# Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'David Billing' _publ_contact_author_email DAVE.BILLING@WITS.AC.ZA _publ_section_title ; Effect of heteroatoms in the inorganic-organic layered perovskite-type hybrids [(ZCnH2nNH3)2PbI4], n = 2, 3, 4, 5, 6; Z = OH, Br and I; and [(H3NC2H4S2C2H4NH3)PbI4] ; _publ_requested_category FM loop_ _publ_author_name 'David Billing' 'Andreas Lemmerer' # Attachment 'B917824-revised.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-08-28 at 20:48:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as87l_a smart data_1 _database_code_depnum_ccdc_archive 'CCDC 746124' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-08-28T20:48:49-00:00 _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(2-ethanolammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C4 H16 I4 N2 O2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C2 H8 N O)' _chemical_formula_weight 838.98 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.167(3) _cell_length_b 9.038(3) _cell_length_c 8.930(3) _cell_angle_alpha 90 _cell_angle_beta 100.572(5) _cell_angle_gamma 90 _cell_volume 806.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 977 _cell_measurement_theta_min 2.794 _cell_measurement_theta_max 28.247 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 3.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.11 0 0 -1 0.11 0 -1 0 0.2 0 1 0 0.2 -1 0 0 0.025 1 0 0 0.025 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 18.096 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0232 _exptl_absorpt_correction_T_max 0.3908 _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 0.0665 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_number 6435 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _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 1944 _reflns_number_gt 1855 _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, 1997)' _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^)+(0.0266P)^2^+0.4455P] 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 0.0188(6) _refine_ls_number_reflns 1944 _refine_ls_number_parameters 63 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.025 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.547 _refine_diff_density_min -1.405 _refine_diff_density_rms 0.266 #----------------------------------------------------------------------------# # 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' 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 0.6739(5) 0.4729(6) 0.8639(6) 0.0253(10) Uani 1 1 d . . . H1D H 0.591 0.4189 0.8204 0.03 Uiso 1 1 calc R . . H1E H 0.7431 0.4482 0.8032 0.03 Uiso 1 1 calc R . . C2 C 0.6478(5) 0.6370(6) 0.8576(6) 0.0255(10) Uani 1 1 d . . . H2A H 0.7312 0.6913 0.8988 0.031 Uiso 1 1 calc R . . H2B H 0.617 0.6684 0.7507 0.031 Uiso 1 1 calc R . . N1 N 0.7204(4) 0.4277(5) 1.0264(4) 0.0242(8) Uani 1 1 d . . . H1A H 0.7362 0.3285 1.0309 0.036 Uiso 1 1 calc R . . H1B H 0.6561 0.4501 1.0815 0.036 Uiso 1 1 calc R . . H1C H 0.797 0.477 1.0655 0.036 Uiso 1 1 calc R . . O1 O 0.5476(4) 0.6696(4) 0.9460(4) 0.0277(7) Uani 1 1 d . . . H1 H 0.546 0.7612 0.9618 0.041 Uiso 1 1 calc R . . I1 I 1.31604(3) 0.95653(4) 1.07025(3) 0.02011(11) Uani 1 1 d . . . I2 I 0.97835(3) 0.70738(4) 1.20238(3) 0.02465(11) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.01596(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(2) 0.027(3) 0.020(2) -0.0020(19) 0.0039(19) 0.0033(19) C2 0.023(2) 0.030(3) 0.024(2) 0.0026(19) 0.0042(17) -0.0013(18) N1 0.031(2) 0.022(2) 0.0186(19) 0.0007(15) 0.0012(15) 0.0048(16) O1 0.0312(17) 0.0201(18) 0.0329(18) -0.0024(15) 0.0090(14) 0.0007(14) I1 0.01615(15) 0.02107(18) 0.02272(17) -0.00046(11) 0.00258(11) 0.00022(10) I2 0.02548(17) 0.02457(18) 0.02276(18) 0.00964(11) 0.00142(12) -0.00272(11) Pb1 0.01584(13) 0.01650(15) 0.01525(14) 0.00002(7) 0.00206(8) 0.00075(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 N1 1.498(6) . ? C1 C2 1.506(7) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 O1 1.430(6) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? O1 H1 0.84 . ? I1 Pb1 3.1830(9) . ? I2 Pb1 3.2265(8) 2_747 ? I2 Pb1 3.2334(7) . ? Pb1 I1 3.1830(9) 3_777 ? Pb1 I2 3.2265(8) 4_575 ? Pb1 I2 3.2265(8) 2_757 ? Pb1 I2 3.2334(8) 3_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.1(4) . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? N1 C1 H1E 109.9 . . ? C2 C1 H1E 109.9 . . ? H1D C1 H1E 108.3 . . ? O1 C2 C1 108.7(4) . . ? O1 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O1 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C2 O1 H1 109.5 . . ? Pb1 I2 Pb1 159.099(12) 2_747 . ? I1 Pb1 I1 180 3_777 . ? I1 Pb1 I2 89.743(9) 3_777 4_575 ? I1 Pb1 I2 90.257(9) . 4_575 ? I1 Pb1 I2 90.257(9) 3_777 2_757 ? I1 Pb1 I2 89.743(9) . 2_757 ? I2 Pb1 I2 180 4_575 2_757 ? I1 Pb1 I2 92.370(10) 3_777 . ? I1 Pb1 I2 87.630(10) . . ? I2 Pb1 I2 89.08(2) 4_575 . ? I2 Pb1 I2 90.92(2) 2_757 . ? I1 Pb1 I2 87.630(10) 3_777 3_777 ? I1 Pb1 I2 92.370(10) . 3_777 ? I2 Pb1 I2 90.92(2) 4_575 3_777 ? I2 Pb1 I2 89.08(2) 2_757 3_777 ? I2 Pb1 I2 180 . 3_777 ? 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 N1 C1 C2 O1 -59.6(5) . . . . ? Pb1 I2 Pb1 I1 -107.85(3) 2_747 . . 3_777 ? Pb1 I2 Pb1 I1 72.15(3) 2_747 . . . ? Pb1 I2 Pb1 I2 162.45(2) 2_747 . . 4_575 ? Pb1 I2 Pb1 I2 -17.55(2) 2_747 . . 2_757 ? 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 O1 H1 I1 0.84 2.95 3.665(4) 144 3_777 O1 H1 I1 0.84 3.22 3.802(4) 129 1_455 N1 H1A I1 0.91 2.75 3.581(5) 152 3_767 N1 H1B O1 0.91 2.31 2.916(5) 124 3_667 N1 H1B I1 0.91 3.07 3.697(4) 128 2_747 N1 H1C I2 0.91 2.9 3.772(4) 161 . _chemical_name_common bis(2-ethanolammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-08-28 at 21:06:32 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as103la smart data_2 _database_code_depnum_ccdc_archive 'CCDC 746125' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-08-28T21:06:32-00:00 _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(3-propanolammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C6 H20 I4 N2 O2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C3 H10 N O)' _chemical_formula_weight 867.03 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.631(3) _cell_length_b 9.199(3) _cell_length_c 9.207(3) _cell_angle_alpha 90 _cell_angle_beta 93.057(6) _cell_angle_gamma 90 _cell_volume 899.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 952 _cell_measurement_theta_min 3.839 _cell_measurement_theta_max 28.305 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.02 -1 0 0 0.02 0 0 -1 0.2 0 0 1 0.2 0 1 0 0.22 0 -1 0 0.22 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.239 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0238 _exptl_absorpt_correction_T_max 0.508 _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 0.0926 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_number 6108 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2160 _reflns_number_gt 2047 _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, 1997)' _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^)+(0.0305P)^2^+2.5121P] 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 0.0100(5) _refine_ls_number_reflns 2160 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0807 _refine_ls_wR_factor_gt 0.0798 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.665 _refine_diff_density_min -2.016 _refine_diff_density_rms 0.263 #----------------------------------------------------------------------------# # 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' 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 0.2838(7) -0.0068(6) 0.4586(7) 0.0248(12) Uani 1 1 d . . . H1D H 0.2048 0.0083 0.3986 0.03 Uiso 1 1 calc R . . H1E H 0.3365 -0.0768 0.4074 0.03 Uiso 1 1 calc R . . C2 C 0.3533(6) 0.1365(6) 0.4777(6) 0.0234(11) Uani 1 1 d . . . H2D H 0.4263 0.1234 0.5478 0.028 Uiso 1 1 calc R . . H2E H 0.2965 0.2095 0.5184 0.028 Uiso 1 1 calc R . . C3 C 0.3993(6) 0.1923(6) 0.3340(6) 0.0247(11) Uani 1 1 d . . . H3A H 0.3281 0.1955 0.2603 0.03 Uiso 1 1 calc R . . H3B H 0.4325 0.2923 0.3472 0.03 Uiso 1 1 calc R . . N1 N 0.2541(5) -0.0669(5) 0.6024(6) 0.0262(10) Uani 1 1 d . . . H1A H 0.213 -0.1531 0.5897 0.039 Uiso 1 1 calc R . . H1B H 0.2043 -0.0032 0.6485 0.039 Uiso 1 1 calc R . . H1C H 0.3269 -0.0813 0.6572 0.039 Uiso 1 1 calc R . . O1 O 0.4970(5) 0.0987(6) 0.2840(5) 0.0323(10) Uani 1 1 d . . . H1 H 0.4765 0.0689 0.1998 0.048 Uiso 1 1 calc R . . I1 I -0.29280(3) 0.06314(4) -0.00965(4) 0.02212(13) Uani 1 1 d . . . I2 I 0.02682(4) 0.27906(4) 0.22391(4) 0.02483(14) Uani 1 1 d . . . Pb1 Pb 0 0 0 0.01973(13) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(3) 0.026(3) 0.019(3) 0.0014(19) 0.003(2) 0.000(2) C2 0.032(3) 0.018(2) 0.020(2) -0.0031(19) 0.004(2) 0.001(2) C3 0.028(3) 0.022(2) 0.024(3) 0.000(2) 0.005(2) 0.000(2) N1 0.026(2) 0.023(2) 0.030(2) 0.0024(19) 0.013(2) -0.0017(19) O1 0.030(2) 0.047(3) 0.0202(19) -0.0087(19) 0.0054(18) 0.004(2) I1 0.0223(2) 0.02192(19) 0.02239(19) -0.00022(12) 0.00298(15) -0.00062(13) I2 0.0276(2) 0.0240(2) 0.0234(2) -0.00732(13) 0.00518(15) -0.00196(14) Pb1 0.02125(18) 0.02096(17) 0.01717(16) 0.00055(9) 0.00293(12) 0.00095(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 N1 1.484(8) . ? C1 C2 1.517(8) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.524(8) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? C3 O1 1.443(7) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? O1 H1 0.84 . ? I1 Pb1 3.1632(9) . ? I2 Pb1 3.2788(7) 2 ? I2 Pb1 3.2953(7) . ? Pb1 I1 3.1632(9) 3 ? Pb1 I2 3.2788(7) 4_565 ? Pb1 I2 3.2788(7) 2_545 ? Pb1 I2 3.2953(7) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.2(5) . . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 . . ? N1 C1 H1E 109.6 . . ? C2 C1 H1E 109.6 . . ? H1D C1 H1E 108.1 . . ? C1 C2 C3 111.7(5) . . ? C1 C2 H2D 109.3 . . ? C3 C2 H2D 109.3 . . ? C1 C2 H2E 109.3 . . ? C3 C2 H2E 109.3 . . ? H2D C2 H2E 107.9 . . ? O1 C3 C2 110.2(5) . . ? O1 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? O1 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C3 O1 H1 109.5 . . ? Pb1 I2 Pb1 163.679(13) 2 . ? I1 Pb1 I1 180.000(12) 3 . ? I1 Pb1 I2 90.542(11) 3 4_565 ? I1 Pb1 I2 89.458(11) . 4_565 ? I1 Pb1 I2 89.458(11) 3 2_545 ? I1 Pb1 I2 90.542(11) . 2_545 ? I2 Pb1 I2 180 4_565 2_545 ? I1 Pb1 I2 94.203(11) 3 . ? I1 Pb1 I2 85.797(11) . . ? I2 Pb1 I2 89.65(2) 4_565 . ? I2 Pb1 I2 90.35(2) 2_545 . ? I1 Pb1 I2 85.797(11) 3 3 ? I1 Pb1 I2 94.203(11) . 3 ? I2 Pb1 I2 90.35(2) 4_565 3 ? I2 Pb1 I2 89.65(2) 2_545 3 ? I2 Pb1 I2 180.000(12) . 3 ? 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 N1 C1 C2 C3 173.1(5) . . . . ? C1 C2 C3 O1 -67.8(7) . . . . ? Pb1 I2 Pb1 I1 -121.84(5) 2 . . 3 ? Pb1 I2 Pb1 I1 58.16(5) 2 . . . ? Pb1 I2 Pb1 I2 147.64(4) 2 . . 4_565 ? Pb1 I2 Pb1 I2 -32.36(4) 2 . . 2_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 I1 0.91 2.85 3.538(5) 133 2_545 N1 H1B I2 0.91 2.9 3.793(5) 166 4_566 N1 H1C O1 0.91 1.93 2.808(7) 162 3_656 N1 H1C I1 0.91 3.29 3.750(5) 114 3_556 O1 H1 I1 0.84 2.83 3.567(5) 148 3 O1 H1 I1 0.84 3.2 3.613(4) 113 1_655 _chemical_name_common bis(3-propanolammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-11-23 at 12:55:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as140_p apex data_3 _database_code_depnum_ccdc_archive 'CCDC 746126' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-11-23T12:55:09-00:00 _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(2-iodoethylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C4 H14 I6 N2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C2 H7 I N)' _chemical_formula_weight 1058.76 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5520(9) _cell_length_b 8.7614(6) _cell_length_c 8.6441(6) _cell_angle_alpha 90 _cell_angle_beta 97.994(2) _cell_angle_gamma 90 _cell_volume 941.38(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6365 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description chunk _exptl_crystal_colour yellow _exptl_crystal_size_max 0.626 _exptl_crystal_size_mid 0.395 _exptl_crystal_size_min 0.161 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.081 1 0 0 0.081 1 4 0 0.22 0 0 -1 0.17 2 -3 3 0.18 2 -1 5 0.18 2 1 0 0.16 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 18.775 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0057 _exptl_absorpt_correction_T_max 0.1028 _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 0.0604 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_number 10642 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.64 _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 2274 _reflns_number_gt 2150 _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, 1997)' _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^)+(0.0318P)^2^+1.4999P] 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 2274 _refine_ls_number_parameters 61 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.034 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.155 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.946 _refine_diff_density_min -3.065 _refine_diff_density_rms 0.318 #----------------------------------------------------------------------------# # 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 0.6862(5) 0.5346(8) 0.9254(9) 0.0252(13) Uani 1 1 d U . . H1D H 0.6925 0.5539 1.0391 0.03 Uiso 1 1 calc R . . H1E H 0.6294 0.4568 0.898 0.03 Uiso 1 1 calc R . . C2 C 0.6551(5) 0.6797(8) 0.8380(9) 0.0284(14) Uani 1 1 d U . . H2A H 0.6486 0.6606 0.7242 0.034 Uiso 1 1 calc R . . H2B H 0.7116 0.7576 0.8654 0.034 Uiso 1 1 calc R . . N1 N 0.7905(5) 0.4759(7) 0.8861(8) 0.0304(13) Uani 1 1 d U . . H1A H 0.808 0.3881 0.94 0.046 Uiso 1 1 calc R . . H1B H 0.8428 0.5468 0.9126 0.046 Uiso 1 1 calc R . . H1C H 0.7843 0.4568 0.7818 0.046 Uiso 1 1 calc R . . I1 I 1.24555(3) -0.09196(5) 1.02581(6) 0.02749(13) Uani 1 1 d . . . I2 I 0.94699(3) -0.29955(5) 1.18824(5) 0.02443(12) Uani 1 1 d . . . I3 I 0.50595(3) 0.76187(6) 0.89536(6) 0.03035(13) Uani 1 1 d . . . Pb1 Pb 1 0 1 0.01743(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.026(3) 0.024(3) -0.001(3) 0.005(3) -0.001(2) C2 0.026(3) 0.026(3) 0.036(4) 0.005(3) 0.014(3) 0.001(2) N1 0.032(3) 0.019(3) 0.041(4) 0.001(2) 0.007(3) 0.001(2) I1 0.0195(2) 0.0215(2) 0.0419(3) 0.00427(17) 0.00583(17) 0.00322(15) I2 0.0303(2) 0.0192(2) 0.0241(2) 0.00770(15) 0.00483(17) 0.00024(15) I3 0.0246(2) 0.0336(3) 0.0337(3) 0.00155(19) 0.00704(18) 0.00394(17) Pb1 0.01886(16) 0.01351(16) 0.02047(19) -0.00056(11) 0.00469(12) 0.00094(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 N1 1.489(9) . ? C1 C2 1.502(10) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 I3 2.127(7) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1634(5) . ? I2 Pb1 3.2062(4) . ? I2 Pb1 3.2079(4) 2_747 ? Pb1 I1 3.1634(4) 3_757 ? Pb1 I2 3.2062(4) 3_757 ? Pb1 I2 3.2079(4) 4 ? Pb1 I2 3.2079(4) 2_757 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.7(6) . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? C2 C1 H1E 109.5 . . ? H1D C1 H1E 108.1 . . ? C1 C2 I3 110.2(5) . . ? C1 C2 H2A 109.6 . . ? I3 C2 H2A 109.6 . . ? C1 C2 H2B 109.6 . . ? I3 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 147.251(15) . 2_747 ? I1 Pb1 I1 180.000(18) 3_757 . ? I1 Pb1 I2 88.589(11) 3_757 . ? I1 Pb1 I2 91.411(11) . . ? I1 Pb1 I2 91.411(11) 3_757 3_757 ? I1 Pb1 I2 88.589(11) . 3_757 ? I2 Pb1 I2 180 . 3_757 ? I1 Pb1 I2 89.655(12) 3_757 4 ? I1 Pb1 I2 90.345(12) . 4 ? I2 Pb1 I2 86.834(6) . 4 ? I2 Pb1 I2 93.166(6) 3_757 4 ? I1 Pb1 I2 90.345(12) 3_757 2_757 ? I1 Pb1 I2 89.655(12) . 2_757 ? I2 Pb1 I2 93.166(6) . 2_757 ? I2 Pb1 I2 86.834(6) 3_757 2_757 ? I2 Pb1 I2 180 4 2_757 ? 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 N1 C1 C2 I3 180.0(5) . . . . ? Pb1 I2 Pb1 I1 -124.41(3) 2_747 . . 3_757 ? Pb1 I2 Pb1 I1 55.59(3) 2_747 . . . ? Pb1 I2 Pb1 I2 145.86(2) 2_747 . . 4 ? Pb1 I2 Pb1 I2 -34.14(2) 2_747 . . 2_757 ? 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 I1 0.91 2.71 3.492(6) 145 3_757 N1 H1B I2 0.91 2.89 3.623(7) 139 1_565 N1 H1C I1 0.91 2.67 3.576(7) 177 2_756 _chemical_name_common bis(2-iodoethylammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-10-24 at 17:37:56 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as141_a smart data_4 _database_code_depnum_ccdc_archive 'CCDC 746127' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-10-24T17:37:56-00:00 _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(3-iodopropylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C6 H18 I6 N2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C3 H9 I N)' _chemical_formula_weight 1086.81 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.0739(15) _cell_length_b 9.0379(10) _cell_length_c 8.4723(10) _cell_angle_alpha 90 _cell_angle_beta 99.246(5) _cell_angle_gamma 90 _cell_volume 1063.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 28.19 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rectangle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 3.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.05 1 0 0 0.05 0 0 1 0.11 0 0 -1 0.11 0 -1 0 0.27 0 1 0 0.27 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.622 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0344 _exptl_absorpt_correction_T_max 0.2033 _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 0.062 _diffrn_reflns_av_unetI/netI 0.044 _diffrn_reflns_number 7335 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.47 _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 2571 _reflns_number_gt 2385 _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, 1997)' _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^)+(0.0225P)^2^+0.7466P] 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 0.0084(3) _refine_ls_number_reflns 2571 _refine_ls_number_parameters 71 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.028 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0574 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.326 _refine_diff_density_min -1.04 _refine_diff_density_rms 0.234 #----------------------------------------------------------------------------# # 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 0.7135(4) 0.0048(6) 0.4276(7) 0.0304(11) Uani 1 1 d U . . H1D H 0.6631 0.0666 0.3642 0.036 Uiso 1 1 calc R . . H1E H 0.7101 0.0199 0.5423 0.036 Uiso 1 1 calc R . . C2 C 0.6961(3) -0.1568(6) 0.3845(7) 0.0307(10) Uani 1 1 d U . . H2A H 0.7503 -0.2165 0.4399 0.037 Uiso 1 1 calc R . . H2B H 0.6941 -0.1693 0.2679 0.037 Uiso 1 1 calc R . . C3 C 0.6014(3) -0.2145(7) 0.4305(7) 0.0341(11) Uani 1 1 d U . . H3A H 0.5983 -0.1848 0.5421 0.041 Uiso 1 1 calc R . . H3B H 0.6017 -0.324 0.4267 0.041 Uiso 1 1 calc R . . N1 N 0.8110(3) 0.0505(6) 0.3939(6) 0.0331(10) Uani 1 1 d U . . H1A H 0.8213 0.1476 0.42 0.05 Uiso 1 1 calc R . . H1B H 0.8136 0.0375 0.2882 0.05 Uiso 1 1 calc R . . H1C H 0.8571 -0.0058 0.4532 0.05 Uiso 1 1 calc R . . I1 I 0.77569(2) 0.07020(4) 0.96507(4) 0.03075(10) Uani 1 1 d . . . I2 I 0.95895(2) -0.19976(4) 0.68384(3) 0.02827(10) Uani 1 1 d . . . I3 I 0.47428(2) -0.13452(4) 0.27765(4) 0.03374(11) Uani 1 1 d . . . Pb1 Pb 1 0 1 0.01987(9) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(2) 0.026(3) 0.042(3) -0.003(2) 0.009(2) 0.0003(18) C2 0.025(2) 0.021(2) 0.046(3) -0.003(2) 0.0045(19) -0.0018(18) C3 0.024(2) 0.030(3) 0.048(3) 0.008(2) 0.0030(19) 0.0010(19) N1 0.029(2) 0.026(2) 0.044(2) 0.001(2) 0.0054(18) -0.0053(17) I1 0.02069(15) 0.0269(2) 0.04270(19) 0.00284(14) -0.00078(12) 0.00087(12) I2 0.03115(16) 0.02788(19) 0.02502(15) -0.01010(12) 0.00223(11) 0.00030(13) I3 0.02455(16) 0.0355(2) 0.03949(19) -0.00437(15) 0.00003(12) 0.00479(13) Pb1 0.02076(12) 0.01870(14) 0.01969(12) -0.00044(8) 0.00184(8) 0.00096(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 N1 1.504(6) . ? C1 C2 1.516(7) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.539(7) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 I3 2.158(5) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1869(4) . ? I2 Pb1 3.2049(4) . ? I2 Pb1 3.2268(4) 2_746 ? Pb1 I1 3.1869(4) 3_757 ? Pb1 I2 3.2049(4) 3_757 ? Pb1 I2 3.2268(4) 4_556 ? Pb1 I2 3.2268(4) 2_756 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.7(4) . . ? N1 C1 H1D 109.7 . . ? C2 C1 H1D 109.7 . . ? N1 C1 H1E 109.7 . . ? C2 C1 H1E 109.7 . . ? H1D C1 H1E 108.2 . . ? C1 C2 C3 112.3(4) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C2 C3 I3 113.7(4) . . ? C2 C3 H3A 108.8 . . ? I3 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? I3 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 148.755(11) . 2_746 ? I1 Pb1 I1 180.000(12) . 3_757 ? I1 Pb1 I2 89.523(10) . . ? I1 Pb1 I2 90.477(10) 3_757 . ? I1 Pb1 I2 90.477(10) . 3_757 ? I1 Pb1 I2 89.523(10) 3_757 3_757 ? I2 Pb1 I2 180 . 3_757 ? I1 Pb1 I2 87.749(9) . 4_556 ? I1 Pb1 I2 92.251(9) 3_757 4_556 ? I2 Pb1 I2 84.691(9) . 4_556 ? I2 Pb1 I2 95.309(9) 3_757 4_556 ? I1 Pb1 I2 92.251(9) . 2_756 ? I1 Pb1 I2 87.749(9) 3_757 2_756 ? I2 Pb1 I2 95.309(9) . 2_756 ? I2 Pb1 I2 84.691(9) 3_757 2_756 ? I2 Pb1 I2 180 4_556 2_756 ? 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 N1 C1 C2 C3 174.7(4) . . . . ? C1 C2 C3 I3 73.3(5) . . . . ? Pb1 I2 Pb1 I1 -137.31(2) 2_746 . . . ? Pb1 I2 Pb1 I1 42.69(2) 2_746 . . 3_757 ? Pb1 I2 Pb1 I2 -49.53(3) 2_746 . . 4_556 ? Pb1 I2 Pb1 I2 130.47(3) 2_746 . . 2_756 ? 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 I1 0.91 2.67 3.529(5) 157 4_565 N1 H1B I1 0.91 2.72 3.592(5) 161 1_554 N1 H1C I2 0.91 2.84 3.721(5) 164 . _chemical_name_common bis(3-iodopropylammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-10-18 at 19:40:14 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as135l_a apex data_5 _database_code_depnum_ccdc_archive 'CCDC 746128' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-10-18T19:40:14-00:00 _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(4-iodobutylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C8 H22 I6 N2 Pb' _chemical_formula_moiety '2(C4 H11 I N), I4 Pb' _chemical_formula_weight 1114.87 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3677(8) _cell_length_b 8.2431(4) _cell_length_c 9.0441(4) _cell_angle_alpha 90 _cell_angle_beta 91.905(1) _cell_angle_gamma 90 _cell_volume 1145.05(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7509 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.31 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.515 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.032 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.02 -1 0 0 0.02 0 1 -1 0.125 0 -1 1 0.13 0 0 1 0.22 1 -3 -1 0.255 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.445 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0318 _exptl_absorpt_correction_T_max 0.528 _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 0.0596 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_number 12811 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.33 _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 2756 _reflns_number_gt 2554 _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, 1997)' _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^)+(0.0378P)^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 2756 _refine_ls_number_parameters 79 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.235 _refine_diff_density_min -1.627 _refine_diff_density_rms 0.293 #----------------------------------------------------------------------------# # 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 0.2589(4) 0.9365(8) 0.4505(7) 0.0338(13) Uani 1 1 d U . . H1D H 0.2557 0.8212 0.4203 0.041 Uiso 1 1 calc R . . H1E H 0.301 0.9916 0.3868 0.041 Uiso 1 1 calc R . . C2 C 0.2907(4) 0.9467(7) 0.6077(6) 0.0274(11) Uani 1 1 d U . . H2A H 0.2549 0.8747 0.6687 0.033 Uiso 1 1 calc R . . H2B H 0.2832 1.0592 0.6435 0.033 Uiso 1 1 calc R . . C3 C 0.3863(4) 0.8984(8) 0.6279(6) 0.0302(11) Uani 1 1 d U . . H3A H 0.3941 0.7856 0.5932 0.036 Uiso 1 1 calc R . . H3B H 0.4224 0.9703 0.5673 0.036 Uiso 1 1 calc R . . C4 C 0.4157(4) 0.9110(8) 0.7872(7) 0.0344(13) Uani 1 1 d U . . H4A H 0.3851 0.8278 0.8449 0.041 Uiso 1 1 calc R . . H4B H 0.3991 1.0188 0.8255 0.041 Uiso 1 1 calc R . . N1 N 0.1711(3) 1.0127(6) 0.4269(6) 0.0284(10) Uani 1 1 d U . . H1A H 0.1536 1.0023 0.3302 0.043 Uiso 1 1 calc R . . H1B H 0.1741 1.1197 0.4511 0.043 Uiso 1 1 calc R . . H1C H 0.1321 0.9623 0.4849 0.043 Uiso 1 1 calc R . . I1 I -0.20344(2) 0.57028(4) 0.46381(4) 0.02572(10) Uani 1 1 d . . . I2 I -0.03774(2) 0.18822(4) 0.30027(4) 0.02342(10) Uani 1 1 d . . . I3 I 0.55370(2) 0.87916(5) 0.82077(4) 0.03374(11) Uani 1 1 d . . . Pb1 Pb 0 0.5 0.5 0.01676(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(3) 0.049(3) 0.027(3) -0.003(2) -0.003(2) 0.010(2) C2 0.021(2) 0.037(3) 0.024(2) 0.003(2) -0.0037(19) 0.000(2) C3 0.024(3) 0.037(3) 0.029(3) 0.001(2) -0.006(2) 0.005(2) C4 0.018(3) 0.059(4) 0.026(3) 0.005(3) -0.004(2) -0.002(3) N1 0.024(2) 0.031(2) 0.029(3) 0.0032(18) -0.007(2) -0.0014(18) I1 0.01704(17) 0.03223(19) 0.02770(19) -0.00241(13) -0.00209(14) 0.00243(13) I2 0.02648(18) 0.02175(16) 0.02201(17) -0.00819(11) 0.00049(13) -0.00041(12) I3 0.02195(19) 0.0432(2) 0.0355(2) 0.00119(16) -0.00671(15) 0.00211(15) Pb1 0.01687(14) 0.01752(13) 0.01571(14) 0.00018(8) -0.00203(10) -0.00011(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 1.491(8) . ? C1 N1 1.497(7) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.526(8) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.499(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 I3 2.148(6) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1857(4) . ? I2 Pb1 3.1835(3) . ? I2 Pb1 3.1974(3) 2_545 ? Pb1 I2 3.1835(3) 3_566 ? Pb1 I1 3.1857(4) 3_566 ? Pb1 I2 3.1974(3) 4_566 ? Pb1 I2 3.1974(3) 2 ? 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 N1 112.2(5) . . ? C2 C1 H1D 109.2 . . ? N1 C1 H1D 109.2 . . ? C2 C1 H1E 109.2 . . ? N1 C1 H1E 109.2 . . ? H1D C1 H1E 107.9 . . ? C1 C2 C3 112.6(5) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 110.8(5) . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C3 C4 I3 113.1(4) . . ? C3 C4 H4A 109 . . ? I3 C4 H4A 109 . . ? C3 C4 H4B 109 . . ? I3 C4 H4B 109 . . ? H4A C4 H4B 107.8 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 147.024(12) . 2_545 ? I2 Pb1 I2 180 . 3_566 ? I2 Pb1 I1 85.919(9) . . ? I2 Pb1 I1 94.081(9) 3_566 . ? I2 Pb1 I1 94.081(9) . 3_566 ? I2 Pb1 I1 85.919(9) 3_566 3_566 ? I1 Pb1 I1 180.000(12) . 3_566 ? I2 Pb1 I2 93.177(5) . 4_566 ? I2 Pb1 I2 86.823(5) 3_566 4_566 ? I1 Pb1 I2 88.303(9) . 4_566 ? I1 Pb1 I2 91.697(9) 3_566 4_566 ? I2 Pb1 I2 86.823(5) . 2 ? I2 Pb1 I2 93.177(5) 3_566 2 ? I1 Pb1 I2 91.697(9) . 2 ? I1 Pb1 I2 88.303(9) 3_566 2 ? I2 Pb1 I2 180 4_566 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 N1 C1 C2 C3 -169.4(5) . . . . ? C1 C2 C3 C4 179.8(5) . . . . ? C2 C3 C4 I3 -171.5(4) . . . . ? Pb1 I2 Pb1 I1 119.31(2) 2_545 . . . ? Pb1 I2 Pb1 I1 -60.69(2) 2_545 . . 3_566 ? Pb1 I2 Pb1 I2 -152.621(17) 2_545 . . 4_566 ? Pb1 I2 Pb1 I2 27.379(17) 2_545 . . 2 ? 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 I1 0.91 2.85 3.616(5) 143 2 N1 H1B I1 0.91 2.7 3.607(5) 173 3_576 N1 H1C I2 0.91 2.76 3.656(5) 170 3_566 _chemical_name_common bis(4-iodobutylammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-23 at 15:00:52 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as112l_a apex data_6 _database_code_depnum_ccdc_archive 'CCDC 746129' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2006-11-23T15:00:52-00:00 _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(5-iodopentylammonium)tetraiodoplumbate(II) ; _chemical_formula_moiety '2(C5 H13 I N), I4 Pb' _chemical_formula_sum 'C10 H26 I6 N2 Pb' _chemical_formula_weight 1142.92 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.2583(11) _cell_length_b 8.9028(5) _cell_length_c 8.6261(6) _cell_angle_alpha 90 _cell_angle_beta 90.071(4) _cell_angle_gamma 90 _cell_volume 1248.58(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4605 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.23 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.016 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.04 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.008 -1 0 0 0.008 0 1 0 0.07 0 -1 0 0.07 0 0 -1 0.1 0 0 1 0.1 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.168 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1541 _exptl_absorpt_correction_T_max 0.7934 _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 0.0707 _diffrn_reflns_av_unetI/netI 0.0555 _diffrn_reflns_number 12289 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.25 _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 3017 _reflns_number_gt 2751 _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, 1997)' _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^)+(0.0582P)^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 3017 _refine_ls_number_parameters 89 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.087 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.325 _refine_diff_density_min -3.521 _refine_diff_density_rms 0.394 #----------------------------------------------------------------------------# # 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 0.1997(7) 1.0432(14) 0.5258(15) 0.032(2) Uani 1 1 d U . . H1D H 0.1712 1.0489 0.627 0.038 Uiso 1 1 calc R . . H1E H 0.1933 1.1415 0.4736 0.038 Uiso 1 1 calc R . . C2 C 0.2888(8) 1.0130(13) 0.5522(17) 0.033(2) Uani 1 1 d U . . H2A H 0.3169 1.0089 0.4506 0.04 Uiso 1 1 calc R . . H2B H 0.2947 0.9132 0.6017 0.04 Uiso 1 1 calc R . . C3 C 0.3312(7) 1.1291(13) 0.6527(16) 0.031(2) Uani 1 1 d U . . H3A H 0.2998 1.142 0.7501 0.037 Uiso 1 1 calc R . . H3B H 0.3318 1.2267 0.5979 0.037 Uiso 1 1 calc R . . C4 C 0.4190(8) 1.0832(14) 0.6913(17) 0.034(3) Uani 1 1 d U . . H4A H 0.4187 0.9813 0.7372 0.041 Uiso 1 1 calc R . . H4B H 0.4516 1.0791 0.5945 0.041 Uiso 1 1 calc R . . C5 C 0.4594(8) 1.1900(14) 0.802(2) 0.038(3) Uani 1 1 d U . . H5A H 0.4259 1.1957 0.8981 0.046 Uiso 1 1 calc R . . H5B H 0.4605 1.2914 0.7555 0.046 Uiso 1 1 calc R . . N1 N 0.1606(7) 0.9252(11) 0.4299(13) 0.034(2) Uani 1 1 d U . . H1A H 0.106 0.9455 0.4193 0.051 Uiso 1 1 calc R . . H1B H 0.1671 0.8344 0.4767 0.051 Uiso 1 1 calc R . . H1C H 0.1846 0.9233 0.3347 0.051 Uiso 1 1 calc R . . I1 I 0.19612(5) 0.96908(8) 0.01775(10) 0.02803(18) Uani 1 1 d . . . I2 I -0.00337(5) 0.80542(7) -0.30808(8) 0.02812(17) Uani 1 1 d . . . Pb1 Pb 0 1 0 0.01753(12) Uani 1 2 d S . . I3 I 0.58244(5) 1.12630(9) 0.86322(12) 0.0360(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 0.028(4) 0.040(5) 0.027(6) -0.003(5) -0.004(5) 0.003(4) C2 0.029(5) 0.035(5) 0.035(6) -0.002(4) -0.004(5) 0.006(4) C3 0.027(4) 0.031(5) 0.036(6) 0.004(4) -0.001(4) -0.005(4) C4 0.034(5) 0.032(5) 0.036(6) -0.005(5) -0.008(5) 0.003(4) C5 0.029(6) 0.026(5) 0.059(8) -0.009(5) -0.011(6) 0.001(5) N1 0.036(5) 0.030(5) 0.036(6) 0.002(4) -0.002(4) -0.003(4) I1 0.0189(3) 0.0303(3) 0.0350(5) 0.0013(3) -0.0004(4) -0.0023(2) I2 0.0376(4) 0.0217(3) 0.0251(3) -0.0092(3) -0.0021(5) 0.0053(3) Pb1 0.0185(2) 0.0142(2) 0.0198(3) -0.00026(19) -0.0004(4) 0.00040(18) I3 0.0249(4) 0.0289(4) 0.0541(5) 0.0026(3) -0.0074(4) -0.0024(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.480(16) . ? C1 C2 1.491(17) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.514(17) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.522(17) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.501(18) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 I3 2.144(12) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.2038(8) . ? I2 Pb1 3.1727(7) . ? I2 Pb1 3.1839(6) 2_544 ? Pb1 I2 3.1727(7) 3_575 ? Pb1 I2 3.1839(6) 4_576 ? Pb1 I2 3.1839(6) 2_554 ? Pb1 I1 3.2038(8) 3_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.0(10) . . ? N1 C1 H1D 109.2 . . ? C2 C1 H1D 109.2 . . ? N1 C1 H1E 109.2 . . ? C2 C1 H1E 109.2 . . ? H1D C1 H1E 107.9 . . ? C1 C2 C3 114.0(10) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 111.6(11) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108 . . ? C5 C4 C3 112.3(11) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C4 C5 I3 113.3(9) . . ? C4 C5 H5A 108.9 . . ? I3 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? I3 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 154.36(3) . 2_544 ? I2 Pb1 I2 180.000(14) . 3_575 ? I2 Pb1 I2 88.221(7) . 4_576 ? I2 Pb1 I2 91.779(7) 3_575 4_576 ? I2 Pb1 I2 91.779(7) . 2_554 ? I2 Pb1 I2 88.221(7) 3_575 2_554 ? I2 Pb1 I2 180.00(2) 4_576 2_554 ? I2 Pb1 I1 89.47(2) . 3_575 ? I2 Pb1 I1 90.53(2) 3_575 3_575 ? I2 Pb1 I1 94.62(2) 4_576 3_575 ? I2 Pb1 I1 85.38(2) 2_554 3_575 ? I2 Pb1 I1 90.53(2) . . ? I2 Pb1 I1 89.47(2) 3_575 . ? I2 Pb1 I1 85.38(2) 4_576 . ? I2 Pb1 I1 94.62(2) 2_554 . ? I1 Pb1 I1 180 3_575 . ? 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 N1 C1 C2 C3 -178.8(11) . . . . ? C1 C2 C3 C4 173.3(11) . . . . ? C2 C3 C4 C5 -174.8(12) . . . . ? C3 C4 C5 I3 178.8(9) . . . . ? Pb1 I2 Pb1 I2 -5.29(8) 2_544 . . 4_576 ? Pb1 I2 Pb1 I2 174.71(8) 2_544 . . 2_554 ? Pb1 I2 Pb1 I1 -99.93(7) 2_544 . . 3_575 ? Pb1 I2 Pb1 I1 80.07(7) 2_544 . . . ? 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 2.94 3.658(11) 137 3_575 N1 H1B I1 0.91 2.77 3.637(10) 161 4_576 N1 H1C I1 0.91 2.77 3.623(11) 157 . _chemical_name_common bis(5-iodopentylammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-11-23 at 15:07:11 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as111_a smart data_7 _database_code_depnum_ccdc_archive 'CCDC 746130' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2006-11-23T15:07:11-00:00 _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 ; bis(6-iodohexylammonium)tetraiodoplumbste(II) ; _chemical_formula_moiety '2(C6 H15 I N), I4 Pb' _chemical_formula_sum 'C12 H30 I6 N2 Pb' _chemical_formula_weight 1170.97 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _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' '-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 9.2206(4) _cell_length_b 8.8513(4) _cell_length_c 31.9795(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2610.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8222 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 28.22 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.98 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.02 0 0 -1 0.02 -1 0 0 0.14 -3 1 0 0.13 4 -1 -1 0.14 3 2 -2 0.14 0 -1 0 0.175 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.56 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0566 _exptl_absorpt_correction_T_max 0.5815 _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 0.0826 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_number 27170 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.27 _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 3145 _reflns_number_gt 2684 _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, 1997)' _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^)+(0.0515P)^2^+2.7128P] 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 3145 _refine_ls_number_parameters 97 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.1032 _refine_ls_wR_factor_gt 0.089 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.498 _refine_diff_density_min -1.558 _refine_diff_density_rms 0.319 #----------------------------------------------------------------------------# # 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 0.0299(10) 0.4437(11) 0.1052(3) 0.050(2) Uani 1 1 d DU . . H1D H 0.034 0.3492 0.0887 0.06 Uiso 1 1 calc R . . H1E H 0.0973 0.4331 0.1291 0.06 Uiso 1 1 calc R . . C2 C -0.1207(8) 0.4656(9) 0.1213(3) 0.0414(18) Uani 1 1 d DU . . H2A H -0.187 0.484 0.0975 0.05 Uiso 1 1 calc R . . H2B H -0.1232 0.5558 0.1396 0.05 Uiso 1 1 calc R . . C3 C -0.1730(9) 0.3299(8) 0.1457(2) 0.0367(16) Uani 1 1 d DU . . H3A H -0.1633 0.2401 0.1274 0.044 Uiso 1 1 calc R . . H3B H -0.2778 0.3438 0.1512 0.044 Uiso 1 1 calc R . . C4 C -0.0996(8) 0.2945(8) 0.1868(2) 0.0363(16) Uani 1 1 d DU . . H4A H -0.1083 0.3826 0.2057 0.044 Uiso 1 1 calc R . . H4B H 0.0048 0.2755 0.1819 0.044 Uiso 1 1 calc R . . C5 C -0.1678(9) 0.1563(10) 0.2074(3) 0.044(2) Uani 1 1 d DU . . H5A H -0.2703 0.1798 0.214 0.053 Uiso 1 1 calc R . . H5B H -0.1675 0.0722 0.187 0.053 Uiso 1 1 calc R . . C6 C -0.0940(11) 0.1034(10) 0.2470(3) 0.048(2) Uani 1 1 d DU . . H6A H 0.0111 0.0914 0.2416 0.057 Uiso 1 1 calc R . . H6B H -0.1333 0.0033 0.255 0.057 Uiso 1 1 calc R . . N1 N 0.0785(7) 0.5742(8) 0.0781(2) 0.0396(16) Uani 1 1 d U . . H1A H 0.0175 0.5835 0.0559 0.059 Uiso 1 1 calc R . . H1B H 0.1702 0.5568 0.0688 0.059 Uiso 1 1 calc R . . H1C H 0.0769 0.661 0.0934 0.059 Uiso 1 1 calc R . . I1 I -0.05544(5) 0.01952(5) -0.097756(16) 0.03023(14) Uani 1 1 d . . . I2 I -0.28654(5) 0.21169(6) 0.007530(18) 0.03223(15) Uani 1 1 d . . . I3 I -0.12523(6) 0.26182(7) 0.299162(19) 0.04622(17) Uani 1 1 d . . . Pb1 Pb 0 0 0 0.02057(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.062(5) 0.031(4) 0.056(6) 0.004(4) 0.030(4) 0.002(4) C2 0.044(4) 0.033(4) 0.047(5) 0.002(3) 0.005(3) -0.005(3) C3 0.044(4) 0.028(4) 0.038(4) -0.003(3) 0.009(3) -0.002(3) C4 0.027(3) 0.036(4) 0.046(4) 0.002(3) 0.004(3) -0.005(3) C5 0.039(4) 0.042(5) 0.052(5) 0.009(3) -0.013(4) -0.013(4) C6 0.058(5) 0.041(5) 0.044(5) 0.002(4) -0.013(4) 0.005(4) N1 0.035(3) 0.031(4) 0.053(5) 0.005(3) 0.013(3) 0.005(3) I1 0.0346(3) 0.0279(3) 0.0281(3) -0.00040(19) 0.0038(2) 0.00058(18) I2 0.0277(2) 0.0248(3) 0.0442(3) 0.0048(2) 0.0072(2) 0.01132(18) I3 0.0413(3) 0.0564(4) 0.0409(3) -0.0037(3) -0.0001(2) 0.0026(3) Pb1 0.01783(18) 0.01673(19) 0.0272(2) -0.00008(14) -0.00032(13) -0.00009(11) #----------------------------------------------------------------------------# # 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 1.494(7) . ? C1 N1 1.511(11) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.510(7) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.512(7) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.526(7) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.512(7) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 I3 2.198(9) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1724(5) . ? I2 Pb1 3.2317(5) 3_455 ? I2 Pb1 3.2480(4) . ? Pb1 I1 3.1724(5) 5 ? Pb1 I2 3.2317(5) 3 ? Pb1 I2 3.2317(5) 7 ? Pb1 I2 3.2480(4) 5 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 112.0(7) . . ? C2 C1 H1D 109.2 . . ? N1 C1 H1D 109.2 . . ? C2 C1 H1E 109.2 . . ? N1 C1 H1E 109.2 . . ? H1D C1 H1E 107.9 . . ? C1 C2 C3 111.8(7) . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C2 C3 C4 118.0(7) . . ? C2 C3 H3A 107.8 . . ? C4 C3 H3A 107.8 . . ? C2 C3 H3B 107.8 . . ? C4 C3 H3B 107.8 . . ? H3A C3 H3B 107.1 . . ? C3 C4 C5 111.0(6) . . ? C3 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108 . . ? C6 C5 C4 115.2(7) . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C5 C6 I3 112.2(6) . . ? C5 C6 H6A 109.2 . . ? I3 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? I3 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 160.984(18) 3_455 . ? I1 Pb1 I1 180.000(17) . 5 ? I1 Pb1 I2 88.951(13) . 3 ? I1 Pb1 I2 91.049(13) 5 3 ? I1 Pb1 I2 91.049(13) . 7 ? I1 Pb1 I2 88.951(13) 5 7 ? I2 Pb1 I2 180.000(11) 3 7 ? I1 Pb1 I2 95.132(13) . 5 ? I1 Pb1 I2 84.868(13) 5 5 ? I2 Pb1 I2 87.398(4) 3 5 ? I2 Pb1 I2 92.602(4) 7 5 ? I1 Pb1 I2 84.868(13) . . ? I1 Pb1 I2 95.132(13) 5 . ? I2 Pb1 I2 92.602(4) 3 . ? I2 Pb1 I2 87.398(4) 7 . ? I2 Pb1 I2 180.00(2) 5 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 175.7(8) . . . . ? C1 C2 C3 C4 67.2(11) . . . . ? C2 C3 C4 C5 178.9(7) . . . . ? C3 C4 C5 C6 175.0(8) . . . . ? C4 C5 C6 I3 69.7(9) . . . . ? Pb1 I2 Pb1 I1 -66.38(6) 3_455 . . . ? Pb1 I2 Pb1 I1 113.62(6) 3_455 . . 5 ? Pb1 I2 Pb1 I2 22.33(5) 3_455 . . 3 ? Pb1 I2 Pb1 I2 -157.67(5) 3_455 . . 7 ? 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 2.87 3.718(7) 156 7_565 N1 H1B I1 0.91 2.78 3.532(7) 141 3 N1 H1C I1 0.91 2.84 3.656(7) 150 5_565 _chemical_name_common bis(6-iodohexylammonium)tetraiodoplumbste(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-08-28 at 21:22:31 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as107l_a smart data_8 _database_code_depnum_ccdc_archive 'CCDC 746131' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-08-28T21:22:31-00:00 _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(2-bromoethylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C4 H14 Br2 I4 N2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C2 H7 Br N)' _chemical_formula_weight 964.78 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.8543(7) _cell_length_b 20.7714(13) _cell_length_c 6.4866(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1731.93(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3519 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 28.2 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description triangle _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.7 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.01 0 -1 0 0.01 -2 0 1 0.14 1 0 0 0.185 -2 -1 -4 0.19 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 21.459 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0302 _exptl_absorpt_correction_T_max 0.6466 _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 0.0717 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_number 8051 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2152 _reflns_number_gt 1855 _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, 1997)' _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^)+(0.0682P)^2^+60.3506P] 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 2152 _refine_ls_number_parameters 64 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1485 _refine_ls_wR_factor_gt 0.143 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.876 _refine_diff_density_min -3.079 _refine_diff_density_rms 0.506 #----------------------------------------------------------------------------# # 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' 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 0.8209(12) 0.6249(8) 0.212(2) 0.028(3) Uani 1 1 d . . . H1D H 0.7847 0.6263 0.0777 0.034 Uiso 1 1 calc R . . H1E H 0.8468 0.6686 0.244 0.034 Uiso 1 1 calc R . . C2 C 0.7435(12) 0.6025(7) 0.384(2) 0.024(3) Uani 1 1 d . . . H2A H 0.6904 0.6362 0.4068 0.029 Uiso 1 1 calc R . . H2B H 0.7819 0.5962 0.5151 0.029 Uiso 1 1 calc R . . N1 N 0.9111(9) 0.5783(7) 0.2015(17) 0.026(3) Uani 1 1 d . . . H1B H 0.9574 0.5921 0.1051 0.038 Uiso 1 1 calc R . . H1C H 0.8872 0.5386 0.1662 0.038 Uiso 1 1 calc R . . H1A H 0.9429 0.5763 0.3266 0.038 Uiso 1 1 calc R . . Br1 Br 0.67491(11) 0.52186(7) 0.30668(19) 0.0207(3) Uani 1 1 d . . . I1 I 0.46642(7) 0.40322(4) 0.20246(12) 0.0188(2) Uani 1 1 d . . . I2 I 0.45115(9) 0.25 -0.27201(17) 0.0181(3) Uani 1 2 d S . . I3 I 0.70295(9) 0.25 0.23702(19) 0.0204(3) Uani 1 2 d S . . Pb1 Pb 0.46061(5) 0.25 0.21904(9) 0.0126(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.019(7) 0.026(8) 0.040(8) 0.003(6) -0.002(6) 0.008(6) C2 0.032(8) 0.013(6) 0.028(7) -0.005(5) -0.006(6) 0.001(6) N1 0.016(6) 0.041(8) 0.020(6) -0.007(5) 0.001(4) -0.005(6) Br1 0.0206(7) 0.0222(7) 0.0192(6) 0.0005(5) 0.0014(5) -0.0037(6) I1 0.0257(5) 0.0130(4) 0.0177(4) 0.0000(3) 0.0021(3) 0.0007(3) I2 0.0201(6) 0.0226(6) 0.0115(5) 0 -0.0014(4) 0 I3 0.0105(5) 0.0239(7) 0.0267(6) 0 0.0008(5) 0 Pb1 0.0127(3) 0.0121(3) 0.0131(3) 0 0.0003(2) 0 #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.51(2) . ? C1 C2 1.56(2) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 Br1 1.958(14) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N1 H1A 0.91 . ? I1 Pb1 3.1853(9) . ? I2 Pb1 3.1876(13) . ? I2 Pb1 3.3036(13) 1_554 ? I3 Pb1 3.1172(13) . ? I3 Pb1 3.3243(13) 6_656 ? Pb1 I1 3.1853(9) 7_565 ? Pb1 I2 3.3036(13) 1_556 ? Pb1 I3 3.3243(13) 6_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 N1 C1 C2 109.3(12) . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? N1 C1 H1E 109.8 . . ? C2 C1 H1E 109.8 . . ? H1D C1 H1E 108.3 . . ? C1 C2 Br1 110.9(10) . . ? C1 C2 H2A 109.5 . . ? Br1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? Br1 C2 H2B 109.5 . . ? H2A C2 H2B 108 . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C1 N1 H1A 109.5 . . ? H1B N1 H1A 109.5 . . ? H1C N1 H1A 109.5 . . ? Pb1 I2 Pb1 175.70(5) . 1_554 ? Pb1 I3 Pb1 177.23(4) . 6_656 ? I3 Pb1 I1 88.73(2) . . ? I3 Pb1 I1 88.73(2) . 7_565 ? I1 Pb1 I1 175.29(4) . 7_565 ? I3 Pb1 I2 94.33(4) . . ? I1 Pb1 I2 88.119(18) . . ? I1 Pb1 I2 88.118(18) 7_565 . ? I3 Pb1 I2 89.97(3) . 1_556 ? I1 Pb1 I2 91.982(18) . 1_556 ? I1 Pb1 I2 91.982(18) 7_565 1_556 ? I2 Pb1 I2 175.70(5) . 1_556 ? I3 Pb1 I3 172.94(2) . 6_556 ? I1 Pb1 I3 91.50(2) . 6_556 ? I1 Pb1 I3 91.50(2) 7_565 6_556 ? I2 Pb1 I3 92.73(3) . 6_556 ? I2 Pb1 I3 82.97(3) 1_556 6_556 ? 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 N1 C1 C2 Br1 -67.9(13) . . . . ? 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 H1B I1 0.91 2.79 3.620(11) 152 2_664 N1 H1C Br1 0.91 2.77 3.480(12) 136 2_664 N1 H1C Br1 0.91 2.9 3.325(12) 110 . N1 H1C I1 0.91 3.11 3.758(15) 130 6_656 N1 H1A I1 0.91 2.74 3.631(11) 168 2_665 _chemical_name_common bis(2-bromoethylammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-08-16 at 16:50:03 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as89l_a smart data_9 _database_code_depnum_ccdc_archive 'CCDC 746132' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-08-16T16:50:03-00:00 _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 ; (2,2'-dithiodiethanammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C8 H28 I8 N4 Pb2 S4' _chemical_formula_moiety 'I8 Pb2, 2(C4 H14 N2 S2)' _chemical_formula_weight 1738.16 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.795(1) _cell_length_b 8.5195(7) _cell_length_c 23.1666(15) _cell_angle_alpha 90 _cell_angle_beta 98.719(5) _cell_angle_gamma 90 _cell_volume 3471.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 995 _cell_measurement_theta_min 3.33 _cell_measurement_theta_max 28.221 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 3.326 _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 0 0 1 0.015 0 0 -1 0.015 1 0 0 0.09 -1 0 0 0.09 0 1 0 0.11 0 -1 0 0.11 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 17.048 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0573 _exptl_absorpt_correction_T_max 0.6022 _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 0.0812 _diffrn_reflns_av_unetI/netI 0.0557 _diffrn_reflns_number 41777 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.35 _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 8376 _reflns_number_gt 6373 _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, 1997)' _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^)+(0.0259P)^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 8376 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0663 _refine_ls_goodness_of_fit_ref 1.02 _refine_ls_restrained_S_all 1.02 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.936 _refine_diff_density_min -2.926 _refine_diff_density_rms 0.326 #----------------------------------------------------------------------------# # 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' S S 0.1246 0.1234 '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 0.3872(4) 0.8431(10) 0.8779(4) 0.034(2) Uani 1 1 d . . . H1D H 0.3371 0.7948 0.8801 0.041 Uiso 1 1 calc R . . H1E H 0.3787 0.9384 0.8534 0.041 Uiso 1 1 calc R . . C2 C 0.4256(5) 0.8890(9) 0.9398(4) 0.033(2) Uani 1 1 d . . . H2D H 0.3909 0.9592 0.9573 0.039 Uiso 1 1 calc R . . H2E H 0.4724 0.9491 0.9365 0.039 Uiso 1 1 calc R . . C3 C 0.3072(4) 0.7614(9) 1.0415(3) 0.0248(17) Uani 1 1 d . . . H3D H 0.3146 0.8698 1.0281 0.03 Uiso 1 1 calc R . . H3E H 0.2518 0.7427 1.038 0.03 Uiso 1 1 calc R . . C4 C 0.3420(4) 0.7483(8) 1.1053(3) 0.0227(16) Uani 1 1 d . . . H4D H 0.3981 0.7521 1.1088 0.027 Uiso 1 1 calc R . . H4E H 0.3253 0.8383 1.1272 0.027 Uiso 1 1 calc R . . C5 C 0.9188(4) 0.8178(9) 0.9142(4) 0.0285(18) Uani 1 1 d . . . H5A H 0.8626 0.8108 0.9068 0.034 Uiso 1 1 calc R . . H5B H 0.9335 0.9206 0.8995 0.034 Uiso 1 1 calc R . . C6 C 0.9457(4) 0.8089(10) 0.9794(4) 0.033(2) Uani 1 1 d . . . H6A H 0.9233 0.8978 0.9984 0.04 Uiso 1 1 calc R . . H6B H 1.0016 0.8219 0.9865 0.04 Uiso 1 1 calc R . . C7 C 0.7707(4) 0.7622(9) 1.0349(3) 0.0234(17) Uani 1 1 d . . . H7A H 0.7815 0.8675 1.0201 0.028 Uiso 1 1 calc R . . H7B H 0.7147 0.7509 1.031 0.028 Uiso 1 1 calc R . . C8 C 0.8032(4) 0.7537(9) 1.0984(3) 0.0230(17) Uani 1 1 d . . . H8A H 0.7818 0.8395 1.1198 0.028 Uiso 1 1 calc R . . H8B H 0.859 0.7677 1.1032 0.028 Uiso 1 1 calc R . . N1 N 0.4354(3) 0.7303(7) 0.8507(3) 0.0247(14) Uani 1 1 d . . . H1A H 0.4114 0.703 0.8146 0.037 Uiso 1 1 calc R . . H1B H 0.4434 0.6429 0.8734 0.037 Uiso 1 1 calc R . . H1C H 0.4808 0.776 0.8475 0.037 Uiso 1 1 calc R . . N2 N 0.3186(3) 0.5981(7) 1.1313(3) 0.0270(15) Uani 1 1 d . . . H2A H 0.3409 0.5915 1.1693 0.04 Uiso 1 1 calc R . . H2B H 0.3336 0.5153 1.111 0.04 Uiso 1 1 calc R . . H2C H 0.2672 0.5962 1.1294 0.04 Uiso 1 1 calc R . . N3 N 0.9510(3) 0.6910(7) 0.8819(3) 0.0283(15) Uani 1 1 d . . . H3A H 0.9328 0.6997 0.8431 0.042 Uiso 1 1 calc R . . H3B H 0.9375 0.5962 0.8952 0.042 Uiso 1 1 calc R . . H3C H 1.0026 0.6992 0.8874 0.042 Uiso 1 1 calc R . . N4 N 0.7851(3) 0.5981(7) 1.1239(3) 0.0259(15) Uani 1 1 d . . . H4A H 0.8051 0.5951 1.1624 0.039 Uiso 1 1 calc R . . H4B H 0.8054 0.5193 1.1047 0.039 Uiso 1 1 calc R . . H4C H 0.7337 0.5858 1.12 0.039 Uiso 1 1 calc R . . I1 I 0.41072(2) 0.31546(6) 0.87597(2) 0.02298(11) Uani 1 1 d . . . I2 I 0.35223(3) 0.30332(6) 0.59569(2) 0.02434(11) Uani 1 1 d . . . I3 I 0.46148(2) -0.02472(6) 0.72799(2) 0.02281(11) Uani 1 1 d . . . I4 I 0.22623(2) 0.10986(6) 0.75082(2) 0.02018(11) Uani 1 1 d . . . I5 I 0.53514(2) 0.48340(6) 0.74094(2) 0.02417(12) Uani 1 1 d . . . I6 I 0.78882(2) 0.63748(6) 0.76345(2) 0.02383(12) Uani 1 1 d . . . I7 I 0.61917(2) 0.78617(6) 0.60932(2) 0.02321(11) Uani 1 1 d . . . I8 I 0.63340(3) 0.81062(6) 0.88774(2) 0.02497(11) Uani 1 1 d . . . Pb1 Pb 0.378290(13) 0.30449(3) 0.738908(12) 0.01706(7) Uani 1 1 d . . . Pb2 Pb 0.627988(13) 0.80727(3) 0.745627(12) 0.01807(7) Uani 1 1 d . . . S1 S 0.45019(10) 0.7258(3) 0.98807(9) 0.0318(5) Uani 1 1 d . . . S2 S 0.34714(10) 0.6240(2) 0.99297(9) 0.0272(4) Uani 1 1 d . . . S3 S 0.92167(10) 0.6277(2) 1.01348(9) 0.0271(4) Uani 1 1 d . . . S4 S 0.80712(9) 0.6137(2) 0.98883(8) 0.0230(4) 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 0.027(4) 0.040(5) 0.037(5) 0.009(4) 0.006(3) 0.001(4) C2 0.044(5) 0.022(5) 0.035(5) -0.007(4) 0.016(4) -0.005(4) C3 0.026(4) 0.026(4) 0.023(4) -0.001(3) 0.005(3) -0.002(3) C4 0.035(4) 0.012(4) 0.021(4) -0.002(3) 0.005(3) 0.003(3) C5 0.039(4) 0.015(4) 0.033(5) 0.000(4) 0.011(4) 0.004(3) C6 0.031(4) 0.037(5) 0.034(5) -0.006(4) 0.013(4) -0.007(4) C7 0.030(4) 0.021(4) 0.021(4) 0.006(3) 0.009(3) 0.008(3) C8 0.034(4) 0.018(4) 0.019(4) -0.003(3) 0.011(3) -0.007(3) N1 0.028(3) 0.026(4) 0.019(4) 0.004(3) 0.000(3) -0.001(3) N2 0.028(3) 0.025(4) 0.026(4) 0.004(3) 0.000(3) 0.001(3) N3 0.032(3) 0.027(4) 0.027(4) -0.006(3) 0.008(3) -0.001(3) N4 0.026(3) 0.033(4) 0.019(4) 0.004(3) 0.004(3) 0.003(3) I1 0.0248(2) 0.0246(3) 0.0186(3) 0.0016(2) 0.00008(18) 0.0010(2) I2 0.0252(2) 0.0266(3) 0.0201(3) 0.0006(2) -0.00015(18) 0.0014(2) I3 0.0188(2) 0.0219(3) 0.0285(3) 0.0057(2) 0.00601(18) 0.00632(19) I4 0.0186(2) 0.0208(3) 0.0213(3) -0.0025(2) 0.00347(17) -0.00531(19) I5 0.0209(2) 0.0228(3) 0.0294(3) -0.0023(2) 0.00567(19) -0.00750(19) I6 0.0190(2) 0.0213(3) 0.0308(3) 0.0029(2) 0.00283(19) 0.00594(19) I7 0.0246(2) 0.0245(3) 0.0205(3) 0.0003(2) 0.00317(18) -0.0008(2) I8 0.0272(2) 0.0246(3) 0.0219(3) -0.0015(2) -0.00036(19) 0.0007(2) Pb1 0.01546(11) 0.01815(15) 0.01743(15) -0.00060(12) 0.00206(10) -0.00018(10) Pb2 0.01581(12) 0.01881(15) 0.01958(15) 0.00186(12) 0.00269(10) 0.00043(10) S1 0.0234(9) 0.0469(14) 0.0245(11) 0.0021(10) 0.0016(8) -0.0005(9) S2 0.0319(9) 0.0270(11) 0.0242(11) -0.0009(9) 0.0091(8) -0.0033(8) S3 0.0219(8) 0.0370(12) 0.0220(11) 0.0024(9) 0.0019(7) 0.0023(8) S4 0.0217(8) 0.0292(11) 0.0184(10) -0.0041(8) 0.0035(7) -0.0020(8) #----------------------------------------------------------------------------# # 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 N1 1.490(10) . ? C1 C2 1.541(11) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 S1 1.797(9) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? C3 C4 1.518(10) . ? C3 S2 1.838(7) . ? C3 H3D 0.99 . ? C3 H3E 0.99 . ? C4 N2 1.499(9) . ? C4 H4D 0.99 . ? C4 H4E 0.99 . ? C5 N3 1.479(9) . ? C5 C6 1.515(11) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 S3 1.814(8) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.500(10) . ? C7 S4 1.836(7) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N4 1.506(9) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? 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 . ? N4 H4A 0.91 . ? N4 H4B 0.91 . ? N4 H4C 0.91 . ? I1 Pb1 3.1414(6) . ? I2 Pb1 3.2798(6) . ? I3 Pb1 3.1992(6) . ? I3 Pb2 3.2601(5) 1_545 ? I4 Pb1 3.2208(5) . ? I4 Pb1 3.2278(5) 2_546 ? I5 Pb1 3.1743(5) . ? I5 Pb2 3.2094(6) . ? I6 Pb2 3.1774(5) . ? I6 Pb2 3.2007(6) 2_646 ? I7 Pb2 3.1429(6) . ? I8 Pb2 3.2791(6) . ? Pb1 I4 3.2278(5) 2_556 ? Pb2 I6 3.2007(6) 2_656 ? Pb2 I3 3.2601(5) 1_565 ? S1 S2 2.047(3) . ? S3 S4 2.035(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.8(6) . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? C2 C1 H1E 109.5 . . ? H1D C1 H1E 108.1 . . ? C1 C2 S1 114.5(6) . . ? C1 C2 H2D 108.6 . . ? S1 C2 H2D 108.6 . . ? C1 C2 H2E 108.6 . . ? S1 C2 H2E 108.6 . . ? H2D C2 H2E 107.6 . . ? C4 C3 S2 114.3(5) . . ? C4 C3 H3D 108.7 . . ? S2 C3 H3D 108.7 . . ? C4 C3 H3E 108.7 . . ? S2 C3 H3E 108.7 . . ? H3D C3 H3E 107.6 . . ? N2 C4 C3 110.9(6) . . ? N2 C4 H4D 109.5 . . ? C3 C4 H4D 109.5 . . ? N2 C4 H4E 109.5 . . ? C3 C4 H4E 109.5 . . ? H4D C4 H4E 108 . . ? N3 C5 C6 112.3(6) . . ? N3 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? N3 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 S3 114.6(6) . . ? C5 C6 H6A 108.6 . . ? S3 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? S3 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 S4 114.8(5) . . ? C8 C7 H7A 108.6 . . ? S4 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? S4 C7 H7B 108.6 . . ? H7A C7 H7B 107.5 . . ? C7 C8 N4 110.7(6) . . ? C7 C8 H8A 109.5 . . ? N4 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C4 N2 H2A 109.5 . . ? C4 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C4 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C5 N3 H3A 109.5 . . ? C5 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C5 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C8 N4 H4A 109.5 . . ? C8 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C8 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? Pb1 I3 Pb2 142.906(18) . 1_545 ? Pb1 I4 Pb1 157.254(17) . 2_546 ? Pb1 I5 Pb2 149.353(18) . . ? Pb2 I6 Pb2 143.907(18) . 2_646 ? I1 Pb1 I5 86.810(15) . . ? I1 Pb1 I3 95.146(15) . . ? I5 Pb1 I3 90.332(14) . . ? I1 Pb1 I4 87.518(14) . . ? I5 Pb1 I4 173.816(16) . . ? I3 Pb1 I4 87.723(14) . . ? I1 Pb1 I4 85.476(14) . 2_556 ? I5 Pb1 I4 97.300(15) . 2_556 ? I3 Pb1 I4 172.366(14) . 2_556 ? I4 Pb1 I4 84.701(8) . 2_556 ? I1 Pb1 I2 177.126(14) . . ? I5 Pb1 I2 90.322(14) . . ? I3 Pb1 I2 85.040(14) . . ? I4 Pb1 I2 95.355(14) . . ? I4 Pb1 I2 94.721(14) 2_556 . ? I7 Pb2 I6 90.651(14) . . ? I7 Pb2 I6 86.408(15) . 2_656 ? I6 Pb2 I6 89.554(9) . 2_656 ? I7 Pb2 I5 88.268(15) . . ? I6 Pb2 I5 93.553(15) . . ? I6 Pb2 I5 173.867(16) 2_656 . ? I7 Pb2 I3 89.610(14) . 1_565 ? I6 Pb2 I3 178.911(16) . 1_565 ? I6 Pb2 I3 91.518(14) 2_656 1_565 ? I5 Pb2 I3 85.398(14) . 1_565 ? I7 Pb2 I8 176.986(16) . . ? I6 Pb2 I8 89.122(14) . . ? I6 Pb2 I8 96.595(15) 2_656 . ? I5 Pb2 I8 88.746(14) . . ? I3 Pb2 I8 90.563(14) 1_565 . ? C2 S1 S2 103.1(3) . . ? C3 S2 S1 101.3(3) . . ? C6 S3 S4 102.7(3) . . ? C7 S4 S3 102.9(3) . . ? 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 N1 C1 C2 S1 -55.3(8) . . . . ? S2 C3 C4 N2 -70.2(6) . . . . ? N3 C5 C6 S3 -59.7(7) . . . . ? S4 C7 C8 N4 -61.0(7) . . . . ? Pb2 I5 Pb1 I1 -86.99(4) . . . . ? Pb2 I5 Pb1 I3 177.87(4) . . . . ? Pb2 I5 Pb1 I4 -1.97(4) . . . 2_556 ? Pb2 I5 Pb1 I2 92.83(4) . . . . ? Pb2 I3 Pb1 I1 -69.60(3) 1_545 . . . ? Pb2 I3 Pb1 I5 17.23(3) 1_545 . . . ? Pb2 I3 Pb1 I4 -156.90(3) 1_545 . . . ? Pb2 I3 Pb1 I2 107.52(3) 1_545 . . . ? Pb1 I4 Pb1 I1 -91.34(4) 2_546 . . . ? Pb1 I4 Pb1 I3 3.91(4) 2_546 . . . ? Pb1 I4 Pb1 I4 -177.02(5) 2_546 . . 2_556 ? Pb1 I4 Pb1 I2 88.71(4) 2_546 . . . ? Pb2 I6 Pb2 I7 -72.99(3) 2_646 . . . ? Pb2 I6 Pb2 I6 -159.39(4) 2_646 . . 2_656 ? Pb2 I6 Pb2 I5 15.32(3) 2_646 . . . ? Pb2 I6 Pb2 I8 104.01(3) 2_646 . . . ? Pb1 I5 Pb2 I7 -98.33(4) . . . . ? Pb1 I5 Pb2 I6 171.13(4) . . . . ? Pb1 I5 Pb2 I3 -8.58(4) . . . 1_565 ? Pb1 I5 Pb2 I8 82.08(4) . . . . ? C1 C2 S1 S2 -61.4(6) . . . . ? C4 C3 S2 S1 -75.0(5) . . . . ? C2 S1 S2 C3 -75.7(4) . . . . ? C5 C6 S3 S4 -54.1(6) . . . . ? C8 C7 S4 S3 -48.4(5) . . . . ? C6 S3 S4 C7 -74.4(4) . . . . ? 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 I4 0.91 2.79 3.578(6) 145 2_556 N1 H1B I1 0.91 2.85 3.620(6) 143 . N1 H1C I8 0.91 2.75 3.564(6) 150 . N2 H2A I5 0.91 2.87 3.699(6) 153 3_667 N2 H2B I8 0.91 2.84 3.628(6) 146 3_667 N2 H2C I7 0.91 2.79 3.644(6) 157 4_576 N3 H3A I6 0.91 2.97 3.697(6) 138 . N3 H3B I7 0.91 2.82 3.685(6) 158 2_646 N3 H3C I2 0.91 2.7 3.590(6) 165 2_656 N4 H4A I3 0.91 3.02 3.710(6) 134 4_666 N4 H4B I2 0.91 2.89 3.713(6) 151 4_666 N4 H4C I1 0.91 2.72 3.561(6) 154 3_667 _chemical_name_common (2,2'-dithiodiethanammonium)tetraiodoplumbate(ii) ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-10-18 at 16:52:49 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\wingx\files\archive.dat # CIF files read : 5as89al_a apex data_10 _database_code_depnum_ccdc_archive 'CCDC 746133' #TrackingRef 'B917824-revised.cif' _audit_creation_date 2005-10-18T16:52:49-00:00 _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(2,2'-dithiodiethanammonium)pentaiodoplumbate(II) iodide ; _chemical_formula_sum 'C8 H28 I6 N4 Pb S4' _chemical_formula_moiety '2(C4 H14 N2 S2), I5 Pb, I' _chemical_formula_weight 1277.17 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3748(2) _cell_length_b 8.7290(1) _cell_length_c 29.2867(4) _cell_angle_alpha 90 _cell_angle_beta 95.004(1) _cell_angle_gamma 90 _cell_volume 2896.81(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7885 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.24 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 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 -2 0 1 0.06 0 -2 -5 0.105 0 2 -1 0.12 1 0 -2 0.045 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.51 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.12 _exptl_absorpt_correction_T_max 0.5134 _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 0.0547 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_number 36616 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.4 _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 6980 _reflns_number_gt 6041 _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, 1997)' _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^)+(0.0380P)^2^+24.9235P] 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 6980 _refine_ls_number_parameters 281 _refine_ls_number_restraints 270 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.338 _refine_diff_density_min -4.742 _refine_diff_density_rms 0.229 #----------------------------------------------------------------------------# # 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' S S 0.1246 0.1234 '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 N1 N 0.2552(6) 0.7867(8) 0.7848(3) 0.0447(16) Uani 1 1 d DU . . H1A H 0.2846 0.8358 0.7609 0.067 Uiso 1 1 calc R . . H1B H 0.3012 0.7041 0.7929 0.067 Uiso 1 1 calc R . . H1C H 0.2548 0.8518 0.809 0.067 Uiso 1 1 calc R . . C1 C 0.1325(7) 0.7347(10) 0.7710(3) 0.0413(15) Uani 1 1 d DU . . H1D H 0.1334 0.6635 0.7447 0.05 Uiso 1 1 calc R . . H1E H 0.0836 0.8243 0.7609 0.05 Uiso 1 1 calc R . . C2 C 0.0776(7) 0.6552(10) 0.8097(3) 0.0413(14) Uani 1 1 d DU . . H2D H 0.1232 0.5609 0.8177 0.05 Uiso 1 1 calc R . . H2E H -0.0036 0.6239 0.7988 0.05 Uiso 1 1 calc R . . S1 S 0.07137(19) 0.7704(3) 0.86141(7) 0.0449(5) Uani 1 1 d DU . . S2 S -0.04340(18) 0.9431(3) 0.84328(9) 0.0475(5) Uani 1 1 d DU . . C3 C -0.1830(7) 0.8812(11) 0.8648(4) 0.0522(19) Uani 1 1 d DU . . H3D H -0.1686 0.8511 0.8974 0.063 Uiso 1 1 calc R . . H3E H -0.2395 0.9678 0.8629 0.063 Uiso 1 1 calc R . . C4 C -0.2335(7) 0.7539(11) 0.8386(3) 0.0486(19) Uani 1 1 d DU . . H4D H -0.182 0.6629 0.8435 0.058 Uiso 1 1 calc R . . H4E H -0.2403 0.7794 0.8056 0.058 Uiso 1 1 calc R . . N2 N -0.3561(6) 0.7190(8) 0.8542(3) 0.0428(16) Uani 1 1 d DU . . H2A H -0.3884 0.6383 0.8379 0.064 Uiso 1 1 calc R . . H2B H -0.4033 0.8026 0.8494 0.064 Uiso 1 1 calc R . . H2C H -0.3492 0.6953 0.8846 0.064 Uiso 1 1 calc R . . N3A N 1.154(4) 0.209(7) 0.9194(15) 0.033(5) Uani 0.465(5) 1 d PDU A 1 H3A1 H 1.184 0.1779 0.8932 0.05 Uiso 0.465(5) 1 calc PR A 1 H3A2 H 1.1357 0.1255 0.936 0.05 Uiso 0.465(5) 1 calc PR A 1 H3A3 H 1.2085 0.2669 0.9362 0.05 Uiso 0.465(5) 1 calc PR A 1 C5A C 1.045(3) 0.302(3) 0.9078(7) 0.038(3) Uani 0.465(5) 1 d PDU A 1 H5A1 H 0.9814 0.2343 0.8943 0.046 Uiso 0.465(5) 1 calc PR A 1 H5A2 H 1.0613 0.3797 0.8845 0.046 Uiso 0.465(5) 1 calc PR A 1 C6A C 1.0045(18) 0.382(2) 0.9496(5) 0.039(2) Uani 0.465(5) 1 d PDU A 1 H6A1 H 0.9282 0.4329 0.941 0.046 Uiso 0.465(5) 1 calc PR A 1 H6A2 H 1.0627 0.4617 0.9597 0.046 Uiso 0.465(5) 1 calc PR A 1 S3A S 0.9868(4) 0.2510(6) 0.99769(16) 0.0439(11) Uani 0.465(5) 1 d PDU A 1 S4A S 0.8599(6) 0.1028(8) 0.9722(3) 0.0754(16) Uani 0.465(5) 1 d PDU A 1 C7A C 0.7522(14) 0.188(3) 1.0124(7) 0.069(3) Uani 0.465(5) 1 d PDU A 1 H7A1 H 0.7587 0.1278 1.0412 0.083 Uiso 0.465(5) 1 calc PR A 1 H7A2 H 0.7779 0.2938 1.0203 0.083 Uiso 0.465(5) 1 calc PR A 1 C8A C 0.6357(17) 0.192(3) 0.9960(9) 0.067(3) Uani 0.465(5) 1 d PDU A 1 H8A1 H 0.5884 0.218 1.0218 0.081 Uiso 0.465(5) 1 calc PR A 1 H8A2 H 0.6121 0.0886 0.9852 0.081 Uiso 0.465(5) 1 calc PR A 1 N4A N 0.6038(17) 0.305(2) 0.9574(7) 0.064(4) Uani 0.465(5) 1 d PDU A 1 H4A1 H 0.5573 0.257 0.9348 0.096 Uiso 0.465(5) 1 calc PR A 1 H4A2 H 0.6708 0.3387 0.9459 0.096 Uiso 0.465(5) 1 calc PR A 1 H4A3 H 0.564 0.3854 0.9682 0.096 Uiso 0.465(5) 1 calc PR A 1 N3B N 1.159(4) 0.218(6) 0.9127(13) 0.037(5) Uani 0.535(5) 1 d PDU A 2 H3B1 H 1.1951 0.2129 0.8862 0.056 Uiso 0.535(5) 1 calc PR A 2 H3B2 H 1.1325 0.124 0.9199 0.056 Uiso 0.535(5) 1 calc PR A 2 H3B3 H 1.2119 0.2521 0.9357 0.056 Uiso 0.535(5) 1 calc PR A 2 C5B C 1.058(2) 0.327(3) 0.9068(7) 0.039(2) Uani 0.535(5) 1 d PDU A 2 H5B1 H 1.0062 0.2982 0.8792 0.046 Uiso 0.535(5) 1 calc PR A 2 H5B2 H 1.088 0.4319 0.9019 0.046 Uiso 0.535(5) 1 calc PR A 2 C6B C 0.9863(15) 0.3276(17) 0.9480(5) 0.039(2) Uani 0.535(5) 1 d PDU A 2 H6B1 H 0.9213 0.4029 0.9433 0.047 Uiso 0.535(5) 1 calc PR A 2 H6B2 H 1.0372 0.3581 0.9756 0.047 Uiso 0.535(5) 1 calc PR A 2 S3B S 0.9246(5) 0.1340(5) 0.95643(13) 0.0495(11) Uani 0.535(5) 1 d PDU A 2 S4B S 0.8962(4) 0.1405(5) 1.02350(13) 0.0447(10) Uani 0.535(5) 1 d PDU A 2 C7B C 0.7582(12) 0.254(2) 1.0238(6) 0.052(3) Uani 0.535(5) 1 d PDU A 2 H7B1 H 0.7282 0.249 1.0545 0.062 Uiso 0.535(5) 1 calc PR A 2 H7B2 H 0.774 0.3625 1.0168 0.062 Uiso 0.535(5) 1 calc PR A 2 C8B C 0.6744(13) 0.194(2) 0.9910(7) 0.060(3) Uani 0.535(5) 1 d PDU A 2 H8B1 H 0.6549 0.0878 0.9995 0.072 Uiso 0.535(5) 1 calc PR A 2 H8B2 H 0.7078 0.1908 0.9609 0.072 Uiso 0.535(5) 1 calc PR A 2 N4B N 0.5630(11) 0.2897(18) 0.9871(6) 0.056(3) Uani 0.535(5) 1 d PDU A 2 H4B1 H 0.5026 0.2338 0.9731 0.084 Uiso 0.535(5) 1 calc PR A 2 H4B2 H 0.5746 0.375 0.9702 0.084 Uiso 0.535(5) 1 calc PR A 2 H4B3 H 0.5449 0.3177 1.0155 0.084 Uiso 0.535(5) 1 calc PR A 2 I1 I 0.81808(4) 0.80938(6) 1.205978(16) 0.03212(11) Uani 1 1 d . . . I2 I 0.26823(4) 0.67284(7) 1.15614(2) 0.04486(14) Uani 1 1 d . . . I3 I 0.46101(5) 1.00524(6) 1.241928(18) 0.04119(13) Uani 1 1 d . . . I4 I 0.62657(4) 0.47668(5) 1.113441(16) 0.03191(11) Uani 1 1 d . . . I5 I 0.56472(5) 0.99374(6) 1.099595(18) 0.03891(13) Uani 1 1 d . . . I6 I 0.70120(6) 0.66714(9) 0.97464(2) 0.0626(2) Uani 1 1 d . . . Pb1 Pb 0.54920(2) 0.74266(3) 1.175380(8) 0.02481(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 N1 0.035(3) 0.036(4) 0.064(5) -0.002(3) 0.010(3) 0.002(3) C1 0.038(3) 0.045(4) 0.040(3) -0.001(3) 0.001(3) 0.000(3) C2 0.038(3) 0.039(4) 0.046(3) 0.003(2) -0.003(3) -0.006(3) S1 0.0423(10) 0.0550(13) 0.0374(10) 0.0068(9) 0.0035(8) -0.0043(9) S2 0.0368(10) 0.0432(12) 0.0650(14) 0.0035(10) 0.0187(9) -0.0103(8) C3 0.041(3) 0.050(5) 0.068(5) -0.004(4) 0.016(3) -0.013(2) C4 0.041(3) 0.051(5) 0.056(5) -0.002(4) 0.011(3) -0.011(3) N2 0.029(3) 0.039(4) 0.059(4) 0.009(3) 0.001(3) -0.003(2) N3A 0.034(7) 0.043(9) 0.023(10) 0.000(7) 0.005(6) 0.000(6) C5A 0.038(5) 0.044(6) 0.032(4) 0.002(4) 0.004(4) 0.002(5) C6A 0.037(5) 0.043(5) 0.037(4) -0.001(4) 0.006(4) 0.003(4) S3A 0.045(2) 0.050(3) 0.037(2) 0.0005(18) 0.0135(17) 0.0031(18) S4A 0.061(3) 0.068(4) 0.098(4) 0.017(3) 0.006(3) -0.020(2) C7A 0.058(3) 0.076(6) 0.075(6) 0.024(5) 0.003(4) -0.016(5) C8A 0.061(4) 0.070(6) 0.070(6) 0.018(5) 0.001(5) -0.012(6) N4A 0.069(8) 0.057(8) 0.064(8) 0.009(6) -0.002(7) -0.013(7) N3B 0.036(6) 0.046(8) 0.030(10) 0.000(8) 0.004(6) 0.001(6) C5B 0.039(5) 0.045(5) 0.032(4) 0.001(4) 0.003(3) 0.002(4) C6B 0.037(5) 0.046(4) 0.036(4) 0.002(4) 0.005(3) 0.003(4) S3B 0.070(3) 0.048(2) 0.0322(17) -0.0074(16) 0.0140(18) -0.009(2) S4B 0.055(2) 0.050(2) 0.0304(16) 0.0037(16) 0.0082(15) 0.0087(17) C7B 0.049(4) 0.049(7) 0.059(6) 0.003(5) 0.017(3) 0.001(4) C8B 0.044(4) 0.066(6) 0.070(6) 0.018(5) 0.008(4) -0.008(5) N4B 0.043(5) 0.055(7) 0.073(8) 0.000(7) 0.016(5) -0.011(5) I1 0.0278(2) 0.0360(3) 0.0326(2) -0.00182(19) 0.00246(17) -0.00497(18) I2 0.0292(2) 0.0489(3) 0.0545(3) -0.0071(3) -0.0076(2) 0.0047(2) I3 0.0551(3) 0.0316(3) 0.0387(3) -0.0155(2) 0.0146(2) -0.0042(2) I4 0.0341(2) 0.0266(2) 0.0355(2) -0.00783(18) 0.00544(18) 0.00060(18) I5 0.0484(3) 0.0265(2) 0.0432(3) 0.0111(2) 0.0115(2) 0.0030(2) I6 0.0650(4) 0.0715(5) 0.0470(3) 0.0120(3) -0.0200(3) -0.0094(3) Pb1 0.02827(13) 0.02008(13) 0.02688(12) 0.00064(9) 0.00696(9) -0.00016(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 N1 C1 1.490(9) . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? C1 C2 1.510(10) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 S1 1.824(8) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? S1 S2 2.034(3) . ? S2 C3 1.840(8) . ? C3 C4 1.441(12) . ? C3 H3D 0.99 . ? C3 H3E 0.99 . ? C4 N2 1.534(10) . ? C4 H4D 0.99 . ? C4 H4E 0.99 . ? N2 H2A 0.91 . ? N2 H2B 0.91 . ? N2 H2C 0.91 . ? N3A C5A 1.494(15) . ? N3A H3A1 0.91 . ? N3A H3A2 0.91 . ? N3A H3A3 0.91 . ? C5A C6A 1.515(16) . ? C5A H5A1 0.99 . ? C5A H5A2 0.99 . ? C6A S3A 1.836(14) . ? C6A H6A1 0.99 . ? C6A H6A2 0.99 . ? S3A S4A 2.032(8) . ? S4A C7A 1.921(17) . ? C7A C8A 1.370(17) . ? C7A H7A1 0.99 . ? C7A H7A2 0.99 . ? C8A N4A 1.516(17) . ? C8A H8A1 0.99 . ? C8A H8A2 0.99 . ? N4A H4A1 0.91 . ? N4A H4A2 0.91 . ? N4A H4A3 0.91 . ? N3B C5B 1.493(14) . ? N3B H3B1 0.91 . ? N3B H3B2 0.91 . ? N3B H3B3 0.91 . ? C5B C6B 1.513(14) . ? C5B H5B1 0.99 . ? C5B H5B2 0.99 . ? C6B S3B 1.855(14) . ? C6B H6B1 0.99 . ? C6B H6B2 0.99 . ? S3B S4B 2.019(5) . ? S4B C7B 1.857(13) . ? C7B C8B 1.394(17) . ? C7B H7B1 0.99 . ? C7B H7B2 0.99 . ? C8B N4B 1.513(16) . ? C8B H8B1 0.99 . ? C8B H8B2 0.99 . ? N4B H4B1 0.91 . ? N4B H4B2 0.91 . ? N4B H4B3 0.91 . ? I1 Pb1 3.1652(5) . ? I2 Pb1 3.2541(6) . ? I3 Pb1 3.1973(5) 2_657 ? I3 Pb1 3.2247(5) . ? I4 Pb1 3.1200(5) . ? I5 Pb1 3.1351(5) . ? Pb1 I3 3.1973(5) 2_647 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C1 C2 112.0(7) . . ? N1 C1 H1D 109.2 . . ? C2 C1 H1D 109.2 . . ? N1 C1 H1E 109.2 . . ? C2 C1 H1E 109.2 . . ? H1D C1 H1E 107.9 . . ? C1 C2 S1 114.8(6) . . ? C1 C2 H2D 108.6 . . ? S1 C2 H2D 108.6 . . ? C1 C2 H2E 108.6 . . ? S1 C2 H2E 108.6 . . ? H2D C2 H2E 107.6 . . ? C2 S1 S2 105.2(3) . . ? C3 S2 S1 104.3(4) . . ? C4 C3 S2 111.1(6) . . ? C4 C3 H3D 109.4 . . ? S2 C3 H3D 109.4 . . ? C4 C3 H3E 109.4 . . ? S2 C3 H3E 109.4 . . ? H3D C3 H3E 108 . . ? C3 C4 N2 109.0(7) . . ? C3 C4 H4D 109.9 . . ? N2 C4 H4D 109.9 . . ? C3 C4 H4E 109.9 . . ? N2 C4 H4E 109.9 . . ? H4D C4 H4E 108.3 . . ? C4 N2 H2A 109.5 . . ? C4 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C4 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C5A N3A H3A1 109.5 . . ? C5A N3A H3A2 109.5 . . ? H3A1 N3A H3A2 109.5 . . ? C5A N3A H3A3 109.5 . . ? H3A1 N3A H3A3 109.5 . . ? H3A2 N3A H3A3 109.5 . . ? N3A C5A C6A 111.7(18) . . ? N3A C5A H5A1 109.3 . . ? C6A C5A H5A1 109.3 . . ? N3A C5A H5A2 109.3 . . ? C6A C5A H5A2 109.3 . . ? H5A1 C5A H5A2 107.9 . . ? C5A C6A S3A 113.4(13) . . ? C5A C6A H6A1 108.9 . . ? S3A C6A H6A1 108.9 . . ? C5A C6A H6A2 108.9 . . ? S3A C6A H6A2 108.9 . . ? H6A1 C6A H6A2 107.7 . . ? C6A S3A S4A 103.6(7) . . ? C7A S4A S3A 89.9(7) . . ? C8A C7A S4A 116.4(17) . . ? C8A C7A H7A1 108.2 . . ? S4A C7A H7A1 108.2 . . ? C8A C7A H7A2 108.2 . . ? S4A C7A H7A2 108.2 . . ? H7A1 C7A H7A2 107.3 . . ? C7A C8A N4A 116.2(18) . . ? C7A C8A H8A1 108.2 . . ? N4A C8A H8A1 108.2 . . ? C7A C8A H8A2 108.2 . . ? N4A C8A H8A2 108.2 . . ? H8A1 C8A H8A2 107.4 . . ? C8A N4A H4A1 109.5 . . ? C8A N4A H4A2 109.5 . . ? H4A1 N4A H4A2 109.5 . . ? C8A N4A H4A3 109.5 . . ? H4A1 N4A H4A3 109.5 . . ? H4A2 N4A H4A3 109.5 . . ? C5B N3B H3B1 109.5 . . ? C5B N3B H3B2 109.5 . . ? H3B1 N3B H3B2 109.5 . . ? C5B N3B H3B3 109.5 . . ? H3B1 N3B H3B3 109.5 . . ? H3B2 N3B H3B3 109.5 . . ? N3B C5B C6B 111.8(15) . . ? N3B C5B H5B1 109.3 . . ? C6B C5B H5B1 109.3 . . ? N3B C5B H5B2 109.3 . . ? C6B C5B H5B2 109.3 . . ? H5B1 C5B H5B2 107.9 . . ? C5B C6B S3B 109.9(12) . . ? C5B C6B H6B1 109.7 . . ? S3B C6B H6B1 109.7 . . ? C5B C6B H6B2 109.7 . . ? S3B C6B H6B2 109.7 . . ? H6B1 C6B H6B2 108.2 . . ? C6B S3B S4B 101.5(5) . . ? C7B S4B S3B 103.1(6) . . ? C8B C7B S4B 108.9(11) . . ? C8B C7B H7B1 109.9 . . ? S4B C7B H7B1 109.9 . . ? C8B C7B H7B2 109.9 . . ? S4B C7B H7B2 109.9 . . ? H7B1 C7B H7B2 108.3 . . ? C7B C8B N4B 111.3(15) . . ? C7B C8B H8B1 109.4 . . ? N4B C8B H8B1 109.4 . . ? C7B C8B H8B2 109.4 . . ? N4B C8B H8B2 109.4 . . ? H8B1 C8B H8B2 108 . . ? C8B N4B H4B1 109.5 . . ? C8B N4B H4B2 109.5 . . ? H4B1 N4B H4B2 109.5 . . ? C8B N4B H4B3 109.5 . . ? H4B1 N4B H4B3 109.5 . . ? H4B2 N4B H4B3 109.5 . . ? Pb1 I3 Pb1 162.22(2) 2_657 . ? I4 Pb1 I5 94.153(15) . . ? I4 Pb1 I1 89.251(14) . . ? I5 Pb1 I1 87.655(15) . . ? I4 Pb1 I3 89.355(15) . 2_647 ? I5 Pb1 I3 175.842(17) . 2_647 ? I1 Pb1 I3 90.165(15) . 2_647 ? I4 Pb1 I3 177.079(16) . . ? I5 Pb1 I3 88.322(15) . . ? I1 Pb1 I3 92.404(15) . . ? I3 Pb1 I3 88.233(7) 2_647 . ? I4 Pb1 I2 94.733(15) . . ? I5 Pb1 I2 97.090(17) . . ? I1 Pb1 I2 173.554(16) . . ? I3 Pb1 I2 84.824(16) 2_647 . ? I3 Pb1 I2 83.409(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 N1 C1 C2 S1 58.0(9) . . . . ? C1 C2 S1 S2 66.6(6) . . . . ? C2 S1 S2 C3 99.6(4) . . . . ? S1 S2 C3 C4 -70.3(8) . . . . ? S2 C3 C4 N2 -173.5(6) . . . . ? N3A C5A C6A S3A -53(3) . . . . ? C5A C6A S3A S4A -61.5(18) . . . . ? C6A S3A S4A C7A -111.1(9) . . . . ? S3A S4A C7A C8A 146.3(18) . . . . ? S4A C7A C8A N4A -70(3) . . . . ? N3B C5B C6B S3B -61(3) . . . . ? C5B C6B S3B S4B 157.5(14) . . . . ? C6B S3B S4B C7B 77.9(9) . . . . ? S3B S4B C7B C8B 49.6(15) . . . . ? S4B C7B C8B N4B -175.5(13) . . . . ? Pb1 I3 Pb1 I5 -112.95(7) 2_657 . . . ? Pb1 I3 Pb1 I1 -25.37(7) 2_657 . . . ? Pb1 I3 Pb1 I3 64.72(7) 2_657 . . 2_647 ? Pb1 I3 Pb1 I2 149.71(7) 2_657 . . . ? 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 3.06 3.801(8) 140 4_575 N1 H1B I3 0.91 3.06 3.750(7) 134 4_575 N1 H1C I1 0.91 3.09 3.639(7) 120 3_677 N2 H2A I2 0.91 3.04 3.583(7) 120 3_567 N2 H2B I5 0.91 3.04 3.783(7) 140 3_577 N2 H2C I6 0.91 2.66 3.559(8) 169 1_455 N3A H3A1 I1 0.91 2.9 3.72(4) 150 3_767 N3A H3A3 I6 0.91 2.78 3.55(5) 143 3_767 N4A H4A1 I5 0.91 2.74 3.56(2) 151 3_667 N4A H4A2 I2 0.91 3.13 3.75(2) 127 3_667 N4A H4A3 I6 0.91 2.91 3.38(2) 113 . N3B H3B1 I1 0.91 2.7 3.52(4) 150 3_767 N3B H3B3 I6 0.91 2.81 3.67(5) 158 3_767 N4B H4B1 I5 0.91 2.96 3.745(17) 145 3_667 N4B H4B2 I6 0.91 2.93 3.682(16) 142 . N4B H4B3 I6 0.91 2.84 3.320(13) 114 3_667 _chemical_name_common "bis(2,2'-dithiodiethanammonium)pentaiodoplumbate(ii) iodide"