####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_JQ69TW53 _database_code_depnum_ccdc_archive 'CCDC 1910032' loop_ _audit_author_name _audit_author_address 'Jim Fettinger' ;University of California, Davis United States of America ; _audit_update_record ; 2019-04-15 deposited with the CCDC. 2019-07-03 downloaded from the CCDC. ; _audit_creation_method SHELXL-2017/1 _shelx_SHELXL_version_number 2017/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Br2 Pb2 Si2' _chemical_formula_sum 'C66 H90 Br2 Pb2 Si2' _chemical_formula_weight 1513.76 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3682(9) _cell_length_b 12.7595(10) _cell_length_c 12.9493(10) _cell_angle_alpha 94.5630(12) _cell_angle_beta 103.1496(10) _cell_angle_gamma 114.1017(10) _cell_volume 1637.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_F_000 748 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.520 _exptl_crystal_size_mid 0.312 _exptl_crystal_size_min 0.078 _exptl_absorpt_coefficient_mu 6.425 _shelx_estimated_absorpt_T_min 0.135 _shelx_estimated_absorpt_T_max 0.634 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1353 _exptl_absorpt_correction_T_max 0.2698 _exptl_absorpt_process_details 'SADABS 2016/2 (Sheldrick, 2016)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7514 _diffrn_reflns_av_unetI/netI 0.0396 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.782 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 7514 _reflns_number_gt 7230 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex2 (2014.9-1) (Bruker, 2014)' _computing_cell_refinement 'SAINT (8.37a) (Bruker, 2016)' _computing_data_reduction 'SAINT (8.37a) (Bruker, 2016)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refined as a 2-component twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+8.4331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7514 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1091 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.90810(2) 0.45005(2) 0.33126(2) 0.02304(8) Uani 1 1 d . . . . . Br1 Br 0.93310(5) 0.63096(5) 0.49660(5) 0.01843(12) Uani 1 1 d . . . . . Si1 Si 0.20717(17) 0.13285(17) 0.20312(15) 0.0228(4) Uani 1 1 d . . . . . C1 C 0.6806(6) 0.3424(5) 0.3136(5) 0.0181(11) Uani 1 1 d . . . . . C2 C 0.6049(7) 0.3481(6) 0.2125(5) 0.0189(12) Uani 1 1 d . . . . . C3 C 0.4654(7) 0.2924(6) 0.1815(5) 0.0208(12) Uani 1 1 d . . . . . H3 H 0.416770 0.301046 0.115309 0.025 Uiso 1 1 calc R U . . . C4 C 0.3952(6) 0.2236(6) 0.2465(5) 0.0190(12) Uani 1 1 d . . . . . C5 C 0.4711(6) 0.2154(6) 0.3444(5) 0.0203(12) Uani 1 1 d . . . . . H5 H 0.425486 0.166617 0.388096 0.024 Uiso 1 1 calc R U . . . C6 C 0.6114(6) 0.2761(6) 0.3805(5) 0.0180(11) Uani 1 1 d . . . . . C7 C 0.6811(6) 0.4092(6) 0.1365(5) 0.0200(12) Uani 1 1 d . . . . . C8 C 0.7259(6) 0.5293(7) 0.1381(5) 0.0244(13) Uani 1 1 d . . . . . C9 C 0.8106(7) 0.5821(7) 0.0754(6) 0.0287(14) Uani 1 1 d . . . . . H9 H 0.844689 0.664198 0.078663 0.034 Uiso 1 1 calc R U . . . C10 C 0.8451(8) 0.5169(8) 0.0092(6) 0.0327(16) Uani 1 1 d . . . . . H10 H 0.903148 0.554661 -0.032438 0.039 Uiso 1 1 calc R U . . . C11 C 0.7967(7) 0.3974(8) 0.0023(6) 0.0301(16) Uani 1 1 d . . . . . H11 H 0.820163 0.353610 -0.045108 0.036 Uiso 1 1 calc R U . . . C12 C 0.7123(6) 0.3398(6) 0.0654(5) 0.0226(13) Uani 1 1 d . . . . . C13 C 0.6835(7) 0.6037(6) 0.2071(5) 0.0241(13) Uani 1 1 d . . . . . H13 H 0.664069 0.565919 0.269956 0.029 Uiso 1 1 calc R U . . . C14 C 0.7897(9) 0.7296(7) 0.2513(8) 0.0401(18) Uani 1 1 d . . . . . H14A H 0.873857 0.730043 0.292079 0.060 Uiso 1 1 calc R U . . . H14B H 0.758566 0.769338 0.299094 0.060 Uiso 1 1 calc R U . . . H14C H 0.804841 0.770510 0.191181 0.060 Uiso 1 1 calc R U . . . C15 C 0.5516(9) 0.6001(9) 0.1379(6) 0.040(2) Uani 1 1 d . . . . . H15A H 0.568522 0.638147 0.076421 0.061 Uiso 1 1 calc R U . . . H15B H 0.518292 0.641345 0.181970 0.061 Uiso 1 1 calc R U . . . H15C H 0.484284 0.518522 0.111180 0.061 Uiso 1 1 calc R U . . . C16 C 0.6608(7) 0.2086(7) 0.0565(6) 0.0282(15) Uani 1 1 d . . . . . H16 H 0.596954 0.182892 0.101312 0.034 Uiso 1 1 calc R U . . . C17 C 0.7758(10) 0.1758(8) 0.1009(7) 0.042(2) Uani 1 1 d . . . . . H17A H 0.740383 0.090395 0.089849 0.062 Uiso 1 1 calc R U . . . H17B H 0.815990 0.209245 0.178280 0.062 Uiso 1 1 calc R U . . . H17C H 0.844287 0.206747 0.062782 0.062 Uiso 1 1 calc R U . . . C18 C 0.5831(9) 0.1439(8) -0.0612(6) 0.0391(18) Uani 1 1 d . . . . . H18A H 0.509951 0.165643 -0.087791 0.059 Uiso 1 1 calc R U . . . H18B H 0.545598 0.059226 -0.064111 0.059 Uiso 1 1 calc R U . . . H18C H 0.644324 0.165673 -0.106561 0.059 Uiso 1 1 calc R U . . . C19 C 0.6812(6) 0.2633(6) 0.4893(5) 0.0200(12) Uani 1 1 d . . . . . C20 C 0.7251(6) 0.1740(6) 0.4951(5) 0.0215(12) Uani 1 1 d . . . . . C21 C 0.7904(7) 0.1647(7) 0.5987(6) 0.0284(14) Uani 1 1 d . . . . . H21 H 0.821903 0.106412 0.604836 0.034 Uiso 1 1 calc R U . . . C22 C 0.8086(7) 0.2374(7) 0.6892(6) 0.0314(15) Uani 1 1 d . . . . . H22 H 0.855113 0.230782 0.757336 0.038 Uiso 1 1 calc R U . . . C23 C 0.7602(7) 0.3221(7) 0.6840(5) 0.0285(14) Uani 1 1 d . . . . . H23 H 0.772211 0.371257 0.748388 0.034 Uiso 1 1 calc R U . . . C24 C 0.6936(6) 0.3343(6) 0.5833(5) 0.0221(12) Uani 1 1 d . . . . . C25 C 0.6985(8) 0.0870(7) 0.3938(6) 0.0278(14) Uani 1 1 d . . . . . H25 H 0.690332 0.126023 0.330331 0.033 Uiso 1 1 calc R U . . . C26 C 0.8080(10) 0.0473(9) 0.3960(9) 0.049(2) Uani 1 1 d . . . . . H26A H 0.895980 0.112625 0.432384 0.074 Uiso 1 1 calc R U . . . H26B H 0.804840 0.020973 0.321783 0.074 Uiso 1 1 calc R U . . . H26C H 0.793654 -0.017456 0.435170 0.074 Uiso 1 1 calc R U . . . C27 C 0.5658(10) -0.0209(8) 0.3755(7) 0.043(2) Uani 1 1 d . . . . . H27A H 0.568386 -0.057335 0.439282 0.065 Uiso 1 1 calc R U . . . H27B H 0.551545 -0.076802 0.312155 0.065 Uiso 1 1 calc R U . . . H27C H 0.492050 0.002013 0.363315 0.065 Uiso 1 1 calc R U . . . C28 C 0.6322(8) 0.4212(7) 0.5794(5) 0.0281(14) Uani 1 1 d . . . . . H28 H 0.636588 0.451751 0.510890 0.034 Uiso 1 1 calc R U . . . C29 C 0.7056(10) 0.5259(8) 0.6738(6) 0.0395(19) Uani 1 1 d . . . . . H29A H 0.690640 0.499552 0.740721 0.059 Uiso 1 1 calc R U . . . H29B H 0.671117 0.583952 0.660333 0.059 Uiso 1 1 calc R U . . . H29C H 0.802180 0.561172 0.680716 0.059 Uiso 1 1 calc R U . . . C30 C 0.4828(9) 0.3603(8) 0.5775(6) 0.0358(17) Uani 1 1 d . . . . . H30A H 0.430756 0.302398 0.510260 0.054 Uiso 1 1 calc R U . . . H30B H 0.448113 0.418881 0.581634 0.054 Uiso 1 1 calc R U . . . H30C H 0.474826 0.321138 0.639376 0.054 Uiso 1 1 calc R U . . . C31 C 0.1750(9) -0.0183(8) 0.1476(7) 0.0394(18) Uani 1 1 d . . . . . H31A H 0.225577 -0.015689 0.095104 0.059 Uiso 1 1 calc R U . . . H31B H 0.078697 -0.064954 0.111946 0.059 Uiso 1 1 calc R U . . . H31C H 0.203782 -0.053954 0.206616 0.059 Uiso 1 1 calc R U . . . C32 C 0.1278(8) 0.1931(9) 0.0986(8) 0.043(2) Uani 1 1 d . . . . . H32A H 0.149097 0.274003 0.128074 0.064 Uiso 1 1 calc R U . . . H32B H 0.030071 0.145767 0.076474 0.064 Uiso 1 1 calc R U . . . H32C H 0.162051 0.191551 0.035859 0.064 Uiso 1 1 calc R U . . . C33 C 0.1380(8) 0.1293(8) 0.3216(7) 0.0377(18) Uani 1 1 d . . . . . H33A H 0.176997 0.093090 0.374625 0.057 Uiso 1 1 calc R U . . . H33B H 0.040008 0.083601 0.297220 0.057 Uiso 1 1 calc R U . . . H33C H 0.160716 0.209336 0.355066 0.057 Uiso 1 1 calc R U . . . 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 0.01652(11) 0.03538(14) 0.01886(12) 0.00792(9) 0.00608(9) 0.01196(11) Br1 0.0134(3) 0.0199(3) 0.0176(3) 0.0001(2) 0.0041(2) 0.0038(2) Si1 0.0146(8) 0.0330(9) 0.0206(8) 0.0027(7) 0.0056(6) 0.0105(7) C1 0.019(3) 0.023(3) 0.013(3) 0.001(2) 0.006(2) 0.010(2) C2 0.022(3) 0.027(3) 0.012(3) 0.003(2) 0.007(2) 0.015(3) C3 0.022(3) 0.032(3) 0.012(3) 0.004(2) 0.003(2) 0.017(3) C4 0.015(3) 0.026(3) 0.018(3) 0.001(2) 0.006(2) 0.012(2) C5 0.018(3) 0.029(3) 0.017(3) 0.004(2) 0.010(2) 0.011(3) C6 0.019(3) 0.028(3) 0.012(3) 0.002(2) 0.005(2) 0.014(3) C7 0.014(3) 0.034(3) 0.012(3) 0.004(2) 0.002(2) 0.011(3) C8 0.016(3) 0.040(4) 0.014(3) 0.007(3) 0.001(2) 0.010(3) C9 0.026(3) 0.041(4) 0.024(3) 0.014(3) 0.012(3) 0.015(3) C10 0.027(4) 0.055(5) 0.020(3) 0.013(3) 0.015(3) 0.017(3) C11 0.022(3) 0.057(5) 0.020(3) 0.011(3) 0.011(3) 0.023(3) C12 0.020(3) 0.043(4) 0.013(3) 0.007(3) 0.009(2) 0.018(3) C13 0.024(3) 0.036(4) 0.019(3) 0.013(3) 0.009(2) 0.017(3) C14 0.047(5) 0.029(4) 0.048(5) 0.011(3) 0.021(4) 0.017(4) C15 0.040(4) 0.072(6) 0.024(4) 0.008(4) 0.008(3) 0.040(5) C16 0.028(3) 0.044(4) 0.022(3) 0.005(3) 0.012(3) 0.023(3) C17 0.051(5) 0.051(5) 0.032(4) 0.001(4) 0.007(4) 0.034(4) C18 0.039(4) 0.049(5) 0.026(4) 0.000(3) 0.005(3) 0.019(4) C19 0.015(3) 0.031(3) 0.016(3) 0.008(2) 0.007(2) 0.011(2) C20 0.020(3) 0.031(3) 0.020(3) 0.010(3) 0.009(2) 0.015(3) C21 0.025(3) 0.039(4) 0.025(3) 0.014(3) 0.007(3) 0.017(3) C22 0.025(3) 0.044(4) 0.020(3) 0.014(3) 0.001(3) 0.012(3) C23 0.029(3) 0.033(4) 0.016(3) 0.004(3) 0.006(3) 0.007(3) C24 0.018(3) 0.027(3) 0.016(3) 0.001(2) 0.004(2) 0.006(3) C25 0.039(4) 0.036(4) 0.023(3) 0.010(3) 0.015(3) 0.026(3) C26 0.041(5) 0.043(5) 0.068(7) -0.004(4) 0.017(4) 0.024(4) C27 0.045(5) 0.046(5) 0.031(4) -0.007(3) 0.014(4) 0.014(4) C28 0.036(4) 0.038(4) 0.018(3) 0.004(3) 0.012(3) 0.021(3) C29 0.053(5) 0.042(4) 0.028(4) -0.003(3) 0.019(4) 0.022(4) C30 0.040(4) 0.056(5) 0.023(3) 0.006(3) 0.011(3) 0.032(4) C31 0.033(4) 0.041(4) 0.037(4) -0.003(3) 0.008(3) 0.012(4) C32 0.018(3) 0.058(5) 0.048(5) 0.018(4) 0.003(3) 0.014(3) C33 0.028(4) 0.048(5) 0.039(4) 0.002(3) 0.020(3) 0.015(3) _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 C1 2.325(6) . ? Pb1 Br1 2.8973(6) . ? Pb1 Br1 3.0587(6) 2_766 ? Si1 C32 1.848(9) . ? Si1 C31 1.858(9) . ? Si1 C33 1.873(8) . ? Si1 C4 1.886(6) . ? C1 C6 1.403(8) . ? C1 C2 1.418(8) . ? C2 C3 1.387(9) . ? C2 C7 1.512(8) . ? C3 C4 1.403(9) . ? C3 H3 0.9500 . ? C4 C5 1.399(9) . ? C5 C6 1.399(9) . ? C5 H5 0.9500 . ? C6 C19 1.508(8) . ? C7 C8 1.400(10) . ? C7 C12 1.426(8) . ? C8 C9 1.397(9) . ? C8 C13 1.539(10) . ? C9 C10 1.374(11) . ? C9 H9 0.9500 . ? C10 C11 1.381(12) . ? C10 H10 0.9500 . ? C11 C12 1.417(9) . ? C11 H11 0.9500 . ? C12 C16 1.515(11) . ? C13 C14 1.524(11) . ? C13 C15 1.542(10) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.535(10) . ? C16 C18 1.542(10) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.402(9) . ? C19 C20 1.419(9) . ? C20 C21 1.417(9) . ? C20 C25 1.536(9) . ? C21 C22 1.355(11) . ? C21 H21 0.9500 . ? C22 C23 1.398(11) . ? C22 H22 0.9500 . ? C23 C24 1.406(9) . ? C23 H23 0.9500 . ? C24 C28 1.530(10) . ? C25 C26 1.520(10) . ? C25 C27 1.522(12) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.530(10) . ? C28 C30 1.546(11) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pb1 Br1 92.11(14) . . ? C1 Pb1 Br1 108.09(15) . 2_766 ? Br1 Pb1 Br1 89.604(18) . 2_766 ? Pb1 Br1 Pb1 90.396(18) . 2_766 ? C32 Si1 C31 110.5(4) . . ? C32 Si1 C33 110.2(4) . . ? C31 Si1 C33 108.8(4) . . ? C32 Si1 C4 109.8(3) . . ? C31 Si1 C4 106.8(3) . . ? C33 Si1 C4 110.6(3) . . ? C6 C1 C2 118.5(6) . . ? C6 C1 Pb1 132.7(4) . . ? C2 C1 Pb1 108.8(4) . . ? C3 C2 C1 121.0(6) . . ? C3 C2 C7 121.1(5) . . ? C1 C2 C7 117.8(5) . . ? C2 C3 C4 121.0(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 117.5(6) . . ? C5 C4 Si1 119.0(5) . . ? C3 C4 Si1 123.3(5) . . ? C6 C5 C4 122.7(6) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C1 119.2(6) . . ? C5 C6 C19 117.6(6) . . ? C1 C6 C19 123.2(5) . . ? C8 C7 C12 120.6(6) . . ? C8 C7 C2 122.6(6) . . ? C12 C7 C2 116.8(6) . . ? C9 C8 C7 119.1(6) . . ? C9 C8 C13 119.6(7) . . ? C7 C8 C13 121.3(6) . . ? C10 C9 C8 120.8(7) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 121.0(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 120.4(7) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 117.9(7) . . ? C11 C12 C16 119.3(6) . . ? C7 C12 C16 122.8(6) . . ? C14 C13 C8 114.3(6) . . ? C14 C13 C15 110.7(7) . . ? C8 C13 C15 107.9(6) . . ? C14 C13 H13 107.9 . . ? C8 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C17 111.4(6) . . ? C12 C16 C18 111.0(6) . . ? C17 C16 C18 110.8(6) . . ? C12 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 121.0(6) . . ? C24 C19 C6 119.6(6) . . ? C20 C19 C6 119.3(6) . . ? C21 C20 C19 117.7(6) . . ? C21 C20 C25 120.7(6) . . ? C19 C20 C25 121.6(6) . . ? C22 C21 C20 121.2(7) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 121.2(6) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 119.9(6) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 118.9(6) . . ? C19 C24 C28 121.8(6) . . ? C23 C24 C28 119.3(6) . . ? C26 C25 C27 108.3(7) . . ? C26 C25 C20 114.7(7) . . ? C27 C25 C20 110.3(6) . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C20 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C24 113.7(6) . . ? C29 C28 C30 108.2(6) . . ? C24 C28 C30 111.0(6) . . ? C29 C28 H28 107.9 . . ? C24 C28 H28 107.9 . . ? C30 C28 H28 107.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.9(9) . . . . ? Pb1 C1 C2 C3 -179.2(5) . . . . ? C6 C1 C2 C7 -173.7(5) . . . . ? Pb1 C1 C2 C7 5.2(7) . . . . ? C1 C2 C3 C4 -3.5(9) . . . . ? C7 C2 C3 C4 172.0(6) . . . . ? C2 C3 C4 C5 1.3(9) . . . . ? C2 C3 C4 Si1 -173.4(5) . . . . ? C32 Si1 C4 C5 161.8(5) . . . . ? C31 Si1 C4 C5 -78.4(6) . . . . ? C33 Si1 C4 C5 39.9(6) . . . . ? C32 Si1 C4 C3 -23.6(7) . . . . ? C31 Si1 C4 C3 96.2(6) . . . . ? C33 Si1 C4 C3 -145.5(6) . . . . ? C3 C4 C5 C6 2.5(9) . . . . ? Si1 C4 C5 C6 177.4(5) . . . . ? C4 C5 C6 C1 -4.1(9) . . . . ? C4 C5 C6 C19 177.8(6) . . . . ? C2 C1 C6 C5 1.8(9) . . . . ? Pb1 C1 C6 C5 -176.8(5) . . . . ? C2 C1 C6 C19 179.7(6) . . . . ? Pb1 C1 C6 C19 1.1(9) . . . . ? C3 C2 C7 C8 94.9(8) . . . . ? C1 C2 C7 C8 -89.4(7) . . . . ? C3 C2 C7 C12 -88.3(7) . . . . ? C1 C2 C7 C12 87.4(7) . . . . ? C12 C7 C8 C9 -5.0(9) . . . . ? C2 C7 C8 C9 171.7(6) . . . . ? C12 C7 C8 C13 174.8(6) . . . . ? C2 C7 C8 C13 -8.5(9) . . . . ? C7 C8 C9 C10 2.9(10) . . . . ? C13 C8 C9 C10 -177.0(6) . . . . ? C8 C9 C10 C11 0.3(11) . . . . ? C9 C10 C11 C12 -1.3(11) . . . . ? C10 C11 C12 C7 -0.8(10) . . . . ? C10 C11 C12 C16 -179.8(6) . . . . ? C8 C7 C12 C11 4.0(9) . . . . ? C2 C7 C12 C11 -172.9(6) . . . . ? C8 C7 C12 C16 -177.0(6) . . . . ? C2 C7 C12 C16 6.1(9) . . . . ? C9 C8 C13 C14 -32.8(9) . . . . ? C7 C8 C13 C14 147.4(7) . . . . ? C9 C8 C13 C15 90.8(8) . . . . ? C7 C8 C13 C15 -89.1(8) . . . . ? C11 C12 C16 C17 66.9(8) . . . . ? C7 C12 C16 C17 -112.1(7) . . . . ? C11 C12 C16 C18 -57.0(8) . . . . ? C7 C12 C16 C18 124.0(7) . . . . ? C5 C6 C19 C24 -84.2(8) . . . . ? C1 C6 C19 C24 97.8(7) . . . . ? C5 C6 C19 C20 91.5(7) . . . . ? C1 C6 C19 C20 -86.5(8) . . . . ? C24 C19 C20 C21 -4.4(9) . . . . ? C6 C19 C20 C21 179.9(6) . . . . ? C24 C19 C20 C25 173.3(6) . . . . ? C6 C19 C20 C25 -2.4(9) . . . . ? C19 C20 C21 C22 0.9(10) . . . . ? C25 C20 C21 C22 -176.8(7) . . . . ? C20 C21 C22 C23 1.9(11) . . . . ? C21 C22 C23 C24 -1.3(11) . . . . ? C20 C19 C24 C23 5.0(10) . . . . ? C6 C19 C24 C23 -179.4(6) . . . . ? C20 C19 C24 C28 -172.7(6) . . . . ? C6 C19 C24 C28 2.9(9) . . . . ? C22 C23 C24 C19 -2.1(10) . . . . ? C22 C23 C24 C28 175.6(7) . . . . ? C21 C20 C25 C26 -35.8(10) . . . . ? C19 C20 C25 C26 146.6(7) . . . . ? C21 C20 C25 C27 86.8(8) . . . . ? C19 C20 C25 C27 -90.8(8) . . . . ? C19 C24 C28 C29 -153.1(7) . . . . ? C23 C24 C28 C29 29.2(9) . . . . ? C19 C24 C28 C30 84.6(8) . . . . ? C23 C24 C28 C30 -93.0(8) . . . . ? _refine_diff_density_max 3.613 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.209 _shelx_res_file ; TITL F1 in P-1 F1 2COMP TWIN 9MAR2018 JQ69TW53.res created by SHELXL-2017/1 at 15:58:00 on 02-Apr-2018 CELL 0.71073 11.3682 12.7595 12.9493 94.5630 103.1496 114.1017 ZERR 1.00 0.0009 0.0010 0.0010 0.0012 0.0010 0.0010 LATT 1 SFAC C H Br Pb Si UNIT 66 90 2 2 2 MERG 0 L.S. 9 HTAB WPDB -2 CONF BOND $H PLAN 20 SIZE 0.078 0.312 0.52 ACTA TEMP -183 FMAP 2 WGHT 0.055550 8.433100 BASF 0.52901 FVAR 0.44705 PB1 4 0.908098 0.450051 0.331261 11.00000 0.01652 0.03538 = 0.01886 0.00792 0.00608 0.01196 BR1 3 0.933098 0.630957 0.496604 11.00000 0.01337 0.01989 = 0.01756 0.00013 0.00413 0.00380 SI1 5 0.207166 0.132845 0.203121 11.00000 0.01464 0.03301 = 0.02061 0.00266 0.00563 0.01053 C1 1 0.680646 0.342427 0.313581 11.00000 0.01869 0.02347 = 0.01292 0.00062 0.00566 0.00980 C2 1 0.604902 0.348076 0.212538 11.00000 0.02232 0.02727 = 0.01221 0.00288 0.00663 0.01513 C3 1 0.465436 0.292420 0.181534 11.00000 0.02184 0.03226 = 0.01249 0.00425 0.00312 0.01681 AFIX 43 H3 2 0.416770 0.301046 0.115309 11.00000 -1.20000 AFIX 0 C4 1 0.395231 0.223598 0.246539 11.00000 0.01526 0.02618 = 0.01829 0.00109 0.00627 0.01152 C5 1 0.471106 0.215396 0.344396 11.00000 0.01767 0.02933 = 0.01699 0.00395 0.00985 0.01093 AFIX 43 H5 2 0.425486 0.166617 0.388096 11.00000 -1.20000 AFIX 0 C6 1 0.611419 0.276123 0.380469 11.00000 0.01865 0.02754 = 0.01221 0.00219 0.00543 0.01413 C7 1 0.681099 0.409213 0.136513 11.00000 0.01431 0.03384 = 0.01196 0.00436 0.00231 0.01138 C8 1 0.725897 0.529267 0.138117 11.00000 0.01596 0.03986 = 0.01394 0.00681 0.00130 0.01017 C9 1 0.810563 0.582138 0.075446 11.00000 0.02599 0.04107 = 0.02353 0.01445 0.01209 0.01493 AFIX 43 H9 2 0.844689 0.664198 0.078663 11.00000 -1.20000 AFIX 0 C10 1 0.845078 0.516933 0.009229 11.00000 0.02738 0.05462 = 0.02011 0.01328 0.01481 0.01674 AFIX 43 H10 2 0.903148 0.554661 -0.032438 11.00000 -1.20000 AFIX 0 C11 1 0.796691 0.397437 0.002295 11.00000 0.02242 0.05698 = 0.02009 0.01093 0.01134 0.02300 AFIX 43 H11 2 0.820163 0.353610 -0.045108 11.00000 -1.20000 AFIX 0 C12 1 0.712257 0.339770 0.065426 11.00000 0.01979 0.04266 = 0.01305 0.00712 0.00909 0.01843 C13 1 0.683474 0.603665 0.207118 11.00000 0.02427 0.03562 = 0.01925 0.01311 0.00908 0.01678 AFIX 13 H13 2 0.664069 0.565919 0.269956 11.00000 -1.20000 AFIX 0 C14 1 0.789661 0.729631 0.251312 11.00000 0.04696 0.02941 = 0.04844 0.01119 0.02088 0.01667 AFIX 137 H14A 2 0.873857 0.730043 0.292079 11.00000 -1.50000 H14B 2 0.758566 0.769338 0.299094 11.00000 -1.50000 H14C 2 0.804841 0.770510 0.191181 11.00000 -1.50000 AFIX 0 C15 1 0.551623 0.600094 0.137858 11.00000 0.04018 0.07187 = 0.02367 0.00787 0.00775 0.03963 AFIX 137 H15A 2 0.568522 0.638147 0.076421 11.00000 -1.50000 H15B 2 0.518292 0.641345 0.181970 11.00000 -1.50000 H15C 2 0.484284 0.518522 0.111180 11.00000 -1.50000 AFIX 0 C16 1 0.660844 0.208610 0.056468 11.00000 0.02765 0.04440 = 0.02218 0.00464 0.01231 0.02254 AFIX 13 H16 2 0.596954 0.182892 0.101312 11.00000 -1.20000 AFIX 0 C17 1 0.775763 0.175782 0.100857 11.00000 0.05064 0.05132 = 0.03157 0.00129 0.00723 0.03436 AFIX 137 H17A 2 0.740383 0.090395 0.089849 11.00000 -1.50000 H17B 2 0.815990 0.209245 0.178280 11.00000 -1.50000 H17C 2 0.844287 0.206747 0.062782 11.00000 -1.50000 AFIX 0 C18 1 0.583100 0.143895 -0.061216 11.00000 0.03920 0.04863 = 0.02563 -0.00043 0.00465 0.01940 AFIX 137 H18A 2 0.509951 0.165643 -0.087791 11.00000 -1.50000 H18B 2 0.545598 0.059226 -0.064111 11.00000 -1.50000 H18C 2 0.644324 0.165673 -0.106561 11.00000 -1.50000 AFIX 0 C19 1 0.681192 0.263349 0.489266 11.00000 0.01516 0.03124 = 0.01633 0.00766 0.00744 0.01062 C20 1 0.725071 0.174034 0.495138 11.00000 0.02031 0.03054 = 0.02000 0.00990 0.00905 0.01476 C21 1 0.790357 0.164709 0.598719 11.00000 0.02548 0.03870 = 0.02521 0.01406 0.00736 0.01660 AFIX 43 H21 2 0.821903 0.106412 0.604836 11.00000 -1.20000 AFIX 0 C22 1 0.808584 0.237429 0.689158 11.00000 0.02532 0.04355 = 0.02008 0.01412 0.00072 0.01166 AFIX 43 H22 2 0.855113 0.230782 0.757336 11.00000 -1.20000 AFIX 0 C23 1 0.760159 0.322089 0.683981 11.00000 0.02914 0.03292 = 0.01612 0.00374 0.00564 0.00711 AFIX 43 H23 2 0.772211 0.371257 0.748388 11.00000 -1.20000 AFIX 0 C24 1 0.693588 0.334346 0.583289 11.00000 0.01834 0.02749 = 0.01562 0.00102 0.00442 0.00620 C25 1 0.698456 0.087011 0.393806 11.00000 0.03861 0.03565 = 0.02333 0.01000 0.01454 0.02615 AFIX 13 H25 2 0.690332 0.126023 0.330331 11.00000 -1.20000 AFIX 0 C26 1 0.807955 0.047259 0.395979 11.00000 0.04064 0.04330 = 0.06840 -0.00418 0.01700 0.02415 AFIX 137 H26A 2 0.895980 0.112625 0.432384 11.00000 -1.50000 H26B 2 0.804840 0.020973 0.321783 11.00000 -1.50000 H26C 2 0.793654 -0.017456 0.435170 11.00000 -1.50000 AFIX 0 C27 1 0.565805 -0.020880 0.375511 11.00000 0.04500 0.04649 = 0.03054 -0.00657 0.01377 0.01402 AFIX 137 H27A 2 0.568386 -0.057335 0.439282 11.00000 -1.50000 H27B 2 0.551545 -0.076802 0.312155 11.00000 -1.50000 H27C 2 0.492050 0.002013 0.363315 11.00000 -1.50000 AFIX 0 C28 1 0.632224 0.421188 0.579364 11.00000 0.03577 0.03831 = 0.01758 0.00367 0.01202 0.02129 AFIX 13 H28 2 0.636588 0.451751 0.510890 11.00000 -1.20000 AFIX 0 C29 1 0.705637 0.525873 0.673766 11.00000 0.05321 0.04161 = 0.02763 -0.00308 0.01930 0.02238 AFIX 137 H29A 2 0.690640 0.499552 0.740721 11.00000 -1.50000 H29B 2 0.671117 0.583952 0.660333 11.00000 -1.50000 H29C 2 0.802180 0.561172 0.680716 11.00000 -1.50000 AFIX 0 C30 1 0.482805 0.360332 0.577487 11.00000 0.04003 0.05641 = 0.02284 0.00601 0.01057 0.03200 AFIX 137 H30A 2 0.430756 0.302398 0.510260 11.00000 -1.50000 H30B 2 0.448113 0.418881 0.581634 11.00000 -1.50000 H30C 2 0.474826 0.321138 0.639376 11.00000 -1.50000 AFIX 0 C31 1 0.175005 -0.018296 0.147641 11.00000 0.03322 0.04085 = 0.03686 -0.00287 0.00787 0.01229 AFIX 137 H31A 2 0.225577 -0.015689 0.095104 11.00000 -1.50000 H31B 2 0.078697 -0.064954 0.111946 11.00000 -1.50000 H31C 2 0.203782 -0.053954 0.206616 11.00000 -1.50000 AFIX 0 C32 1 0.127775 0.193118 0.098612 11.00000 0.01828 0.05805 = 0.04761 0.01807 0.00262 0.01444 AFIX 137 H32A 2 0.149097 0.274003 0.128074 11.00000 -1.50000 H32B 2 0.030071 0.145767 0.076474 11.00000 -1.50000 H32C 2 0.162051 0.191551 0.035859 11.00000 -1.50000 AFIX 0 C33 1 0.137976 0.129295 0.321631 11.00000 0.02844 0.04827 = 0.03882 0.00248 0.02032 0.01458 AFIX 137 H33A 2 0.176997 0.093090 0.374625 11.00000 -1.50000 H33B 2 0.040008 0.083601 0.297220 11.00000 -1.50000 H33C 2 0.160716 0.209336 0.355066 11.00000 -1.50000 rem PART -1 rem PB2 4 0.1019 0.3125 0.1367 0.02000 10.025 1.84 AFIX 0 HKLF 5 REM F1 in P-1 F1 2COMP TWIN 9MAR2018 REM R1 = 0.0402 for 7230 Fo > 4sig(Fo) and 0.0416 for all 7514 data REM 337 parameters refined using 0 restraints END WGHT 0.0555 8.4333 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 3.613, deepest hole -1.892, 1-sigma level 0.209 Q1 1 0.9042 0.4738 0.3857 11.00000 0.05 2.02 Q2 1 0.1019 0.3125 0.1367 11.00000 0.05 1.84 Q3 1 0.9000 0.5172 0.3327 11.00000 0.05 1.43 Q4 1 0.9504 0.4051 0.3380 11.00000 0.05 1.37 Q5 1 0.9096 0.2013 0.7843 11.00000 0.05 1.31 Q6 1 0.8471 0.3820 0.3161 11.00000 0.05 1.07 Q7 1 0.9638 0.5178 0.3462 11.00000 0.05 1.05 Q8 1 0.9209 0.2585 0.1841 11.00000 0.05 0.90 Q9 1 -0.0882 -0.0545 0.2586 11.00000 0.05 0.80 Q10 1 0.9802 0.6209 0.6249 11.00000 0.05 0.79 Q11 1 0.9136 -0.0385 0.4203 11.00000 0.05 0.76 Q12 1 0.7937 0.7166 0.3025 11.00000 0.05 0.69 Q13 1 0.1930 0.0670 0.1943 11.00000 0.05 0.69 Q14 1 0.9055 0.4012 0.2476 11.00000 0.05 0.62 Q15 1 0.8976 0.5061 0.6998 11.00000 0.05 0.62 Q16 1 0.9312 0.5215 0.4586 11.00000 0.05 0.59 Q17 1 0.2700 0.1878 0.2209 11.00000 0.05 0.57 Q18 1 0.8059 0.1029 0.3456 11.00000 0.05 0.57 Q19 1 0.8183 0.5816 0.5260 11.00000 0.05 0.57 Q20 1 0.9169 0.6996 0.7255 11.00000 0.05 0.54 ; _shelx_res_checksum 23238 _shelx_hkl_file ; 1 0 0 2209.26 70.6405 -1 1 0 0 2209.26 70.6405 2 2 0 0 221.193 7.47527 -1 2 0 0 221.193 7.47527 2 3 0 0 547.715 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