# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1527 data_manuscript loop_ _publ_author_name _publ_author_address 'Harald Krautscheid' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; 'Frieder Vielsack' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author ; 'Dr. Harald Krautscheid' Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude Nr. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author_email 'harald@achibm6.chemie.uni-karlsruhe.de' _publ_contact_author_fax 'Int + 721 661921' _publ_contact_author_phone 'Int + 721 608 2970' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_section_title ; Discrete and polymeric iodoplumbates with Pb3I10 building blocks: [Pb3I10]4-, [Pb7I22]8-, [Pb10I28]8-, 1-dim [Pb3I10]4-, 2-dim [Pb7I18]4- ; data_fv313 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Bu3N-(CH2)4-NBu3]2[Pb3I10]*DMF*0.5Et2O _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C61 H136 I10 N5 O1.5 Pb3' _chemical_formula_weight 2854.32 _chemical_melting_point ? _chemical_compound_source ? 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' 0.0000 0.0000 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1 (No. 2)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3391(9) _cell_length_b 16.9204(10) _cell_length_c 20.6738(14) _cell_angle_alpha 72.963(5) _cell_angle_beta 70.719(5) _cell_angle_gamma 74.467(4) _cell_volume 4754.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 68 _cell_measurement_theta_min '10 deg.' _cell_measurement_theta_max '12.5 deg.' _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method ? _exptl_crystal_F_000 2650 _exptl_absorpt_coefficient_mu 8.578 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE STADI IV' _diffrn_measurement_method 'theta omega scans (1:1)' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% '+/- 2%' _diffrn_reflns_number 19324 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.02 _reflns_number_total 14940 _reflns_number_observed 11658 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 68 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Carbon Atoms C55 and C56 are disordered, refined with split positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+48.1399P] 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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14940 _refine_ls_number_parameters 696 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1071 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.50803(3) 0.80899(3) 0.33659(2) 0.03990(12) Uani 1 d . . . Pb2 Pb 0.49125(3) 0.70487(3) 0.16976(2) 0.04147(12) Uani 1 d . . . Pb3 Pb 0.76063(3) 0.70149(3) 0.19845(3) 0.04611(13) Uani 1 d . . . I1 I 0.59724(6) 0.86569(5) 0.16735(4) 0.0468(2) Uani 1 d . . . I2 I 0.61203(6) 0.60367(5) 0.29210(4) 0.0458(2) Uani 1 d . . . I3 I 0.73071(7) 0.76797(6) 0.33947(5) 0.0546(2) Uani 1 d . . . I4 I 0.33250(6) 0.78119(6) 0.29780(5) 0.0557(2) Uani 1 d . . . I5 I 0.70964(8) 0.66755(6) 0.06735(5) 0.0596(3) Uani 1 d . . . I6 I 0.43400(6) 0.74358(5) 0.49952(4) 0.0497(2) Uani 1 d . . . I7 I 0.44342(6) 0.99677(5) 0.33032(4) 0.0476(2) Uani 1 d . . . I8 I 0.42519(8) 0.53901(6) 0.20539(5) 0.0635(3) Uani 1 d . . . I9 I 0.39167(7) 0.78557(5) 0.05280(5) 0.0533(2) Uani 1 d . . . I10 I 0.94097(10) 0.57245(11) 0.20684(11) 0.1377(7) Uani 1 d . . . N1 N 0.3018(7) 0.5059(5) 0.4764(5) 0.037(2) Uani 1 d . . . C1 C 0.3991(8) 0.5291(7) 0.4569(6) 0.037(3) Uani 1 d . . . H1A H 0.4391 0.5083 0.4151 0.045 Uiso 1 calc R . . H1B H 0.3917 0.5906 0.4446 0.045 Uiso 1 calc R . . C2 C 0.4492(8) 0.4936(7) 0.5154(6) 0.037(3) Uani 1 d . . . H2A H 0.4175 0.5228 0.5539 0.044 Uiso 1 calc R . . H2B H 0.4477 0.4335 0.5341 0.044 Uiso 1 calc R . . C3 C 0.3140(9) 0.4128(7) 0.4790(7) 0.046(3) Uani 1 d . . . H3A H 0.3460 0.3805 0.5153 0.055 Uiso 1 calc R . . H3B H 0.2513 0.3987 0.4943 0.055 Uiso 1 calc R . . C4 C 0.3668(10) 0.3837(8) 0.4129(7) 0.053(3) Uani 1 d . . . H4A H 0.4336 0.3848 0.4025 0.064 Uiso 1 calc R . . H4B H 0.3434 0.4218 0.3738 0.064 Uiso 1 calc R . . C5 C 0.3549(12) 0.2946(9) 0.4204(8) 0.067(4) Uani 1 d . . . H5A H 0.3721 0.2584 0.4627 0.080 Uiso 1 calc R . . H5B H 0.2885 0.2952 0.4271 0.080 Uiso 1 calc R . . C6 C 0.4127(16) 0.2574(11) 0.3589(10) 0.103(7) Uani 1 d . . . H6A H 0.4018 0.2009 0.3671 0.154 Uiso 1 calc R . . H6B H 0.4787 0.2551 0.3526 0.154 Uiso 1 calc R . . H6C H 0.3950 0.2919 0.3169 0.154 Uiso 1 calc R . . C7 C 0.2549(8) 0.5609(7) 0.4195(6) 0.041(3) Uani 1 d . . . H7A H 0.2970 0.5531 0.3736 0.050 Uiso 1 calc R . . H7B H 0.2468 0.6201 0.4205 0.050 Uiso 1 calc R . . C8 C 0.1590(9) 0.5427(9) 0.4270(8) 0.057(4) Uani 1 d . . . H8A H 0.1671 0.4865 0.4190 0.068 Uiso 1 calc R . . H8B H 0.1183 0.5438 0.4747 0.068 Uiso 1 calc R . . C9 C 0.1139(12) 0.6079(12) 0.3742(9) 0.079(5) Uani 1 d . . . H9A H 0.1546 0.6061 0.3266 0.095 Uiso 1 calc R . . H9B H 0.1072 0.6640 0.3818 0.095 Uiso 1 calc R . . C10 C 0.0154(12) 0.5925(13) 0.3806(10) 0.097(6) Uani 1 d . . . H10A H -0.0118 0.6353 0.3461 0.146 Uiso 1 calc R . . H10B H -0.0253 0.5951 0.4275 0.146 Uiso 1 calc R . . H10C H 0.0221 0.5374 0.3723 0.146 Uiso 1 calc R . . C11 C 0.2445(9) 0.5187(8) 0.5493(6) 0.047(3) Uani 1 d . . . H11A H 0.2799 0.4845 0.5829 0.056 Uiso 1 calc R . . H11B H 0.1862 0.4974 0.5618 0.056 Uiso 1 calc R . . C12 C 0.2189(10) 0.6093(9) 0.5576(7) 0.056(3) Uani 1 d . . . H12A H 0.2756 0.6341 0.5395 0.067 Uiso 1 calc R . . H12B H 0.1745 0.6425 0.5304 0.067 Uiso 1 calc R . . C13 C 0.1752(15) 0.6117(12) 0.6341(9) 0.095(6) Uani 1 d . . . H13A H 0.1201 0.5847 0.6525 0.115 Uiso 1 calc R . . H13B H 0.2206 0.5798 0.6609 0.115 Uiso 1 calc R . . C14 C 0.146(2) 0.7000(14) 0.6442(11) 0.150(12) Uani 1 d . . . H14A H 0.1180 0.6993 0.6938 0.224 Uiso 1 calc R . . H14B H 0.1006 0.7316 0.6181 0.224 Uiso 1 calc R . . H14C H 0.2008 0.7264 0.6271 0.224 Uiso 1 calc R . . N2 N 0.7224(6) -0.0077(6) 0.4374(5) 0.039(2) Uani 1 d . . . C15 C 0.6317(8) -0.0421(7) 0.4702(7) 0.040(3) Uani 1 d . . . H15A H 0.6299 -0.0780 0.4413 0.048 Uiso 1 calc R . . H15B H 0.6334 -0.0779 0.5167 0.048 Uiso 1 calc R . . C16 C 0.5414(7) 0.0228(7) 0.4784(6) 0.035(3) Uani 1 d . . . H16A H 0.5326 0.0534 0.4321 0.042 Uiso 1 calc R . . H16B H 0.5443 0.0635 0.5027 0.042 Uiso 1 calc R . . C17 C 0.8050(8) -0.0807(7) 0.4238(7) 0.043(3) Uani 1 d . . . H17A H 0.7926 -0.1107 0.3948 0.051 Uiso 1 calc R . . H17B H 0.8616 -0.0573 0.3965 0.051 Uiso 1 calc R . . C18 C 0.8250(9) -0.1432(8) 0.4882(7) 0.052(3) Uani 1 d . . . H18A H 0.7668 -0.1617 0.5192 0.062 Uiso 1 calc R . . H18B H 0.8477 -0.1162 0.5139 0.062 Uiso 1 calc R . . C19 C 0.8982(11) -0.2190(9) 0.4687(9) 0.069(4) Uani 1 d . . . H19A H 0.8735 -0.2469 0.4450 0.083 Uiso 1 calc R . . H19B H 0.9544 -0.1993 0.4350 0.083 Uiso 1 calc R . . C20 C 0.9267(12) -0.2829(10) 0.5303(10) 0.085(5) Uani 1 d . . . H20A H 0.9734 -0.3292 0.5135 0.128 Uiso 1 calc R . . H20B H 0.8719 -0.3041 0.5634 0.128 Uiso 1 calc R . . H20C H 0.9529 -0.2565 0.5534 0.128 Uiso 1 calc R . . C21 C 0.7212(9) 0.0572(8) 0.3682(7) 0.047(3) Uani 1 d . . . H21A H 0.6693 0.1044 0.3778 0.056 Uiso 1 calc R . . H21B H 0.7799 0.0789 0.3507 0.056 Uiso 1 calc R . . C22 C 0.7106(10) 0.0245(9) 0.3107(7) 0.054(3) Uani 1 d . . . H22A H 0.7668 -0.0168 0.2954 0.065 Uiso 1 calc R . . H22B H 0.6564 -0.0037 0.3292 0.065 Uiso 1 calc R . . C23 C 0.6969(12) 0.0960(10) 0.2491(8) 0.069(4) Uani 1 d . . . H23A H 0.7470 0.1284 0.2347 0.082 Uiso 1 calc R . . H23B H 0.6367 0.1336 0.2634 0.082 Uiso 1 calc R . . C24 C 0.6979(15) 0.0648(13) 0.1864(10) 0.097(6) Uani 1 d . . . H24A H 0.6886 0.1126 0.1480 0.145 Uiso 1 calc R . . H24B H 0.6478 0.0334 0.2002 0.145 Uiso 1 calc R . . H24C H 0.7579 0.0287 0.1713 0.145 Uiso 1 calc R . . C25 C 0.7323(8) 0.0356(8) 0.4888(7) 0.041(3) Uani 1 d . . . H25A H 0.6803 0.0840 0.4934 0.049 Uiso 1 calc R . . H25B H 0.7239 -0.0036 0.5350 0.049 Uiso 1 calc R . . C26 C 0.8234(9) 0.0665(8) 0.4720(7) 0.050(3) Uani 1 d . . . H26A H 0.8767 0.0192 0.4686 0.060 Uiso 1 calc R . . H26B H 0.8328 0.1076 0.4268 0.060 Uiso 1 calc R . . C27 C 0.8172(11) 0.1072(11) 0.5303(8) 0.071(5) Uani 1 d . . . H27A H 0.7692 0.1587 0.5281 0.085 Uiso 1 calc R . . H27B H 0.7954 0.0689 0.5755 0.085 Uiso 1 calc R . . C28 C 0.9065(11) 0.1294(12) 0.5294(9) 0.082(5) Uani 1 d . . . H28A H 0.8943 0.1551 0.5685 0.123 Uiso 1 calc R . . H28B H 0.9283 0.1687 0.4855 0.123 Uiso 1 calc R . . H28C H 0.9543 0.0788 0.5335 0.123 Uiso 1 calc R . . N3 N 0.2814(7) 0.5711(7) 0.0063(6) 0.047(3) Uani 1 d . . . C29 C 0.3811(9) 0.5739(8) 0.0068(7) 0.051(3) Uani 1 d . . . H29A H 0.4053 0.6180 -0.0330 0.061 Uiso 1 calc R . . H29B H 0.3762 0.5898 0.0500 0.061 Uiso 1 calc R . . C30 C 0.4517(8) 0.4921(8) 0.0027(7) 0.048(3) Uani 1 d . . . H30A H 0.4550 0.4731 -0.0387 0.057 Uiso 1 calc R . . H30B H 0.4324 0.4484 0.0447 0.057 Uiso 1 calc R . . C31 C 0.2233(9) 0.6569(8) 0.0177(8) 0.056(4) Uani 1 d . . . H31A H 0.2534 0.7009 -0.0187 0.067 Uiso 1 calc R . . H31B H 0.2234 0.6632 0.0633 0.067 Uiso 1 calc R . . C32 C 0.1194(10) 0.6704(10) 0.0159(9) 0.069(4) Uani 1 d . . . H32A H 0.1174 0.6675 -0.0302 0.083 Uiso 1 calc R . . H32B H 0.0878 0.6270 0.0519 0.083 Uiso 1 calc R . . C33 C 0.0711(13) 0.7573(15) 0.0301(14) 0.121(9) Uani 1 d . . . H33A H 0.0834 0.7641 0.0717 0.145 Uiso 1 calc R . . H33B H 0.0943 0.8013 -0.0102 0.145 Uiso 1 calc R . . C34 C -0.031(3) 0.763(2) 0.042(2) 0.25(2) Uani 1 d . . . H34A H -0.0648 0.8167 0.0526 0.380 Uiso 1 calc R . . H34B H -0.0523 0.7179 0.0816 0.380 Uiso 1 calc R . . H34C H -0.0418 0.7570 0.0004 0.380 Uiso 1 calc R . . C35 C 0.2846(10) 0.5572(8) -0.0633(7) 0.052(3) Uani 1 d . . . H35A H 0.3238 0.5017 -0.0677 0.062 Uiso 1 calc R . . H35B H 0.2207 0.5543 -0.0613 0.062 Uiso 1 calc R . . C36 C 0.3197(12) 0.6186(9) -0.1287(8) 0.067(4) Uani 1 d . . . H36A H 0.3861 0.6179 -0.1352 0.080 Uiso 1 calc R . . H36B H 0.2844 0.6754 -0.1246 0.080 Uiso 1 calc R . . C37 C 0.3091(12) 0.5980(10) -0.1932(9) 0.073(5) Uani 1 d . . . H37A H 0.3389 0.5391 -0.1937 0.088 Uiso 1 calc R . . H37B H 0.2420 0.6035 -0.1879 0.088 Uiso 1 calc R . . C38 C 0.3512(17) 0.6526(13) -0.2630(10) 0.107(7) Uani 1 d . . . H38A H 0.3414 0.6355 -0.3005 0.161 Uiso 1 calc R . . H38B H 0.4181 0.6464 -0.2696 0.161 Uiso 1 calc R . . H38C H 0.3211 0.7110 -0.2637 0.161 Uiso 1 calc R . . C39 C 0.2406(9) 0.5004(9) 0.0637(7) 0.055(3) Uani 1 d . . . H39A H 0.1781 0.5017 0.0600 0.066 Uiso 1 calc R . . H39B H 0.2802 0.4468 0.0543 0.066 Uiso 1 calc R . . C40 C 0.2312(11) 0.5014(12) 0.1375(9) 0.077(5) Uani 1 d . . . H40A H 0.1884 0.5528 0.1493 0.093 Uiso 1 calc R . . H40B H 0.2927 0.5008 0.1426 0.093 Uiso 1 calc R . . C41 C 0.1927(14) 0.4243(12) 0.1870(9) 0.100(7) Uani 1 d . . . H41A H 0.1309 0.4259 0.1820 0.120 Uiso 1 calc R . . H41B H 0.2348 0.3733 0.1737 0.120 Uiso 1 calc R . . C42 C 0.1837(19) 0.420(2) 0.2623(11) 0.154(11) Uani 1 d . . . H42A H 0.1587 0.3709 0.2920 0.232 Uiso 1 calc R . . H42B H 0.1416 0.4705 0.2758 0.232 Uiso 1 calc R . . H42C H 0.2451 0.4171 0.2677 0.232 Uiso 1 calc R . . N4 N 0.3191(7) 0.0732(6) 0.1115(5) 0.042(2) Uani 1 d . . . C43 C 0.4062(9) 0.0100(7) 0.0875(6) 0.042(3) Uani 1 d . . . H43A H 0.3897 -0.0460 0.1023 0.051 Uiso 1 calc R . . H43B H 0.4527 0.0083 0.1112 0.051 Uiso 1 calc R . . C44 C 0.4513(8) 0.0284(8) 0.0083(6) 0.042(3) Uani 1 d . . . H44A H 0.4577 0.0876 -0.0087 0.050 Uiso 1 calc R . . H44B H 0.4113 0.0182 -0.0156 0.050 Uiso 1 calc R . . C45 C 0.3443(9) 0.1577(7) 0.1000(7) 0.047(3) Uani 1 d . . . H45A H 0.3674 0.1796 0.0492 0.056 Uiso 1 calc R . . H45B H 0.2867 0.1966 0.1174 0.056 Uiso 1 calc R . . C46 C 0.4166(11) 0.1584(8) 0.1342(7) 0.055(4) Uani 1 d . . . H46A H 0.4792 0.1332 0.1087 0.066 Uiso 1 calc R . . H46B H 0.4025 0.1255 0.1828 0.066 Uiso 1 calc R . . C47 C 0.4147(13) 0.2496(10) 0.1330(10) 0.078(5) Uani 1 d . . . H47A H 0.4238 0.2829 0.0845 0.094 Uiso 1 calc R . . H47B H 0.3530 0.2732 0.1609 0.094 Uiso 1 calc R . . C48 C 0.4902(14) 0.2557(12) 0.1620(10) 0.094(6) Uani 1 d . . . H48A H 0.4872 0.3142 0.1604 0.141 Uiso 1 calc R . . H48B H 0.5514 0.2332 0.1340 0.141 Uiso 1 calc R . . H48C H 0.4805 0.2237 0.2103 0.141 Uiso 1 calc R . . C49 C 0.2790(9) 0.0377(8) 0.1892(6) 0.048(3) Uani 1 d . . . H49A H 0.3293 0.0236 0.2124 0.057 Uiso 1 calc R . . H49B H 0.2590 -0.0147 0.1945 0.057 Uiso 1 calc R . . C50 C 0.1963(11) 0.0953(10) 0.2273(8) 0.070(4) Uani 1 d . . . H50A H 0.2152 0.1483 0.2223 0.084 Uiso 1 calc R . . H50B H 0.1446 0.1085 0.2057 0.084 Uiso 1 calc R . . C51 C 0.1636(12) 0.0567(13) 0.3019(8) 0.085(5) Uani 1 d . . . H51A H 0.2166 0.0412 0.3225 0.102 Uiso 1 calc R . . H51B H 0.1433 0.0047 0.3063 0.102 Uiso 1 calc R . . C52 C 0.0831(18) 0.1122(17) 0.3442(12) 0.162(13) Uani 1 d . . . H52A H 0.0655 0.0820 0.3929 0.244 Uiso 1 calc R . . H52B H 0.0295 0.1268 0.3252 0.244 Uiso 1 calc R . . H52C H 0.1029 0.1632 0.3416 0.244 Uiso 1 calc R . . C53 C 0.2490(10) 0.0879(9) 0.0704(8) 0.057(4) Uani 1 d . . . H53A H 0.2789 0.1094 0.0206 0.068 Uiso 1 calc R . . H53B H 0.1959 0.1316 0.0861 0.068 Uiso 1 calc R . . C54 C 0.2114(13) 0.0102(11) 0.0772(11) 0.086(5) Uani 1 d . . . H54A H 0.1603 0.0010 0.1205 0.103 Uiso 1 calc R A 1 H54B H 0.2614 -0.0399 0.0781 0.103 Uiso 1 calc R A 1 C55A C 0.172(3) 0.030(2) 0.007(2) 0.097(11) Uiso 0.60 d P B 1 H55A H 0.1224 0.0802 0.0068 0.117 Uiso 0.60 calc PR B 1 H55B H 0.2237 0.0407 -0.0359 0.117 Uiso 0.60 calc PR B 1 C56A C 0.136(3) -0.042(2) 0.009(2) 0.120(13) Uiso 0.60 d P B 1 H56A H 0.1136 -0.0311 -0.0326 0.180 Uiso 0.60 calc PR B 1 H56B H 0.0843 -0.0521 0.0507 0.180 Uiso 0.60 calc PR B 1 H56C H 0.1856 -0.0919 0.0088 0.180 Uiso 0.60 calc PR B 1 C55B C 0.132(3) 0.028(3) 0.046(2) 0.076(12) Uiso 0.40 d P B 2 H55C H 0.0877 0.0796 0.0566 0.091 Uiso 0.40 calc PR B 2 H55D H 0.0981 -0.0188 0.0635 0.091 Uiso 0.40 calc PR B 2 C56B C 0.186(6) 0.040(6) -0.040(4) 0.18(4) Uiso 0.40 d P B 2 H56D H 0.1392 0.0535 -0.0659 0.269 Uiso 0.40 calc PR B 2 H56E H 0.2290 -0.0115 -0.0490 0.269 Uiso 0.40 calc PR B 2 H56F H 0.2205 0.0858 -0.0555 0.269 Uiso 0.40 calc PR B 2 O1 O 0.0026(15) 0.9368(14) 0.2918(11) 0.167(7) Uiso 1 d . . . C57 C 0.0628(18) 0.8766(15) 0.2711(13) 0.116(7) Uiso 1 d . . . H57 H 0.1180 0.8612 0.2858 0.139 Uiso 1 calc R . . N5 N 0.0555(13) 0.8335(11) 0.2311(9) 0.104(5) Uiso 1 d . . . C58 C 0.1314(18) 0.7752(16) 0.2019(13) 0.130(8) Uiso 1 d . . . H58A H 0.1122 0.7501 0.1735 0.195 Uiso 1 calc R . . H58B H 0.1516 0.7316 0.2394 0.195 Uiso 1 calc R . . H58C H 0.1830 0.8037 0.1727 0.195 Uiso 1 calc R . . C59 C -0.033(2) 0.8525(18) 0.2095(15) 0.155(11) Uiso 1 d . . . H59A H -0.0276 0.8154 0.1797 0.233 Uiso 1 calc R . . H59B H -0.0435 0.9105 0.1836 0.233 Uiso 1 calc R . . H59C H -0.0856 0.8437 0.2509 0.233 Uiso 1 calc R . . C60 C -0.062(3) 0.175(3) 0.184(2) 0.105(13) Uiso 0.50 d P . . H60A H -0.0419 0.1173 0.1792 0.157 Uiso 0.50 calc PR . . H60B H -0.1170 0.2010 0.1668 0.157 Uiso 0.50 calc PR . . H60C H -0.0761 0.1772 0.2326 0.157 Uiso 0.50 calc PR . . C61 C 0.010(2) 0.219(2) 0.1442(18) 0.071(9) Uiso 0.50 d P . . H61A H 0.0664 0.1918 0.1603 0.086 Uiso 0.50 calc PR . . H61B H 0.0247 0.2167 0.0948 0.086 Uiso 0.50 calc PR . . O2 O -0.014(4) 0.296(3) 0.150(3) 0.185(17) Uiso 0.50 d P . . C62 C 0.046(5) 0.331(5) 0.101(4) 0.19(3) Uiso 0.50 d P . . H62A H 0.0993 0.3326 0.1169 0.226 Uiso 0.50 calc PR . . H62B H 0.0688 0.3055 0.0607 0.226 Uiso 0.50 calc PR . . C63 C 0.006(4) 0.388(3) 0.092(3) 0.116(15) Uiso 0.50 d P . . H63A H 0.0434 0.4251 0.0540 0.174 Uiso 0.50 calc PR . . H63B H -0.0167 0.4101 0.1337 0.174 Uiso 0.50 calc PR . . H63C H -0.0464 0.3834 0.0778 0.174 Uiso 0.50 calc PR . . 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 Pb1 0.0448(3) 0.0422(3) 0.0360(2) -0.0129(2) -0.0114(2) -0.0086(2) Pb2 0.0487(3) 0.0418(3) 0.0397(3) -0.0118(2) -0.0165(2) -0.0097(2) Pb3 0.0398(3) 0.0502(3) 0.0464(3) -0.0100(2) -0.0115(2) -0.0069(2) I1 0.0590(5) 0.0404(4) 0.0382(4) -0.0058(3) -0.0164(4) -0.0043(4) I2 0.0560(5) 0.0466(5) 0.0374(4) -0.0038(3) -0.0182(4) -0.0134(4) I3 0.0642(6) 0.0611(5) 0.0526(5) -0.0146(4) -0.0246(5) -0.0221(5) I4 0.0459(5) 0.0611(6) 0.0634(6) -0.0184(4) -0.0138(4) -0.0118(4) I5 0.0856(7) 0.0513(5) 0.0422(5) -0.0185(4) -0.0120(5) -0.0116(5) I6 0.0602(5) 0.0418(4) 0.0425(5) -0.0099(4) -0.0102(4) -0.0066(4) I7 0.0543(5) 0.0463(5) 0.0442(5) -0.0148(4) -0.0117(4) -0.0097(4) I8 0.0853(7) 0.0567(6) 0.0640(6) -0.0053(5) -0.0345(5) -0.0299(5) I9 0.0667(6) 0.0476(5) 0.0537(5) -0.0071(4) -0.0294(5) -0.0124(4) I10 0.0591(8) 0.1214(13) 0.1752(17) 0.0017(11) -0.0217(9) 0.0244(8) N1 0.039(5) 0.029(5) 0.042(5) -0.002(4) -0.008(4) -0.013(4) C1 0.029(6) 0.041(6) 0.044(7) -0.005(5) -0.016(5) -0.010(5) C2 0.038(7) 0.034(6) 0.037(6) -0.006(5) -0.012(5) -0.004(5) C3 0.055(8) 0.037(7) 0.053(8) -0.002(6) -0.021(7) -0.021(6) C4 0.062(9) 0.037(7) 0.060(9) -0.008(6) -0.019(7) -0.009(6) C5 0.077(11) 0.057(9) 0.079(11) -0.018(8) -0.028(9) -0.020(8) C6 0.16(2) 0.057(11) 0.107(15) -0.033(10) -0.040(15) -0.020(12) C7 0.034(7) 0.041(7) 0.042(7) -0.004(5) -0.012(5) -0.001(5) C8 0.044(8) 0.064(9) 0.063(9) -0.009(7) -0.020(7) -0.012(7) C9 0.069(11) 0.097(13) 0.072(11) -0.001(9) -0.037(9) -0.014(9) C10 0.066(11) 0.141(18) 0.105(15) -0.042(13) -0.059(11) 0.008(11) C11 0.034(7) 0.061(8) 0.037(7) -0.009(6) 0.003(5) -0.014(6) C12 0.041(8) 0.065(9) 0.053(8) -0.017(7) -0.003(6) -0.007(7) C13 0.106(15) 0.094(14) 0.060(11) -0.020(10) -0.006(10) 0.008(11) C14 0.20(3) 0.119(19) 0.086(15) -0.056(14) -0.028(17) 0.065(18) N2 0.028(5) 0.046(6) 0.048(6) -0.025(5) -0.005(4) -0.005(4) C15 0.031(6) 0.040(7) 0.050(7) -0.019(6) -0.003(5) -0.008(5) C16 0.033(6) 0.035(6) 0.041(6) -0.016(5) -0.010(5) -0.005(5) C17 0.024(6) 0.048(7) 0.056(8) -0.027(6) 0.004(5) -0.009(5) C18 0.046(8) 0.044(7) 0.070(9) -0.015(7) -0.021(7) -0.007(6) C19 0.055(9) 0.062(9) 0.099(13) -0.044(9) -0.028(9) 0.011(7) C20 0.068(11) 0.050(9) 0.134(17) -0.013(10) -0.037(11) -0.001(8) C21 0.034(7) 0.054(8) 0.056(8) -0.019(6) -0.007(6) -0.014(6) C22 0.045(8) 0.062(9) 0.059(9) -0.026(7) -0.010(7) -0.011(7) C23 0.076(11) 0.072(10) 0.067(10) -0.020(8) -0.018(9) -0.027(9) C24 0.111(16) 0.109(15) 0.081(13) -0.031(11) -0.024(12) -0.031(13) C25 0.031(6) 0.049(7) 0.055(8) -0.025(6) -0.013(6) -0.012(5) C26 0.035(7) 0.044(7) 0.070(9) -0.008(6) -0.013(6) -0.014(6) C27 0.059(9) 0.101(12) 0.072(10) -0.045(9) -0.003(8) -0.037(9) C28 0.058(10) 0.115(15) 0.093(13) -0.047(11) -0.011(9) -0.034(10) N3 0.039(6) 0.057(7) 0.056(7) -0.031(5) -0.019(5) 0.002(5) C29 0.049(8) 0.054(8) 0.062(9) -0.026(7) -0.023(7) -0.009(6) C30 0.040(7) 0.052(8) 0.059(8) -0.024(6) -0.017(6) -0.004(6) C31 0.039(7) 0.051(8) 0.089(11) -0.031(8) -0.029(7) 0.008(6) C32 0.054(9) 0.074(10) 0.085(11) -0.028(9) -0.024(8) -0.005(8) C33 0.056(12) 0.15(2) 0.18(2) -0.098(18) -0.051(14) 0.044(12) C34 0.20(4) 0.20(4) 0.24(4) -0.06(3) 0.03(3) 0.06(3) C35 0.056(8) 0.046(8) 0.070(9) -0.031(7) -0.025(7) -0.007(6) C36 0.076(11) 0.061(9) 0.073(10) -0.031(8) -0.027(9) -0.002(8) C37 0.079(11) 0.067(10) 0.085(12) -0.030(9) -0.037(10) 0.000(9) C38 0.15(2) 0.104(16) 0.076(13) -0.014(11) -0.032(13) -0.037(14) C39 0.036(7) 0.059(9) 0.067(9) -0.020(7) -0.007(7) -0.008(6) C40 0.041(9) 0.111(14) 0.079(12) -0.030(10) -0.013(8) -0.008(9) C41 0.089(14) 0.094(14) 0.065(11) -0.005(10) -0.007(10) 0.035(11) C42 0.13(2) 0.25(3) 0.063(13) -0.007(17) -0.014(14) -0.05(2) N4 0.042(6) 0.036(5) 0.042(6) -0.007(4) -0.012(5) 0.000(4) C43 0.045(7) 0.036(6) 0.037(7) -0.005(5) -0.013(6) 0.007(5) C44 0.043(7) 0.046(7) 0.033(6) -0.011(5) -0.012(6) -0.001(6) C45 0.057(8) 0.030(6) 0.047(7) -0.007(5) -0.014(6) 0.000(6) C46 0.075(10) 0.048(8) 0.042(7) -0.006(6) -0.013(7) -0.023(7) C47 0.085(12) 0.065(10) 0.098(13) -0.026(9) -0.030(10) -0.020(9) C48 0.115(16) 0.100(14) 0.087(13) -0.033(11) -0.024(12) -0.046(12) C49 0.053(8) 0.043(7) 0.040(7) -0.008(6) -0.007(6) -0.008(6) C50 0.065(10) 0.078(11) 0.059(9) -0.023(8) -0.017(8) 0.010(8) C51 0.055(10) 0.129(16) 0.054(10) -0.029(10) 0.006(8) -0.008(10) C52 0.15(2) 0.17(2) 0.091(16) -0.057(17) 0.043(16) 0.027(19) C53 0.055(9) 0.055(8) 0.060(9) -0.014(7) -0.028(7) 0.007(7) C54 0.077(12) 0.074(11) 0.123(16) -0.020(11) -0.055(12) -0.011(9) _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 Pb1 I7 3.0415(10) . ? Pb1 I6 3.1342(10) . ? Pb1 I4 3.2310(10) . ? Pb1 I1 3.2572(9) . ? Pb1 I3 3.3156(11) . ? Pb1 I2 3.6600(10) . ? Pb2 I8 3.0437(10) . ? Pb2 I9 3.0710(10) . ? Pb2 I4 3.2660(11) . ? Pb2 I5 3.3271(12) . ? Pb2 I2 3.4087(9) . ? Pb2 I1 3.5054(10) . ? Pb3 I2 2.9853(10) . ? Pb3 I10 3.0512(14) . ? Pb3 I1 3.2714(10) . ? Pb3 I3 3.2768(10) . ? Pb3 I5 3.2924(11) . ? N1 C11 1.518(15) . ? N1 C3 1.522(14) . ? N1 C7 1.525(14) . ? N1 C1 1.539(14) . ? C1 C2 1.535(15) . ? C2 C2 1.52(2) 2_666 ? C3 C4 1.488(18) . ? C4 C5 1.525(18) . ? C5 C6 1.49(2) . ? C7 C8 1.534(17) . ? C8 C9 1.507(19) . ? C9 C10 1.56(2) . ? C11 C12 1.524(18) . ? C12 C13 1.51(2) . ? C13 C14 1.50(3) . ? N2 C25 1.521(14) . ? N2 C15 1.522(14) . ? N2 C21 1.529(16) . ? N2 C17 1.529(14) . ? C15 C16 1.514(15) . ? C16 C16 1.54(2) 2_656 ? C17 C18 1.502(18) . ? C18 C19 1.516(17) . ? C19 C20 1.51(2) . ? C21 C22 1.519(17) . ? C22 C23 1.51(2) . ? C23 C24 1.53(2) . ? C25 C26 1.520(15) . ? C26 C27 1.520(18) . ? C27 C28 1.507(19) . ? N3 C35 1.508(16) . ? N3 C39 1.520(17) . ? N3 C31 1.525(15) . ? N3 C29 1.546(15) . ? C29 C30 1.516(17) . ? C30 C30 1.54(2) 2_665 ? C31 C32 1.560(18) . ? C32 C33 1.52(2) . ? C33 C34 1.48(4) . ? C35 C36 1.48(2) . ? C36 C37 1.54(2) . ? C37 C38 1.51(2) . ? C39 C40 1.49(2) . ? C40 C41 1.53(2) . ? C41 C42 1.50(3) . ? N4 C53 1.510(16) . ? N4 C43 1.511(14) . ? N4 C45 1.512(15) . ? N4 C49 1.516(15) . ? C43 C44 1.525(16) . ? C44 C44 1.54(2) 2_655 ? C45 C46 1.504(18) . ? C46 C47 1.528(19) . ? C47 C48 1.51(2) . ? C49 C50 1.519(18) . ? C50 C51 1.46(2) . ? C51 C52 1.52(2) . ? C53 C54 1.53(2) . ? C54 C55B 1.48(5) . ? C54 C55A 1.66(4) . ? C55A C56A 1.46(5) . ? C55B C56B 1.68(9) . ? O1 C57 1.25(3) . ? C57 N5 1.30(3) . ? N5 C58 1.40(3) . ? N5 C59 1.49(3) . ? C60 C61 1.38(5) . ? C61 O2 1.29(5) . ? C61 C62 1.99(8) . ? O2 C62 1.24(7) . ? C62 C63 0.99(7) . ? 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 I7 Pb1 I6 98.30(3) . . ? I7 Pb1 I4 97.24(3) . . ? I6 Pb1 I4 96.13(3) . . ? I7 Pb1 I1 85.09(2) . . ? I6 Pb1 I1 175.96(3) . . ? I4 Pb1 I1 85.58(3) . . ? I7 Pb1 I3 104.89(3) . . ? I6 Pb1 I3 93.52(3) . . ? I4 Pb1 I3 154.27(3) . . ? I1 Pb1 I3 83.45(3) . . ? I7 Pb1 I2 164.21(3) . . ? I6 Pb1 I2 97.48(2) . . ? I4 Pb1 I2 81.64(2) . . ? I1 Pb1 I2 79.12(2) . . ? I3 Pb1 I2 73.47(2) . . ? I8 Pb2 I9 93.48(3) . . ? I8 Pb2 I4 96.37(3) . . ? I9 Pb2 I4 99.08(3) . . ? I8 Pb2 I5 103.71(3) . . ? I9 Pb2 I5 97.78(3) . . ? I4 Pb2 I5 152.83(3) . . ? I8 Pb2 I2 84.37(3) . . ? I9 Pb2 I2 175.47(3) . . ? I4 Pb2 I2 85.13(2) . . ? I5 Pb2 I2 78.92(2) . . ? I8 Pb2 I1 163.71(3) . . ? I9 Pb2 I1 102.81(2) . . ? I4 Pb2 I1 81.14(2) . . ? I5 Pb2 I1 74.44(2) . . ? I2 Pb2 I1 79.39(2) . . ? I2 Pb3 I10 102.26(4) . . ? I2 Pb3 I1 89.68(3) . . ? I10 Pb3 I1 168.06(4) . . ? I2 Pb3 I3 83.65(3) . . ? I10 Pb3 I3 97.41(5) . . ? I1 Pb3 I3 83.84(3) . . ? I2 Pb3 I5 85.85(3) . . ? I10 Pb3 I5 102.44(5) . . ? I1 Pb3 I5 78.10(3) . . ? I3 Pb3 I5 159.12(3) . . ? I2 Pb3 Pb1 57.02(2) . . ? I10 Pb3 Pb1 139.28(4) . . ? I1 Pb3 Pb1 48.730(17) . . ? I3 Pb3 Pb1 49.749(19) . . ? I5 Pb3 Pb1 109.56(2) . . ? Pb1 I1 Pb3 82.26(2) . . ? Pb1 I1 Pb2 81.33(2) . . ? Pb3 I1 Pb2 79.73(2) . . ? Pb3 I2 Pb2 85.41(2) . . ? Pb3 I2 Pb1 79.80(2) . . ? Pb2 I2 Pb1 77.13(2) . . ? Pb3 I3 Pb1 81.29(2) . . ? Pb1 I4 Pb2 85.52(2) . . ? Pb3 I5 Pb2 82.11(2) . . ? C11 N1 C3 106.5(9) . . ? C11 N1 C7 112.3(9) . . ? C3 N1 C7 111.3(9) . . ? C11 N1 C1 110.9(9) . . ? C3 N1 C1 109.4(9) . . ? C7 N1 C1 106.5(8) . . ? C2 C1 N1 114.2(9) . . ? C2 C2 C1 108.4(11) 2_666 . ? C4 C3 N1 117.3(10) . . ? C3 C4 C5 110.3(11) . . ? C6 C5 C4 113.9(14) . . ? N1 C7 C8 114.4(10) . . ? C9 C8 C7 109.6(12) . . ? C8 C9 C10 111.3(14) . . ? N1 C11 C12 115.5(10) . . ? C13 C12 C11 110.0(12) . . ? C14 C13 C12 111.6(16) . . ? C25 N2 C15 107.7(8) . . ? C25 N2 C21 108.1(9) . . ? C15 N2 C21 112.1(9) . . ? C25 N2 C17 110.9(9) . . ? C15 N2 C17 108.9(8) . . ? C21 N2 C17 109.2(9) . . ? C16 C15 N2 116.0(9) . . ? C15 C16 C16 108.6(11) . 2_656 ? C18 C17 N2 115.7(10) . . ? C17 C18 C19 111.1(12) . . ? C20 C19 C18 114.5(14) . . ? C22 C21 N2 115.1(10) . . ? C23 C22 C21 110.4(11) . . ? C22 C23 C24 112.1(14) . . ? C26 C25 N2 117.8(10) . . ? C27 C26 C25 108.5(11) . . ? C28 C27 C26 116.6(13) . . ? C35 N3 C39 107.6(10) . . ? C35 N3 C31 111.8(10) . . ? C39 N3 C31 111.0(10) . . ? C35 N3 C29 109.9(10) . . ? C39 N3 C29 112.2(10) . . ? C31 N3 C29 104.3(9) . . ? C30 C29 N3 115.1(10) . . ? C29 C30 C30 108.3(13) . 2_665 ? N3 C31 C32 113.7(11) . . ? C33 C32 C31 106.9(13) . . ? C34 C33 C32 106(2) . . ? C36 C35 N3 119.0(11) . . ? C35 C36 C37 111.2(13) . . ? C38 C37 C36 114.9(15) . . ? C40 C39 N3 116.9(12) . . ? C39 C40 C41 109.3(15) . . ? C42 C41 C40 112(2) . . ? C53 N4 C43 112.0(10) . . ? C53 N4 C45 106.2(9) . . ? C43 N4 C45 110.4(9) . . ? C53 N4 C49 111.9(10) . . ? C43 N4 C49 105.8(8) . . ? C45 N4 C49 110.7(9) . . ? N4 C43 C44 114.3(9) . . ? C43 C44 C44 109.7(12) . 2_655 ? C46 C45 N4 116.1(10) . . ? C45 C46 C47 108.5(12) . . ? C48 C47 C46 111.5(15) . . ? N4 C49 C50 115.5(10) . . ? C51 C50 C49 111.6(13) . . ? C50 C51 C52 114.7(17) . . ? N4 C53 C54 114.7(11) . . ? C55B C54 C53 114(2) . . ? C55B C54 C55A 30.3(19) . . ? C53 C54 C55A 105.6(18) . . ? C56A C55A C54 109(3) . . ? C54 C55B C56B 103(4) . . ? O1 C57 N5 126(3) . . ? C57 N5 C58 122(2) . . ? C57 N5 C59 119(2) . . ? C58 N5 C59 119(2) . . ? O2 C61 C60 111(4) . . ? O2 C61 C62 37(3) . . ? C60 C61 C62 146(4) . . ? C62 O2 C61 104(6) . . ? C63 C62 O2 98(8) . . ? C63 C62 C61 130(8) . . ? O2 C62 C61 39(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.907 _refine_diff_density_min -3.451 _refine_diff_density_rms 0.180 #===END data_311neu _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Bu3N-(CH2)4-NBu3]4[Pb7I22] _chemical_formula_sum 'C112 H248 I22 N8 Pb7' _chemical_formula_weight 5949.31 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' 0.0000 0.0000 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n, No. 14' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.730(2) _cell_length_b 26.823(3) _cell_length_c 20.496(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.870(10) _cell_angle_gamma 90.00 _cell_volume 8847.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5432 _exptl_absorpt_coefficient_mu 10.511 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2057 _exptl_absorpt_correction_T_max 0.3208 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32340 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.00 _reflns_number_total 13110 _reflns_number_gt 9337 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992)' _computing_publication_material ? _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. Carbon atoms C47, C48, C56 have been refined with a reduced site occupation factor (0.6 instead of 1.0). Restraints i(DFIX) have been used for the atoms C44, C47, C48 and C56 in three butyl groups. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13110 _refine_ls_number_parameters 393 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.53320(2) 0.245107(16) 0.033097(19) 0.05232(11) Uani 1 d . . . Pb2 Pb 0.42416(3) 0.249217(15) 0.202199(19) 0.05087(11) Uani 1 d . . . Pb3 Pb 0.47381(2) 0.109056(14) 0.123807(19) 0.04760(10) Uani 1 d . . . Pb4 Pb 0.5000 0.0000 0.0000 0.06002(16) Uani 1 d S . . I1 I 0.35168(4) 0.19433(2) 0.05421(3) 0.04997(16) Uani 1 d . . . I2 I 0.60668(4) 0.19417(3) 0.18213(3) 0.05293(17) Uani 1 d . . . I3 I 0.52476(5) 0.11893(3) -0.01951(4) 0.06010(19) Uani 1 d . . . I4 I 0.48089(5) 0.33334(3) 0.11183(4) 0.0684(2) Uani 1 d . . . I5 I 0.42653(5) 0.13321(4) 0.26298(4) 0.0740(2) Uani 1 d . . . I6 I 0.71055(5) 0.28238(4) 0.04741(4) 0.0792(3) Uani 1 d . . . I7 I 0.45625(5) 0.28520(4) -0.11120(4) 0.0780(3) Uani 1 d . . . I8 I 0.48897(5) 0.30204(4) 0.34024(4) 0.0832(3) Uani 1 d . . . I9 I 0.24664(5) 0.28564(3) 0.18252(4) 0.0666(2) Uani 1 d . . . I10 I 0.59724(6) 0.01361(4) 0.15722(5) 0.0932(3) Uani 1 d . . . I11 I 0.33729(6) 0.03144(3) 0.04295(6) 0.0857(3) Uani 1 d . . . N1 N 0.6908(6) 0.1620(3) 0.4378(4) 0.061(2) Uani 1 d . . . N2 N 0.7548(6) 0.3581(4) 0.2861(4) 0.062(2) Uani 1 d . . . C1 C 0.7347(7) 0.2102(4) 0.4307(5) 0.052(2) Uiso 1 d . . . H1A H 0.7271 0.2338 0.4650 0.063 Uiso 1 calc R . . H1B H 0.7944 0.2035 0.4401 0.063 Uiso 1 calc R . . C2 C 0.7047(7) 0.2342(4) 0.3616(5) 0.059(3) Uiso 1 d . . . H2A H 0.6438 0.2351 0.3477 0.071 Uiso 1 calc R . . H2B H 0.7231 0.2145 0.3282 0.071 Uiso 1 calc R . . C3 C 0.7388(7) 0.2871(4) 0.3637(5) 0.056(2) Uiso 1 d . . . H3A H 0.7168 0.3076 0.3944 0.067 Uiso 1 calc R . . H3B H 0.7995 0.2865 0.3808 0.067 Uiso 1 calc R . . C4 C 0.7140(7) 0.3090(4) 0.2939(5) 0.057(3) Uiso 1 d . . . H4A H 0.6536 0.3139 0.2804 0.069 Uiso 1 calc R . . H4B H 0.7270 0.2849 0.2624 0.069 Uiso 1 calc R . . C5 C 0.6000(8) 0.1717(5) 0.4372(7) 0.077(3) Uiso 1 d . . . H5A H 0.5703 0.1842 0.3921 0.093 Uiso 1 calc R . . H5B H 0.5747 0.1398 0.4435 0.093 Uiso 1 calc R . . C6 C 0.5863(9) 0.2063(5) 0.4872(7) 0.080(4) Uiso 1 d . . . H6A H 0.5996 0.2403 0.4759 0.097 Uiso 1 calc R . . H6B H 0.6226 0.1979 0.5321 0.097 Uiso 1 calc R . . C7 C 0.4925(12) 0.2035(8) 0.4883(10) 0.125(6) Uiso 1 d . . . H7A H 0.4570 0.2068 0.4418 0.150 Uiso 1 calc R . . H7B H 0.4820 0.1706 0.5050 0.150 Uiso 1 calc R . . C8 C 0.4707(18) 0.2393(11) 0.5279(14) 0.180(10) Uiso 1 d . . . H8A H 0.4126 0.2354 0.5264 0.270 Uiso 1 calc R . . H8B H 0.4794 0.2720 0.5110 0.270 Uiso 1 calc R . . H8C H 0.5046 0.2358 0.5743 0.270 Uiso 1 calc R . . C9 C 0.7392(8) 0.1405(5) 0.5058(6) 0.076(3) Uiso 1 d . . . H9A H 0.7435 0.1661 0.5407 0.091 Uiso 1 calc R . . H9B H 0.7958 0.1329 0.5036 0.091 Uiso 1 calc R . . C10 C 0.7019(11) 0.0929(7) 0.5284(9) 0.106(5) Uiso 1 d . . . H10A H 0.6476 0.1005 0.5353 0.127 Uiso 1 calc R . . H10B H 0.6940 0.0674 0.4928 0.127 Uiso 1 calc R . . C11 C 0.7595(13) 0.0730(8) 0.5937(10) 0.126(6) Uiso 1 d . . . H11A H 0.7819 0.1008 0.6243 0.152 Uiso 1 calc R . . H11B H 0.7286 0.0510 0.6163 0.152 Uiso 1 calc R . . C12 C 0.8222(16) 0.0475(10) 0.5793(12) 0.158(8) Uiso 1 d . . . H12A H 0.8592 0.0348 0.6210 0.237 Uiso 1 calc R . . H12B H 0.8529 0.0696 0.5574 0.237 Uiso 1 calc R . . H12C H 0.7997 0.0200 0.5493 0.237 Uiso 1 calc R . . C13 C 0.6906(9) 0.1264(5) 0.3806(7) 0.082(4) Uiso 1 d . . . H13A H 0.6608 0.0962 0.3874 0.099 Uiso 1 calc R . . H13B H 0.6581 0.1417 0.3382 0.099 Uiso 1 calc R . . C14 C 0.7676(10) 0.1116(6) 0.3714(8) 0.095(4) Uiso 1 d . . . H14A H 0.7962 0.0897 0.4088 0.114 Uiso 1 calc R . . H14B H 0.8024 0.1411 0.3722 0.114 Uiso 1 calc R . . C15 C 0.7559(13) 0.0833(8) 0.3022(10) 0.131(6) Uiso 1 d . . . H15A H 0.7188 0.0549 0.3013 0.157 Uiso 1 calc R . . H15B H 0.7280 0.1058 0.2653 0.157 Uiso 1 calc R . . C16 C 0.8324(16) 0.0650(10) 0.2887(13) 0.168(9) Uiso 1 d . . . H16A H 0.8190 0.0483 0.2451 0.252 Uiso 1 calc R . . H16B H 0.8598 0.0418 0.3240 0.252 Uiso 1 calc R . . H16C H 0.8692 0.0929 0.2882 0.252 Uiso 1 calc R . . C17 C 0.7142(8) 0.3746(5) 0.2151(6) 0.077(3) Uiso 1 d . . . H17A H 0.7164 0.3470 0.1843 0.092 Uiso 1 calc R . . H17B H 0.6555 0.3815 0.2110 0.092 Uiso 1 calc R . . C18 C 0.7516(13) 0.4192(8) 0.1929(10) 0.125(6) Uiso 1 d . . . H18A H 0.8096 0.4123 0.1943 0.150 Uiso 1 calc R . . H18B H 0.7507 0.4471 0.2236 0.150 Uiso 1 calc R . . C19 C 0.7026(18) 0.4333(11) 0.1203(14) 0.182(10) Uiso 1 d . . . H19A H 0.6534 0.4530 0.1207 0.218 Uiso 1 calc R . . H19B H 0.6846 0.4033 0.0929 0.218 Uiso 1 calc R . . C20 C 0.765(2) 0.4651(15) 0.0904(19) 0.260(17) Uiso 1 d . . . H20A H 0.7368 0.4753 0.0444 0.390 Uiso 1 calc R . . H20B H 0.8129 0.4450 0.0903 0.390 Uiso 1 calc R . . H20C H 0.7823 0.4945 0.1183 0.390 Uiso 1 calc R . . C21 C 0.7412(10) 0.3970(6) 0.3361(8) 0.094(4) Uiso 1 d . . . H21A H 0.7676 0.3849 0.3820 0.113 Uiso 1 calc R . . H21B H 0.7704 0.4275 0.3296 0.113 Uiso 1 calc R . . C22 C 0.6545(15) 0.4104(10) 0.3323(12) 0.150(8) Uiso 1 d . . . H22A H 0.6220 0.3795 0.3256 0.180 Uiso 1 calc R . . H22B H 0.6333 0.4307 0.2915 0.180 Uiso 1 calc R . . C23 C 0.6353(17) 0.4393(10) 0.3934(13) 0.165(9) Uiso 1 d . . . H23A H 0.5783 0.4338 0.3960 0.198 Uiso 1 calc R . . H23B H 0.6748 0.4311 0.4370 0.198 Uiso 1 calc R . . C24 C 0.647(2) 0.4874(15) 0.3715(19) 0.250(16) Uiso 1 d . . . H24A H 0.6376 0.5115 0.4038 0.374 Uiso 1 calc R . . H24B H 0.6081 0.4933 0.3275 0.374 Uiso 1 calc R . . H24C H 0.7034 0.4906 0.3679 0.374 Uiso 1 calc R . . C25 C 0.8453(9) 0.3525(6) 0.2962(7) 0.087(4) Uiso 1 d . . . H25A H 0.8683 0.3852 0.2902 0.104 Uiso 1 calc R . . H25B H 0.8704 0.3422 0.3432 0.104 Uiso 1 calc R . . C26 C 0.8709(9) 0.3167(6) 0.2511(7) 0.084(4) Uiso 1 d . . . H26A H 0.8383 0.3222 0.2041 0.101 Uiso 1 calc R . . H26B H 0.8611 0.2826 0.2640 0.101 Uiso 1 calc R . . C27 C 0.9632(13) 0.3242(8) 0.2574(11) 0.136(7) Uiso 1 d . . . H27A H 0.9729 0.3579 0.2425 0.163 Uiso 1 calc R . . H27B H 0.9957 0.3202 0.3048 0.163 Uiso 1 calc R . . C28 C 0.9887(18) 0.2864(11) 0.2143(14) 0.186(10) Uiso 1 d . . . H28A H 1.0473 0.2905 0.2174 0.279 Uiso 1 calc R . . H28B H 0.9564 0.2907 0.1675 0.279 Uiso 1 calc R . . H28C H 0.9792 0.2533 0.2296 0.279 Uiso 1 calc R . . N3 N 0.1903(7) 0.1441(4) 0.3355(6) 0.081(3) Uani 1 d . . . N4 N 0.2645(11) 0.3752(4) 0.3993(11) 0.148(8) Uani 1 d . . . C29 C 0.1671(12) 0.1984(7) 0.3475(10) 0.114(5) Uiso 1 d . . . H29A H 0.1228 0.2091 0.3079 0.137 Uiso 1 calc R . . H29B H 0.1439 0.1987 0.3866 0.137 Uiso 1 calc R . . C30 C 0.2315(11) 0.2343(7) 0.3592(9) 0.103(5) Uiso 1 d . . . H30A H 0.2548 0.2338 0.3202 0.123 Uiso 1 calc R . . H30B H 0.2756 0.2236 0.3989 0.123 Uiso 1 calc R . . C31 C 0.2109(11) 0.2860(7) 0.3703(9) 0.105(5) Uiso 1 d . . . H31A H 0.1655 0.2964 0.3313 0.126 Uiso 1 calc R . . H31B H 0.1893 0.2867 0.4102 0.126 Uiso 1 calc R . . C32 C 0.2756(12) 0.3229(7) 0.3802(9) 0.111(5) Uiso 1 d . . . H32A H 0.2922 0.3243 0.3379 0.133 Uiso 1 calc R . . H32B H 0.3234 0.3097 0.4150 0.133 Uiso 1 calc R . . C33 C 0.2025(11) 0.1416(7) 0.2616(9) 0.110(5) Uiso 1 d . . . H33A H 0.2468 0.1653 0.2607 0.132 Uiso 1 calc R . . H33B H 0.2241 0.1083 0.2566 0.132 Uiso 1 calc R . . C34 C 0.1375(12) 0.1505(8) 0.2032(9) 0.115(5) Uiso 1 d . . . H34A H 0.1204 0.1854 0.2033 0.138 Uiso 1 calc R . . H34B H 0.0899 0.1297 0.2050 0.138 Uiso 1 calc R . . C35 C 0.159(2) 0.1400(13) 0.1366(16) 0.199(12) Uiso 1 d . . . H35A H 0.2101 0.1581 0.1386 0.239 Uiso 1 calc R . . H35B H 0.1720 0.1044 0.1368 0.239 Uiso 1 calc R . . C36 C 0.106(2) 0.1499(15) 0.0751(17) 0.232(14) Uiso 1 d . . . H36A H 0.1312 0.1405 0.0398 0.347 Uiso 1 calc R . . H36B H 0.0930 0.1852 0.0717 0.347 Uiso 1 calc R . . H36C H 0.0547 0.1311 0.0698 0.347 Uiso 1 calc R . . C37 C 0.1204(14) 0.1132(8) 0.3383(10) 0.134(7) Uiso 1 d . . . H37A H 0.1242 0.0822 0.3140 0.161 Uiso 1 calc R . . H37B H 0.0698 0.1303 0.3127 0.161 Uiso 1 calc R . . C38 C 0.1087(11) 0.0994(7) 0.4048(9) 0.106(5) Uiso 1 d . . . H38A H 0.1531 0.0763 0.4274 0.128 Uiso 1 calc R . . H38B H 0.1144 0.1294 0.4330 0.128 Uiso 1 calc R . . C39 C 0.0293(18) 0.0764(12) 0.4012(14) 0.187(10) Uiso 1 d . . . H39A H 0.0232 0.0467 0.3724 0.224 Uiso 1 calc R . . H39B H -0.0150 0.0997 0.3793 0.224 Uiso 1 calc R . . C40 C 0.0173(17) 0.0612(11) 0.4691(13) 0.181(10) Uiso 1 d . . . H40A H -0.0370 0.0460 0.4622 0.271 Uiso 1 calc R . . H40B H 0.0212 0.0905 0.4976 0.271 Uiso 1 calc R . . H40C H 0.0600 0.0375 0.4909 0.271 Uiso 1 calc R . . C41 C 0.2693(14) 0.1292(8) 0.3868(11) 0.129(6) Uiso 1 d . . . H41A H 0.3142 0.1510 0.3817 0.155 Uiso 1 calc R . . H41B H 0.2627 0.1346 0.4324 0.155 Uiso 1 calc R . . C42 C 0.2922(15) 0.0805(9) 0.3816(12) 0.148(7) Uiso 1 d D . . H42A H 0.3050 0.0744 0.3384 0.178 Uiso 1 calc R . . H42B H 0.2485 0.0574 0.3859 0.178 Uiso 1 calc R . . C43 C 0.3697(19) 0.0754(14) 0.4413(15) 0.261(17) Uiso 1 d D . . H43A H 0.4073 0.1032 0.4399 0.313 Uiso 1 calc R . . H43B H 0.3532 0.0784 0.4835 0.313 Uiso 1 calc R . . C44 C 0.417(3) 0.0269(18) 0.443(3) 0.41(3) Uiso 1 d D . . H44A H 0.4659 0.0270 0.4813 0.610 Uiso 1 calc R . . H44B H 0.4332 0.0234 0.4013 0.610 Uiso 1 calc R . . H44C H 0.3813 -0.0009 0.4472 0.610 Uiso 1 calc R . . C45 C 0.3380(19) 0.4010(10) 0.3954(16) 0.196(11) Uiso 1 d D . . H45A H 0.3383 0.4026 0.3477 0.235 Uiso 1 calc R . . H45B H 0.3864 0.3813 0.4196 0.235 Uiso 1 calc R . . C46 C 0.348(2) 0.4540(11) 0.4243(17) 0.237(15) Uiso 1 d D . . H46A H 0.3663 0.4524 0.4740 0.284 Uiso 1 calc R . . H46B H 0.2948 0.4712 0.4108 0.284 Uiso 1 calc R . . C47 C 0.413(4) 0.4836(18) 0.399(2) 0.27(3) Uiso 0.60 d PD . . H47A H 0.4458 0.4610 0.3792 0.320 Uiso 0.60 calc PR . . H47B H 0.3847 0.5076 0.3641 0.320 Uiso 0.60 calc PR . . C48 C 0.469(4) 0.511(3) 0.460(3) 0.36(5) Uiso 0.60 d PD . . H48A H 0.5094 0.5306 0.4458 0.541 Uiso 0.60 calc PR . . H48B H 0.4970 0.4868 0.4939 0.541 Uiso 0.60 calc PR . . H48C H 0.4351 0.5327 0.4798 0.541 Uiso 0.60 calc PR . . C49 C 0.2581(11) 0.3747(7) 0.4801(8) 0.105(5) Uiso 1 d . . . H49A H 0.2491 0.4093 0.4918 0.126 Uiso 1 calc R . . H49B H 0.2073 0.3564 0.4799 0.126 Uiso 1 calc R . . C50 C 0.3215(15) 0.3555(10) 0.5340(12) 0.153(8) Uiso 1 d . . . H50A H 0.3739 0.3727 0.5362 0.183 Uiso 1 calc R . . H50B H 0.3291 0.3199 0.5267 0.183 Uiso 1 calc R . . C51 C 0.2989(18) 0.3628(11) 0.5984(13) 0.171(9) Uiso 1 d . . . H51A H 0.2423 0.3507 0.5935 0.206 Uiso 1 calc R . . H51B H 0.3009 0.3983 0.6098 0.206 Uiso 1 calc R . . C52 C 0.360(3) 0.3341(17) 0.654(2) 0.275(18) Uiso 1 d . . . H52A H 0.3455 0.3387 0.6967 0.413 Uiso 1 calc R . . H52B H 0.4157 0.3464 0.6591 0.413 Uiso 1 calc R . . H52C H 0.3572 0.2990 0.6428 0.413 Uiso 1 calc R . . C53 C 0.1873(12) 0.4032(8) 0.3594(9) 0.121(6) Uiso 1 d D . . H53A H 0.1915 0.4372 0.3774 0.145 Uiso 1 calc R . . H53B H 0.1395 0.3877 0.3703 0.145 Uiso 1 calc R . . C54 C 0.164(2) 0.4078(14) 0.2748(17) 0.241(15) Uiso 1 d D . . H54A H 0.2108 0.4211 0.2602 0.290 Uiso 1 calc R . . H54B H 0.1475 0.3755 0.2530 0.290 Uiso 1 calc R . . C55 C 0.091(2) 0.4442(15) 0.2593(15) 0.270(18) Uiso 1 d D . . H55A H 0.0470 0.4306 0.2772 0.323 Uiso 1 calc R . . H55B H 0.1095 0.4758 0.2827 0.323 Uiso 1 calc R . . C56 C 0.056(5) 0.454(4) 0.1839(19) 0.46(7) Uiso 0.60 d PD . . H56A H 0.0052 0.4736 0.1765 0.687 Uiso 0.60 calc PR . . H56B H 0.0442 0.4231 0.1596 0.687 Uiso 0.60 calc PR . . H56C H 0.0963 0.4731 0.1675 0.687 Uiso 0.60 calc PR . . 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 Pb1 0.0519(2) 0.0613(3) 0.0434(2) -0.00141(18) 0.01247(18) -0.0067(2) Pb2 0.0550(2) 0.0535(2) 0.0448(2) -0.00363(18) 0.01477(19) 0.00789(19) Pb3 0.0532(2) 0.0390(2) 0.0496(2) -0.00523(17) 0.01218(18) 0.00227(18) Pb4 0.0631(4) 0.0450(3) 0.0677(4) -0.0184(3) 0.0109(3) -0.0006(3) I1 0.0518(4) 0.0495(4) 0.0435(3) 0.0003(3) 0.0045(3) 0.0076(3) I2 0.0541(4) 0.0563(4) 0.0422(3) -0.0039(3) 0.0026(3) -0.0044(3) I3 0.0668(5) 0.0626(4) 0.0555(4) -0.0131(3) 0.0245(4) -0.0039(4) I4 0.0762(5) 0.0487(4) 0.0752(5) -0.0067(4) 0.0122(4) -0.0015(4) I5 0.0743(5) 0.0972(6) 0.0570(4) 0.0069(4) 0.0290(4) -0.0007(5) I6 0.0608(5) 0.1125(7) 0.0640(5) -0.0047(5) 0.0165(4) -0.0210(5) I7 0.0565(4) 0.1158(7) 0.0572(4) 0.0211(5) 0.0082(4) -0.0112(5) I8 0.0565(4) 0.1255(8) 0.0629(5) -0.0347(5) 0.0088(4) 0.0124(5) I9 0.0624(4) 0.0795(5) 0.0601(4) 0.0002(4) 0.0203(4) 0.0146(4) I10 0.0957(7) 0.0677(6) 0.0884(6) -0.0236(5) -0.0218(5) 0.0372(5) I11 0.0667(5) 0.0613(5) 0.1286(8) -0.0160(5) 0.0261(6) -0.0189(4) N1 0.068(6) 0.056(6) 0.049(5) -0.005(4) -0.001(5) -0.012(5) N2 0.058(5) 0.065(6) 0.055(5) -0.002(5) -0.001(5) -0.016(5) N3 0.073(7) 0.059(6) 0.130(9) 0.013(6) 0.061(7) 0.008(5) N4 0.179(14) 0.046(6) 0.30(2) -0.021(9) 0.199(16) 0.001(8) _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 Pb1 I6 3.0680(9) . ? Pb1 I7 3.0787(9) . ? Pb1 I4 3.1216(9) . ? Pb1 I2 3.2643(8) . ? Pb1 I1 3.4617(8) . ? Pb1 I3 3.5430(9) . ? Pb2 I9 3.0467(9) . ? Pb2 I8 3.0838(9) . ? Pb2 I4 3.2226(9) . ? Pb2 I1 3.2904(8) . ? Pb2 I5 3.3478(11) . ? Pb2 I2 3.5157(8) . ? Pb3 I1 3.1380(8) . ? Pb3 I2 3.1826(8) . ? Pb3 I11 3.1980(10) . ? Pb3 I5 3.2273(8) . ? Pb3 I10 3.2427(10) . ? Pb3 I3 3.2855(8) . ? Pb4 I11 3.1949(9) . ? Pb4 I11 3.1949(9) 3_655 ? Pb4 I10 3.2089(10) . ? Pb4 I10 3.2089(10) 3_655 ? Pb4 I3 3.2556(8) . ? Pb4 I3 3.2556(8) 3_655 ? N1 C13 1.513(16) . ? N1 C1 1.513(13) . ? N1 C9 1.521(16) . ? N1 C5 1.538(15) . ? N2 C25 1.478(16) . ? N2 C17 1.494(16) . ? N2 C4 1.511(14) . ? N2 C21 1.523(17) . ? C1 C2 1.512(15) . ? C2 C3 1.524(16) . ? C3 C4 1.498(14) . ? C5 C6 1.447(17) . ? C6 C7 1.58(2) . ? C7 C8 1.37(3) . ? C9 C10 1.55(2) . ? C10 C11 1.52(2) . ? C11 C12 1.35(3) . ? C13 C14 1.410(19) . ? C14 C15 1.57(2) . ? C15 C16 1.47(3) . ? C17 C18 1.48(2) . ? C18 C19 1.54(3) . ? C19 C20 1.59(4) . ? C21 C22 1.48(3) . ? C22 C23 1.58(3) . ? C23 C24 1.40(4) . ? C25 C26 1.474(19) . ? C26 C27 1.53(2) . ? C27 C28 1.48(3) . ? N3 C37 1.45(2) . ? N3 C41 1.50(2) . ? N3 C29 1.55(2) . ? N3 C33 1.584(18) . ? N4 C45 1.43(3) . ? N4 C32 1.48(2) . ? N4 C53 1.52(2) . ? N4 C49 1.69(2) . ? C29 C30 1.42(2) . ? C30 C31 1.46(2) . ? C31 C32 1.44(2) . ? C33 C34 1.40(2) . ? C34 C35 1.53(3) . ? C35 C36 1.35(4) . ? C37 C38 1.48(2) . ? C38 C39 1.45(3) . ? C39 C40 1.51(3) . ? C41 C42 1.37(3) . ? C42 C43 1.526(10) . ? C43 C44 1.517(10) . ? C45 C46 1.532(10) . ? C46 C47 1.538(10) . ? C47 C48 1.534(10) . ? C49 C50 1.40(3) . ? C50 C51 1.48(3) . ? C51 C52 1.52(4) . ? C53 C54 1.67(4) . ? C54 C55 1.524(10) . ? C55 C56 1.521(10) . ? 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 I6 Pb1 I7 96.75(3) . . ? I6 Pb1 I4 95.97(3) . . ? I7 Pb1 I4 97.42(3) . . ? I6 Pb1 I2 86.56(2) . . ? I7 Pb1 I2 175.35(3) . . ? I4 Pb1 I2 85.45(2) . . ? I6 Pb1 I1 167.10(2) . . ? I7 Pb1 I1 96.13(2) . . ? I4 Pb1 I1 81.61(2) . . ? I2 Pb1 I1 80.62(2) . . ? I6 Pb1 I3 107.30(3) . . ? I7 Pb1 I3 94.01(3) . . ? I4 Pb1 I3 152.63(2) . . ? I2 Pb1 I3 81.86(2) . . ? I1 Pb1 I3 72.475(18) . . ? I9 Pb2 I8 93.42(2) . . ? I9 Pb2 I4 97.42(2) . . ? I8 Pb2 I4 96.93(3) . . ? I9 Pb2 I1 85.49(2) . . ? I8 Pb2 I1 178.84(2) . . ? I4 Pb2 I1 82.86(2) . . ? I9 Pb2 I5 105.02(2) . . ? I8 Pb2 I5 96.91(3) . . ? I4 Pb2 I5 152.78(2) . . ? I1 Pb2 I5 83.74(2) . . ? I9 Pb2 I2 164.92(2) . . ? I8 Pb2 I2 101.63(2) . . ? I4 Pb2 I2 79.93(2) . . ? I1 Pb2 I2 79.464(19) . . ? I5 Pb2 I2 74.39(2) . . ? I1 Pb3 I2 87.07(2) . . ? I1 Pb3 I11 87.42(3) . . ? I2 Pb3 I11 171.16(3) . . ? I1 Pb3 I5 88.22(2) . . ? I2 Pb3 I5 80.72(2) . . ? I11 Pb3 I5 106.01(3) . . ? I1 Pb3 I10 165.79(2) . . ? I2 Pb3 I10 98.51(3) . . ? I11 Pb3 I10 85.34(3) . . ? I5 Pb3 I10 105.53(3) . . ? I1 Pb3 I3 80.25(2) . . ? I2 Pb3 I3 87.29(2) . . ? I11 Pb3 I3 84.97(3) . . ? I5 Pb3 I3 163.78(3) . . ? I10 Pb3 I3 86.94(3) . . ? I11 Pb4 I11 180.0 . 3_655 ? I11 Pb4 I10 85.96(3) . . ? I11 Pb4 I10 94.04(3) 3_655 . ? I11 Pb4 I10 94.04(3) . 3_655 ? I11 Pb4 I10 85.96(3) 3_655 3_655 ? I10 Pb4 I10 180.0 . 3_655 ? I11 Pb4 I3 85.52(2) . . ? I11 Pb4 I3 94.48(2) 3_655 . ? I10 Pb4 I3 88.01(2) . . ? I10 Pb4 I3 91.99(2) 3_655 . ? I11 Pb4 I3 94.48(2) . 3_655 ? I11 Pb4 I3 85.52(2) 3_655 3_655 ? I10 Pb4 I3 91.99(2) . 3_655 ? I10 Pb4 I3 88.01(2) 3_655 3_655 ? I3 Pb4 I3 180.0 . 3_655 ? Pb3 I1 Pb2 82.94(2) . . ? Pb3 I1 Pb1 81.91(2) . . ? Pb2 I1 Pb1 79.889(19) . . ? Pb3 I2 Pb1 84.44(2) . . ? Pb3 I2 Pb2 78.781(19) . . ? Pb1 I2 Pb2 79.44(2) . . ? Pb4 I3 Pb3 74.832(16) . . ? Pb4 I3 Pb1 153.44(2) . . ? Pb3 I3 Pb1 78.666(16) . . ? Pb1 I4 Pb2 86.24(2) . . ? Pb3 I5 Pb2 80.711(19) . . ? Pb4 I10 Pb3 76.05(2) . . ? Pb4 I11 Pb3 76.88(2) . . ? C13 N1 C1 111.3(8) . . ? C13 N1 C9 111.0(10) . . ? C1 N1 C9 105.1(9) . . ? C13 N1 C5 107.9(9) . . ? C1 N1 C5 111.0(9) . . ? C9 N1 C5 110.5(9) . . ? C25 N2 C17 110.0(9) . . ? C25 N2 C4 111.9(10) . . ? C17 N2 C4 105.2(9) . . ? C25 N2 C21 108.2(10) . . ? C17 N2 C21 109.9(11) . . ? C4 N2 C21 111.7(9) . . ? C2 C1 N1 114.1(9) . . ? C1 C2 C3 110.1(9) . . ? C4 C3 C2 109.6(9) . . ? C3 C4 N2 115.4(9) . . ? C6 C5 N1 116.8(11) . . ? C5 C6 C7 109.3(13) . . ? C8 C7 C6 114(2) . . ? N1 C9 C10 115.4(12) . . ? C11 C10 C9 110.0(15) . . ? C12 C11 C10 109.3(18) . . ? C14 C13 N1 118.2(13) . . ? C13 C14 C15 111.3(15) . . ? C16 C15 C14 115.5(19) . . ? C18 C17 N2 115.0(13) . . ? C17 C18 C19 109.8(19) . . ? C18 C19 C20 106(2) . . ? C22 C21 N2 117.3(15) . . ? C21 C22 C23 119(2) . . ? C24 C23 C22 97(2) . . ? C26 C25 N2 116.2(13) . . ? C25 C26 C27 108.8(14) . . ? C28 C27 C26 108(2) . . ? C37 N3 C41 112.8(14) . . ? C37 N3 C29 107.0(12) . . ? C41 N3 C29 110.6(14) . . ? C37 N3 C33 109.3(14) . . ? C41 N3 C33 109.8(11) . . ? C29 N3 C33 107.2(12) . . ? C45 N4 C32 105.7(14) . . ? C45 N4 C53 110.3(18) . . ? C32 N4 C53 118.2(18) . . ? C45 N4 C49 110(2) . . ? C32 N4 C49 107.3(13) . . ? C53 N4 C49 105.0(10) . . ? C30 C29 N3 117.1(15) . . ? C29 C30 C31 118.1(16) . . ? C32 C31 C30 118.3(15) . . ? C31 C32 N4 122.9(15) . . ? C34 C33 N3 122.5(14) . . ? C33 C34 C35 114.7(18) . . ? C36 C35 C34 123(3) . . ? N3 C37 C38 119.5(18) . . ? C39 C38 C37 114(2) . . ? C38 C39 C40 115(2) . . ? C42 C41 N3 114.2(19) . . ? C41 C42 C43 103(2) . . ? C44 C43 C42 115(2) . . ? N4 C45 C46 116(2) . . ? C45 C46 C47 111.3(18) . . ? C48 C47 C46 107.2(19) . . ? C50 C49 N4 122.5(15) . . ? C49 C50 C51 109(2) . . ? C50 C51 C52 109(2) . . ? N4 C53 C54 121.1(16) . . ? C55 C54 C53 102(2) . . ? C56 C55 C54 113(2) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 1.108 _refine_diff_density_min -0.935 _refine_diff_density_rms 0.153 #===END data_fv314y _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Bu3N-(CH2)4-NBu3]4[Pb10I28] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C112 H248 I28 N8 Pb10' _chemical_formula_weight 7332.28 _chemical_melting_point ? _chemical_compound_source ? 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' 0.0000 0.0000 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P-42c, No. 112' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z+1/2' 'x, -y, -z+1/2' '-y, x, -z' 'y, -x, -z' 'y, x, z+1/2' '-y, -x, z+1/2' _cell_length_a 22.9116(9) _cell_length_b 22.9116(9) _cell_length_c 18.5203(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9722.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description 'flat octahedron' _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.505 _exptl_crystal_density_method ? _exptl_crystal_F_000 6560 _exptl_absorpt_coefficient_mu 13.105 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1723 _exptl_absorpt_correction_T_max 0.2737 _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'STOE IPDS' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39676 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8541 _reflns_number_observed 7772 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. C56 disordered, refined with split positions. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[s^2^(Fo^2^)+( 0.0302P)^2^+22.3512P] 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 'idelized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(4) _refine_ls_number_reflns 8532 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_obs 0.0278 _refine_ls_wR_factor_all 0.0630 _refine_ls_wR_factor_obs 0.0605 _refine_ls_goodness_of_fit_all 1.033 _refine_ls_goodness_of_fit_obs 1.042 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pb1 Pb 0.08171(2) 0.5000 0.7500 0.0695(2) Uani 1 d S . Pb2 Pb 0.029009(14) 0.309805(14) 0.85785(2) 0.04544(8) Uani 1 d . . Pb3 Pb 0.20199(2) 0.368256(15) 0.84116(2) 0.05009(9) Uani 1 d . . I1 I 0.09360(3) 0.36733(3) 0.69750(3) 0.05311(15) Uani 1 d . . I2 I 0.07809(4) 0.44068(3) 0.90826(5) 0.0735(2) Uani 1 d . . I3 I 0.21097(4) 0.5000 0.7500 0.0600(2) Uani 1 d S . I4 I 0.15124(3) 0.24855(3) 0.88878(4) 0.0588(2) Uani 1 d . . I5 I 0.0000 0.20708(4) 0.7500 0.0688(3) Uani 1 d S . I6 I -0.02837(4) 0.26184(4) 0.98881(4) 0.0753(2) Uani 1 d . . I7 I 0.26320(3) 0.39293(3) 0.97856(4) 0.0673(2) Uani 1 d . . I8 I 0.30324(3) 0.31255(4) 0.76572(4) 0.0845(2) Uani 1 d . . N1 N 0.6018(4) 0.2333(4) 0.5098(5) 0.063(2) Uani 1 d . . N2 N 0.8470(3) 0.2124(4) 0.3562(5) 0.064(2) Uani 1 d . . C1 C 0.6675(4) 0.2337(5) 0.5053(6) 0.061(3) Uani 1 d . . H1A H 0.6810(4) 0.2747(5) 0.5074(6) 0.073 Uiso 1 calc R . H1B H 0.6831(4) 0.2135(5) 0.5485(6) 0.073 Uiso 1 calc R . C2 C 0.6932(4) 0.2057(5) 0.4395(5) 0.057(2) Uani 1 d . . H2A H 0.6771(4) 0.2242(5) 0.3955(5) 0.069 Uiso 1 calc R . H2B H 0.6830(4) 0.1637(5) 0.4385(5) 0.069 Uiso 1 calc R . C3 C 0.7589(4) 0.2128(5) 0.4409(6) 0.062(3) Uani 1 d . . H3A H 0.7763(4) 0.1850(5) 0.4757(6) 0.075 Uiso 1 calc R . H3B H 0.7692(4) 0.2529(5) 0.4560(6) 0.075 Uiso 1 calc R . C4 C 0.7825(4) 0.2009(5) 0.3651(5) 0.059(3) Uani 1 d . . H4A H 0.7747(4) 0.1596(5) 0.3526(5) 0.071 Uiso 1 calc R . H4B H 0.7609(4) 0.2255(5) 0.3302(5) 0.071 Uiso 1 calc R . C5 C 0.5765(4) 0.1717(5) 0.5111(7) 0.075(3) Uani 1 d . . H5A H 0.5335(4) 0.1745(5) 0.5137(7) 0.090 Uiso 1 calc R . H5B H 0.5865(4) 0.1520(5) 0.4651(7) 0.090 Uiso 1 calc R . C6 C 0.5976(6) 0.1341(6) 0.5729(8) 0.083(4) Uani 1 d . . H6A H 0.6404(6) 0.1287(6) 0.5695(8) 0.100 Uiso 1 calc R . H6B H 0.5888(6) 0.1535(6) 0.6194(8) 0.100 Uiso 1 calc R . C7 C 0.5681(7) 0.0763(7) 0.5701(10) 0.110(5) Uani 1 d . . H7A H 0.5773(7) 0.0574(7) 0.5234(10) 0.132 Uiso 1 calc R . H7B H 0.5253(7) 0.0824(7) 0.5720(10) 0.132 Uiso 1 calc R . C8 C 0.5858(9) 0.0358(8) 0.6309(13) 0.142(7) Uani 1 d . . H8A H 0.5649(9) -0.0014(8) 0.6261(13) 0.213 Uiso 1 calc R . H8B H 0.5760(9) 0.0538(8) 0.6773(13) 0.213 Uiso 1 calc R . H8C H 0.6280(9) 0.0287(8) 0.6286(13) 0.213 Uiso 1 calc R . C9 C 0.5742(5) 0.2627(6) 0.4452(7) 0.081(4) Uani 1 d . . H9A H 0.5314(5) 0.2627(6) 0.4525(7) 0.098 Uiso 1 calc R . H9B H 0.5823(5) 0.2384(6) 0.4022(7) 0.098 Uiso 1 calc R . C10 C 0.5927(7) 0.3247(6) 0.4281(9) 0.108(5) Uani 1 d . . H10A H 0.5891(7) 0.3490(6) 0.4721(9) 0.129 Uiso 1 calc R . H10B H 0.6341(7) 0.3249(6) 0.4130(9) 0.129 Uiso 1 calc R . C11 C 0.5561(9) 0.3497(8) 0.3699(11) 0.141(7) Uani 1 d . . H11A H 0.5656(9) 0.3291(8) 0.3244(11) 0.169 Uiso 1 calc R 1 H11B H 0.5148(9) 0.3412(8) 0.3813(11) 0.169 Uiso 1 calc R 1 C12A C 0.5615(12) 0.4080(12) 0.3583(17) 0.111(8) Uiso 0.60 d P 1 H12A H 0.5357(12) 0.4197(12) 0.3187(17) 0.167 Uiso 0.60 calc PR 1 H12B H 0.6020(12) 0.4171(12) 0.3456(17) 0.167 Uiso 0.60 calc PR 1 H12C H 0.5507(12) 0.4293(12) 0.4022(17) 0.167 Uiso 0.60 calc PR 1 C12B C 0.5139(19) 0.3822(19) 0.3772(25) 0.117(13) Uiso 0.40 d P 2 H12D H 0.4982(19) 0.3922(19) 0.3296(25) 0.175 Uiso 0.40 calc PR 2 H12E H 0.5261(19) 0.4179(19) 0.4022(25) 0.175 Uiso 0.40 calc PR 2 H12F H 0.4838(19) 0.3624(19) 0.4057(25) 0.175 Uiso 0.40 calc PR 2 C13 C 0.5892(6) 0.2695(6) 0.5778(6) 0.077(3) Uani 1 d . . H13A H 0.6072(6) 0.2493(6) 0.6195(6) 0.092 Uiso 1 calc R . H13B H 0.6091(6) 0.3076(6) 0.5726(6) 0.092 Uiso 1 calc R . C14 C 0.5292(6) 0.2804(10) 0.5948(10) 0.137(8) Uani 1 d . . H14A H 0.5095(6) 0.2429(10) 0.6053(10) 0.164 Uiso 1 calc R . H14B H 0.5097(6) 0.2981(10) 0.5524(10) 0.164 Uiso 1 calc R . C15 C 0.5227(8) 0.3217(11) 0.6607(9) 0.139(8) Uani 1 d . . H15A H 0.4807(8) 0.3256(11) 0.6722(9) 0.167 Uiso 1 calc R . H15B H 0.5419(8) 0.3033(11) 0.7029(9) 0.167 Uiso 1 calc R . C16 C 0.9169(8) 0.0075(9) 0.4055(11) 0.153(8) Uani 1 d . . H16A H 0.9405(8) -0.0153(9) 0.4395(11) 0.230 Uiso 1 calc R . H16B H 0.9341(8) 0.0048(9) 0.3571(11) 0.230 Uiso 1 calc R . H16C H 0.8770(8) -0.0079(9) 0.4045(11) 0.230 Uiso 1 calc R . C17 C 0.8644(5) 0.2744(6) 0.3801(7) 0.080(4) Uani 1 d . . H17A H 0.8559(5) 0.2781(6) 0.4323(7) 0.096 Uiso 1 calc R . H17B H 0.9072(5) 0.2783(6) 0.3742(7) 0.096 Uiso 1 calc R . C18 C 0.8362(6) 0.3243(6) 0.3421(7) 0.091(4) Uani 1 d . . H18A H 0.7943(6) 0.3250(6) 0.3548(7) 0.110 Uiso 1 calc R . H18B H 0.8392(6) 0.3179(6) 0.2893(7) 0.110 Uiso 1 calc R . C19 C 0.8626(8) 0.3826(8) 0.3601(11) 0.125(7) Uani 1 d . . H19A H 0.8577(8) 0.3902(8) 0.4124(11) 0.150 Uiso 1 calc R . H19B H 0.9050(8) 0.3814(8) 0.3496(11) 0.150 Uiso 1 calc R . C20 C 0.8363(11) 0.4296(8) 0.3197(14) 0.168(10) Uani 1 d . . H20A H 0.8548(11) 0.4666(8) 0.3331(14) 0.252 Uiso 1 calc R . H20B H 0.7945(11) 0.4315(8) 0.3308(14) 0.252 Uiso 1 calc R . H20C H 0.8416(11) 0.4227(8) 0.2679(14) 0.252 Uiso 1 calc R . C21 C 0.8588(4) 0.2039(6) 0.2746(5) 0.068(3) Uani 1 d . . H21A H 0.8490(4) 0.1632(6) 0.2615(5) 0.081 Uiso 1 calc R . H21B H 0.8323(4) 0.2299(6) 0.2472(5) 0.081 Uiso 1 calc R . C22 C 0.9206(5) 0.2162(7) 0.2513(7) 0.085(4) Uani 1 d . . H22A H 0.9305(5) 0.2576(7) 0.2604(7) 0.102 Uiso 1 calc R . H22B H 0.9481(5) 0.1914(7) 0.2790(7) 0.102 Uiso 1 calc R . C23 C 0.9253(6) 0.2030(8) 0.1731(8) 0.101(5) Uani 1 d . . H23A H 0.8911(6) 0.2201(8) 0.1482(8) 0.121 Uiso 1 calc R . H23B H 0.9606(6) 0.2226(8) 0.1539(8) 0.121 Uiso 1 calc R . C24 C 0.9285(6) 0.1411(9) 0.1550(9) 0.119(6) Uani 1 d . . H24A H 0.9314(6) 0.1367(9) 0.1025(9) 0.179 Uiso 1 calc R . H24B H 0.8934(6) 0.1213(9) 0.1724(9) 0.179 Uiso 1 calc R . H24C H 0.9630(6) 0.1239(9) 0.1779(9) 0.179 Uiso 1 calc R . C25 C 0.8825(5) 0.1699(6) 0.4020(7) 0.078(4) Uani 1 d . . H25A H 0.9238(5) 0.1828(6) 0.4013(7) 0.093 Uiso 1 calc R . H25B H 0.8687(5) 0.1728(6) 0.4525(7) 0.093 Uiso 1 calc R . C26 C 0.8806(5) 0.1082(7) 0.3802(7) 0.088(4) Uani 1 d . . H26A H 0.8956(5) 0.1044(7) 0.3303(7) 0.106 Uiso 1 calc R . H26B H 0.8395(5) 0.0946(7) 0.3805(7) 0.106 Uiso 1 calc R . C27 C 0.9158(6) 0.0707(8) 0.4293(9) 0.107(5) Uani 1 d . . H27A H 0.8993(6) 0.0731(8) 0.4786(9) 0.129 Uiso 1 calc R . H27B H 0.9562(6) 0.0858(8) 0.4311(9) 0.129 Uiso 1 calc R . C28 C 0.5485(11) 0.3834(12) 0.6505(15) 0.185(11) Uani 1 d . . H28A H 0.5423(11) 0.4064(12) 0.6945(15) 0.277 Uiso 1 calc R . H28B H 0.5291(11) 0.4027(12) 0.6097(15) 0.277 Uiso 1 calc R . H28C H 0.5904(11) 0.3804(12) 0.6407(15) 0.277 Uiso 1 calc R . 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 Pb1 0.0402(3) 0.0473(3) 0.1210(6) 0.0159(3) 0.000 0.000 Pb2 0.0521(2) 0.0446(2) 0.0397(2) 0.00462(14) -0.00496(14) 0.00039(14) Pb3 0.0547(2) 0.0459(2) 0.0497(2) 0.0009(2) -0.0067(2) 0.00771(15) I1 0.0547(3) 0.0605(4) 0.0440(3) -0.0018(3) -0.0013(3) -0.0111(3) I2 0.0814(5) 0.0565(4) 0.0827(6) -0.0193(4) 0.0273(4) -0.0045(3) I3 0.0420(4) 0.0511(5) 0.0869(7) 0.0068(5) 0.000 0.000 I4 0.0689(4) 0.0474(3) 0.0603(4) 0.0057(3) -0.0166(3) 0.0084(3) I5 0.0977(7) 0.0425(4) 0.0661(6) 0.000 -0.0222(6) 0.000 I6 0.0827(5) 0.0910(5) 0.0521(4) 0.0260(4) 0.0080(4) -0.0003(4) I7 0.0858(5) 0.0523(4) 0.0638(4) -0.0092(3) -0.0215(4) 0.0084(3) I8 0.0655(4) 0.1203(7) 0.0677(5) -0.0299(5) -0.0093(4) 0.0288(4) N1 0.052(5) 0.082(6) 0.055(5) -0.018(4) 0.003(4) -0.004(4) N2 0.053(4) 0.098(6) 0.042(5) 0.002(4) -0.003(4) -0.022(4) C1 0.049(5) 0.066(6) 0.068(7) -0.019(5) -0.009(5) -0.010(4) C2 0.041(5) 0.073(6) 0.059(6) -0.011(5) -0.006(4) -0.011(4) C3 0.039(5) 0.092(7) 0.055(6) 0.008(5) 0.001(4) -0.014(5) C4 0.045(5) 0.088(7) 0.044(5) 0.006(5) -0.011(4) -0.016(5) C5 0.041(5) 0.098(9) 0.086(9) -0.014(7) 0.008(5) -0.018(5) C6 0.070(7) 0.091(9) 0.089(10) -0.009(7) 0.001(6) -0.007(7) C7 0.108(12) 0.083(10) 0.139(15) 0.006(10) 0.032(10) -0.009(8) C8 0.148(17) 0.117(14) 0.161(20) 0.000(14) 0.014(15) -0.007(12) C9 0.055(6) 0.104(10) 0.085(9) -0.039(7) -0.011(6) 0.006(6) C10 0.117(12) 0.098(11) 0.108(12) -0.022(9) -0.054(10) 0.003(9) C11 0.142(15) 0.134(15) 0.147(18) -0.030(13) -0.057(14) 0.036(13) C13 0.093(9) 0.082(8) 0.055(7) -0.028(6) 0.003(6) 0.003(6) C14 0.072(9) 0.231(22) 0.107(13) -0.072(14) 0.002(8) 0.028(11) C15 0.116(13) 0.220(23) 0.082(11) -0.044(14) -0.006(10) 0.064(14) C16 0.148(16) 0.151(17) 0.161(19) 0.083(15) -0.029(14) 0.048(14) C17 0.054(6) 0.118(10) 0.068(8) -0.015(7) 0.000(6) -0.042(7) C18 0.091(9) 0.111(10) 0.072(9) -0.009(8) 0.007(7) -0.043(8) C19 0.116(12) 0.129(14) 0.131(15) -0.052(12) 0.031(11) -0.059(11) C20 0.236(27) 0.086(12) 0.182(23) -0.017(13) 0.035(19) -0.054(15) C21 0.061(6) 0.102(8) 0.040(6) 0.006(5) 0.002(4) -0.001(6) C22 0.054(6) 0.148(12) 0.052(7) 0.008(7) 0.002(5) -0.007(7) C23 0.072(8) 0.154(15) 0.077(10) 0.013(10) 0.006(7) -0.006(9) C24 0.080(9) 0.196(19) 0.082(11) -0.016(12) 0.025(8) -0.005(11) C25 0.050(6) 0.127(11) 0.056(7) 0.014(7) 0.001(5) -0.007(6) C26 0.059(7) 0.134(12) 0.072(8) 0.043(8) -0.012(6) -0.004(7) C27 0.059(7) 0.158(15) 0.106(12) 0.051(11) -0.012(7) 0.011(8) C28 0.187(23) 0.201(25) 0.165(24) -0.045(21) 0.033(19) 0.067(20) _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 Pb1 I3 2.9617(10) . ? Pb1 I1 3.2028(7) 4_566 ? Pb1 I1 3.2029(7) . ? Pb1 I2 3.2318(9) 4_566 ? Pb1 I2 3.2318(9) . ? Pb1 Pb1 3.7441(10) 2_565 ? Pb2 I6 2.9696(8) . ? Pb2 I5 3.1577(7) . ? Pb2 I4 3.1845(7) . ? Pb2 I1 3.2680(7) 3_556 ? Pb2 I2 3.3358(8) . ? Pb2 I1 3.5703(7) . ? Pb3 I7 2.9601(8) . ? Pb3 I8 2.9938(8) . ? Pb3 I4 3.1067(8) . ? Pb3 I3 3.4647(4) . ? Pb3 I2 3.5150(8) . ? Pb3 I1 3.6396(7) . ? I1 Pb2 3.2680(7) 3_556 ? I3 Pb3 3.4645(4) 4_566 ? I5 Pb2 3.1576(7) 3_556 ? N1 C1 1.506(12) . ? N1 C9 1.51(2) . ? N1 C5 1.527(14) . ? N1 C13 1.536(13) . ? N2 C4 1.510(11) . ? N2 C25 1.525(14) . ? N2 C17 1.540(14) . ? N2 C21 1.548(13) . ? C1 C2 1.498(14) . ? C2 C3 1.514(12) . ? C3 C4 1.529(14) . ? C5 C6 1.51(2) . ? C6 C7 1.49(2) . ? C7 C8 1.52(2) . ? C9 C10 1.51(2) . ? C10 C11 1.48(2) . ? C11 C12B 1.23(4) . ? C11 C12A 1.36(3) . ? C13 C14 1.43(2) . ? C14 C15 1.55(2) . ? C15 C28 1.54(3) . ? C16 C27 1.51(3) . ? C17 C18 1.49(2) . ? C18 C19 1.50(2) . ? C19 C20 1.44(3) . ? C21 C22 1.507(14) . ? C22 C23 1.48(2) . ? C23 C24 1.46(2) . ? C25 C26 1.47(2) . ? C26 C27 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I3 Pb1 I1 85.122(14) . 4_566 ? I3 Pb1 I1 85.119(14) . . ? I1 Pb1 I1 170.24(3) 4_566 . ? I3 Pb1 I2 91.47(2) . 4_566 ? I1 Pb1 I2 83.01(2) 4_566 4_566 ? I1 Pb1 I2 97.23(2) . 4_566 ? I3 Pb1 I2 91.47(2) . . ? I1 Pb1 I2 97.24(2) 4_566 . ? I1 Pb1 I2 83.01(2) . . ? I2 Pb1 I2 177.07(3) 4_566 . ? I3 Pb1 Pb1 180.0 . 2_565 ? I1 Pb1 Pb1 94.879(14) 4_566 2_565 ? I1 Pb1 Pb1 94.880(14) . 2_565 ? I2 Pb1 Pb1 88.54(2) 4_566 2_565 ? I2 Pb1 Pb1 88.53(2) . 2_565 ? I6 Pb2 I5 98.49(2) . . ? I6 Pb2 I4 94.55(2) . . ? I5 Pb2 I4 88.30(2) . . ? I6 Pb2 I1 91.43(2) . 3_556 ? I5 Pb2 I1 85.48(2) . 3_556 ? I4 Pb2 I1 171.95(2) . 3_556 ? I6 Pb2 I2 104.68(2) . . ? I5 Pb2 I2 156.63(2) . . ? I4 Pb2 I2 92.83(2) . . ? I1 Pb2 I2 90.86(2) 3_556 . ? I6 Pb2 I1 178.17(2) . . ? I5 Pb2 I1 80.575(15) . . ? I4 Pb2 I1 87.01(2) . . ? I1 Pb2 I1 86.93(2) 3_556 . ? I2 Pb2 I1 76.18(2) . . ? I7 Pb3 I8 96.63(2) . . ? I7 Pb3 I4 95.85(2) . . ? I8 Pb3 I4 92.64(3) . . ? I7 Pb3 I3 102.97(2) . . ? I8 Pb3 I3 95.62(2) . . ? I4 Pb3 I3 158.39(2) . . ? I7 Pb3 I2 89.34(2) . . ? I8 Pb3 I2 172.75(3) . . ? I4 Pb3 I2 90.81(2) . . ? I3 Pb3 I2 78.99(2) . . ? I7 Pb3 I1 162.33(2) . . ? I8 Pb3 I1 100.66(2) . . ? I4 Pb3 I1 86.97(2) . . ? I3 Pb3 I1 71.90(2) . . ? I2 Pb3 I1 73.15(2) . . ? Pb1 I1 Pb2 113.88(2) . 3_556 ? Pb1 I1 Pb2 93.59(2) . . ? Pb2 I1 Pb2 75.86(2) 3_556 . ? Pb1 I1 Pb3 80.25(2) . . ? Pb2 I1 Pb3 144.90(2) 3_556 . ? Pb2 I1 Pb3 71.148(14) . . ? Pb1 I2 Pb2 97.64(2) . . ? Pb1 I2 Pb3 81.79(2) . . ? Pb2 I2 Pb3 75.46(2) . . ? Pb1 I3 Pb3 86.595(15) . 4_566 ? Pb1 I3 Pb3 86.594(15) . . ? Pb3 I3 Pb3 173.19(3) 4_566 . ? Pb3 I4 Pb2 83.63(2) . . ? Pb2 I5 Pb2 83.62(2) 3_556 . ? C1 N1 C9 111.9(9) . . ? C1 N1 C5 112.7(8) . . ? C9 N1 C5 105.4(9) . . ? C1 N1 C13 103.3(8) . . ? C9 N1 C13 109.2(9) . . ? C5 N1 C13 114.5(9) . . ? C4 N2 C25 110.5(8) . . ? C4 N2 C17 112.6(9) . . ? C25 N2 C17 106.9(9) . . ? C4 N2 C21 104.8(7) . . ? C25 N2 C21 111.7(9) . . ? C17 N2 C21 110.5(8) . . ? C2 C1 N1 115.8(8) . . ? C1 C2 C3 109.4(8) . . ? C2 C3 C4 108.5(8) . . ? N2 C4 C3 114.5(8) . . ? C6 C5 N1 114.6(10) . . ? C7 C6 C5 109.5(12) . . ? C6 C7 C8 113.4(16) . . ? N1 C9 C10 117.7(9) . . ? C11 C10 C9 110.8(13) . . ? C12B C11 C10 126.9(30) . . ? C12A C11 C10 116.4(19) . . ? C14 C13 N1 117.1(11) . . ? C13 C14 C15 111.8(13) . . ? C28 C15 C14 115.2(19) . . ? C18 C17 N2 117.3(9) . . ? C17 C18 C19 113.7(13) . . ? C20 C19 C18 112.4(16) . . ? C22 C21 N2 114.9(9) . . ? C23 C22 C21 108.0(10) . . ? C24 C23 C22 115.1(14) . . ? C26 C25 N2 116.4(10) . . ? C25 C26 C27 111.8(13) . . ? C26 C27 C16 112.6(14) . . ? _refine_diff_density_max 0.810 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.110 #===END data_fv352poly _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Me3N-(CH2)5-NMe3]2[Pb3I10] _chemical_formula_sum 'C22 H56 I10 N4 Pb3' _chemical_formula_weight 2267.28 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' 0.0000 0.0000 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/c, No. 15' 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 20.889(2) _cell_length_b 13.2764(10) _cell_length_c 18.4226(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.245(10) _cell_angle_gamma 90.00 _cell_volume 5011.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 24 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 16.233 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1317 _exptl_absorpt_correction_T_max 0.5701 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14017 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.08 _reflns_number_total 3844 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+294.0152P] 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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3844 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1334 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.55703(3) 0.57549(4) 0.35911(3) 0.0448(2) Uani 1 d . . . Pb2 Pb 0.5000 0.85880(6) 0.2500 0.0479(3) Uani 1 d S . . I1 I 0.40670(5) 0.66423(8) 0.28914(6) 0.0485(3) Uani 1 d . . . I2 I 0.5000 0.38584(12) 0.2500 0.0709(6) Uani 1 d S . . I3 I 0.57760(7) 0.80841(10) 0.41710(7) 0.0667(4) Uani 1 d . . . I4 I 0.5000 0.5000 0.5000 0.0798(6) Uani 1 d S . . I5 I 0.59882(9) 1.01154(12) 0.21321(10) 0.0902(5) Uani 1 d . . . I6 I 0.69859(9) 0.50992(17) 0.42049(14) 0.1148(7) Uani 1 d . . . N1 N 0.9025(8) 0.3377(11) 0.5355(8) 0.057(4) Uani 1 d . . . N2 N 0.8003(8) 0.1728(13) 0.8445(9) 0.059(4) Uani 1 d . . . C1 C 0.8401(16) 0.350(3) 0.5671(19) 0.119(10) Uiso 1 d . . . H1A H 0.8366 0.4209 0.5829 0.143 Uiso 1 calc R . . H1B H 0.8016 0.3352 0.5279 0.143 Uiso 1 calc R . . C2 C 0.840(2) 0.284(4) 0.630(3) 0.183(18) Uiso 1 d . . . H2A H 0.8750 0.3026 0.6719 0.219 Uiso 1 calc R . . H2B H 0.8463 0.2128 0.6160 0.219 Uiso 1 calc R . . C3 C 0.769(2) 0.300(4) 0.649(3) 0.193(19) Uiso 1 d . . . H3A H 0.7335 0.2899 0.6055 0.232 Uiso 1 calc R . . H3B H 0.7644 0.3681 0.6701 0.232 Uiso 1 calc R . . C4 C 0.769(3) 0.199(5) 0.720(3) 0.23(3) Uiso 1 d . . . H4A H 0.7243 0.1779 0.7213 0.282 Uiso 1 calc R . . H4B H 0.7940 0.1400 0.7076 0.282 Uiso 1 calc R . . C5 C 0.796(3) 0.234(4) 0.780(3) 0.19(2) Uiso 1 d . . . H5A H 0.7718 0.2960 0.7877 0.230 Uiso 1 calc R . . H5B H 0.8404 0.2541 0.7757 0.230 Uiso 1 calc R . . C6 C 0.961(2) 0.366(3) 0.588(2) 0.159(15) Uiso 1 d . . . H6A H 0.9553 0.4336 0.6079 0.238 Uiso 1 calc R . . H6B H 0.9985 0.3673 0.5631 0.238 Uiso 1 calc R . . H6C H 0.9694 0.3176 0.6288 0.238 Uiso 1 calc R . . C7 C 0.9098(18) 0.237(3) 0.505(2) 0.144(13) Uiso 1 d . . . H7A H 0.8697 0.2190 0.4695 0.216 Uiso 1 calc R . . H7B H 0.9177 0.1871 0.5447 0.216 Uiso 1 calc R . . H7C H 0.9467 0.2370 0.4789 0.216 Uiso 1 calc R . . C8 C 0.8933(17) 0.407(3) 0.4709(19) 0.131(11) Uiso 1 d . . . H8A H 0.8537 0.3882 0.4355 0.196 Uiso 1 calc R . . H8B H 0.9311 0.4025 0.4469 0.196 Uiso 1 calc R . . H8C H 0.8890 0.4764 0.4877 0.196 Uiso 1 calc R . . C9 C 0.807(2) 0.059(4) 0.835(3) 0.192(19) Uiso 1 d . . . H9A H 0.7681 0.0340 0.8005 0.288 Uiso 1 calc R . . H9B H 0.8102 0.0258 0.8828 0.288 Uiso 1 calc R . . H9C H 0.8459 0.0451 0.8146 0.288 Uiso 1 calc R . . C10 C 0.740(2) 0.166(3) 0.871(2) 0.167(16) Uiso 1 d . . . H10A H 0.7047 0.1478 0.8304 0.251 Uiso 1 calc R . . H10B H 0.7307 0.2318 0.8914 0.251 Uiso 1 calc R . . H10C H 0.7444 0.1151 0.9102 0.251 Uiso 1 calc R . . C11 C 0.857(3) 0.198(5) 0.893(3) 0.24(3) Uiso 1 d . . . H11A H 0.8612 0.1562 0.9378 0.366 Uiso 1 calc R . . H11B H 0.8559 0.2690 0.9064 0.366 Uiso 1 calc R . . H11C H 0.8946 0.1853 0.8695 0.366 Uiso 1 calc R . . 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 Pb1 0.0526(4) 0.0368(3) 0.0461(4) 0.0055(3) 0.0127(3) 0.0032(3) Pb2 0.0618(6) 0.0321(4) 0.0490(5) 0.000 0.0089(4) 0.000 I1 0.0507(6) 0.0469(6) 0.0514(6) -0.0029(5) 0.0184(5) 0.0014(5) I2 0.0988(15) 0.0330(8) 0.0890(14) 0.000 0.0386(12) 0.000 I3 0.0793(9) 0.0629(8) 0.0544(7) -0.0088(6) 0.0041(7) -0.0121(6) I4 0.1145(17) 0.0735(13) 0.0607(11) 0.0206(10) 0.0402(12) 0.0034(12) I5 0.1105(13) 0.0622(9) 0.1019(12) 0.0042(8) 0.0303(10) -0.0292(8) I6 0.0691(10) 0.1244(16) 0.1432(18) 0.0070(13) 0.0013(11) 0.0359(10) N1 0.081(11) 0.039(8) 0.055(9) -0.002(7) 0.027(8) 0.013(7) N2 0.054(9) 0.066(10) 0.057(9) 0.004(8) 0.012(8) -0.004(8) _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 Pb1 I6 3.0785(18) . ? Pb1 I1 3.1982(12) 2_655 ? Pb1 I4 3.2196(6) . ? Pb1 I3 3.2726(15) . ? Pb1 I2 3.2962(14) . ? Pb1 I1 3.3663(13) . ? Pb1 Pb1 4.2548(14) 2_655 ? Pb1 Pb2 4.3213(10) . ? Pb2 I5 3.0623(16) . ? Pb2 I5 3.0623(16) 2_655 ? Pb2 I3 3.2566(14) 2_655 ? Pb2 I3 3.2566(14) . ? Pb2 I1 3.3969(13) . ? Pb2 I1 3.3969(13) 2_655 ? Pb2 Pb1 4.3213(10) 2_655 ? I1 Pb1 3.1982(12) 2_655 ? I2 Pb1 3.2962(14) 2_655 ? I4 Pb1 3.2196(6) 5_666 ? N1 C6 1.46(4) . ? N1 C7 1.48(4) . ? N1 C8 1.49(4) . ? N1 C1 1.54(3) . ? N2 C11 1.38(6) . ? N2 C5 1.43(5) . ? N2 C10 1.44(4) . ? N2 C9 1.53(5) . ? C1 C2 1.45(5) . ? C2 C3 1.62(6) . ? C3 C4 1.87(7) . ? C4 C5 1.22(6) . ? 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 I6 Pb1 I1 92.71(5) . 2_655 ? I6 Pb1 I4 95.50(5) . . ? I1 Pb1 I4 171.73(3) 2_655 . ? I6 Pb1 I3 95.26(6) . . ? I1 Pb1 I3 83.84(3) 2_655 . ? I4 Pb1 I3 94.40(3) . . ? I6 Pb1 I2 102.42(5) . . ? I1 Pb1 I2 83.01(3) 2_655 . ? I4 Pb1 I2 96.16(2) . . ? I3 Pb1 I2 158.39(4) . . ? I6 Pb1 I1 175.67(5) . . ? I1 Pb1 I1 84.41(3) 2_655 . ? I4 Pb1 I1 87.34(2) . . ? I3 Pb1 I1 81.23(4) . . ? I2 Pb1 I1 80.48(3) . . ? I6 Pb1 Pb1 131.90(5) . 2_655 ? I1 Pb1 Pb1 51.34(2) 2_655 2_655 ? I4 Pb1 Pb1 122.32(2) . 2_655 ? I3 Pb1 Pb1 108.79(3) . 2_655 ? I2 Pb1 Pb1 49.80(2) . 2_655 ? I1 Pb1 Pb1 47.89(2) . 2_655 ? I6 Pb1 Pb2 125.09(5) . . ? I1 Pb1 Pb2 51.08(2) 2_655 . ? I4 Pb1 Pb2 122.288(17) . . ? I3 Pb1 Pb2 48.40(3) . . ? I2 Pb1 Pb2 110.31(3) . . ? I1 Pb1 Pb2 50.60(2) . . ? Pb1 Pb1 Pb2 60.508(11) 2_655 . ? I5 Pb2 I5 97.07(7) . 2_655 ? I5 Pb2 I3 99.18(4) . 2_655 ? I5 Pb2 I3 96.46(4) 2_655 2_655 ? I5 Pb2 I3 96.46(4) . . ? I5 Pb2 I3 99.18(4) 2_655 . ? I3 Pb2 I3 156.29(5) 2_655 . ? I5 Pb2 I1 171.86(4) . . ? I5 Pb2 I1 90.98(4) 2_655 . ? I3 Pb2 I1 81.02(3) 2_655 . ? I3 Pb2 I1 81.00(3) . . ? I5 Pb2 I1 90.98(4) . 2_655 ? I5 Pb2 I1 171.86(5) 2_655 2_655 ? I3 Pb2 I1 81.00(3) 2_655 2_655 ? I3 Pb2 I1 81.02(3) . 2_655 ? I1 Pb2 I1 80.99(4) . 2_655 ? I5 Pb2 Pb1 127.59(4) . 2_655 ? I5 Pb2 Pb1 122.87(4) 2_655 2_655 ? I3 Pb2 Pb1 48.72(3) 2_655 2_655 ? I3 Pb2 Pb1 107.59(3) . 2_655 ? I1 Pb2 Pb1 47.10(2) . 2_655 ? I1 Pb2 Pb1 49.98(2) 2_655 2_655 ? I5 Pb2 Pb1 122.87(4) . . ? I5 Pb2 Pb1 127.59(4) 2_655 . ? I3 Pb2 Pb1 107.59(3) 2_655 . ? I3 Pb2 Pb1 48.72(3) . . ? I1 Pb2 Pb1 49.98(2) . . ? I1 Pb2 Pb1 47.10(2) 2_655 . ? Pb1 Pb2 Pb1 58.98(2) 2_655 . ? Pb1 I1 Pb1 80.76(3) 2_655 . ? Pb1 I1 Pb2 81.81(3) 2_655 . ? Pb1 I1 Pb2 79.43(3) . . ? Pb1 I2 Pb1 80.39(4) . 2_655 ? Pb2 I3 Pb1 82.88(3) . . ? Pb1 I4 Pb1 180.0 5_666 . ? C6 N1 C7 111(2) . . ? C6 N1 C8 109(2) . . ? C7 N1 C8 105(2) . . ? C6 N1 C1 113(2) . . ? C7 N1 C1 114(2) . . ? C8 N1 C1 104(2) . . ? C11 N2 C5 108(3) . . ? C11 N2 C10 119(3) . . ? C5 N2 C10 113(3) . . ? C11 N2 C9 103(3) . . ? C5 N2 C9 117(3) . . ? C10 N2 C9 95(3) . . ? C2 C1 N1 112(3) . . ? C1 C2 C3 104(4) . . ? C2 C3 C4 100(4) . . ? C5 C4 C3 107(6) . . ? C4 C5 N2 119(6) . . ? _diffrn_measured_fraction_theta_max 0.461 _diffrn_reflns_theta_full 24.08 _diffrn_measured_fraction_theta_full 0.461 _refine_diff_density_max 4.606 _refine_diff_density_min -2.855 _refine_diff_density_rms 0.244 #===END data_fv361n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Pr3N-(CH2)5-NPr3]2[Pb7I18] _chemical_formula_sum 'C46 H104 I18 N4 Pb7' _chemical_formula_weight 4447.86 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' 0.0000 0.0000 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n, No. 14' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9140(10) _cell_length_b 28.112(4) _cell_length_c 15.368(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.248(9) _cell_angle_gamma 90.00 _cell_volume 4829.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 10 _cell_measurement_theta_max 12.5 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3872 _exptl_absorpt_coefficient_mu 17.938 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0618 _exptl_absorpt_correction_T_max 0.6152 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE STADI IV' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '2 h' _diffrn_standards_decay_% +/- 2%' _diffrn_reflns_number 10801 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6723 _reflns_number_gt 5261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE STADI4 software' _computing_cell_refinement 'STOE STADI4 software' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL92 (Keller, 1992); DIAMOND2 (Brandenburg 1998)' _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+20.7347P] 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 'idealized positions' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6723 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.52199(4) 0.277478(18) 0.64463(3) 0.05234(14) Uani 1 d . . . Pb2 Pb 0.78307(4) 0.305389(17) 0.90475(3) 0.04595(12) Uani 1 d . . . Pb3 Pb 0.64760(4) 0.419538(17) 0.71878(3) 0.04791(13) Uani 1 d . . . Pb4 Pb 0.5000 0.5000 0.5000 0.0582(2) Uani 1 d S . . I1 I 0.78487(7) 0.32421(3) 0.69247(5) 0.0491(2) Uani 1 d . . . I2 I 0.50433(7) 0.34702(3) 0.80987(5) 0.0546(2) Uani 1 d . . . I3 I 0.45284(9) 0.38768(4) 0.52352(6) 0.0770(3) Uani 1 d . . . I4 I 0.66404(8) 0.20868(3) 0.80268(6) 0.0627(2) Uani 1 d . . . I5 I 0.83749(7) 0.41920(3) 0.92973(5) 0.0536(2) Uani 1 d . . . I6 I 0.47542(9) 0.50745(4) 0.70686(6) 0.0743(3) Uani 1 d . . . I7 I 0.78298(8) 0.48220(4) 0.61415(6) 0.0715(3) Uani 1 d . . . I8 I 0.77255(8) 0.27672(4) 1.10219(6) 0.0762(3) Uani 1 d . . . I9 I 1.05329(7) 0.27338(3) 0.97286(5) 0.0579(2) Uani 1 d . . . N1 N 0.2335(8) 0.4266(3) 0.9379(5) 0.041(2) Uani 1 d . . . N2 N 0.1419(9) 0.6349(3) 0.6101(6) 0.050(3) Uani 1 d . . . C1 C 0.1574(9) 0.4692(4) 0.8962(7) 0.043(3) Uani 1 d . . . H1A H 0.0741 0.4598 0.8787 0.052 Uiso 1 calc R . . H1B H 0.1721 0.4933 0.9439 0.052 Uiso 1 calc R . . C2 C 0.1754(10) 0.4914(4) 0.8130(7) 0.044(3) Uani 1 d . . . H2A H 0.1381 0.4714 0.7593 0.053 Uiso 1 calc R . . H2B H 0.2604 0.4926 0.8233 0.053 Uiso 1 calc R . . C3 C 0.1238(10) 0.5414(4) 0.7923(7) 0.047(3) Uani 1 d . . . H3A H 0.0381 0.5404 0.7790 0.056 Uiso 1 calc R . . H3B H 0.1592 0.5616 0.8460 0.056 Uiso 1 calc R . . C4 C 0.1498(12) 0.5616(4) 0.7094(8) 0.055(3) Uani 1 d . . . H4A H 0.2338 0.5569 0.7186 0.066 Uiso 1 calc R . . H4B H 0.1034 0.5443 0.6541 0.066 Uiso 1 calc R . . C5 C 0.1205(11) 0.6142(4) 0.6944(7) 0.050(3) Uani 1 d . . . H5A H 0.1688 0.6315 0.7492 0.060 Uiso 1 calc R . . H5B H 0.0372 0.6188 0.6876 0.060 Uiso 1 calc R . . C6 C 0.3645(10) 0.4414(4) 0.9810(8) 0.053(3) Uani 1 d . . . H6A H 0.3919 0.4518 0.9316 0.064 Uiso 1 calc R . . H6B H 0.3688 0.4687 1.0208 0.064 Uiso 1 calc R . . C7 C 0.4502(10) 0.4039(5) 1.0372(8) 0.059(3) Uani 1 d . . . H7A H 0.4316 0.3964 1.0923 0.071 Uiso 1 calc R . . H7B H 0.4416 0.3751 1.0007 0.071 Uiso 1 calc R . . C8 C 0.5750(11) 0.4216(5) 1.0643(9) 0.077(4) Uani 1 d . . . H8A H 0.6290 0.3977 1.0998 0.115 Uiso 1 calc R . . H8B H 0.5834 0.4499 1.1010 0.115 Uiso 1 calc R . . H8C H 0.5932 0.4287 1.0095 0.115 Uiso 1 calc R . . C9 C 0.1891(10) 0.4041(4) 1.0109(7) 0.045(3) Uani 1 d . . . H9A H 0.1056 0.3956 0.9811 0.055 Uiso 1 calc R . . H9B H 0.2333 0.3749 1.0324 0.055 Uiso 1 calc R . . C10 C 0.2003(13) 0.4347(5) 1.0945(8) 0.065(4) Uani 1 d . . . H10A H 0.2816 0.4465 1.1212 0.078 Uiso 1 calc R . . H10B H 0.1472 0.4619 1.0755 0.078 Uiso 1 calc R . . C11 C 0.1694(13) 0.4067(5) 1.1650(8) 0.075(4) Uani 1 d . . . H11A H 0.1766 0.4265 1.2175 0.113 Uiso 1 calc R . . H11B H 0.2229 0.3801 1.1844 0.113 Uiso 1 calc R . . H11C H 0.0887 0.3953 1.1385 0.113 Uiso 1 calc R . . C12 C 0.2244(9) 0.3898(4) 0.8625(7) 0.048(3) Uani 1 d . . . H12A H 0.2610 0.4035 0.8208 0.058 Uiso 1 calc R . . H12B H 0.2727 0.3626 0.8921 0.058 Uiso 1 calc R . . C13 C 0.1042(10) 0.3717(4) 0.8049(7) 0.051(3) Uani 1 d . . . H13A H 0.0575 0.3969 0.7659 0.061 Uiso 1 calc R . . H13B H 0.0617 0.3602 0.8443 0.061 Uiso 1 calc R . . C14 C 0.1231(11) 0.3309(5) 0.7444(8) 0.070(4) Uani 1 d . . . H14A H 0.0468 0.3184 0.7064 0.104 Uiso 1 calc R . . H14B H 0.1692 0.3061 0.7837 0.104 Uiso 1 calc R . . H14C H 0.1650 0.3427 0.7056 0.104 Uiso 1 calc R . . C15 C 0.2751(11) 0.6326(5) 0.6220(8) 0.057(3) Uani 1 d . . . H15A H 0.3009 0.5997 0.6322 0.068 Uiso 1 calc R . . H15B H 0.2844 0.6428 0.5646 0.068 Uiso 1 calc R . . C16 C 0.3559(12) 0.6620(6) 0.6998(9) 0.079(4) Uani 1 d . . . H16A H 0.3465 0.6523 0.7575 0.094 Uiso 1 calc R . . H16B H 0.3324 0.6951 0.6892 0.094 Uiso 1 calc R . . C17 C 0.4859(12) 0.6573(6) 0.7091(10) 0.086(5) Uani 1 d . . . H17A H 0.5341 0.6767 0.7596 0.129 Uiso 1 calc R . . H17B H 0.4960 0.6674 0.6527 0.129 Uiso 1 calc R . . H17C H 0.5101 0.6246 0.7210 0.129 Uiso 1 calc R . . C18 C 0.0716(11) 0.6067(4) 0.5236(8) 0.055(3) Uani 1 d . . . H18A H 0.0849 0.6210 0.4705 0.066 Uiso 1 calc R . . H18B H 0.1031 0.5746 0.5300 0.066 Uiso 1 calc R . . C19 C -0.0621(13) 0.6042(5) 0.5039(8) 0.074(4) Uani 1 d . . . H19A H -0.0772 0.5936 0.5589 0.089 Uiso 1 calc R . . H19B H -0.0975 0.6354 0.4872 0.089 Uiso 1 calc R . . C20 C -0.1172(16) 0.5696(6) 0.4249(9) 0.107(6) Uani 1 d . . . H20A H -0.2019 0.5677 0.4122 0.161 Uiso 1 calc R . . H20B H -0.0821 0.5387 0.4421 0.161 Uiso 1 calc R . . H20C H -0.1027 0.5805 0.3706 0.161 Uiso 1 calc R . . C21 C 0.0988(11) 0.6858(4) 0.6003(7) 0.052(3) Uani 1 d . . . H21A H 0.1415 0.7027 0.6572 0.062 Uiso 1 calc R . . H21B H 0.0146 0.6860 0.5928 0.062 Uiso 1 calc R . . C22 C 0.1151(15) 0.7129(4) 0.5188(9) 0.077(4) Uani 1 d . . . H22A H 0.1967 0.7089 0.5207 0.092 Uiso 1 calc R . . H22B H 0.0624 0.6993 0.4611 0.092 Uiso 1 calc R . . C23 C 0.0896(13) 0.7639(5) 0.5198(10) 0.077(4) Uani 1 d . . . H23A H 0.1016 0.7791 0.4677 0.116 Uiso 1 calc R . . H23B H 0.1423 0.7778 0.5762 0.116 Uiso 1 calc R . . H23C H 0.0081 0.7683 0.5161 0.116 Uiso 1 calc R . . 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 Pb1 0.0501(3) 0.0590(3) 0.0495(3) -0.0138(2) 0.0193(2) -0.0092(2) Pb2 0.0460(3) 0.0482(3) 0.0412(2) 0.0003(2) 0.0120(2) 0.0030(2) Pb3 0.0520(3) 0.0461(3) 0.0456(2) 0.0014(2) 0.0169(2) 0.0049(2) Pb4 0.0661(5) 0.0578(5) 0.0503(4) 0.0073(3) 0.0195(3) 0.0121(4) I1 0.0446(5) 0.0578(5) 0.0509(4) -0.0061(4) 0.0242(4) -0.0008(4) I2 0.0475(5) 0.0687(6) 0.0570(4) -0.0051(4) 0.0300(4) 0.0022(4) I3 0.0890(7) 0.0703(7) 0.0537(5) -0.0058(4) 0.0017(5) 0.0055(6) I4 0.0724(6) 0.0480(5) 0.0733(5) -0.0046(4) 0.0323(5) -0.0065(5) I5 0.0515(5) 0.0534(5) 0.0519(4) -0.0136(4) 0.0127(4) -0.0030(4) I6 0.0753(6) 0.0688(7) 0.0818(6) -0.0100(5) 0.0310(5) 0.0227(5) I7 0.0685(6) 0.0749(7) 0.0827(6) 0.0052(5) 0.0411(5) -0.0028(5) I8 0.0618(6) 0.1200(9) 0.0522(5) 0.0105(5) 0.0264(4) 0.0303(6) I9 0.0532(5) 0.0631(6) 0.0627(5) 0.0191(4) 0.0270(4) 0.0069(4) N1 0.045(6) 0.036(6) 0.044(5) 0.000(4) 0.019(4) 0.002(4) N2 0.075(7) 0.037(6) 0.048(5) -0.004(4) 0.036(5) 0.006(5) C1 0.035(6) 0.051(8) 0.043(6) -0.001(5) 0.013(5) 0.009(6) C2 0.048(7) 0.043(7) 0.045(6) 0.009(5) 0.022(5) 0.004(6) C3 0.044(7) 0.056(8) 0.045(6) 0.011(6) 0.021(5) 0.007(6) C4 0.090(10) 0.031(7) 0.057(7) 0.008(6) 0.041(7) 0.010(7) C5 0.077(9) 0.044(8) 0.039(6) -0.008(5) 0.033(6) -0.002(7) C6 0.045(7) 0.054(8) 0.059(7) -0.005(6) 0.015(6) -0.013(6) C7 0.040(8) 0.071(10) 0.066(8) -0.012(7) 0.015(6) -0.007(7) C8 0.047(8) 0.091(12) 0.083(9) -0.008(8) 0.012(7) -0.001(8) C9 0.038(7) 0.042(7) 0.056(7) 0.009(6) 0.016(5) 0.002(5) C10 0.093(10) 0.064(9) 0.053(7) -0.006(6) 0.045(7) 0.001(8) C11 0.093(11) 0.091(12) 0.059(8) 0.014(7) 0.049(8) 0.010(9) C12 0.039(7) 0.048(8) 0.058(7) 0.000(6) 0.017(6) 0.002(6) C13 0.044(7) 0.060(9) 0.046(6) 0.000(6) 0.013(5) -0.014(6) C14 0.057(9) 0.080(11) 0.060(8) -0.025(7) 0.006(7) 0.002(8) C15 0.068(9) 0.052(8) 0.067(8) 0.000(6) 0.043(7) 0.011(7) C16 0.058(9) 0.105(13) 0.083(10) -0.009(9) 0.038(8) 0.009(9) C17 0.074(11) 0.088(12) 0.109(11) 0.016(10) 0.047(9) 0.010(9) C18 0.074(9) 0.047(8) 0.051(7) -0.015(6) 0.032(6) -0.009(7) C19 0.087(11) 0.083(11) 0.053(8) -0.013(7) 0.025(7) -0.010(9) C20 0.142(16) 0.110(15) 0.069(10) -0.019(10) 0.034(10) -0.034(12) C21 0.065(8) 0.040(8) 0.057(7) -0.002(6) 0.028(6) 0.013(6) C22 0.134(14) 0.035(8) 0.082(9) 0.017(7) 0.064(10) 0.013(8) C23 0.086(11) 0.053(9) 0.099(10) 0.006(8) 0.039(9) 0.009(8) _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 Pb1 I4 3.1079(11) . ? Pb1 I9 3.1357(9) 4_565 ? Pb1 I8 3.1996(10) 4_565 ? Pb1 I1 3.2376(9) . ? Pb1 I2 3.2687(9) . ? Pb1 I3 3.5607(12) . ? Pb1 Pb2 4.2029(8) . ? Pb1 Pb3 4.2786(9) . ? Pb1 Pb2 4.4560(8) 4_565 ? Pb2 I9 3.1524(10) . ? Pb2 I8 3.1836(10) . ? Pb2 I4 3.2129(10) . ? Pb2 I5 3.2608(11) . ? Pb2 I1 3.3124(9) . ? Pb2 I2 3.3425(10) . ? Pb2 Pb3 4.2282(8) . ? Pb2 Pb1 4.4560(8) 4_666 ? Pb3 I7 3.1756(10) . ? Pb3 I6 3.1764(11) . ? Pb3 I3 3.2205(10) . ? Pb3 I1 3.2369(10) . ? Pb3 I5 3.2484(10) . ? Pb3 I2 3.2686(10) . ? Pb3 Pb4 3.9269(6) . ? Pb4 I3 3.2492(11) 3_666 ? Pb4 I3 3.2492(11) . ? Pb4 I7 3.2558(10) 3_666 ? Pb4 I7 3.2558(10) . ? Pb4 I6 3.2985(10) 3_666 ? Pb4 I6 3.2985(10) . ? Pb4 Pb3 3.9269(6) 3_666 ? I8 Pb1 3.1996(10) 4_666 ? I9 Pb1 3.1357(9) 4_666 ? N1 C1 1.504(13) . ? N1 C6 1.527(13) . ? N1 C12 1.530(13) . ? N1 C9 1.532(13) . ? N2 C21 1.509(13) . ? N2 C5 1.522(12) . ? N2 C18 1.525(14) . ? N2 C15 1.535(15) . ? C1 C2 1.503(13) . ? C2 C3 1.523(15) . ? C3 C4 1.522(14) . ? C4 C5 1.517(15) . ? C6 C7 1.514(16) . ? C7 C8 1.484(16) . ? C9 C10 1.514(15) . ? C10 C11 1.485(16) . ? C12 C13 1.488(14) . ? C13 C14 1.541(16) . ? C15 C16 1.498(17) . ? C16 C17 1.511(17) . ? C18 C19 1.516(17) . ? C19 C20 1.516(18) . ? C21 C22 1.534(15) . ? C22 C23 1.466(16) . ? 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 I4 Pb1 I9 100.54(3) . 4_565 ? I4 Pb1 I8 94.54(3) . 4_565 ? I9 Pb1 I8 89.08(3) 4_565 4_565 ? I4 Pb1 I1 81.53(3) . . ? I9 Pb1 I1 89.35(2) 4_565 . ? I8 Pb1 I1 175.43(3) 4_565 . ? I4 Pb1 I2 85.93(3) . . ? I9 Pb1 I2 170.09(3) 4_565 . ? I8 Pb1 I2 97.94(3) 4_565 . ? I1 Pb1 I2 84.16(2) . . ? I4 Pb1 I3 156.18(3) . . ? I9 Pb1 I3 91.72(3) 4_565 . ? I8 Pb1 I3 106.09(3) 4_565 . ? I1 Pb1 I3 78.25(3) . . ? I2 Pb1 I3 79.65(3) . . ? I4 Pb1 Pb2 49.40(2) . . ? I9 Pb1 Pb2 128.41(2) 4_565 . ? I8 Pb1 Pb2 127.75(2) 4_565 . ? I1 Pb1 Pb2 50.871(16) . . ? I2 Pb1 Pb2 51.306(18) . . ? I3 Pb1 Pb2 107.21(2) . . ? I4 Pb1 Pb3 109.09(2) . . ? I9 Pb1 Pb3 121.15(2) 4_565 . ? I8 Pb1 Pb3 135.51(3) 4_565 . ? I1 Pb1 Pb3 48.629(17) . . ? I2 Pb1 Pb3 49.117(17) . . ? I3 Pb1 Pb3 47.427(18) . . ? Pb2 Pb1 Pb3 59.796(11) . . ? I4 Pb1 Pb2 109.90(2) . 4_565 ? I9 Pb1 Pb2 45.027(18) 4_565 4_565 ? I8 Pb1 Pb2 45.578(18) 4_565 4_565 ? I1 Pb1 Pb2 133.693(19) . 4_565 ? I2 Pb1 Pb2 139.55(2) . 4_565 ? I3 Pb1 Pb2 93.23(2) . 4_565 ? Pb2 Pb1 Pb2 159.238(15) . 4_565 ? Pb3 Pb1 Pb2 140.598(15) . 4_565 ? I9 Pb2 I8 89.07(2) . . ? I9 Pb2 I4 98.52(3) . . ? I8 Pb2 I4 95.44(3) . . ? I9 Pb2 I5 95.88(3) . . ? I8 Pb2 I5 102.01(3) . . ? I4 Pb2 I5 157.51(3) . . ? I9 Pb2 I1 91.07(2) . . ? I8 Pb2 I1 174.24(3) . . ? I4 Pb2 I1 78.85(2) . . ? I5 Pb2 I1 83.71(2) . . ? I9 Pb2 I2 172.35(2) . . ? I8 Pb2 I2 98.25(2) . . ? I4 Pb2 I2 83.06(3) . . ? I5 Pb2 I2 80.50(2) . . ? I1 Pb2 I2 81.87(2) . . ? I9 Pb2 Pb1 126.66(2) . . ? I8 Pb2 Pb1 126.80(2) . . ? I4 Pb2 Pb1 47.262(19) . . ? I5 Pb2 Pb1 110.287(19) . . ? I1 Pb2 Pb1 49.306(17) . . ? I2 Pb2 Pb1 49.753(17) . . ? I9 Pb2 Pb3 123.24(2) . . ? I8 Pb2 Pb3 134.80(2) . . ? I4 Pb2 Pb3 108.15(2) . . ? I5 Pb2 Pb3 49.362(17) . . ? I1 Pb2 Pb3 49.012(17) . . ? I2 Pb2 Pb3 49.475(17) . . ? Pb1 Pb2 Pb3 60.991(14) . . ? I9 Pb2 Pb1 44.724(17) . 4_666 ? I8 Pb2 Pb1 45.873(19) . 4_666 ? I4 Pb2 Pb1 90.53(2) . 4_666 ? I5 Pb2 Pb1 111.81(2) . 4_666 ? I1 Pb2 Pb1 132.71(2) . 4_666 ? I2 Pb2 Pb1 142.913(19) . 4_666 ? Pb1 Pb2 Pb1 137.720(14) . 4_666 ? Pb3 Pb2 Pb1 160.234(15) . 4_666 ? I7 Pb3 I6 88.29(3) . . ? I7 Pb3 I3 90.63(3) . . ? I6 Pb3 I3 85.41(3) . . ? I7 Pb3 I1 91.66(3) . . ? I6 Pb3 I1 168.84(3) . . ? I3 Pb3 I1 83.43(3) . . ? I7 Pb3 I5 101.92(3) . . ? I6 Pb3 I5 105.82(3) . . ? I3 Pb3 I5 163.23(3) . . ? I1 Pb3 I5 85.11(2) . . ? I7 Pb3 I2 174.19(3) . . ? I6 Pb3 I2 95.02(3) . . ? I3 Pb3 I2 84.89(3) . . ? I1 Pb3 I2 84.17(2) . . ? I5 Pb3 I2 81.80(2) . . ? I7 Pb3 Pb4 53.30(2) . . ? I6 Pb3 Pb4 54.095(19) . . ? I3 Pb3 Pb4 52.96(2) . . ? I1 Pb3 Pb4 117.765(19) . . ? I5 Pb3 Pb4 143.80(2) . . ? I2 Pb3 Pb4 125.48(2) . . ? I7 Pb3 Pb2 128.41(2) . . ? I6 Pb3 Pb2 135.83(2) . . ? I3 Pb3 Pb2 113.71(2) . . ? I1 Pb3 Pb2 50.576(17) . . ? I5 Pb3 Pb2 49.618(18) . . ? I2 Pb3 Pb2 51.014(18) . . ? Pb4 Pb3 Pb2 165.689(14) . . ? I7 Pb3 Pb1 125.10(2) . . ? I6 Pb3 Pb1 123.47(3) . . ? I3 Pb3 Pb1 54.51(2) . . ? I1 Pb3 Pb1 48.643(18) . . ? I5 Pb3 Pb1 108.77(2) . . ? I2 Pb3 Pb1 49.120(17) . . ? Pb4 Pb3 Pb1 107.332(15) . . ? Pb2 Pb3 Pb1 59.213(14) . . ? I3 Pb4 I3 180.0 3_666 . ? I3 Pb4 I7 88.71(3) 3_666 3_666 ? I3 Pb4 I7 91.29(3) . 3_666 ? I3 Pb4 I7 91.29(3) 3_666 . ? I3 Pb4 I7 88.71(3) . . ? I7 Pb4 I7 180.0 3_666 . ? I3 Pb4 I6 83.00(2) 3_666 3_666 ? I3 Pb4 I6 97.00(2) . 3_666 ? I7 Pb4 I6 84.91(2) 3_666 3_666 ? I7 Pb4 I6 95.09(2) . 3_666 ? I3 Pb4 I6 97.00(2) 3_666 . ? I3 Pb4 I6 83.00(2) . . ? I7 Pb4 I6 95.09(2) 3_666 . ? I7 Pb4 I6 84.91(2) . . ? I6 Pb4 I6 180.0 3_666 . ? I3 Pb4 Pb3 52.297(17) 3_666 3_666 ? I3 Pb4 Pb3 127.703(17) . 3_666 ? I7 Pb4 Pb3 51.448(18) 3_666 3_666 ? I7 Pb4 Pb3 128.552(18) . 3_666 ? I6 Pb4 Pb3 51.261(19) 3_666 3_666 ? I6 Pb4 Pb3 128.739(19) . 3_666 ? I3 Pb4 Pb3 127.703(17) 3_666 . ? I3 Pb4 Pb3 52.297(17) . . ? I7 Pb4 Pb3 128.552(18) 3_666 . ? I7 Pb4 Pb3 51.448(18) . . ? I6 Pb4 Pb3 128.739(19) 3_666 . ? I6 Pb4 Pb3 51.261(19) . . ? Pb3 Pb4 Pb3 180.0 3_666 . ? Pb3 I1 Pb1 82.73(2) . . ? Pb3 I1 Pb2 80.41(2) . . ? Pb1 I1 Pb2 79.82(2) . . ? Pb3 I2 Pb1 81.76(2) . . ? Pb3 I2 Pb2 79.51(2) . . ? Pb1 I2 Pb2 78.94(2) . . ? Pb3 I3 Pb4 74.74(2) . . ? Pb3 I3 Pb1 78.06(2) . . ? Pb4 I3 Pb1 152.38(3) . . ? Pb1 I4 Pb2 83.34(3) . . ? Pb3 I5 Pb2 81.02(2) . . ? Pb3 I6 Pb4 74.64(2) . . ? Pb3 I7 Pb4 75.25(2) . . ? Pb2 I8 Pb1 88.55(2) . 4_666 ? Pb1 I9 Pb2 90.25(2) 4_666 . ? C1 N1 C6 110.0(8) . . ? C1 N1 C12 109.9(8) . . ? C6 N1 C12 107.9(8) . . ? C1 N1 C9 109.4(8) . . ? C6 N1 C9 110.8(8) . . ? C12 N1 C9 108.9(8) . . ? C21 N2 C5 107.3(8) . . ? C21 N2 C18 109.9(9) . . ? C5 N2 C18 109.9(9) . . ? C21 N2 C15 110.8(9) . . ? C5 N2 C15 110.6(9) . . ? C18 N2 C15 108.3(8) . . ? C2 C1 N1 116.8(8) . . ? C1 C2 C3 113.3(9) . . ? C4 C3 C2 109.6(9) . . ? C5 C4 C3 112.8(9) . . ? C4 C5 N2 113.9(8) . . ? C7 C6 N1 116.3(10) . . ? C8 C7 C6 109.8(11) . . ? C10 C9 N1 115.7(9) . . ? C11 C10 C9 110.2(11) . . ? C13 C12 N1 118.9(9) . . ? C12 C13 C14 107.6(10) . . ? C16 C15 N2 115.0(9) . . ? C15 C16 C17 112.4(12) . . ? C19 C18 N2 114.9(9) . . ? C20 C19 C18 109.0(12) . . ? N2 C21 C22 114.7(9) . . ? C23 C22 C21 113.1(11) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.176 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.167 #=END