# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM loop_ _publ_author_name A.Lemmerer D.G.Billing _publ_contact_author_name 'Andreas Lemmerer' _publ_contact_author_email andreas.lemmerer@wits.ac.za data_1a_805427 _database_code_depnum_ccdc_archive 'CCDC 805427' #TrackingRef '- Dalton Cif C7-C10.cif' _iucr_refine_instructions_details ; TITL 5aS23a_a in P2(1)/c CELL 0.71073 8.5886 8.9418 17.2431 90.000 96.902 90.000 ZERR 2.00 0.0043 0.0044 0.0088 0.000 0.011 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 28 72 4 8 2 MERG 2 OMIT -2.00 51.00 TWIN -1.00 0.00 0.00 0.00 -1.00 0.00 0.48 0.00 1.00 2 SIMU 0.01 0.02 C1 > N1 DELU 0.003 0.005 C1 > N1 DFIX 1.50 0.001 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 DANG 2.54 0.002 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 DFIX 1.45 0.001 C1 N1 DANG 2.45 0.002 N1 C2 EQIV $2 x+1/2, -y+3/2, z EQIV $3 x-1/2, -y+3/2, z HTAB N1 I1 HTAB N1 I2_$2 HTAB N1 I1_$3 FMAP 2 PLAN 1 ACTA BOND BOND $H CONF L.S. 4 TEMP -20.00 WGHT 0.200000 BASF 0.27202 FVAR 0.08343 C1 1 0.959538 0.492555 0.776102 11.00000 0.02407 0.04504 = 0.02615 0.01437 0.00806 0.00329 AFIX 23 H1D 2 1.071760 0.476074 0.786315 11.00000 -1.20000 H1E 2 0.941374 0.568161 0.735687 11.00000 -1.20000 AFIX 0 C2 1 0.881062 0.349807 0.747279 11.00000 0.03656 0.04922 = 0.03181 0.00838 -0.00456 0.00383 AFIX 23 H2A 2 0.768555 0.365896 0.740550 11.00000 -1.20000 H2B 2 0.903620 0.274066 0.787326 11.00000 -1.20000 AFIX 0 C3 1 0.927664 0.290005 0.672125 11.00000 0.04294 0.05586 = 0.02979 0.00733 -0.00854 0.00985 AFIX 23 H3A 2 1.039260 0.306434 0.671956 11.00000 -1.20000 H3B 2 0.910221 0.182809 0.670875 11.00000 -1.20000 AFIX 0 C4 1 0.843325 0.356434 0.598946 11.00000 0.04433 0.06002 = 0.03223 0.00737 -0.01393 0.00723 AFIX 23 H4A 2 0.731392 0.348015 0.601301 11.00000 -1.20000 H4B 2 0.868397 0.462137 0.597956 11.00000 -1.20000 AFIX 0 C5 1 0.879759 0.287599 0.523870 11.00000 0.04958 0.06371 = 0.03100 0.00474 -0.01807 0.00753 AFIX 23 H5A 2 0.840494 0.185786 0.521440 11.00000 -1.20000 H5B 2 0.992815 0.282599 0.524925 11.00000 -1.20000 AFIX 0 C6 1 0.813589 0.367289 0.450705 11.00000 0.05498 0.06825 = 0.03143 0.00533 -0.02193 0.00623 AFIX 23 H6A 2 0.703389 0.386918 0.453680 11.00000 -1.20000 H6B 2 0.865863 0.463194 0.449040 11.00000 -1.20000 AFIX 0 C7 1 0.827978 0.286299 0.375718 11.00000 0.05164 0.07754 = 0.03071 0.00565 -0.01228 -0.00064 AFIX 33 H7A 2 0.784595 0.346819 0.332446 11.00000 -1.50000 H7B 2 0.771956 0.193329 0.375177 11.00000 -1.50000 H7C 2 0.936593 0.266914 0.371539 11.00000 -1.50000 AFIX 0 N1 3 0.902347 0.546908 0.846688 11.00000 0.01772 0.02472 = 0.03276 0.02003 0.01416 0.00543 AFIX 33 H1A 2 0.943528 0.636456 0.858798 11.00000 -1.50000 H1B 2 0.930119 0.483469 0.885676 11.00000 -1.50000 H1C 2 0.798289 0.554161 0.838914 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 0.980003 0.918532 0.818243 11.00000 0.04754 0.02702 = 0.02221 -0.00305 -0.00233 -0.00750 I2 4 0.693671 1.205249 0.964173 11.00000 0.01572 0.01862 = 0.03399 0.00307 0.00396 0.00994 PB1 5 1.000000 1.000000 1.000000 10.50000 0.01257 0.00554 = 0.01849 -0.00061 0.00090 0.00049 HKLF 4 REM 5aS23a_a in P2(1)/c REM R1 = 0.1458 for 2197 Fo > 4sig(Fo) and 0.1584 for all 2412 data REM 98 parameters refined using 68 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 13.755, deepest hole -4.552, 1-sigma level 0.903 Q1 1 1.0000 0.5000 1.0000 10.50000 0.05 13.76 ; _audit_creation_date 2011-05-18T08:37:38-00:00 _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(heptylammonium)tetraiodoplumbate(II) PHASE IV ; _chemical_formula_moiety '2(C7 H18 N), I4 Pb' _chemical_formula_sum 'C14 H36 I4 N2 Pb' _chemical_formula_weight 947.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.589(4) _cell_length_b 8.942(4) _cell_length_c 17.243(9) _cell_angle_alpha 90 _cell_angle_beta 96.902(11) _cell_angle_gamma 90 _cell_volume 1314.6(11) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 917 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 28.128 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.01 -1 0 0 0.01 0 1 0 0.155 0 -1 0 0.155 -1 0 2 0.18 1 0 -2 0.18 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of the fracturing and twinning of the crystal caused by the phase transition. The space group was assigned from systematic absences using the program XPREP. Related compounds we have investigated have the same space group in their lowest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 11.112 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0859 _exptl_absorpt_correction_T_max 0.7995 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 253(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 0.1077 _diffrn_reflns_av_unetI/netI 0.0722 _diffrn_reflns_number 6268 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 2412 _reflns_number_gt 2197 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The crystal structure contains significant high residual electron density. The highest peak of 13.76 is located 2.708 A from N1 and 4.471 A from Pb1. It is in fact co-planar with the lead atoms and located in the middle of the voids formed by the corner- sharing octahedra. No atom position can be located there and hence this residual density is an artifact. The cause of the artifact and of the high R-factors, R(int) and GOF is that the two phase transitions going from phase II at room temp to phase IV has substantial movement of the inorganic layers and the organic chain, causing fracturing of the crystal, especially the transition from III to IV. This causes non-merohedral twinning and a twin law was applied that lowered the R-factor from 23 to 15%. Many crystals were attempted to go from phase II to IV and this gave the best data and we have the most confidence in this structural model. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.500 \%A and 112-116\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. The smaller ADP's compared to phase III are most likely due to the disorder-order phase transition from phase III. The data collection was definitely at 253 K. Included in this cif is the final res file, given above under _iucr_refine_instructions_details. ; _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^)+(0.2000P)^2^] 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 2412 _refine_ls_number_parameters 98 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1584 _refine_ls_R_factor_gt 0.1458 _refine_ls_wR_factor_ref 0.4512 _refine_ls_wR_factor_gt 0.4231 _refine_ls_goodness_of_fit_ref 2.127 _refine_ls_restrained_S_all 2.1 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 13.755 _refine_diff_density_min -4.552 _refine_diff_density_rms 0.903 #----------------------------------------------------------------------------# # 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 0.960(4) 0.493(3) 0.7761(19) 0.031(6) Uani 1 1 d DU . . H1D H 1.0718 0.4761 0.7863 0.038 Uiso 1 1 calc R . . H1E H 0.9414 0.5682 0.7357 0.038 Uiso 1 1 calc R . . C2 C 0.881(4) 0.350(3) 0.7473(12) 0.040(6) Uani 1 1 d DU . . H2A H 0.7686 0.3659 0.7405 0.048 Uiso 1 1 calc R . . H2B H 0.9036 0.2741 0.7873 0.048 Uiso 1 1 calc R . . C3 C 0.928(4) 0.290(4) 0.6721(11) 0.044(6) Uani 1 1 d DU . . H3A H 1.0393 0.3064 0.672 0.053 Uiso 1 1 calc R . . H3B H 0.9102 0.1828 0.6709 0.053 Uiso 1 1 calc R . . C4 C 0.843(5) 0.356(5) 0.5989(12) 0.047(6) Uani 1 1 d DU . . H4A H 0.7314 0.348 0.6013 0.056 Uiso 1 1 calc R . . H4B H 0.8684 0.4621 0.598 0.056 Uiso 1 1 calc R . . C5 C 0.880(7) 0.288(5) 0.5239(11) 0.050(7) Uani 1 1 d DU . . H5A H 0.8405 0.1858 0.5214 0.06 Uiso 1 1 calc R . . H5B H 0.9928 0.2826 0.5249 0.06 Uiso 1 1 calc R . . C6 C 0.814(7) 0.367(5) 0.4507(12) 0.054(7) Uani 1 1 d DU . . H6A H 0.7034 0.3869 0.4537 0.065 Uiso 1 1 calc R . . H6B H 0.8659 0.4632 0.449 0.065 Uiso 1 1 calc R . . C7 C 0.828(8) 0.286(6) 0.3757(11) 0.055(10) Uani 1 1 d DU . . H7A H 0.7846 0.3468 0.3324 0.082 Uiso 1 1 calc R . . H7B H 0.772 0.1933 0.3752 0.082 Uiso 1 1 calc R . . H7C H 0.9366 0.2669 0.3715 0.082 Uiso 1 1 calc R . . N1 N 0.902(4) 0.547(3) 0.8467(17) 0.024(6) Uani 1 1 d DU . . H1A H 0.9435 0.6365 0.8588 0.036 Uiso 1 1 calc R . . H1B H 0.9301 0.4835 0.8857 0.036 Uiso 1 1 calc R . . H1C H 0.7983 0.5542 0.8389 0.036 Uiso 1 1 calc R . . I1 I 0.9800(4) 0.9185(3) 0.81824(19) 0.0328(10) Uani 1 1 d . . . I2 I 0.6937(3) 1.2052(3) 0.96417(19) 0.0227(8) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0123(7) 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 0.024(13) 0.045(14) 0.026(12) 0.014(10) 0.008(11) 0.003(11) C2 0.037(13) 0.049(14) 0.032(11) 0.008(11) -0.005(10) 0.004(11) C3 0.043(13) 0.056(14) 0.030(11) 0.007(11) -0.009(10) 0.010(12) C4 0.044(13) 0.060(15) 0.032(11) 0.007(11) -0.014(11) 0.007(12) C5 0.050(14) 0.064(16) 0.031(11) 0.005(12) -0.018(12) 0.008(13) C6 0.055(16) 0.068(18) 0.031(12) 0.005(13) -0.022(13) 0.006(15) C7 0.05(2) 0.08(2) 0.031(12) 0.006(16) -0.012(17) 0.00(2) N1 0.018(14) 0.025(15) 0.033(15) 0.020(11) 0.014(12) 0.005(13) I1 0.048(2) 0.0270(17) 0.0222(17) -0.0031(12) -0.0023(14) -0.0075(13) I2 0.0157(12) 0.0186(15) 0.0340(17) 0.0031(11) 0.0040(12) 0.0099(9) Pb1 0.0126(11) 0.0055(10) 0.0185(12) -0.0006(6) 0.0009(12) 0.0005(6) #----------------------------------------------------------------------------# # 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 1.4500(12) . ? C1 C2 1.5000(12) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.5000(12) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.5000(11) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.5000(12) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.5000(11) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.5000(12) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.202(4) . ? I2 Pb1 3.206(3) . ? I2 Pb1 3.216(3) 2_657 ? Pb1 I1 3.202(4) 3_777 ? Pb1 I2 3.206(3) 3_777 ? Pb1 I2 3.216(3) 4_685 ? Pb1 I2 3.216(3) 2_647 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.29(17) . . ? N1 C1 H1D 109.1 . . ? C2 C1 H1D 109.1 . . ? N1 C1 H1E 109.1 . . ? C2 C1 H1E 109.1 . . ? H1D C1 H1E 107.9 . . ? C1 C2 C3 115.70(17) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C2 115.69(17) . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 115.71(17) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C4 C5 C6 115.70(17) . . ? C4 C5 H5A 108.4 . . ? C6 C5 H5A 108.4 . . ? C4 C5 H5B 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 115.69(17) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 149.71(11) . 2_657 ? I1 Pb1 I1 180.0000(10) . 3_777 ? I1 Pb1 I2 90.26(9) . 3_777 ? I1 Pb1 I2 89.74(9) 3_777 3_777 ? I1 Pb1 I2 89.74(9) . . ? I1 Pb1 I2 90.26(9) 3_777 . ? I2 Pb1 I2 180.0000(10) 3_777 . ? I1 Pb1 I2 88.08(8) . 4_685 ? I1 Pb1 I2 91.92(8) 3_777 4_685 ? I2 Pb1 I2 94.29(4) 3_777 4_685 ? I2 Pb1 I2 85.71(4) . 4_685 ? I1 Pb1 I2 91.92(8) . 2_647 ? I1 Pb1 I2 88.08(8) 3_777 2_647 ? I2 Pb1 I2 85.71(4) 3_777 2_647 ? I2 Pb1 I2 94.29(4) . 2_647 ? I2 Pb1 I2 180.0000(10) 4_685 2_647 ? 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(2) . . . . ? C1 C2 C3 C4 -83(4) . . . . ? C2 C3 C4 C5 -175(4) . . . . ? C3 C4 C5 C6 -172(5) . . . . ? C4 C5 C6 C7 -171(6) . . . . ? Pb1 I2 Pb1 I1 -144.4(2) 2_657 . . . ? Pb1 I2 Pb1 I1 35.6(2) 2_657 . . 3_777 ? Pb1 I2 Pb1 I2 -56.3(2) 2_657 . . 4_685 ? Pb1 I2 Pb1 I2 123.7(2) 2_657 . . 2_647 ? 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 2.65 3.44(3) 148 . N1 H1B I2 0.89 3.01 3.77(4) 145 4_675 N1 H1C I1 0.89 2.72 3.61(3) 179 4_575 _chemical_name_common 'bis(heptylammonium)tetraiodoplumbate(ii) PHASE IV' # Attachment 'web_deposit_cif_file_1_DrAndreasLemmerer_1307029515.cifdep 1b 805428.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_1b _database_code_depnum_ccdc_archive 'CCDC 805428' #TrackingRef 'web_deposit_cif_file_1_DrAndreasLemmerer_1307029515.cifdep 1b 805428.cif' _iucr_refine_instructions_details ; TITL 5aS23rt_a in Pbca CELL 0.71073 9.0126 8.7087 34.5612 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0010 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 56 144 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 2 2 1 OMIT 0 0 2 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 PLAN 2 ACTA BOND BOND $H CONF L.S. 4 TEMP 5.00 WGHT 0.000000 114.295990 FVAR 0.06545 C1 1 0.967369 0.465972 0.910899 11.00000 0.14140 0.15040 = 0.21860 -0.02176 -0.00230 -0.03815 AFIX 23 H1D 2 0.867784 0.498158 0.917793 11.00000 -1.20000 H1E 2 0.984154 0.363364 0.920902 11.00000 -1.20000 AFIX 0 C2 1 0.988523 0.469876 0.867795 11.00000 0.16997 0.15879 = 0.21448 -0.02439 -0.01709 -0.01509 AFIX 23 H2A 2 1.086368 0.429516 0.862027 11.00000 -1.20000 H2B 2 0.987172 0.576348 0.859561 11.00000 -1.20000 AFIX 0 C3 1 0.875863 0.381951 0.843564 11.00000 0.17538 0.16633 = 0.22987 -0.01402 -0.04310 -0.00668 AFIX 23 H3A 2 0.897990 0.272974 0.844163 11.00000 -1.20000 H3B 2 0.776811 0.397255 0.853843 11.00000 -1.20000 AFIX 0 C4 1 0.884334 0.441476 0.802252 11.00000 0.20227 0.18422 = 0.23216 -0.00636 -0.05064 0.00285 AFIX 23 H4A 2 0.815188 0.526273 0.799797 11.00000 -1.20000 H4B 2 0.983144 0.482493 0.798134 11.00000 -1.20000 AFIX 0 C5 1 0.852224 0.328644 0.770334 11.00000 0.21295 0.19212 = 0.22788 -0.01119 -0.04090 0.00716 AFIX 23 H5A 2 0.748456 0.299363 0.771349 11.00000 -1.20000 H5B 2 0.911370 0.236880 0.774229 11.00000 -1.20000 AFIX 0 C6 1 0.886761 0.396233 0.730578 11.00000 0.22759 0.20676 = 0.23152 -0.00359 -0.03708 0.01536 AFIX 23 H6A 2 0.838048 0.495105 0.728203 11.00000 -1.20000 H6B 2 0.992851 0.413057 0.728491 11.00000 -1.20000 AFIX 0 C7 1 0.836974 0.293814 0.697769 11.00000 0.27245 0.27082 = 0.23231 -0.03593 -0.04089 0.02884 AFIX 33 H7A 2 0.857879 0.343034 0.673520 11.00000 -1.50000 H7B 2 0.732251 0.275479 0.699872 11.00000 -1.50000 H7C 2 0.889159 0.197853 0.699067 11.00000 -1.50000 AFIX 0 N1 3 1.077649 0.573498 0.926203 11.00000 0.05534 0.10308 = 0.17200 0.02691 0.00134 0.00677 AFIX 33 H1A 2 1.075741 0.571168 0.951943 11.00000 -1.50000 H1B 2 1.056749 0.667998 0.918053 11.00000 -1.50000 H1C 2 1.167481 0.546679 0.917914 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.039017 0.982839 0.908103 11.00000 0.07908 0.07417 = 0.07921 0.00385 -0.00751 0.00752 I2 4 0.702187 1.199654 0.995208 11.00000 0.04761 0.04744 = 0.11484 -0.00792 -0.01260 0.01977 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03377 0.03466 = 0.07819 0.00127 0.00014 0.00029 HKLF 4 REM 5aS23rt_a in Pbca REM R1 = 0.0764 for 1783 Fo > 4sig(Fo) and 0.1033 for all 2524 data REM 97 parameters refined using 68 restraints END WGHT 0.0000 112.0765 REM Highest difference peak 1.585, deepest hole -1.378, 1-sigma level 0.207 Q1 1 1.0518 1.0879 0.9108 11.00000 0.05 1.58 Q2 1 1.0017 0.9846 0.9664 11.00000 0.05 1.51 ; _audit_creation_date 2011-05-18T09:36:56-00:00 _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(heptylammonium)tetraiodoplumbate(II) PHASE III ; _chemical_formula_moiety '2(C7 H18 N), I4 Pb' _chemical_formula_sum 'C14 H36 I4 N2 Pb' _chemical_formula_weight 947.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.0126(2) _cell_length_b 8.7087(2) _cell_length_c 34.5612(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2712.64(12) _cell_formula_units_Z 4 _cell_measurement_temperature 278(2) _cell_measurement_reflns_used 3812 _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 27.12 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.005 0 0 1 0.005 0 1 1 0.12 0 -1 -1 0.12 -1 0 1 0.14 1 0 -1 0.14 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.771 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1327 _exptl_absorpt_correction_T_max 0.8979 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 278(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 0.0746 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_number 17122 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2524 _reflns_number_gt 1783 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.52 \%A and 105-117\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. Included in this cif is the final res file, given above under _iucr_refine_instructions_details. ; _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^)^2^+114.2960P] 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 2524 _refine_ls_number_parameters 97 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.153 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.585 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.207 #----------------------------------------------------------------------------# # 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 0.967(4) 0.466(4) 0.9109(7) 0.170(10) Uani 1 1 d DU . . H1D H 0.8678 0.4982 0.9178 0.204 Uiso 1 1 calc R . . H1E H 0.9842 0.3634 0.9209 0.204 Uiso 1 1 calc R . . C2 C 0.989(4) 0.470(5) 0.8678(7) 0.181(10) Uani 1 1 d DU . . H2A H 1.0864 0.4295 0.862 0.217 Uiso 1 1 calc R . . H2B H 0.9872 0.5763 0.8596 0.217 Uiso 1 1 calc R . . C3 C 0.876(4) 0.382(4) 0.8436(7) 0.191(10) Uani 1 1 d DU . . H3A H 0.898 0.273 0.8442 0.229 Uiso 1 1 calc R . . H3B H 0.7768 0.3973 0.8538 0.229 Uiso 1 1 calc R . . C4 C 0.884(5) 0.441(4) 0.8023(7) 0.206(11) Uani 1 1 d DU . . H4A H 0.8152 0.5263 0.7998 0.247 Uiso 1 1 calc R . . H4B H 0.9831 0.4825 0.7981 0.247 Uiso 1 1 calc R . . C5 C 0.852(5) 0.329(4) 0.7703(7) 0.211(11) Uani 1 1 d DU . . H5A H 0.7485 0.2994 0.7713 0.253 Uiso 1 1 calc R . . H5B H 0.9114 0.2369 0.7742 0.253 Uiso 1 1 calc R . . C6 C 0.887(6) 0.396(5) 0.7306(8) 0.222(13) Uani 1 1 d DU . . H6A H 0.838 0.4951 0.7282 0.266 Uiso 1 1 calc R . . H6B H 0.9929 0.4131 0.7285 0.266 Uiso 1 1 calc R . . C7 C 0.837(6) 0.294(6) 0.6978(8) 0.259(18) Uani 1 1 d DU . . H7A H 0.8579 0.343 0.6735 0.388 Uiso 1 1 calc R . . H7B H 0.7323 0.2755 0.6999 0.388 Uiso 1 1 calc R . . H7C H 0.8892 0.1979 0.6991 0.388 Uiso 1 1 calc R . . N1 N 1.078(2) 0.573(3) 0.9262(7) 0.110(7) Uani 1 1 d DU . . H1A H 1.0757 0.5712 0.9519 0.165 Uiso 1 1 calc R . . H1B H 1.0567 0.668 0.9181 0.165 Uiso 1 1 calc R . . H1C H 1.1675 0.5467 0.9179 0.165 Uiso 1 1 calc R . . I1 I 1.03902(18) 0.9828(2) 0.90810(5) 0.0775(5) Uani 1 1 d . . . I2 I 0.70219(14) 1.19965(16) 0.99521(5) 0.0700(5) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0489(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 0.14(2) 0.15(2) 0.219(19) -0.02(2) 0.00(2) -0.038(16) C2 0.17(2) 0.16(2) 0.214(19) -0.02(2) -0.02(2) -0.015(18) C3 0.18(2) 0.17(2) 0.23(2) -0.014(19) -0.04(2) -0.007(19) C4 0.20(2) 0.18(2) 0.23(2) -0.006(19) -0.05(2) 0.00(2) C5 0.21(2) 0.19(2) 0.23(2) -0.01(2) -0.04(2) 0.01(2) C6 0.23(3) 0.21(3) 0.23(2) 0.00(2) -0.04(3) 0.02(3) C7 0.27(4) 0.27(4) 0.23(2) -0.04(3) -0.04(4) 0.03(4) N1 0.055(12) 0.103(17) 0.172(19) 0.027(15) 0.001(13) 0.007(11) I1 0.0791(10) 0.0742(11) 0.0792(11) 0.0039(9) -0.0075(8) 0.0075(10) I2 0.0476(7) 0.0474(7) 0.1148(13) -0.0079(9) -0.0126(8) 0.0198(6) Pb1 0.0338(5) 0.0347(5) 0.0782(7) 0.0013(6) 0.0001(5) 0.0003(4) #----------------------------------------------------------------------------# # 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 1.464(18) . ? C1 C2 1.502(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.523(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.521(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.505(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.527(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.511(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1990(17) . ? I2 Pb1 3.1921(12) 4_477 ? I2 Pb1 3.2023(12) . ? Pb1 I2 3.1921(12) 4_577 ? Pb1 I2 3.1921(12) 8_755 ? Pb1 I1 3.1990(17) 5_777 ? Pb1 I2 3.2023(12) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 104.9(19) . . ? N1 C1 H1D 110.8 . . ? C2 C1 H1D 110.8 . . ? N1 C1 H1E 110.8 . . ? C2 C1 H1E 110.8 . . ? H1D C1 H1E 108.8 . . ? C1 C2 C3 116.7(15) . . ? C1 C2 H2A 108.1 . . ? C3 C2 H2A 108.1 . . ? C1 C2 H2B 108.1 . . ? C3 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? C4 C3 C2 108.1(14) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C3 117.1(15) . . ? C5 C4 H4A 108 . . ? C3 C4 H4A 108 . . ? C5 C4 H4B 108 . . ? C3 C4 H4B 108 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C6 111.6(15) . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108 . . ? C7 C6 C5 112.8(15) . . ? C7 C6 H6A 109 . . ? C5 C6 H6A 109 . . ? C7 C6 H6B 109 . . ? C5 C6 H6B 109 . . ? H6A C6 H6B 107.8 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 157.03(5) 4_477 . ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I1 88.45(4) 4_577 5_777 ? I2 Pb1 I1 91.55(4) 8_755 5_777 ? I2 Pb1 I1 91.55(4) 4_577 . ? I2 Pb1 I1 88.45(4) 8_755 . ? I1 Pb1 I1 180.0000(10) 5_777 . ? I2 Pb1 I2 92.078(9) 4_577 . ? I2 Pb1 I2 87.922(9) 8_755 . ? I1 Pb1 I2 86.21(4) 5_777 . ? I1 Pb1 I2 93.79(4) . . ? I2 Pb1 I2 87.922(9) 4_577 5_777 ? I2 Pb1 I2 92.078(9) 8_755 5_777 ? I1 Pb1 I2 93.79(4) 5_777 5_777 ? I1 Pb1 I2 86.21(4) . 5_777 ? I2 Pb1 I2 180.0000(10) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -173(3) . . . . ? C1 C2 C3 C4 162(4) . . . . ? C2 C3 C4 C5 148(4) . . . . ? C3 C4 C5 C6 -172(4) . . . . ? C4 C5 C6 C7 -172(5) . . . . ? Pb1 I2 Pb1 I2 -11.92(13) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 168.08(13) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 76.39(16) 4_477 . . 5_777 ? Pb1 I2 Pb1 I1 -103.61(16) 4_477 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.12 3.64(2) 119 8_755 N1 H1B I1 0.89 2.77 3.64(2) 165 . N1 H1C I1 0.89 2.72 3.60(2) 168 8_855 _chemical_name_common 'bis(heptylammonium)tetraiodoplumbate(ii) PHASE III' # Attachment 'web_deposit_cif_file_2_DrAndreasLemmerer_1307029515.cifdep 1c 805429.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_1c _database_code_depnum_ccdc_archive 'CCDC 805429' _iucr_refine_instructions_details ; TITL 5aS23rt6cm_a in Pbca CELL 0.71073 8.8549 8.6840 36.6125 90.000 90.000 90.000 ZERR 4.00 0.0015 0.0019 0.0127 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 56 144 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 OMIT 0 0 4 OMIT 2 2 0 OMIT 2 2 2 OMIT 0 2 6 OMIT 0 2 0 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 PLAN 2 ACTA BOND BOND $H CONF L.S. 4 TEMP 20.00 WGHT 0.000000 290.376282 FVAR 0.06757 0.60646 C1 1 0.970739 0.468285 0.900538 11.00000 21.00000 AFIX 23 H1D 2 0.864454 0.464589 0.906891 11.00000 -1.20000 H1E 2 1.011124 0.364961 0.902969 11.00000 -1.20000 AFIX 0 C2 1 0.986107 0.519464 0.861017 11.00000 21.00000 AFIX 23 H2A 2 1.092296 0.520967 0.854520 11.00000 -1.20000 H2B 2 0.947851 0.623681 0.858718 11.00000 -1.20000 AFIX 0 C3 1 0.902215 0.416172 0.834350 11.00000 21.00000 AFIX 23 H3A 2 0.797560 0.408416 0.841957 11.00000 -1.20000 H3B 2 0.945645 0.313711 0.835344 11.00000 -1.20000 AFIX 0 C4 1 0.907533 0.473455 0.795164 11.00000 21.00000 AFIX 23 H4A 2 0.975960 0.560485 0.793776 11.00000 -1.20000 H4B 2 0.807830 0.509337 0.788235 11.00000 -1.20000 AFIX 0 C5 1 0.958544 0.351260 0.768082 11.00000 21.00000 AFIX 23 H5A 2 0.953154 0.251161 0.779767 11.00000 -1.20000 H5B 2 1.063260 0.370080 0.761712 11.00000 -1.20000 AFIX 0 C6 1 0.864924 0.347400 0.733256 11.00000 21.00000 AFIX 23 H6A 2 0.779018 0.415643 0.736129 11.00000 -1.20000 H6B 2 0.826324 0.243908 0.729761 11.00000 -1.20000 AFIX 0 C7 1 0.952508 0.394829 0.699354 11.00000 21.00000 AFIX 33 H7A 2 0.927847 0.499241 0.693138 11.00000 -1.50000 H7B 2 0.926123 0.328242 0.679420 11.00000 -1.50000 H7C 2 1.058854 0.386949 0.704097 11.00000 -1.50000 AFIX 0 N1 3 1.047959 0.568744 0.925891 11.00000 21.00000 AFIX 33 H1A 2 0.998401 0.570108 0.947036 11.00000 -1.50000 H1B 2 1.051561 0.663597 0.916725 11.00000 -1.50000 H1C 2 1.141452 0.534369 0.929517 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.034778 0.987480 0.912568 11.00000 0.13273 0.11192 = 0.49394 0.03560 -0.00427 0.02124 I2 4 0.697187 1.194740 0.996144 11.00000 0.05499 0.05615 = 0.56914 0.04779 -0.01791 0.02350 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03883 0.03953 = 0.49803 0.06004 0.00826 0.00051 HKLF 4 REM 5aS23rt6cm_a in Pbca REM R1 = 0.1740 for 800 Fo > 4sig(Fo) and 0.3144 for all 2615 data REM 50 parameters refined using 20 restraints END WGHT 0.0000 256.2924 REM Highest difference peak 1.130, deepest hole -1.507, 1-sigma level 0.205 Q1 1 0.7975 1.2553 0.9599 11.00000 0.05 1.13 Q2 1 0.7170 1.3017 0.9883 11.00000 0.05 0.85 ; _audit_creation_date 2011-05-18T10:12:53-00:00 _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(heptylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C7 H18 N), I4 Pb' _chemical_formula_sum 'C14 H36 I4 N2 Pb' _chemical_formula_weight 947.24 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.8549(15) _cell_length_b 8.6840(19) _cell_length_c 36.612(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2815.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 878 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 24.18 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.005 0 0 -1 0.005 -1 0 0 0.14 1 0 0 0.14 0 1 0 0.12 0 -1 0 0.12 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is due to the crystal quality. Phase II is stable at room temperature and all the harvested crystals from the crystal growth showed striations all through out. The diffraction data has many streaky spots, causing the high R(int). The cooling of such a crystal we presume to be a disorder-order transition from phase II to III. The crystal does not fracture much, and the quality of the diffraction pattern improves considerably, seen in the excellent data of phase II in terms of R-factor. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.378 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1569 _exptl_absorpt_correction_T_max 0.8969 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 0.2791 _diffrn_reflns_av_unetI/netI 0.1948 _diffrn_reflns_number 8183 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 2615 _reflns_number_gt 800 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The high R(int) is due to the crystal quality. Phase II is stable at room temperature and all the harvested crystals from the crystal growth showed striations all through out. The diffraction data has many streaky spots, causing the high R(int). About two years were spent obtaining better crystals, but no attempt was more successful than the other. The cooling of such a crystal from phase II to III we presume to be a disorder-order transition. The crystal does not fracture much during this transition, and the quality of the diffraction pattern improves considerably, seen in the excellent data of phase II in terms of R-factor and anisotropic displacement ellipsoids, using the same crystal for both phases III and II. Due to the disorder, and possibly being in a mixed phase, the displacement ellipsoids for the model of phase II were left isotropic for the organic chain. The current model is only an approximation to the position of the organic chain. There is no doubt substantial thermal motion occurs at room temperature, which becomes less as cooling the crystal down to phases III and IV. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.52 \%A and 115\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)^2^+290.3763P] 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 2615 _refine_ls_number_parameters 50 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.3144 _refine_ls_R_factor_gt 0.174 _refine_ls_wR_factor_ref 0.3394 _refine_ls_wR_factor_gt 0.2889 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.13 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.205 #----------------------------------------------------------------------------# # 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 0.97(2) 0.468(17) 0.901(3) 0.61(5) Uiso 1 1 d DU . . H1D H 0.8645 0.4646 0.9069 0.728 Uiso 1 1 calc R . . H1E H 1.0111 0.365 0.903 0.728 Uiso 1 1 calc R . . C2 C 0.99(2) 0.519(16) 0.861(3) 0.61(5) Uiso 1 1 d DU . . H2A H 1.0923 0.521 0.8545 0.728 Uiso 1 1 calc R . . H2B H 0.9479 0.6237 0.8587 0.728 Uiso 1 1 calc R . . C3 C 0.902(15) 0.416(15) 0.834(3) 0.61(5) Uiso 1 1 d DU . . H3A H 0.7976 0.4084 0.842 0.728 Uiso 1 1 calc R . . H3B H 0.9456 0.3137 0.8353 0.728 Uiso 1 1 calc R . . C4 C 0.908(18) 0.473(12) 0.795(3) 0.61(5) Uiso 1 1 d DU . . H4A H 0.976 0.5605 0.7938 0.728 Uiso 1 1 calc R . . H4B H 0.8078 0.5093 0.7882 0.728 Uiso 1 1 calc R . . C5 C 0.959(18) 0.35(2) 0.768(3) 0.61(5) Uiso 1 1 d DU . . H5A H 0.9532 0.2512 0.7798 0.728 Uiso 1 1 calc R . . H5B H 1.0633 0.3701 0.7617 0.728 Uiso 1 1 calc R . . C6 C 0.865(13) 0.35(2) 0.733(4) 0.61(5) Uiso 1 1 d DU . . H6A H 0.779 0.4156 0.7361 0.728 Uiso 1 1 calc R . . H6B H 0.8263 0.2439 0.7298 0.728 Uiso 1 1 calc R . . C7 C 0.95(2) 0.39(2) 0.699(3) 0.61(5) Uiso 1 1 d DU . . H7A H 0.9278 0.4992 0.6931 0.91 Uiso 1 1 calc R . . H7B H 0.9261 0.3282 0.6794 0.91 Uiso 1 1 calc R . . H7C H 1.0589 0.3869 0.7041 0.91 Uiso 1 1 calc R . . N1 N 1.048(17) 0.569(17) 0.926(3) 0.61(5) Uiso 1 1 d DU . . H1A H 0.9984 0.5701 0.947 0.91 Uiso 1 1 calc R . . H1B H 1.0516 0.6636 0.9167 0.91 Uiso 1 1 calc R . . H1C H 1.1415 0.5344 0.9295 0.91 Uiso 1 1 calc R . . I1 I 1.0348(5) 0.9875(6) 0.9126(2) 0.246(4) Uani 1 1 d . . . I2 I 0.6972(3) 1.1947(3) 0.9961(2) 0.227(4) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.192(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 I1 0.133(4) 0.112(3) 0.494(13) 0.036(5) -0.004(6) 0.021(3) I2 0.0550(16) 0.0561(16) 0.569(11) 0.048(4) -0.018(4) 0.0235(13) Pb1 0.0388(10) 0.0395(11) 0.498(8) 0.060(3) 0.008(3) 0.0005(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.45(2) . ? C1 C2 1.520(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.520(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.519(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.521(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.521(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.520(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.218(9) . ? I2 Pb1 3.173(3) . ? I2 Pb1 3.177(3) 4_477 ? Pb1 I2 3.173(3) 5_777 ? Pb1 I2 3.177(3) 4_577 ? Pb1 I2 3.177(3) 8_755 ? Pb1 I1 3.218(9) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113(3) . . ? N1 C1 H1D 109 . . ? C2 C1 H1D 109 . . ? N1 C1 H1E 109 . . ? C2 C1 H1E 109 . . ? H1D C1 H1E 107.8 . . ? C1 C2 C3 113.3(16) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 113.5(16) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 113.4(16) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 113.6(16) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 113.6(16) . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? 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 155.09(13) . 4_477 ? I2 Pb1 I2 180.000(2) 5_777 . ? I2 Pb1 I2 88.76(3) 5_777 4_577 ? I2 Pb1 I2 91.24(3) . 4_577 ? I2 Pb1 I2 91.24(3) 5_777 8_755 ? I2 Pb1 I2 88.76(3) . 8_755 ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I1 86.87(18) 5_777 . ? I2 Pb1 I1 93.13(18) . . ? I2 Pb1 I1 91.13(18) 4_577 . ? I2 Pb1 I1 88.87(18) 8_755 . ? I2 Pb1 I1 93.13(18) 5_777 5_777 ? I2 Pb1 I1 86.87(18) . 5_777 ? I2 Pb1 I1 88.87(18) 4_577 5_777 ? I2 Pb1 I1 91.13(18) 8_755 5_777 ? I1 Pb1 I1 180.000(2) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -179(19) . . . . ? C1 C2 C3 C4 176(17) . . . . ? C2 C3 C4 C5 129(16) . . . . ? C3 C4 C5 C6 136(9) . . . . ? C4 C5 C6 C7 113(16) . . . . ? Pb1 I2 Pb1 I2 -9.1(5) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 170.9(5) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 -100.3(7) 4_477 . . . ? Pb1 I2 Pb1 I1 79.7(7) 4_477 . . 5_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 2.72 3.54(14) 153 8_755 N1 H1B I1 0.89 2.82 3.67(15) 160 . N1 H1C I1 0.89 2.96 3.79(16) 156 8_855 _chemical_name_common 'bis(heptylammonium)tetraiodoplumbate(ii) PHASE II' # Attachment 'web_deposit_cif_file_3_DrAndreasLemmerer_1307029515.cifdep 2a 805430.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_2a _database_code_depnum_ccdc_archive 'CCDC 805430' #TrackingRef 'web_deposit_cif_file_3_DrAndreasLemmerer_1307029515.cifdep 2a 805430.cif' _iucr_refine_instructions_details ; TITL 6aS24_100_a in P2(1)/c CELL 0.71073 8.4542 8.9916 18.7383 90.000 96.301 90.000 ZERR 2.00 0.0009 0.0010 0.0028 0.000 0.008 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 32 80 4 8 2 MERG 2 OMIT -2.00 51.00 TWIN -1.00 0.00 0.00 0.00 -1.00 0.00 0.49 0.00 1.00 2 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.50 0.001 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 DANG 2.54 0.002 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 DFIX 1.45 0.001 C1 N1 DANG 2.45 0.002 N1 C2 EQIV $2 x+1/2, -y+3/2, z EQIV $3 x-1/2, -y+3/2, z HTAB N1 I1 HTAB N1 I2_$2 HTAB N1 I1_$3 ISOR 0.01 0.02 N1 C1 C2 C3 C4 C5 C6 C7 C8 FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 4 TEMP -100.00 WGHT 0.200000 EXTI 0.010754 BASF 0.23674 FVAR 0.21744 C1 1 0.957874 0.499842 0.791163 11.00000 0.02830 0.02708 = 0.03412 0.00581 0.00630 -0.00670 AFIX 23 H1D 2 1.075258 0.493634 0.793602 11.00000 -1.20000 H1E 2 0.921224 0.575525 0.754674 11.00000 -1.20000 AFIX 0 C2 1 0.887406 0.351965 0.768330 11.00000 0.03796 0.03099 = 0.04095 -0.00724 -0.00290 -0.00130 AFIX 23 H2A 2 0.770023 0.361139 0.763512 11.00000 -1.20000 H2B 2 0.917873 0.279059 0.806997 11.00000 -1.20000 AFIX 0 C3 1 0.935355 0.290917 0.699376 11.00000 0.04428 0.03906 = 0.04148 -0.00227 0.00367 -0.00014 AFIX 23 H3A 2 1.052907 0.293515 0.701905 11.00000 -1.20000 H3B 2 0.902328 0.185341 0.695410 11.00000 -1.20000 AFIX 0 C4 1 0.868148 0.370169 0.632380 11.00000 0.04494 0.04541 = 0.04405 0.00287 0.00424 0.00023 AFIX 23 H4A 2 0.750948 0.374001 0.631637 11.00000 -1.20000 H4B 2 0.907606 0.473909 0.634773 11.00000 -1.20000 AFIX 0 C5 1 0.906857 0.302863 0.563138 11.00000 0.05059 0.04378 = 0.04371 0.00025 0.00149 -0.00258 AFIX 23 H5A 2 1.022337 0.314939 0.560146 11.00000 -1.20000 H5B 2 0.884679 0.194843 0.564426 11.00000 -1.20000 AFIX 0 C6 1 0.818468 0.366253 0.496219 11.00000 0.04914 0.04731 = 0.04460 0.00003 0.00310 0.00264 AFIX 23 H6A 2 0.844422 0.473378 0.493832 11.00000 -1.20000 H6B 2 0.702960 0.358228 0.500159 11.00000 -1.20000 AFIX 0 C7 1 0.852106 0.294611 0.427183 11.00000 0.04830 0.04856 = 0.04497 -0.00085 0.00261 0.00371 AFIX 23 H7A 2 0.831131 0.186751 0.431052 11.00000 -1.20000 H7B 2 0.967145 0.306200 0.422931 11.00000 -1.20000 AFIX 0 C8 1 0.755695 0.353250 0.353460 11.00000 0.04547 0.04552 = 0.04403 0.00340 0.00619 0.00144 AFIX 33 H8A 2 0.791887 0.299443 0.312766 11.00000 -1.50000 H8B 2 0.775057 0.459916 0.348091 11.00000 -1.50000 H8C 2 0.641585 0.336007 0.354749 11.00000 -1.50000 AFIX 0 N1 3 0.914118 0.546519 0.860421 11.00000 0.04262 0.00690 = 0.03847 0.00395 0.00775 0.00177 AFIX 33 H1A 2 0.956313 0.637820 0.871508 11.00000 -1.50000 H1B 2 0.952353 0.479876 0.894591 11.00000 -1.50000 H1C 2 0.806228 0.551153 0.858627 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 0.984509 0.922817 0.832511 11.00000 0.04097 0.01989 = 0.04028 -0.00158 -0.00064 -0.00478 I2 4 0.693094 1.205144 0.967018 11.00000 0.01068 0.02296 = 0.05045 0.00275 0.00306 0.01047 PB1 5 1.000000 1.000000 1.000000 10.50000 0.00630 0.00735 = 0.04059 -0.00057 0.00111 0.00103 HKLF 4 REM 6aS24_100_a in P2(1)/c REM R1 = 0.1484 for 2376 Fo > 4sig(Fo) and 0.1621 for all 2625 data REM 108 parameters refined using 130 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 10.377, deepest hole -5.150, 1-sigma level 0.943 Q1 1 1.0000 0.5000 1.0000 10.50000 0.05 10.38 Q2 1 1.0111 1.0008 1.0522 11.00000 0.05 9.31 Q3 1 0.9080 0.9214 0.8334 11.00000 0.05 8.94 Q4 1 1.0613 0.9994 0.9981 11.00000 0.05 7.58 Q5 1 0.7060 1.2048 1.0199 11.00000 0.05 7.43 ; _audit_creation_date 2011-05-18T10:42:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(octylammonium)tetraiodoplumbate(II) PHASE III ; _chemical_formula_moiety '2(C8 H20 N), I4 Pb' _chemical_formula_sum 'C16 H40 I4 N2 Pb' _chemical_formula_weight 975.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.4542(9) _cell_length_b 8.9916(10) _cell_length_c 18.738(3) _cell_angle_alpha 90 _cell_angle_beta 96.301(8) _cell_angle_gamma 90 _cell_volume 1415.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6502 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 28.53 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.288 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.01 -1 0 0 0.01 0 -1 0 0.1 0 1 0 0.1 0 0 1 0.275 0 0 -1 0.275 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of the fracturing and twinning of the crystal caused by the phase transition. The space group was assigned from systematic absences using the program XPREP. Related compounds we have investigated have the same space group in their lowest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 10.322 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1108 _exptl_absorpt_correction_T_max 0.8127 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 0.166 _diffrn_reflns_av_unetI/netI 0.0919 _diffrn_reflns_number 11528 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2625 _reflns_number_gt 2376 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The crystal structure contains significant high residual electron density. The highest peak of 10.38 is located 2.669 A from N1 and 4.496 A from Pb1. It is in fact co-planar with the lead atoms and located in the middle of the voids formed by the corner- sharing octahedra. No atom position can be located there and hence this residual density is an artifact. The cause of the artifact and of the high R-factors, R(int) and GOF is that the phase transitions going from phase II at room temp to phase III has substantial movement of the inorganic layers and the organic chain, causing fracturing of the crystal. This causes non-merohedral twinning and a twin law was applied. The phases of C8PbI were all done on one crystal, and attempts to get a better crystal for phase III were unsuccessful. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.500 \%A and 115-118\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. Included in this cif is the final res file, given above under _iucr_refine_instructions_details. ; _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^)+(0.2000P)^2^] 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 0.011(3) _refine_ls_number_reflns 2625 _refine_ls_number_parameters 108 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.1621 _refine_ls_R_factor_gt 0.1484 _refine_ls_wR_factor_ref 0.4379 _refine_ls_wR_factor_gt 0.41 _refine_ls_goodness_of_fit_ref 1.986 _refine_ls_restrained_S_all 1.94 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 10.377 _refine_diff_density_min -5.15 _refine_diff_density_rms 0.943 #----------------------------------------------------------------------------# # 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 0.958(5) 0.500(2) 0.7912(15) 0.030(6) Uani 1 1 d DU . . H1D H 1.0753 0.4936 0.7936 0.036 Uiso 1 1 calc R . . H1E H 0.9212 0.5755 0.7547 0.036 Uiso 1 1 calc R . . C2 C 0.887(4) 0.352(3) 0.7683(9) 0.037(6) Uani 1 1 d DU . . H2A H 0.77 0.3611 0.7635 0.045 Uiso 1 1 calc R . . H2B H 0.9179 0.2791 0.807 0.045 Uiso 1 1 calc R . . C3 C 0.935(4) 0.291(3) 0.6994(9) 0.042(6) Uani 1 1 d DU . . H3A H 1.0529 0.2935 0.7019 0.05 Uiso 1 1 calc R . . H3B H 0.9023 0.1853 0.6954 0.05 Uiso 1 1 calc R . . C4 C 0.868(5) 0.370(4) 0.6324(9) 0.045(6) Uani 1 1 d DU . . H4A H 0.7509 0.374 0.6316 0.054 Uiso 1 1 calc R . . H4B H 0.9076 0.4739 0.6348 0.054 Uiso 1 1 calc R . . C5 C 0.907(5) 0.303(5) 0.5631(9) 0.046(6) Uani 1 1 d DU . . H5A H 1.0223 0.3149 0.5601 0.056 Uiso 1 1 calc R . . H5B H 0.8847 0.1948 0.5644 0.056 Uiso 1 1 calc R . . C6 C 0.818(5) 0.366(5) 0.4962(9) 0.047(6) Uani 1 1 d DU . . H6A H 0.8444 0.4734 0.4938 0.057 Uiso 1 1 calc R . . H6B H 0.703 0.3582 0.5002 0.057 Uiso 1 1 calc R . . C7 C 0.852(7) 0.295(5) 0.4272(9) 0.047(7) Uani 1 1 d DU . . H7A H 0.8311 0.1868 0.4311 0.057 Uiso 1 1 calc R . . H7B H 0.9671 0.3062 0.4229 0.057 Uiso 1 1 calc R . . C8 C 0.756(7) 0.353(6) 0.353(3) 0.045(9) Uani 1 1 d U . . H8A H 0.7919 0.2994 0.3128 0.067 Uiso 1 1 calc R . . H8B H 0.7751 0.4599 0.3481 0.067 Uiso 1 1 calc R . . H8C H 0.6416 0.336 0.3547 0.067 Uiso 1 1 calc R . . N1 N 0.914(5) 0.547(3) 0.8604(14) 0.029(6) Uani 1 1 d DU . . H1A H 0.9563 0.6378 0.8715 0.044 Uiso 1 1 calc R . . H1B H 0.9524 0.4799 0.8946 0.044 Uiso 1 1 calc R . . H1C H 0.8062 0.5512 0.8586 0.044 Uiso 1 1 calc R . . I1 I 0.9845(4) 0.9228(3) 0.83251(15) 0.0341(10) Uani 1 1 d . . . I2 I 0.6931(3) 1.2051(3) 0.96702(15) 0.0281(9) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0182(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(10) 0.027(8) 0.034(8) 0.006(6) 0.006(8) -0.007(7) C2 0.038(9) 0.031(8) 0.041(6) -0.007(6) -0.003(7) -0.001(7) C3 0.044(9) 0.039(9) 0.041(6) -0.002(6) 0.004(7) 0.000(8) C4 0.045(10) 0.045(10) 0.044(6) 0.003(6) 0.004(7) 0.000(8) C5 0.051(10) 0.044(10) 0.044(6) 0.000(7) 0.001(7) -0.003(8) C6 0.049(10) 0.047(10) 0.045(6) 0.000(7) 0.003(7) 0.003(8) C7 0.048(11) 0.049(11) 0.045(7) -0.001(7) 0.003(7) 0.004(8) C8 0.045(16) 0.046(17) 0.044(8) 0.003(12) 0.006(12) 0.001(14) N1 0.043(15) 0.007(11) 0.038(11) 0.004(8) 0.008(10) 0.002(11) I1 0.0410(18) 0.0199(15) 0.0403(16) -0.0016(10) -0.0006(13) -0.0048(11) I2 0.0107(12) 0.0230(16) 0.0505(17) 0.0027(10) 0.0031(11) 0.0105(9) Pb1 0.0063(10) 0.0073(11) 0.0406(13) -0.0006(6) 0.0011(11) 0.0010(6) #----------------------------------------------------------------------------# # 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 1.4500(10) . ? C1 C2 1.5000(10) . ? C1 H1D 0.99 . ? C1 H1E 0.99 . ? C2 C3 1.5000(10) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.5000(10) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.5000(10) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.5000(10) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.5000(10) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.61(6) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.203(3) . ? I2 Pb1 3.188(2) . ? I2 Pb1 3.209(2) 2_657 ? Pb1 I2 3.188(2) 3_777 ? Pb1 I1 3.203(3) 3_777 ? Pb1 I2 3.209(2) 4_685 ? Pb1 I2 3.209(2) 2_647 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.30(16) . . ? N1 C1 H1D 109.1 . . ? C2 C1 H1D 109.1 . . ? N1 C1 H1E 109.1 . . ? C2 C1 H1E 109.1 . . ? H1D C1 H1E 107.9 . . ? C1 C2 C3 115.70(17) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C2 115.70(17) . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 115.70(17) . . ? C5 C4 H4A 108.4 . . ? C3 C4 H4A 108.4 . . ? C5 C4 H4B 108.4 . . ? C3 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? C6 C5 C4 115.71(17) . . ? C6 C5 H5A 108.4 . . ? C4 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C4 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 115.69(17) . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6B 108.4 . . ? C7 C6 H6B 108.4 . . ? H6A C6 H6B 107.4 . . ? C6 C7 C8 118(3) . . ? C6 C7 H7A 107.8 . . ? C8 C7 H7A 107.8 . . ? C6 C7 H7B 107.8 . . ? C8 C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 149.44(9) . 2_657 ? I2 Pb1 I2 180.0000(10) . 3_777 ? I2 Pb1 I1 90.54(8) . 3_777 ? I2 Pb1 I1 89.46(8) 3_777 3_777 ? I2 Pb1 I1 89.46(8) . . ? I2 Pb1 I1 90.54(8) 3_777 . ? I1 Pb1 I1 180.0000(10) 3_777 . ? I2 Pb1 I2 84.55(2) . 4_685 ? I2 Pb1 I2 95.45(2) 3_777 4_685 ? I1 Pb1 I2 92.45(7) 3_777 4_685 ? I1 Pb1 I2 87.55(7) . 4_685 ? I2 Pb1 I2 95.45(2) . 2_647 ? I2 Pb1 I2 84.55(2) 3_777 2_647 ? I1 Pb1 I2 87.55(7) 3_777 2_647 ? I1 Pb1 I2 92.45(7) . 2_647 ? I2 Pb1 I2 180.0000(10) 4_685 2_647 ? 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(2) . . . . ? C1 C2 C3 C4 -71(3) . . . . ? C2 C3 C4 C5 -176(3) . . . . ? C3 C4 C5 C6 170(4) . . . . ? C4 C5 C6 C7 -178(5) . . . . ? C5 C6 C7 C8 178(5) . . . . ? Pb1 I2 Pb1 I1 36.46(18) 2_657 . . 3_777 ? Pb1 I2 Pb1 I1 -143.54(18) 2_657 . . . ? Pb1 I2 Pb1 I2 -55.9(2) 2_657 . . 4_685 ? Pb1 I2 Pb1 I2 124.1(2) 2_657 . . 2_647 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I1 0.91 2.68 3.48(3) 148 . N1 H1B I2 0.91 2.85 3.69(4) 154 4_675 N1 H1C I1 0.91 2.72 3.62(4) 172 4_575 _chemical_name_common 'bis(octylammonium)tetraiodoplumbate(ii) PHASE III' # Attachment 'web_deposit_cif_file_4_DrAndreasLemmerer_1307029515.cifdep 2b 805431.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_2b _database_code_depnum_ccdc_archive 'CCDC 805431' #TrackingRef 'web_deposit_cif_file_4_DrAndreasLemmerer_1307029515.cifdep 2b 805431.cif' _iucr_refine_instructions_details ; TITL 5aS24_a in Pbca CELL 0.71073 8.9817 8.6886 37.4821 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0003 0.0018 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 64 160 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 PLAN 2 ACTA BOND BOND $H CONF L.S. 4 TEMP 20.00 WGHT 0.000000 63.421501 EXTI 0.001204 FVAR 0.13558 C1 1 0.968075 0.471118 0.916975 11.00000 0.13101 0.14463 = 0.17098 -0.02319 0.00567 -0.03517 AFIX 23 H1D 2 0.868646 0.504219 0.923547 11.00000 -1.20000 H1E 2 0.983341 0.367008 0.925573 11.00000 -1.20000 AFIX 0 C2 1 0.988862 0.478831 0.877471 11.00000 0.16284 0.16403 = 0.16834 -0.02457 -0.00449 -0.00525 AFIX 23 H2A 2 1.088912 0.444320 0.871909 11.00000 -1.20000 H2B 2 0.981303 0.585613 0.870140 11.00000 -1.20000 AFIX 0 C3 1 0.879035 0.384288 0.855323 11.00000 0.16652 0.17904 = 0.17295 -0.01831 -0.02910 0.00730 AFIX 23 H3A 2 0.896832 0.275035 0.858510 11.00000 -1.20000 H3B 2 0.777338 0.407053 0.862252 11.00000 -1.20000 AFIX 0 C4 1 0.906552 0.431220 0.816815 11.00000 0.19174 0.21234 = 0.17526 -0.00407 -0.03303 0.02194 AFIX 23 H4A 2 0.868449 0.534801 0.813678 11.00000 -1.20000 H4B 2 1.013364 0.435607 0.813128 11.00000 -1.20000 AFIX 0 C5 1 0.841184 0.332149 0.787965 11.00000 0.20579 0.22883 = 0.16966 -0.01734 -0.02581 0.03158 AFIX 23 H5A 2 0.733392 0.332850 0.789552 11.00000 -1.20000 H5B 2 0.875355 0.226874 0.790638 11.00000 -1.20000 AFIX 0 C6 1 0.890674 0.396120 0.751912 11.00000 0.22990 0.25200 = 0.17315 -0.00403 -0.01649 0.05348 AFIX 23 H6A 2 0.860185 0.502999 0.750320 11.00000 -1.20000 H6B 2 0.998534 0.393380 0.750773 11.00000 -1.20000 AFIX 0 C7 1 0.829148 0.310712 0.720349 11.00000 0.24723 0.26670 = 0.16835 -0.00769 -0.01475 0.05744 AFIX 23 H7A 2 0.721246 0.313345 0.721251 11.00000 -1.20000 H7B 2 0.860094 0.203894 0.721624 11.00000 -1.20000 AFIX 0 C8 1 0.881195 0.379037 0.685201 11.00000 0.27478 0.25830 = 0.17067 0.01326 -0.01668 0.09004 AFIX 33 H8A 2 0.847645 0.315434 0.665863 11.00000 -1.50000 H8B 2 0.987960 0.384142 0.684970 11.00000 -1.50000 H8C 2 0.840878 0.480726 0.682553 11.00000 -1.50000 AFIX 0 N1 3 1.079174 0.574396 0.931673 11.00000 0.05988 0.07296 = 0.14588 0.01479 0.00734 0.01579 AFIX 33 H1A 2 1.075552 0.570947 0.955388 11.00000 -1.50000 H1B 2 1.060951 0.669976 0.924335 11.00000 -1.50000 H1C 2 1.169178 0.545625 0.924313 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.034783 0.983818 0.915070 11.00000 0.07824 0.07042 = 0.06795 0.00341 -0.00708 0.00559 I2 4 0.699372 1.196828 0.996352 11.00000 0.04668 0.04626 = 0.10465 -0.00692 -0.01226 0.01865 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03327 0.03485 = 0.06743 0.00116 -0.00007 0.00008 HKLF 4 REM 5aS24_a in Pbca REM R1 = 0.0650 for 2081 Fo > 4sig(Fo) and 0.0821 for all 2724 data REM 107 parameters refined using 78 restraints END WGHT 0.0000 63.4429 REM Highest difference peak 0.958, deepest hole -1.033, 1-sigma level 0.198 Q1 1 1.0665 0.4655 0.8994 11.00000 0.05 0.96 Q2 1 1.0510 1.0862 0.9179 11.00000 0.05 0.92 ; _audit_creation_date 2011-05-18T11:09:02-00:00 _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(octylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C8 H20 N), I4 Pb' _chemical_formula_sum 'C16 H40 I4 N2 Pb' _chemical_formula_weight 975.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9817(4) _cell_length_b 8.6886(3) _cell_length_c 37.4821(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2925.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3892 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 27.99 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.01 0 0 -1 0.01 1 0 0 0.1 -1 0 0 0.1 0 -1 0 0.275 0 1 0 0.275 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.992 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0871 _exptl_absorpt_correction_T_max 0.8035 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 0.0687 _diffrn_reflns_av_unetI/netI 0.0458 _diffrn_reflns_number 10421 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2724 _reflns_number_gt 2081 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.52 \%A and 105-115\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+63.4215P] 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 0.00120(7) _refine_ls_number_reflns 2724 _refine_ls_number_parameters 107 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.065 _refine_ls_wR_factor_ref 0.1334 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.278 _refine_ls_restrained_S_all 1.286 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.958 _refine_diff_density_min -1.033 _refine_diff_density_rms 0.198 #----------------------------------------------------------------------------# # 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 0.968(3) 0.471(3) 0.9170(5) 0.149(8) Uani 1 1 d DU . . H1D H 0.8686 0.5042 0.9235 0.179 Uiso 1 1 calc R . . H1E H 0.9833 0.367 0.9256 0.179 Uiso 1 1 calc R . . C2 C 0.989(3) 0.479(3) 0.8775(5) 0.165(8) Uani 1 1 d DU . . H2A H 1.0889 0.4443 0.8719 0.198 Uiso 1 1 calc R . . H2B H 0.9813 0.5856 0.8701 0.198 Uiso 1 1 calc R . . C3 C 0.879(3) 0.384(3) 0.8553(5) 0.173(8) Uani 1 1 d DU . . H3A H 0.8968 0.275 0.8585 0.207 Uiso 1 1 calc R . . H3B H 0.7773 0.4071 0.8623 0.207 Uiso 1 1 calc R . . C4 C 0.907(4) 0.431(4) 0.8168(5) 0.193(8) Uani 1 1 d DU . . H4A H 0.8684 0.5348 0.8137 0.232 Uiso 1 1 calc R . . H4B H 1.0134 0.4356 0.8131 0.232 Uiso 1 1 calc R . . C5 C 0.841(4) 0.332(4) 0.7880(5) 0.201(9) Uani 1 1 d DU . . H5A H 0.7334 0.3329 0.7896 0.242 Uiso 1 1 calc R . . H5B H 0.8754 0.2269 0.7906 0.242 Uiso 1 1 calc R . . C6 C 0.891(4) 0.396(4) 0.7519(5) 0.218(10) Uani 1 1 d DU . . H6A H 0.8602 0.503 0.7503 0.262 Uiso 1 1 calc R . . H6B H 0.9985 0.3934 0.7508 0.262 Uiso 1 1 calc R . . C7 C 0.829(4) 0.311(4) 0.7203(6) 0.227(11) Uani 1 1 d DU . . H7A H 0.7212 0.3133 0.7213 0.273 Uiso 1 1 calc R . . H7B H 0.8601 0.2039 0.7216 0.273 Uiso 1 1 calc R . . C8 C 0.881(5) 0.379(5) 0.6852(6) 0.235(15) Uani 1 1 d DU . . H8A H 0.8476 0.3154 0.6659 0.352 Uiso 1 1 calc R . . H8B H 0.988 0.3841 0.685 0.352 Uiso 1 1 calc R . . H8C H 0.8409 0.4807 0.6826 0.352 Uiso 1 1 calc R . . N1 N 1.0792(16) 0.5744(17) 0.9317(5) 0.093(5) Uani 1 1 d DU . . H1A H 1.0756 0.5709 0.9554 0.139 Uiso 1 1 calc R . . H1B H 1.061 0.67 0.9243 0.139 Uiso 1 1 calc R . . H1C H 1.1692 0.5456 0.9243 0.139 Uiso 1 1 calc R . . I1 I 1.03478(14) 0.98382(14) 0.91507(3) 0.0722(4) Uani 1 1 d . . . I2 I 0.69937(11) 1.19683(11) 0.99635(3) 0.0659(4) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0452(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 0.131(16) 0.145(17) 0.171(12) -0.023(17) 0.006(15) -0.035(13) C2 0.163(17) 0.164(17) 0.168(12) -0.025(16) -0.004(14) -0.005(15) C3 0.167(18) 0.179(18) 0.173(12) -0.018(15) -0.029(15) 0.007(16) C4 0.192(19) 0.212(19) 0.175(12) -0.004(16) -0.033(16) 0.022(18) C5 0.21(2) 0.23(2) 0.170(12) -0.017(16) -0.026(18) 0.03(2) C6 0.23(2) 0.25(2) 0.173(12) -0.004(18) -0.02(2) 0.05(2) C7 0.25(3) 0.27(2) 0.168(13) -0.01(2) -0.01(2) 0.06(2) C8 0.27(4) 0.26(3) 0.171(13) 0.01(2) -0.02(3) 0.09(3) N1 0.060(9) 0.073(10) 0.146(12) 0.015(10) 0.007(9) 0.016(8) I1 0.0782(8) 0.0704(8) 0.0679(7) 0.0034(6) -0.0071(6) 0.0056(7) I2 0.0467(6) 0.0463(6) 0.1047(9) -0.0069(6) -0.0123(6) 0.0186(5) Pb1 0.0333(4) 0.0348(4) 0.0674(5) 0.0012(4) -0.0001(4) 0.0001(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.451(16) . ? C1 C2 1.494(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.529(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.520(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.502(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.527(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.502(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.519(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.2017(12) . ? I2 Pb1 3.1881(9) 4_477 ? I2 Pb1 3.1991(9) . ? Pb1 I2 3.1881(9) 4_577 ? Pb1 I2 3.1881(9) 8_755 ? Pb1 I2 3.1991(9) 5_777 ? Pb1 I1 3.2018(12) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 105.2(16) . . ? N1 C1 H1D 110.7 . . ? C2 C1 H1D 110.7 . . ? N1 C1 H1E 110.7 . . ? C2 C1 H1E 110.7 . . ? H1D C1 H1E 108.8 . . ? C1 C2 C3 115.7(13) . . ? C1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? C1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C2 105.5(12) . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.8 . . ? C5 C4 C3 117.8(14) . . ? C5 C4 H4A 107.9 . . ? C3 C4 H4A 107.9 . . ? C5 C4 H4B 107.9 . . ? C3 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? C4 C5 C6 108.3(13) . . ? C4 C5 H5A 110 . . ? C6 C5 H5A 110 . . ? C4 C5 H5B 110 . . ? C6 C5 H5B 110 . . ? H5A C5 H5B 108.4 . . ? C7 C6 C5 114.2(14) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 112.1(15) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 156.06(4) 4_477 . ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I2 88.039(8) 4_577 5_777 ? I2 Pb1 I2 91.961(8) 8_755 5_777 ? I2 Pb1 I2 91.961(8) 4_577 . ? I2 Pb1 I2 88.039(8) 8_755 . ? I2 Pb1 I2 180.0000(10) 5_777 . ? I2 Pb1 I1 88.62(3) 4_577 5_777 ? I2 Pb1 I1 91.38(3) 8_755 5_777 ? I2 Pb1 I1 93.63(3) 5_777 5_777 ? I2 Pb1 I1 86.37(3) . 5_777 ? I2 Pb1 I1 91.38(3) 4_577 . ? I2 Pb1 I1 88.62(3) 8_755 . ? I2 Pb1 I1 86.37(3) 5_777 . ? I2 Pb1 I1 93.63(3) . . ? I1 Pb1 I1 180.0000(10) 5_777 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -177(2) . . . . ? C1 C2 C3 C4 171(3) . . . . ? C2 C3 C4 C5 166(3) . . . . ? C3 C4 C5 C6 -177(3) . . . . ? C4 C5 C6 C7 -178(3) . . . . ? C5 C6 C7 C8 180(3) . . . . ? Pb1 I2 Pb1 I2 -9.28(9) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 170.72(9) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 79.21(11) 4_477 . . 5_777 ? Pb1 I2 Pb1 I1 -100.79(11) 4_477 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.11 3.642(16) 121 8_755 N1 H1B I1 0.89 2.76 3.633(15) 168 . N1 H1C I1 0.89 2.73 3.610(15) 168 8_855 _chemical_name_common 'bis(octylammonium)tetraiodoplumbate(ii) PHASE II' # Attachment 'web_deposit_cif_file_5_DrAndreasLemmerer_1307029515.cifdep 2c 805432.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_2c _database_code_depnum_ccdc_archive 'CCDC 805432' #TrackingRef 'web_deposit_cif_file_5_DrAndreasLemmerer_1307029515.cifdep 2c 805432.cif' _iucr_refine_instructions_details ; TITL 5As24HT_A in Cmca CELL 0.71073 8.7436 8.7440 40.0276 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0003 0.0018 0.000 0.000 0.000 LATT 5 SYMM - X, - Y, Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 64 160 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 EQIV $3 x+1/2, -y+3/2, -z+2 EQIV $4 -x+3/2, y-1/2, z HTAB N1 I2_$3 HTAB N1 I2_$4 DFIX 1.52 0.001 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 DANG 2.54 0.002 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 DFIX 1.45 0.001 C1 N1 DANG 2.45 0.002 N1 C2 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 FMAP 2 PLAN 1 ACTA BOND $H CONF L.S. 4 TEMP 41.00 WGHT 0.062900 4.819800 FVAR 0.03931 PART -1 C1 1 1.016369 0.450972 0.909444 10.50000 0.30735 0.19924 = 0.32961 0.02356 -0.03055 0.04445 AFIX 23 H1D 2 0.928490 0.401354 0.919508 10.50000 -1.20000 H1E 2 1.096237 0.374946 0.906787 10.50000 -1.20000 AFIX 0 C2 1 0.972099 0.513695 0.875375 10.50000 0.34371 0.22851 = 0.32645 0.01834 -0.04680 0.04434 AFIX 23 H2A 2 0.862330 0.529558 0.874825 10.50000 -1.20000 H2B 2 1.020828 0.612336 0.872270 10.50000 -1.20000 AFIX 0 C3 1 1.016941 0.409262 0.846642 10.50000 0.38264 0.26258 = 0.33907 -0.00703 -0.04749 0.03809 AFIX 23 H3A 2 1.088548 0.333190 0.854793 10.50000 -1.20000 H3B 2 1.068805 0.469331 0.829710 10.50000 -1.20000 AFIX 0 C4 1 0.881505 0.328192 0.830732 10.50000 0.40889 0.28256 = 0.36668 -0.01914 -0.05537 0.01826 AFIX 23 H4A 2 0.820425 0.281375 0.848186 10.50000 -1.20000 H4B 2 0.818062 0.403287 0.819503 10.50000 -1.20000 AFIX 0 C5 1 0.927881 0.205835 0.805733 10.50000 0.42759 0.28147 = 0.38335 -0.02781 -0.05014 0.01191 AFIX 23 H5A 2 1.038247 0.207063 0.803289 10.50000 -1.20000 H5B 2 0.883639 0.230350 0.784165 10.50000 -1.20000 AFIX 0 C6 1 0.877715 0.045891 0.815791 10.50000 0.44312 0.28272 = 0.39818 -0.02209 -0.04784 0.01094 AFIX 23 H6A 2 0.907957 0.027613 0.838762 10.50000 -1.20000 H6B 2 0.767029 0.040155 0.814739 10.50000 -1.20000 AFIX 0 C7 1 0.945008 -0.078989 0.793842 10.50000 0.44557 0.27780 = 0.40793 -0.01603 -0.04496 0.01880 AFIX 23 H7A 2 0.875293 -0.099057 0.775508 10.50000 -1.20000 H7B 2 0.953887 -0.172155 0.806853 10.50000 -1.20000 AFIX 0 C8 1 1.101125 -0.038539 0.779665 10.50000 0.44438 0.30137 = 0.41855 -0.00181 -0.03943 0.02933 AFIX 33 H8A 2 1.136791 -0.120724 0.765802 10.50000 -1.50000 H8B 2 1.171953 -0.022497 0.797653 10.50000 -1.50000 H8C 2 1.093229 0.053152 0.766587 10.50000 -1.50000 AFIX 0 N1 3 1.070120 0.571824 0.931293 10.50000 0.16872 0.13009 = 0.24881 0.06779 0.06170 0.05479 AFIX 33 H1A 2 1.146145 0.536692 0.943930 10.50000 -1.50000 H1B 2 0.993738 0.603009 0.944316 10.50000 -1.50000 H1C 2 1.103469 0.649952 0.919044 10.50000 -1.50000 AFIX 0 MOLE 1 PART 0 PB1 5 1.000000 1.000000 1.000000 10.25000 0.03844 0.03497 = 0.14315 0.00000 0.00000 -0.00014 I1 4 1.000000 1.000000 0.920025 10.50000 0.12656 0.12309 = 0.12083 0.00000 0.00000 0.00067 I2 4 0.690669 1.190699 1.000000 10.50000 0.05506 0.05124 = 0.19161 0.00000 0.00000 0.02129 HKLF 4 REM 5As24HT_A in Cmca REM R1 = 0.0428 for 1028 Fo > 4sig(Fo) and 0.0636 for all 1449 data REM 97 parameters refined using 78 restraints END WGHT 0.0629 4.8152 REM Highest difference peak 3.018, deepest hole -0.835, 1-sigma level 0.191 Q1 1 0.8085 1.3077 1.0000 10.50000 0.05 3.02 ; _audit_creation_date 2011-05-18T13:37:29-00:00 _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(octylammonium)tetraiodoplumbate(II) PHASE I ; _chemical_formula_moiety ' 4(C4 H10 N0.50), I4 Pb' _chemical_formula_sum 'C16 H40 I4 N2 Pb' _chemical_formula_weight 975.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Acam _symmetry_space_group_name_Hall '-A 2 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' '-x-1/2, y, z+1/2' 'x-1/2, -y, z+1/2' _cell_length_a 8.7436(3) _cell_length_b 8.7440(3) _cell_length_c 40.0276(18) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3060.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 314(2) _cell_measurement_reflns_used 2900 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 27.73 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.117 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1776 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -2 0 0 0.01 2 0 0 0.01 0 0 1 0.1 0 0 -1 0.1 1 1 0 0.275 -1 -1 0 0.275 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of some fracturing of the crystal caused by the phase transition from phase II to I. The space group was assigned from systematic absences using the program XPREP. Related compounds in the literature have the same space group in their highest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.551 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0766 _exptl_absorpt_correction_T_max 0.8095 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 314(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 0.0913 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_number 8378 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1449 _reflns_number_gt 1028 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The position of the octylammonium chain shows evidence of much thermal motion of the atoms as well as predominantly the entire chain. The average chain is split over two positions, related by a two fold axis around which it sits in the asymmetric unit. Out of this reason the occupancy of the chain is 0.5. We suggest this to be only a probable model for the organic chain, seeing that the literature does not contain any information using a accurate technique such as X-ray diffraction. However, the position of the N atom relative to the inorganic chain is most important, showing their relative movements. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.520 \%A and 112-116\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+(0.0629P)^2^+4.8198P] 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 1449 _refine_ls_number_parameters 97 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.018 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.191 #----------------------------------------------------------------------------# # 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 1.016(6) 0.451(3) 0.9094(10) 0.279(16) Uani 0.5 1 d PDU A -1 H1D H 0.9285 0.4014 0.9195 0.334 Uiso 0.5 1 calc PR A -1 H1E H 1.0962 0.3749 0.9068 0.334 Uiso 0.5 1 calc PR A -1 C2 C 0.972(6) 0.514(4) 0.8754(9) 0.300(15) Uani 0.5 1 d PDU A -1 H2A H 0.8623 0.5296 0.8748 0.359 Uiso 0.5 1 calc PR A -1 H2B H 1.0208 0.6123 0.8723 0.359 Uiso 0.5 1 calc PR A -1 C3 C 1.017(4) 0.409(6) 0.8466(10) 0.328(16) Uani 0.5 1 d PDU A -1 H3A H 1.0885 0.3332 0.8548 0.394 Uiso 0.5 1 calc PR A -1 H3B H 1.0688 0.4693 0.8297 0.394 Uiso 0.5 1 calc PR A -1 C4 C 0.882(4) 0.328(4) 0.8307(13) 0.353(17) Uani 0.5 1 d PDU A -1 H4A H 0.8204 0.2814 0.8482 0.423 Uiso 0.5 1 calc PR A -1 H4B H 0.8181 0.4033 0.8195 0.423 Uiso 0.5 1 calc PR A -1 C5 C 0.928(7) 0.206(3) 0.8057(10) 0.364(18) Uani 0.5 1 d PDU A -1 H5A H 1.0382 0.2071 0.8033 0.437 Uiso 0.5 1 calc PR A -1 H5B H 0.8836 0.2304 0.7842 0.437 Uiso 0.5 1 calc PR A -1 C6 C 0.878(6) 0.046(3) 0.8158(15) 0.375(19) Uani 0.5 1 d PDU A -1 H6A H 0.908 0.0276 0.8388 0.45 Uiso 0.5 1 calc PR A -1 H6B H 0.767 0.0402 0.8147 0.45 Uiso 0.5 1 calc PR A -1 C7 C 0.945(5) -0.079(4) 0.794(2) 0.38(2) Uani 0.5 1 d PDU A -1 H7A H 0.8753 -0.0991 0.7755 0.453 Uiso 0.5 1 calc PR A -1 H7B H 0.9539 -0.1722 0.8069 0.453 Uiso 0.5 1 calc PR A -1 C8 C 1.101(7) -0.039(7) 0.7797(19) 0.39(3) Uani 0.5 1 d PDU A -1 H8A H 1.1368 -0.1207 0.7658 0.582 Uiso 0.5 1 calc PR A -1 H8B H 1.172 -0.0225 0.7977 0.582 Uiso 0.5 1 calc PR A -1 H8C H 1.0932 0.0532 0.7666 0.582 Uiso 0.5 1 calc PR A -1 N1 N 1.070(4) 0.572(3) 0.9313(6) 0.183(10) Uani 0.5 1 d PDU A -1 H1A H 1.1461 0.5367 0.9439 0.274 Uiso 0.5 1 calc PR A -1 H1B H 0.9937 0.603 0.9443 0.274 Uiso 0.5 1 calc PR A -1 H1C H 1.1035 0.65 0.919 0.274 Uiso 0.5 1 calc PR A -1 Pb1 Pb 1 1 1 0.0722(3) Uani 1 4 d S . . I1 I 1 1 0.92002(3) 0.1235(5) Uani 1 2 d S . . I2 I 0.69067(10) 1.19070(8) 1 0.0993(4) 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 0.31(3) 0.20(3) 0.33(3) 0.02(2) -0.03(3) 0.04(3) C2 0.34(3) 0.23(3) 0.33(3) 0.02(2) -0.05(3) 0.04(3) C3 0.38(4) 0.26(3) 0.34(3) -0.01(2) -0.05(3) 0.04(3) C4 0.41(4) 0.28(3) 0.37(4) -0.02(2) -0.06(3) 0.02(3) C5 0.43(4) 0.28(3) 0.38(4) -0.03(2) -0.05(3) 0.01(3) C6 0.44(4) 0.28(3) 0.40(4) -0.02(3) -0.05(3) 0.01(4) C7 0.45(5) 0.28(3) 0.41(4) -0.02(3) -0.04(4) 0.02(4) C8 0.44(5) 0.30(5) 0.42(5) 0.00(4) -0.04(4) 0.03(5) N1 0.17(3) 0.130(18) 0.25(3) 0.068(17) 0.06(2) 0.055(18) Pb1 0.0384(4) 0.0350(3) 0.1431(7) 0 0 -0.0001(2) I1 0.1266(13) 0.1231(11) 0.1208(10) 0 0 0.0007(6) I2 0.0551(5) 0.0512(4) 0.1916(11) 0 0 0.0213(4) #----------------------------------------------------------------------------# # 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 1.4500(12) . ? C1 C2 1.5200(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.5200(11) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.5200(13) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.5200(11) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.5200(13) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.5200(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.5200(15) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C8 H8C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? Pb1 I2 3.1771(7) 3_577 ? Pb1 I2 3.1771(7) 11_755 ? Pb1 I2 3.1774(8) . ? Pb1 I2 3.1774(8) 9_777 ? Pb1 I1 3.2012(14) 9_777 ? Pb1 I1 3.2012(14) . ? I2 Pb1 3.1771(7) 3_477 ? 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 111.14(17) . . ? N1 C1 H1D 109.4 . . ? C2 C1 H1D 109.4 . . ? N1 C1 H1E 109.4 . . ? C2 C1 H1E 109.4 . . ? H1D C1 H1E 108 . . ? C3 C2 C1 113.35(17) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 113.34(18) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 113.34(17) . . ? 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 . . ? C4 C5 C6 113.35(17) . . ? C4 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? C4 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 113.34(17) . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 113.34(18) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? 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 . . ? I2 Pb1 I2 180 3_577 11_755 ? I2 Pb1 I2 89.996(6) 3_577 . ? I2 Pb1 I2 90.004(6) 11_755 . ? I2 Pb1 I2 90.004(6) 3_577 9_777 ? I2 Pb1 I2 89.996(6) 11_755 9_777 ? I2 Pb1 I2 180.0000(10) . 9_777 ? I2 Pb1 I1 90 3_577 9_777 ? I2 Pb1 I1 90 11_755 9_777 ? I2 Pb1 I1 90 . 9_777 ? I2 Pb1 I1 90 9_777 9_777 ? I2 Pb1 I1 90 3_577 . ? I2 Pb1 I1 90 11_755 . ? I2 Pb1 I1 90 . . ? I2 Pb1 I1 90 9_777 . ? I1 Pb1 I1 180 9_777 . ? Pb1 I2 Pb1 153.31(3) 3_477 . ? 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 141(3) . . . . ? C1 C2 C3 C4 107(4) . . . . ? C2 C3 C4 C5 -171(3) . . . . ? C3 C4 C5 C6 117(6) . . . . ? C4 C5 C6 C7 -171(4) . . . . ? C5 C6 C7 C8 30(10) . . . . ? I2 Pb1 I2 Pb1 0 3_577 . . 3_477 ? I2 Pb1 I2 Pb1 180 11_755 . . 3_477 ? I1 Pb1 I2 Pb1 90 9_777 . . 3_477 ? I1 Pb1 I2 Pb1 -90 . . . 3_477 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.02 3.73(2) 138.2 3_567 N1 H1B I2 0.89 2.86 3.72(3) 164.4 11_755 N1 H1C I1 0.89 3.19 3.82(3) 129.5 . _chemical_name_common 'bis(octylammonium)tetraiodoplumbate(ii) PHASE I' # Attachment 'web_deposit_cif_file_6_DrAndreasLemmerer_1307029515.cifdep 3a 805433.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_3a _database_code_depnum_ccdc_archive 'CCDC 805433' #TrackingRef 'web_deposit_cif_file_6_DrAndreasLemmerer_1307029515.cifdep 3a 805433.cif' _iucr_refine_instructions_details ; TITL 6aS25d_a in P2(1)/c CELL 0.71073 8.7054 8.8401 19.7911 90.000 96.376 90.000 ZERR 2.00 0.0011 0.0010 0.0027 0.000 0.009 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 36 88 4 8 2 MERG 2 OMIT -2.00 51.00 OMIT 0 0 1 OMIT 1 2 1 OMIT -1 1 2 OMIT 1 1 8 TWIN -1.00 0.00 0.00 0.00 -1.00 0.00 0.50 0.00 1.00 2 SIMU 0.01 C1 > N1 DELU 0.003 C1 > N1 DFIX 1.50 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 DFIX 1.45 0.01 C1 N1 DANG 2.45 0.02 N1 C2 EQIV $2 x+1/2, -y+3/2, z EQIV $3 x-1/2, -y+3/2, z HTAB N1 I1 HTAB N1 I2_$2 HTAB N1 I1_$3 FMAP 2 PLAN 5 ACTA BOND BOND $H CONF L.S. 8 TEMP -50.00 WGHT 0.050500 152.353210 BASF 0.37195 FVAR 0.18336 C1 1 0.975533 0.486240 0.802420 11.00000 0.09774 0.06861 = 0.06878 -0.00661 -0.00075 0.02264 AFIX 23 H1D 2 1.087196 0.468175 0.809920 11.00000 -1.20000 H1E 2 0.956543 0.559889 0.765425 11.00000 -1.20000 AFIX 0 C2 1 0.896083 0.340980 0.780844 11.00000 0.10351 0.07641 = 0.07178 -0.01329 -0.00158 0.01709 AFIX 23 H2A 2 0.784142 0.357613 0.776845 11.00000 -1.20000 H2B 2 0.921282 0.265556 0.816652 11.00000 -1.20000 AFIX 0 C3 1 0.937323 0.277409 0.714948 11.00000 0.10498 0.08834 = 0.07136 -0.01724 -0.00120 0.01056 AFIX 23 H3A 2 0.907976 0.170343 0.712946 11.00000 -1.20000 H3B 2 1.049924 0.282102 0.715479 11.00000 -1.20000 AFIX 0 C4 1 0.865931 0.352332 0.651024 11.00000 0.10387 0.09715 = 0.07158 -0.01413 -0.00260 0.00544 AFIX 23 H4A 2 0.753349 0.351611 0.650981 11.00000 -1.20000 H4B 2 0.899303 0.458241 0.651537 11.00000 -1.20000 AFIX 0 C5 1 0.905091 0.280457 0.586475 11.00000 0.10588 0.10665 = 0.07149 -0.01391 0.00232 0.00184 AFIX 23 H5A 2 1.017643 0.283307 0.586535 11.00000 -1.20000 H5B 2 0.874585 0.173796 0.587068 11.00000 -1.20000 AFIX 0 C6 1 0.833728 0.348475 0.521196 11.00000 0.10910 0.11462 = 0.07174 -0.00855 0.00491 -0.00018 AFIX 23 H6A 2 0.866956 0.454189 0.519453 11.00000 -1.20000 H6B 2 0.721165 0.348238 0.521237 11.00000 -1.20000 AFIX 0 C7 1 0.872651 0.269771 0.458052 11.00000 0.11020 0.12021 = 0.07113 -0.00771 0.00776 -0.00104 AFIX 23 H7A 2 0.984876 0.274445 0.457140 11.00000 -1.20000 H7B 2 0.844477 0.162867 0.461163 11.00000 -1.20000 AFIX 0 C8 1 0.796610 0.330953 0.392017 11.00000 0.11197 0.12276 = 0.07118 -0.00749 0.00730 -0.00199 AFIX 23 H8A 2 0.825217 0.437656 0.388514 11.00000 -1.20000 H8B 2 0.684314 0.326519 0.392716 11.00000 -1.20000 AFIX 0 C9 1 0.837120 0.249650 0.329763 11.00000 0.11286 0.13047 = 0.07223 -0.01560 0.00681 -0.01260 AFIX 33 H9A 2 0.775583 0.289758 0.289911 11.00000 -1.50000 H9B 2 0.815995 0.142521 0.333938 11.00000 -1.50000 H9C 2 0.945946 0.264159 0.325229 11.00000 -1.50000 AFIX 0 N1 3 0.925640 0.550568 0.863551 11.00000 0.09137 0.08032 = 0.04258 -0.00346 -0.03529 0.04486 AFIX 33 H1A 2 0.971703 0.640819 0.871917 11.00000 -1.50000 H1B 2 0.951783 0.487961 0.898818 11.00000 -1.50000 H1C 2 0.822392 0.562946 0.857951 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 0.986779 0.916178 0.842932 11.00000 0.05784 0.05362 = 0.05346 -0.00504 0.00804 -0.00975 I2 4 0.695721 1.204311 0.969338 11.00000 0.02622 0.02907 = 0.07321 0.00551 0.01331 0.01373 PB1 5 1.000000 1.000000 1.000000 10.50000 0.01883 0.01704 = 0.04993 -0.00192 0.00772 0.00067 HKLF 4 REM 6aS25d_a in P2(1)/c REM R1 = 0.0862 for 2176 Fo > 4sig(Fo) and 0.1177 for all 2785 data REM 116 parameters refined using 88 restraints END WGHT 0.0491 152.4203 REM Highest difference peak 3.321, deepest hole -3.488, 1-sigma level 0.388 Q1 1 0.9941 0.9902 1.0497 11.00000 0.05 3.32 Q2 1 1.0000 0.5000 1.0000 10.50000 0.05 2.94 Q3 1 0.7465 1.1372 0.9702 11.00000 0.05 2.19 Q4 1 0.7179 1.2066 0.9214 11.00000 0.05 2.05 Q5 1 0.7014 1.2062 1.0235 11.00000 0.05 1.93 ; _audit_creation_date 2011-05-19T15:13:02-00:00 _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(nonylammonium)tetraiodoplumbate(II) PHASE III ; _chemical_formula_moiety '2(C9 H22 N), I4 Pb' _chemical_formula_sum 'C18 H44 I4 N2 Pb' _chemical_formula_weight 1003.34 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/a _symmetry_space_group_name_Hall '-P 2yab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.7054(11) _cell_length_b 8.8401(10) _cell_length_c 19.791(3) _cell_angle_alpha 90 _cell_angle_beta 96.376(9) _cell_angle_gamma 90 _cell_volume 1513.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4222 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.89 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.01 -1 0 0 0.01 1 1 -2 0.1 -1 -2 -1 0.18 1 2 2 0.1 -2 -2 1 0.1 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of the fracturing and twinning of the crystal caused by the phase transition. The space group was assigned from systematic absences using the program XPREP. Related compounds we have investigated have the same space group in their lowest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.658 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1984 _exptl_absorpt_correction_T_max 0.8232 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(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 0.1394 _diffrn_reflns_av_unetI/netI 0.0971 _diffrn_reflns_number 9425 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 2785 _reflns_number_gt 2176 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The crystal structure contains some high residual electron density. The second highest peak of 2.94 is located 2.743 A from N1 and 4.420 A from Pb1. It is in fact co-planar with the lead atoms and located in the middle of the voids formed by the corner- sharing octahedra. No atom position can be located there and hence this residual density is an artifact. The cause of the artifact and of the high R-factors, R(int) and GOF is that the phase transitions going from phase II at room temp to phase III has substantial movement of the inorganic layers and the organic chain, causing fracturing of the crystal. This causes non-merohedral twinning and a twin law was applied. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.500 \%A and 114-117\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.01 and 0.003 \%A^2^ respectively. Included in this cif is the final res file, given above under _iucr_refine_instructions_details. ; _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^)+(0.0505P)^2^+152.3532P] 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 2785 _refine_ls_number_parameters 116 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2299 _refine_ls_wR_factor_gt 0.2025 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.321 _refine_diff_density_min -3.488 _refine_diff_density_rms 0.388 #----------------------------------------------------------------------------# # 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 0.976(5) 0.486(4) 0.8024(17) 0.079(7) Uani 1 1 d DU . . H1D H 1.0872 0.4682 0.8099 0.095 Uiso 1 1 calc R . . H1E H 0.9565 0.5599 0.7654 0.095 Uiso 1 1 calc R . . C2 C 0.896(5) 0.341(4) 0.7808(13) 0.085(7) Uani 1 1 d DU . . H2A H 0.7841 0.3576 0.7768 0.102 Uiso 1 1 calc R . . H2B H 0.9213 0.2656 0.8167 0.102 Uiso 1 1 calc R . . C3 C 0.937(6) 0.277(4) 0.7149(11) 0.089(7) Uani 1 1 d DU . . H3A H 0.908 0.1703 0.7129 0.107 Uiso 1 1 calc R . . H3B H 1.0499 0.2821 0.7155 0.107 Uiso 1 1 calc R . . C4 C 0.866(6) 0.352(5) 0.6510(11) 0.092(7) Uani 1 1 d DU . . H4A H 0.7533 0.3516 0.651 0.11 Uiso 1 1 calc R . . H4B H 0.8993 0.4582 0.6515 0.11 Uiso 1 1 calc R . . C5 C 0.905(6) 0.280(5) 0.5865(11) 0.095(7) Uani 1 1 d DU . . H5A H 1.0176 0.2833 0.5865 0.114 Uiso 1 1 calc R . . H5B H 0.8746 0.1738 0.5871 0.114 Uiso 1 1 calc R . . C6 C 0.834(6) 0.348(5) 0.5212(11) 0.099(7) Uani 1 1 d DU . . H6A H 0.867 0.4542 0.5195 0.119 Uiso 1 1 calc R . . H6B H 0.7212 0.3482 0.5212 0.119 Uiso 1 1 calc R . . C7 C 0.873(7) 0.270(6) 0.4581(11) 0.101(7) Uani 1 1 d DU . . H7A H 0.9849 0.2744 0.4571 0.121 Uiso 1 1 calc R . . H7B H 0.8445 0.1629 0.4612 0.121 Uiso 1 1 calc R . . C8 C 0.797(7) 0.331(6) 0.3920(13) 0.102(8) Uani 1 1 d DU . . H8A H 0.8252 0.4377 0.3885 0.123 Uiso 1 1 calc R . . H8B H 0.6843 0.3265 0.3927 0.123 Uiso 1 1 calc R . . C9 C 0.837(8) 0.250(7) 0.3298(14) 0.105(10) Uani 1 1 d DU . . H9A H 0.7756 0.2898 0.2899 0.158 Uiso 1 1 calc R . . H9B H 0.816 0.1425 0.3339 0.158 Uiso 1 1 calc R . . H9C H 0.9459 0.2642 0.3252 0.158 Uiso 1 1 calc R . . N1 N 0.926(4) 0.551(4) 0.8636(13) 0.075(8) Uani 1 1 d DU . . H1A H 0.9717 0.6408 0.8719 0.112 Uiso 1 1 calc R . . H1B H 0.9518 0.488 0.8988 0.112 Uiso 1 1 calc R . . H1C H 0.8224 0.5629 0.858 0.112 Uiso 1 1 calc R . . I1 I 0.9868(3) 0.9162(3) 0.84293(14) 0.0548(7) Uani 1 1 d . . . I2 I 0.6957(2) 1.2043(2) 0.96934(14) 0.0422(6) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0283(4) 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 0.098(17) 0.069(14) 0.069(12) -0.007(11) -0.001(13) 0.023(13) C2 0.104(16) 0.076(14) 0.072(11) -0.013(11) -0.002(13) 0.017(13) C3 0.105(16) 0.088(14) 0.071(11) -0.017(10) -0.001(13) 0.011(14) C4 0.104(15) 0.097(14) 0.072(11) -0.014(11) -0.003(13) 0.005(14) C5 0.106(16) 0.107(15) 0.071(11) -0.014(11) 0.002(13) 0.002(14) C6 0.109(16) 0.115(16) 0.072(11) -0.009(12) 0.005(13) 0.000(15) C7 0.110(17) 0.120(17) 0.071(11) -0.008(13) 0.008(14) -0.001(16) C8 0.112(18) 0.123(18) 0.071(11) -0.007(15) 0.007(15) -0.002(17) C9 0.11(2) 0.13(2) 0.072(12) -0.016(19) 0.01(2) -0.01(2) N1 0.091(19) 0.080(16) 0.043(14) -0.003(12) -0.035(13) 0.045(15) I1 0.0578(15) 0.0536(14) 0.0535(15) -0.0050(12) 0.0080(13) -0.0098(12) I2 0.0262(8) 0.0291(9) 0.0732(15) 0.0055(10) 0.0133(11) 0.0137(8) Pb1 0.0188(6) 0.0170(6) 0.0499(9) -0.0019(6) 0.0077(11) 0.0007(6) #----------------------------------------------------------------------------# # 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(10) . ? C1 C2 1.498(10) . ? C1 H1D 0.98 . ? C1 H1E 0.98 . ? C2 C3 1.500(10) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C3 C4 1.500(10) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C4 C5 1.500(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C5 C6 1.496(10) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C6 C7 1.502(10) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C7 C8 1.499(10) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C8 C9 1.502(10) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C9 H9C 0.97 . ? N1 H1A 0.9 . ? N1 H1B 0.9 . ? N1 H1C 0.9 . ? I1 Pb1 3.185(3) . ? I2 Pb1 3.2078(19) . ? I2 Pb1 3.2146(19) 2_657 ? Pb1 I1 3.185(3) 3_777 ? Pb1 I2 3.2078(19) 3_777 ? Pb1 I2 3.2146(19) 4_685 ? Pb1 I2 3.2146(19) 2_647 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.8(15) . . ? N1 C1 H1D 108.8 . . ? C2 C1 H1D 108.8 . . ? N1 C1 H1E 108.8 . . ? C2 C1 H1E 108.8 . . ? H1D C1 H1E 107.7 . . ? C1 C2 C3 114.9(15) . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C2 C3 C4 116.8(15) . . ? C2 C3 H3A 108.1 . . ? C4 C3 H3A 108.1 . . ? C2 C3 H3B 108.1 . . ? C4 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C5 C4 C3 114.8(14) . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C4 117.0(15) . . ? C6 C5 H5A 108.1 . . ? C4 C5 H5A 108.1 . . ? C6 C5 H5B 108.1 . . ? C4 C5 H5B 108.1 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 115.0(14) . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6B 108.5 . . ? C7 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C8 C7 C6 116.1(15) . . ? C8 C7 H7A 108.3 . . ? C6 C7 H7A 108.3 . . ? C8 C7 H7B 108.3 . . ? C6 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C7 C8 C9 114.9(15) . . ? C7 C8 H8A 108.5 . . ? C9 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? C9 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 150.00(9) . 2_657 ? I1 Pb1 I1 180.0000(10) 3_777 . ? I1 Pb1 I2 90.39(7) 3_777 3_777 ? I1 Pb1 I2 89.61(7) . 3_777 ? I1 Pb1 I2 89.61(7) 3_777 . ? I1 Pb1 I2 90.39(7) . . ? I2 Pb1 I2 180.0000(10) 3_777 . ? I1 Pb1 I2 91.87(7) 3_777 4_685 ? I1 Pb1 I2 88.13(7) . 4_685 ? I2 Pb1 I2 92.85(2) 3_777 4_685 ? I2 Pb1 I2 87.15(2) . 4_685 ? I1 Pb1 I2 88.13(7) 3_777 2_647 ? I1 Pb1 I2 91.87(7) . 2_647 ? I2 Pb1 I2 87.15(2) 3_777 2_647 ? I2 Pb1 I2 92.85(2) . 2_647 ? I2 Pb1 I2 180 4_685 2_647 ? 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) . . . . ? C1 C2 C3 C4 -76(5) . . . . ? C2 C3 C4 C5 -177(4) . . . . ? C3 C4 C5 C6 179(5) . . . . ? C4 C5 C6 C7 -178(6) . . . . ? C5 C6 C7 C8 177(6) . . . . ? C6 C7 C8 C9 -180(6) . . . . ? Pb1 I2 Pb1 I1 35.90(16) 2_657 . . 3_777 ? Pb1 I2 Pb1 I1 -144.10(16) 2_657 . . . ? Pb1 I2 Pb1 I2 -56.0(2) 2_657 . . 4_685 ? Pb1 I2 Pb1 I2 124.0(2) 2_657 . . 2_647 ? 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 0.9 2.51 3.31(4) 148 . N1 H1B I2 0.9 2.95 3.73(3) 146 4_675 N1 H1C I1 0.9 2.91 3.81(4) 176 4_575 _chemical_name_common 'bis(nonylammonium)tetraiodoplumbate(ii) PHASE III' # Attachment 'web_deposit_cif_file_7_DrAndreasLemmerer_1307029515.cifdep 3b 805434.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_3b _database_code_depnum_ccdc_archive 'CCDC 805434' #TrackingRef 'web_deposit_cif_file_7_DrAndreasLemmerer_1307029515.cifdep 3b 805434.cif' _iucr_refine_instructions_details ; TITL 5aS25_a in Pbca CELL 0.71073 9.0232 8.7054 39.7578 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0009 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 72 176 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 ACTA BOND BOND $H CONF L.S. 8 TEMP 20.00 WGHT 0.023100 61.044106 EXTI 0.000480 FVAR 0.07756 C1 1 0.960255 0.473526 0.922439 11.00000 0.16020 0.17005 = 0.27701 -0.00976 0.01531 -0.03358 AFIX 23 H1D 2 0.863611 0.517111 0.927244 11.00000 -1.20000 H1E 2 0.965416 0.371530 0.932192 11.00000 -1.20000 AFIX 0 C2 1 0.987211 0.467381 0.885208 11.00000 0.18452 0.16244 = 0.26891 -0.01595 -0.01104 -0.01819 AFIX 23 H2A 2 1.084108 0.422343 0.881414 11.00000 -1.20000 H2B 2 0.990294 0.571819 0.876733 11.00000 -1.20000 AFIX 0 C3 1 0.873946 0.377587 0.864663 11.00000 0.17342 0.17051 = 0.29483 0.01175 -0.04438 -0.00921 AFIX 23 H3A 2 0.902864 0.270461 0.863259 11.00000 -1.20000 H3B 2 0.777300 0.383288 0.875274 11.00000 -1.20000 AFIX 0 C4 1 0.867611 0.447582 0.829737 11.00000 0.19790 0.18924 = 0.29572 0.01671 -0.04624 -0.00460 AFIX 23 H4A 2 0.784529 0.518215 0.829017 11.00000 -1.20000 H4B 2 0.956996 0.507556 0.826381 11.00000 -1.20000 AFIX 0 C5 1 0.852625 0.337412 0.800589 11.00000 0.20445 0.19448 = 0.29458 0.01044 -0.02493 0.00778 AFIX 23 H5A 2 0.751125 0.301244 0.799217 11.00000 -1.20000 H5B 2 0.916237 0.249183 0.804279 11.00000 -1.20000 AFIX 0 C6 1 0.894918 0.415028 0.767806 11.00000 0.21639 0.19694 = 0.30096 0.01371 -0.02045 0.00361 AFIX 23 H6A 2 0.854180 0.518143 0.767802 11.00000 -1.20000 H6B 2 1.001985 0.424262 0.766967 11.00000 -1.20000 AFIX 0 C7 1 0.843538 0.333941 0.736447 11.00000 0.22677 0.19757 = 0.29553 0.01112 -0.01421 0.00754 AFIX 23 H7A 2 0.736085 0.330747 0.736265 11.00000 -1.20000 H7B 2 0.879393 0.228909 0.736796 11.00000 -1.20000 AFIX 0 C8 1 0.897608 0.412217 0.704535 11.00000 0.24624 0.20028 = 0.30122 0.01635 -0.00805 0.01097 AFIX 23 H8A 2 0.862359 0.517477 0.704334 11.00000 -1.20000 H8B 2 1.005074 0.414897 0.704726 11.00000 -1.20000 AFIX 0 C9 1 0.846097 0.332700 0.672828 11.00000 0.29246 0.24085 = 0.29604 -0.01267 0.01553 0.01634 AFIX 33 H9A 2 0.879749 0.389271 0.653560 11.00000 -1.50000 H9B 2 0.739813 0.327791 0.672662 11.00000 -1.50000 H9C 2 0.886011 0.230528 0.672123 11.00000 -1.50000 AFIX 0 N1 3 1.077478 0.571014 0.935727 11.00000 0.06856 0.11642 = 0.19203 0.05086 0.01832 0.02326 AFIX 33 H1A 2 1.075613 0.568257 0.958100 11.00000 -1.50000 H1B 2 1.063632 0.667120 0.928769 11.00000 -1.50000 H1C 2 1.164872 0.537280 0.928437 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.039989 0.984725 0.920217 11.00000 0.08885 0.08705 = 0.07940 0.00459 -0.00640 0.00462 I2 4 0.703150 1.200528 0.995459 11.00000 0.05409 0.05116 = 0.11955 -0.00953 -0.01424 0.02229 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03795 0.03759 = 0.07943 0.00083 0.00068 0.00026 HKLF 4 REM 5aS25_a in Pbca REM R1 = 0.0672 for 2083 Fo > 4sig(Fo) and 0.0890 for all 2906 data REM 116 parameters refined using 88 restraints END WGHT 0.0001 60.0332 REM Highest difference peak 1.057, deepest hole -1.711, 1-sigma level 0.184 Q1 1 1.0586 1.0932 0.9207 11.00000 0.05 1.06 Q2 1 0.8716 0.4503 0.8997 11.00000 0.05 0.91 Q3 1 0.8350 0.3595 0.8710 11.00000 0.05 0.76 Q4 1 0.7752 1.2822 1.0140 11.00000 0.05 0.73 Q5 1 0.8930 0.4892 0.8921 11.00000 0.05 0.72 Q6 1 1.1943 0.6656 0.9127 11.00000 0.05 0.67 Q7 1 0.6969 1.1963 0.9693 11.00000 0.05 0.67 Q8 1 1.0004 0.3882 0.9860 11.00000 0.05 0.65 Q9 1 1.0693 0.4536 0.9015 11.00000 0.05 0.64 Q10 1 0.7856 0.6644 0.9121 11.00000 0.05 0.61 Q11 1 0.8576 0.3892 0.8032 11.00000 0.05 0.60 Q12 1 0.9780 0.3817 0.9172 11.00000 0.05 0.59 Q13 1 0.8383 0.4242 0.9273 11.00000 0.05 0.57 Q14 1 0.8389 0.2748 0.8395 11.00000 0.05 0.57 Q15 1 1.0068 0.4529 0.6610 11.00000 0.05 0.56 Q16 1 0.6362 1.2143 1.0125 11.00000 0.05 0.55 Q17 1 0.8852 1.0635 0.9213 11.00000 0.05 0.54 Q18 1 1.0900 0.8936 0.9190 11.00000 0.05 0.54 Q19 1 0.9955 0.9741 0.9207 11.00000 0.05 0.51 Q20 1 0.9953 0.4145 0.8175 11.00000 0.05 0.51 ; _audit_creation_date 2008-06-20T14:34:21-00:00 _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(nonylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C9 H22 N), I4 Pb' _chemical_formula_sum 'C18 H44 I4 N2 Pb' _chemical_formula_weight 1003.34 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.0232(2) _cell_length_b 8.7054(2) _cell_length_c 39.7578(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3123.00(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4798 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 27.35 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.01 0 0 -1 0.01 1 0 0 0.1 -1 0 0 0.1 0 -1 0 0.1 0 1 0 0.1 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.362 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2104 _exptl_absorpt_correction_T_max 0.8266 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 'omega scans' _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_number 14537 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2906 _reflns_number_gt 2083 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.52 \%A and 105-117\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+61.0441P] 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 0.00048(8) _refine_ls_number_reflns 2906 _refine_ls_number_parameters 116 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.089 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.148 _refine_ls_wR_factor_gt 0.1417 _refine_ls_goodness_of_fit_ref 1.237 _refine_ls_restrained_S_all 1.235 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.057 _refine_diff_density_min -1.711 _refine_diff_density_rms 0.184 #----------------------------------------------------------------------------# # 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 0.960(3) 0.474(4) 0.9224(6) 0.202(9) Uani 1 1 d DU . . H1D H 0.8636 0.5171 0.9272 0.243 Uiso 1 1 calc R . . H1E H 0.9654 0.3715 0.9322 0.243 Uiso 1 1 calc R . . C2 C 0.987(3) 0.467(4) 0.8852(6) 0.205(9) Uani 1 1 d DU . . H2A H 1.0841 0.4223 0.8814 0.246 Uiso 1 1 calc R . . H2B H 0.9903 0.5718 0.8767 0.246 Uiso 1 1 calc R . . C3 C 0.874(3) 0.378(3) 0.8647(5) 0.213(9) Uani 1 1 d DU . . H3A H 0.9029 0.2705 0.8633 0.256 Uiso 1 1 calc R . . H3B H 0.7773 0.3833 0.8753 0.256 Uiso 1 1 calc R . . C4 C 0.868(4) 0.448(3) 0.8297(6) 0.228(9) Uani 1 1 d DU . . H4A H 0.7845 0.5182 0.829 0.273 Uiso 1 1 calc R . . H4B H 0.957 0.5076 0.8264 0.273 Uiso 1 1 calc R . . C5 C 0.853(4) 0.337(3) 0.8006(5) 0.231(10) Uani 1 1 d DU . . H5A H 0.7511 0.3012 0.7992 0.277 Uiso 1 1 calc R . . H5B H 0.9162 0.2492 0.8043 0.277 Uiso 1 1 calc R . . C6 C 0.895(4) 0.415(4) 0.7678(6) 0.238(10) Uani 1 1 d DU . . H6A H 0.8542 0.5181 0.7678 0.286 Uiso 1 1 calc R . . H6B H 1.002 0.4243 0.767 0.286 Uiso 1 1 calc R . . C7 C 0.844(4) 0.334(4) 0.7364(6) 0.240(10) Uani 1 1 d DU . . H7A H 0.7361 0.3307 0.7363 0.288 Uiso 1 1 calc R . . H7B H 0.8794 0.2289 0.7368 0.288 Uiso 1 1 calc R . . C8 C 0.898(5) 0.412(4) 0.7045(6) 0.249(12) Uani 1 1 d DU . . H8A H 0.8624 0.5175 0.7043 0.299 Uiso 1 1 calc R . . H8B H 1.0051 0.4149 0.7047 0.299 Uiso 1 1 calc R . . C9 C 0.846(5) 0.333(5) 0.6728(6) 0.276(16) Uani 1 1 d DU . . H9A H 0.8797 0.3893 0.6536 0.415 Uiso 1 1 calc R . . H9B H 0.7398 0.3278 0.6727 0.415 Uiso 1 1 calc R . . H9C H 0.886 0.2305 0.6721 0.415 Uiso 1 1 calc R . . N1 N 1.0775(17) 0.571(2) 0.9357(5) 0.126(6) Uani 1 1 d DU . . H1A H 1.0756 0.5683 0.9581 0.189 Uiso 1 1 calc R . . H1B H 1.0636 0.6671 0.9288 0.189 Uiso 1 1 calc R . . H1C H 1.1649 0.5373 0.9284 0.189 Uiso 1 1 calc R . . I1 I 1.03999(16) 0.98472(15) 0.92022(3) 0.0851(5) Uani 1 1 d . . . I2 I 0.70315(12) 1.20053(12) 0.99546(3) 0.0749(4) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0517(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 0.160(18) 0.170(19) 0.277(18) -0.01(2) 0.015(19) -0.034(15) C2 0.185(18) 0.162(18) 0.269(18) -0.016(18) -0.011(18) -0.018(15) C3 0.173(18) 0.171(19) 0.295(19) 0.012(16) -0.044(19) -0.009(16) C4 0.198(18) 0.19(2) 0.30(2) 0.017(15) -0.046(19) -0.005(19) C5 0.204(19) 0.19(2) 0.295(19) 0.010(16) -0.02(2) 0.01(2) C6 0.22(2) 0.20(2) 0.30(2) 0.014(17) -0.02(2) 0.00(2) C7 0.23(2) 0.20(2) 0.296(19) 0.011(19) -0.01(2) 0.01(2) C8 0.25(3) 0.20(3) 0.30(2) 0.02(2) -0.01(3) 0.01(2) C9 0.29(4) 0.24(4) 0.30(2) -0.01(3) 0.02(3) 0.02(3) N1 0.069(11) 0.116(14) 0.192(17) 0.051(12) 0.018(11) 0.023(10) I1 0.0888(9) 0.0870(9) 0.0794(8) 0.0046(7) -0.0064(7) 0.0046(8) I2 0.0541(6) 0.0512(6) 0.1195(10) -0.0095(7) -0.0142(7) 0.0223(5) Pb1 0.0380(4) 0.0376(4) 0.0794(6) 0.0008(4) 0.0007(4) 0.0003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.455(17) . ? C1 C2 1.501(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.524(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.517(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.510(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.517(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.506(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.521(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.511(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1952(13) . ? I2 Pb1 3.1921(9) 4_477 ? I2 Pb1 3.2023(10) . ? Pb1 I2 3.1921(10) 4_577 ? Pb1 I2 3.1921(10) 8_755 ? Pb1 I1 3.1952(13) 5_777 ? Pb1 I2 3.2023(10) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 105.1(17) . . ? N1 C1 H1D 110.7 . . ? C2 C1 H1D 110.7 . . ? N1 C1 H1E 110.7 . . ? C2 C1 H1E 110.7 . . ? H1D C1 H1E 108.8 . . ? C1 C2 C3 116.0(14) . . ? C1 C2 H2A 108.3 . . ? C3 C2 H2A 108.3 . . ? C1 C2 H2B 108.3 . . ? C3 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? C4 C3 C2 108.0(13) . . ? C4 C3 H3A 110.1 . . ? C2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? C2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C5 C4 C3 116.8(14) . . ? C5 C4 H4A 108.1 . . ? C3 C4 H4A 108.1 . . ? C5 C4 H4B 108.1 . . ? C3 C4 H4B 108.1 . . ? H4A C4 H4B 107.3 . . ? C4 C5 C6 110.7(14) . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 115.2(14) . . ? C7 C6 H6A 108.5 . . ? C5 C6 H6A 108.5 . . ? C7 C6 H6B 108.5 . . ? C5 C6 H6B 108.5 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 112.5(14) . . ? C6 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 113.1(15) . . ? C9 C8 H8A 109 . . ? C7 C8 H8A 109 . . ? C9 C8 H8B 109 . . ? C7 C8 H8B 109 . . ? H8A C8 H8B 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 157.28(4) 4_477 . ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I1 91.45(3) 4_577 . ? I2 Pb1 I1 88.55(3) 8_755 . ? I2 Pb1 I1 88.55(3) 4_577 5_777 ? I2 Pb1 I1 91.45(3) 8_755 5_777 ? I1 Pb1 I1 180.0000(10) . 5_777 ? I2 Pb1 I2 92.195(7) 4_577 . ? I2 Pb1 I2 87.805(7) 8_755 . ? I1 Pb1 I2 93.51(3) . . ? I1 Pb1 I2 86.49(3) 5_777 . ? I2 Pb1 I2 87.805(7) 4_577 5_777 ? I2 Pb1 I2 92.195(7) 8_755 5_777 ? I1 Pb1 I2 86.49(3) . 5_777 ? I1 Pb1 I2 93.51(3) 5_777 5_777 ? I2 Pb1 I2 180.00(5) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -177(3) . . . . ? C1 C2 C3 C4 151(3) . . . . ? C2 C3 C4 C5 141(3) . . . . ? C3 C4 C5 C6 -162(3) . . . . ? C4 C5 C6 C7 -163(3) . . . . ? C5 C6 C7 C8 -176(4) . . . . ? C6 C7 C8 C9 -180(4) . . . . ? Pb1 I2 Pb1 I2 -13.22(10) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 166.78(10) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 -104.81(12) 4_477 . . . ? Pb1 I2 Pb1 I1 75.19(12) 4_477 . . 5_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.14 3.65(2) 119 8_755 N1 H1B I1 0.89 2.79 3.67(2) 168 . N1 H1C I1 0.89 2.72 3.59(2) 164 8_855 _chemical_name_common 'bis(nonylammonium)tetraiodoplumbate(ii) PHASE II' # Attachment 'web_deposit_cif_file_8_DrAndreasLemmerer_1307029515.cifdep 4a 805435.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_4a _database_code_depnum_ccdc_archive 'CCDC 805435' #TrackingRef 'web_deposit_cif_file_8_DrAndreasLemmerer_1307029515.cifdep 4a 805435.cif' _iucr_refine_instructions_details ; TITL 6aS99d_a in P2(1)/c CELL 0.71073 8.4329 8.9501 21.3297 90.000 96.107 90.000 ZERR 2.00 0.0034 0.0037 0.0086 0.000 0.010 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 40 96 4 8 2 MERG 2 OMIT -2.00 51.00 OMIT -2 1 2 OMIT -2 0 6 OMIT 0 0 1 TWIN -1.00 0.00 0.00 0.00 -1.00 0.00 0.54 0.00 1.00 2 SIMU 0.01 C1 > N1 DELU 0.003 C1 > N1 DFIX 1.50 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 DFIX 1.45 0.01 C1 N1 DANG 2.45 0.02 N1 C2 EQIV $2 x+1/2, -y+3/2, z EQIV $3 x-1/2, -y+3/2, z HTAB N1 I1 HTAB N1 I2_$2 HTAB N1 I1_$3 OMIT 1 2 1 OMIT -5 2 1 OMIT 1 2 2 FMAP 2 PLAN 2 ACTA BOND BOND $H CONF L.S. 8 TEMP -30.00 WGHT 0.144500 155.058594 BASF 0.40998 FVAR 0.16109 C1 1 0.960715 0.501855 0.815145 11.00000 0.04957 0.03888 = 0.05831 -0.01258 0.00421 -0.00347 AFIX 23 H1D 2 1.076762 0.497812 0.814839 11.00000 -1.20000 H1E 2 0.918835 0.575714 0.783728 11.00000 -1.20000 AFIX 0 C2 1 0.890933 0.351266 0.797399 11.00000 0.05584 0.03781 = 0.05025 -0.02050 0.00858 0.00026 AFIX 23 H2A 2 0.928588 0.279655 0.830430 11.00000 -1.20000 H2B 2 0.774676 0.357654 0.796389 11.00000 -1.20000 AFIX 0 C3 1 0.930400 0.291636 0.735300 11.00000 0.06327 0.04959 = 0.04787 -0.01473 0.01478 -0.00168 AFIX 23 H3A 2 0.902490 0.185337 0.733092 11.00000 -1.20000 H3B 2 1.045995 0.299039 0.734133 11.00000 -1.20000 AFIX 0 C4 1 0.849823 0.367368 0.677692 11.00000 0.06790 0.05668 = 0.05069 -0.00775 0.01621 -0.00290 AFIX 23 H4A 2 0.734346 0.353418 0.676824 11.00000 -1.20000 H4B 2 0.871350 0.474841 0.680982 11.00000 -1.20000 AFIX 0 C5 1 0.901409 0.311540 0.616687 11.00000 0.07235 0.06227 = 0.04938 -0.00586 0.01930 -0.00657 AFIX 23 H5A 2 1.016762 0.326713 0.617786 11.00000 -1.20000 H5B 2 0.881968 0.203638 0.614256 11.00000 -1.20000 AFIX 0 C6 1 0.822672 0.381716 0.557543 11.00000 0.07466 0.06752 = 0.05088 -0.00437 0.01836 -0.00472 AFIX 23 H6A 2 0.856024 0.486470 0.556302 11.00000 -1.20000 H6B 2 0.706931 0.380317 0.559032 11.00000 -1.20000 AFIX 0 C7 1 0.860006 0.306224 0.497927 11.00000 0.07455 0.06801 = 0.04927 -0.00175 0.01934 -0.00354 AFIX 23 H7A 2 0.976059 0.305382 0.497382 11.00000 -1.20000 H7B 2 0.824846 0.202009 0.499220 11.00000 -1.20000 AFIX 0 C8 1 0.786941 0.374202 0.437502 11.00000 0.07602 0.06978 = 0.05056 0.00131 0.01983 -0.00458 AFIX 23 H8A 2 0.817704 0.479756 0.437060 11.00000 -1.20000 H8B 2 0.670671 0.370325 0.436986 11.00000 -1.20000 AFIX 0 C9 1 0.831417 0.302380 0.378295 11.00000 0.07740 0.07085 = 0.04920 0.00280 0.02158 -0.00688 AFIX 23 H9A 2 0.947754 0.305506 0.378987 11.00000 -1.20000 H9B 2 0.799856 0.197023 0.378583 11.00000 -1.20000 AFIX 0 C10 1 0.759348 0.371108 0.317765 11.00000 0.09103 0.11082 = 0.05484 0.00160 -0.01557 0.02983 AFIX 33 H10A 2 0.793591 0.315978 0.282439 11.00000 -1.50000 H10B 2 0.793833 0.474221 0.315706 11.00000 -1.50000 H10C 2 0.643991 0.367593 0.315988 11.00000 -1.50000 AFIX 0 N1 3 0.923638 0.548535 0.876736 11.00000 0.03969 0.04497 = 0.06578 -0.03347 -0.01202 0.01270 AFIX 33 H1A 2 0.967147 0.638809 0.885845 11.00000 -1.50000 H1B 2 0.963524 0.481783 0.905800 11.00000 -1.50000 H1C 2 0.817135 0.554104 0.876948 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 0.983516 0.923153 0.853420 11.00000 0.05779 0.03548 = 0.02754 -0.00102 0.00347 -0.00428 I2 4 0.694289 1.206470 0.971572 11.00000 0.02437 0.03389 = 0.04006 0.00293 0.00487 0.01357 PB1 5 1.000000 1.000000 1.000000 10.50000 0.01841 0.01794 = 0.02591 -0.00106 0.00557 0.00074 HKLF 4 REM 6aS99d_a in P2(1)/c REM R1 = 0.0952 for 2664 Fo > 4sig(Fo) and 0.1075 for all 2965 data REM 125 parameters refined using 90 restraints END WGHT 0.1440 154.9457 REM Highest difference peak 4.361, deepest hole -3.529, 1-sigma level 0.495 Q1 1 0.9963 0.5696 0.8574 11.00000 0.05 4.36 Q2 1 1.0169 0.9205 0.8689 11.00000 0.05 4.20 ; _audit_creation_date 2011-05-19T15:36:22-00:00 _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(decylammonium)tetraiodoplumbate(II) PHASE IV ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # 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+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.433(3) _cell_length_b 8.950(4) _cell_length_c 21.330(9) _cell_angle_alpha 90 _cell_angle_beta 96.107(10) _cell_angle_gamma 90 _cell_volume 1600.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5987 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 28.33 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.14 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.04 1 0 0 0.04 0 -1 0 0.14 0 1 0 0.14 0 0 -1 0.32 0 0 1 0.32 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of the fracturing and twinning of the crystal caused by the phase transition. The space group was assigned from systematic absences using the program XPREP. Related compounds we have investigated have the same space group in their lowest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.136 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0689 _exptl_absorpt_correction_T_max 0.486 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 243(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 0.1522 _diffrn_reflns_av_unetI/netI 0.0696 _diffrn_reflns_number 19089 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2965 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The crystal structure contains significant high residual electron density. The highest peak of 4.36 is located 0.797 A from N1. This could indicate a disorder of the N atom over two positions. However, the displacement ellipsoids are reasonable, even taking into account the restraints applied on them, and hence this residual density could be an artifact. The high R-factors, R(int) and GOF are due to fracturing of the crystal, shown clearly in the figure in the paper in going from phase II at room temp to phase IV, due to the substantial movement of the inorganic layers and the organic chain, causing fracturing of the crystal, especially the transition from II to III. This causes non-merohedral twinning and a twin law was applied. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.500 \%A and 112-117\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. Included in this cif is the final res file, given above under _iucr_refine_instructions_details. ; _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^)+(0.1445P)^2^+155.0586P] 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 2965 _refine_ls_number_parameters 125 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.2768 _refine_ls_wR_factor_gt 0.2602 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.361 _refine_diff_density_min -3.529 _refine_diff_density_rms 0.495 #----------------------------------------------------------------------------# # 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 0.961(6) 0.502(3) 0.8151(14) 0.049(5) Uani 1 1 d DU . . H1D H 1.0768 0.4978 0.8148 0.059 Uiso 1 1 calc R . . H1E H 0.9188 0.5757 0.7837 0.059 Uiso 1 1 calc R . . C2 C 0.891(4) 0.351(3) 0.7974(10) 0.048(5) Uani 1 1 d DU . . H2A H 0.9286 0.2797 0.8304 0.057 Uiso 1 1 calc R . . H2B H 0.7747 0.3577 0.7964 0.057 Uiso 1 1 calc R . . C3 C 0.930(5) 0.292(3) 0.7353(9) 0.053(5) Uani 1 1 d DU . . H3A H 0.9025 0.1853 0.7331 0.064 Uiso 1 1 calc R . . H3B H 1.046 0.299 0.7341 0.064 Uiso 1 1 calc R . . C4 C 0.850(5) 0.367(4) 0.6777(9) 0.058(5) Uani 1 1 d DU . . H4A H 0.7343 0.3534 0.6768 0.069 Uiso 1 1 calc R . . H4B H 0.8713 0.4748 0.681 0.069 Uiso 1 1 calc R . . C5 C 0.901(5) 0.312(4) 0.6167(9) 0.060(5) Uani 1 1 d DU . . H5A H 1.0168 0.3267 0.6178 0.072 Uiso 1 1 calc R . . H5B H 0.882 0.2036 0.6143 0.072 Uiso 1 1 calc R . . C6 C 0.823(6) 0.382(4) 0.5575(9) 0.064(5) Uani 1 1 d DU . . H6A H 0.856 0.4865 0.5563 0.076 Uiso 1 1 calc R . . H6B H 0.7069 0.3803 0.559 0.076 Uiso 1 1 calc R . . C7 C 0.860(6) 0.306(4) 0.4979(9) 0.063(6) Uani 1 1 d DU . . H7A H 0.9761 0.3054 0.4974 0.076 Uiso 1 1 calc R . . H7B H 0.8248 0.202 0.4992 0.076 Uiso 1 1 calc R . . C8 C 0.787(6) 0.374(4) 0.4375(10) 0.065(6) Uani 1 1 d DU . . H8A H 0.8177 0.4798 0.4371 0.077 Uiso 1 1 calc R . . H8B H 0.6707 0.3703 0.437 0.077 Uiso 1 1 calc R . . C9 C 0.831(6) 0.302(4) 0.3783(11) 0.065(7) Uani 1 1 d DU . . H9A H 0.9478 0.3055 0.379 0.078 Uiso 1 1 calc R . . H9B H 0.7999 0.197 0.3786 0.078 Uiso 1 1 calc R . . N1 N 0.924(4) 0.549(3) 0.8767(13) 0.051(7) Uani 1 1 d DU . . H1A H 0.9671 0.6388 0.8858 0.077 Uiso 1 1 calc R . . H1B H 0.9635 0.4818 0.9058 0.077 Uiso 1 1 calc R . . H1C H 0.8171 0.5541 0.8769 0.077 Uiso 1 1 calc R . . C10 C 0.759(8) 0.371(7) 0.3178(12) 0.087(18) Uani 1 1 d D . . H10A H 0.7936 0.316 0.2824 0.131 Uiso 1 1 calc R . . H10B H 0.7938 0.4742 0.3157 0.131 Uiso 1 1 calc R . . H10C H 0.644 0.3676 0.316 0.131 Uiso 1 1 calc R . . I1 I 0.9835(3) 0.9232(2) 0.85342(11) 0.0403(6) Uani 1 1 d . . . I2 I 0.6943(2) 1.2065(2) 0.97157(11) 0.0327(5) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0205(4) 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 0.050(12) 0.039(11) 0.058(10) -0.013(9) 0.004(11) -0.003(10) C2 0.056(12) 0.038(10) 0.050(8) -0.021(8) 0.009(10) 0.000(9) C3 0.063(12) 0.050(10) 0.048(8) -0.015(8) 0.015(10) -0.002(10) C4 0.068(12) 0.057(11) 0.051(8) -0.008(8) 0.016(10) -0.003(10) C5 0.072(12) 0.062(12) 0.049(8) -0.006(9) 0.019(10) -0.007(11) C6 0.075(13) 0.068(12) 0.051(8) -0.004(9) 0.018(11) -0.005(11) C7 0.075(14) 0.068(13) 0.049(8) -0.002(10) 0.019(11) -0.004(12) C8 0.076(15) 0.070(14) 0.051(9) 0.001(10) 0.020(12) -0.005(13) C9 0.077(17) 0.071(16) 0.049(9) 0.003(12) 0.022(13) -0.007(14) N1 0.040(14) 0.045(14) 0.066(13) -0.033(11) -0.012(12) 0.013(12) C10 0.09(4) 0.11(5) 0.05(3) 0.00(3) -0.02(3) 0.03(4) I1 0.0578(15) 0.0355(11) 0.0275(10) -0.0010(8) 0.0035(11) -0.0043(11) I2 0.0244(9) 0.0339(11) 0.0401(11) 0.0029(8) 0.0049(10) 0.0136(8) Pb1 0.0184(7) 0.0179(7) 0.0259(7) -0.0011(5) 0.0056(10) 0.0007(6) #----------------------------------------------------------------------------# # 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 1.444(10) . ? C1 C2 1.503(10) . ? C1 H1D 0.98 . ? C1 H1E 0.98 . ? C2 C3 1.498(10) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C3 C4 1.501(10) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C4 C5 1.501(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C5 C6 1.500(10) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C6 C7 1.503(10) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C7 C8 1.497(10) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C8 C9 1.500(10) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C9 C10 1.499(10) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? N1 H1A 0.9 . ? N1 H1B 0.9 . ? N1 H1C 0.9 . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C10 H10C 0.97 . ? I1 Pb1 3.190(3) . ? I2 Pb1 3.177(2) . ? I2 Pb1 3.188(2) 2_657 ? Pb1 I2 3.177(2) 3_777 ? Pb1 I2 3.188(2) 4_685 ? Pb1 I2 3.188(2) 2_647 ? Pb1 I1 3.190(3) 3_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.8(14) . . ? N1 C1 H1D 109.3 . . ? C2 C1 H1D 109.3 . . ? N1 C1 H1E 109.3 . . ? C2 C1 H1E 109.3 . . ? H1D C1 H1E 107.9 . . ? C3 C2 C1 115.1(15) . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2B 108.5 . . ? C1 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C2 C3 C4 116.0(15) . . ? 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 . . ? C5 C4 C3 114.3(14) . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4B 108.7 . . ? C3 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 116.5(14) . . ? C6 C5 H5A 108.2 . . ? C4 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? C4 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? C5 C6 C7 114.2(14) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C6 116.2(14) . . ? C8 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? C8 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? C7 C8 C9 115.7(15) . . ? C7 C8 H8A 108.4 . . ? C9 C8 H8A 108.4 . . ? C7 C8 H8B 108.4 . . ? C9 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C10 C9 C8 115.8(15) . . ? C10 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? 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 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Pb1 I2 Pb1 149.98(8) . 2_657 ? I2 Pb1 I2 180.0000(10) . 3_777 ? I2 Pb1 I2 84.69(4) . 4_685 ? I2 Pb1 I2 95.31(4) 3_777 4_685 ? I2 Pb1 I2 95.31(4) . 2_647 ? I2 Pb1 I2 84.69(4) 3_777 2_647 ? I2 Pb1 I2 180 4_685 2_647 ? I2 Pb1 I1 90.66(7) . 3_777 ? I2 Pb1 I1 89.34(7) 3_777 3_777 ? I2 Pb1 I1 92.24(6) 4_685 3_777 ? I2 Pb1 I1 87.76(6) 2_647 3_777 ? I2 Pb1 I1 89.34(7) . . ? I2 Pb1 I1 90.66(7) 3_777 . ? I2 Pb1 I1 87.76(6) 4_685 . ? I2 Pb1 I1 92.24(6) 2_647 . ? I1 Pb1 I1 180.0000(10) 3_777 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -177(3) . . . . ? C1 C2 C3 C4 -72(4) . . . . ? C2 C3 C4 C5 176(3) . . . . ? C3 C4 C5 C6 179(4) . . . . ? C4 C5 C6 C7 -171(4) . . . . ? C5 C6 C7 C8 -179(4) . . . . ? C6 C7 C8 C9 177(5) . . . . ? C7 C8 C9 C10 -180(5) . . . . ? Pb1 I2 Pb1 I2 14E1(10) 2_657 . . 3_777 ? Pb1 I2 Pb1 I2 -56.11(19) 2_657 . . 4_685 ? Pb1 I2 Pb1 I2 123.89(19) 2_657 . . 2_647 ? Pb1 I2 Pb1 I1 36.07(16) 2_657 . . 3_777 ? Pb1 I2 Pb1 I1 -143.93(16) 2_657 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I1 0.9 2.64 3.43(3) 147 . N1 H1B I2 0.9 2.83 3.68(3) 157 4_675 N1 H1C I1 0.9 2.81 3.70(3) 169 4_575 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE IV' # Attachment 'web_deposit_cif_file_9_DrAndreasLemmerer_1307029515.cifdep 4b 805436.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_4b _database_code_depnum_ccdc_archive 'CCDC 805436' #TrackingRef 'web_deposit_cif_file_9_DrAndreasLemmerer_1307029515.cifdep 4b 805436.cif' _iucr_refine_instructions_details ; TITL 5aS99c_a in Pbca CELL 0.71073 8.8314 8.4871 43.9491 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0013 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 80 192 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 EQIV $2 -x+5/2, y-1/2, z EQIV $3 x, y-1, z EQIV $4 -x+3/2, y-1/2, z HTAB N1 I1_$2 HTAB N1 I1_$3 HTAB N1 I2_$4 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 ACTA BOND BOND $H CONF L.S. 4 TEMP -5.00 WGHT 0.000000 174.642395 EXTI 0.000423 FVAR 0.09036 C1 1 1.016660 0.529650 0.911108 11.00000 0.17601 0.13300 = 0.08776 0.02133 -0.05104 0.01576 AFIX 23 H1D 2 1.104397 0.515448 0.898117 11.00000 -1.20000 H1E 2 1.006480 0.641126 0.915526 11.00000 -1.20000 AFIX 0 C2 1 0.876475 0.471127 0.895026 11.00000 0.17870 0.15090 = 0.07534 0.01704 -0.04311 0.00438 AFIX 23 H2A 2 0.790801 0.478571 0.908762 11.00000 -1.20000 H2B 2 0.890007 0.360981 0.889801 11.00000 -1.20000 AFIX 0 C3 1 0.841802 0.563974 0.866227 11.00000 0.15493 0.13128 = 0.06779 0.00827 -0.03427 0.00296 AFIX 23 H3A 2 0.732918 0.575363 0.864339 11.00000 -1.20000 H3B 2 0.884710 0.668696 0.868181 11.00000 -1.20000 AFIX 0 C4 1 0.902714 0.488505 0.837420 11.00000 0.12432 0.12260 = 0.07592 0.01148 -0.02809 0.00151 AFIX 23 H4A 2 0.872084 0.378775 0.836951 11.00000 -1.20000 H4B 2 1.012482 0.491540 0.837921 11.00000 -1.20000 AFIX 0 C5 1 0.848144 0.568736 0.808541 11.00000 0.10363 0.11162 = 0.06824 0.01035 -0.01481 -0.00433 AFIX 23 H5A 2 0.888330 0.675062 0.807969 11.00000 -1.20000 H5B 2 0.738595 0.576332 0.809165 11.00000 -1.20000 AFIX 0 C6 1 0.894256 0.483604 0.779582 11.00000 0.09538 0.11059 = 0.07300 0.01053 -0.00643 -0.01002 AFIX 23 H6A 2 1.003135 0.468560 0.779652 11.00000 -1.20000 H6B 2 0.847232 0.380327 0.779301 11.00000 -1.20000 AFIX 0 C7 1 0.849534 0.572223 0.750939 11.00000 0.09173 0.11385 = 0.06801 0.00852 -0.00639 -0.01436 AFIX 23 H7A 2 0.740612 0.586929 0.750906 11.00000 -1.20000 H7B 2 0.896100 0.675713 0.751347 11.00000 -1.20000 AFIX 0 C8 1 0.895380 0.489173 0.721757 11.00000 0.09790 0.12443 = 0.07269 0.00393 0.00183 -0.02005 AFIX 23 H8A 2 1.004434 0.475576 0.721646 11.00000 -1.20000 H8B 2 0.849698 0.385251 0.721416 11.00000 -1.20000 AFIX 0 C9 1 0.848783 0.577548 0.693281 11.00000 0.10661 0.13508 = 0.06723 0.00004 -0.00282 -0.01801 AFIX 23 H9A 2 0.897149 0.680161 0.693334 11.00000 -1.20000 H9B 2 0.740161 0.594298 0.693769 11.00000 -1.20000 AFIX 0 C10 1 0.889567 0.492822 0.663966 11.00000 0.14126 0.17530 = 0.07257 -0.01093 0.00513 -0.00714 AFIX 33 H10A 2 0.858675 0.555567 0.646884 11.00000 -1.50000 H10B 2 0.838749 0.392890 0.663299 11.00000 -1.50000 H10C 2 0.997056 0.476454 0.663185 11.00000 -1.50000 AFIX 0 N1 3 1.036993 0.442585 0.939165 11.00000 0.09569 0.06389 = 0.07640 -0.00023 -0.01646 0.01338 AFIX 33 H1A 2 1.123638 0.471346 0.947889 11.00000 -1.50000 H1B 2 1.039467 0.339850 0.935134 11.00000 -1.50000 H1C 2 0.960366 0.463071 0.951709 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.066976 1.019747 0.928679 11.00000 0.07895 0.07470 = 0.04629 -0.00241 0.00593 0.00153 I2 4 0.698988 1.195434 0.988015 11.00000 0.04778 0.04371 = 0.08274 0.00444 0.00581 0.02119 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03483 0.03524 = 0.04729 0.00014 0.00293 -0.00164 HKLF 4 REM 5aS99c_a in Pbca REM R1 = 0.0847 for 2647 Fo > 4sig(Fo) and 0.0960 for all 3069 data REM 125 parameters refined using 98 restraints END WGHT 0.0000 174.4634 REM Highest difference peak 2.812, deepest hole -3.430, 1-sigma level 0.258 Q1 1 0.7990 1.3049 1.0122 11.00000 0.05 2.81 Q2 1 0.6586 1.2515 1.0139 11.00000 0.05 1.58 Q3 1 0.9995 0.3875 0.9764 11.00000 0.05 1.52 Q4 1 0.9158 0.5184 0.9191 11.00000 0.05 1.40 Q5 1 1.1272 0.3262 0.9427 11.00000 0.05 1.34 Q6 1 0.7289 1.3230 0.9877 11.00000 0.05 1.32 Q7 1 0.9214 1.0402 0.9323 11.00000 0.05 1.31 Q8 1 0.7184 1.1108 1.0113 11.00000 0.05 1.25 Q9 1 0.8920 1.2052 1.0119 11.00000 0.05 1.23 Q10 1 0.8014 1.0921 0.9908 11.00000 0.05 1.17 Q11 1 0.9941 0.4566 0.8908 11.00000 0.05 1.15 Q12 1 1.2615 0.3262 0.9409 11.00000 0.05 1.11 Q13 1 1.0042 0.5531 0.6406 11.00000 0.05 1.11 Q14 1 0.9968 0.9203 0.9243 11.00000 0.05 1.10 Q15 1 0.8857 1.2956 0.9877 11.00000 0.05 1.09 Q16 1 0.9995 0.8889 0.9991 11.00000 0.05 1.08 Q17 1 0.7752 0.2209 0.9173 11.00000 0.05 1.07 Q18 1 0.6135 1.3019 0.9869 11.00000 0.05 1.07 Q19 1 0.8409 1.2506 0.9806 11.00000 0.05 1.07 Q20 1 0.8635 0.7198 0.9181 11.00000 0.05 1.05 ; _audit_creation_date 2008-06-23T12:18:57-00:00 _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(decylammonium)tetraiodoplumbate(II) PHASE III ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.8314(2) _cell_length_b 8.4871(2) _cell_length_c 43.9491(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3294.12(15) _cell_formula_units_Z 4 _cell_measurement_temperature 268(2) _cell_measurement_reflns_used 5447 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 28.29 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.08 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.04 0 0 1 0.04 0 1 0 0.32 0 -1 0 0.32 -1 0 0 0.14 1 0 0 0.14 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.879 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0635 _exptl_absorpt_correction_T_max 0.4467 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 268(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 'omega scans' _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_unetI/netI 0.0324 _diffrn_reflns_number 22073 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 3069 _reflns_number_gt 2647 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.520 \%A and 109-114\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+174.6424P] 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 0.00042(6) _refine_ls_number_reflns 3069 _refine_ls_number_parameters 125 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.096 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 1.404 _refine_ls_restrained_S_all 1.387 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 2.812 _refine_diff_density_min -3.43 _refine_diff_density_rms 0.258 #----------------------------------------------------------------------------# # 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 1.017(4) 0.530(4) 0.9111(7) 0.132(9) Uani 1 1 d DU . . H1D H 1.1044 0.5154 0.8981 0.159 Uiso 1 1 calc R . . H1E H 1.0065 0.6411 0.9155 0.159 Uiso 1 1 calc R . . C2 C 0.876(4) 0.471(4) 0.8950(4) 0.135(8) Uani 1 1 d DU . . H2A H 0.7908 0.4786 0.9088 0.162 Uiso 1 1 calc R . . H2B H 0.89 0.361 0.8898 0.162 Uiso 1 1 calc R . . C3 C 0.842(4) 0.564(4) 0.8662(4) 0.118(8) Uani 1 1 d DU . . H3A H 0.7329 0.5754 0.8643 0.142 Uiso 1 1 calc R . . H3B H 0.8847 0.6687 0.8682 0.142 Uiso 1 1 calc R . . C4 C 0.903(4) 0.489(4) 0.8374(4) 0.108(7) Uani 1 1 d DU . . H4A H 0.8721 0.3788 0.837 0.129 Uiso 1 1 calc R . . H4B H 1.0125 0.4915 0.8379 0.129 Uiso 1 1 calc R . . C5 C 0.848(4) 0.569(3) 0.8085(3) 0.094(7) Uani 1 1 d DU . . H5A H 0.8883 0.6751 0.808 0.113 Uiso 1 1 calc R . . H5B H 0.7386 0.5763 0.8092 0.113 Uiso 1 1 calc R . . C6 C 0.894(4) 0.484(3) 0.7796(3) 0.093(6) Uani 1 1 d DU . . H6A H 1.0031 0.4686 0.7797 0.112 Uiso 1 1 calc R . . H6B H 0.8472 0.3803 0.7793 0.112 Uiso 1 1 calc R . . C7 C 0.850(4) 0.572(3) 0.7509(3) 0.091(6) Uani 1 1 d DU . . H7A H 0.7406 0.5869 0.7509 0.109 Uiso 1 1 calc R . . H7B H 0.8961 0.6757 0.7513 0.109 Uiso 1 1 calc R . . C8 C 0.895(4) 0.489(3) 0.7218(4) 0.098(7) Uani 1 1 d DU . . H8A H 1.0044 0.4756 0.7216 0.118 Uiso 1 1 calc R . . H8B H 0.8497 0.3853 0.7214 0.118 Uiso 1 1 calc R . . C9 C 0.849(4) 0.578(3) 0.6933(4) 0.103(8) Uani 1 1 d DU . . H9A H 0.8971 0.6802 0.6933 0.124 Uiso 1 1 calc R . . H9B H 0.7402 0.5943 0.6938 0.124 Uiso 1 1 calc R . . C10 C 0.890(5) 0.493(5) 0.6640(4) 0.130(12) Uani 1 1 d DU . . H10A H 0.8587 0.5556 0.6469 0.195 Uiso 1 1 calc R . . H10B H 0.8387 0.3929 0.6633 0.195 Uiso 1 1 calc R . . H10C H 0.9971 0.4765 0.6632 0.195 Uiso 1 1 calc R . . N1 N 1.037(3) 0.443(3) 0.9392(5) 0.079(6) Uani 1 1 d DU . . H1A H 1.1236 0.4713 0.9479 0.118 Uiso 1 1 calc R . . H1B H 1.0395 0.3399 0.9351 0.118 Uiso 1 1 calc R . . H1C H 0.9604 0.4631 0.9517 0.118 Uiso 1 1 calc R . . I1 I 1.0670(2) 1.0197(2) 0.92868(4) 0.0666(5) Uani 1 1 d . . . I2 I 0.69899(17) 1.19543(17) 0.98801(4) 0.0581(5) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0391(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 0.18(2) 0.13(2) 0.088(14) 0.021(13) -0.051(13) 0.016(19) C2 0.18(2) 0.151(19) 0.075(8) 0.017(13) -0.043(11) 0.004(18) C3 0.155(18) 0.131(17) 0.068(7) 0.008(12) -0.034(11) 0.003(16) C4 0.124(16) 0.123(16) 0.076(7) 0.011(11) -0.028(12) 0.002(15) C5 0.104(15) 0.112(16) 0.068(7) 0.010(10) -0.015(12) -0.004(14) C6 0.095(14) 0.111(15) 0.073(7) 0.011(10) -0.006(12) -0.010(14) C7 0.092(14) 0.114(15) 0.068(7) 0.009(10) -0.006(11) -0.014(14) C8 0.098(15) 0.124(17) 0.073(7) 0.004(11) 0.002(12) -0.020(15) C9 0.107(17) 0.135(19) 0.067(8) 0.000(12) -0.003(13) -0.018(17) C10 0.14(3) 0.18(3) 0.073(8) -0.011(17) 0.005(19) -0.01(3) N1 0.096(16) 0.064(13) 0.076(13) 0.000(11) -0.016(11) 0.013(13) I1 0.0790(12) 0.0747(11) 0.0463(9) -0.0024(8) 0.0059(8) 0.0015(10) I2 0.0478(8) 0.0437(8) 0.0827(11) 0.0044(8) 0.0058(8) 0.0212(7) Pb1 0.0348(5) 0.0352(5) 0.0473(6) 0.0001(5) 0.0029(4) -0.0016(4) #----------------------------------------------------------------------------# # 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 1.449(18) . ? C1 C2 1.510(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.522(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.517(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.519(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.519(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.519(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.518(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.516(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.519(10) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.1942(16) . ? I2 Pb1 3.1698(13) 4_477 ? I2 Pb1 3.1773(14) . ? Pb1 I2 3.1698(14) 4_577 ? Pb1 I2 3.1698(14) 8_755 ? Pb1 I2 3.1773(14) 5_777 ? Pb1 I1 3.1942(16) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.4(19) . . ? N1 C1 H1D 109.8 . . ? C2 C1 H1D 109.8 . . ? N1 C1 H1E 109.8 . . ? C2 C1 H1E 109.8 . . ? H1D C1 H1E 108.2 . . ? C1 C2 C3 112.6(14) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 113.8(14) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 113.3(13) . . ? C3 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 C6 113.7(12) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 112.9(12) . . ? C7 C6 H6A 109 . . ? C5 C6 H6A 109 . . ? C7 C6 H6B 109 . . ? C5 C6 H6B 109 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 113.6(12) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 113.3(13) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 113.7(14) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 149.54(6) 4_477 . ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I2 86.233(14) 4_577 5_777 ? I2 Pb1 I2 93.767(14) 8_755 5_777 ? I2 Pb1 I2 93.767(14) 4_577 . ? I2 Pb1 I2 86.233(14) 8_755 . ? I2 Pb1 I2 180.0000(10) 5_777 . ? I2 Pb1 I1 91.01(5) 4_577 . ? I2 Pb1 I1 88.99(5) 8_755 . ? I2 Pb1 I1 92.01(5) 5_777 . ? I2 Pb1 I1 87.99(5) . . ? I2 Pb1 I1 88.99(5) 4_577 5_777 ? I2 Pb1 I1 91.01(5) 8_755 5_777 ? I2 Pb1 I1 87.99(5) 5_777 5_777 ? I2 Pb1 I1 92.01(5) . 5_777 ? I1 Pb1 I1 180.0000(10) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 176(3) . . . . ? C1 C2 C3 C4 96(4) . . . . ? C2 C3 C4 C5 172(3) . . . . ? C3 C4 C5 C6 -174(3) . . . . ? C4 C5 C6 C7 -175(3) . . . . ? C5 C6 C7 C8 180(3) . . . . ? C6 C7 C8 C9 179(3) . . . . ? C7 C8 C9 C10 -178(3) . . . . ? Pb1 I2 Pb1 I2 -29.11(9) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 150.89(9) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 -119.99(12) 4_477 . . . ? Pb1 I2 Pb1 I1 60.01(12) 4_477 . . 5_777 ? 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 3.59(3) 137 8_855 N1 H1B I1 0.89 2.74 3.63(2) 173 1_545 N1 H1C I2 0.89 2.9 3.68(2) 147 8_755 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE III' # Attachment 'web_deposit_cif_file_10_DrAndreasLemmerer_1307029515.cifdep 4c 805437.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_4c _database_code_depnum_ccdc_archive 'CCDC 805437' #TrackingRef 'web_deposit_cif_file_10_DrAndreasLemmerer_1307029515.cifdep 4c 805437.cif' _iucr_refine_instructions_details ; TITL 6aS66e_a in Pbca CELL 0.71073 8.8339 8.4845 43.9647 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0008 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 80 192 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 OMIT 0 0 4 EQIV $2 -x+5/2, y-1/2, z EQIV $3 x, y-1, z EQIV $4 -x+3/2, y-1/2, z HTAB N1 I1_$2 HTAB N1 I1_$3 HTAB N1 I2_$4 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 ACTA BOND BOND $H CONF L.S. 4 TEMP -5.00 WGHT 0.000000 282.181213 FVAR 0.05425 C1 1 1.017498 0.530952 0.910922 11.00000 0.17205 0.12264 = 0.08820 0.02422 -0.04278 0.01115 AFIX 23 H1D 2 1.105928 0.516528 0.898142 11.00000 -1.20000 H1E 2 1.006524 0.642614 0.915112 11.00000 -1.20000 AFIX 0 C2 1 0.878089 0.470421 0.894702 11.00000 0.17461 0.13839 = 0.07836 0.01869 -0.03408 -0.00042 AFIX 23 H2A 2 0.792358 0.475592 0.908451 11.00000 -1.20000 H2B 2 0.893550 0.360752 0.889298 11.00000 -1.20000 AFIX 0 C3 1 0.841600 0.563683 0.866093 11.00000 0.15636 0.12827 = 0.07117 0.01150 -0.03007 -0.00293 AFIX 23 H3A 2 0.732553 0.572367 0.864124 11.00000 -1.20000 H3B 2 0.882091 0.669388 0.868203 11.00000 -1.20000 AFIX 0 C4 1 0.905121 0.490032 0.837317 11.00000 0.13267 0.12247 = 0.07796 0.01269 -0.02672 -0.00394 AFIX 23 H4A 2 0.877610 0.379384 0.836809 11.00000 -1.20000 H4B 2 1.014717 0.496462 0.837868 11.00000 -1.20000 AFIX 0 C5 1 0.848487 0.568936 0.808476 11.00000 0.11270 0.11595 = 0.07123 0.01059 -0.01745 -0.00826 AFIX 23 H5A 2 0.887257 0.675835 0.807768 11.00000 -1.20000 H5B 2 0.738907 0.575009 0.809256 11.00000 -1.20000 AFIX 0 C6 1 0.894646 0.483832 0.779512 11.00000 0.10284 0.11534 = 0.07587 0.01105 -0.00838 -0.01347 AFIX 23 H6A 2 1.003449 0.468439 0.779633 11.00000 -1.20000 H6B 2 0.847359 0.380664 0.779195 11.00000 -1.20000 AFIX 0 C7 1 0.850587 0.572606 0.750853 11.00000 0.09849 0.11744 = 0.07100 0.00997 -0.00501 -0.01800 AFIX 23 H7A 2 0.741828 0.588342 0.750848 11.00000 -1.20000 H7B 2 0.898008 0.675702 0.751232 11.00000 -1.20000 AFIX 0 C8 1 0.895412 0.489181 0.721661 11.00000 0.10247 0.12525 = 0.07514 0.00457 -0.00077 -0.02284 AFIX 23 H8A 2 0.849745 0.385218 0.721443 11.00000 -1.20000 H8B 2 1.004428 0.475564 0.721417 11.00000 -1.20000 AFIX 0 C9 1 0.847899 0.577143 0.693138 11.00000 0.10984 0.13424 = 0.07041 0.00365 -0.00064 -0.02176 AFIX 23 H9A 2 0.739177 0.592936 0.693643 11.00000 -1.20000 H9B 2 0.895408 0.680214 0.693160 11.00000 -1.20000 AFIX 0 C10 1 0.889214 0.492622 0.663850 11.00000 0.13594 0.17204 = 0.07466 -0.00643 0.00737 -0.01485 AFIX 33 H10A 2 0.858336 0.555341 0.646768 11.00000 -1.50000 H10B 2 0.838700 0.392507 0.663151 11.00000 -1.50000 H10C 2 0.996726 0.476581 0.663114 11.00000 -1.50000 AFIX 0 N1 3 1.036543 0.444782 0.939271 11.00000 0.11865 0.06254 = 0.07951 0.00531 -0.01566 0.01248 AFIX 33 H1A 2 1.123096 0.473393 0.948038 11.00000 -1.50000 H1B 2 1.038472 0.341803 0.935437 11.00000 -1.50000 H1C 2 0.959713 0.466432 0.951681 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.067039 1.020117 0.928688 11.00000 0.08475 0.07181 = 0.04930 -0.00180 0.00596 0.00246 I2 4 0.698999 1.195577 0.988018 11.00000 0.05179 0.04221 = 0.08414 0.00437 0.00555 0.02188 PB1 5 1.000000 1.000000 1.000000 10.50000 0.04086 0.03347 = 0.04911 0.00033 0.00299 -0.00159 HKLF 4 REM 6aS66e_a in Pbca REM R1 = 0.1010 for 2594 Fo > 4sig(Fo) and 0.1133 for all 3043 data REM 124 parameters refined using 98 restraints END WGHT 0.0000 281.9069 REM Highest difference peak 3.664, deepest hole -4.513, 1-sigma level 0.328 Q1 1 0.8006 1.3043 1.0125 11.00000 0.05 3.66 Q2 1 0.9998 0.3894 0.9765 11.00000 0.05 2.20 Q3 1 0.6345 1.2257 1.0171 11.00000 0.05 2.15 Q4 1 0.7629 1.1611 1.0191 11.00000 0.05 1.96 Q5 1 0.9204 1.0450 0.9317 11.00000 0.05 1.90 Q6 1 0.8842 1.2973 0.9873 11.00000 0.05 1.86 Q7 1 0.7385 1.3366 0.9830 11.00000 0.05 1.81 Q8 1 0.8071 1.0959 0.9896 11.00000 0.05 1.71 Q9 1 1.1263 0.3269 0.9436 11.00000 0.05 1.71 Q10 1 0.7030 1.2012 0.9681 11.00000 0.05 1.58 Q11 1 0.8425 1.2464 0.9820 11.00000 0.05 1.56 Q12 1 1.1105 0.8068 0.9873 11.00000 0.05 1.55 Q13 1 0.7728 0.2254 0.9164 11.00000 0.05 1.50 Q14 1 0.9999 0.9345 0.9264 11.00000 0.05 1.48 Q15 1 0.8757 0.3294 0.9418 11.00000 0.05 1.46 Q16 1 0.8025 0.8981 1.0184 11.00000 0.05 1.46 Q17 1 0.6032 1.2922 0.9880 11.00000 0.05 1.44 Q18 1 0.8664 0.7348 0.9183 11.00000 0.05 1.35 Q19 1 1.2655 0.3390 0.9420 11.00000 0.05 1.30 Q20 1 1.1135 0.8827 0.9756 11.00000 0.05 1.25 ; _audit_creation_date 2008-06-23T12:24:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(decylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.8339(2) _cell_length_b 8.4845(2) _cell_length_c 43.9647(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3295.21(12) _cell_formula_units_Z 4 _cell_measurement_temperature 268(2) _cell_measurement_reflns_used 9961 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 28.18 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.04 0 0 1 0.04 0 -1 0 0.12 0 1 0 0.12 -1 0 0 0.14 1 0 0 0.14 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.876 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1586 _exptl_absorpt_correction_T_max 0.4947 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 268(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 'omega scans' _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_unetI/netI 0.0225 _diffrn_reflns_number 25905 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 3043 _reflns_number_gt 2594 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The cause of the high refinement statistics is that this crystal has undergone three phase transitions at this stage, from II to III to IV and back to III, and these have substantial movement of the organic chain and inroganic layers, causing fracturing of the crystal. In fact, only one third of the crystal was left over at this stage , as the upper two thirds had already broken off in going from IV to III. Furthermore we were able to continue monitoring all the transitions on this one crystal. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.520 \%A and 109-114\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+282.1812P] 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 3043 _refine_ls_number_parameters 124 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.1133 _refine_ls_R_factor_gt 0.101 _refine_ls_wR_factor_ref 0.2423 _refine_ls_wR_factor_gt 0.2367 _refine_ls_goodness_of_fit_ref 1.421 _refine_ls_restrained_S_all 1.402 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.664 _refine_diff_density_min -4.513 _refine_diff_density_rms 0.328 #----------------------------------------------------------------------------# # 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 1.017(5) 0.531(5) 0.9109(8) 0.128(10) Uani 1 1 d DU . . H1D H 1.1059 0.5165 0.8981 0.153 Uiso 1 1 calc R . . H1E H 1.0065 0.6426 0.9151 0.153 Uiso 1 1 calc R . . C2 C 0.878(4) 0.470(5) 0.8947(5) 0.130(9) Uani 1 1 d DU . . H2A H 0.7924 0.4756 0.9085 0.157 Uiso 1 1 calc R . . H2B H 0.8936 0.3608 0.8893 0.157 Uiso 1 1 calc R . . C3 C 0.842(4) 0.564(4) 0.8661(4) 0.119(9) Uani 1 1 d DU . . H3A H 0.7326 0.5724 0.8641 0.142 Uiso 1 1 calc R . . H3B H 0.8821 0.6694 0.8682 0.142 Uiso 1 1 calc R . . C4 C 0.905(5) 0.490(5) 0.8373(4) 0.111(8) Uani 1 1 d DU . . H4A H 0.8776 0.3794 0.8368 0.133 Uiso 1 1 calc R . . H4B H 1.0147 0.4965 0.8379 0.133 Uiso 1 1 calc R . . C5 C 0.848(5) 0.569(4) 0.8085(4) 0.100(8) Uani 1 1 d DU . . H5A H 0.8873 0.6758 0.8078 0.12 Uiso 1 1 calc R . . H5B H 0.7389 0.575 0.8093 0.12 Uiso 1 1 calc R . . C6 C 0.895(5) 0.484(4) 0.7795(4) 0.098(8) Uani 1 1 d DU . . H6A H 1.0034 0.4684 0.7796 0.118 Uiso 1 1 calc R . . H6B H 0.8474 0.3807 0.7792 0.118 Uiso 1 1 calc R . . C7 C 0.851(5) 0.573(4) 0.7509(4) 0.096(7) Uani 1 1 d DU . . H7A H 0.7418 0.5883 0.7508 0.115 Uiso 1 1 calc R . . H7B H 0.898 0.6757 0.7512 0.115 Uiso 1 1 calc R . . C8 C 0.895(5) 0.489(4) 0.7217(4) 0.101(8) Uani 1 1 d DU . . H8A H 0.8497 0.3852 0.7214 0.121 Uiso 1 1 calc R . . H8B H 1.0044 0.4756 0.7214 0.121 Uiso 1 1 calc R . . C9 C 0.848(5) 0.577(4) 0.6931(5) 0.105(9) Uani 1 1 d DU . . H9A H 0.7392 0.5929 0.6936 0.126 Uiso 1 1 calc R . . H9B H 0.8954 0.6802 0.6932 0.126 Uiso 1 1 calc R . . C10 C 0.889(6) 0.493(6) 0.6639(5) 0.128(14) Uani 1 1 d DU . . H10A H 0.8583 0.5553 0.6468 0.191 Uiso 1 1 calc R . . H10B H 0.8387 0.3925 0.6632 0.191 Uiso 1 1 calc R . . H10C H 0.9967 0.4766 0.6631 0.191 Uiso 1 1 calc R . . N1 N 1.037(4) 0.445(3) 0.9393(6) 0.087(9) Uani 1 1 d DU . . H1A H 1.1231 0.4734 0.948 0.13 Uiso 1 1 calc R . . H1B H 1.0385 0.3418 0.9354 0.13 Uiso 1 1 calc R . . H1C H 0.9597 0.4664 0.9517 0.13 Uiso 1 1 calc R . . I1 I 1.0670(3) 1.0201(3) 0.92869(5) 0.0686(7) Uani 1 1 d . . . I2 I 0.6990(2) 1.1956(2) 0.98802(5) 0.0594(6) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0411(4) 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 0.17(2) 0.12(2) 0.088(15) 0.024(15) -0.043(15) 0.01(2) C2 0.17(2) 0.14(2) 0.078(10) 0.019(14) -0.034(14) 0.00(2) C3 0.16(2) 0.128(19) 0.071(9) 0.012(14) -0.030(13) -0.003(19) C4 0.133(19) 0.122(19) 0.078(8) 0.013(13) -0.027(14) -0.004(18) C5 0.113(18) 0.116(18) 0.071(8) 0.011(13) -0.017(14) -0.008(17) C6 0.103(17) 0.115(18) 0.076(8) 0.011(12) -0.008(14) -0.013(16) C7 0.098(17) 0.117(18) 0.071(8) 0.010(12) -0.005(14) -0.018(16) C8 0.102(18) 0.125(19) 0.075(8) 0.005(13) -0.001(14) -0.023(17) C9 0.11(2) 0.13(2) 0.070(9) 0.004(15) -0.001(16) -0.02(2) C10 0.14(3) 0.17(3) 0.075(9) -0.01(2) 0.01(2) -0.01(3) N1 0.12(2) 0.063(17) 0.080(16) 0.005(14) -0.016(15) 0.012(17) I1 0.0847(15) 0.0718(14) 0.0493(11) -0.0018(11) 0.0060(10) 0.0025(13) I2 0.0518(10) 0.0422(10) 0.0841(14) 0.0044(10) 0.0056(10) 0.0219(9) Pb1 0.0409(7) 0.0335(7) 0.0491(8) 0.0003(7) 0.0030(6) -0.0016(6) #----------------------------------------------------------------------------# # 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 1.455(18) . ? C1 C2 1.513(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.521(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.519(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.519(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.520(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.519(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.518(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.518(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.518(10) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.195(2) . ? I2 Pb1 3.1685(17) 4_477 ? I2 Pb1 3.1783(18) . ? Pb1 I2 3.1685(18) 8_755 ? Pb1 I2 3.1685(18) 4_577 ? Pb1 I2 3.1783(18) 5_777 ? Pb1 I1 3.195(2) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109(2) . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 109.9 . . ? N1 C1 H1E 109.9 . . ? C2 C1 H1E 109.9 . . ? H1D C1 H1E 108.3 . . ? C1 C2 C3 112.7(15) . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 113.4(15) . . ? 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 . . ? C3 C4 C5 113.1(13) . . ? C3 C4 H4A 109 . . ? C5 C4 H4A 109 . . ? C3 C4 H4B 109 . . ? C5 C4 H4B 109 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C6 113.7(13) . . ? C4 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? C4 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C7 C6 C5 113.0(13) . . ? C7 C6 H6A 109 . . ? C5 C6 H6A 109 . . ? C7 C6 H6B 109 . . ? C5 C6 H6B 109 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 113.8(13) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 113.4(14) . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 113.7(14) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 149.57(8) 4_477 . ? I2 Pb1 I2 180 8_755 4_577 ? I2 Pb1 I2 93.792(18) 8_755 5_777 ? I2 Pb1 I2 86.208(18) 4_577 5_777 ? I2 Pb1 I2 86.208(18) 8_755 . ? I2 Pb1 I2 93.792(18) 4_577 . ? I2 Pb1 I2 180.0000(10) 5_777 . ? I2 Pb1 I1 90.96(6) 8_755 5_777 ? I2 Pb1 I1 89.04(6) 4_577 5_777 ? I2 Pb1 I1 87.97(6) 5_777 5_777 ? I2 Pb1 I1 92.03(6) . 5_777 ? I2 Pb1 I1 89.04(6) 8_755 . ? I2 Pb1 I1 90.96(6) 4_577 . ? I2 Pb1 I1 92.03(6) 5_777 . ? I2 Pb1 I1 87.97(6) . . ? I1 Pb1 I1 180.0000(10) 5_777 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 175(3) . . . . ? C1 C2 C3 C4 95(4) . . . . ? C2 C3 C4 C5 171(3) . . . . ? C3 C4 C5 C6 -173(4) . . . . ? C4 C5 C6 C7 -174(4) . . . . ? C5 C6 C7 C8 -180(4) . . . . ? C6 C7 C8 C9 179(4) . . . . ? C7 C8 C9 C10 -179(4) . . . . ? Pb1 I2 Pb1 I2 150.84(12) 4_477 . . 8_755 ? Pb1 I2 Pb1 I2 -29.16(12) 4_477 . . 4_577 ? Pb1 I2 Pb1 I1 60.01(15) 4_477 . . 5_777 ? Pb1 I2 Pb1 I1 -119.99(15) 4_477 . . . ? 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 3.59(3) 136 8_855 N1 H1B I1 0.89 2.76 3.64(3) 174 1_545 N1 H1C I2 0.89 2.88 3.67(3) 148 8_755 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE II' data_4d _database_code_depnum_ccdc_archive 'CCDC 805438' #TrackingRef 'web_deposit_cif_file_0_DrAndreasLemmerer_1307029628.cifdep 4d 805438.cif' _iucr_refine_instructions_details ; TITL 5aS9910C6cm_a in Pbca CELL 0.71073 8.9708 8.6733 42.5696 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0012 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 80 192 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 ACTA PLAN 2 BOND BOND $H CONF L.S. 10 TEMP 20.00 WGHT 0.018100 178.421021 FVAR 0.07399 C1 1 0.963822 0.475557 0.926541 11.00000 0.15095 0.14912 = 0.19982 -0.03043 -0.01398 -0.02123 AFIX 23 H1D 2 0.865615 0.518913 0.930129 11.00000 -1.20000 H1E 2 0.967985 0.374029 0.936056 11.00000 -1.20000 AFIX 0 C2 1 0.996463 0.465995 0.891804 11.00000 0.17260 0.15907 = 0.19670 -0.03054 -0.02023 -0.00745 AFIX 23 H2A 2 1.089837 0.411463 0.888874 11.00000 -1.20000 H2B 2 1.009469 0.569674 0.883712 11.00000 -1.20000 AFIX 0 C3 1 0.876089 0.385538 0.872663 11.00000 0.16823 0.16955 = 0.19996 -0.02195 -0.03748 0.00578 AFIX 23 H3A 2 0.900147 0.276985 0.870579 11.00000 -1.20000 H3B 2 0.781106 0.393944 0.883416 11.00000 -1.20000 AFIX 0 C4 1 0.864396 0.458473 0.840261 11.00000 0.18427 0.18707 = 0.20054 -0.01517 -0.02757 0.00579 AFIX 23 H4A 2 0.774618 0.520697 0.839516 11.00000 -1.20000 H4B 2 0.948646 0.527075 0.837323 11.00000 -1.20000 AFIX 0 C5 1 0.860615 0.344889 0.813227 11.00000 0.18074 0.19455 = 0.19737 -0.01704 -0.01388 0.01269 AFIX 23 H5A 2 0.762341 0.298662 0.811955 11.00000 -1.20000 H5B 2 0.932154 0.263195 0.817087 11.00000 -1.20000 AFIX 0 C6 1 0.896998 0.423200 0.782227 11.00000 0.18481 0.21045 = 0.20248 -0.00943 -0.00933 0.01674 AFIX 23 H6A 2 0.850161 0.523991 0.781943 11.00000 -1.20000 H6B 2 1.003927 0.438712 0.781014 11.00000 -1.20000 AFIX 0 C7 1 0.847032 0.334355 0.753509 11.00000 0.18304 0.22168 = 0.19858 -0.01326 -0.00839 0.02586 AFIX 23 H7A 2 0.739329 0.324571 0.753834 11.00000 -1.20000 H7B 2 0.889140 0.231405 0.754223 11.00000 -1.20000 AFIX 0 C8 1 0.894168 0.412379 0.723117 11.00000 0.18658 0.22449 = 0.20141 -0.00715 -0.00672 0.03724 AFIX 23 H8A 2 0.851951 0.515293 0.722482 11.00000 -1.20000 H8B 2 1.001846 0.422533 0.722921 11.00000 -1.20000 AFIX 0 C9 1 0.845534 0.324989 0.694008 11.00000 0.19168 0.23365 = 0.19947 -0.01150 -0.00658 0.04432 AFIX 23 H9A 2 0.738090 0.312593 0.694419 11.00000 -1.20000 H9B 2 0.889855 0.222990 0.694326 11.00000 -1.20000 AFIX 0 N1 3 1.078580 0.575229 0.939661 11.00000 0.06962 0.10352 = 0.15625 0.01613 -0.00575 0.02104 AFIX 33 H1A 2 1.074098 0.572149 0.960537 11.00000 -1.50000 H1B 2 1.063963 0.671532 0.933132 11.00000 -1.50000 H1C 2 1.167840 0.542944 0.933335 11.00000 -1.50000 AFIX 0 C10 1 0.889805 0.405965 0.663788 11.00000 0.37231 0.15386 = 0.12515 -0.00747 -0.07577 0.08453 AFIX 33 H10A 2 0.840539 0.357740 0.646345 11.00000 -1.50000 H10B 2 0.995792 0.398898 0.661023 11.00000 -1.50000 H10C 2 0.861072 0.512448 0.664889 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.033980 0.983349 0.925237 11.00000 0.08034 0.06459 = 0.06662 0.00448 -0.00649 0.01344 I2 4 0.698513 1.195578 0.996694 11.00000 0.04682 0.04567 = 0.10052 -0.00567 -0.01164 0.01862 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03385 0.03418 = 0.06474 0.00280 0.00002 -0.00011 HKLF 4 REM 5aS9910C6cm_a in Pbca REM R1 = 0.0919 for 2147 Fo > 4sig(Fo) and 0.1230 for all 3085 data REM 124 parameters refined using 90 restraints END WGHT 0.0181 178.4061 REM Highest difference peak 1.745, deepest hole -1.964, 1-sigma level 0.234 Q1 1 1.0546 1.0863 0.9278 11.00000 0.05 1.74 Q2 1 1.1989 0.2705 0.9307 11.00000 0.05 1.71 ; _audit_creation_date 2008-06-20T14:41:35-00:00 _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(decylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9708(2) _cell_length_b 8.6733(2) _cell_length_c 42.5696(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3312.19(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3217 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 27.3 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.01 0 0 -1 0.01 2 0 1 0.09 -2 0 -1 0.09 0 1 0 0.18 -3 -4 5 0.16 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.83 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1109 _exptl_absorpt_correction_T_max 0.8378 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 'omega scans' _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_number 14642 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 3085 _reflns_number_gt 2147 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.520 \%A and 106-115\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+(0.0181P)^2^+178.4210P] 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 3085 _refine_ls_number_parameters 124 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.123 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2085 _refine_ls_wR_factor_gt 0.1991 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.299 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.745 _refine_diff_density_min -1.964 _refine_diff_density_rms 0.234 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.964(4) 0.476(5) 0.9265(7) 0.167(11) Uani 1 1 d DU . . H1D H 0.8656 0.5189 0.9301 0.2 Uiso 1 1 calc R . . H1E H 0.968 0.374 0.9361 0.2 Uiso 1 1 calc R . . C2 C 0.996(4) 0.466(6) 0.8918(7) 0.176(11) Uani 1 1 d DU . . H2A H 1.0898 0.4115 0.8889 0.211 Uiso 1 1 calc R . . H2B H 1.0095 0.5697 0.8837 0.211 Uiso 1 1 calc R . . C3 C 0.876(5) 0.386(5) 0.8727(6) 0.179(10) Uani 1 1 d DU . . H3A H 0.9001 0.277 0.8706 0.215 Uiso 1 1 calc R . . H3B H 0.7811 0.3939 0.8834 0.215 Uiso 1 1 calc R . . C4 C 0.864(5) 0.458(4) 0.8403(6) 0.191(11) Uani 1 1 d DU . . H4A H 0.7746 0.5207 0.8395 0.229 Uiso 1 1 calc R . . H4B H 0.9486 0.5271 0.8373 0.229 Uiso 1 1 calc R . . C5 C 0.861(6) 0.345(4) 0.8132(6) 0.191(11) Uani 1 1 d DU . . H5A H 0.7623 0.2987 0.812 0.229 Uiso 1 1 calc R . . H5B H 0.9322 0.2632 0.8171 0.229 Uiso 1 1 calc R . . C6 C 0.897(6) 0.423(5) 0.7822(6) 0.199(11) Uani 1 1 d DU . . H6A H 0.8502 0.524 0.7819 0.239 Uiso 1 1 calc R . . H6B H 1.0039 0.4387 0.781 0.239 Uiso 1 1 calc R . . C7 C 0.847(6) 0.334(5) 0.7535(6) 0.201(12) Uani 1 1 d DU . . H7A H 0.7393 0.3246 0.7538 0.241 Uiso 1 1 calc R . . H7B H 0.8891 0.2314 0.7542 0.241 Uiso 1 1 calc R . . C8 C 0.894(6) 0.412(5) 0.7231(6) 0.204(13) Uani 1 1 d DU . . H8A H 0.852 0.5153 0.7225 0.245 Uiso 1 1 calc R . . H8B H 1.0018 0.4225 0.7229 0.245 Uiso 1 1 calc R . . C9 C 0.846(6) 0.325(5) 0.6940(7) 0.208(14) Uani 1 1 d DU . . H9A H 0.7381 0.3126 0.6944 0.25 Uiso 1 1 calc R . . H9B H 0.8899 0.223 0.6943 0.25 Uiso 1 1 calc R . . N1 N 1.079(3) 0.575(3) 0.9397(7) 0.110(8) Uani 1 1 d DU . . H1A H 1.0741 0.5721 0.9605 0.165 Uiso 1 1 calc R . . H1B H 1.064 0.6715 0.9331 0.165 Uiso 1 1 calc R . . H1C H 1.1678 0.5429 0.9333 0.165 Uiso 1 1 calc R . . C10 C 0.890(7) 0.406(5) 0.6638(7) 0.22(3) Uani 1 1 d D . . H10A H 0.8405 0.3577 0.6463 0.326 Uiso 1 1 calc R . . H10B H 0.9958 0.3989 0.661 0.326 Uiso 1 1 calc R . . H10C H 0.8611 0.5124 0.6649 0.326 Uiso 1 1 calc R . . I1 I 1.0340(2) 0.9833(2) 0.92524(4) 0.0705(6) Uani 1 1 d . . . I2 I 0.69851(17) 1.19558(18) 0.99669(5) 0.0643(5) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0443(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 0.15(2) 0.15(2) 0.20(2) -0.03(2) -0.01(2) -0.021(18) C2 0.17(2) 0.16(2) 0.20(2) -0.03(2) -0.02(2) -0.007(19) C3 0.17(2) 0.17(2) 0.20(2) -0.022(19) -0.04(2) 0.01(2) C4 0.18(2) 0.19(2) 0.20(2) -0.015(18) -0.03(2) 0.01(2) C5 0.18(2) 0.19(2) 0.20(2) -0.017(19) -0.01(2) 0.01(2) C6 0.18(2) 0.21(3) 0.20(2) -0.01(2) -0.01(2) 0.02(2) C7 0.18(2) 0.22(3) 0.20(2) -0.01(2) -0.01(3) 0.03(2) C8 0.19(3) 0.22(3) 0.20(2) -0.01(2) -0.01(3) 0.04(3) C9 0.19(3) 0.23(3) 0.20(2) -0.01(3) -0.01(3) 0.04(3) N1 0.070(16) 0.10(2) 0.16(2) 0.016(17) -0.006(16) 0.021(14) C10 0.37(10) 0.15(5) 0.13(4) -0.01(4) -0.08(5) 0.08(6) I1 0.0803(12) 0.0646(11) 0.0666(12) 0.0045(10) -0.0065(9) 0.0134(10) I2 0.0468(8) 0.0457(8) 0.1005(14) -0.0057(10) -0.0116(9) 0.0186(7) Pb1 0.0339(6) 0.0342(6) 0.0647(8) 0.0028(7) 0.0000(6) -0.0001(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.456(18) . ? C1 C2 1.510(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.522(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.521(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.515(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.520(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.513(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.520(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.517(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.519(10) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? I1 Pb1 3.2004(19) . ? I2 Pb1 3.1879(14) 4_477 ? I2 Pb1 3.1956(14) . ? Pb1 I2 3.1879(15) 4_577 ? Pb1 I2 3.1879(15) 8_755 ? Pb1 I2 3.1956(14) 5_777 ? Pb1 I1 3.2004(19) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 106(2) . . ? N1 C1 H1D 110.6 . . ? C2 C1 H1D 110.6 . . ? N1 C1 H1E 110.6 . . ? C2 C1 H1E 110.6 . . ? H1D C1 H1E 108.7 . . ? C1 C2 C3 114.3(15) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 110.1(15) . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 114.8(15) . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? C4 C5 C6 111.4(14) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108 . . ? C7 C6 C5 114.2(14) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 C8 112.2(14) . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 113.1(15) . . ? C9 C8 H8A 109 . . ? C7 C8 H8A 109 . . ? C9 C8 H8B 109 . . ? C7 C8 H8B 109 . . ? H8A C8 H8B 107.8 . . ? C8 C9 C10 112.7(15) . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 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 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Pb1 I2 Pb1 155.57(6) 4_477 . ? I2 Pb1 I2 180 4_577 8_755 ? I2 Pb1 I2 87.990(11) 4_577 5_777 ? I2 Pb1 I2 92.010(11) 8_755 5_777 ? I2 Pb1 I2 92.010(11) 4_577 . ? I2 Pb1 I2 87.990(11) 8_755 . ? I2 Pb1 I2 180.0000(10) 5_777 . ? I2 Pb1 I1 91.61(5) 4_577 . ? I2 Pb1 I1 88.39(5) 8_755 . ? I2 Pb1 I1 86.52(5) 5_777 . ? I2 Pb1 I1 93.48(5) . . ? I2 Pb1 I1 88.39(5) 4_577 5_777 ? I2 Pb1 I1 91.61(5) 8_755 5_777 ? I2 Pb1 I1 93.48(5) 5_777 5_777 ? I2 Pb1 I1 86.52(5) . 5_777 ? I1 Pb1 I1 180.0000(10) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -172(4) . . . . ? C1 C2 C3 C4 146(4) . . . . ? C2 C3 C4 C5 133(4) . . . . ? C3 C4 C5 C6 -162(4) . . . . ? C4 C5 C6 C7 -161(5) . . . . ? C5 C6 C7 C8 -177(5) . . . . ? C6 C7 C8 C9 180(5) . . . . ? C7 C8 C9 C10 179(5) . . . . ? Pb1 I2 Pb1 I2 -9.32(14) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 170.68(14) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 -101.06(18) 4_477 . . . ? Pb1 I2 Pb1 I1 78.94(18) 4_477 . . 5_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.08 3.63(3) 122 8_755 N1 H1B I1 0.89 2.74 3.61(3) 168 . N1 H1C I1 0.89 2.75 3.62(3) 167 8_855 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE II' # Attachment 'web_deposit_cif_file_1_DrAndreasLemmerer_1307029628.cifdep 4e 805439.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_4e _database_code_depnum_ccdc_archive 'CCDC 805439' #TrackingRef 'web_deposit_cif_file_1_DrAndreasLemmerer_1307029628.cifdep 4e 805439.cif' _iucr_refine_instructions_details ; TITL 6aS99f_a in Pbca CELL 0.71073 8.9807 8.6742 42.5253 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0014 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N I PB UNIT 80 192 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 DFIX 1.52 0.01 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.54 0.02 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 DFIX 1.45 N1 C1 DANG 2.45 N1 C2 EQIV $2 -x+3/2, y-1/2, z EQIV $3 -x+5/2, y-1/2, z HTAB N1 I2_$2 HTAB N1 I1 HTAB N1 I1_$3 ACTA BOND BOND $H CONF L.S. 10 TEMP 20.00 WGHT 0.000000 581.298828 FVAR 0.05481 C1 1 0.953818 0.502211 0.924821 11.00000 0.11671 0.18579 = 0.20984 0.01244 -0.00658 -0.01229 AFIX 23 H1D 2 0.873309 0.575853 0.922459 11.00000 -1.20000 H1E 2 0.918989 0.417995 0.937901 11.00000 -1.20000 AFIX 0 C2 1 1.000535 0.441491 0.892831 11.00000 0.13515 0.18919 = 0.21102 0.00959 -0.00637 -0.00715 AFIX 23 H2A 2 1.071062 0.358059 0.895803 11.00000 -1.20000 H2B 2 1.051093 0.523109 0.881468 11.00000 -1.20000 AFIX 0 C3 1 0.871512 0.383342 0.872992 11.00000 0.14178 0.19297 = 0.21123 0.00826 -0.01356 -0.00198 AFIX 23 H3A 2 0.778887 0.403221 0.884002 11.00000 -1.20000 H3B 2 0.880864 0.272697 0.870341 11.00000 -1.20000 AFIX 0 C4 1 0.865428 0.459258 0.840786 11.00000 0.15590 0.19861 = 0.21159 0.00995 -0.01193 0.00187 AFIX 23 H4A 2 0.777946 0.524648 0.839752 11.00000 -1.20000 H4B 2 0.952242 0.524648 0.838284 11.00000 -1.20000 AFIX 0 C5 1 0.860323 0.344880 0.813755 11.00000 0.16250 0.20234 = 0.21110 0.00831 -0.00869 0.00647 AFIX 23 H5A 2 0.759201 0.307344 0.811385 11.00000 -1.20000 H5B 2 0.923240 0.257408 0.818794 11.00000 -1.20000 AFIX 0 C6 1 0.911429 0.414426 0.782795 11.00000 0.16884 0.20627 = 0.21142 0.01172 -0.00956 0.00933 AFIX 23 H6A 2 0.886800 0.523304 0.782664 11.00000 -1.20000 H6B 2 1.018889 0.405542 0.781382 11.00000 -1.20000 AFIX 0 C7 1 0.842302 0.338820 0.754094 11.00000 0.17337 0.20940 = 0.21203 0.01054 -0.01342 0.01429 AFIX 23 H7A 2 0.734932 0.349691 0.755198 11.00000 -1.20000 H7B 2 0.865235 0.229553 0.754369 11.00000 -1.20000 AFIX 0 C8 1 0.897145 0.407686 0.723336 11.00000 0.17851 0.20942 = 0.21142 0.01278 -0.01348 0.02055 AFIX 23 H8A 2 0.861649 0.513009 0.721737 11.00000 -1.20000 H8B 2 1.005110 0.410629 0.723608 11.00000 -1.20000 AFIX 0 C9 1 0.846225 0.318548 0.694532 11.00000 0.18352 0.20949 = 0.21219 0.01095 -0.01527 0.02540 AFIX 23 H9A 2 0.739425 0.302991 0.695764 11.00000 -1.20000 H9B 2 0.893250 0.217878 0.694594 11.00000 -1.20000 AFIX 0 C10 1 0.882875 0.399693 0.663814 11.00000 0.19389 0.19692 = 0.21237 0.01817 -0.02837 0.03990 AFIX 33 H10A 2 0.832267 0.349153 0.646811 11.00000 -1.50000 H10B 2 0.988378 0.395957 0.660262 11.00000 -1.50000 H10C 2 0.851130 0.505222 0.664968 11.00000 -1.50000 AFIX 0 N1 3 1.081618 0.576220 0.939438 11.00000 0.08052 0.15974 = 0.19221 0.02988 -0.00651 0.02101 AFIX 33 H1A 2 1.073280 0.570315 0.960258 11.00000 -1.50000 H1B 2 1.085093 0.674756 0.933650 11.00000 -1.50000 H1C 2 1.164676 0.528873 0.933350 11.00000 -1.50000 AFIX 0 MOLE 1 I1 4 1.033430 0.981552 0.925189 11.00000 0.08388 0.06049 = 0.07173 0.00642 -0.00474 0.02615 I2 4 0.699637 1.196711 0.996306 11.00000 0.04958 0.04773 = 0.10663 -0.00334 -0.01424 0.01991 PB1 5 1.000000 1.000000 1.000000 10.50000 0.03924 0.03421 = 0.06890 0.00603 0.00040 0.00032 HKLF 4 REM 6aS99f_a in Pbca REM R1 = 0.1516 for 2476 Fo > 4sig(Fo) and 0.1738 for all 3088 data REM 124 parameters refined using 98 restraints END WGHT 0.0000 581.3649 REM Highest difference peak 4.115, deepest hole -4.751, 1-sigma level 0.444 Q1 1 1.0622 1.0781 0.9283 11.00000 0.05 4.11 Q2 1 0.9143 1.0594 0.9279 11.00000 0.05 3.92 Q3 1 1.1976 0.2710 0.9297 11.00000 0.05 3.83 Q4 1 1.2027 0.6575 0.9204 11.00000 0.05 3.68 Q5 1 0.7907 0.6594 0.9198 11.00000 0.05 3.67 Q6 1 0.8047 0.2671 0.9294 11.00000 0.05 3.41 Q7 1 1.0033 0.4555 0.6517 11.00000 0.05 3.20 Q8 1 0.7925 1.3147 1.0125 11.00000 0.05 2.93 Q9 1 0.9938 0.9696 0.9241 11.00000 0.05 2.65 Q10 1 0.7157 1.3050 0.9886 11.00000 0.05 2.36 Q11 1 1.0752 0.8928 0.9245 11.00000 0.05 2.31 Q12 1 0.9843 0.4660 0.7280 11.00000 0.05 2.23 Q13 1 0.5012 1.1176 1.0121 11.00000 0.05 2.10 Q14 1 0.7783 1.2005 1.0121 11.00000 0.05 1.93 Q15 1 0.7356 0.3069 0.6383 11.00000 0.05 1.69 Q16 1 1.1495 0.9715 0.9277 11.00000 0.05 1.59 Q17 1 0.7194 0.1971 0.8315 11.00000 0.05 1.57 Q18 1 1.0869 0.8873 0.9873 11.00000 0.05 1.53 Q19 1 0.6362 1.1959 1.0125 11.00000 0.05 1.46 Q20 1 0.9676 0.3803 0.9198 11.00000 0.05 1.43 ; _audit_creation_date 2008-06-20T14:48:06-00:00 _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(decylammonium)tetraiodoplumbate(II) PHASE II ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 8.9807(2) _cell_length_b 8.6742(2) _cell_length_c 42.5253(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3312.74(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5527 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 28.35 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.04 0 0 1 0.04 0 -1 0 0.12 0 1 0 0.12 1 0 0 0.14 -1 0 0 0.14 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.829 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1636 _exptl_absorpt_correction_T_max 0.4971 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # 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 0.0573 _diffrn_reflns_av_unetI/netI 0.025 _diffrn_reflns_number 29126 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.49 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 3088 _reflns_number_gt 2476 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The cause of the high refinement statistics is that this crystal has undergone four phase transitions at this stage, from II to III to IV and back from IV to III and from III to II, and these have substantial movement of the organic chain and inroganic layers, causing fracturing of the crystal. In fact, only one third of the crystal was left over at this stage , as the upper two thirds had already broken off in going from IV to III. Furthermore we were able to continue monitoring all the transitions on this one crystal. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.520 \%A and 109-114\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+581.2988P] 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 3088 _refine_ls_number_parameters 124 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.1738 _refine_ls_R_factor_gt 0.1516 _refine_ls_wR_factor_ref 0.3501 _refine_ls_wR_factor_gt 0.3404 _refine_ls_goodness_of_fit_ref 1.44 _refine_ls_restrained_S_all 1.419 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.115 _refine_diff_density_min -4.751 _refine_diff_density_rms 0.444 #----------------------------------------------------------------------------# # 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 0.954(6) 0.502(11) 0.9248(13) 0.171(16) Uani 1 1 d DU . . H1D H 0.8733 0.5759 0.9225 0.205 Uiso 1 1 calc R . . H1E H 0.919 0.418 0.9379 0.205 Uiso 1 1 calc R . . C2 C 1.001(5) 0.441(10) 0.8928(12) 0.178(16) Uani 1 1 d DU . . H2A H 1.0711 0.3581 0.8958 0.214 Uiso 1 1 calc R . . H2B H 1.0511 0.5231 0.8815 0.214 Uiso 1 1 calc R . . C3 C 0.872(8) 0.383(8) 0.8730(10) 0.182(15) Uani 1 1 d DU . . H3A H 0.7789 0.4032 0.884 0.218 Uiso 1 1 calc R . . H3B H 0.8809 0.2727 0.8703 0.218 Uiso 1 1 calc R . . C4 C 0.865(9) 0.459(7) 0.8408(11) 0.189(15) Uani 1 1 d DU . . H4A H 0.7779 0.5246 0.8398 0.226 Uiso 1 1 calc R . . H4B H 0.9522 0.5246 0.8383 0.226 Uiso 1 1 calc R . . C5 C 0.860(11) 0.345(7) 0.8138(10) 0.192(16) Uani 1 1 d DU . . H5A H 0.7592 0.3073 0.8114 0.23 Uiso 1 1 calc R . . H5B H 0.9232 0.2574 0.8188 0.23 Uiso 1 1 calc R . . C6 C 0.911(9) 0.414(10) 0.7828(10) 0.196(16) Uani 1 1 d DU . . H6A H 0.8868 0.5233 0.7827 0.235 Uiso 1 1 calc R . . H6B H 1.0189 0.4055 0.7814 0.235 Uiso 1 1 calc R . . C7 C 0.842(9) 0.339(10) 0.7541(10) 0.198(16) Uani 1 1 d DU . . H7A H 0.7349 0.3497 0.7552 0.238 Uiso 1 1 calc R . . H7B H 0.8652 0.2296 0.7544 0.238 Uiso 1 1 calc R . . C8 C 0.897(10) 0.408(9) 0.7233(10) 0.200(17) Uani 1 1 d DU . . H8A H 0.8616 0.513 0.7217 0.24 Uiso 1 1 calc R . . H8B H 1.0051 0.4106 0.7236 0.24 Uiso 1 1 calc R . . C9 C 0.846(11) 0.319(9) 0.6945(11) 0.202(18) Uani 1 1 d DU . . H9A H 0.7394 0.303 0.6958 0.242 Uiso 1 1 calc R . . H9B H 0.8933 0.2179 0.6946 0.242 Uiso 1 1 calc R . . C10 C 0.883(11) 0.400(10) 0.6638(11) 0.20(2) Uani 1 1 d DU . . H10A H 0.8323 0.3492 0.6468 0.302 Uiso 1 1 calc R . . H10B H 0.9884 0.396 0.6603 0.302 Uiso 1 1 calc R . . H10C H 0.8511 0.5052 0.665 0.302 Uiso 1 1 calc R . . N1 N 1.082(6) 0.576(7) 0.9394(13) 0.144(17) Uani 1 1 d DU . . H1A H 1.0733 0.5703 0.9603 0.216 Uiso 1 1 calc R . . H1B H 1.0851 0.6748 0.9337 0.216 Uiso 1 1 calc R . . H1C H 1.1647 0.5289 0.9333 0.216 Uiso 1 1 calc R . . I1 I 1.0334(4) 0.9816(4) 0.92519(8) 0.0720(10) Uani 1 1 d . . . I2 I 0.6996(3) 1.1967(3) 0.99631(9) 0.0680(10) Uani 1 1 d . . . Pb1 Pb 1 1 1 0.0475(6) 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 0.12(3) 0.19(4) 0.21(3) 0.01(3) -0.01(3) -0.01(3) C2 0.14(3) 0.19(4) 0.21(3) 0.01(3) -0.01(3) -0.01(3) C3 0.14(3) 0.19(4) 0.21(3) 0.01(3) -0.01(3) 0.00(3) C4 0.16(3) 0.20(4) 0.21(3) 0.01(3) -0.01(3) 0.00(3) C5 0.16(3) 0.20(4) 0.21(3) 0.01(3) -0.01(3) 0.01(3) C6 0.17(3) 0.21(4) 0.21(3) 0.01(3) -0.01(3) 0.01(3) C7 0.17(3) 0.21(4) 0.21(3) 0.01(3) -0.01(3) 0.01(3) C8 0.18(4) 0.21(4) 0.21(3) 0.01(3) -0.01(4) 0.02(3) C9 0.18(4) 0.21(4) 0.21(3) 0.01(4) -0.02(4) 0.03(4) C10 0.19(5) 0.20(5) 0.21(3) 0.02(4) -0.03(5) 0.04(5) N1 0.08(3) 0.16(4) 0.19(4) 0.03(3) -0.01(3) 0.02(3) I1 0.084(2) 0.0605(18) 0.072(2) 0.0064(16) -0.0047(17) 0.0261(18) I2 0.0496(16) 0.0477(15) 0.107(2) -0.0033(17) -0.0142(17) 0.0199(13) Pb1 0.0392(11) 0.0342(10) 0.0689(14) 0.0060(11) 0.0004(10) 0.0003(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.45(2) . ? C1 C2 1.518(10) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.519(10) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.521(10) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.519(10) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.519(10) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.518(10) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.520(10) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.519(10) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.520(10) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? I1 Pb1 3.200(3) . ? I2 Pb1 3.187(3) 4_477 ? I2 Pb1 3.196(3) . ? Pb1 I2 3.187(3) 4_577 ? Pb1 I2 3.187(3) 8_755 ? Pb1 I2 3.196(3) 5_777 ? Pb1 I1 3.200(3) 5_777 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109(3) . . ? N1 C1 H1D 110 . . ? C2 C1 H1D 110 . . ? N1 C1 H1E 110 . . ? C2 C1 H1E 110 . . ? H1D C1 H1E 108.4 . . ? C1 C2 C3 113.7(16) . . ? C1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C2 C3 C4 112.6(16) . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 113.6(16) . . ? 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 . . ? C4 C5 C6 112.8(15) . . ? C4 C5 H5A 109 . . ? C6 C5 H5A 109 . . ? C4 C5 H5B 109 . . ? C6 C5 H5B 109 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 113.7(15) . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 112.9(15) . . ? C6 C7 H7A 109 . . ? C8 C7 H7A 109 . . ? C6 C7 H7B 109 . . ? C8 C7 H7B 109 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 113.3(15) . . ? C9 C8 H8A 108.9 . . ? C7 C8 H8A 108.9 . . ? C9 C8 H8B 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 113.1(16) . . ? C8 C9 H9A 109 . . ? C10 C9 H9A 109 . . ? C8 C9 H9B 109 . . ? C10 C9 H9B 109 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 155.93(11) 4_477 . ? I2 Pb1 I2 180.0000(10) 4_577 8_755 ? I2 Pb1 I2 87.91(2) 4_577 5_777 ? I2 Pb1 I2 92.09(2) 8_755 5_777 ? I2 Pb1 I2 92.09(2) 4_577 . ? I2 Pb1 I2 87.91(2) 8_755 . ? I2 Pb1 I2 180.000(2) 5_777 . ? I2 Pb1 I1 92.15(9) 4_577 . ? I2 Pb1 I1 87.85(9) 8_755 . ? I2 Pb1 I1 86.73(9) 5_777 . ? I2 Pb1 I1 93.27(9) . . ? I2 Pb1 I1 87.85(9) 4_577 5_777 ? I2 Pb1 I1 92.15(9) 8_755 5_777 ? I2 Pb1 I1 93.27(9) 5_777 5_777 ? I2 Pb1 I1 86.73(9) . 5_777 ? I1 Pb1 I1 180.000(2) . 5_777 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -171(7) . . . . ? C1 C2 C3 C4 126(6) . . . . ? C2 C3 C4 C5 127(6) . . . . ? C3 C4 C5 C6 -159(6) . . . . ? C4 C5 C6 C7 -152(8) . . . . ? C5 C6 C7 C8 -179(8) . . . . ? C6 C7 C8 C9 172(9) . . . . ? C7 C8 C9 C10 172(9) . . . . ? Pb1 I2 Pb1 I2 -10.6(3) 4_477 . . 4_577 ? Pb1 I2 Pb1 I2 169.4(3) 4_477 . . 8_755 ? Pb1 I2 Pb1 I1 -102.9(3) 4_477 . . . ? Pb1 I2 Pb1 I1 77.1(3) 4_477 . . 5_777 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.89 3.09 3.65(6) 123 8_755 N1 H1B I1 0.89 2.73 3.59(6) 166 . N1 H1C I1 0.89 2.76 3.60(5) 158 8_855 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE II' # Attachment 'web_deposit_cif_file_2_DrAndreasLemmerer_1307029628.cifdep 4f 805440.cif' # # CCDC ELECTRONIC DATA DEPOSITION FORM (CIF) # # This electronic data deposition form can be used: # # (a) WHEN SUBMITTING A PAPER TO A JOURNAL FOR PUBLICATION or # (b) WHEN SUBMITTING A PRIVATE COMMUNICATION TO THE CCDC # # A comprehensive archive of CIF resources is maintained by the IUCr # at its Chester office. This can be accessed # by anonymous ftp to ftp.iucr.org # or via the WWW at http://www.iucr.org/cif/home.html # If data items in this form are not available or not applicable # then ignore these items # A few items specific to CCDC input are indicated by _ccdc_ # # Submission and help information is provided at the end of this form #------------------------------------------------------------------------- #1 Global data block identification for start of deposition data_4f _database_code_depnum_ccdc_archive 'CCDC 805440' #TrackingRef 'web_deposit_cif_file_2_DrAndreasLemmerer_1307029628.cifdep 4f 805440.cif' _iucr_refine_instructions_details ; TITL 6aS99g_a in Acam CELL 0.71073 8.7152 8.7115 47.4785 90.000 90.000 90.000 ZERR 4.00 0.0018 0.0019 0.0111 0.000 0.000 0.000 LATT 5 SYMM - X, - Y, Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N I PB UNIT 80 192 8 16 4 MERG 2 OMIT -2.00 51.00 OMIT 0 0 2 DFIX 1.5 0.001 C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C6 C7 C7 C8 C8 C9 C9 C10 DANG 2.4 0.002 C1 C3 C2 C4 C3 C5 C4 C6 C5 C7 C6 C8 C7 C9 C8 C10 DFIX 1.45 0.001 C1 N1 DANG 2.4 0.002 N1 C2 SIMU 0.02 C1 > N1 DELU 0.005 C1 > N1 EQIV $8 x+1/2, -y+3/2, -z+2 EQIV $7 -x+3/2, y-1/2, z HTAB N1 I2_$8 HTAB N1 I2_$7 FMAP 2 PLAN 1 ACTA BOND $H CONF L.S. 20 TEMP 70.00 WGHT 0.154300 155.291397 FVAR 0.09076 PART -1 C1 1 0.984074 0.493589 0.906580 10.50000 0.82556 0.27929 = 0.33176 -0.00456 -0.01009 0.08423 AFIX 23 H1D 2 1.054740 0.565179 0.897829 10.50000 -1.20000 H1E 2 0.880507 0.522000 0.901213 10.50000 -1.20000 AFIX 0 C2 1 1.018129 0.333374 0.896839 10.50000 0.82861 0.27828 = 0.33266 -0.00518 -0.01140 0.08165 AFIX 23 H2A 2 0.981196 0.259054 0.910458 10.50000 -1.20000 H2B 2 1.127741 0.319164 0.894437 10.50000 -1.20000 AFIX 0 C3 1 0.936539 0.314028 0.869249 10.50000 0.83176 0.27930 = 0.33317 -0.00391 -0.01255 0.07978 AFIX 23 H3A 2 0.865951 0.398396 0.866106 10.50000 -1.20000 H3B 2 0.879090 0.218667 0.869039 10.50000 -1.20000 AFIX 0 C4 1 1.058682 0.312174 0.846992 10.50000 0.83553 0.28153 = 0.33257 -0.00468 -0.01092 0.07791 AFIX 23 H4A 2 1.059661 0.408534 0.836757 10.50000 -1.20000 H4B 2 1.158872 0.296564 0.855416 10.50000 -1.20000 AFIX 0 C5 1 1.019841 0.181829 0.827619 10.50000 0.83799 0.28219 = 0.33597 -0.00656 -0.00839 0.07602 AFIX 23 H5A 2 1.016557 0.216910 0.808239 10.50000 -1.20000 H5B 2 0.920682 0.138636 0.832445 10.50000 -1.20000 AFIX 0 C6 1 1.144011 0.064392 0.831406 10.50000 0.83816 0.28280 = 0.33969 -0.00740 -0.00575 0.07688 AFIX 23 H6A 2 1.139878 0.020897 0.850197 10.50000 -1.20000 H6B 2 1.244150 0.110594 0.828640 10.50000 -1.20000 AFIX 0 C7 1 1.115410 -0.057355 0.809690 10.50000 0.83936 0.28375 = 0.34204 -0.00911 -0.00393 0.07509 AFIX 23 H7A 2 1.151519 -0.156227 0.816350 10.50000 -1.20000 H7B 2 1.006650 -0.065179 0.805594 10.50000 -1.20000 AFIX 0 C8 1 1.202412 -0.009321 0.783894 10.50000 0.84007 0.28323 = 0.34169 -0.01004 -0.00383 0.07407 AFIX 23 H8A 2 1.243771 0.093239 0.786270 10.50000 -1.20000 H8B 2 1.286578 -0.079504 0.780305 10.50000 -1.20000 AFIX 0 C9 1 1.089680 -0.012805 0.760030 10.50000 0.84077 0.28243 = 0.34174 -0.01039 -0.00416 0.07374 AFIX 23 H9A 2 1.010034 0.063417 0.762869 10.50000 -1.20000 H9B 2 1.042034 -0.113149 0.758644 10.50000 -1.20000 AFIX 0 C10 1 1.179499 0.022097 0.733851 10.50000 0.84169 0.28112 = 0.34136 -0.01202 -0.00402 0.07213 AFIX 33 H10A 2 1.114105 0.011731 0.717692 10.50000 -1.50000 H10B 2 1.263826 -0.048301 0.732307 10.50000 -1.50000 H10C 2 1.218049 0.125197 0.734802 10.50000 -1.50000 AFIX 0 N1 3 1.000000 0.500000 0.936957 10.50000 0.81797 0.27584 = 0.32921 0.00000 0.00000 0.09161 AFIX 33 H1A 2 0.970542 0.591900 0.943107 10.50000 -1.50000 H1B 2 1.097629 0.484182 0.941627 10.50000 -1.50000 H1C 2 0.941604 0.427853 0.944784 10.50000 -1.50000 AFIX 0 PART 0 MOLE 1 PB1 5 1.000000 1.000000 1.000000 10.25000 0.02304 0.02203 = 0.19181 0.00000 0.00000 -0.00004 I1 4 1.000000 1.000000 0.933089 10.50000 0.16948 0.15646 = 0.16083 0.00000 0.00000 0.00185 I2 4 0.694018 1.194328 1.000000 10.50000 0.04244 0.04332 = 0.28907 0.00000 0.00000 0.02729 HKLF 4 REM 6aS99g_a in Cmca REM R1 = 0.1086 for 984 Fo > 4sig(Fo) and 0.1606 for all 1715 data REM 111 parameters refined using 98 restraints END WGHT 0.1500 151.1241 REM Highest difference peak 6.221, deepest hole -1.962, 1-sigma level 0.478 Q1 1 0.8075 1.3098 1.0000 10.50000 0.05 5.49 ; _audit_creation_date 2008-06-24T12:37:43-00:00 _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(decylammonium)tetraiodoplumbate(II) PHASE I ; _chemical_formula_moiety '2(C10 H24 N), I4 Pb' _chemical_formula_sum 'C20 H48 I4 N2 Pb' _chemical_formula_weight 1031.39 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Acam _symmetry_space_group_name_Hall '-A 2 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, -z+1/2' '-x+1/2, y+1, -z+1/2' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' '-x, -y+1/2, -z+1/2' 'x, y+1/2, -z+1/2' '-x-1/2, y, z+1/2' 'x-1/2, -y, z+1/2' _cell_length_a 8.7152(18) _cell_length_b 8.7115(19) _cell_length_c 47.479(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3604.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 343(2) _cell_measurement_reflns_used 2969 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.87 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.9 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.04 1 0 0 0.04 0 0 1 0.14 0 0 -1 0.14 0 1 0 0.12 0 -1 0 0.12 _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 2004). The high R(int) is because of large fracturing of the crystal caused by having undergone five phase trnasitions. The space group was assigned from systematic absences using the program XPREP. The systematic absences indicate an A centred unit cell. Related compounds in the literature have the same space group in their highest temperature phase and this gave us confirmation that we have chosen the correct space goup. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 8.114 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1509 _exptl_absorpt_correction_T_max 0.5322 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 343(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 'omega scans' _diffrn_reflns_av_R_equivalents 0.1775 _diffrn_reflns_av_unetI/netI 0.0912 _diffrn_reflns_number 11412 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.5 _diffrn_reflns_theta_full 25.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 1715 _reflns_number_gt 984 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker, 2004)' _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. The position of the decylammonium chain shows evidence of much thermal motion of the atoms as well as predominantly the entire chain. The average chain is split over two positions, related by a two fold axis around which it sits in the asymmetric unit. Out of this reason the occupancy of the chain is 0.5. We suggest this to be only a probable model for the organic chain, seeing that the literature does not contain any information using a accurate technique such as X-ray diffraction. However, the position of the N atom relative to the inorganic chain is most important, showing their relative movements. The bond lengths and angles were restrained to values similar to those in related structures in the Cambridge Structural Database, to be 1.500 \%A and 106-109\%. The atomic displacement parameters of all C and N atoms were restrained using similarity and rigid bond restraints with effective standard deviations of 0.02 and 0.005 \%A^2^ respectively. ; _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^)+(0.1543P)^2^+155.2914P] 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 1715 _refine_ls_number_parameters 111 _refine_ls_number_restraints 98 _refine_ls_R_factor_all 0.1606 _refine_ls_R_factor_gt 0.1086 _refine_ls_wR_factor_ref 0.3295 _refine_ls_wR_factor_gt 0.2622 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.011 _refine_diff_density_max 6.221 _refine_diff_density_min -1.962 _refine_diff_density_rms 0.478 #----------------------------------------------------------------------------# # 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 0.984(15) 0.494(4) 0.9066(9) 0.48(4) Uani 0.5 1 d PDU . . H1D H 1.0547 0.5652 0.8978 0.575 Uiso 0.5 1 calc PR . . H1E H 0.8805 0.522 0.9012 0.575 Uiso 0.5 1 calc PR . . C2 C 1.018(7) 0.333(6) 0.8968(10) 0.48(4) Uani 0.5 1 d PDU . . H2A H 0.9812 0.2591 0.9105 0.576 Uiso 0.5 1 calc PR . . H2B H 1.1277 0.3192 0.8944 0.576 Uiso 0.5 1 calc PR . . C3 C 0.937(4) 0.314(9) 0.8692(12) 0.48(4) Uani 0.5 1 d PDU . . H3A H 0.866 0.3984 0.8661 0.578 Uiso 0.5 1 calc PR . . H3B H 0.8791 0.2187 0.869 0.578 Uiso 0.5 1 calc PR . . C4 C 1.059(6) 0.312(4) 0.8470(10) 0.48(4) Uani 0.5 1 d PDU . . H4A H 1.0597 0.4085 0.8368 0.58 Uiso 0.5 1 calc PR . . H4B H 1.1589 0.2966 0.8554 0.58 Uiso 0.5 1 calc PR . . C5 C 1.020(5) 0.182(6) 0.8276(12) 0.49(4) Uani 0.5 1 d PDU . . H5A H 1.0166 0.2169 0.8082 0.582 Uiso 0.5 1 calc PR . . H5B H 0.9207 0.1386 0.8324 0.582 Uiso 0.5 1 calc PR . . C6 C 1.144(8) 0.064(6) 0.8314(19) 0.49(4) Uani 0.5 1 d PDU . . H6A H 1.1399 0.0209 0.8502 0.584 Uiso 0.5 1 calc PR . . H6B H 1.2442 0.1106 0.8286 0.584 Uiso 0.5 1 calc PR . . C7 C 1.115(7) -0.057(6) 0.810(2) 0.49(4) Uani 0.5 1 d PDU . . H7A H 1.1515 -0.1562 0.8163 0.586 Uiso 0.5 1 calc PR . . H7B H 1.0067 -0.0652 0.8056 0.586 Uiso 0.5 1 calc PR . . C8 C 1.202(5) -0.009(19) 0.784(2) 0.49(4) Uani 0.5 1 d PDU . . H8A H 1.2438 0.0932 0.7863 0.586 Uiso 0.5 1 calc PR . . H8B H 1.2866 -0.0795 0.7803 0.586 Uiso 0.5 1 calc PR . . C9 C 1.090(7) -0.01(3) 0.760(2) 0.49(4) Uani 0.5 1 d PDU . . H9A H 1.01 0.0634 0.7629 0.586 Uiso 0.5 1 calc PR . . H9B H 1.042 -0.1131 0.7586 0.586 Uiso 0.5 1 calc PR . . C10 C 1.179(13) 0.02(3) 0.734(2) 0.49(5) Uani 0.5 1 d PDU . . H10A H 1.1141 0.0117 0.7177 0.732 Uiso 0.5 1 calc PR . . H10B H 1.2638 -0.0483 0.7323 0.732 Uiso 0.5 1 calc PR . . H10C H 1.218 0.1252 0.7348 0.732 Uiso 0.5 1 calc PR . . N1 N 1 0.5 0.9370(9) 0.47(5) Uani 1 2 d SDU . . H1A H 0.9705 0.5919 0.9431 0.712 Uiso 0.5 1 calc PR . . H1B H 1.0976 0.4842 0.9416 0.712 Uiso 0.5 1 calc PR . . H1C H 0.9416 0.4279 0.9448 0.712 Uiso 0.5 1 calc PR . . Pb1 Pb 1 1 1 0.0790(9) Uani 1 4 d S . . I1 I 1 1 0.93309(11) 0.162(2) Uani 1 2 d S . . I2 I 0.6940(2) 1.1943(2) 1 0.1249(16) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.83(11) 0.28(6) 0.33(6) 0.00(2) -0.01(4) 0.08(8) C2 0.83(11) 0.28(6) 0.33(6) -0.01(2) -0.01(4) 0.08(8) C3 0.83(11) 0.28(6) 0.33(6) 0.00(3) -0.01(4) 0.08(8) C4 0.84(11) 0.28(6) 0.33(6) 0.00(3) -0.01(4) 0.08(8) C5 0.84(11) 0.28(6) 0.34(6) -0.01(3) -0.01(4) 0.08(8) C6 0.84(11) 0.28(6) 0.34(6) -0.01(3) -0.01(5) 0.08(8) C7 0.84(11) 0.28(6) 0.34(6) -0.01(4) 0.00(5) 0.08(8) C8 0.84(11) 0.28(7) 0.34(6) -0.01(4) 0.00(5) 0.07(8) C9 0.84(12) 0.28(7) 0.34(6) -0.01(4) 0.00(5) 0.07(8) C10 0.84(12) 0.28(8) 0.34(6) -0.01(6) 0.00(6) 0.07(9) N1 0.82(12) 0.28(7) 0.33(6) 0 0 0.09(8) Pb1 0.0230(7) 0.0220(7) 0.192(2) 0 0 0.0000(5) I1 0.169(5) 0.156(5) 0.161(4) 0 0 0.002(3) I2 0.0424(11) 0.0433(12) 0.289(4) 0 0 0.0273(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.4500(10) . ? C1 C2 1.5000(13) . ? C1 H1D 0.97 . ? C1 H1E 0.97 . ? C2 C3 1.5000(14) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 C4 1.5000(12) . ? C3 H3A 0.97 . ? C3 H3B 0.97 . ? C4 C5 1.5000(16) . ? C4 H4A 0.97 . ? C4 H4B 0.97 . ? C5 C6 1.5000(11) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 C7 1.5000(16) . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C7 C8 1.500(2) . ? C7 H7A 0.97 . ? C7 H7B 0.97 . ? C8 C9 1.500(2) . ? C8 H8A 0.97 . ? C8 H8B 0.97 . ? C9 C10 1.500(3) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.96 . ? C10 H10B 0.96 . ? C10 H10C 0.96 . ? N1 H1A 0.89 . ? N1 H1B 0.89 . ? N1 H1C 0.89 . ? Pb1 I2 3.154(2) 3_577 ? Pb1 I2 3.154(2) 11_755 ? Pb1 I2 3.1587(19) 9_777 ? Pb1 I2 3.1587(19) . ? Pb1 I1 3.177(5) 9_777 ? Pb1 I1 3.177(5) . ? I2 Pb1 3.1544(19) 3_477 ? 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 108.88(16) . . ? N1 C1 H1D 109.9 . . ? C2 C1 H1D 110 . . ? N1 C1 H1E 109.9 . . ? C2 C1 H1E 109.9 . . ? H1D C1 H1E 108.3 . . ? C1 C2 C3 106.26(15) . . ? C1 C2 H2A 110.5 . . ? C3 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? C3 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C2 C3 C4 106.26(17) . . ? C2 C3 H3A 110.5 . . ? C4 C3 H3A 110.3 . . ? C2 C3 H3B 110.5 . . ? C4 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? C5 C4 C3 106.3(2) . . ? C5 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? C5 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.7 . . ? C4 C5 C6 106.26(17) . . ? C4 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? C4 C5 H5B 110.4 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.7 . . ? C5 C6 C7 106.26(17) . . ? C5 C6 H6A 110.4 . . ? C7 C6 H6A 110.3 . . ? C5 C6 H6B 110.7 . . ? C7 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C8 C7 C6 106.3(2) . . ? C8 C7 H7A 110.4 . . ? C6 C7 H7A 110.7 . . ? C8 C7 H7B 110.4 . . ? C6 C7 H7B 110.4 . . ? H7A C7 H7B 108.7 . . ? C9 C8 C7 106.3(2) . . ? C9 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? C9 C8 H8B 110.6 . . ? C7 C8 H8B 110.6 . . ? H8A C8 H8B 108.7 . . ? C8 C9 C10 106.3(3) . . ? C8 C9 H9A 110.6 . . ? C10 C9 H9A 110.4 . . ? C8 C9 H9B 110.4 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.4 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? I2 Pb1 I2 180 3_577 11_755 ? I2 Pb1 I2 89.99(2) 3_577 9_777 ? I2 Pb1 I2 90.01(2) 11_755 9_777 ? I2 Pb1 I2 90.01(2) 3_577 . ? I2 Pb1 I2 89.99(2) 11_755 . ? I2 Pb1 I2 180.000(2) 9_777 . ? I2 Pb1 I1 90 3_577 9_777 ? I2 Pb1 I1 90 11_755 9_777 ? I2 Pb1 I1 90 9_777 9_777 ? I2 Pb1 I1 90 . 9_777 ? I2 Pb1 I1 90 3_577 . ? I2 Pb1 I1 90 11_755 . ? I2 Pb1 I1 90 9_777 . ? I2 Pb1 I1 90 . . ? I1 Pb1 I1 180.0000(10) 9_777 . ? Pb1 I2 Pb1 154.82(9) 3_477 . ? 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 156(6) . . . . ? C1 C2 C3 C4 108(6) . . . . ? C2 C3 C4 C5 135(3) . . . . ? C3 C4 C5 C6 -113(7) . . . . ? C4 C5 C6 C7 -174(5) . . . . ? C5 C6 C7 C8 90(9) . . . . ? C6 C7 C8 C9 -128(12) . . . . ? C7 C8 C9 C10 -175(18) . . . . ? I2 Pb1 I2 Pb1 0 3_577 . . 3_477 ? I2 Pb1 I2 Pb1 180 11_755 . . 3_477 ? I1 Pb1 I2 Pb1 90 9_777 . . 3_477 ? I1 Pb1 I2 Pb1 -90 . . . 3_477 ? 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 0.89 3.29 3.83(3) 122 3_567 N1 H1A I2 0.89 3.19 3.83(3) 131 11_755 _chemical_name_common 'bis(decylammonium)tetraiodoplumbate(ii) PHASE I'