# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Lemmerer, Andreas' 'Billing, David' _publ_contact_author_name 'Dr Andreas Lemmerer' _publ_contact_author_email dave.billing@wits.ac.za _publ_section_title ; Lead halide inorganic-organic hybrids incorporating diammonium cations ; _publ_requested_category FM # Attachment '- Diamines.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-10-30 at 15:31:51 # 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 : 4ad58_a smart data_1 _database_code_depnum_ccdc_archive 'CCDC 853206' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-10-30T15:31:51-00:00 _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 ; (1,4-diammoniumbutane)tetrabromoplumbate(II) ; _chemical_formula_sum 'C4 H14 Br4 N2 Pb' _chemical_formula_moiety 'Br4 Pb, C4 H14 N2' _chemical_formula_weight 617 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0070(18) _cell_length_b 8.389(2) _cell_length_c 10.586(3) _cell_angle_alpha 78.572(7) _cell_angle_beta 70.445(7) _cell_angle_gamma 89.192(7) _cell_volume 655.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 806 _cell_measurement_theta_min 3.5635 _cell_measurement_theta_max 28.3025 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description polyhedral _exptl_crystal_colour colourles _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 3.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.06 0 0 -1 0.06 1 -1 1 0.11 1 -1 -1 0.125 0 2 1 0.145 -1 1 -1 0.11 -1 1 0 0.13 0 -1 -1 0.14 -1 -1 0 0.13 3 3 1 0.14 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 25.007 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0162 _exptl_absorpt_correction_T_max 0.0957 _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 0.0412 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_number 3549 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 2276 _reflns_number_gt 1909 _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^)+(0.0528P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0227(9) _refine_ls_number_reflns 2276 _refine_ls_number_parameters 104 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.516 _refine_diff_density_min -1.59 _refine_diff_density_rms 0.316 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7561(13) 0.4498(11) 0.3799(9) 0.020(2) Uani 1 1 d DU . . H1D H 0.6478 0.4633 0.3544 0.024 Uiso 1 1 calc R . . H1E H 0.7508 0.5211 0.4452 0.024 Uiso 1 1 calc R . . C2 C 0.7599(13) 0.2753(10) 0.4486(9) 0.022(2) Uani 1 1 d DU . . H2D H 0.8574 0.2649 0.4871 0.026 Uiso 1 1 calc R . . H2E H 0.7835 0.2055 0.38 0.026 Uiso 1 1 calc R . . C3 C 0.5863(13) 0.2179(11) 0.5617(9) 0.022(2) Uani 1 1 d DU . . H3A H 0.4892 0.2407 0.5235 0.026 Uiso 1 1 calc R . . H3B H 0.5694 0.2834 0.6327 0.026 Uiso 1 1 calc R . . C4 C 0.5680(14) 0.0401(11) 0.6299(10) 0.019(2) Uani 1 1 d DU . . H4A H 0.4405 0.0043 0.669 0.023 Uiso 1 1 calc R . . H4B H 0.6266 -0.0244 0.5599 0.023 Uiso 1 1 calc R . . N1 N 0.9152(11) 0.5009(12) 0.2549(9) 0.026(2) Uani 1 1 d DU . . H1A H 0.9185 0.6106 0.2247 0.039 Uiso 1 1 calc R . . H1B H 0.9094 0.4494 0.1884 0.039 Uiso 1 1 calc R . . H1C H 1.0151 0.4741 0.2754 0.039 Uiso 1 1 calc R . . N2 N 0.6476(11) 0.0057(11) 0.7413(9) 0.024(2) Uani 1 1 d D . . H2A H 0.6561 -0.1036 0.7655 0.036 Uiso 1 1 calc R . . H2B H 0.5774 0.0434 0.8153 0.036 Uiso 1 1 calc R . . H2C H 0.7577 0.0565 0.7107 0.036 Uiso 1 1 calc R . . Br1 Br 0.29789(14) 0.38929(13) 0.29666(10) 0.0240(3) Uani 1 1 d . . . Br2 Br 0.32898(14) 0.20972(13) -0.05019(11) 0.0232(3) Uani 1 1 d . . . Br3 Br 0.21666(14) 0.71099(13) -0.05594(11) 0.0241(3) Uani 1 1 d . . . Br4 Br -0.06312(14) -0.11451(13) 0.29945(10) 0.0223(3) Uani 1 1 d . . . Pb1 Pb 0.5 0.5 0 0.01509(19) Uani 1 2 d S . . Pb2 Pb 0 0 0 0.01502(19) 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(5) 0.015(4) 0.019(5) -0.004(3) -0.007(3) 0.002(4) C2 0.027(5) 0.017(4) 0.020(5) -0.003(3) -0.007(3) 0.004(4) C3 0.026(5) 0.021(4) 0.018(5) -0.002(3) -0.008(3) 0.000(4) C4 0.023(5) 0.019(5) 0.020(5) -0.001(4) -0.014(4) -0.008(4) N1 0.021(5) 0.025(5) 0.029(5) 0.003(4) -0.008(3) -0.002(4) N2 0.021(5) 0.025(5) 0.023(5) 0.000(4) -0.008(4) -0.003(4) Br1 0.0256(6) 0.0284(6) 0.0171(5) -0.0042(4) -0.0062(4) 0.0011(4) Br2 0.0233(6) 0.0236(6) 0.0233(5) -0.0057(4) -0.0081(4) -0.0078(4) Br3 0.0250(6) 0.0228(6) 0.0263(6) -0.0069(4) -0.0105(4) 0.0097(4) Br4 0.0234(6) 0.0235(6) 0.0203(5) -0.0043(4) -0.0079(4) -0.0013(4) Pb1 0.0156(3) 0.0140(3) 0.0161(3) -0.0025(2) -0.0061(2) -0.0005(2) Pb2 0.0159(3) 0.0129(3) 0.0164(3) -0.0021(2) -0.0061(2) -0.0003(2) #----------------------------------------------------------------------------# # 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 1.505(9) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.508(9) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? C3 C4 1.509(9) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 N2 1.498(10) . ? C4 H4A 0.99 . ? C4 H4B 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 . ? Br1 Pb1 2.9714(12) . ? Br2 Pb2 3.0232(11) . ? Br2 Pb1 3.0302(11) . ? Br3 Pb1 3.0002(11) . ? Br3 Pb2 3.0003(11) 1_565 ? Br4 Pb2 2.9937(12) . ? Pb1 Br1 2.9714(12) 2_665 ? Pb1 Br3 3.0002(11) 2_665 ? Pb1 Br2 3.0302(11) 2_665 ? Pb2 Br4 2.9937(12) 2 ? Pb2 Br3 3.0003(11) 1_545 ? Pb2 Br3 3.0003(11) 2_565 ? Pb2 Br2 3.0232(11) 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 111.9(8) . . ? 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 111.1(8) . . ? C1 C2 H2D 109.4 . . ? C3 C2 H2D 109.4 . . ? C1 C2 H2E 109.4 . . ? C3 C2 H2E 109.4 . . ? H2D C2 H2E 108 . . ? C2 C3 C4 116.0(9) . . ? C2 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? C2 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N2 C4 C3 113.0(8) . . ? N2 C4 H4A 109 . . ? C3 C4 H4A 109 . . ? N2 C4 H4B 109 . . ? C3 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 . . ? 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 . . ? Pb2 Br2 Pb1 149.43(4) . . ? Pb1 Br3 Pb2 147.28(4) . 1_565 ? Br1 Pb1 Br1 180.00(4) . 2_665 ? Br1 Pb1 Br3 85.52(3) . 2_665 ? Br1 Pb1 Br3 94.48(3) 2_665 2_665 ? Br1 Pb1 Br3 94.48(3) . . ? Br1 Pb1 Br3 85.52(3) 2_665 . ? Br3 Pb1 Br3 180.00(4) 2_665 . ? Br1 Pb1 Br2 88.00(3) . . ? Br1 Pb1 Br2 92.00(3) 2_665 . ? Br3 Pb1 Br2 89.55(3) 2_665 . ? Br3 Pb1 Br2 90.45(3) . . ? Br1 Pb1 Br2 92.00(3) . 2_665 ? Br1 Pb1 Br2 88.00(3) 2_665 2_665 ? Br3 Pb1 Br2 90.45(3) 2_665 2_665 ? Br3 Pb1 Br2 89.55(3) . 2_665 ? Br2 Pb1 Br2 180.00(4) . 2_665 ? Br4 Pb2 Br4 180.00(4) 2 . ? Br4 Pb2 Br3 90.64(3) 2 1_545 ? Br4 Pb2 Br3 89.36(3) . 1_545 ? Br4 Pb2 Br3 89.36(3) 2 2_565 ? Br4 Pb2 Br3 90.64(3) . 2_565 ? Br3 Pb2 Br3 180.00(5) 1_545 2_565 ? Br4 Pb2 Br2 94.20(3) 2 2 ? Br4 Pb2 Br2 85.80(3) . 2 ? Br3 Pb2 Br2 88.67(3) 1_545 2 ? Br3 Pb2 Br2 91.33(3) 2_565 2 ? Br4 Pb2 Br2 85.80(3) 2 . ? Br4 Pb2 Br2 94.20(3) . . ? Br3 Pb2 Br2 91.33(3) 1_545 . ? Br3 Pb2 Br2 88.67(3) 2_565 . ? Br2 Pb2 Br2 180.00(4) 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 -171.4(9) . . . . ? C1 C2 C3 C4 174.7(8) . . . . ? C2 C3 C4 N2 84.0(11) . . . . ? Pb2 Br3 Pb1 Br1 62.42(8) 1_565 . . . ? Pb2 Br3 Pb1 Br1 -117.58(8) 1_565 . . 2_665 ? Pb2 Br3 Pb1 Br2 150.45(8) 1_565 . . . ? Pb2 Br3 Pb1 Br2 -29.55(8) 1_565 . . 2_665 ? Pb2 Br2 Pb1 Br1 46.87(8) . . . . ? Pb2 Br2 Pb1 Br1 -133.13(8) . . . 2_665 ? Pb2 Br2 Pb1 Br3 132.40(8) . . . 2_665 ? Pb2 Br2 Pb1 Br3 -47.60(8) . . . . ? Pb1 Br2 Pb2 Br4 115.50(8) . . . 2 ? Pb1 Br2 Pb2 Br4 -64.50(8) . . . . ? Pb1 Br2 Pb2 Br3 -153.96(8) . . . 1_545 ? Pb1 Br2 Pb2 Br3 26.04(8) . . . 2_565 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Br4 0.91 2.6 3.367(10) 142 1_665 N1 H1B Br3 0.91 2.56 3.427(10) 161 2_665 N1 H1C Br1 0.91 2.43 3.335(9) 171 1_655 N2 H2A Br1 0.91 2.6 3.421(10) 151 2_656 N2 H2B Br2 0.91 2.6 3.452(9) 157 1_556 N2 H2C Br4 0.91 2.46 3.325(8) 158 2_656 ### END # CIF produced by WinGX routine CIF_UPDATE # Created on 2004-11-17 at 15:47:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : c:\wingx\files\archive.dat # CIF files read : 4ad18_a smart data_2 _database_code_depnum_ccdc_archive 'CCDC 853207' #TrackingRef '- Diamines.cif' _audit_creation_date 2004-11-17T15:47:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; (1,4-diammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C4 H14 I4 N2 Pb' _chemical_formula_moiety 'C4 H14 N2, I4 Pb' _chemical_formula_weight 804.96 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.119(4) _cell_length_b 8.5018(14) _cell_length_c 8.8936(15) _cell_angle_alpha 90 _cell_angle_beta 103.648(3) _cell_angle_gamma 90 _cell_volume 1551.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 943 _cell_measurement_theta_min 2.593 _cell_measurement_theta_max 28.174 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 3.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 -1 0.08 -1 0 1 0.08 0 -1 0 0.145 0 1 0 0.145 -7 2 2 0.15 -3 -1 1 0.16 1 0 0 0.22 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 18.796 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0174 _exptl_absorpt_correction_T_max 0.1044 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_unetI/netI 0.0528 _diffrn_reflns_number 5014 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.98 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 1863 _reflns_number_gt 1594 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0047(2) _refine_ls_number_reflns 1863 _refine_ls_number_parameters 63 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.3 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.321 #----------------------------------------------------------------------------# # 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 0.0606(5) 0.3287(15) 0.9478(10) 0.070(3) Uani 1 1 d DU . . H1D H 0.0698 0.4228 1.0108 0.084 Uiso 0.41(2) 1 calc PR A 1 H1E H 0.0258 0.2747 0.9812 0.084 Uiso 0.41(2) 1 calc PR A 1 H1F H 0.073 0.4387 0.9509 0.084 Uiso 0.59(2) 1 d PR A 2 H1G H 0.0307 0.3136 1.0143 0.084 Uiso 0.59(2) 1 d PR A 2 C2A C 0.0299(8) 0.387(3) 0.7824(16) 0.055(5) Uani 0.41(2) 1 d PDU . 1 H2A1 H 0.0611 0.3811 0.7182 0.067 Uiso 0.41(2) 1 calc PR A 1 H2A2 H 0.0155 0.4955 0.7843 0.067 Uiso 0.41(2) 1 calc PR A 1 C2B C 0.0287(7) 0.278(2) 0.7801(15) 0.059(4) Uani 0.59(2) 1 d PDU . 2 H2B1 H 0.0599 0.2854 0.7161 0.071 Uiso 0.59(2) 1 calc PR A 2 H2B2 H 0.014 0.1693 0.7787 0.071 Uiso 0.59(2) 1 calc PR A 2 N1 N 0.1175(4) 0.2298(11) 0.9969(11) 0.068(2) Uani 1 1 d U A . H1A H 0.1327 0.2386 1.0988 0.102 Uiso 1 1 calc R . . H1B H 0.148 0.2597 0.9491 0.102 Uiso 1 1 calc R . . H1C H 0.1067 0.1301 0.9731 0.102 Uiso 1 1 calc R . . I1 I 0.40210(2) 0.32359(7) 0.61154(6) 0.0556(2) Uani 1 1 d . . . I2 I 0.22208(3) 0.55957(7) 0.28897(6) 0.0528(2) Uani 1 1 d . . . Pb1 Pb 0.25 0.25 0.5 0.03823(17) 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 0.053(5) 0.106(8) 0.052(4) 0.001(5) 0.016(3) 0.009(4) C2A 0.040(8) 0.076(12) 0.050(7) -0.008(8) 0.009(6) -0.003(8) C2B 0.053(6) 0.068(10) 0.057(6) -0.006(6) 0.013(4) 0.013(6) N1 0.064(5) 0.076(5) 0.061(5) 0.006(4) 0.012(3) 0.001(4) I1 0.0390(3) 0.0675(4) 0.0599(4) 0.0036(3) 0.0108(2) -0.0003(2) I2 0.0590(3) 0.0544(3) 0.0477(3) 0.0185(2) 0.0182(2) 0.0022(2) Pb1 0.0392(2) 0.0428(3) 0.0327(2) -0.00084(13) 0.00867(14) 0.00153(14) #----------------------------------------------------------------------------# # 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 1.447(13) . ? C1 C2A 1.544(14) . ? C1 C2B 1.547(13) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C1 H1F 0.97 . ? C1 H1G 0.97 . ? C2A C2B 1.544(13) 2_556 ? C2A H2A1 0.97 . ? C2A H2A2 0.97 . ? C2B C2A 1.544(13) 2_556 ? C2B H2B1 0.97 . ? C2B H2B2 0.97 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1922(7) . ? I2 Pb1 3.2054(6) . ? I2 Pb1 3.2076(6) 4 ? Pb1 I1 3.1922(7) 7_556 ? Pb1 I2 3.2054(6) 7_556 ? Pb1 I2 3.2076(6) 6_566 ? Pb1 I2 3.2076(6) 4_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2A 127.4(12) . . ? N1 C1 C2B 105.6(10) . . ? N1 C1 H1D 105.4 . . ? C2A C1 H1D 105.4 . . ? C2B C1 H1D 140.5 . . ? N1 C1 H1E 105.4 . . ? C2A C1 H1E 105.4 . . ? C2B C1 H1E 88.4 . . ? H1D C1 H1E 106 . . ? N1 C1 H1F 110.6 . . ? C2A C1 H1F 76.5 . . ? C2B C1 H1F 110.6 . . ? H1E C1 H1F 131.9 . . ? N1 C1 H1G 110.6 . . ? C2A C1 H1G 115.9 . . ? C2B C1 H1G 110.6 . . ? H1D C1 H1G 80 . . ? H1F C1 H1G 108.7 . . ? C1 C2A C2B 105.6(15) . 2_556 ? C1 C2A H2A1 110.6 . . ? C2B C2A H2A1 110.6 2_556 . ? C1 C2A H2A2 110.6 . . ? C2B C2A H2A2 110.6 2_556 . ? H2A1 C2A H2A2 108.8 . . ? C2A C2B C1 107.8(13) 2_556 . ? C2A C2B H2B1 110.1 2_556 . ? C1 C2B H2B1 110.1 . . ? C2A C2B H2B2 110.1 2_556 . ? C1 C2B H2B2 110.1 . . ? H2B1 C2B H2B2 108.5 . . ? 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 147.175(19) . 4 ? I1 Pb1 I1 180.000(7) 7_556 . ? I1 Pb1 I2 86.926(15) 7_556 . ? I1 Pb1 I2 93.074(15) . . ? I1 Pb1 I2 93.074(15) 7_556 7_556 ? I1 Pb1 I2 86.926(15) . 7_556 ? I2 Pb1 I2 180 . 7_556 ? I1 Pb1 I2 89.207(16) 7_556 6_566 ? I1 Pb1 I2 90.793(16) . 6_566 ? I2 Pb1 I2 90.659(13) . 6_566 ? I2 Pb1 I2 89.341(13) 7_556 6_566 ? I1 Pb1 I2 90.793(16) 7_556 4_545 ? I1 Pb1 I2 89.207(16) . 4_545 ? I2 Pb1 I2 89.341(13) . 4_545 ? I2 Pb1 I2 90.659(13) 7_556 4_545 ? I2 Pb1 I2 180 6_566 4_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2A C2B 99.8(16) . . . 2_556 ? C2B C1 C2A C2B 39.6(19) . . . 2_556 ? N1 C1 C2B C2A -176.2(12) . . . 2_556 ? C2A C1 C2B C2A -42(2) . . . 2_556 ? Pb1 I2 Pb1 I1 -118.32(4) 4 . . 7_556 ? Pb1 I2 Pb1 I1 61.68(4) 4 . . . ? Pb1 I2 Pb1 I2 152.51(3) 4 . . 6_566 ? Pb1 I2 Pb1 I2 -27.49(3) 4 . . 4_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I1 0.89 2.89 3.631(9) 142 7_557 N1 H1B I2 0.89 2.81 3.665(9) 162 6_566 N1 H1C I1 0.89 2.71 3.583(9) 168 4_546 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2006-08-04 at 13:49:48 # 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 : 3ad23l_a smart data_3 _database_code_depnum_ccdc_archive 'CCDC 853208' #TrackingRef '- Diamines.cif' _audit_creation_date 2006-08-04T13:49:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; tetrakis(1,7-diammoniumheptane)dodecaiodotriplumbate(II) diiodide ; _chemical_formula_moiety '4(C7 H20 N2), I12 Pb3, 2(I)' _chemical_formula_sum 'C28 H80 I14 N8 Pb3' _chemical_formula_weight 2927.17 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.639(3) _cell_length_b 11.877(3) _cell_length_c 13.828(3) _cell_angle_alpha 68.680(5) _cell_angle_beta 71.022(5) _cell_angle_gamma 86.892(4) _cell_volume 1679.5(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 871 _cell_measurement_theta_min 2.989 _cell_measurement_theta_max 28.237 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 2.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1292 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.03 0 0 1 0.03 0 1 0 0.105 0 -1 0 0.105 -5 -5 -2 0.16 5 -4 1 0.19 -3 0 -1 0.2 3 0 1 0.2 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.959 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0555 _exptl_absorpt_correction_T_max 0.4242 _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 0.0304 _diffrn_reflns_av_unetI/netI 0.0383 _diffrn_reflns_number 8884 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 5863 _reflns_number_gt 4930 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0419P)^2^+16.5696P] 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 5863 _refine_ls_number_parameters 269 _refine_ls_number_restraints 152 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.674 _refine_diff_density_min -1.931 _refine_diff_density_rms 0.231 #----------------------------------------------------------------------------# # 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 0.8989(10) 0.7443(10) 0.1200(9) 0.033(3) Uani 1 1 d . . . H1D H 0.8641 0.7988 0.0647 0.04 Uiso 1 1 calc R . . H1E H 0.8333 0.7162 0.1921 0.04 Uiso 1 1 calc R . . C2 C 0.9452(10) 0.6367(10) 0.0893(9) 0.032(3) Uani 1 1 d . . . H2D H 0.9741 0.5798 0.1479 0.039 Uiso 1 1 calc R . . H2E H 1.0158 0.6648 0.0207 0.039 Uiso 1 1 calc R . . C3 C 0.8502(12) 0.5699(11) 0.0730(11) 0.043(3) Uani 1 1 d . . . H3D H 0.778 0.5466 0.1404 0.051 Uiso 1 1 calc R . . H3E H 0.8835 0.4942 0.0646 0.051 Uiso 1 1 calc R . . C4 C 0.8077(11) 0.6402(10) -0.0267(10) 0.038(3) Uani 1 1 d . . . H4D H 0.7596 0.5829 -0.0382 0.046 Uiso 1 1 calc R . . H4E H 0.7529 0.7017 -0.0087 0.046 Uiso 1 1 calc R . . C5 C 0.9103(11) 0.7035(10) -0.1337(10) 0.036(3) Uani 1 1 d . . . H5A H 0.951 0.769 -0.1255 0.043 Uiso 1 1 calc R . . H5B H 0.9712 0.6445 -0.1464 0.043 Uiso 1 1 calc R . . C6 C 0.8702(11) 0.7572(11) -0.2331(10) 0.038(3) Uani 1 1 d . . . H6A H 0.7862 0.7822 -0.2101 0.045 Uiso 1 1 calc R . . H6B H 0.8687 0.6942 -0.2638 0.045 Uiso 1 1 calc R . . C7 C 0.9530(12) 0.8671(11) -0.3233(10) 0.042(3) Uani 1 1 d . . . H7A H 0.9264 0.8932 -0.3888 0.051 Uiso 1 1 calc R . . H7B H 0.945 0.9351 -0.2968 0.051 Uiso 1 1 calc R . . C8 C 0.4193(18) 0.7777(12) 0.9696(13) 0.074(4) Uani 1 1 d DU A . H8A H 0.3314 0.7633 0.9833 0.089 Uiso 1 1 calc R . . H8B H 0.4287 0.769 1.0405 0.089 Uiso 1 1 calc R . . C9 C 0.4830(19) 0.6836(15) 0.9349(15) 0.085(4) Uani 1 1 d DU . . H9A H 0.4653 0.6049 0.9973 0.102 Uiso 0.607(19) 1 calc PR A 1 H9B H 0.5721 0.704 0.9052 0.102 Uiso 0.607(19) 1 calc PR A 1 H9C H 0.4249 0.6112 0.9779 0.102 Uiso 0.393(19) 1 d PR A 2 H9D H 0.5491 0.6687 0.9676 0.102 Uiso 0.393(19) 1 d PR A 2 C10A C 0.438(3) 0.678(3) 0.849(2) 0.088(5) Uani 0.607(19) 1 d PDU A 1 H10A H 0.3482 0.6606 0.8813 0.106 Uiso 0.607(19) 1 calc PR A 1 H10B H 0.4535 0.7595 0.7901 0.106 Uiso 0.607(19) 1 calc PR A 1 C11A C 0.489(3) 0.590(2) 0.800(2) 0.078(5) Uani 0.607(19) 1 d PDU A 1 H11A H 0.5735 0.5848 0.8025 0.093 Uiso 0.607(19) 1 calc PR A 1 H11B H 0.4453 0.5116 0.8542 0.093 Uiso 0.607(19) 1 calc PR A 1 C12A C 0.501(3) 0.584(2) 0.6938(16) 0.072(5) Uani 0.607(19) 1 d PDU A 1 H12A H 0.5494 0.5161 0.6837 0.086 Uiso 0.607(19) 1 calc PR A 1 H12B H 0.4188 0.5698 0.6914 0.086 Uiso 0.607(19) 1 calc PR A 1 C10B C 0.540(3) 0.671(4) 0.829(2) 0.076(5) Uani 0.393(19) 1 d PDU A 2 H10C H 0.5957 0.6043 0.8349 0.092 Uiso 0.393(19) 1 calc PR A 2 H10D H 0.5853 0.7469 0.7725 0.092 Uiso 0.393(19) 1 calc PR A 2 C11B C 0.434(4) 0.642(5) 0.806(3) 0.084(6) Uani 0.393(19) 1 d PDU A 2 H11C H 0.3706 0.6958 0.8258 0.101 Uiso 0.393(19) 1 calc PR A 2 H11D H 0.4026 0.5579 0.8566 0.101 Uiso 0.393(19) 1 calc PR A 2 C12B C 0.445(3) 0.649(5) 0.696(3) 0.089(6) Uani 0.393(19) 1 d PDU A 2 H12C H 0.4275 0.5662 0.7004 0.107 Uiso 0.393(19) 1 calc PR A 2 H12D H 0.3803 0.6987 0.6743 0.107 Uiso 0.393(19) 1 calc PR A 2 C13 C 0.559(2) 0.6972(18) 0.6059(15) 0.100(5) Uani 1 1 d DU . . H13A H 0.6376 0.7145 0.6128 0.12 Uiso 0.607(19) 1 calc PR A 1 H13B H 0.5068 0.7641 0.6139 0.12 Uiso 0.607(19) 1 calc PR A 1 H13C H 0.6243 0.6538 0.6326 0.12 Uiso 0.393(19) 1 d PR A 2 H13D H 0.5719 0.7831 0.5955 0.12 Uiso 0.393(19) 1 d PR A 2 C14 C 0.581(2) 0.6936(18) 0.4947(16) 0.091(5) Uani 1 1 d U A . H14A H 0.5052 0.6711 0.4868 0.109 Uiso 1 1 calc R . . H14B H 0.6423 0.6351 0.4802 0.109 Uiso 1 1 calc R . . N1 N 0.9990(8) 0.8125(8) 0.1257(8) 0.032(2) Uani 1 1 d . . . H1A H 0.9694 0.8777 0.1431 0.048 Uiso 1 1 calc R . . H1B H 1.0594 0.8383 0.0594 0.048 Uiso 1 1 calc R . . H1C H 1.0294 0.7632 0.1781 0.048 Uiso 1 1 calc R . . N2 N 1.0828(10) 0.8383(10) -0.3547(9) 0.051(3) Uani 1 1 d . . . H2A H 1.1294 0.9049 -0.4083 0.076 Uiso 1 1 calc R . . H2B H 1.0905 0.7765 -0.38 0.076 Uiso 1 1 calc R . . H2C H 1.1079 0.8158 -0.2949 0.076 Uiso 1 1 calc R . . N3 N 0.4561(8) 0.8990(8) 0.8964(8) 0.034(2) Uani 1 1 d . . . H3A H 0.4112 0.9503 0.9265 0.052 Uiso 1 1 calc R A . H3B H 0.4444 0.9098 0.8317 0.052 Uiso 1 1 calc R . . H3C H 0.5364 0.9146 0.8838 0.052 Uiso 1 1 calc R . . N4 N 0.6294(10) 0.8226(10) 0.4178(10) 0.051(3) Uani 1 1 d . . . H4A H 0.6489 0.828 0.3469 0.076 Uiso 1 1 calc R A . H4B H 0.697 0.8426 0.4292 0.076 Uiso 1 1 calc R . . H4C H 0.5712 0.8743 0.4312 0.076 Uiso 1 1 calc R . . I1 I 0.19244(6) 0.57711(6) 0.25470(6) 0.02770(16) Uani 1 1 d . . . I2 I -0.20469(7) 0.42983(7) 0.41767(6) 0.03634(19) Uani 1 1 d . . . I3 I -0.05041(7) 0.78359(6) 0.42523(6) 0.03497(18) Uani 1 1 d . . . I4 I 0.25297(6) 0.98961(6) 0.11258(6) 0.02864(17) Uani 1 1 d . . . I5 I 0.34799(7) 0.98126(7) 0.41197(6) 0.03690(19) Uani 1 1 d . . . I6 I 0.53706(7) 0.76322(7) 0.21591(7) 0.0396(2) Uani 1 1 d . . . I7 I 0.17643(6) 0.94006(6) 0.82910(6) 0.03179(17) Uani 1 1 d . . . Pb1 Pb 0 0.5 0.5 0.02653(14) Uani 1 2 d S . . Pb2 Pb 0.26775(4) 0.78500(3) 0.32562(3) 0.02454(11) 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 0.035(6) 0.037(6) 0.026(6) -0.008(5) -0.013(5) 0.003(5) C2 0.036(6) 0.027(6) 0.028(6) -0.004(5) -0.009(5) 0.000(5) C3 0.048(7) 0.031(6) 0.043(7) -0.006(6) -0.015(6) -0.007(5) C4 0.039(7) 0.031(6) 0.042(7) -0.006(5) -0.016(6) -0.011(5) C5 0.040(7) 0.027(6) 0.040(7) -0.015(5) -0.010(6) 0.008(5) C6 0.039(7) 0.044(7) 0.035(7) -0.020(6) -0.012(6) 0.002(5) C7 0.065(9) 0.035(7) 0.024(6) -0.005(5) -0.016(6) 0.001(6) C8 0.122(13) 0.038(7) 0.052(8) -0.006(6) -0.028(8) 0.005(7) C9 0.115(11) 0.060(8) 0.076(8) -0.029(7) -0.022(8) 0.007(7) C10A 0.116(12) 0.070(10) 0.072(9) -0.029(7) -0.016(9) -0.006(10) C11A 0.100(12) 0.061(10) 0.072(7) -0.024(6) -0.027(9) -0.007(9) C12A 0.086(12) 0.058(10) 0.077(8) -0.028(6) -0.031(10) 0.002(9) C10B 0.096(12) 0.059(11) 0.071(9) -0.026(8) -0.020(9) -0.006(10) C11B 0.098(12) 0.071(12) 0.074(8) -0.017(10) -0.026(9) -0.009(11) C12B 0.106(12) 0.079(12) 0.081(8) -0.028(10) -0.029(8) -0.010(11) C13 0.122(11) 0.094(10) 0.071(7) -0.017(7) -0.027(8) -0.016(9) C14 0.111(13) 0.084(11) 0.075(7) -0.023(8) -0.034(9) -0.007(10) N1 0.035(5) 0.034(5) 0.027(5) -0.010(4) -0.011(4) 0.000(4) N2 0.050(7) 0.053(7) 0.035(6) -0.015(5) 0.005(5) -0.002(5) N3 0.034(5) 0.023(5) 0.041(6) -0.008(4) -0.010(5) -0.002(4) N4 0.037(6) 0.048(7) 0.059(8) -0.009(6) -0.017(6) -0.001(5) I1 0.0281(3) 0.0251(3) 0.0275(4) -0.0089(3) -0.0067(3) -0.0006(3) I2 0.0411(4) 0.0342(4) 0.0313(4) -0.0033(3) -0.0182(3) -0.0003(3) I3 0.0395(4) 0.0267(4) 0.0320(4) -0.0055(3) -0.0102(3) 0.0087(3) I4 0.0325(4) 0.0253(4) 0.0246(4) -0.0044(3) -0.0099(3) -0.0002(3) I5 0.0442(4) 0.0341(4) 0.0334(4) -0.0152(3) -0.0099(4) -0.0030(3) I6 0.0264(4) 0.0420(4) 0.0500(5) -0.0180(4) -0.0105(3) 0.0018(3) I7 0.0297(4) 0.0327(4) 0.0313(4) -0.0074(3) -0.0123(3) 0.0002(3) Pb1 0.0283(3) 0.0207(3) 0.0243(3) -0.0010(2) -0.0082(2) -0.0029(2) Pb2 0.0267(2) 0.0218(2) 0.0225(2) -0.00510(16) -0.00751(17) -0.00185(15) #----------------------------------------------------------------------------# # 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 1.494(14) . ? C1 C2 1.507(15) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.514(16) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? C3 C4 1.550(17) . ? C3 H3D 0.99 . ? C3 H3E 0.99 . ? C4 C5 1.523(16) . ? C4 H4D 0.99 . ? C4 H4E 0.99 . ? C5 C6 1.503(16) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.536(17) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 N2 1.488(16) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N3 1.417(17) . ? C8 C9 1.449(12) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10B 1.455(13) . ? C9 C10A 1.465(12) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C9 H9C 0.99 . ? C9 H9D 0.99 . ? C10A C11A 1.457(12) . ? C10A H10A 0.99 . ? C10A H10B 0.99 . ? C11A C12A 1.455(12) . ? C11A H11A 0.99 . ? C11A H11B 0.99 . ? C12A C13 1.455(12) . ? C12A H12A 0.99 . ? C12A H12B 0.99 . ? C10B C11B 1.458(13) . ? C10B H10C 0.99 . ? C10B H10D 0.99 . ? C11B C12B 1.458(13) . ? C11B H11C 0.99 . ? C11B H11D 0.99 . ? C12B C13 1.454(13) . ? C12B H12C 0.99 . ? C12B H12D 0.99 . ? C13 C14 1.49(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C13 H13C 0.99 . ? C13 H13D 0.99 . ? C14 N4 1.52(2) . ? C14 H14A 0.99 . ? C14 H14B 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 Pb2 3.2221(10) . ? I1 Pb1 3.2224(9) . ? I2 Pb1 3.2150(9) . ? I2 Pb2 3.4019(11) 2_566 ? I3 Pb1 3.2260(10) . ? I3 Pb2 3.5047(12) . ? I4 Pb2 3.1133(10) . ? I5 Pb2 3.2735(10) . ? I6 Pb2 3.0493(11) . ? Pb1 I2 3.2150(9) 2_566 ? Pb1 I1 3.2224(9) 2_566 ? Pb1 I3 3.2260(10) 2_566 ? Pb2 I2 3.4019(11) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.0(9) . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? N1 C1 H1E 109.4 . . ? C2 C1 H1E 109.4 . . ? H1D C1 H1E 108 . . ? C1 C2 C3 113.4(10) . . ? C1 C2 H2D 108.9 . . ? C3 C2 H2D 108.9 . . ? C1 C2 H2E 108.9 . . ? C3 C2 H2E 108.9 . . ? H2D C2 H2E 107.7 . . ? C2 C3 C4 116.0(10) . . ? C2 C3 H3D 108.3 . . ? C4 C3 H3D 108.3 . . ? C2 C3 H3E 108.3 . . ? C4 C3 H3E 108.3 . . ? H3D C3 H3E 107.4 . . ? C5 C4 C3 114.7(10) . . ? C5 C4 H4D 108.6 . . ? C3 C4 H4D 108.6 . . ? C5 C4 H4E 108.6 . . ? C3 C4 H4E 108.6 . . ? H4D C4 H4E 107.6 . . ? C6 C5 C4 114.5(10) . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C5 C6 C7 113.4(10) . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C6 111.6(10) . . ? N2 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 108 . . ? N3 C8 C9 116.8(14) . . ? N3 C8 H8A 108.1 . . ? C9 C8 H8A 108.1 . . ? N3 C8 H8B 108.1 . . ? C9 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C8 C9 C10B 135(2) . . ? C8 C9 C10A 105.4(18) . . ? C10B C9 C10A 46(2) . . ? C8 C9 H9A 110.7 . . ? C10B C9 H9A 112.5 . . ? C10A C9 H9A 110.7 . . ? C8 C9 H9B 110.7 . . ? C10B C9 H9B 67.1 . . ? C10A C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? C8 C9 H9C 103.6 . . ? C10B C9 H9C 103.6 . . ? C10A C9 H9C 80.2 . . ? H9B C9 H9C 139 . . ? C8 C9 H9D 103.5 . . ? C10B C9 H9D 103.5 . . ? C10A C9 H9D 148.4 . . ? H9A C9 H9D 69.9 . . ? H9B C9 H9D 45.6 . . ? H9C C9 H9D 105.3 . . ? C11A C10A C9 116(2) . . ? C11A C10A H10A 108.3 . . ? C9 C10A H10A 108.3 . . ? C11A C10A H10B 108.3 . . ? C9 C10A H10B 108.3 . . ? H10A C10A H10B 107.4 . . ? C12A C11A C10A 131(3) . . ? C12A C11A H11A 104.4 . . ? C10A C11A H11A 104.4 . . ? C12A C11A H11B 104.4 . . ? C10A C11A H11B 104.4 . . ? H11A C11A H11B 105.6 . . ? C13 C12A C11A 110(2) . . ? C13 C12A H12A 109.6 . . ? C11A C12A H12A 109.6 . . ? C13 C12A H12B 109.6 . . ? C11A C12A H12B 109.6 . . ? H12A C12A H12B 108.1 . . ? C11A C12A H13C 96.1 . . ? H12A C12A H13C 81.7 . . ? H12B C12A H13C 146.4 . . ? C9 C10B C11B 102(3) . . ? C9 C10B H10C 111.5 . . ? C11B C10B H10C 111.5 . . ? C9 C10B H10D 111.5 . . ? C11B C10B H10D 111.5 . . ? H10C C10B H10D 109.3 . . ? C10B C11B C12B 120(4) . . ? C10B C11B H11C 107.3 . . ? C12B C11B H11C 107.3 . . ? C10B C11B H11D 107.3 . . ? C12B C11B H11D 107.3 . . ? H11C C11B H11D 106.9 . . ? C13 C12B C11B 120(4) . . ? C13 C12B H12C 107.3 . . ? C11B C12B H12C 107.3 . . ? C13 C12B H12D 107.3 . . ? C11B C12B H12D 107.3 . . ? H12C C12B H12D 106.9 . . ? C12B C13 C14 123(2) . . ? C12A C13 C14 112.6(19) . . ? C12B C13 H13A 126.3 . . ? C12A C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12B C13 H13B 70.1 . . ? C12A C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C12B C13 H13C 106.1 . . ? C12A C13 H13C 74 . . ? C14 C13 H13C 106.6 . . ? H13B C13 H13C 139 . . ? C12B C13 H13D 107.2 . . ? C12A C13 H13D 138.7 . . ? C14 C13 H13D 106.8 . . ? H13A C13 H13D 67.7 . . ? H13C C13 H13D 106.6 . . ? C13 C14 N4 103.4(15) . . ? C13 C14 H14A 111.1 . . ? N4 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? N4 C14 H14B 111.1 . . ? H14A C14 H14B 109 . . ? 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 . . ? C7 N2 H2A 109.5 . . ? C7 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C7 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C8 N3 H3A 109.5 . . ? C8 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C8 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C14 N4 H4A 109.5 . . ? C14 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C14 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? Pb2 I1 Pb1 80.41(2) . . ? Pb1 I2 Pb2 77.85(2) . 2_566 ? Pb1 I3 Pb2 76.227(17) . . ? I2 Pb1 I2 180 2_566 . ? I2 Pb1 I1 90.05(3) 2_566 2_566 ? I2 Pb1 I1 89.95(3) . 2_566 ? I2 Pb1 I1 89.95(3) 2_566 . ? I2 Pb1 I1 90.05(3) . . ? I1 Pb1 I1 180 2_566 . ? I2 Pb1 I3 86.11(2) 2_566 . ? I2 Pb1 I3 93.89(2) . . ? I1 Pb1 I3 95.818(19) 2_566 . ? I1 Pb1 I3 84.182(19) . . ? I2 Pb1 I3 93.89(2) 2_566 2_566 ? I2 Pb1 I3 86.11(2) . 2_566 ? I1 Pb1 I3 84.182(19) 2_566 2_566 ? I1 Pb1 I3 95.818(19) . 2_566 ? I3 Pb1 I3 180 . 2_566 ? I6 Pb2 I4 91.60(3) . . ? I6 Pb2 I1 90.82(2) . . ? I4 Pb2 I1 92.17(3) . . ? I6 Pb2 I5 88.54(3) . . ? I4 Pb2 I5 91.77(3) . . ? I1 Pb2 I5 176.02(2) . . ? I6 Pb2 I2 103.35(2) . 2_566 ? I4 Pb2 I2 165.02(2) . 2_566 ? I1 Pb2 I2 86.72(3) . 2_566 ? I5 Pb2 I2 89.60(3) . 2_566 ? I6 Pb2 I3 170.26(2) . . ? I4 Pb2 I3 86.03(2) . . ? I1 Pb2 I3 79.85(2) . . ? I5 Pb2 I3 100.96(2) . . ? I2 Pb2 I3 79.07(2) 2_566 . ? 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 -175.2(9) . . . . ? C1 C2 C3 C4 66.7(14) . . . . ? C2 C3 C4 C5 46.8(15) . . . . ? C3 C4 C5 C6 172.1(10) . . . . ? C4 C5 C6 C7 152.0(10) . . . . ? C5 C6 C7 N2 53.7(14) . . . . ? N3 C8 C9 C10B -32(4) . . . . ? N3 C8 C9 C10A -74(2) . . . . ? C8 C9 C10A C11A 180(3) . . . . ? C10B C9 C10A C11A 41(3) . . . . ? C9 C10A C11A C12A -156(3) . . . . ? C10A C11A C12A C13 53(5) . . . . ? C8 C9 C10B C11B -78(5) . . . . ? C10A C9 C10B C11B -14(3) . . . . ? C9 C10B C11B C12B 165(5) . . . . ? C10B C11B C12B C13 -6(8) . . . . ? C11B C12B C13 C12A 86(5) . . . . ? C11B C12B C13 C14 173(4) . . . . ? C11A C12A C13 C12B -70(4) . . . . ? C11A C12A C13 C14 176(2) . . . . ? C12B C13 C14 N4 131(3) . . . . ? C12A C13 C14 N4 174(2) . . . . ? Pb2 I2 Pb1 I1 -36.213(19) 2_566 . . 2_566 ? Pb2 I2 Pb1 I1 143.787(19) 2_566 . . . ? Pb2 I2 Pb1 I3 -132.04(2) 2_566 . . . ? Pb2 I2 Pb1 I3 47.96(2) 2_566 . . 2_566 ? Pb2 I1 Pb1 I2 -38.202(18) . . . 2_566 ? Pb2 I1 Pb1 I2 141.798(18) . . . . ? Pb2 I1 Pb1 I3 47.89(2) . . . . ? Pb2 I1 Pb1 I3 -132.11(2) . . . 2_566 ? Pb2 I3 Pb1 I2 46.52(2) . . . 2_566 ? Pb2 I3 Pb1 I2 -133.48(2) . . . . ? Pb2 I3 Pb1 I1 136.176(18) . . . 2_566 ? Pb2 I3 Pb1 I1 -43.824(18) . . . . ? Pb1 I1 Pb2 I6 139.16(2) . . . . ? Pb1 I1 Pb2 I4 -129.21(2) . . . . ? Pb1 I1 Pb2 I2 35.832(19) . . . 2_566 ? Pb1 I1 Pb2 I3 -43.644(17) . . . . ? Pb1 I3 Pb2 I4 137.35(2) . . . . ? Pb1 I3 Pb2 I1 44.42(2) . . . . ? Pb1 I3 Pb2 I5 -131.62(2) . . . . ? Pb1 I3 Pb2 I2 -44.170(18) . . . 2_566 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I7 0.91 2.74 3.613(9) 162 2_676 N1 H1B I7 0.91 2.83 3.700(9) 160 1_654 N1 H1C I1 0.91 2.96 3.791(9) 153 1_655 N2 H2A I5 0.91 2.82 3.596(10) 143 1_654 N2 H2B I2 0.91 2.86 3.692(11) 153 2_665 N2 H2C I7 0.91 2.93 3.645(12) 136 1_654 N3 H3A I4 0.91 2.82 3.627(10) 149 1_556 N3 H3B I7 0.91 3.13 3.628(10) 117 . N3 H3C I4 0.91 2.78 3.651(9) 161 2_676 N4 H4A I6 0.91 2.87 3.593(12) 138 . N4 H4B I3 0.91 2.97 3.760(10) 146 1_655 N4 H4C I5 0.91 2.88 3.699(11) 151 . ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-11-03 at 10:38:56 # 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 : 3ad21_a smart data_4 _database_code_depnum_ccdc_archive 'CCDC 853209' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-11-03T10:38:56-00:00 _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(1,8-diammoniumoctane)tetraiodoplumbate(II) ; _chemical_formula_moiety 'C8 H22 N2, I4 Pb ' _chemical_formula_sum 'C8 H22 I4 N2 Pb' _chemical_formula_weight 861.07 #----------------------------------------------------------------------------# # 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 13.815(3) _cell_length_b 8.3815(15) _cell_length_c 9.0264(16) _cell_angle_alpha 90 _cell_angle_beta 106.749(3) _cell_angle_gamma 90 _cell_volume 1000.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 873 _cell_measurement_theta_min 2.877 _cell_measurement_theta_max 28.242 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description polyhedral _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 2.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 5 -3 0.155 5 -2 -3 0.12 -7 -3 2 0.18 5 2 -3 0.16 -1 0 2 0.105 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 14.581 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0324 _exptl_absorpt_correction_T_max 0.1177 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.1245 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_number 6543 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2399 _reflns_number_gt 2164 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0923P)^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 2399 _refine_ls_number_parameters 70 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0616 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1372 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.701 _refine_diff_density_min -6.126 _refine_diff_density_rms 0.481 #----------------------------------------------------------------------------# # 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 0.2978(10) 0.931(2) 0.5668(13) 0.080(3) Uani 1 1 d U . . H1D H 0.3446 0.9703 0.5132 0.096 Uiso 1 1 calc R . . H1E H 0.2885 0.8175 0.5466 0.096 Uiso 1 1 calc R . . C2 C 0.3415(9) 0.959(2) 0.7391(14) 0.073(3) Uani 1 1 d U . . H2A H 0.2956 0.9153 0.7925 0.088 Uiso 1 1 calc R . . H2B H 0.3474 1.0724 0.7591 0.088 Uiso 1 1 calc R . . C3 C 0.4443(11) 0.882(2) 0.8026(13) 0.083(3) Uani 1 1 d U . . H3A H 0.49 0.9235 0.7482 0.099 Uiso 1 1 calc R . . H3B H 0.4383 0.7674 0.7843 0.099 Uiso 1 1 calc R . . C4 C 0.4890(9) 0.9126(19) 0.9775(12) 0.070(3) Uani 1 1 d U . . H4A H 0.4422 0.8718 1.0304 0.084 Uiso 1 1 calc R . . H4B H 0.5514 0.8526 1.0143 0.084 Uiso 1 1 calc R . . N1 N 0.2001(8) 1.0134(11) 0.5079(12) 0.061(2) Uani 1 1 d U . . H1A H 0.175 0.9949 0.407 0.091 Uiso 1 1 calc R . . H1B H 0.209 1.1178 0.5241 0.091 Uiso 1 1 calc R . . H1C H 0.1572 0.9773 0.5572 0.091 Uiso 1 1 calc R . . I1 I 0.23650(4) 1.07287(8) 1.13054(7) 0.0552(2) Uani 1 1 d . . . I2 I -0.04399(4) 1.19109(7) 1.28221(6) 0.0499(2) Uani 1 1 d . . . Pb1 Pb 0 1 1 0.03666(17) 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 0.065(6) 0.105(9) 0.062(5) 0.004(6) 0.005(4) 0.021(6) C2 0.052(5) 0.103(7) 0.061(4) 0.003(5) 0.009(4) 0.002(6) C3 0.071(6) 0.095(8) 0.068(5) -0.005(6) -0.002(5) 0.014(6) C4 0.055(5) 0.086(8) 0.065(5) 0.000(5) 0.010(4) 0.002(5) N1 0.053(5) 0.068(5) 0.056(5) 0.002(3) 0.007(4) 0.001(4) I1 0.0411(3) 0.0649(4) 0.0600(4) 0.0031(3) 0.0154(2) -0.0048(2) I2 0.0569(3) 0.0502(3) 0.0448(3) -0.0158(2) 0.0181(2) 0.0011(2) Pb1 0.0391(2) 0.0400(3) 0.0319(2) -0.00047(12) 0.01176(16) -0.00035(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.472(15) . ? C1 C2 1.515(16) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.515(18) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.543(14) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C4 1.53(3) 3_677 ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1965(8) . ? I2 Pb1 3.2014(7) 2_557 ? I2 Pb1 3.2118(6) . ? Pb1 I1 3.1965(8) 3_577 ? Pb1 I2 3.2014(6) 4_585 ? Pb1 I2 3.2014(6) 2_547 ? Pb1 I2 3.2118(6) 3_577 ? 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 110.6(11) . . ? 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 C3 112.1(12) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 C4 111.7(12) . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C4 C4 C3 115.1(14) 3_677 . ? C4 C4 H4A 108.5 3_677 . ? C3 C4 H4A 108.5 . . ? C4 C4 H4B 108.5 3_677 . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? 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 147.62(2) 2_557 . ? I1 Pb1 I1 180.000(9) 3_577 . ? I1 Pb1 I2 86.283(16) 3_577 4_585 ? I1 Pb1 I2 93.717(16) . 4_585 ? I1 Pb1 I2 93.717(16) 3_577 2_547 ? I1 Pb1 I2 86.283(16) . 2_547 ? I2 Pb1 I2 180 4_585 2_547 ? I1 Pb1 I2 91.105(18) 3_577 3_577 ? I1 Pb1 I2 88.895(18) . 3_577 ? I2 Pb1 I2 87.827(14) 4_585 3_577 ? I2 Pb1 I2 92.173(14) 2_547 3_577 ? I1 Pb1 I2 88.895(18) 3_577 . ? I1 Pb1 I2 91.105(18) . . ? I2 Pb1 I2 92.172(14) 4_585 . ? I2 Pb1 I2 87.827(14) 2_547 . ? I2 Pb1 I2 180 3_577 . ? 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 -177.5(13) . . . . ? C1 C2 C3 C4 179.0(14) . . . . ? C2 C3 C4 C4 -63.7(18) . . . 3_677 ? Pb1 I2 Pb1 I1 -136.77(4) 2_557 . . 3_577 ? Pb1 I2 Pb1 I1 43.23(4) 2_557 . . . ? Pb1 I2 Pb1 I2 -50.54(5) 2_557 . . 4_585 ? Pb1 I2 Pb1 I2 129.46(5) 2_557 . . 2_547 ? 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 0.89 2.93 3.618(11) 135 1_554 N1 H1B I1 0.89 2.75 3.631(9) 169 4_585 N1 H1C I2 0.89 2.8 3.678(11) 169 3_577 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-11-03 at 11:11:06 # 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 : 4ad65l_n smart data_5 _database_code_depnum_ccdc_archive 'CCDC 853210' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-11-03T11:11:06-00:00 _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(1,10-diammoniumdecane)tetrabromoplumbate(II) ; _chemical_formula_sum 'C10 H26 Br4 N2 Pb' _chemical_formula_moiety 'C10 H26 N2, Br4 Pb' _chemical_formula_weight 701.16 #----------------------------------------------------------------------------# # 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 14.651(6) _cell_length_b 7.926(3) _cell_length_c 8.455(3) _cell_angle_alpha 90 _cell_angle_beta 96.709(8) _cell_angle_gamma 90 _cell_volume 975.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 909 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 28.1735 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.025 -1 0 0 0.025 0 0 1 0.17 0 0 -1 0.17 0 -1 0 0.22 -1 4 -3 0.18 1 4 4 0.2 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.833 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0217 _exptl_absorpt_correction_T_max 0.4354 _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 0.0735 _diffrn_reflns_av_unetI/netI 0.0426 _diffrn_reflns_number 7935 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.4 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1710 _reflns_number_gt 1551 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0845P)^2^+28.9177P] 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 1710 _refine_ls_number_parameters 80 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1667 _refine_ls_wR_factor_gt 0.1597 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.582 _refine_diff_density_min -1.953 _refine_diff_density_rms 0.452 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7641(9) -0.0100(16) 0.4381(18) 0.027(3) Uani 1 1 d DU . . H1D H 0.7807 -0.131 0.4381 0.033 Uiso 1 1 calc R . . H1E H 0.7691 0.0368 0.3309 0.033 Uiso 1 1 calc R . . C2 C 0.6660(9) 0.0117(18) 0.4811(19) 0.034(3) Uani 1 1 d DU . . H2A H 0.6615 -0.0404 0.5863 0.041 Uiso 1 1 calc R . . H2B H 0.6523 0.1335 0.4894 0.041 Uiso 1 1 calc R . . C3 C 0.5945(11) -0.069(2) 0.3570(14) 0.033(3) Uani 1 1 d DU . . H3A H 0.6129 -0.1871 0.3391 0.04 Uiso 1 1 calc R . . H3B H 0.5345 -0.0716 0.3997 0.04 Uiso 1 1 calc R . . C4 C 0.5835(11) 0.0243(19) 0.1974(14) 0.031(3) Uani 1 1 d DU . . H4A H 0.5724 0.1453 0.217 0.037 Uiso 1 1 calc R . . H4B H 0.6416 0.0153 0.1489 0.037 Uiso 1 1 calc R . . C5 C 0.5048(10) -0.044(2) 0.0797(17) 0.031(3) Uani 1 1 d DU . . H5A H 0.5149 -0.1655 0.0632 0.037 Uiso 1 1 calc R . . H5B H 0.4465 -0.0313 0.1271 0.037 Uiso 1 1 calc R . . N1 N 0.8264(8) 0.0828(15) 0.5608(13) 0.025(2) Uani 1 1 d U . . H1A H 0.8106 0.1939 0.5594 0.038 Uiso 1 1 calc R . . H1B H 0.8855 0.0723 0.5389 0.038 Uiso 1 1 calc R . . H1C H 0.8211 0.0388 0.6587 0.038 Uiso 1 1 calc R . . Br1 Br 0.79390(11) 0.00919(16) 0.9455(2) 0.0274(4) Uani 1 1 d . . . Br2 Br 0.99283(11) 0.17690(16) 1.31395(15) 0.0250(4) Uani 1 1 d . . . Pb1 Pb 1 0 1 0.0161(3) 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 0.036(5) 0.024(6) 0.017(6) 0.001(4) -0.019(5) 0.005(5) C2 0.037(5) 0.037(6) 0.026(6) 0.002(5) -0.006(5) -0.005(5) C3 0.036(5) 0.037(6) 0.025(5) 0.003(5) -0.001(5) -0.007(5) C4 0.035(6) 0.036(6) 0.021(5) -0.002(5) 0.001(5) -0.004(5) C5 0.031(7) 0.037(6) 0.024(6) -0.001(6) 0.002(5) -0.003(6) N1 0.031(5) 0.027(6) 0.017(5) -0.001(4) -0.004(4) -0.002(5) Br1 0.0264(8) 0.0256(8) 0.0305(9) -0.0031(5) 0.0046(7) -0.0027(5) Br2 0.0375(8) 0.0198(7) 0.0181(7) -0.0060(5) 0.0047(5) 0.0044(6) Pb1 0.0224(4) 0.0137(4) 0.0125(4) 0.0000(2) 0.0036(3) 0.0007(2) #----------------------------------------------------------------------------# # 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 1.493(17) . ? C1 C2 1.533(11) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.532(11) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.531(11) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.529(11) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C5 1.51(3) 3_655 ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? Br1 Pb1 3.002(2) . ? Br2 Pb1 3.0008(15) 2_757 ? Br2 Pb1 3.0148(16) . ? Pb1 Br2 3.0008(15) 2_747 ? Pb1 Br2 3.0008(15) 4_565 ? Pb1 Br1 3.002(2) 3_757 ? Pb1 Br2 3.0148(16) 3_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 107.2(12) . . ? N1 C1 H1D 110.3 . . ? C2 C1 H1D 110.3 . . ? N1 C1 H1E 110.3 . . ? C2 C1 H1E 110.3 . . ? H1D C1 H1E 108.5 . . ? C3 C2 C1 112.1(13) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 113.3(12) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 113.5(13) . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4B 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C5 C5 C4 113.9(16) 3_655 . ? C5 C5 H5A 108.8 3_655 . ? C4 C5 H5A 108.8 . . ? C5 C5 H5B 108.8 3_655 . ? C4 C5 H5B 108.8 . . ? 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 Br2 Pb1 148.85(5) 2_757 . ? Br2 Pb1 Br2 180 2_747 4_565 ? Br2 Pb1 Br1 94.26(4) 2_747 . ? Br2 Pb1 Br1 85.74(4) 4_565 . ? Br2 Pb1 Br1 85.74(4) 2_747 3_757 ? Br2 Pb1 Br1 94.26(4) 4_565 3_757 ? Br1 Pb1 Br1 180 . 3_757 ? Br2 Pb1 Br2 86.44(3) 2_747 . ? Br2 Pb1 Br2 93.56(3) 4_565 . ? Br1 Pb1 Br2 89.20(4) . . ? Br1 Pb1 Br2 90.80(4) 3_757 . ? Br2 Pb1 Br2 93.56(3) 2_747 3_757 ? Br2 Pb1 Br2 86.44(3) 4_565 3_757 ? Br1 Pb1 Br2 90.80(4) . 3_757 ? Br1 Pb1 Br2 89.20(4) 3_757 3_757 ? Br2 Pb1 Br2 180 . 3_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 C3 176.3(11) . . . . ? C1 C2 C3 C4 -69.6(17) . . . . ? C2 C3 C4 C5 -173.5(14) . . . . ? C3 C4 C5 C5 -178.1(17) . . . 3_655 ? Pb1 Br2 Pb1 Br2 170.72(14) 2_757 . . 2_747 ? Pb1 Br2 Pb1 Br2 -9.28(14) 2_757 . . 4_565 ? Pb1 Br2 Pb1 Br1 -94.96(11) 2_757 . . . ? Pb1 Br2 Pb1 Br1 85.04(11) 2_757 . . 3_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 H1B Br2 0.91 2.73 3.471(12) 139 1_554 N1 H1C Br1 0.91 2.51 3.393(12) 162 . N1 H1A Br1 0.91 2.54 3.395(12) 156 4_565 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-11-25 at 09:47:21 # 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 : 5ad111l_a apex data_6 _database_code_depnum_ccdc_archive 'CCDC 853211' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-11-25T09:47:21-00:00 _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(1,12-diammoniumdodecane)tetraiodoplumbate(II) ; _chemical_formula_sum 'C12 H30 I4 N2 Pb' _chemical_formula_moiety 'C12 H30 N2, I4 Pb' _chemical_formula_weight 917.17 #----------------------------------------------------------------------------# # 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 15.8186(8) _cell_length_b 8.4304(4) _cell_length_c 8.8539(4) _cell_angle_alpha 90 _cell_angle_beta 90.231(3) _cell_angle_gamma 90 _cell_volume 1180.72(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3366 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.24 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 2.58 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.005 1 0 0 0.005 0 -1 0 0.1 0 1 0 0.1 0 -1 -1 0.16 0 -2 3 0.16 0 1 -1 0.16 0 1 1 0.15 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.368 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1313 _exptl_absorpt_correction_T_max 0.876 _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 0.0703 _diffrn_reflns_av_unetI/netI 0.0559 _diffrn_reflns_number 8492 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 2840 _reflns_number_gt 2393 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0628P)^2^+35.6924P] 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 2840 _refine_ls_number_parameters 88 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1684 _refine_ls_goodness_of_fit_ref 1.286 _refine_ls_restrained_S_all 1.275 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.41 _refine_diff_density_min -3.443 _refine_diff_density_rms 0.526 #----------------------------------------------------------------------------# # 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 0.2266(10) 0.999(2) 0.499(2) 0.035(3) Uani 1 1 d DU . . H1D H 0.2224 0.9595 0.3941 0.042 Uiso 1 1 calc R . . H1E H 0.2103 1.1127 0.4993 0.042 Uiso 1 1 calc R . . C2 C 0.3177(9) 0.982(3) 0.556(2) 0.044(4) Uani 1 1 d DU . . H2A H 0.3228 1.0264 0.6594 0.053 Uiso 1 1 calc R . . H2B H 0.3334 0.8681 0.5605 0.053 Uiso 1 1 calc R . . C3 C 0.3768(12) 1.070(3) 0.4492(18) 0.047(4) Uani 1 1 d DU . . H3A H 0.4299 1.0961 0.503 0.056 Uiso 1 1 calc R . . H3B H 0.3499 1.1707 0.4176 0.056 Uiso 1 1 calc R . . C4 C 0.3971(10) 0.971(2) 0.3092(16) 0.038(3) Uani 1 1 d DU . . H4A H 0.4239 0.8705 0.3418 0.045 Uiso 1 1 calc R . . H4B H 0.3435 0.9438 0.2571 0.045 Uiso 1 1 calc R . . C5 C 0.4554(12) 1.054(3) 0.1974(17) 0.043(4) Uani 1 1 d DU . . H5A H 0.51 1.0766 0.2483 0.052 Uiso 1 1 calc R . . H5B H 0.4299 1.1572 0.1689 0.052 Uiso 1 1 calc R . . C6 C 0.4726(14) 0.959(3) 0.054(2) 0.048(4) Uani 1 1 d DU . . H6A H 0.4991 0.8571 0.0818 0.058 Uiso 1 1 calc R . . H6B H 0.418 0.9356 0.0034 0.058 Uiso 1 1 calc R . . N1 N 0.1662(10) 0.904(2) 0.6024(18) 0.041(4) Uani 1 1 d U . . H1B H 0.1125 0.9112 0.566 0.062 Uiso 1 1 calc R . . H1A H 0.1683 0.9441 0.6977 0.062 Uiso 1 1 calc R . . H1C H 0.1824 0.8003 0.6041 0.062 Uiso 1 1 calc R . . I1 I 0.20267(6) 1.00138(12) 0.99749(12) 0.0261(3) Uani 1 1 d . . . I2 I 0.00356(7) 0.82412(11) 1.31772(10) 0.0251(3) Uani 1 1 d . . . Pb1 Pb 0 1 1 0.0169(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 0.032(6) 0.035(8) 0.037(8) 0.005(6) 0.009(6) 0.003(6) C2 0.033(6) 0.059(10) 0.041(7) -0.003(7) 0.006(6) -0.008(7) C3 0.035(7) 0.065(10) 0.040(7) -0.003(7) 0.007(6) -0.007(8) C4 0.021(7) 0.055(9) 0.037(7) 0.006(6) 0.000(5) 0.011(6) C5 0.031(8) 0.060(10) 0.039(7) 0.002(7) 0.004(6) 0.002(7) C6 0.043(10) 0.061(11) 0.040(8) -0.001(8) 0.008(7) -0.004(9) N1 0.036(7) 0.040(8) 0.049(9) -0.003(7) 0.005(6) -0.014(7) I1 0.0194(5) 0.0298(5) 0.0292(5) -0.0005(4) -0.0004(4) -0.0018(4) I2 0.0362(5) 0.0192(4) 0.0199(4) 0.0054(4) 0.0017(3) 0.0025(4) Pb1 0.0180(4) 0.0165(3) 0.0162(3) 0.0003(2) 0.0005(3) 0.0005(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 C2 1.533(13) . ? C1 N1 1.55(2) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.527(13) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.529(13) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.527(13) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.529(13) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C6 1.46(4) 3_675 ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? N1 H1B 0.91 . ? N1 H1A 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.2061(10) . ? I2 Pb1 3.1741(9) 2_547 ? I2 Pb1 3.1802(9) . ? Pb1 I2 3.1741(9) 4_575 ? Pb1 I2 3.1741(9) 2_557 ? Pb1 I2 3.1802(9) 3_577 ? Pb1 I1 3.2061(10) 3_577 ? 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 109.6(14) . . ? C2 C1 H1D 109.7 . . ? N1 C1 H1D 109.7 . . ? C2 C1 H1E 109.7 . . ? N1 C1 H1E 109.7 . . ? H1D C1 H1E 108.2 . . ? C3 C2 C1 108.9(16) . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 C3 C4 111.6(17) . . ? 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 113.8(17) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 114.2(17) . . ? C4 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? C4 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C6 C6 C5 114(2) 3_675 . ? C6 C6 H6A 108.8 3_675 . ? C5 C6 H6A 108.8 . . ? C6 C6 H6B 108.8 3_675 . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C1 N1 H1B 109.5 . . ? C1 N1 H1A 109.5 . . ? H1B N1 H1A 109.5 . . ? C1 N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? Pb1 I2 Pb1 148.30(3) 2_547 . ? I2 Pb1 I2 180 4_575 2_557 ? I2 Pb1 I2 92.757(9) 4_575 . ? I2 Pb1 I2 87.243(9) 2_557 . ? I2 Pb1 I2 87.243(9) 4_575 3_577 ? I2 Pb1 I2 92.757(9) 2_557 3_577 ? I2 Pb1 I2 180 . 3_577 ? I2 Pb1 I1 88.84(3) 4_575 . ? I2 Pb1 I1 91.16(3) 2_557 . ? I2 Pb1 I1 89.64(3) . . ? I2 Pb1 I1 90.36(3) 3_577 . ? I2 Pb1 I1 91.16(3) 4_575 3_577 ? I2 Pb1 I1 88.84(3) 2_557 3_577 ? I2 Pb1 I1 90.36(3) . 3_577 ? I2 Pb1 I1 89.64(3) 3_577 3_577 ? I1 Pb1 I1 180 . 3_577 ? 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 177.4(15) . . . . ? C1 C2 C3 C4 -81(2) . . . . ? C2 C3 C4 C5 179.5(16) . . . . ? C3 C4 C5 C6 -177.2(18) . . . . ? C4 C5 C6 C6 179(2) . . . 3_675 ? Pb1 I2 Pb1 I2 -4.65(9) 2_547 . . 4_575 ? Pb1 I2 Pb1 I2 175.35(9) 2_547 . . 2_557 ? Pb1 I2 Pb1 I1 -93.47(7) 2_547 . . . ? Pb1 I2 Pb1 I1 86.53(7) 2_547 . . 3_577 ? 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 I2 0.91 2.88 3.657(16) 144 1_554 N1 H1A I1 0.91 2.75 3.637(16) 165 . N1 H1C I1 0.91 2.73 3.588(17) 157 4_575 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-11-03 at 11:44:34 # 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 : 4ad37l_a smart data_7 _database_code_depnum_ccdc_archive 'CCDC 853212' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-11-03T11:44:34-00:00 _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(1,5-diammoniumnaphthalene)tetraiodoplumbate(II) ; _chemical_formula_sum 'C10 H12 I4 N2 Pb' _chemical_formula_moiety 'C10 H12 N2, I4 Pb' _chemical_formula_weight 875.01 #----------------------------------------------------------------------------# # 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 11.163(3) _cell_length_b 8.960(2) _cell_length_c 8.737(2) _cell_angle_alpha 90 _cell_angle_beta 90.314(4) _cell_angle_gamma 90 _cell_volume 873.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 949 _cell_measurement_theta_min 5.826 _cell_measurement_theta_max 56.626 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description triangle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 3.326 _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 0.03 -1 0 0 0.03 2 3 -3 0.12 1 1 0 0.1 1 -3 -1 0.12 -1 -1 5 0.14 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.704 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0386 _exptl_absorpt_correction_T_max 0.3813 _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 0.066 _diffrn_reflns_av_unetI/netI 0.0406 _diffrn_reflns_number 8461 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _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 1.82 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 2089 _reflns_number_gt 2015 _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,2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0173P)^2^+9.4978P] 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 2089 _refine_ls_number_parameters 81 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.18 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.769 _refine_diff_density_min -1.481 _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' 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 0.6116(8) 0.3251(10) -0.1763(10) 0.0218(16) Uani 1 1 d U . . H1 H 0.6351 0.2524 -0.2494 0.026 Uiso 1 1 calc R . . C2 C 0.6985(9) 0.4060(10) -0.0984(10) 0.0244(16) Uani 1 1 d U . . H2 H 0.7809 0.3893 -0.1189 0.029 Uiso 1 1 calc R . . C3 C 0.6654(7) 0.5099(9) 0.0079(11) 0.0204(14) Uani 1 1 d U . . C4 C 0.5446(8) 0.5416(9) 0.0407(10) 0.0205(15) Uani 1 1 d U . . C5 C 0.5095(8) 0.6512(10) 0.1488(9) 0.0217(15) Uani 1 1 d U . . H5 H 0.5683 0.7079 0.202 0.026 Uiso 1 1 calc R . . N1 N 0.7593(7) 0.5945(9) 0.0895(9) 0.0237(14) Uani 1 1 d U . . H1A H 0.7535 0.6929 0.0648 0.036 Uiso 1 1 calc R . . H1B H 0.8326 0.5596 0.062 0.036 Uiso 1 1 calc R . . H1C H 0.7497 0.5832 0.1922 0.036 Uiso 1 1 calc R . . I1 I 0.71751(5) -0.03376(6) -0.01510(7) 0.02264(13) Uani 1 1 d . . . I2 I 0.99181(6) 0.31392(6) 0.18378(6) 0.02181(13) Uani 1 1 d . . . Pb1 Pb 1 0 0 0.01805(11) 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(4) 0.025(4) 0.021(4) 0.002(3) 0.003(3) 0.003(3) C2 0.026(4) 0.028(4) 0.019(4) 0.002(3) -0.002(3) 0.003(3) C3 0.017(3) 0.022(3) 0.022(3) 0.006(3) 0.001(3) 0.002(3) C4 0.019(3) 0.019(4) 0.023(4) 0.005(3) -0.001(3) 0.001(3) C5 0.018(4) 0.022(4) 0.024(4) 0.002(3) 0.002(3) -0.001(3) N1 0.018(3) 0.025(4) 0.027(4) 0.002(3) -0.002(3) 0.005(3) I1 0.0218(3) 0.0230(3) 0.0231(3) -0.0003(2) -0.0002(2) 0.00159(19) I2 0.0263(3) 0.0198(3) 0.0193(2) -0.00522(17) -0.0010(2) 0.0021(2) Pb1 0.0215(2) 0.01575(18) 0.01694(19) -0.00011(15) -0.00196(18) -0.00190(16) #----------------------------------------------------------------------------# # 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 1.387(13) . ? C1 C5 1.390(12) 3_665 ? C1 H1 0.95 . ? C2 C3 1.367(13) . ? C2 H2 0.95 . ? C3 C4 1.409(11) . ? C3 N1 1.474(11) . ? C4 C5 1.419(12) . ? C4 C4 1.430(17) 3_665 ? C5 C1 1.390(12) 3_665 ? C5 H5 0.95 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1699(10) . ? I2 Pb1 3.2277(8) 2_755 ? I2 Pb1 3.2403(8) . ? Pb1 I1 3.1699(10) 3_755 ? Pb1 I2 3.2277(8) 4_565 ? Pb1 I2 3.2277(8) 2_745 ? Pb1 I2 3.2403(8) 3_755 ? 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 C5 120.9(8) . 3_665 ? C2 C1 H1 119.6 . . ? C5 C1 H1 119.6 3_665 . ? C3 C2 C1 119.9(9) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 122.5(8) . . ? C2 C3 N1 119.0(7) . . ? C4 C3 N1 118.5(8) . . ? C3 C4 C5 122.9(8) . . ? C3 C4 C4 117.3(10) . 3_665 ? C5 C4 C4 119.8(10) . 3_665 ? C1 C5 C4 119.6(8) 3_665 . ? C1 C5 H5 120.2 3_665 . ? C4 C5 H5 120.2 . . ? C3 N1 H1A 109.5 . . ? C3 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C3 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 150.669(18) 2_755 . ? I1 Pb1 I1 180 . 3_755 ? I1 Pb1 I2 89.437(16) . 4_565 ? I1 Pb1 I2 90.563(16) 3_755 4_565 ? I1 Pb1 I2 90.563(16) . 2_745 ? I1 Pb1 I2 89.437(16) 3_755 2_745 ? I2 Pb1 I2 180.000(15) 4_565 2_745 ? I1 Pb1 I2 94.169(15) . . ? I1 Pb1 I2 85.831(15) 3_755 . ? I2 Pb1 I2 88.569(18) 4_565 . ? I2 Pb1 I2 91.431(18) 2_745 . ? I1 Pb1 I2 85.831(15) . 3_755 ? I1 Pb1 I2 94.169(15) 3_755 3_755 ? I2 Pb1 I2 91.431(18) 4_565 3_755 ? I2 Pb1 I2 88.569(18) 2_745 3_755 ? I2 Pb1 I2 180.00(3) . 3_755 ? 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 C5 C1 C2 C3 0.5(13) 3_665 . . . ? C1 C2 C3 C4 -1.3(14) . . . . ? C1 C2 C3 N1 179.9(8) . . . . ? C2 C3 C4 C5 -178.8(8) . . . . ? N1 C3 C4 C5 0.0(13) . . . . ? C2 C3 C4 C4 0.8(15) . . . 3_665 ? N1 C3 C4 C4 179.7(9) . . . 3_665 ? C3 C4 C5 C1 -179.3(8) . . . 3_665 ? C4 C4 C5 C1 1.1(14) 3_665 . . 3_665 ? Pb1 I2 Pb1 I1 95.29(4) 2_755 . . . ? Pb1 I2 Pb1 I1 -84.71(4) 2_755 . . 3_755 ? Pb1 I2 Pb1 I2 -175.38(3) 2_755 . . 4_565 ? Pb1 I2 Pb1 I2 4.62(3) 2_755 . . 2_745 ? 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 I2 0.91 3.02 3.703(7) 133 . N1 H1C I1 0.91 2.62 3.530(8) 176 4_566 N1 H1A I1 0.91 2.58 3.485(8) 175 1_565 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-05-04 at 11:13:03 # 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 : 5ad67l_a smart data_8 _database_code_depnum_ccdc_archive 'CCDC 853213' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-05-04T11:13:03-00:00 _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 ; tetrakis(1,2-diammoniumethane)nonabromodiplumbate(II) tribromide ; _chemical_formula_sum 'C8 H40 Br12 N8 Pb2' _chemical_formula_moiety 'Br9 Pb2, 4(C2 H10 N2), 3(Br)' _chemical_formula_weight 1621.78 #----------------------------------------------------------------------------# # 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 8.9023(8) _cell_length_b 27.727(2) _cell_length_c 14.7100(12) _cell_angle_alpha 90 _cell_angle_beta 102.226(6) _cell_angle_gamma 90 _cell_volume 3548.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 940 _cell_measurement_theta_min 2.9275 _cell_measurement_theta_max 28.2635 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 3.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 2 1 0.12 0 -2 -1 0.12 0 -2 1 0.07 0 2 -1 0.07 3 1 -2 0.24 -2 1 2 0.23 -2 -2 -1 0.24 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 23.004 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0103 _exptl_absorpt_correction_T_max 0.0917 _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 0.1072 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_number 21917 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 8504 _reflns_number_gt 6389 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0394P)^2^+199.5020P] 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 0.00110(6) _refine_ls_number_reflns 8504 _refine_ls_number_parameters 275 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.061 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1529 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.729 _refine_diff_density_min -6.086 _refine_diff_density_rms 0.408 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5124(18) 0.0916(7) 0.4424(12) 0.028(3) Uani 1 1 d U . . H1D H 0.4446 0.0684 0.402 0.033 Uiso 1 1 calc R . . H1E H 0.6119 0.0923 0.4225 0.033 Uiso 1 1 calc R . . C2 C 0.439(2) 0.1423(7) 0.4289(14) 0.034(3) Uani 1 1 d U . . H2D H 0.4982 0.1645 0.4757 0.041 Uiso 1 1 calc R . . H2E H 0.4449 0.1546 0.3665 0.041 Uiso 1 1 calc R . . C3 C 0.8253(18) 0.1198(6) 0.9394(12) 0.026(3) Uani 1 1 d U . . H3D H 0.8823 0.1126 1.0033 0.031 Uiso 1 1 calc R . . H3E H 0.8366 0.0917 0.8999 0.031 Uiso 1 1 calc R . . C4 C 0.6557(18) 0.1261(6) 0.9406(11) 0.024(3) Uani 1 1 d U . . H4D H 0.6239 0.1001 0.9785 0.028 Uiso 1 1 calc R . . H4E H 0.6417 0.1572 0.9708 0.028 Uiso 1 1 calc R . . C5 C 0.4451(18) 0.2348(6) 0.0499(12) 0.024(3) Uani 1 1 d U . . H5D H 0.4962 0.2058 0.0811 0.029 Uiso 1 1 calc R . . H5E H 0.4456 0.2324 -0.0171 0.029 Uiso 1 1 calc R . . C6 C 0.2779(18) 0.2362(6) 0.0622(11) 0.024(3) Uani 1 1 d U . . H6D H 0.2357 0.2689 0.0471 0.028 Uiso 1 1 calc R . . H6E H 0.2158 0.2134 0.0178 0.028 Uiso 1 1 calc R . . C7 C 0.680(2) 0.4925(8) 0.2625(15) 0.043(4) Uani 1 1 d U . . H7D H 0.6998 0.5048 0.3271 0.051 Uiso 1 1 calc R . . H7E H 0.7669 0.4712 0.2569 0.051 Uiso 1 1 calc R . . C8 C 0.534(2) 0.4635(7) 0.2443(13) 0.035(3) Uani 1 1 d U . . H8D H 0.5395 0.4397 0.2949 0.042 Uiso 1 1 calc R . . H8E H 0.447 0.4854 0.2461 0.042 Uiso 1 1 calc R . . N1 N 0.5387(15) 0.0746(5) 0.5395(9) 0.025(3) Uani 1 1 d U . . H1A H 0.5822 0.0447 0.5437 0.037 Uiso 1 1 calc R . . H1B H 0.4473 0.0731 0.5579 0.037 Uiso 1 1 calc R . . H1C H 0.6026 0.0954 0.5769 0.037 Uiso 1 1 calc R . . N2 N 0.2758(16) 0.1428(6) 0.4375(9) 0.029(3) Uani 1 1 d U . . H2A H 0.2382 0.1733 0.4289 0.043 Uiso 1 1 calc R . . H2B H 0.2693 0.1323 0.4951 0.043 Uiso 1 1 calc R . . H2C H 0.2198 0.1229 0.3937 0.043 Uiso 1 1 calc R . . N3 N 0.8961(14) 0.1626(5) 0.9042(9) 0.022(3) Uani 1 1 d U . . H3A H 0.9968 0.1565 0.9051 0.033 Uiso 1 1 calc R . . H3B H 0.8889 0.1885 0.9411 0.033 Uiso 1 1 calc R . . H3C H 0.8459 0.1691 0.8449 0.033 Uiso 1 1 calc R . . N4 N 0.5550(15) 0.1253(5) 0.8468(10) 0.026(3) Uani 1 1 d U . . H4A H 0.4557 0.1296 0.8516 0.039 Uiso 1 1 calc R . . H4B H 0.5645 0.0963 0.8194 0.039 Uiso 1 1 calc R . . H4C H 0.5829 0.1494 0.8117 0.039 Uiso 1 1 calc R . . N5 N 0.5344(15) 0.2787(5) 0.0894(10) 0.023(3) Uani 1 1 d U . . H5A H 0.6327 0.2762 0.0814 0.035 Uiso 1 1 calc R . . H5B H 0.5348 0.281 0.1512 0.035 Uiso 1 1 calc R . . H5C H 0.4897 0.3055 0.0596 0.035 Uiso 1 1 calc R . . N6 N 0.2641(18) 0.2234(5) 0.1582(10) 0.031(3) Uani 1 1 d U . . H6A H 0.1637 0.2249 0.1624 0.046 Uiso 1 1 calc R . . H6B H 0.3202 0.2445 0.1993 0.046 Uiso 1 1 calc R . . H6C H 0.3 0.1929 0.1717 0.046 Uiso 1 1 calc R . . N7 N 0.676(2) 0.5328(6) 0.1995(12) 0.044(4) Uani 1 1 d U . . H7A H 0.7669 0.549 0.2134 0.065 Uiso 1 1 calc R . . H7B H 0.5982 0.5531 0.2054 0.065 Uiso 1 1 calc R . . H7C H 0.6598 0.5218 0.14 0.065 Uiso 1 1 calc R . . N8 N 0.5028(16) 0.4377(5) 0.1538(11) 0.030(3) Uani 1 1 d U . . H8A H 0.413 0.421 0.1473 0.045 Uiso 1 1 calc R . . H8B H 0.5809 0.4167 0.1521 0.045 Uiso 1 1 calc R . . H8C H 0.4954 0.4594 0.1066 0.045 Uiso 1 1 calc R . . Br1 Br 0 0.5 0.5 0.0393(6) Uani 1 2 d S . . Br2 Br -0.25352(18) 0.37883(6) 0.44028(12) 0.0272(4) Uani 1 1 d . . . Br3 Br -0.1109(2) 0.51790(6) 0.75370(12) 0.0312(4) Uani 1 1 d . . . Br4 Br 0.0592(2) 0.38448(6) 0.69067(12) 0.0301(4) Uani 1 1 d . . . Br5 Br -0.4089(2) 0.38971(7) 0.71246(13) 0.0334(4) Uani 1 1 d . . . Br6 Br -0.5 0.5 0.5 0.0312(5) Uani 1 2 d S . . Br7 Br 0.40079(18) 0.36767(6) 0.93837(11) 0.0258(3) Uani 1 1 d . . . Br8 Br 0.10975(18) 0.25235(6) 0.81430(11) 0.0261(3) Uani 1 1 d . . . Br9 Br 0.60629(17) 0.25434(5) 0.84317(11) 0.0226(3) Uani 1 1 d . . . Br10 Br 0.38058(18) 0.26512(6) 0.58069(11) 0.0252(3) Uani 1 1 d . . . Br11 Br 0.78540(18) -0.01261(6) 0.50604(12) 0.0262(3) Uani 1 1 d . . . Br12 Br 0.76866(18) 0.15294(5) 0.68065(11) 0.0229(3) Uani 1 1 d . . . Br13 Br 0.79352(18) 0.36748(6) 0.15841(11) 0.0274(3) Uani 1 1 d . . . Pb1 Pb -0.20942(6) 0.44870(2) 0.59941(4) 0.01855(15) Uani 1 1 d . . . Pb2 Pb 0.34395(6) 0.31478(2) 0.76198(4) 0.01869(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(6) 0.038(7) 0.026(6) -0.011(6) 0.006(6) -0.005(5) C2 0.031(7) 0.033(7) 0.041(9) 0.010(6) 0.011(7) -0.009(6) C3 0.023(5) 0.023(7) 0.031(8) 0.000(6) 0.001(5) 0.004(5) C4 0.023(6) 0.024(7) 0.024(6) 0.000(6) 0.006(5) -0.006(5) C5 0.025(6) 0.023(6) 0.028(7) 0.000(6) 0.010(5) 0.004(5) C6 0.022(5) 0.029(7) 0.020(6) -0.005(6) 0.006(5) -0.003(5) C7 0.047(9) 0.039(9) 0.042(9) -0.003(6) 0.011(8) -0.017(7) C8 0.028(7) 0.040(8) 0.040(8) 0.000(7) 0.015(7) -0.004(6) N1 0.021(6) 0.022(6) 0.028(6) -0.007(5) -0.001(5) -0.003(5) N2 0.030(6) 0.036(8) 0.018(6) 0.002(6) 0.001(5) 0.005(5) N3 0.012(5) 0.028(6) 0.026(7) -0.005(5) 0.006(5) 0.003(5) N4 0.023(6) 0.026(7) 0.028(6) -0.005(6) 0.003(5) -0.004(5) N5 0.021(6) 0.019(6) 0.030(7) 0.013(5) 0.007(5) 0.001(4) N6 0.039(8) 0.029(7) 0.028(7) -0.005(6) 0.016(6) -0.011(6) N7 0.060(11) 0.038(8) 0.035(8) -0.007(7) 0.016(8) -0.016(7) N8 0.026(7) 0.020(7) 0.044(8) 0.002(6) 0.006(6) 0.000(5) Br1 0.0417(14) 0.0294(12) 0.0546(17) 0.0063(12) 0.0278(13) -0.0086(11) Br2 0.0211(7) 0.0272(8) 0.0350(9) -0.0104(7) 0.0100(6) -0.0051(6) Br3 0.0406(9) 0.0260(8) 0.0276(8) -0.0047(7) 0.0081(7) -0.0055(7) Br4 0.0324(8) 0.0240(8) 0.0307(9) -0.0004(7) -0.0007(7) 0.0080(6) Br5 0.0365(9) 0.0315(9) 0.0329(9) 0.0065(7) 0.0089(7) -0.0095(7) Br6 0.0276(11) 0.0222(11) 0.0396(14) -0.0038(10) -0.0023(10) 0.0052(9) Br7 0.0266(8) 0.0256(8) 0.0254(8) 0.0001(6) 0.0059(6) 0.0048(6) Br8 0.0280(8) 0.0242(8) 0.0262(8) 0.0034(6) 0.0058(6) -0.0050(6) Br9 0.0235(7) 0.0220(7) 0.0228(7) 0.0024(6) 0.0058(6) 0.0051(6) Br10 0.0228(7) 0.0293(8) 0.0236(8) 0.0016(7) 0.0051(6) -0.0031(6) Br11 0.0244(7) 0.0212(7) 0.0351(9) -0.0062(7) 0.0110(6) -0.0033(6) Br12 0.0267(7) 0.0195(7) 0.0239(7) -0.0015(6) 0.0085(6) -0.0020(6) Br13 0.0256(8) 0.0308(8) 0.0253(8) 0.0008(7) 0.0047(6) -0.0007(6) Pb1 0.0194(3) 0.0156(3) 0.0213(3) 0.0015(2) 0.0060(2) 0.0002(2) Pb2 0.0175(3) 0.0184(3) 0.0201(3) 0.0009(2) 0.0041(2) 0.0015(2) #----------------------------------------------------------------------------# # 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 1.48(2) . ? C1 C2 1.55(3) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 N2 1.48(2) . ? C2 H2D 0.99 . ? C2 H2E 0.99 . ? C3 N3 1.49(2) . ? C3 C4 1.52(2) . ? C3 H3D 0.99 . ? C3 H3E 0.99 . ? C4 N4 1.48(2) . ? C4 H4D 0.99 . ? C4 H4E 0.99 . ? C5 N5 1.50(2) . ? C5 C6 1.54(2) . ? C5 H5D 0.99 . ? C5 H5E 0.99 . ? C6 N6 1.49(2) . ? C6 H6D 0.99 . ? C6 H6E 0.99 . ? C7 N7 1.45(3) . ? C7 C8 1.50(3) . ? C7 H7D 0.99 . ? C7 H7E 0.99 . ? C8 N8 1.49(2) . ? C8 H8D 0.99 . ? C8 H8E 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 . ? N5 H5A 0.91 . ? N5 H5B 0.91 . ? N5 H5C 0.91 . ? N6 H6A 0.91 . ? N6 H6B 0.91 . ? N6 H6C 0.91 . ? N7 H7A 0.91 . ? N7 H7B 0.91 . ? N7 H7C 0.91 . ? N8 H8A 0.91 . ? N8 H8B 0.91 . ? N8 H8C 0.91 . ? Br1 Pb1 2.9651(6) 3_566 ? Br1 Pb1 2.9651(6) . ? Br2 Pb1 2.9996(17) . ? Br3 Pb1 2.9595(18) . ? Br4 Pb1 3.0546(17) . ? Br4 Pb2 3.1836(17) . ? Br5 Pb1 3.1373(18) . ? Br5 Pb2 3.2200(17) 1_455 ? Br6 Pb1 3.0416(6) . ? Br6 Pb1 3.0416(6) 3_466 ? Br7 Pb2 2.9296(17) . ? Br8 Pb2 2.9352(16) . ? Br9 Pb2 2.9168(16) . ? Br10 Pb2 3.0793(17) . ? Pb2 Br5 3.2200(18) 1_655 ? 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 113.0(14) . . ? N1 C1 H1D 109 . . ? C2 C1 H1D 109 . . ? N1 C1 H1E 109 . . ? C2 C1 H1E 109 . . ? H1D C1 H1E 107.8 . . ? N2 C2 C1 113.1(14) . . ? N2 C2 H2D 109 . . ? C1 C2 H2D 109 . . ? N2 C2 H2E 109 . . ? C1 C2 H2E 109 . . ? H2D C2 H2E 107.8 . . ? N3 C3 C4 113.9(13) . . ? N3 C3 H3D 108.8 . . ? C4 C3 H3D 108.8 . . ? N3 C3 H3E 108.8 . . ? C4 C3 H3E 108.8 . . ? H3D C3 H3E 107.7 . . ? N4 C4 C3 113.2(13) . . ? N4 C4 H4D 108.9 . . ? C3 C4 H4D 108.9 . . ? N4 C4 H4E 108.9 . . ? C3 C4 H4E 108.9 . . ? H4D C4 H4E 107.7 . . ? N5 C5 C6 112.4(13) . . ? N5 C5 H5D 109.1 . . ? C6 C5 H5D 109.1 . . ? N5 C5 H5E 109.1 . . ? C6 C5 H5E 109.1 . . ? H5D C5 H5E 107.8 . . ? N6 C6 C5 112.5(14) . . ? N6 C6 H6D 109.1 . . ? C5 C6 H6D 109.1 . . ? N6 C6 H6E 109.1 . . ? C5 C6 H6E 109.1 . . ? H6D C6 H6E 107.8 . . ? N7 C7 C8 113.2(18) . . ? N7 C7 H7D 108.9 . . ? C8 C7 H7D 108.9 . . ? N7 C7 H7E 108.9 . . ? C8 C7 H7E 108.9 . . ? H7D C7 H7E 107.8 . . ? N8 C8 C7 114.1(15) . . ? N8 C8 H8D 108.7 . . ? C7 C8 H8D 108.7 . . ? N8 C8 H8E 108.7 . . ? C7 C8 H8E 108.7 . . ? H8D C8 H8E 107.6 . . ? 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 N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C2 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C3 N3 H3A 109.5 . . ? C3 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C3 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C4 N4 H4A 109.5 . . ? C4 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C4 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C5 N5 H5A 109.5 . . ? C5 N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? C5 N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? C6 N6 H6A 109.5 . . ? C6 N6 H6B 109.5 . . ? H6A N6 H6B 109.5 . . ? C6 N6 H6C 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? C7 N7 H7A 109.5 . . ? C7 N7 H7B 109.5 . . ? H7A N7 H7B 109.5 . . ? C7 N7 H7C 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? C8 N8 H8A 109.5 . . ? C8 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? C8 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? Pb1 Br1 Pb1 180.000(18) 3_566 . ? Pb1 Br4 Pb2 173.34(7) . . ? Pb1 Br5 Pb2 161.23(7) . 1_455 ? Pb1 Br6 Pb1 180 . 3_466 ? Br3 Pb1 Br1 87.25(4) . . ? Br3 Pb1 Br2 170.31(5) . . ? Br1 Pb1 Br2 85.24(3) . . ? Br3 Pb1 Br6 98.58(4) . . ? Br1 Pb1 Br6 95.630(17) . . ? Br2 Pb1 Br6 88.25(4) . . ? Br3 Pb1 Br4 87.92(5) . . ? Br1 Pb1 Br4 88.91(4) . . ? Br2 Pb1 Br4 85.83(5) . . ? Br6 Pb1 Br4 172.22(4) . . ? Br3 Pb1 Br5 92.32(5) . . ? Br1 Pb1 Br5 175.54(4) . . ? Br2 Pb1 Br5 94.69(5) . . ? Br6 Pb1 Br5 88.82(4) . . ? Br4 Pb1 Br5 86.64(5) . . ? Br9 Pb2 Br7 87.23(5) . . ? Br9 Pb2 Br8 96.05(5) . . ? Br7 Pb2 Br8 93.55(5) . . ? Br9 Pb2 Br10 82.83(5) . . ? Br7 Pb2 Br10 163.89(5) . . ? Br8 Pb2 Br10 100.06(5) . . ? Br9 Pb2 Br4 175.09(5) . . ? Br7 Pb2 Br4 87.95(5) . . ? Br8 Pb2 Br4 83.34(5) . . ? Br10 Pb2 Br4 102.07(5) . . ? Br9 Pb2 Br5 86.39(5) . 1_655 ? Br7 Pb2 Br5 83.07(5) . 1_655 ? Br8 Pb2 Br5 175.75(5) . 1_655 ? Br10 Pb2 Br5 83.67(5) . 1_655 ? Br4 Pb2 Br5 93.93(5) . 1_655 ? 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 N2 -70.9(19) . . . . ? N3 C3 C4 N4 72.4(18) . . . . ? N5 C5 C6 N6 -78.1(17) . . . . ? N7 C7 C8 N8 66(2) . . . . ? Pb2 Br5 Pb1 Br3 166.2(2) 1_455 . . . ? Pb2 Br5 Pb1 Br2 -20.5(2) 1_455 . . . ? Pb2 Br5 Pb1 Br6 67.6(2) 1_455 . . . ? Pb2 Br5 Pb1 Br4 -106.1(2) 1_455 . . . ? 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 Br11 0.91 2.56 3.371(14) 150 . N1 H1B Br11 0.91 2.68 3.302(13) 127 3_656 N1 H1B Br13 0.91 2.76 3.467(14) 135 4_566 N1 H1C Br12 0.91 2.47 3.380(13) 178 . N2 H2A Br9 0.91 2.52 3.385(15) 158 4_565 N2 H2B Br13 0.91 2.37 3.233(14) 159 4_566 N2 H2C Br5 0.91 2.69 3.488(14) 147 4_665 N3 H3A Br2 0.91 2.38 3.261(12) 162 4_766 N3 H3B Br10 0.91 2.44 3.305(13) 160 4_666 N3 H3C Br12 0.91 2.41 3.255(14) 154 . N4 H4A Br2 0.91 2.5 3.324(14) 151 4_666 N4 H4B Br3 0.91 2.5 3.407(14) 176 2_546 N4 H4C Br12 0.91 2.79 3.485(14) 134 . N4 H4C Br9 0.91 2.95 3.609(14) 131 . N5 H5A Br10 0.91 2.49 3.341(13) 156 4_665 N5 H5B Br8 0.91 2.53 3.346(14) 150 4_665 N5 H5C Br7 0.91 2.49 3.363(13) 162 1_554 N6 H6A Br9 0.91 2.87 3.373(14) 116 4_565 N6 H6B Br8 0.91 2.77 3.493(16) 137 4_665 N6 H6B Br12 0.91 2.88 3.444(15) 121 4_565 N6 H6C Br5 0.91 3.09 3.656(14) 122 4_665 N7 H7A Br4 0.91 2.62 3.437(17) 150 3_666 N7 H7B Br5 0.91 2.77 3.639(19) 160 3_566 N7 H7C Br11 0.91 2.49 3.360(17) 160 2_655 N8 H8A Br12 0.91 2.52 3.341(14) 150 4_565 N8 H8B Br13 0.91 2.32 3.227(14) 175 . N8 H8C Br11 0.91 2.59 3.318(15) 138 4_565 N8 H8C Br11 0.91 2.92 3.586(15) 131 2_655 ### END #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2005-04-14 at 11:26:11 # 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 : 4ad55l_a smart data_9 _database_code_depnum_ccdc_archive 'CCDC 853214' #TrackingRef '- Diamines.cif' _audit_creation_date 2005-04-14T11:26:11-00:00 _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 ; (4,4-methylenedianilinium)hexaiododiplumbate(II) ; _chemical_formula_sum 'C13 H16 I6 N2 Pb2' _chemical_formula_moiety 'C13 H16 N2, 2(I3 Pb)' _chemical_formula_weight 1376.06 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 25.333(8) _cell_length_b 42.923(14) _cell_length_c 4.5149(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4909(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1017 _cell_measurement_theta_min 2.4875 _cell_measurement_theta_max 28.202 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.025 _exptl_crystal_density_diffrn 3.724 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4720 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 -1 0 0 0.065 1 0 0 0.065 2 1 2 0.19 2 -4 -3 0.19 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 21.246 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0444 _exptl_absorpt_correction_T_max 0.6543 _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 0.0492 _diffrn_reflns_av_unetI/netI 0.0351 _diffrn_reflns_number 11693 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 56 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.87 _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 2938 _reflns_number_gt 2706 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0369P)^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 2938 _refine_ls_number_parameters 93 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0633 _refine_ls_wR_factor_gt 0.0625 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 1283 Friedel pairs' _refine_ls_abs_structure_Flack 0.008(5) _refine_diff_density_max 1.261 _refine_diff_density_min -1.674 _refine_diff_density_rms 0.262 #----------------------------------------------------------------------------# # 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 0.77120(19) 0.17342(10) 0.9399(10) 0.0207(15) Uani 1 1 d G . . C2 C 0.72080(16) 0.18129(11) 0.8439(10) 0.0227(18) Uani 1 1 d G . . H2 H 0.691 0.1703 0.9175 0.027 Uiso 1 1 calc R . . C3 C 0.71397(14) 0.20524(12) 0.6404(10) 0.0221(17) Uani 1 1 d G . . H3 H 0.6795 0.2106 0.5748 0.027 Uiso 1 1 calc R . . C4 C 0.75756(18) 0.22134(10) 0.5328(9) 0.0165(15) Uani 1 1 d G . . C5 C 0.80796(15) 0.21347(10) 0.6288(10) 0.0178(16) Uani 1 1 d G . . H5 H 0.8377 0.2245 0.5552 0.021 Uiso 1 1 calc R . . C6 C 0.81478(14) 0.18952(11) 0.8323(11) 0.0197(17) Uani 1 1 d G . . H6 H 0.8492 0.1841 0.8979 0.024 Uiso 1 1 calc R . . C7 C 0.75 0.25 0.344(2) 0.023(3) Uani 1 2 d S . . H7A H 0.7812 0.2529 0.2152 0.027 Uiso 0.5 1 calc PR . . H7B H 0.7188 0.2471 0.2152 0.027 Uiso 0.5 1 calc PR . . N1 N 0.7793(3) 0.14950(16) 1.1635(19) 0.0326(17) Uani 1 1 d . . . H1A H 0.8144 0.1476 1.2025 0.049 Uiso 1 1 calc R . . H1B H 0.7666 0.131 1.0957 0.049 Uiso 1 1 calc R . . H1C H 0.7619 0.1549 1.3323 0.049 Uiso 1 1 calc R . . I1 I 0.671777(18) -0.010215(11) 0.69560(12) 0.02145(11) Uani 1 1 d . . . I2 I 0.845551(19) 0.099621(11) 0.67675(13) 0.02212(11) Uani 1 1 d . . . I3 I 0.693605(19) 0.082704(12) 0.17638(13) 0.02399(12) Uani 1 1 d . . . Pb1 Pb 0.762971(11) 0.048165(6) 0.69027(6) 0.01957(8) 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 0.033(4) 0.018(4) 0.011(3) -0.002(3) -0.002(4) -0.001(3) C2 0.032(5) 0.021(4) 0.015(4) -0.004(3) 0.008(3) -0.001(4) C3 0.024(4) 0.027(4) 0.016(4) -0.005(3) 0.000(3) 0.000(3) C4 0.025(4) 0.015(4) 0.009(3) -0.004(3) 0.001(3) 0.001(3) C5 0.024(4) 0.016(4) 0.013(4) -0.004(3) 0.001(3) -0.003(3) C6 0.022(4) 0.021(4) 0.016(3) -0.005(3) -0.004(3) 0.009(3) C7 0.019(6) 0.027(6) 0.023(6) 0 0 0.009(5) N1 0.059(5) 0.016(3) 0.023(4) 0.004(4) -0.002(4) 0.006(3) I1 0.0193(2) 0.0226(2) 0.0224(2) 0.0015(3) -0.0042(2) 0.00126(18) I2 0.0213(2) 0.0201(2) 0.0249(2) 0.0017(3) 0.0005(2) -0.00180(18) I3 0.0202(2) 0.0281(3) 0.0237(2) -0.0009(3) 0.0042(2) 0.00421(19) Pb1 0.02062(14) 0.01918(13) 0.01892(13) -0.00077(14) 0.00232(13) -0.00077(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 1.39 . ? C1 C6 1.39 . ? C1 N1 1.455(8) . ? C2 C3 1.39 . ? C2 H2 0.95 . ? C3 C4 1.39 . ? C3 H3 0.95 . ? C4 C5 1.39 . ? C4 C7 1.509(7) . ? C5 C6 1.39 . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C4 1.509(8) 14_655 ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.2208(9) 10_655 ? I1 Pb1 3.2544(9) 10_654 ? I1 Pb1 3.4083(10) . ? I2 Pb1 3.0427(9) . ? I3 Pb1 3.1784(9) 1_554 ? I3 Pb1 3.2663(9) . ? Pb1 I3 3.1784(9) 1_556 ? Pb1 I1 3.2208(9) 10_654 ? Pb1 I1 3.2544(9) 10_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 120 . . ? C2 C1 N1 121.1(5) . . ? C6 C1 N1 118.8(5) . . ? C3 C2 C1 120 . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C2 C3 C4 120 . . ? C2 C3 H3 120 . . ? C4 C3 H3 120 . . ? C5 C4 C3 120 . . ? C5 C4 C7 119.4(3) . . ? C3 C4 C7 120.1(3) . . ? C4 C5 C6 120 . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 120 . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C4 C7 C4 111.3(9) 14_655 . ? C4 C7 H7A 109.4 14_655 . ? C4 C7 H7A 109.4 . . ? C4 C7 H7B 109.4 14_655 . ? C4 C7 H7B 109.4 . . ? H7A C7 H7B 108 . . ? 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 I1 Pb1 88.41(3) 10_655 10_654 ? Pb1 I1 Pb1 91.65(2) 10_655 . ? Pb1 I1 Pb1 91.08(2) 10_654 . ? Pb1 I3 Pb1 88.93(3) 1_554 . ? I2 Pb1 I3 93.17(3) . 1_556 ? I2 Pb1 I1 90.02(3) . 10_654 ? I3 Pb1 I1 176.797(16) 1_556 10_654 ? I2 Pb1 I1 91.61(2) . 10_655 ? I3 Pb1 I1 91.73(3) 1_556 10_655 ? I1 Pb1 I1 88.41(3) 10_654 10_655 ? I2 Pb1 I3 91.50(2) . . ? I3 Pb1 I3 88.93(3) 1_556 . ? I1 Pb1 I3 90.75(3) 10_654 . ? I1 Pb1 I3 176.776(16) 10_655 . ? I2 Pb1 I1 178.927(17) . . ? I3 Pb1 I1 87.90(2) 1_556 . ? I1 Pb1 I1 88.91(2) 10_654 . ? I1 Pb1 I1 88.36(2) 10_655 . ? I3 Pb1 I1 88.51(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0 . . . . ? N1 C1 C2 C3 177.0(6) . . . . ? C1 C2 C3 C4 0 . . . . ? C2 C3 C4 C5 0 . . . . ? C2 C3 C4 C7 -171.9(6) . . . . ? C3 C4 C5 C6 0 . . . . ? C7 C4 C5 C6 171.9(6) . . . . ? C4 C5 C6 C1 0 . . . . ? C2 C1 C6 C5 0 . . . . ? N1 C1 C6 C5 -177.0(6) . . . . ? C5 C4 C7 C4 -87.2(5) . . . 14_655 ? C3 C4 C7 C4 84.7(5) . . . 14_655 ? Pb1 I3 Pb1 I2 86.85(2) 1_554 . . . ? Pb1 I3 Pb1 I3 180 1_554 . . 1_556 ? Pb1 I3 Pb1 I1 -3.188(16) 1_554 . . 10_654 ? Pb1 I3 Pb1 I1 -92.08(2) 1_554 . . . ? Pb1 I1 Pb1 I3 -92.40(3) 10_655 . . 1_556 ? Pb1 I1 Pb1 I3 179.154(15) 10_654 . . 1_556 ? Pb1 I1 Pb1 I1 87.83(3) 10_655 . . 10_654 ? Pb1 I1 Pb1 I1 -0.611(16) 10_654 . . 10_654 ? Pb1 I1 Pb1 I1 -0.611(16) 10_655 . . 10_655 ? Pb1 I1 Pb1 I1 -89.05(3) 10_654 . . 10_655 ? Pb1 I1 Pb1 I3 178.611(16) 10_655 . . . ? Pb1 I1 Pb1 I3 90.17(3) 10_654 . . . ? 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 3.08 3.574(7) 116 1_556 N1 H1B I3 0.91 2.8 3.596(8) 147 1_556 N1 H1B I2 0.91 3.06 3.498(8) 111 . ###END