Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'David G. Billing' _publ_contact_author_address ; University of the Witwatersrand Johannesburg 2050 SOUTH AFRICA ; _publ_contact_author_email DAVE@CHEM.WITS.AC.ZA _publ_section_title ; Inorganic-organic hybrid materials incorporating primary cyclic ammonium cations: The lead iodide series ; _publ_requested_category FM loop_ _publ_author_name D.G.Billing A.Lemmerer data_1 _database_code_depnum_ccdc_archive 'CCDC 609992' _audit_creation_date 2005-02-11T12:48:58-00:00 _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(cyclopropylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C6 H16 I4 N2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C3 H8 N)' _chemical_formula_weight 831 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.475(5) _cell_length_b 8.656(5) _cell_length_c 8.750(5) _cell_angle_alpha 90 _cell_angle_beta 110.275(5) _cell_angle_gamma 90 _cell_volume 886.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 965 _cell_measurement_theta_min 2.927 _cell_measurement_theta_max 27.988 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 3.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.03 0 1 0 0.03 1 0 0 0.02 -1 0 0 0.02 1 1 -2 0.09 -1 0 2 0.1 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.459 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2432 _exptl_absorpt_correction_T_max 0.5325 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_unetI/netI 0.0576 _diffrn_reflns_number 5635 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 2105 _reflns_number_gt 1466 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+3.4535P] 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 0.0015(2) _refine_ls_number_reflns 2105 _refine_ls_number_parameters 62 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0652 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.094 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.862 _refine_diff_density_min -2.199 _refine_diff_density_rms 0.222 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.3591(12) 0.9877(17) 0.7332(18) 0.102(4) Uani 1 1 d DU . . H1 H 0.4151 1.0598 0.8095 0.123 Uiso 1 1 calc R . . C2 C 0.3874(19) 0.8239(18) 0.738(2) 0.120(5) Uani 1 1 d DU . . H2A H 0.3245 0.7485 0.7206 0.144 Uiso 1 1 calc R . . H2B H 0.4621 0.7904 0.8167 0.144 Uiso 1 1 calc R . . C3 C 0.3877(16) 0.919(2) 0.5974(17) 0.105(4) Uani 1 1 d DU . . H3A H 0.4625 0.9456 0.5884 0.126 Uiso 1 1 calc R . . H3B H 0.3248 0.9036 0.4922 0.126 Uiso 1 1 calc R . . N1 N 0.2330(11) 1.0221(14) 0.6858(13) 0.085(3) Uani 1 1 d DU . . H1A H 0.2222 1.1261 0.6849 0.127 Uiso 1 1 calc R . . H1B H 0.2056 0.9777 0.7591 0.127 Uiso 1 1 calc R . . H1C H 0.1952 0.9831 0.5848 0.127 Uiso 1 1 calc R . . I1 I -0.26352(7) 0.91441(11) 0.89545(9) 0.0622(3) Uani 1 1 d . . . I2 I -0.05202(8) 1.19500(8) 0.67008(8) 0.0535(3) Uani 1 1 d . . . Pb1 Pb 0 1 1 0.03825(19) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.125(8) 0.116(10) 0.084(9) 0.014(8) 0.061(8) 0.020(9) C2 0.124(11) 0.121(10) 0.120(10) 0.024(9) 0.047(10) 0.031(8) C3 0.111(10) 0.131(12) 0.084(8) -0.007(8) 0.046(8) 0.011(9) N1 0.122(8) 0.083(8) 0.053(6) -0.003(6) 0.034(6) 0.020(7) I1 0.0642(6) 0.0757(6) 0.0447(4) -0.0050(4) 0.0163(4) -0.0037(4) I2 0.0983(7) 0.0354(4) 0.0355(4) 0.0094(3) 0.0340(4) 0.0007(4) Pb1 0.0653(4) 0.0276(3) 0.0257(3) -0.00100(19) 0.0207(2) -0.0050(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.459(9) . ? C1 C3 1.478(9) . ? C1 N1 1.511(9) . ? C1 H1 1 . ? C2 C3 1.485(9) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.1794(15) 3_577 ? I1 Pb1 3.1794(15) . ? I2 Pb1 3.2055(15) 2_556 ? I2 Pb1 3.2102(16) 3_577 ? I2 Pb1 3.2102(16) . ? Pb1 I1 3.1794(15) 3_577 ? Pb1 I2 3.2055(15) 2_546 ? Pb1 I2 3.2055(15) 4_586 ? Pb1 I2 3.2102(16) 3_577 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C3 60.7(5) . . ? C2 C1 N1 114.7(15) . . ? C3 C1 N1 112.1(13) . . ? C2 C1 H1 118.7 . . ? C3 C1 H1 118.7 . . ? N1 C1 H1 118.7 . . ? C1 C2 C3 60.3(5) . . ? C1 C2 H2A 117.7 . . ? C3 C2 H2A 117.7 . . ? C1 C2 H2B 117.7 . . ? C3 C2 H2B 117.7 . . ? H2A C2 H2B 114.9 . . ? C1 C3 C2 59.0(5) . . ? C1 C3 H3A 117.9 . . ? C2 C3 H3A 117.9 . . ? C1 C3 H3B 117.9 . . ? C2 C3 H3B 117.9 . . ? H3A C3 H3B 115 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 147.16(3) 2_556 3_577 ? Pb1 I2 Pb1 147.16(3) 2_556 . ? I1 Pb1 I1 180 . 3_577 ? I1 Pb1 I2 91.72(3) . 2_546 ? I1 Pb1 I2 88.28(3) 3_577 2_546 ? I1 Pb1 I2 88.28(3) . 4_586 ? I1 Pb1 I2 91.72(3) 3_577 4_586 ? I2 Pb1 I2 180 2_546 4_586 ? I1 Pb1 I2 90.17(2) . 3_577 ? I1 Pb1 I2 89.83(2) 3_577 3_577 ? I2 Pb1 I2 88.51(4) 2_546 3_577 ? I2 Pb1 I2 91.49(4) 4_586 3_577 ? I1 Pb1 I2 89.83(2) . . ? I1 Pb1 I2 90.17(2) 3_577 . ? I2 Pb1 I2 91.49(4) 2_546 . ? I2 Pb1 I2 88.51(4) 4_586 . ? I2 Pb1 I2 180 3_577 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 102.6(15) . . . . ? N1 C1 C3 C2 -106.8(16) . . . . ? Pb1 I2 Pb1 I1 140.14(5) 2_556 . . . ? Pb1 I2 Pb1 I1 -39.86(5) 2_556 . . 3_577 ? Pb1 I2 Pb1 I2 -128.15(7) 2_556 . . 2_546 ? Pb1 I2 Pb1 I2 51.85(7) 2_556 . . 4_586 ? 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 2.69 3.517(13) 151.5 2_556 N1 H1B I1 0.91 3.00 3.592(11) 124.1 3_577 N1 H1C I2 0.91 2.79 3.668(12) 162.6 3_576 _chemical_name_common bis(cyclopropylammonium)tetraiodoplumbate(ii) ####END data_2 _database_code_depnum_ccdc_archive 'CCDC 609993' _audit_creation_date 2004-11-12T15:48:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; bis(cyclobutylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C8 H20 I4 N2 Pb' _chemical_formula_moiety 'I4 Pb, 2(C4 H10 N)' _chemical_formula_weight 859.05 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.355(3) _cell_length_b 8.3560(17) _cell_length_c 9.0583(18) _cell_angle_alpha 90 _cell_angle_beta 107.747(4) _cell_angle_gamma 90 _cell_volume 962.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 3.2045 _cell_measurement_theta_max 28.2405 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.963 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 0 0.02 -1 0 0 0.02 -1 -1 1 0.15 0 1 0 0.18 0 0 1 0.14 0 0 -1 0.14 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 15.158 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0311 _exptl_absorpt_correction_T_max 0.5518 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0451 _diffrn_reflns_number 5951 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 2297 _reflns_number_gt 1962 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2297 _refine_ls_number_parameters 70 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0573 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.908 _refine_diff_density_min -1.907 _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 -0.2963(5) 0.0889(7) -0.1793(7) 0.0333(12) Uani 1 1 d DU . . H1 H -0.281 0.2036 -0.196 0.04 Uiso 1 1 calc R . . C2 C -0.4031(6) 0.0389(10) -0.2895(8) 0.0507(16) Uani 1 1 d U . . H2A H -0.4085 -0.0764 -0.3158 0.061 Uiso 1 1 calc R . . H2B H -0.4279 0.106 -0.3837 0.061 Uiso 1 1 calc R . . C3 C -0.4512(6) 0.0848(13) -0.1596(9) 0.071(2) Uani 1 1 d DU . . H3A H -0.4811 0.1941 -0.1701 0.086 Uiso 1 1 calc R . . H3B H -0.5017 0.0052 -0.1435 0.086 Uiso 1 1 calc R . . C4 C -0.3409(5) 0.0721(9) -0.0422(8) 0.0483(16) Uani 1 1 d DU . . H4A H -0.326 -0.0326 0.0114 0.058 Uiso 1 1 calc R . . H4B H -0.3225 0.1617 0.0327 0.058 Uiso 1 1 calc R . . N1 N -0.2052(4) -0.0137(5) -0.1751(6) 0.0318(11) Uani 1 1 d U . . H1A H -0.1461 0.0273 -0.1063 0.048 Uiso 1 1 calc R . . H1B H -0.1968 -0.0173 -0.271 0.048 Uiso 1 1 calc R . . H1C H -0.2165 -0.1144 -0.1452 0.048 Uiso 1 1 calc R . . I1 I -0.24582(3) 0.57673(4) -0.08295(4) 0.02924(10) Uani 1 1 d . . . I2 I 0.04611(3) 0.80999(4) -0.17712(4) 0.02578(10) Uani 1 1 d . . . Pb1 Pb 0 0.5 0 0.02026(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(3) 0.037(3) 0.033(3) 0.001(2) 0.007(2) 0.004(2) C2 0.034(3) 0.079(4) 0.034(3) -0.003(3) 0.002(2) 0.001(3) C3 0.029(3) 0.130(7) 0.054(4) -0.011(5) 0.010(3) 0.015(4) C4 0.037(3) 0.077(4) 0.032(3) -0.006(3) 0.012(2) 0.011(3) N1 0.032(3) 0.034(2) 0.030(3) -0.001(2) 0.011(2) 0.001(2) I1 0.0264(2) 0.03212(19) 0.0278(2) 0.00359(14) 0.00634(15) 0.00176(15) I2 0.0304(2) 0.02513(17) 0.02152(18) 0.00728(13) 0.00752(15) 0.00016(14) Pb1 0.02325(15) 0.02070(14) 0.01733(14) -0.00036(10) 0.00694(11) -0.00027(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 1.480(7) . ? C1 C2 1.529(9) . ? C1 C4 1.540(7) . ? C1 H1 1 . ? C2 C3 1.550(10) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.535(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.2015(7) . ? I2 Pb1 3.2039(6) . ? I2 Pb1 3.2181(6) 2_554 ? Pb1 I1 3.2015(7) 3_565 ? Pb1 I2 3.2039(5) 3_565 ? Pb1 I2 3.2181(6) 2_544 ? Pb1 I2 3.2181(6) 4_576 ? 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 117.1(5) . . ? N1 C1 C4 116.3(5) . . ? C2 C1 C4 89.3(5) . . ? N1 C1 H1 110.8 . . ? C2 C1 H1 110.8 . . ? C4 C1 H1 110.8 . . ? C1 C2 C3 87.5(5) . . ? C1 C2 H2A 114.1 . . ? C3 C2 H2A 114.1 . . ? C1 C2 H2B 114.1 . . ? C3 C2 H2B 114.1 . . ? H2A C2 H2B 111.2 . . ? C4 C3 C2 88.7(5) . . ? C4 C3 H3A 113.9 . . ? C2 C3 H3A 113.9 . . ? C4 C3 H3B 113.9 . . ? C2 C3 H3B 113.9 . . ? H3A C3 H3B 111.1 . . ? C3 C4 C1 87.7(5) . . ? C3 C4 H4A 114 . . ? C1 C4 H4A 114 . . ? C3 C4 H4B 114 . . ? C1 C4 H4B 114 . . ? H4A C4 H4B 111.2 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I2 Pb1 147.271(12) . 2_554 ? I1 Pb1 I1 180.000(4) 3_565 . ? I1 Pb1 I2 86.536(11) 3_565 . ? I1 Pb1 I2 93.464(11) . . ? I1 Pb1 I2 93.464(11) 3_565 3_565 ? I1 Pb1 I2 86.536(11) . 3_565 ? I2 Pb1 I2 180 . 3_565 ? I1 Pb1 I2 90.742(10) 3_565 2_544 ? I1 Pb1 I2 89.258(10) . 2_544 ? I2 Pb1 I2 87.507(15) . 2_544 ? I2 Pb1 I2 92.493(15) 3_565 2_544 ? I1 Pb1 I2 89.258(10) 3_565 4_576 ? I1 Pb1 I2 90.742(10) . 4_576 ? I2 Pb1 I2 92.493(15) . 4_576 ? I2 Pb1 I2 87.507(15) 3_565 4_576 ? I2 Pb1 I2 180.000(12) 2_544 4_576 ? 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 138.9(6) . . . . ? C4 C1 C2 C3 19.5(6) . . . . ? C1 C2 C3 C4 -19.5(6) . . . . ? C2 C3 C4 C1 19.4(6) . . . . ? N1 C1 C4 C3 -139.8(6) . . . . ? C2 C1 C4 C3 -19.7(6) . . . . ? Pb1 I2 Pb1 I1 118.97(2) 2_554 . . 3_565 ? Pb1 I2 Pb1 I1 -61.03(2) 2_554 . . . ? Pb1 I2 Pb1 I2 28.075(18) 2_554 . . 2_544 ? Pb1 I2 Pb1 I2 -151.925(18) 2_554 . . 4_576 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.91 2.85 3.668(5) 150 3_565 N1 H1B I1 0.91 2.74 3.606(5) 158.3 4_565 N1 H1C I1 0.91 2.7 3.602(4) 174.1 1_545 _chemical_name_common bis(cyclobutylammonium)tetraiodoplumbate(ii) ####END data_3 _database_code_depnum_ccdc_archive 'CCDC 609994' _audit_creation_date 2005-10-26T14:51:07-00:00 _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(cyclopentylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C10 H24 I4 N2 Pb' _chemical_formula_moiety '2(C5 H12 N), I4 Pb' _chemical_formula_weight 887.1 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.00(2) _cell_length_b 8.928(14) _cell_length_c 8.949(15) _cell_angle_alpha 90 _cell_angle_beta 108.57(4) _cell_angle_gamma 90 _cell_volume 1060(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 3.0695 _cell_measurement_theta_max 27.982 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 2.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 0 0.02 1 0 0 0.02 1 0 -2 0.12 -1 0 2 0.12 0 -1 0 0.19 0 1 0 0.19 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.765 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0473 _exptl_absorpt_correction_T_max 0.5485 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.1114 _diffrn_reflns_av_unetI/netI 0.0729 _diffrn_reflns_number 5946 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 1864 _reflns_number_gt 1625 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1999P)^2^+4.2325P] 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 1864 _refine_ls_number_parameters 135 _refine_ls_number_restraints 211 _refine_ls_R_factor_all 0.1012 _refine_ls_R_factor_gt 0.093 _refine_ls_wR_factor_ref 0.261 _refine_ls_wR_factor_gt 0.2339 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 7.066 _refine_diff_density_min -4.087 _refine_diff_density_rms 0.566 #----------------------------------------------------------------------------# # 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 C1A C 0.277(3) 0.447(7) 0.104(7) 0.072(7) Uani 0.40(3) 1 d PDU A 1 H1A H 0.2651 0.3654 0.0273 0.086 Uiso 0.40(3) 1 calc PR A 1 C2A C 0.282(4) 0.567(8) 0.007(9) 0.073(7) Uani 0.40(3) 1 d PDU A 1 H2A1 H 0.2456 0.6532 0.0275 0.087 Uiso 0.40(3) 1 calc PR A 1 H2A2 H 0.2541 0.5397 -0.1033 0.087 Uiso 0.40(3) 1 calc PR A 1 C3A C 0.384(4) 0.594(8) 0.050(10) 0.078(7) Uani 0.40(3) 1 d PDU A 1 H3A1 H 0.4043 0.5956 -0.0444 0.093 Uiso 0.40(3) 1 calc PR A 1 H3A2 H 0.3983 0.6919 0.0987 0.093 Uiso 0.40(3) 1 calc PR A 1 C4A C 0.441(3) 0.487(9) 0.153(9) 0.078(7) Uani 0.40(3) 1 d PDU A 1 H4A1 H 0.4908 0.5348 0.2415 0.094 Uiso 0.40(3) 1 calc PR A 1 H4A2 H 0.4751 0.4218 0.1001 0.094 Uiso 0.40(3) 1 calc PR A 1 C5A C 0.372(3) 0.408(8) 0.203(9) 0.076(7) Uani 0.40(3) 1 d PDU A 1 H5A1 H 0.3782 0.4338 0.3115 0.091 Uiso 0.40(3) 1 calc PR A 1 H5A2 H 0.3823 0.3012 0.1976 0.091 Uiso 0.40(3) 1 calc PR A 1 N1A N 0.187(4) 0.431(8) 0.153(8) 0.061(10) Uani 0.40(3) 1 d PDU A 1 H1A1 H 0.2052 0.3997 0.253 0.092 Uiso 0.40(3) 1 calc PR A 1 H1A2 H 0.1455 0.3635 0.0919 0.092 Uiso 0.40(3) 1 calc PR A 1 H1A3 H 0.1554 0.5183 0.145 0.092 Uiso 0.40(3) 1 calc PR A 1 C1B C 0.283(3) 0.524(5) 0.220(5) 0.068(6) Uani 0.60(3) 1 d PDU A 2 H1B H 0.2698 0.6011 0.2889 0.081 Uiso 0.60(3) 1 calc PR A 2 C2B C 0.277(3) 0.602(6) 0.083(5) 0.072(7) Uani 0.60(3) 1 d PDU A 2 H2B1 H 0.2464 0.5412 -0.0099 0.086 Uiso 0.60(3) 1 calc PR A 2 H2B2 H 0.2386 0.6937 0.0753 0.086 Uiso 0.60(3) 1 calc PR A 2 C3B C 0.377(3) 0.632(6) 0.102(6) 0.076(7) Uani 0.60(3) 1 d PDU A 2 H3B1 H 0.3917 0.6005 0.0075 0.091 Uiso 0.60(3) 1 calc PR A 2 H3B2 H 0.3884 0.7387 0.1137 0.091 Uiso 0.60(3) 1 calc PR A 2 C4B C 0.443(3) 0.560(7) 0.230(6) 0.080(7) Uani 0.60(3) 1 d PDU A 2 H4B1 H 0.484 0.6321 0.3044 0.096 Uiso 0.60(3) 1 calc PR A 2 H4B2 H 0.4871 0.4929 0.1975 0.096 Uiso 0.60(3) 1 calc PR A 2 C5B C 0.382(2) 0.480(6) 0.298(7) 0.077(7) Uani 0.60(3) 1 d PDU A 2 H5B1 H 0.4004 0.5028 0.4096 0.092 Uiso 0.60(3) 1 calc PR A 2 H5B2 H 0.3902 0.3735 0.2857 0.092 Uiso 0.60(3) 1 calc PR A 2 N1B N 0.2027(18) 0.412(4) 0.208(4) 0.040(6) Uani 0.60(3) 1 d PDU A 2 H1B1 H 0.2117 0.3711 0.3024 0.06 Uiso 0.60(3) 1 calc PR A 2 H1B2 H 0.2055 0.3407 0.14 0.06 Uiso 0.60(3) 1 calc PR A 2 H1B3 H 0.1427 0.4563 0.1749 0.06 Uiso 0.60(3) 1 calc PR A 2 I1 I 0.23966(13) 1.0312(3) 0.1161(5) 0.0861(8) Uani 1 1 d . . . I2 I -0.00357(13) 1.19336(13) 0.30415(17) 0.0555(5) Uani 1 1 d . . . Pb1 Pb 0 1 0 0.0496(5) 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 C1A 0.062(9) 0.094(14) 0.062(15) 0.016(12) 0.023(10) 0.005(11) C2A 0.064(10) 0.096(16) 0.067(16) 0.014(12) 0.032(12) 0.006(11) C3A 0.065(10) 0.101(16) 0.075(16) 0.011(12) 0.033(12) 0.003(11) C4A 0.063(9) 0.102(16) 0.076(17) 0.009(13) 0.031(12) 0.006(12) C5A 0.059(9) 0.099(15) 0.073(15) 0.013(11) 0.026(11) 0.008(11) N1A 0.058(12) 0.07(2) 0.06(2) 0.016(19) 0.021(15) 0.011(16) C1B 0.057(8) 0.092(14) 0.058(14) 0.017(11) 0.025(10) 0.009(9) C2B 0.062(9) 0.094(15) 0.067(14) 0.020(11) 0.032(10) -0.001(11) C3B 0.063(10) 0.101(15) 0.075(15) 0.009(12) 0.038(10) 0.004(11) C4B 0.061(8) 0.104(15) 0.082(16) 0.009(12) 0.031(10) 0.002(11) C5B 0.054(9) 0.098(16) 0.076(16) 0.015(12) 0.018(11) -0.001(11) N1B 0.040(9) 0.065(14) 0.019(13) 0.020(11) 0.015(10) 0.030(9) I1 0.0501(9) 0.1034(16) 0.0934(15) 0.0000(17) 0.0068(15) 0.0177(9) I2 0.0611(8) 0.0478(8) 0.0573(10) -0.0149(6) 0.0185(12) -0.0079(6) Pb1 0.0507(7) 0.0452(6) 0.0490(8) 0.0018(4) 0.0101(10) 0.0053(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 C1A C2A 1.39(2) . ? C1A C5A 1.39(2) . ? C1A N1A 1.47(5) . ? C1A H1A 0.98 . ? C2A C3A 1.39(2) . ? C2A H2A1 0.97 . ? C2A H2A2 0.97 . ? C3A C4A 1.39(2) . ? C3A H3A1 0.97 . ? C3A H3A2 0.97 . ? C4A C5A 1.39(2) . ? C4A H4A1 0.97 . ? C4A H4A2 0.97 . ? C5A H5A1 0.97 . ? C5A H5A2 0.97 . ? N1A H1A1 0.89 . ? N1A H1A2 0.89 . ? N1A H1A3 0.89 . ? C1B C2B 1.39(3) . ? C1B C5B 1.40(3) . ? C1B N1B 1.48(5) . ? C1B H1B 0.98 . ? C2B C3B 1.39(3) . ? C2B H2B1 0.97 . ? C2B H2B2 0.97 . ? C3B C4B 1.38(3) . ? C3B H3B1 0.97 . ? C3B H3B2 0.97 . ? C4B C5B 1.39(3) . ? C4B H4B1 0.97 . ? C4B H4B2 0.97 . ? C5B H5B1 0.97 . ? C5B H5B2 0.97 . ? N1B H1B1 0.89 . ? N1B H1B2 0.89 . ? N1B H1B3 0.89 . ? I1 Pb1 3.193(6) . ? I2 Pb1 3.237(4) . ? I2 Pb1 3.242(4) 2 ? Pb1 I1 3.193(6) 3_575 ? Pb1 I2 3.237(4) 3_575 ? Pb1 I2 3.242(4) 4_585 ? Pb1 I2 3.242(4) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A C5A 111(3) . . ? C2A C1A N1A 119(4) . . ? C5A C1A N1A 121(4) . . ? C2A C1A H1A 99.7 . . ? C5A C1A H1A 99.7 . . ? N1A C1A H1A 99.7 . . ? C1A C2A C3A 103(3) . . ? C1A C2A H2A1 111.3 . . ? C3A C2A H2A1 111.3 . . ? C1A C2A H2A2 111.3 . . ? C3A C2A H2A2 111.3 . . ? H2A1 C2A H2A2 109.2 . . ? C4A C3A C2A 113(3) . . ? C4A C3A H3A1 109.1 . . ? C2A C3A H3A1 109.1 . . ? C4A C3A H3A2 109.1 . . ? C2A C3A H3A2 109.1 . . ? H3A1 C3A H3A2 107.8 . . ? C3A C4A C5A 105(3) . . ? C3A C4A H4A1 110.8 . . ? C5A C4A H4A1 110.8 . . ? C3A C4A H4A2 110.8 . . ? C5A C4A H4A2 110.8 . . ? H4A1 C4A H4A2 108.9 . . ? C4A C5A C1A 107(3) . . ? C4A C5A H5A1 110.4 . . ? C1A C5A H5A1 110.4 . . ? C4A C5A H5A2 110.4 . . ? C1A C5A H5A2 110.4 . . ? H5A1 C5A H5A2 108.6 . . ? C1A N1A H1A1 109.5 . . ? C1A N1A H1A2 109.5 . . ? H1A1 N1A H1A2 109.5 . . ? C1A N1A H1A3 109.5 . . ? H1A1 N1A H1A3 109.5 . . ? H1A2 N1A H1A3 109.5 . . ? C2B C1B C5B 110(3) . . ? C2B C1B N1B 117(3) . . ? C5B C1B N1B 117(3) . . ? C2B C1B H1B 103.5 . . ? C5B C1B H1B 103.5 . . ? N1B C1B H1B 103.5 . . ? C3B C2B C1B 103(3) . . ? C3B C2B H2B1 111.3 . . ? C1B C2B H2B1 111.3 . . ? C3B C2B H2B2 111.3 . . ? C1B C2B H2B2 111.3 . . ? H2B1 C2B H2B2 109.2 . . ? C4B C3B C2B 113(3) . . ? C4B C3B H3B1 108.9 . . ? C2B C3B H3B1 108.9 . . ? C4B C3B H3B2 108.9 . . ? C2B C3B H3B2 108.9 . . ? H3B1 C3B H3B2 107.7 . . ? C3B C4B C5B 105(3) . . ? C3B C4B H4B1 110.7 . . ? C5B C4B H4B1 110.7 . . ? C3B C4B H4B2 110.7 . . ? C5B C4B H4B2 110.7 . . ? H4B1 C4B H4B2 108.8 . . ? C4B C5B C1B 107(3) . . ? C4B C5B H5B1 110.3 . . ? C1B C5B H5B1 110.3 . . ? C4B C5B H5B2 110.3 . . ? C1B C5B H5B2 110.3 . . ? H5B1 C5B H5B2 108.6 . . ? C1B N1B H1B1 109.5 . . ? C1B N1B H1B2 109.5 . . ? H1B1 N1B H1B2 109.5 . . ? C1B N1B H1B3 109.5 . . ? H1B1 N1B H1B3 109.5 . . ? H1B2 N1B H1B3 109.5 . . ? Pb1 I2 Pb1 154.57(5) . 2 ? I1 Pb1 I1 180.00(9) . 3_575 ? I1 Pb1 I2 88.62(9) . . ? I1 Pb1 I2 91.38(9) 3_575 . ? I1 Pb1 I2 91.38(9) . 3_575 ? I1 Pb1 I2 88.62(9) 3_575 3_575 ? I2 Pb1 I2 180 . 3_575 ? I1 Pb1 I2 86.33(7) . 4_585 ? I1 Pb1 I2 93.67(7) 3_575 4_585 ? I2 Pb1 I2 90.14(12) . 4_585 ? I2 Pb1 I2 89.86(12) 3_575 4_585 ? I1 Pb1 I2 93.67(7) . 2_545 ? I1 Pb1 I2 86.33(7) 3_575 2_545 ? I2 Pb1 I2 89.86(12) . 2_545 ? I2 Pb1 I2 90.14(12) 3_575 2_545 ? I2 Pb1 I2 180 4_585 2_545 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5A C1A C2A C3A 2(9) . . . . ? N1A C1A C2A C3A 150(7) . . . . ? C1A C2A C3A C4A 7(10) . . . . ? C2A C3A C4A C5A -13(11) . . . . ? C3A C4A C5A C1A 13(9) . . . . ? C2A C1A C5A C4A -10(9) . . . . ? N1A C1A C5A C4A -157(7) . . . . ? C5B C1B C2B C3B -13(6) . . . . ? N1B C1B C2B C3B -150(5) . . . . ? C1B C2B C3B C4B 8(7) . . . . ? C2B C3B C4B C5B 0(8) . . . . ? C3B C4B C5B C1B -8(7) . . . . ? C2B C1B C5B C4B 14(7) . . . . ? N1B C1B C5B C4B 150(5) . . . . ? Pb1 I2 Pb1 I1 81.77(15) 2 . . . ? Pb1 I2 Pb1 I1 -98.23(15) 2 . . 3_575 ? Pb1 I2 Pb1 I2 -4.56(17) 2 . . 4_585 ? Pb1 I2 Pb1 I2 175.44(17) 2 . . 2_545 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1A1 I1 0.89 3.19 3.98(7) 149.7 4_576 N1A H1A2 I2 0.89 2.8 3.58(7) 146.9 4_575 N1A H1A3 I2 0.89 2.79 3.59(7) 149.5 2_545 N1B H1B1 I1 0.89 2.85 3.56(3) 138 4_576 N1B H1B2 I1 0.89 2.82 3.57(4) 142.8 1_545 N1B H1B3 I2 0.89 2.92 3.73(3) 151.5 2_545 _chemical_name_common bis(cyclopentylammonium)tetraiodoplumbate(ii) ###END data_3ac2l_a _database_code_depnum_ccdc_archive 'CCDC 609995' _audit_creation_date 2005-10-27T11:25:20-00:00 _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(cyclohexylammonium)tetraiodoplumbate(II) ; _chemical_formula_sum 'C12 H28 I4 N2 Pb' _chemical_formula_moiety '2(C6 H14 N), I4 Pb' _chemical_formula_weight 915.15 #----------------------------------------------------------------------------# # 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 9.1677(15) _cell_length_b 8.7335(14) _cell_length_c 27.276(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2183.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 906 _cell_measurement_theta_min 2.675 _cell_measurement_theta_max 28.285 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.025 0 0 -1 0.025 -3 -1 -3 0.11 2 3 1 0.155 2 -1 0 0.13 0 1 0 0.17 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.373 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0577 _exptl_absorpt_correction_T_max 0.512 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_unetI/netI 0.043 _diffrn_reflns_number 13519 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2633 _reflns_number_gt 1986 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+1.3770P] 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 2633 _refine_ls_number_parameters 152 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.069 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.864 _refine_diff_density_min -1.695 _refine_diff_density_rms 0.214 #----------------------------------------------------------------------------# # 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 C1A C 0.024(2) -0.0580(19) 0.6352(7) 0.035(3) Uani 0.315(8) 1 d PDU A 1 H1A H 0.121 -0.1086 0.6314 0.041 Uiso 0.315(8) 1 calc PR A 1 C2A C -0.043(3) -0.107(3) 0.6840(6) 0.036(4) Uani 0.315(8) 1 d PDU A 1 H2A1 H -0.1432 -0.0659 0.6865 0.043 Uiso 0.315(8) 1 calc PR A 1 H2A2 H -0.0485 -0.22 0.6853 0.043 Uiso 0.315(8) 1 calc PR A 1 C3A C 0.048(3) -0.048(2) 0.7268(7) 0.043(3) Uani 0.315(8) 1 d PDU A 1 H3A1 H -0.0012 -0.074 0.758 0.052 Uiso 0.315(8) 1 calc PR A 1 H3A2 H 0.1445 -0.0997 0.7266 0.052 Uiso 0.315(8) 1 calc PR A 1 C4A C 0.069(3) 0.124(2) 0.7233(8) 0.042(3) Uani 0.315(8) 1 d PDU A 1 H4A1 H 0.1328 0.1585 0.7504 0.051 Uiso 0.315(8) 1 calc PR A 1 H4A2 H -0.0266 0.1752 0.7269 0.051 Uiso 0.315(8) 1 calc PR A 1 C5A C 0.137(3) 0.170(4) 0.6743(6) 0.041(4) Uani 0.315(8) 1 d PDU A 1 H5A1 H 0.1472 0.2824 0.6729 0.049 Uiso 0.315(8) 1 calc PR A 1 H5A2 H 0.2361 0.1245 0.6717 0.049 Uiso 0.315(8) 1 calc PR A 1 C6A C 0.044(2) 0.1149(19) 0.6315(7) 0.036(3) Uani 0.315(8) 1 d PDU A 1 H6A1 H -0.0523 0.1662 0.6324 0.043 Uiso 0.315(8) 1 calc PR A 1 H6A2 H 0.0921 0.1411 0.6001 0.043 Uiso 0.315(8) 1 calc PR A 1 N1A N -0.075(6) -0.110(5) 0.594(2) 0.033(7) Uani 0.315(8) 1 d PU A 1 H1A1 H -0.1648 -0.0673 0.5975 0.049 Uiso 0.315(8) 1 calc PR A 1 H1A2 H -0.0826 -0.2136 0.5941 0.049 Uiso 0.315(8) 1 calc PR A 1 H1A3 H -0.0363 -0.0794 0.5645 0.049 Uiso 0.315(8) 1 calc PR A 1 C1B C -0.0427(9) 0.0258(10) 0.6386(3) 0.0304(17) Uani 0.685(8) 1 d PDU A 2 H1B H -0.0938 0.1269 0.6376 0.036 Uiso 0.685(8) 1 calc PR A 2 C2B C -0.0832(12) -0.0572(12) 0.6856(3) 0.037(2) Uani 0.685(8) 1 d PDU A 2 H2B1 H -0.038 -0.1601 0.6858 0.044 Uiso 0.685(8) 1 calc PR A 2 H2B2 H -0.1903 -0.0699 0.6873 0.044 Uiso 0.685(8) 1 calc PR A 2 C3B C -0.0305(11) 0.0336(13) 0.7296(3) 0.047(2) Uani 0.685(8) 1 d PDU A 2 H3B1 H -0.0807 0.1339 0.7306 0.056 Uiso 0.685(8) 1 calc PR A 2 H3B2 H -0.0549 -0.0224 0.7601 0.056 Uiso 0.685(8) 1 calc PR A 2 C4B C 0.1325(11) 0.0581(13) 0.7269(4) 0.048(2) Uani 0.685(8) 1 d PDU A 2 H4B1 H 0.1827 -0.042 0.7289 0.058 Uiso 0.685(8) 1 calc PR A 2 H4B2 H 0.1644 0.1211 0.7551 0.058 Uiso 0.685(8) 1 calc PR A 2 C5B C 0.1750(13) 0.1376(14) 0.6795(3) 0.040(3) Uani 0.685(8) 1 d PDU A 2 H5B1 H 0.1339 0.2424 0.6793 0.049 Uiso 0.685(8) 1 calc PR A 2 H5B2 H 0.2825 0.1463 0.6779 0.049 Uiso 0.685(8) 1 calc PR A 2 C6B C 0.1206(9) 0.0516(11) 0.6349(3) 0.0357(18) Uani 0.685(8) 1 d PDU A 2 H6B1 H 0.1712 -0.0483 0.6325 0.043 Uiso 0.685(8) 1 calc PR A 2 H6B2 H 0.1428 0.1111 0.6049 0.043 Uiso 0.685(8) 1 calc PR A 2 N1B N -0.093(3) -0.072(2) 0.5954(11) 0.033(4) Uani 0.685(8) 1 d PU A 2 H1B1 H -0.0548 -0.0329 0.5671 0.05 Uiso 0.685(8) 1 calc PR A 2 H1B2 H -0.1918 -0.0703 0.5936 0.05 Uiso 0.685(8) 1 calc PR A 2 H1B3 H -0.0613 -0.1695 0.5995 0.05 Uiso 0.685(8) 1 calc PR A 2 Pb1 Pb 0.5 0 0.5 0.02677(9) Uani 1 2 d S . . I2 I 0.80358(4) 0.19311(4) 0.495814(12) 0.02673(11) Uani 1 1 d . . . I1 I 0.53781(5) 0.01107(5) 0.615659(17) 0.04459(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.034(7) 0.041(6) 0.029(5) 0.003(6) 0.004(5) 0.001(6) C2A 0.048(9) 0.036(8) 0.022(5) -0.002(6) 0.009(6) 0.001(7) C3A 0.052(8) 0.049(7) 0.029(5) -0.002(6) 0.000(6) 0.005(7) C4A 0.045(8) 0.050(7) 0.032(5) -0.011(6) 0.001(7) 0.001(6) C5A 0.030(9) 0.048(8) 0.045(7) -0.005(6) 0.003(6) -0.004(7) C6A 0.034(7) 0.041(6) 0.032(6) 0.000(6) 0.008(6) -0.002(7) N1A 0.041(15) 0.037(15) 0.019(7) 0.002(12) 0.010(9) 0.000(13) C1B 0.034(4) 0.030(4) 0.027(3) 0.003(3) 0.004(3) -0.001(3) C2B 0.042(5) 0.047(6) 0.021(3) 0.002(3) 0.009(3) -0.004(4) C3B 0.056(5) 0.061(6) 0.023(3) -0.003(4) 0.003(4) -0.004(5) C4B 0.053(5) 0.062(6) 0.029(4) -0.007(4) -0.004(4) 0.004(4) C5B 0.035(5) 0.044(6) 0.043(4) -0.007(4) -0.001(4) -0.001(4) C6B 0.033(4) 0.045(5) 0.029(3) 0.000(4) 0.003(3) 0.003(3) N1B 0.033(6) 0.046(10) 0.021(4) 0.003(6) 0.004(5) 0.002(6) Pb1 0.02562(15) 0.02813(17) 0.02654(17) 0.00421(14) 0.00216(12) 0.00089(11) I2 0.02501(17) 0.02519(19) 0.0300(2) 0.00068(16) 0.00305(16) -0.00726(14) I1 0.0460(2) 0.0626(3) 0.0252(2) 0.0062(2) 0.00710(19) 0.0020(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A N1A 1.52(5) . ? C1A C6A 1.525(14) . ? C1A C2A 1.525(14) . ? C1A H1A 1 . ? C2A C3A 1.523(14) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C4A 1.519(14) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C4A C5A 1.528(14) . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? C5A C6A 1.525(14) . ? C5A H5A1 0.99 . ? C5A H5A2 0.99 . ? C6A H6A1 0.99 . ? C6A H6A2 0.99 . ? N1A H1A1 0.91 . ? N1A H1A2 0.91 . ? N1A H1A3 0.91 . ? C1B C6B 1.517(8) . ? C1B C2B 1.518(8) . ? C1B N1B 1.53(2) . ? C1B H1B 1 . ? C2B C3B 1.518(8) . ? C2B H2B1 0.99 . ? C2B H2B2 0.99 . ? C3B C4B 1.511(8) . ? C3B H3B1 0.99 . ? C3B H3B2 0.99 . ? C4B C5B 1.517(8) . ? C4B H4B1 0.99 . ? C4B H4B2 0.99 . ? C5B C6B 1.515(8) . ? C5B H5B1 0.99 . ? C5B H5B2 0.99 . ? C6B H6B1 0.99 . ? C6B H6B2 0.99 . ? N1B H1B1 0.91 . ? N1B H1B2 0.91 . ? N1B H1B3 0.91 . ? Pb1 I1 3.1752(7) . ? Pb1 I1 3.1752(7) 5_656 ? Pb1 I2 3.2310(5) 4_456 ? Pb1 I2 3.2310(5) 8_755 ? Pb1 I2 3.2563(5) . ? Pb1 I2 3.2563(5) 5_656 ? I2 Pb1 3.2310(5) 4_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A C1A C6A 109(2) . . ? N1A C1A C2A 109(3) . . ? C6A C1A C2A 112.5(16) . . ? N1A C1A H1A 108.9 . . ? C6A C1A H1A 108.9 . . ? C2A C1A H1A 108.9 . . ? C3A C2A C1A 110.8(19) . . ? C3A C2A H2A1 109.5 . . ? C1A C2A H2A1 109.5 . . ? C3A C2A H2A2 109.5 . . ? C1A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? C4A C3A C2A 110.7(17) . . ? C4A C3A H3A1 109.5 . . ? C2A C3A H3A1 109.5 . . ? C4A C3A H3A2 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 108.1 . . ? C3A C4A C5A 111.5(19) . . ? C3A C4A H4A1 109.3 . . ? C5A C4A H4A1 109.3 . . ? C3A C4A H4A2 109.3 . . ? C5A C4A H4A2 109.3 . . ? H4A1 C4A H4A2 108 . . ? C6A C5A C4A 110.9(19) . . ? C6A C5A H5A1 109.5 . . ? C4A C5A H5A1 109.5 . . ? C6A C5A H5A2 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 108 . . ? C1A C6A C5A 109.2(18) . . ? C1A C6A H6A1 109.8 . . ? C5A C6A H6A1 109.8 . . ? C1A C6A H6A2 109.8 . . ? C5A C6A H6A2 109.8 . . ? H6A1 C6A H6A2 108.3 . . ? C1A N1A H1A1 109.5 . . ? C1A N1A H1A2 109.5 . . ? H1A1 N1A H1A2 109.5 . . ? C1A N1A H1A3 109.5 . . ? H1A1 N1A H1A3 109.5 . . ? H1A2 N1A H1A3 109.5 . . ? C6B C1B C2B 111.6(8) . . ? C6B C1B N1B 109.1(12) . . ? C2B C1B N1B 108.3(13) . . ? C6B C1B H1B 109.3 . . ? C2B C1B H1B 109.3 . . ? N1B C1B H1B 109.3 . . ? C1B C2B C3B 109.9(8) . . ? C1B C2B H2B1 109.7 . . ? C3B C2B H2B1 109.7 . . ? C1B C2B H2B2 109.7 . . ? C3B C2B H2B2 109.7 . . ? H2B1 C2B H2B2 108.2 . . ? C4B C3B C2B 110.4(9) . . ? C4B C3B H3B1 109.6 . . ? C2B C3B H3B1 109.6 . . ? C4B C3B H3B2 109.6 . . ? C2B C3B H3B2 109.6 . . ? H3B1 C3B H3B2 108.1 . . ? C3B C4B C5B 111.2(9) . . ? C3B C4B H4B1 109.4 . . ? C5B C4B H4B1 109.4 . . ? C3B C4B H4B2 109.4 . . ? C5B C4B H4B2 109.4 . . ? H4B1 C4B H4B2 108 . . ? C6B C5B C4B 111.9(9) . . ? C6B C5B H5B1 109.2 . . ? C4B C5B H5B1 109.2 . . ? C6B C5B H5B2 109.2 . . ? C4B C5B H5B2 109.2 . . ? H5B1 C5B H5B2 107.9 . . ? C5B C6B C1B 110.2(8) . . ? C5B C6B H6B1 109.6 . . ? C1B C6B H6B1 109.6 . . ? C5B C6B H6B2 109.6 . . ? C1B C6B H6B2 109.6 . . ? H6B1 C6B H6B2 108.1 . . ? C1B N1B H1B1 109.5 . . ? C1B N1B H1B2 109.5 . . ? H1B1 N1B H1B2 109.5 . . ? C1B N1B H1B3 109.5 . . ? H1B1 N1B H1B3 109.5 . . ? H1B2 N1B H1B3 109.5 . . ? I1 Pb1 I1 180 . 5_656 ? I1 Pb1 I2 90.026(10) . 4_456 ? I1 Pb1 I2 89.974(10) 5_656 4_456 ? I1 Pb1 I2 89.974(10) . 8_755 ? I1 Pb1 I2 90.026(10) 5_656 8_755 ? I2 Pb1 I2 180 4_456 8_755 ? I1 Pb1 I2 85.742(10) . . ? I1 Pb1 I2 94.258(10) 5_656 . ? I2 Pb1 I2 92.748(12) 4_456 . ? I2 Pb1 I2 87.252(12) 8_755 . ? I1 Pb1 I2 94.258(10) . 5_656 ? I1 Pb1 I2 85.742(10) 5_656 5_656 ? I2 Pb1 I2 87.252(12) 4_456 5_656 ? I2 Pb1 I2 92.748(12) 8_755 5_656 ? I2 Pb1 I2 180 . 5_656 ? Pb1 I2 Pb1 154.792(12) 4_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A C1A C2A C3A -176(2) . . . . ? C6A C1A C2A C3A -56(3) . . . . ? C1A C2A C3A C4A 55(3) . . . . ? C2A C3A C4A C5A -56(3) . . . . ? C3A C4A C5A C6A 58(3) . . . . ? N1A C1A C6A C5A 177(3) . . . . ? C2A C1A C6A C5A 57(3) . . . . ? C4A C5A C6A C1A -57(3) . . . . ? C6B C1B C2B C3B 57.9(11) . . . . ? N1B C1B C2B C3B 178.1(11) . . . . ? C1B C2B C3B C4B -57.7(12) . . . . ? C2B C3B C4B C5B 56.7(13) . . . . ? C3B C4B C5B C6B -55.5(13) . . . . ? C4B C5B C6B C1B 54.4(12) . . . . ? C2B C1B C6B C5B -56.0(11) . . . . ? N1B C1B C6B C5B -175.6(13) . . . . ? I1 Pb1 I2 Pb1 -82.69(3) . . . 4_556 ? I1 Pb1 I2 Pb1 97.31(3) 5_656 . . 4_556 ? I2 Pb1 I2 Pb1 7.13(2) 4_456 . . 4_556 ? I2 Pb1 I2 Pb1 -172.87(2) 8_755 . . 4_556 ? 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 N1A H1A1 I1 0.91 2.85 3.75(6) 169.4 1_455 N1A H1A2 I1 0.91 2.51 3.38(5) 161 8_655 N1A H1A3 I2 0.91 2.87 3.56(6) 133.5 5_656 N1B H1B1 I2 0.91 3.06 3.69(3) 128 1_455 N1B H1B2 I1 0.91 2.65 3.51(3) 157.9 1_455 N1B H1B3 I1 0.91 2.83 3.72(2) 165.9 8_655 _chemical_name_common bis(cyclohexylammonium)tetraiodoplumbate(ii) ###END data_5 _database_code_depnum_ccdc_archive 'CCDC 609996' _audit_creation_date 2006-05-04T15:28:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; tris(cycloheptylammonium)pentaiodoplumbate(II) ; _chemical_formula_sum 'C21 H48 I5 N3 Pb' _chemical_formula_moiety '3(C7 H16 N), I5 Pb' _chemical_formula_weight 1184.31 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.587(5) _cell_length_b 8.7821(12) _cell_length_c 26.662(3) _cell_angle_alpha 90 _cell_angle_beta 124.255(2) _cell_angle_gamma 90 _cell_volume 6693.8(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 949 _cell_measurement_theta_min 3.155 _cell_measurement_theta_max 28.269 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 2.35 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 0 1 0.085 1 0 -1 0.085 1 0 0 0.21 -1 0 0 0.21 0 0 1 0.19 -1 1 1 0.2 1 -1 -1 0.2 -3 -3 -2 0.21 1 0 -2 0.14 1 -1 1 0.22 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 9.666 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0531 _exptl_absorpt_correction_T_max 0.2309 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_unetI/netI 0.0638 _diffrn_reflns_number 21787 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_full 28 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 8054 _reflns_number_gt 6809 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+25.8359P] 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 8054 _refine_ls_number_parameters 271 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.087 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.563 _refine_diff_density_min -2.307 _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 0.6286(2) 0.1552(7) 1.0818(2) 0.0313(12) Uani 1 1 d DU . . H1 H 0.6401 0.051 1.0816 0.038 Uiso 1 1 calc R . . C2 C 0.6014(2) 0.1428(8) 1.1111(3) 0.0426(15) Uani 1 1 d DU . . H2E H 0.5841 0.0451 1.0983 0.051 Uiso 1 1 calc R . . H2D H 0.6243 0.138 1.1557 0.051 Uiso 1 1 calc R . . C3 C 0.5667(2) 0.2696(8) 1.0973(3) 0.0441(15) Uani 1 1 d DU . . H3E H 0.5799 0.3675 1.0952 0.053 Uiso 1 1 calc R . . H3D H 0.5625 0.2767 1.131 0.053 Uiso 1 1 calc R . . C4 C 0.5190(2) 0.2458(11) 1.0379(3) 0.0555(19) Uani 1 1 d DU . . H4A H 0.5073 0.1441 1.0393 0.067 Uiso 1 1 calc R . . H4B H 0.4971 0.3221 1.036 0.067 Uiso 1 1 calc R . . C5 C 0.5166(3) 0.2565(11) 0.9791(3) 0.060(2) Uani 1 1 d DU . . H5A H 0.4848 0.2257 0.9451 0.072 Uiso 1 1 calc R . . H5B H 0.5209 0.3645 0.9725 0.072 Uiso 1 1 calc R . . C6 C 0.5520(2) 0.1611(10) 0.9762(3) 0.0491(16) Uani 1 1 d DU . . H6A H 0.5431 0.1604 0.9338 0.059 Uiso 1 1 calc R . . H6B H 0.5503 0.0549 0.9873 0.059 Uiso 1 1 calc R . . C7 C 0.60242(19) 0.2160(8) 1.0174(2) 0.0346(13) Uani 1 1 d DU . . H7A H 0.6196 0.1857 0.9992 0.042 Uiso 1 1 calc R . . H7B H 0.6024 0.3286 1.0189 0.042 Uiso 1 1 calc R . . C8 C 0.6322(2) 0.6992(6) 0.9312(3) 0.0299(11) Uani 1 1 d DU . . H8 H 0.6402 0.6903 0.9734 0.036 Uiso 1 1 calc R . . C9 C 0.6011(2) 0.8384(7) 0.9011(3) 0.0406(14) Uani 1 1 d DU . . H9A H 0.6172 0.9276 0.9275 0.049 Uiso 1 1 calc R . . H9B H 0.5981 0.8571 0.8624 0.049 Uiso 1 1 calc R . . C10 C 0.5525(2) 0.8296(10) 0.8878(4) 0.0537(17) Uani 1 1 d DU . . H10A H 0.5552 0.7941 0.9249 0.064 Uiso 1 1 calc R . . H10B H 0.5393 0.9337 0.879 0.064 Uiso 1 1 calc R . . C11 C 0.5182(3) 0.7277(8) 0.8360(3) 0.0540(18) Uani 1 1 d DU . . H11A H 0.522 0.7436 0.8023 0.065 Uiso 1 1 calc R . . H11B H 0.4862 0.7608 0.8217 0.065 Uiso 1 1 calc R . . C12 C 0.5221(2) 0.5596(8) 0.8493(3) 0.0542(18) Uani 1 1 d DU . . H12A H 0.512 0.5044 0.8114 0.065 Uiso 1 1 calc R . . H12B H 0.4996 0.5341 0.8597 0.065 Uiso 1 1 calc R . . C13 C 0.5695(2) 0.4979(8) 0.8991(3) 0.0439(15) Uani 1 1 d DU . . H13A H 0.5681 0.3853 0.8968 0.053 Uiso 1 1 calc R . . H13B H 0.5753 0.527 0.9387 0.053 Uiso 1 1 calc R . . C14 C 0.6110(2) 0.5503(7) 0.8982(3) 0.0382(13) Uani 1 1 d DU . . H14A H 0.6354 0.4704 0.917 0.046 Uiso 1 1 calc R . . H14B H 0.6009 0.5617 0.8555 0.046 Uiso 1 1 calc R . . C15 C 0.6384(3) 0.2449(10) 0.7574(3) 0.0582(18) Uani 1 1 d DU . . H15 H 0.6464 0.137 0.7548 0.07 Uiso 1 1 calc R . . C16 C 0.6510(3) 0.2721(8) 0.8204(3) 0.0516(16) Uani 1 1 d DU . . H16A H 0.6852 0.2596 0.849 0.062 Uiso 1 1 calc R . . H16B H 0.6435 0.3793 0.8231 0.062 Uiso 1 1 calc R . . C17 C 0.6276(3) 0.1721(10) 0.8410(4) 0.0626(19) Uani 1 1 d DU . . H17A H 0.6368 0.0653 0.8413 0.075 Uiso 1 1 calc R . . H17B H 0.6392 0.1997 0.8833 0.075 Uiso 1 1 calc R . . C18 C 0.5754(3) 0.1809(11) 0.8033(4) 0.070(2) Uani 1 1 d DU . . H18A H 0.5661 0.2893 0.7945 0.083 Uiso 1 1 calc R . . H18B H 0.5639 0.1401 0.8272 0.083 Uiso 1 1 calc R . . C19 C 0.5519(4) 0.0952(14) 0.7438(5) 0.087(3) Uani 1 1 d DU . . H19A H 0.5641 -0.0103 0.7535 0.104 Uiso 1 1 calc R . . H19B H 0.5182 0.0891 0.7276 0.104 Uiso 1 1 calc R . . C20 C 0.5549(4) 0.1443(15) 0.6974(4) 0.100(4) Uani 1 1 d DU . . H20A H 0.5232 0.1764 0.6638 0.12 Uiso 1 1 calc R . . H20B H 0.5633 0.0549 0.6827 0.12 Uiso 1 1 calc R . . C21 C 0.5879(3) 0.2707(14) 0.7075(4) 0.089(3) Uani 1 1 d DU . . H21A H 0.5856 0.2878 0.6692 0.107 Uiso 1 1 calc R . . H21B H 0.5774 0.3651 0.7166 0.107 Uiso 1 1 calc R . . N1 N 0.6708(2) 0.2557(7) 1.1195(3) 0.0398(13) Uani 1 1 d U . . H1A H 0.6868 0.2617 1.1018 0.06 Uiso 1 1 calc R . . H1B H 0.6896 0.2157 1.1574 0.06 Uiso 1 1 calc R . . H1C H 0.6614 0.3505 1.1221 0.06 Uiso 1 1 calc R . . N2 N 0.67601(19) 0.7281(6) 0.9342(2) 0.0325(11) Uani 1 1 d U . . H2C H 0.6889 0.8177 0.9537 0.049 Uiso 1 1 calc R . . H2B H 0.6692 0.7331 0.896 0.049 Uiso 1 1 calc R . . H2A H 0.6966 0.651 0.9548 0.049 Uiso 1 1 calc R . . N3 N 0.6684(3) 0.3470(8) 0.7474(4) 0.069(2) Uani 1 1 d U . . H3A H 0.699 0.333 0.7778 0.103 Uiso 1 1 calc R . . H3B H 0.6604 0.4459 0.7471 0.103 Uiso 1 1 calc R . . H3C H 0.6639 0.3241 0.7112 0.103 Uiso 1 1 calc R . . I1 I 0.775131(14) 0.50976(4) 0.937797(18) 0.02877(9) Uani 1 1 d . . . I2 I 0.647903(14) 0.72547(5) 0.781042(18) 0.03077(9) Uani 1 1 d . . . I3 I 0.762710(15) 1.02281(5) 0.934656(18) 0.03171(10) Uani 1 1 d . . . I4 I 0.870314(14) 0.82813(5) 0.912880(18) 0.03159(10) Uani 1 1 d . . . I5 I 0.736582(13) 1.03122(4) 0.744437(17) 0.02619(9) Uani 1 1 d . . . Pb1 Pb 0.760923(7) 0.77530(2) 0.852357(9) 0.02318(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(3) 0.028(3) 0.030(3) -0.001(2) 0.014(2) 0.001(2) C2 0.042(3) 0.051(4) 0.036(3) 0.005(3) 0.022(3) 0.000(3) C3 0.047(3) 0.051(4) 0.040(3) 0.001(3) 0.029(3) 0.003(3) C4 0.039(3) 0.069(5) 0.055(4) 0.005(4) 0.024(3) 0.000(3) C5 0.034(3) 0.087(6) 0.042(3) 0.003(4) 0.012(3) 0.000(4) C6 0.045(3) 0.063(5) 0.025(3) -0.009(3) 0.012(2) -0.014(3) C7 0.036(3) 0.036(3) 0.030(3) 0.000(3) 0.018(2) -0.003(3) C8 0.033(3) 0.029(3) 0.026(3) 0.003(2) 0.015(2) -0.002(2) C9 0.039(3) 0.025(3) 0.047(4) 0.001(3) 0.018(3) 0.000(2) C10 0.047(3) 0.052(4) 0.056(4) 0.003(4) 0.025(3) 0.007(3) C11 0.038(3) 0.070(4) 0.041(4) 0.011(3) 0.014(3) -0.005(3) C12 0.040(3) 0.064(4) 0.047(4) -0.013(4) 0.018(3) -0.013(3) C13 0.052(3) 0.039(3) 0.037(4) -0.001(3) 0.023(3) -0.014(3) C14 0.043(3) 0.026(3) 0.041(4) -0.006(3) 0.021(3) -0.004(2) C15 0.065(4) 0.049(4) 0.088(5) -0.016(4) 0.059(4) -0.015(4) C16 0.044(4) 0.030(3) 0.051(3) 0.004(3) 0.009(3) -0.008(3) C17 0.100(5) 0.036(4) 0.055(4) 0.001(4) 0.045(4) -0.004(4) C18 0.097(5) 0.062(5) 0.090(5) -0.024(5) 0.077(5) -0.025(5) C19 0.092(6) 0.104(7) 0.098(5) -0.044(5) 0.073(5) -0.057(6) C20 0.101(6) 0.119(8) 0.041(4) -0.015(5) 0.016(5) -0.073(6) C21 0.083(4) 0.120(8) 0.044(4) 0.006(5) 0.024(4) -0.049(5) N1 0.030(3) 0.040(3) 0.036(3) 0.000(3) 0.011(2) -0.001(2) N2 0.032(2) 0.038(3) 0.024(2) -0.002(2) 0.014(2) -0.001(2) N3 0.084(5) 0.038(4) 0.126(7) -0.019(4) 0.084(5) -0.013(4) I1 0.0352(2) 0.02328(18) 0.02837(19) 0.00358(15) 0.01826(17) 0.00081(15) I2 0.0310(2) 0.0311(2) 0.02642(19) 0.00087(16) 0.01389(17) 0.00189(15) I3 0.0403(2) 0.02628(19) 0.0282(2) -0.00181(16) 0.01900(18) 0.00518(16) I4 0.0303(2) 0.0315(2) 0.0311(2) -0.00288(17) 0.01611(17) -0.00248(16) I5 0.03026(18) 0.02375(18) 0.02421(18) 0.00486(14) 0.01512(16) 0.00244(14) Pb1 0.02823(11) 0.02091(10) 0.02112(11) -0.00001(8) 0.01433(9) -0.00089(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.506(8) . ? C1 C7 1.518(6) . ? C1 C2 1.527(6) . ? C1 H1 1 . ? C2 C3 1.522(6) . ? C2 H2E 0.99 . ? C2 H2D 0.99 . ? C3 C4 1.528(6) . ? C3 H3E 0.99 . ? C3 H3D 0.99 . ? C4 C5 1.524(7) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.522(7) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.523(6) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 N2 1.492(8) . ? C8 C14 1.515(6) . ? C8 C9 1.524(6) . ? C8 H8 1 . ? C9 C10 1.515(6) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.505(6) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.506(7) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.515(6) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.521(6) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 C16 1.498(7) . ? C15 C21 1.502(7) . ? C15 N3 1.503(10) . ? C15 H15 1 . ? C16 C17 1.495(7) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.492(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.513(7) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.370(13) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.504(7) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? N2 H2C 0.91 . ? N2 H2B 0.91 . ? N2 H2A 0.91 . ? N3 H3A 0.91 . ? N3 H3B 0.91 . ? N3 H3C 0.91 . ? I1 Pb1 3.0999(5) . ? I2 Pb1 3.2741(6) . ? I3 Pb1 3.0644(5) . ? I4 Pb1 3.2033(6) . ? I5 Pb1 3.3634(5) . ? I5 Pb1 3.3931(5) 4_656 ? Pb1 I5 3.3931(5) 4_646 ? 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 C7 106.6(5) . . ? N1 C1 C2 110.2(5) . . ? C7 C1 C2 117.2(5) . . ? N1 C1 H1 107.5 . . ? C7 C1 H1 107.5 . . ? C2 C1 H1 107.5 . . ? C3 C2 C1 116.8(6) . . ? C3 C2 H2E 108.1 . . ? C1 C2 H2E 108.1 . . ? C3 C2 H2D 108.1 . . ? C1 C2 H2D 108.1 . . ? H2E C2 H2D 107.3 . . ? C2 C3 C4 113.3(6) . . ? C2 C3 H3E 108.9 . . ? C4 C3 H3E 108.9 . . ? C2 C3 H3D 108.9 . . ? C4 C3 H3D 108.9 . . ? H3E C3 H3D 107.7 . . ? C5 C4 C3 117.3(6) . . ? C5 C4 H4A 108 . . ? C3 C4 H4A 108 . . ? C5 C4 H4B 108 . . ? C3 C4 H4B 108 . . ? H4A C4 H4B 107.2 . . ? C6 C5 C4 116.0(7) . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 114.6(6) . . ? C5 C6 H6A 108.6 . . ? C7 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? C7 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C1 C7 C6 114.6(5) . . ? C1 C7 H7A 108.6 . . ? C6 C7 H7A 108.6 . . ? C1 C7 H7B 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? N2 C8 C14 108.9(5) . . ? N2 C8 C9 106.6(5) . . ? C14 C8 C9 114.8(5) . . ? N2 C8 H8 108.8 . . ? C14 C8 H8 108.8 . . ? C9 C8 H8 108.8 . . ? C10 C9 C8 116.3(6) . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? C8 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 116.2(6) . . ? C11 C10 H10A 108.2 . . ? C9 C10 H10A 108.2 . . ? C11 C10 H10B 108.2 . . ? C9 C10 H10B 108.2 . . ? H10A C10 H10B 107.4 . . ? C10 C11 C12 116.6(7) . . ? C10 C11 H11A 108.1 . . ? C12 C11 H11A 108.1 . . ? C10 C11 H11B 108.1 . . ? C12 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C11 C12 C13 117.8(6) . . ? C11 C12 H12A 107.9 . . ? C13 C12 H12A 107.9 . . ? C11 C12 H12B 107.9 . . ? C13 C12 H12B 107.9 . . ? H12A C12 H12B 107.2 . . ? C12 C13 C14 116.3(6) . . ? C12 C13 H13A 108.2 . . ? C14 C13 H13A 108.2 . . ? C12 C13 H13B 108.2 . . ? C14 C13 H13B 108.2 . . ? H13A C13 H13B 107.4 . . ? C8 C14 C13 113.9(5) . . ? C8 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? C8 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C21 115.3(7) . . ? C16 C15 N3 108.0(7) . . ? C21 C15 N3 109.1(7) . . ? C16 C15 H15 108.1 . . ? C21 C15 H15 108.1 . . ? N3 C15 H15 108.1 . . ? C17 C16 C15 116.4(6) . . ? C17 C16 H16A 108.2 . . ? C15 C16 H16A 108.2 . . ? C17 C16 H16B 108.2 . . ? C15 C16 H16B 108.2 . . ? H16A C16 H16B 107.3 . . ? C18 C17 C16 114.9(7) . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17B 108.5 . . ? C16 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C17 C18 C19 114.5(8) . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18B 108.6 . . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C20 C19 C18 121.3(8) . . ? C20 C19 H19A 107 . . ? C18 C19 H19A 107 . . ? C20 C19 H19B 107 . . ? C18 C19 H19B 107 . . ? H19A C19 H19B 106.7 . . ? C19 C20 C21 120.5(9) . . ? C19 C20 H20A 107.2 . . ? C21 C20 H20A 107.2 . . ? C19 C20 H20B 107.2 . . ? C21 C20 H20B 107.2 . . ? H20A C20 H20B 106.8 . . ? C15 C21 C20 115.8(9) . . ? C15 C21 H21A 108.3 . . ? C20 C21 H21A 108.3 . . ? C15 C21 H21B 108.3 . . ? C20 C21 H21B 108.3 . . ? H21A C21 H21B 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 . . ? C8 N2 H2C 109.5 . . ? C8 N2 H2B 109.5 . . ? H2C N2 H2B 109.5 . . ? C8 N2 H2A 109.5 . . ? H2C N2 H2A 109.5 . . ? H2B N2 H2A 109.5 . . ? C15 N3 H3A 109.5 . . ? C15 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C15 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Pb1 I5 Pb1 166.299(13) . 4_656 ? I3 Pb1 I1 94.385(16) . . ? I3 Pb1 I4 89.685(13) . . ? I1 Pb1 I4 94.878(12) . . ? I3 Pb1 I2 92.690(13) . . ? I1 Pb1 I2 88.270(12) . . ? I4 Pb1 I2 175.904(12) . . ? I3 Pb1 I5 91.895(16) . . ? I1 Pb1 I5 172.397(12) . . ? I4 Pb1 I5 89.431(11) . . ? I2 Pb1 I5 87.157(11) . . ? I3 Pb1 I5 173.625(12) . 4_646 ? I1 Pb1 I5 91.277(15) . 4_646 ? I4 Pb1 I5 86.913(12) . 4_646 ? I2 Pb1 I5 90.404(12) . 4_646 ? I5 Pb1 I5 82.689(12) . 4_646 ? 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 84.0(7) . . . . ? C7 C1 C2 C3 -38.0(9) . . . . ? C1 C2 C3 C4 84.3(8) . . . . ? C2 C3 C4 C5 -67.9(10) . . . . ? C3 C4 C5 C6 50.8(12) . . . . ? C4 C5 C6 C7 -69.8(10) . . . . ? N1 C1 C7 C6 -163.0(6) . . . . ? C2 C1 C7 C6 -39.1(9) . . . . ? C5 C6 C7 C1 86.4(8) . . . . ? N2 C8 C9 C10 174.7(6) . . . . ? C14 C8 C9 C10 54.1(8) . . . . ? C8 C9 C10 C11 -73.2(9) . . . . ? C9 C10 C11 C12 79.7(10) . . . . ? C10 C11 C12 C13 -27.1(11) . . . . ? C11 C12 C13 C14 -46.5(10) . . . . ? N2 C8 C14 C13 172.6(5) . . . . ? C9 C8 C14 C13 -68.0(8) . . . . ? C12 C13 C14 C8 86.7(8) . . . . ? C21 C15 C16 C17 62.3(11) . . . . ? N3 C15 C16 C17 -175.4(7) . . . . ? C15 C16 C17 C18 -59.5(11) . . . . ? C16 C17 C18 C19 77.1(11) . . . . ? C17 C18 C19 C20 -69.8(17) . . . . ? C18 C19 C20 C21 10(2) . . . . ? C16 C15 C21 C20 -79.0(13) . . . . ? N3 C15 C21 C20 159.2(10) . . . . ? C19 C20 C21 C15 57(2) . . . . ? Pb1 I5 Pb1 I3 106.06(6) 4_656 . . . ? Pb1 I5 Pb1 I4 16.40(6) 4_656 . . . ? Pb1 I5 Pb1 I2 -161.34(6) 4_656 . . . ? Pb1 I5 Pb1 I5 -70.56(6) 4_656 . . 4_646 ? 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 I3 0.91 3.08 3.860(6) 145 7_667 N1 H1B I5 0.91 2.91 3.753(6) 154.4 6_566 N1 H1C I4 0.91 2.98 3.839(6) 158 7_667 N2 H2C I1 0.91 2.86 3.648(5) 146.3 7_667 N2 H2B I2 0.91 2.72 3.627(5) 175.8 . N2 H2A I3 0.91 2.88 3.637(6) 140.9 7_667 N3 H3A I5 0.91 3.14 3.558(6) 110.5 4_646 N3 H3B I2 0.91 2.73 3.615(7) 163.4 . N3 H3C I4 0.91 2.82 3.693(9) 161.9 4_646 _chemical_name_common tris(cycloheptylammonium)pentaiodoplumbate(ii) ###END data_6 _database_code_depnum_ccdc_archive 'CCDC 609997' _audit_creation_date 2005-10-26T12:02:12-00:00 _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 ; (cyclooctylammonium)triiodoplumbate(II) ; _chemical_formula_sum 'C8 H18 I3 N Pb' _chemical_formula_moiety 'C8 H18 N, I3 Pb' _chemical_formula_weight 716.12 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.9889(12) _cell_length_b 8.6291(13) _cell_length_c 22.455(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1548.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2.529 _cell_measurement_theta_max 28.253 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rectangular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 3.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 -1 0.025 0 1 1 0.025 0 0 -1 0.055 0 0 1 0.055 -1 0 0 0.15 1 0 0 0.15 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.851 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0487 _exptl_absorpt_correction_T_max 0.4598 _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 1999)' _exptl_special_details ; Numerical integration absorption corrections based on indexed crystal faces were applied using the XPREP routine (Bruker, 1999) ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_unetI/netI 0.0648 _diffrn_reflns_number 15336 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_full 27.99 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 3743 _reflns_number_gt 3313 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART-NT (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT+ (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT+ (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2002) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 3743 _refine_ls_number_parameters 119 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.049 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), 1580 Friedel Pairs' _refine_ls_abs_structure_Flack 0.286(9) _refine_diff_density_max 2.136 _refine_diff_density_min -2.3 _refine_diff_density_rms 0.3 #----------------------------------------------------------------------------# # 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 0.8265(10) 0.3153(14) 0.8711(4) 0.030(2) Uani 1 1 d DU . . H1 H 0.8732 0.4181 0.8832 0.037 Uiso 1 1 calc R . . C2 C 0.9346(12) 0.2523(15) 0.8210(4) 0.036(2) Uani 1 1 d DU . . H2A H 1.0459 0.2256 0.8375 0.043 Uiso 1 1 calc R . . H2B H 0.8834 0.1552 0.8062 0.043 Uiso 1 1 calc R . . C3 C 0.9592(15) 0.3609(19) 0.7688(5) 0.056(3) Uani 1 1 d DU . . H3A H 1.0089 0.4578 0.7844 0.067 Uiso 1 1 calc R . . H3B H 1.0434 0.3134 0.7421 0.067 Uiso 1 1 calc R . . C4 C 0.8105(15) 0.4055(17) 0.7310(6) 0.070(4) Uani 1 1 d DU . . H4A H 0.8527 0.4457 0.6925 0.084 Uiso 1 1 calc R . . H4B H 0.7511 0.4916 0.751 0.084 Uiso 1 1 calc R . . C5 C 0.6844(14) 0.2782(18) 0.7180(5) 0.064(3) Uani 1 1 d DU . . H5A H 0.6498 0.2882 0.6758 0.076 Uiso 1 1 calc R . . H5B H 0.7427 0.1775 0.722 0.076 Uiso 1 1 calc R . . C6 C 0.5268(13) 0.271(2) 0.7556(5) 0.061(4) Uani 1 1 d DU . . H6A H 0.4482 0.1977 0.7366 0.073 Uiso 1 1 calc R . . H6B H 0.4734 0.3748 0.7548 0.073 Uiso 1 1 calc R . . C7 C 0.5482(16) 0.2238(18) 0.8203(5) 0.059(4) Uani 1 1 d DU . . H7A H 0.4356 0.2063 0.8374 0.07 Uiso 1 1 calc R . . H7B H 0.6079 0.1233 0.8212 0.07 Uiso 1 1 calc R . . C8 C 0.6409(10) 0.3354(16) 0.8604(5) 0.045(3) Uani 1 1 d DU . . H8A H 0.624 0.4408 0.8441 0.054 Uiso 1 1 calc R . . H8B H 0.5851 0.3328 0.8998 0.054 Uiso 1 1 calc R . . N1 N 0.8468(12) 0.2040(12) 0.9238(4) 0.036(2) Uani 1 1 d U . . H1A H 0.9575 0.1916 0.9321 0.054 Uiso 1 1 calc R . . H1B H 0.8011 0.1106 0.9144 0.054 Uiso 1 1 calc R . . H1C H 0.7939 0.2438 0.9563 0.054 Uiso 1 1 calc R . . I1 I 0.77423(8) 0.79183(8) 0.88832(3) 0.02684(16) Uani 1 1 d . . . I2 I 0.25737(9) 1.02159(7) 0.95537(3) 0.02664(15) Uani 1 1 d . . . I3 I 0.23571(9) 0.50604(7) 0.93755(3) 0.02778(16) Uani 1 1 d . . . Pb1 Pb 0.51441(4) 0.74980(6) 0.998017(19) 0.02417(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.028(4) 0.037(6) 0.027(4) 0.000(4) 0.004(3) 0.004(4) C2 0.030(4) 0.044(7) 0.034(4) -0.007(5) 0.005(4) 0.002(5) C3 0.062(7) 0.070(9) 0.036(6) 0.005(6) 0.014(5) -0.005(6) C4 0.077(8) 0.074(9) 0.059(8) 0.030(7) 0.002(6) -0.008(6) C5 0.083(7) 0.074(9) 0.034(5) 0.002(7) -0.008(4) 0.002(6) C6 0.065(6) 0.072(10) 0.045(5) 0.008(7) -0.019(5) -0.010(7) C7 0.048(6) 0.081(10) 0.047(5) 0.016(7) -0.011(4) -0.015(7) C8 0.032(4) 0.071(8) 0.032(5) 0.002(5) 0.001(4) 0.016(5) N1 0.051(5) 0.030(6) 0.027(4) -0.004(4) -0.003(4) 0.012(4) I1 0.0343(3) 0.0216(3) 0.0246(3) -0.0006(3) -0.0010(3) 0.0007(3) I2 0.0313(3) 0.0169(3) 0.0317(3) 0.0027(2) -0.0013(3) -0.0002(3) I3 0.0289(3) 0.0213(3) 0.0332(3) -0.0055(3) -0.0016(3) 0.0023(3) Pb1 0.02254(16) 0.0180(2) 0.0320(2) 0.00053(16) -0.00010(14) -0.00046(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C8 1.512(7) . ? C1 C2 1.518(7) . ? C1 N1 1.533(13) . ? C1 H1 1 . ? C2 C3 1.515(8) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 C4 1.510(8) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? C4 C5 1.519(8) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 C6 1.517(8) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 C7 1.519(8) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C8 1.513(8) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? N1 H1A 0.91 . ? N1 H1B 0.91 . ? N1 H1C 0.91 . ? I1 Pb1 3.2131(8) 4_567 ? I1 Pb1 3.2415(8) . ? I2 Pb1 3.2167(8) 4_467 ? I2 Pb1 3.2610(8) . ? I3 Pb1 3.1078(8) 4_467 ? I3 Pb1 3.3505(9) . ? Pb1 I3 3.1078(8) 4_567 ? Pb1 I1 3.2131(8) 4_467 ? Pb1 I2 3.2167(8) 4_567 ? 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 C8 C1 C2 118.8(9) . . ? C8 C1 N1 107.3(9) . . ? C2 C1 N1 106.7(8) . . ? C8 C1 H1 107.9 . . ? C2 C1 H1 107.9 . . ? N1 C1 H1 107.9 . . ? C3 C2 C1 115.2(10) . . ? 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 . . ? C4 C3 C2 119.4(10) . . ? C4 C3 H3A 107.5 . . ? C2 C3 H3A 107.5 . . ? C4 C3 H3B 107.5 . . ? C2 C3 H3B 107.5 . . ? H3A C3 H3B 107 . . ? C3 C4 C5 116.4(12) . . ? C3 C4 H4A 108.2 . . ? C5 C4 H4A 108.2 . . ? C3 C4 H4B 108.2 . . ? C5 C4 H4B 108.2 . . ? H4A C4 H4B 107.3 . . ? C6 C5 C4 118.2(12) . . ? C6 C5 H5A 107.8 . . ? C4 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? C4 C5 H5B 107.8 . . ? H5A C5 H5B 107.1 . . ? C5 C6 C7 116.7(10) . . ? C5 C6 H6A 108.1 . . ? C7 C6 H6A 108.1 . . ? C5 C6 H6B 108.1 . . ? C7 C6 H6B 108.1 . . ? H6A C6 H6B 107.3 . . ? C8 C7 C6 116.9(13) . . ? C8 C7 H7A 108.1 . . ? C6 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? C6 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C1 C8 C7 120.1(10) . . ? C1 C8 H8A 107.3 . . ? C7 C8 H8A 107.3 . . ? C1 C8 H8B 107.3 . . ? C7 C8 H8B 107.3 . . ? H8A C8 H8B 106.9 . . ? C1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pb1 I1 Pb1 76.485(17) 4_567 . ? Pb1 I2 Pb1 76.162(17) 4_467 . ? Pb1 I3 Pb1 76.334(17) 4_467 . ? I3 Pb1 I1 92.62(2) 4_567 4_467 ? I3 Pb1 I2 89.93(2) 4_567 4_567 ? I1 Pb1 I2 91.17(2) 4_467 4_567 ? I3 Pb1 I1 85.05(2) 4_567 . ? I1 Pb1 I1 176.83(2) 4_467 . ? I2 Pb1 I1 86.692(19) 4_567 . ? I3 Pb1 I2 90.42(2) 4_567 . ? I1 Pb1 I2 86.424(19) 4_467 . ? I2 Pb1 I2 177.59(2) 4_567 . ? I1 Pb1 I2 95.72(2) . . ? I3 Pb1 I3 172.91(2) 4_567 . ? I1 Pb1 I3 81.66(2) 4_467 . ? I2 Pb1 I3 94.35(2) 4_567 . ? I1 Pb1 I3 100.83(2) . . ? I2 Pb1 I3 85.07(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 C1 C2 C3 70.0(15) . . . . ? N1 C1 C2 C3 -168.7(10) . . . . ? C1 C2 C3 C4 -65.1(17) . . . . ? C2 C3 C4 C5 -39(2) . . . . ? C3 C4 C5 C6 98.7(16) . . . . ? C4 C5 C6 C7 -70(2) . . . . ? C5 C6 C7 C8 68(2) . . . . ? C2 C1 C8 C7 33.5(17) . . . . ? N1 C1 C8 C7 -87.5(13) . . . . ? C6 C7 C8 C1 -94.9(16) . . . . ? Pb1 I1 Pb1 I3 47.542(18) 4_567 . . 4_567 ? Pb1 I1 Pb1 I2 -42.676(17) 4_567 . . 4_567 ? Pb1 I1 Pb1 I2 137.47(3) 4_567 . . . ? Pb1 I1 Pb1 I3 -136.48(3) 4_567 . . . ? Pb1 I2 Pb1 I3 -135.05(2) 4_467 . . 4_567 ? Pb1 I2 Pb1 I1 -42.448(15) 4_467 . . 4_467 ? Pb1 I2 Pb1 I1 139.89(2) 4_467 . . . ? Pb1 I2 Pb1 I3 39.474(16) 4_467 . . . ? Pb1 I3 Pb1 I1 45.987(16) 4_467 . . 4_467 ? Pb1 I3 Pb1 I2 136.54(2) 4_467 . . 4_567 ? Pb1 I3 Pb1 I1 -136.01(2) 4_467 . . . ? Pb1 I3 Pb1 I2 -41.111(17) 4_467 . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A I2 0.91 2.86 3.706(9) 155.8 1_645 N1 H1B I1 0.91 2.82 3.691(10) 160.5 1_545 N1 H1C I2 0.91 2.85 3.671(9) 150.8 4_567 ###END _chemical_name_common (cyclooctylammonium)triiodoplumbate(ii)