15 122.3(4) . . ? C14 C9 C15 117.6(4) . . ? C11 C10 C9 120 . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C10 C11 C12 120 . . ? C10 C11 H11 120 . . ? C12 C11 H11 120 . . ? C13 C12 C11 120 . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C14 C13 C12 120 . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C13 C14 C9 120 . . ? C13 C14 H14 120 . . ? C9 C14 H14 120 . . ? C16 C15 N2 111.9(6) . . ? C16 C15 C9 113.5(6) . . ? N2 C15 C9 109.3(5) . . ? C16 C15 H15 107.3 . . ? N2 C15 H15 107.3 . . ? C9 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120 . . ? C18 C17 C23 123.9(4) . . ? C22 C17 C23 116.1(4) . . ? C17 C18 C19 120 . . ? C17 C18 H18 120 . . ? C19 C18 H18 120 . . ? C20 C19 C18 120 . . ? C20 C19 H19 120 . . ? C18 C19 H19 120 . . ? C19 C20 C21 120 . . ? C19 C20 H20 120 . . ? C21 C20 H20 120 . . ? C22 C21 C20 120 . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C21 C22 C17 120 . . ? C21 C22 H22 120 . . ? C17 C22 H22 120 . . ? C24 C23 C17 113.7(5) . . ? C24 C23 N3 108.4(5) . . ? C17 C23 N3 110.8(5) . . ? C24 C23 H23 107.9 . . ? C17 C23 H23 107.9 . . ? N3 C23 H23 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C15 N2 H2A 109.5 . . ? C15 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C15 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C23 N3 H3A 109.5 . . ? C23 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C23 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? H1D O1 H1E 107.8 . . ? Pb1 Br3 Pb1 163.56(2) . 4 ? Br4 Pb1 Br5 94.83(2) . . ? Br4 Pb1 Br2 93.776(19) . . ? Br5 Pb1 Br2 85.470(19) . . ? Br4 Pb1 Br1 83.695(19) . . ? Br5 Pb1 Br1 98.391(18) . . ? Br2 Pb1 Br1 175.533(18) . . ? Br4 Pb1 Br3 90.02(2) . . ? Br5 Pb1 Br3 171.251(18) . . ? Br2 Pb1 Br3 86.951(18) . . ? Br1 Pb1 Br3 89.363(18) . . ? Br4 Pb1 Br3 171.303(18) . 4_545 ? Br5 Pb1 Br3 93.52(2) . 4_545 ? Br2 Pb1 Br3 84.471(17) . 4_545 ? Br1 Pb1 Br3 97.479(17) . 4_545 ? Br3 Pb1 Br3 81.392(13) . 4_545 ? 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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 179.8(4) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 -179.8(4) . . . . ? C2 C1 C7 C8 -39.4(6) . . . . ? C6 C1 C7 C8 140.4(5) . . . . ? C2 C1 C7 N1 84.8(5) . . . . ? C6 C1 C7 N1 -95.4(4) . . . . ? C14 C9 C10 C11 0 . . . . ? C15 C9 C10 C11 -176.0(5) . . . . ? C9 C10 C11 C12 0 . . . . ? C10 C11 C12 C13 0 . . . . ? C11 C12 C13 C14 0 . . . . ? C12 C13 C14 C9 0 . . . . ? C10 C9 C14 C13 0 . . . . ? C15 C9 C14 C13 176.2(4) . . . . ? C10 C9 C15 C16 64.8(7) . . . . ? C14 C9 C15 C16 -111.3(6) . . . . ? C10 C9 C15 N2 -60.9(6) . . . . ? C14 C9 C15 N2 123.0(5) . . . . ? C22 C17 C18 C19 0 . . . . ? C23 C17 C18 C19 178.2(4) . . . . ? C17 C18 C19 C20 0 . . . . ? C18 C19 C20 C21 0 . . . . ? C19 C20 C21 C22 0 . . . . ? C20 C21 C22 C17 0 . . . . ? C18 C17 C22 C21 0 . . . . ? C23 C17 C22 C21 -178.3(4) . . . . ? C18 C17 C23 C24 -94.4(5) . . . . ? C22 C17 C23 C24 83.8(5) . . . . ? C18 C17 C23 N3 27.9(6) . . . . ? C22 C17 C23 N3 -153.9(4) . . . . ? Pb1 Br3 Pb1 Br4 -10.99(8) 4 . . . ? Pb1 Br3 Pb1 Br2 -104.77(8) 4 . . . ? Pb1 Br3 Pb1 Br1 72.71(8) 4 . . . ? Pb1 Br3 Pb1 Br3 170.37(9) 4 . . 4_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1 0.91 2.08 2.856(7) 142 . N1 H1B O1 0.91 1.97 2.874(6) 171.6 7_565 N1 H1C Br1 0.91 2.6 3.406(5) 148.2 . N2 H2A Br4 0.91 2.77 3.366(5) 124.1 . N2 H2A Br5 0.91 2.74 3.391(5) 129.8 1_565 N2 H2B Br3 0.91 2.63 3.396(5) 142.4 4 N2 H2C Br2 0.91 2.48 3.372(5) 168.1 1_565 N3 H3A Br3 0.91 2.8 3.390(5) 123.5 . N3 H3B Br2 0.91 2.45 3.358(5) 174.2 . N3 H3C Br1 0.91 2.51 3.411(5) 168.5 4_545 O1 H1D Br5 0.95 2.33 3.280(4) 174.6 . O1 H1E Br5 0.95 2.45 3.369(4) 163 7 _chemical_name_common tris((racemic)-beta-phenethylammonium)pentachloroplumbate(ii) ###END data_7 _database_code_depnum_ccdc_archive 'CCDC 607740' _audit_creation_date 2006-04-04T10:53:17-00:00 _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 ; bis((R)-\b-phenethylammonium)tetraiodoplumbate(II) ; _chemical_formula_moiety 'I4 Pb, 2(C8 H12 N)' _chemical_formula_sum 'C16 H24 I4 N2 Pb' _chemical_formula_weight 959.16 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.868(5) _cell_length_b 9.247(5) _cell_length_c 28.729(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2355.8(19) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 914 _cell_measurement_theta_min 3.484 _cell_measurement_theta_max 28.245 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description polyhedral _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.04 0 0 1 0.04 0 2 -1 0.07 0 -2 1 0.07 -2 -2 -1 0.1 1 -1 -2 0.11 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.405 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_absorpt_correction_T_min 0.0962 _exptl_absorpt_correction_T_max 0.4044 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_unetI/netI 0.042 _diffrn_reflns_number 12963 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 4381 _reflns_number_gt 3874 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0172P)^2^+29.8048P] 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 4381 _refine_ls_number_parameters 184 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0851 _refine_ls_wR_factor_gt 0.083 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1849 Friedel Pairs' _refine_ls_abs_structure_Flack 0.095(16) _refine_diff_density_max 1.587 _refine_diff_density_min -1.722 _refine_diff_density_rms 0.222 #----------------------------------------------------------------------------# # 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' 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' I I -0.4742 1.8119 '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 0.8857(10) 0.4203(9) 0.1776(2) 0.0212(18) Uani 1 1 d GU . . C2 C 0.7871(8) 0.3321(9) 0.2022(3) 0.023(2) Uani 1 1 d GU . . H2 H 0.7028 0.29 0.1869 0.028 Uiso 1 1 calc R . . C3 C 0.8118(10) 0.3053(9) 0.2492(3) 0.028(2) Uani 1 1 d GU . . H3 H 0.7444 0.245 0.266 0.033 Uiso 1 1 calc R . . C4 C 0.9351(11) 0.3668(11) 0.2716(2) 0.027(2) Uani 1 1 d GU . . H4 H 0.952 0.3485 0.3037 0.033 Uiso 1 1 calc R . . C5 C 1.0337(9) 0.4551(10) 0.2469(3) 0.026(2) Uani 1 1 d GU . . H5 H 1.118 0.4971 0.2622 0.032 Uiso 1 1 calc R . . C6 C 1.0090(9) 0.4819(9) 0.1999(3) 0.0218(19) Uani 1 1 d GU . . H6 H 1.0764 0.5422 0.1831 0.026 Uiso 1 1 calc R . . C7 C 0.8525(15) 0.4624(13) 0.1277(4) 0.0271(19) Uani 1 1 d DU . . H7 H 0.7551 0.4152 0.1188 0.033 Uiso 1 1 calc R . . C8 C 0.837(2) 0.6207(14) 0.1178(5) 0.037(3) Uani 1 1 d DU . . H8A H 0.8123 0.6348 0.0848 0.055 Uiso 1 1 calc R . . H8B H 0.9316 0.67 0.1251 0.055 Uiso 1 1 calc R . . H8C H 0.7556 0.661 0.137 0.055 Uiso 1 1 calc R . . C9 C 0.4395(10) 0.0201(9) 0.1717(2) 0.0229(18) Uani 1 1 d GU . . C10 C 0.3290(9) 0.1155(9) 0.1871(3) 0.023(2) Uani 1 1 d GU . . H10 H 0.256 0.1517 0.1658 0.028 Uiso 1 1 calc R . . C11 C 0.3251(10) 0.1580(9) 0.2335(3) 0.028(2) Uani 1 1 d GU . . H11 H 0.2496 0.2232 0.2439 0.033 Uiso 1 1 calc R . . C12 C 0.4319(11) 0.1051(11) 0.2645(2) 0.028(2) Uani 1 1 d GU . . H12 H 0.4293 0.1341 0.2963 0.034 Uiso 1 1 calc R . . C13 C 0.5424(10) 0.0097(10) 0.2492(3) 0.027(2) Uani 1 1 d GU . . H13 H 0.6153 -0.0264 0.2705 0.033 Uiso 1 1 calc R . . C14 C 0.5462(9) -0.0328(9) 0.2028(3) 0.027(2) Uani 1 1 d GU . . H14 H 0.6217 -0.098 0.1924 0.032 Uiso 1 1 calc R . . C15 C 0.4399(14) -0.0367(13) 0.1220(4) 0.0235(18) Uani 1 1 d DU . . H15 H 0.5182 -0.1141 0.1197 0.028 Uiso 1 1 calc R . . C16 C 0.2952(15) -0.0958(15) 0.1038(5) 0.029(3) Uani 1 1 d DU . . H16A H 0.3088 -0.1262 0.0714 0.044 Uiso 1 1 calc R . . H16B H 0.217 -0.021 0.1054 0.044 Uiso 1 1 calc R . . H16C H 0.2645 -0.1792 0.1226 0.044 Uiso 1 1 calc R . . N1 N 0.9790(15) 0.3918(15) 0.0976(4) 0.027(3) Uani 1 1 d DU . . H1A H 0.9604 0.4089 0.0669 0.041 Uiso 1 1 calc R . . H1B H 0.9807 0.2948 0.1028 0.041 Uiso 1 1 calc R . . H1C H 1.0698 0.4306 0.1055 0.041 Uiso 1 1 calc R . . N2 N 0.4863(14) 0.0893(12) 0.0891(4) 0.019(2) Uani 1 1 d DU . . H2A H 0.5757 0.1272 0.0987 0.029 Uiso 1 1 calc R . . H2B H 0.4141 0.1592 0.0897 0.029 Uiso 1 1 calc R . . H2C H 0.4963 0.0551 0.0595 0.029 Uiso 1 1 calc R . . Pb1 Pb 0.89467(4) 0.99367(4) -0.00163(2) 0.01796(10) Uani 1 1 d . . . I1 I 0.87614(13) 1.03142(12) 0.10937(3) 0.0219(2) Uani 1 1 d . . . I2 I 1.20284(7) 1.20236(6) 0.00001(4) 0.02044(15) Uani 1 1 d . . . I3 I 1.08479(7) 0.68139(7) 0.00049(4) 0.02319(15) Uani 1 1 d . . . I4 I 0.88276(13) 1.02376(13) -0.11151(3) 0.0260(3) 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 C1 0.023(4) 0.019(4) 0.022(3) -0.001(3) 0.004(3) 0.000(3) C2 0.028(4) 0.017(4) 0.025(3) 0.002(3) 0.002(3) -0.003(3) C3 0.032(4) 0.027(5) 0.024(3) 0.003(4) 0.004(4) -0.003(4) C4 0.031(5) 0.028(5) 0.023(4) 0.001(4) 0.002(3) 0.002(4) C5 0.029(5) 0.024(5) 0.026(3) -0.001(4) -0.001(3) -0.001(3) C6 0.025(4) 0.015(4) 0.025(3) -0.002(3) 0.003(3) -0.001(3) C7 0.025(4) 0.033(4) 0.023(3) 0.004(3) 0.004(3) -0.004(4) C8 0.046(7) 0.036(4) 0.029(6) 0.007(4) 0.001(6) 0.010(5) C9 0.022(4) 0.021(4) 0.025(3) 0.001(3) 0.006(3) 0.002(3) C10 0.023(4) 0.019(4) 0.027(3) -0.002(3) 0.004(3) 0.001(3) C11 0.030(5) 0.025(5) 0.029(4) -0.005(4) 0.006(3) 0.000(3) C12 0.035(5) 0.024(5) 0.025(4) -0.001(4) 0.004(3) -0.006(4) C13 0.029(5) 0.026(5) 0.027(3) 0.004(4) 0.001(4) -0.005(3) C14 0.023(4) 0.027(5) 0.029(3) 0.001(4) 0.002(3) 0.002(3) C15 0.024(4) 0.018(4) 0.029(3) -0.004(3) 0.003(3) 0.002(4) C16 0.022(5) 0.028(5) 0.037(6) -0.003(5) -0.001(4) 0.002(4) N1 0.032(6) 0.031(5) 0.019(4) -0.002(4) 0.001(4) -0.002(4) N2 0.019(5) 0.019(5) 0.020(4) -0.004(4) -0.001(4) 0.007(4) Pb1 0.01791(19) 0.02027(18) 0.01569(19) -0.0009(3) 0.0010(3) -0.00083(14) I1 0.0222(6) 0.0252(6) 0.0181(4) 0.0007(4) 0.0005(4) 0.0054(5) I2 0.0186(3) 0.0212(3) 0.0216(3) 0.0035(6) -0.0014(6) -0.0028(2) I3 0.0200(3) 0.0234(3) 0.0262(3) -0.0023(6) -0.0035(6) 0.0055(2) I4 0.0270(6) 0.0315(7) 0.0194(4) -0.0032(5) 0.0023(5) -0.0056(5) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.514(14) . ? C2 C3 1.39 . ? C2 H2 0.95 . ? C3 C4 1.39 . ? C3 H3 0.95 . ? C4 C5 1.39 . ? C4 H4 0.95 . ? C5 C6 1.39 . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.498(14) . ? C7 N1 1.560(12) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C9 C15 1.521(13) . ? C10 C11 1.39 . ? C10 H10 0.95 . ? C11 C12 1.39 . ? C11 H11 0.95 . ? C12 C13 1.39 . ? C12 H12 0.95 . ? C13 C14 1.39 . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 C16 1.491(13) . ? C15 N2 1.557(12) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N2 H2C 0.91 . ? Pb1 I4 3.1709(15) . ? Pb1 I3 3.1895(16) 4_465 ? Pb1 I1 3.2122(14) . ? Pb1 I2 3.2858(16) 4_475 ? Pb1 I3 3.3444(16) . ? Pb1 I2 3.3459(16) . ? I2 Pb1 3.2858(16) 4_575 ? I3 Pb1 3.1895(16) 4_565 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 120.7(7) . . ? C6 C1 C7 119.1(7) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120 . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C8 C7 C1 116.6(11) . . ? C8 C7 N1 111.8(12) . . ? C1 C7 N1 106.1(10) . . ? C8 C7 H7 107.3 . . ? C1 C7 H7 107.3 . . ? N1 C7 H7 107.3 . . ? 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 C14 120 . . ? C10 C9 C15 121.2(7) . . ? C14 C9 C15 118.7(7) . . ? C9 C10 C11 120 . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C12 C11 C10 120 . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C13 C12 C11 120 . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C14 C13 C12 120 . . ? C14 C13 H13 120 . . ? C12 C13 H13 120 . . ? C13 C14 C9 120 . . ? C13 C14 H14 120 . . ? C9 C14 H14 120 . . ? C16 C15 C9 117.0(10) . . ? C16 C15 N2 106.7(11) . . ? C9 C15 N2 108.3(9) . . ? C16 C15 H15 108.2 . . ? C9 C15 H15 108.2 . . ? N2 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C15 N2 H2A 109.5 . . ? C15 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C15 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? I4 Pb1 I3 91.49(4) . 4_465 ? I4 Pb1 I1 167.72(2) . . ? I3 Pb1 I1 90.05(4) 4_465 . ? I4 Pb1 I2 85.52(3) . 4_475 ? I3 Pb1 I2 89.31(4) 4_465 4_475 ? I1 Pb1 I2 82.33(3) . 4_475 ? I4 Pb1 I3 96.36(4) . . ? I3 Pb1 I3 89.77(4) 4_465 . ? I1 Pb1 I3 95.83(3) . . ? I2 Pb1 I3 177.93(3) 4_475 . ? I4 Pb1 I2 89.46(3) . . ? I3 Pb1 I2 175.07(2) 4_465 . ? I1 Pb1 I2 88.00(3) . . ? I2 Pb1 I2 85.95(4) 4_475 . ? I3 Pb1 I2 94.93(4) . . ? Pb1 I2 Pb1 156.41(2) 4_575 . ? Pb1 I3 Pb1 150.78(2) 4_565 . ? 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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 -174.1(9) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 174.2(9) . . . . ? C2 C1 C7 C8 119.9(12) . . . . ? C6 C1 C7 C8 -54.2(14) . . . . ? C2 C1 C7 N1 -114.9(10) . . . . ? C6 C1 C7 N1 71.0(11) . . . . ? C14 C9 C10 C11 0 . . . . ? C15 C9 C10 C11 175.6(9) . . . . ? C9 C10 C11 C12 0 . . . . ? C10 C11 C12 C13 0 . . . . ? C11 C12 C13 C14 0 . . . . ? C12 C13 C14 C9 0 . . . . ? C10 C9 C14 C13 0 . . . . ? C15 C9 C14 C13 -175.7(9) . . . . ? C10 C9 C15 C16 -49.1(13) . . . . ? C14 C9 C15 C16 126.5(10) . . . . ? C10 C9 C15 N2 71.5(11) . . . . ? C14 C9 C15 N2 -112.9(9) . . . . ? I4 Pb1 I2 Pb1 84.97(11) . . . 4_575 ? I1 Pb1 I2 Pb1 -83.02(11) . . . 4_575 ? I2 Pb1 I2 Pb1 -0.57(8) 4_475 . . 4_575 ? I3 Pb1 I2 Pb1 -178.70(10) . . . 4_575 ? I4 Pb1 I3 Pb1 88.44(9) . . . 4_565 ? I3 Pb1 I3 Pb1 179.92(11) 4_465 . . 4_565 ? I1 Pb1 I3 Pb1 -90.06(9) . . . 4_565 ? I2 Pb1 I3 Pb1 -1.57(9) . . . 4_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.91 3.16 3.823(14) 131.6 4_465 N1 H1B I1 0.91 2.61 3.472(15) 157.7 1_545 N1 H1C I4 0.91 2.81 3.686(15) 161.3 4_565 N2 H2A I1 0.91 2.82 3.546(13) 137.2 1_545 N2 H2B I4 0.91 3.01 3.750(12) 139.5 4_465 N2 H2C I3 0.91 2.89 3.694(12) 147.7 4_455 _chemical_name_common bis((R)-beta-phenethylammonium)tetraiodoplumbate(ii) ###END data_8 _database_code_depnum_ccdc_archive 'CCDC 607741' _audit_creation_date 2006-04-04T11:09:49-00:00 _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 ; bis((S)-\b-phenethylammonium)tetraiodoplumbate(II) ; _chemical_formula_moiety 'I4 Pb, 2(C8 H12 N)' _chemical_formula_sum 'C16 H24 I4 N2 Pb' _chemical_formula_weight 959.16 _chemical_absolute_configuration rmad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 8.8531(17) _cell_length_b 9.2312(18) _cell_length_c 28.650(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2341.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 909 _cell_measurement_theta_min 3.188 _cell_measurement_theta_max 25.956 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.13 -1 0 0 0.13 0 0 1 0.03 0 0 -1 0.03 0 -1 0 0.065 0 1 0 0.065 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.481 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_absorpt_correction_T_min 0.1634 _exptl_absorpt_correction_T_max 0.4781 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_unetI/netI 0.0403 _diffrn_reflns_number 13643 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 4142 _reflns_number_gt 3445 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # 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^)+(0.0397P)^2^+1.0814P] 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 4142 _refine_ls_number_parameters 184 _refine_ls_number_restraints 258 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1691 Friedel Pairs' _refine_ls_abs_structure_Flack 0.057(13) _refine_diff_density_max 1.272 _refine_diff_density_min -1.987 _refine_diff_density_rms 0.4 #----------------------------------------------------------------------------# # 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' 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' I I -0.4742 1.8119 '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 0.1141(7) 0.5790(7) 0.82271(16) 0.0171(15) Uani 1 1 d GU . . C2 C 0.2130(6) 0.6688(7) 0.7986(2) 0.0207(17) Uani 1 1 d GU . . H2 H 0.2968 0.7108 0.8142 0.025 Uiso 1 1 calc R . . C3 C 0.1891(7) 0.6972(7) 0.7515(2) 0.0245(18) Uani 1 1 d GU . . H3 H 0.2567 0.7586 0.735 0.029 Uiso 1 1 calc R . . C4 C 0.0664(8) 0.6358(8) 0.72856(17) 0.0247(19) Uani 1 1 d GU . . H4 H 0.0502 0.6552 0.6964 0.03 Uiso 1 1 calc R . . C5 C -0.0324(7) 0.5460(7) 0.7527(2) 0.026(2) Uani 1 1 d GU . . H5 H -0.1163 0.504 0.7371 0.031 Uiso 1 1 calc R . . C6 C -0.0086(7) 0.5176(7) 0.7998(2) 0.0198(18) Uani 1 1 d GU . . H6 H -0.0761 0.4562 0.8163 0.024 Uiso 1 1 calc R . . C7 C 0.1495(11) 0.5475(10) 0.8732(3) 0.0241(16) Uani 1 1 d DU . . H7 H 0.2469 0.5958 0.8815 0.029 Uiso 1 1 calc R . . C8 C 0.1641(14) 0.3837(10) 0.8830(4) 0.030(3) Uani 1 1 d DU . . H8A H 0.1885 0.3687 0.916 0.044 Uiso 1 1 calc R . . H8B H 0.2447 0.343 0.8636 0.044 Uiso 1 1 calc R . . H8C H 0.0684 0.3355 0.8757 0.044 Uiso 1 1 calc R . . C9 C 0.5607(8) 0.9810(7) 0.82837(15) 0.0178(15) Uani 1 1 d GU . . C10 C 0.6732(7) 0.8877(7) 0.8129(2) 0.0193(17) Uani 1 1 d GU . . H10 H 0.7471 0.8526 0.8341 0.023 Uiso 1 1 calc R . . C11 C 0.6777(7) 0.8457(7) 0.7663(2) 0.0225(18) Uani 1 1 d GU . . H11 H 0.7546 0.7819 0.7557 0.027 Uiso 1 1 calc R . . C12 C 0.5696(8) 0.8970(8) 0.73523(16) 0.0229(19) Uani 1 1 d GU . . H12 H 0.5727 0.8683 0.7034 0.027 Uiso 1 1 calc R . . C13 C 0.4571(7) 0.9903(7) 0.75073(19) 0.0233(19) Uani 1 1 d GU . . H13 H 0.3832 1.0254 0.7295 0.028 Uiso 1 1 calc R . . C14 C 0.4526(7) 1.0323(6) 0.7973(2) 0.0198(17) Uani 1 1 d GU . . H14 H 0.3757 1.0961 0.8079 0.024 Uiso 1 1 calc R . . C15 C 0.5598(11) 1.0340(10) 0.8775(3) 0.0230(16) Uani 1 1 d DU . . H15 H 0.4831 1.1133 0.8795 0.028 Uiso 1 1 calc R . . C16 C 0.7081(10) 1.0944(12) 0.8956(4) 0.025(2) Uani 1 1 d DU . . H16A H 0.6957 1.1252 0.9281 0.037 Uiso 1 1 calc R . . H16B H 0.7382 1.1777 0.8765 0.037 Uiso 1 1 calc R . . H16C H 0.7862 1.0194 0.8938 0.037 Uiso 1 1 calc R . . N1 N 0.0251(10) 0.6083(10) 0.9040(3) 0.024(2) Uani 1 1 d DU . . H1A H 0.0468 0.5894 0.9344 0.035 Uiso 1 1 calc R . . H1B H -0.0644 0.5661 0.8963 0.035 Uiso 1 1 calc R . . H1C H 0.0184 0.7057 0.8997 0.035 Uiso 1 1 calc R . . N2 N 0.5103(11) 0.9156(10) 0.9103(3) 0.020(2) Uani 1 1 d DU . . H2A H 0.4208 0.8783 0.9004 0.03 Uiso 1 1 calc R . . H2B H 0.499 0.9525 0.9395 0.03 Uiso 1 1 calc R . . H2C H 0.5814 0.8443 0.9108 0.03 Uiso 1 1 calc R . . Pb1 Pb 0.10535(3) 0.00664(3) 1.00157(2) 0.01789(10) Uani 1 1 d . . . I1 I 0.12437(10) -0.02841(10) 0.89062(3) 0.0204(2) Uani 1 1 d . . . I2 I -0.20286(5) -0.20271(5) 1.00001(3) 0.02030(13) Uani 1 1 d . . . I3 I -0.08469(5) 0.31917(5) 0.99942(3) 0.02264(14) Uani 1 1 d . . . I4 I 0.11721(10) -0.02747(11) 1.11148(3) 0.0253(2) 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 C1 0.014(4) 0.011(4) 0.026(3) -0.002(2) 0.003(2) -0.001(3) C2 0.020(4) 0.010(4) 0.032(3) -0.002(3) 0.003(3) -0.007(3) C3 0.026(4) 0.010(4) 0.037(3) 0.009(3) 0.002(3) 0.002(3) C4 0.026(4) 0.019(4) 0.029(4) 0.003(3) 0.000(3) 0.009(3) C5 0.024(4) 0.021(4) 0.033(3) -0.004(3) -0.004(3) -0.001(3) C6 0.016(4) 0.009(4) 0.035(3) 0.002(3) -0.001(3) -0.004(3) C7 0.023(4) 0.020(3) 0.030(3) 0.005(3) -0.001(3) 0.000(3) C8 0.037(6) 0.017(4) 0.034(5) 0.000(3) -0.007(5) 0.003(4) C9 0.019(4) 0.009(4) 0.025(2) 0.004(2) 0.005(2) 0.006(3) C10 0.020(4) 0.008(4) 0.030(3) 0.002(3) 0.000(3) 0.007(3) C11 0.025(4) 0.009(4) 0.033(3) -0.005(3) 0.007(3) -0.001(3) C12 0.034(4) 0.012(4) 0.023(3) -0.001(3) 0.004(3) -0.007(3) C13 0.026(4) 0.015(4) 0.029(3) 0.005(3) -0.003(3) -0.003(3) C14 0.018(4) 0.011(4) 0.030(3) 0.004(3) 0.002(3) 0.006(3) C15 0.027(4) 0.014(4) 0.028(3) -0.003(3) 0.002(3) 0.000(3) C16 0.015(4) 0.030(5) 0.029(5) -0.002(4) 0.004(4) 0.007(3) N1 0.032(5) 0.015(4) 0.023(4) -0.005(4) -0.001(3) -0.004(3) N2 0.021(4) 0.019(4) 0.021(3) -0.001(3) 0.003(4) 0.008(3) Pb1 0.01776(18) 0.01757(17) 0.01833(18) -0.0007(3) 0.0010(3) -0.00067(10) I1 0.0209(5) 0.0187(5) 0.0214(4) 0.0004(4) 0.0003(4) 0.0008(4) I2 0.0183(3) 0.0181(3) 0.0245(3) 0.0019(6) -0.0011(5) -0.00320(18) I3 0.0199(3) 0.0197(3) 0.0284(3) -0.0026(5) -0.0029(5) 0.00568(19) I4 0.0235(6) 0.0318(6) 0.0205(4) -0.0016(4) 0.0018(4) -0.0016(5) #----------------------------------------------------------------------------# # 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 C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C7 1.508(11) . ? C2 C3 1.39 . ? C2 H2 0.95 . ? C3 C4 1.39 . ? C3 H3 0.95 . ? C4 C5 1.39 . ? C4 H4 0.95 . ? C5 C6 1.39 . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 N1 1.519(10) . ? C7 C8 1.543(10) . ? C7 H7 1 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 C10 1.39 . ? C9 C14 1.39 . ? C9 C15 1.491(10) . ? C10 C11 1.39 . ? C10 H10 0.95 . ? C11 C12 1.39 . ? C11 H11 0.95 . ? C12 C13 1.39 . ? C12 H12 0.95 . ? C13 C14 1.39 . ? C13 H13 0.95 . ? C14 H14 0.95 . ? C15 N2 1.506(9) . ? C15 C16 1.518(10) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N2 H2C 0.91 . ? Pb1 I4 3.1665(13) . ? Pb1 I3 3.1807(7) 4_557 ? Pb1 I1 3.1994(13) . ? Pb1 I2 3.2797(7) 4_547 ? Pb1 I3 3.3403(7) . ? Pb1 I2 3.3439(7) . ? I2 Pb1 3.2797(7) 4_447 ? I3 Pb1 3.1807(7) 4_457 ? 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 C2 C1 C6 120 . . ? C2 C1 C7 117.5(6) . . ? C6 C1 C7 122.5(6) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C6 C5 C4 120 . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C1 C7 N1 109.6(7) . . ? C1 C7 C8 112.4(8) . . ? N1 C7 C8 108.5(9) . . ? C1 C7 H7 108.8 . . ? N1 C7 H7 108.8 . . ? C8 C7 H7 108.8 . . ? 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 C14 120 . . ? C10 C9 C15 120.6(6) . . ? C14 C9 C15 119.3(5) . . ? C9 C10 C11 120 . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C12 C11 C10 120 . . ? C12 C11 H11 120 . . ? C10 C11 H11 120 . . ? C13 C12 C11 120 . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C12 C13 C14 120 . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C13 C14 C9 120 . . ? C13 C14 H14 120 . . ? C9 C14 H14 120 . . ? C9 C15 N2 110.6(7) . . ? C9 C15 C16 116.0(8) . . ? N2 C15 C16 107.8(8) . . ? C9 C15 H15 107.4 . . ? N2 C15 H15 107.4 . . ? C16 C15 H15 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7 N1 H1A 109.5 . . ? C7 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C7 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C15 N2 H2A 109.5 . . ? C15 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C15 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? I4 Pb1 I3 91.75(3) . 4_557 ? I4 Pb1 I1 167.476(17) . . ? I3 Pb1 I1 89.82(3) 4_557 . ? I4 Pb1 I2 84.92(3) . 4_547 ? I3 Pb1 I2 89.180(19) 4_557 4_547 ? I1 Pb1 I2 82.68(3) . 4_547 ? I4 Pb1 I3 96.94(3) . . ? I3 Pb1 I3 89.869(16) 4_557 . ? I1 Pb1 I3 95.49(3) . . ? I2 Pb1 I3 177.93(3) 4_547 . ? I4 Pb1 I2 89.02(3) . . ? I3 Pb1 I2 174.900(17) 4_557 . ? I1 Pb1 I2 88.36(3) . . ? I2 Pb1 I2 85.864(16) 4_547 . ? I3 Pb1 I2 95.04(2) . . ? Pb1 I2 Pb1 156.493(18) 4_447 . ? Pb1 I3 Pb1 150.616(18) 4_457 . ? 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 C6 C1 C2 C3 0 . . . . ? C7 C1 C2 C3 177.6(6) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C3 C4 C5 C6 0 . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? C7 C1 C6 C5 -177.5(7) . . . . ? C2 C1 C7 N1 116.3(7) . . . . ? C6 C1 C7 N1 -66.2(9) . . . . ? C2 C1 C7 C8 -123.0(8) . . . . ? C6 C1 C7 C8 54.5(10) . . . . ? C14 C9 C10 C11 0 . . . . ? C15 C9 C10 C11 -176.3(7) . . . . ? C9 C10 C11 C12 0 . . . . ? C10 C11 C12 C13 0 . . . . ? C11 C12 C13 C14 0 . . . . ? C12 C13 C14 C9 0 . . . . ? C10 C9 C14 C13 0 . . . . ? C15 C9 C14 C13 176.4(7) . . . . ? C10 C9 C15 N2 -74.0(8) . . . . ? C14 C9 C15 N2 109.6(8) . . . . ? C10 C9 C15 C16 49.1(10) . . . . ? C14 C9 C15 C16 -127.2(8) . . . . ? I4 Pb1 I2 Pb1 -84.47(8) . . . 4_447 ? I1 Pb1 I2 Pb1 83.28(8) . . . 4_447 ? I2 Pb1 I2 Pb1 0.51(6) 4_547 . . 4_447 ? I3 Pb1 I2 Pb1 178.64(8) . . . 4_447 ? I4 Pb1 I3 Pb1 -87.93(7) . . . 4_457 ? I3 Pb1 I3 Pb1 -179.68(9) 4_557 . . 4_457 ? I1 Pb1 I3 Pb1 90.51(7) . . . 4_457 ? I2 Pb1 I3 Pb1 1.69(7) . . . 4_457 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.91 3.09 3.758(10) 132 4_557 N1 H1B I4 0.91 2.85 3.714(10) 159.1 4_457 N1 H1C I1 0.91 2.64 3.488(10) 155.4 1_565 N2 H2A I1 0.91 2.78 3.502(10) 137.5 1_565 N2 H2B I3 0.91 2.84 3.660(9) 151 4_567 N2 H2C I4 0.91 3.01 3.757(9) 140.5 4_557 ###END _chemical_name_common bis((S)-beta-phenethylammonium)tetraiodoplumbate(ii)