data_sab14 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H31 B Br N O5 S' _chemical_formula_weight 548.29 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' 'B' 'B' 0.0013 0.0007 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.1308(9) _cell_length_b 19.2458(10) _cell_length_c 18.6533(10) _cell_angle_alpha 90 _cell_angle_beta 115.2273(6) _cell_angle_gamma 90 _cell_volume 5888.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9813 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.58 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas not_measured _exptl_crystal_density_method not_measured _exptl_crystal_density_diffrn 1.237 _exptl_crystal_F_000 2272 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.557 _exptl_crystal_size_mid 0.465 _exptl_crystal_size_min 0.400 _exptl_absorpt_coefficient_mu 1.498 _shelx_estimated_absorpt_T_min 0.489 _shelx_estimated_absorpt_T_max 0.586 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5569 _exptl_absorpt_correction_T_max 0.6648 _exptl_absorpt_process_details 'Bruker SADABS 2014/5' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 67751 _diffrn_reflns_av_unetI/netI 0.0297 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.312 _diffrn_reflns_theta_max 27.102 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 12992 _reflns_number_gt 10471 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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 'Bruker APEX2 2014.11-0, 2014' _computing_cell_refinement 'Bruker SAINT 8.34a, 2013' _computing_data_reduction 'Bruker SAINT 8.34a, 2013' _computing_structure_solution 'Bruker SHELXTL 2014/7' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; A colorless crystal of approximate dimensions 0.557 x 0.465 x 0.400 mm was mounted on a glass fiber and transferred to a Bruker SMART APEX II diffractometer. The APEX2 program package was used to determine the unit-cell parameters and for data collection (10 sec/frame scan time for a sphere of diffraction data). The raw frame data was processed using SAINT and SADABS to yield the reflection data file. Subsequent calculations were carried out using the SHELXTL program. The diffraction symmetry was 2/m and the systematic absences were consistent with the monoclinic space group P21/n that was later determined to be correct. The structure was solved by direct methods and refined on F2 by full-matrix least-squares techniques. The analytical scattering factors for neutral atoms were used throughout the analysis. Hydrogen atoms were included using a riding model. There were two molecules of the formula-unit present. Atoms C(37), C(41) and C(43) were disordered and included using multiple components with partial site-occupancy factors. At convergence, wR2 = 0.0882 and Goof = 1.041 for 650 variables refined against 12992 data (0.78Å), R1 = 0.0344 for those 10471 data with I > 2.0sigma(I). There were several high residuals present in the final difference-Fourier map. It was not possible to determine the nature of the residuals although it was probable that hexane solvent was present. The SQUEEZE routine in the PLATON program package was used to account for the electrons in the solvent accessible voids. ; _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^)+(0.0428P)^2^+2.5436P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12992 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _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 Br1 Br 0.65300(2) 0.98912(2) 0.71850(2) 0.03568(7) Uani 1 1 d . . . . . S1 S 0.67446(3) 0.61500(2) 0.76366(3) 0.02144(10) Uani 1 1 d . . . . . O1 O 0.48933(8) 0.85557(7) 0.85982(8) 0.0245(3) Uani 1 1 d . . . . . O2 O 0.44019(8) 0.74716(7) 0.86423(9) 0.0279(3) Uani 1 1 d . . . . . O3 O 0.75057(8) 0.63276(7) 0.76320(8) 0.0265(3) Uani 1 1 d . . . . . O4 O 0.66840(8) 0.55764(7) 0.80918(8) 0.0266(3) Uani 1 1 d . . . . . O5 O 0.42731(9) 0.59335(9) 0.43457(9) 0.0359(4) Uani 1 1 d . . . . . N1 N 0.64623(9) 0.68647(8) 0.79807(9) 0.0186(3) Uani 1 1 d . . . . . B1 B 0.49535(12) 0.78589(11) 0.85007(12) 0.0199(4) Uani 1 1 d . . . . . C1 C 0.65555(11) 0.75389(9) 0.77257(10) 0.0179(4) Uani 1 1 d . . . . . C2 C 0.70607(11) 0.77883(10) 0.73928(11) 0.0225(4) Uani 1 1 d . . . . . H2A H 0.7415 0.7487 0.7284 0.027 Uiso 1 1 calc R U . . . C3 C 0.70279(12) 0.84896(10) 0.72262(12) 0.0249(4) Uani 1 1 d . . . . . H3A H 0.7364 0.8676 0.6997 0.030 Uiso 1 1 calc R U . . . C4 C 0.65068(12) 0.89277(10) 0.73907(11) 0.0229(4) Uani 1 1 d . . . . . C5 C 0.60036(11) 0.86892(10) 0.77163(11) 0.0205(4) Uani 1 1 d . . . . . H5A H 0.5653 0.8996 0.7824 0.025 Uiso 1 1 calc R U . . . C6 C 0.60256(10) 0.79780(9) 0.78842(10) 0.0175(4) Uani 1 1 d . . . . . C7 C 0.55848(10) 0.75665(9) 0.82257(10) 0.0174(4) Uani 1 1 d . . . . . C8 C 0.58532(10) 0.68961(10) 0.82686(10) 0.0178(4) Uani 1 1 d . . . . . C9 C 0.56428(11) 0.62833(10) 0.86394(11) 0.0203(4) Uani 1 1 d . . . . . H9A H 0.5555 0.5874 0.8291 0.024 Uiso 1 1 calc R U . . . H9B H 0.5125 0.6379 0.8679 0.024 Uiso 1 1 calc R U . . . C10 C 0.63079(12) 0.61100(10) 0.94700(11) 0.0242(4) Uani 1 1 d . . . . . H10A H 0.6233 0.5626 0.9605 0.029 Uiso 1 1 calc R U . . . H10B H 0.6849 0.6141 0.9461 0.029 Uiso 1 1 calc R U . . . C11 C 0.62917(13) 0.65909(11) 1.01046(12) 0.0289(4) Uani 1 1 d . . . . . H11A H 0.5766 0.6534 1.0140 0.035 Uiso 1 1 calc R U . . . H11B H 0.6325 0.7078 0.9949 0.035 Uiso 1 1 calc R U . . . C12 C 0.69864(16) 0.64547(12) 1.09171(13) 0.0417(6) Uani 1 1 d . . . . . H12A H 0.6949 0.6782 1.1303 0.063 Uiso 1 1 calc R U . . . H12B H 0.7510 0.6516 1.0888 0.063 Uiso 1 1 calc R U . . . H12C H 0.6947 0.5978 1.1083 0.063 Uiso 1 1 calc R U . . . C13 C 0.41623(12) 0.86650(11) 0.87347(13) 0.0289(5) Uani 1 1 d . . . . . C14 C 0.40092(12) 0.79392(11) 0.89995(13) 0.0296(5) Uani 1 1 d . . . . . C15 C 0.34967(15) 0.88903(16) 0.79465(16) 0.0516(7) Uani 1 1 d . . . . . H15A H 0.3004 0.9008 0.8015 0.077 Uiso 1 1 calc R U . . . H15B H 0.3375 0.8510 0.7563 0.077 Uiso 1 1 calc R U . . . H15C H 0.3680 0.9298 0.7752 0.077 Uiso 1 1 calc R U . . . C16 C 0.43545(16) 0.92277(13) 0.93568(17) 0.0486(7) Uani 1 1 d . . . . . H16A H 0.3893 0.9281 0.9495 0.073 Uiso 1 1 calc R U . . . H16B H 0.4452 0.9668 0.9147 0.073 Uiso 1 1 calc R U . . . H16C H 0.4843 0.9098 0.9831 0.073 Uiso 1 1 calc R U . . . C17 C 0.31183(14) 0.77306(14) 0.86868(17) 0.0474(7) Uani 1 1 d . . . . . H17A H 0.2824 0.8076 0.8851 0.071 Uiso 1 1 calc R U . . . H17B H 0.3077 0.7274 0.8901 0.071 Uiso 1 1 calc R U . . . H17C H 0.2879 0.7707 0.8107 0.071 Uiso 1 1 calc R U . . . C18 C 0.44442(15) 0.78137(15) 0.98886(14) 0.0454(6) Uani 1 1 d . . . . . H18A H 0.4181 0.8087 1.0158 0.068 Uiso 1 1 calc R U . . . H18B H 0.5016 0.7954 1.0082 0.068 Uiso 1 1 calc R U . . . H18C H 0.4415 0.7319 0.9999 0.068 Uiso 1 1 calc R U . . . C19 C 0.60017(12) 0.60700(10) 0.66604(11) 0.0228(4) Uani 1 1 d . . . . . C20 C 0.61350(13) 0.63604(11) 0.60401(12) 0.0286(4) Uani 1 1 d . . . . . H20A H 0.6630 0.6597 0.6145 0.034 Uiso 1 1 calc R U . . . C21 C 0.55427(13) 0.63008(12) 0.52740(13) 0.0330(5) Uani 1 1 d . . . . . H21A H 0.5631 0.6496 0.4850 0.040 Uiso 1 1 calc R U . . . C22 C 0.48157(12) 0.59559(11) 0.51191(12) 0.0281(4) Uani 1 1 d . . . . . C23 C 0.46861(12) 0.56630(11) 0.57372(12) 0.0272(4) Uani 1 1 d . . . . . H23A H 0.4191 0.5426 0.5631 0.033 Uiso 1 1 calc R U . . . C24 C 0.52785(12) 0.57181(10) 0.65043(12) 0.0252(4) Uani 1 1 d . . . . . H24A H 0.5193 0.5515 0.6927 0.030 Uiso 1 1 calc R U . . . C25 C 0.35328(13) 0.55544(13) 0.41402(13) 0.0364(5) Uani 1 1 d . . . . . H25A H 0.3221 0.5552 0.3563 0.055 Uiso 1 1 calc R U . . . H25B H 0.3209 0.5775 0.4385 0.055 Uiso 1 1 calc R U . . . H25C H 0.3661 0.5076 0.4332 0.055 Uiso 1 1 calc R U . . . Br2 Br 0.84558(2) 0.65309(2) 0.64160(2) 0.03165(6) Uani 1 1 d . . . . . S2 S 0.77051(3) 0.34416(3) 0.39456(3) 0.02839(12) Uani 1 1 d . . . . . O6 O 0.60171(9) 0.64477(8) 0.34721(10) 0.0409(4) Uani 1 1 d . . . . . O7 O 0.54370(9) 0.57338(9) 0.24043(9) 0.0413(4) Uani 1 1 d . . . . . O8 O 0.85197(9) 0.33795(8) 0.45420(10) 0.0361(4) Uani 1 1 d . . . . . O9 O 0.75037(9) 0.32356(8) 0.31527(9) 0.0369(4) Uani 1 1 d . . . . . O10 O 0.55163(10) 0.20863(10) 0.50937(10) 0.0498(5) Uani 1 1 d . . . . . N2 N 0.74810(10) 0.42967(8) 0.39204(10) 0.0251(4) Uani 1 1 d . . . . . B2 B 0.60407(14) 0.58226(13) 0.31433(14) 0.0282(5) Uani 1 1 d . . . . . C26 C 0.77781(11) 0.47225(10) 0.46048(11) 0.0223(4) Uani 1 1 d . . . . . C27 C 0.84300(11) 0.46354(10) 0.53472(12) 0.0252(4) Uani 1 1 d . . . . . H27A H 0.8743 0.4220 0.5480 0.030 Uiso 1 1 calc R U . . . C28 C 0.86029(12) 0.51759(11) 0.58820(12) 0.0261(4) Uani 1 1 d . . . . . H28A H 0.9038 0.5131 0.6395 0.031 Uiso 1 1 calc R U . . . C29 C 0.81443(12) 0.57873(10) 0.56749(11) 0.0244(4) Uani 1 1 d . . . . . C30 C 0.74928(11) 0.58751(10) 0.49489(11) 0.0232(4) Uani 1 1 d . . . . . H30A H 0.7182 0.6292 0.4823 0.028 Uiso 1 1 calc R U . . . C31 C 0.73037(11) 0.53318(10) 0.44039(11) 0.0216(4) Uani 1 1 d . . . . . C32 C 0.66921(11) 0.52660(11) 0.35969(11) 0.0241(4) Uani 1 1 d . . . . . C33 C 0.68080(11) 0.46372(11) 0.33198(12) 0.0252(4) Uani 1 1 d . . . . . C34 C 0.63709(12) 0.43686(11) 0.24927(12) 0.0297(5) Uani 1 1 d . . . . . H34A H 0.5827 0.4590 0.2239 0.036 Uiso 1 1 calc R U . . . H34B H 0.6288 0.3862 0.2512 0.036 Uiso 1 1 calc R U . . . C35 C 0.68344(14) 0.45081(14) 0.19853(13) 0.0395(6) Uani 1 1 d . . . . . H35A H 0.6984 0.5006 0.2025 0.047 Uiso 1 1 calc R U . . . H35B H 0.7345 0.4234 0.2196 0.047 Uiso 1 1 calc R U . . . C36 C 0.63317(16) 0.43201(15) 0.11143(14) 0.0481(7) Uani 1 1 d . . . . . H36A H 0.6137 0.3835 0.1081 0.058 Uiso 0.55 1 calc R U P A 1 H36B H 0.6686 0.4344 0.0832 0.058 Uiso 0.55 1 calc R U P A 1 H36C H 0.6073 0.3861 0.1079 0.058 Uiso 0.45 1 calc R U P B 2 H36D H 0.5894 0.4668 0.0866 0.058 Uiso 0.45 1 calc R U P B 2 C37 C 0.5551(3) 0.4830(2) 0.0674(2) 0.0455(12) Uani 0.55 1 d . . P C 1 H37A H 0.5266 0.4699 0.0115 0.068 Uiso 0.55 1 calc R U P C 1 H37B H 0.5738 0.5312 0.0715 0.068 Uiso 0.55 1 calc R U P C 1 H37C H 0.5179 0.4785 0.0928 0.068 Uiso 0.55 1 calc R U P C 1 C37B C 0.6870(4) 0.4299(3) 0.0668(3) 0.0552(16) Uani 0.45 1 d . . P C 2 H37D H 0.6540 0.4161 0.0117 0.083 Uiso 0.45 1 calc R U P C 2 H37E H 0.7310 0.3962 0.0921 0.083 Uiso 0.45 1 calc R U P C 2 H37F H 0.7103 0.4760 0.0680 0.083 Uiso 0.45 1 calc R U P C 2 C38 C 0.54175(13) 0.68816(13) 0.28409(15) 0.0415(6) Uani 1 1 d . . . . . C39 C 0.48836(13) 0.63279(13) 0.22454(13) 0.0371(5) Uani 1 1 d . . . . . C40 C 0.49850(17) 0.73297(14) 0.32058(17) 0.0573(8) Uani 1 1 d . . . . . H40A H 0.4564 0.7606 0.2791 0.086 Uiso 1 1 calc R U . . . H40B H 0.5379 0.7641 0.3599 0.086 Uiso 1 1 calc R U . . . H40C H 0.4731 0.7033 0.3464 0.086 Uiso 1 1 calc R U . . . C41 C 0.5921(3) 0.7373(3) 0.2609(4) 0.0319(12) Uiso 0.5 1 d . . P D 1 H41A H 0.6320 0.7605 0.3083 0.048 Uiso 0.5 1 calc R U P D 1 H41B H 0.5564 0.7721 0.2241 0.048 Uiso 0.5 1 calc R U P D 1 H41C H 0.6206 0.7113 0.2352 0.048 Uiso 0.5 1 calc R U P D 1 C41B C 0.5859(4) 0.7200(4) 0.2313(5) 0.0458(18) Uiso 0.4 1 d . . P D 2 H41D H 0.6067 0.6819 0.2102 0.069 Uiso 0.4 1 calc R U P D 2 H41E H 0.6313 0.7500 0.2646 0.069 Uiso 0.4 1 calc R U P D 2 H41F H 0.5464 0.7472 0.1873 0.069 Uiso 0.4 1 calc R U P D 2 C41C C 0.5923(12) 0.7535(11) 0.2854(13) 0.019(5) Uiso 0.1 1 d . . P D 3 H41G H 0.6187 0.7718 0.3395 0.028 Uiso 0.1 1 calc R U P D 3 H41H H 0.5561 0.7890 0.2502 0.028 Uiso 0.1 1 calc R U P D 3 H41I H 0.6339 0.7411 0.2672 0.028 Uiso 0.1 1 calc R U P D 3 C42 C 0.41850(14) 0.60826(14) 0.24206(19) 0.0532(7) Uani 1 1 d . . . . . H42A H 0.3787 0.6459 0.2311 0.080 Uiso 1 1 calc R U . . . H42B H 0.4393 0.5948 0.2979 0.080 Uiso 1 1 calc R U . . . H42C H 0.3921 0.5682 0.2085 0.080 Uiso 1 1 calc R U . . . C43 C 0.4664(6) 0.6625(4) 0.1402(6) 0.0418(18) Uani 0.55 1 d . . P E 1 H43A H 0.4297 0.7024 0.1306 0.063 Uiso 0.55 1 calc R U P E 1 H43B H 0.4393 0.6265 0.1005 0.063 Uiso 0.55 1 calc R U P E 1 H43C H 0.5163 0.6774 0.1364 0.063 Uiso 0.55 1 calc R U P E 1 C43B C 0.4465(8) 0.6376(5) 0.1353(8) 0.054(3) Uani 0.45 1 d . . P E 2 H43D H 0.4102 0.6780 0.1198 0.081 Uiso 0.45 1 calc R U P E 2 H43E H 0.4146 0.5953 0.1137 0.081 Uiso 0.45 1 calc R U P E 2 H43F H 0.4875 0.6426 0.1144 0.081 Uiso 0.45 1 calc R U P E 2 C44 C 0.70434(12) 0.30358(10) 0.42740(12) 0.0258(4) Uani 1 1 d . . . . . C45 C 0.72694(13) 0.29560(11) 0.50821(12) 0.0312(5) Uani 1 1 d . . . . . H45A H 0.7783 0.3123 0.5456 0.037 Uiso 1 1 calc R U . . . C46 C 0.67490(14) 0.26356(12) 0.53375(13) 0.0359(5) Uani 1 1 d . . . . . H46A H 0.6904 0.2579 0.5889 0.043 Uiso 1 1 calc R U . . . C47 C 0.59919(13) 0.23924(12) 0.47900(13) 0.0341(5) Uani 1 1 d . . . . . C48 C 0.57701(13) 0.24662(11) 0.39845(12) 0.0318(5) Uani 1 1 d . . . . . H48A H 0.5259 0.2295 0.3612 0.038 Uiso 1 1 calc R U . . . C49 C 0.62941(12) 0.27896(11) 0.37232(12) 0.0290(5) Uani 1 1 d . . . . . H49A H 0.6143 0.2843 0.3172 0.035 Uiso 1 1 calc R U . . . C50 C 0.47417(18) 0.18127(18) 0.45744(19) 0.0685(9) Uani 1 1 d . . . . . H50A H 0.4471 0.1622 0.4887 0.103 Uiso 1 1 calc R U . . . H50B H 0.4816 0.1444 0.4249 0.103 Uiso 1 1 calc R U . . . H50C H 0.4406 0.2184 0.4230 0.103 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 Br1 0.04574(14) 0.02162(11) 0.04714(14) 0.00433(9) 0.02695(11) -0.00419(9) S1 0.0221(2) 0.0208(2) 0.0233(2) -0.00030(18) 0.0115(2) 0.00428(18) O1 0.0222(7) 0.0266(7) 0.0295(7) -0.0051(6) 0.0156(6) 0.0007(6) O2 0.0235(7) 0.0294(8) 0.0384(8) -0.0065(6) 0.0206(7) -0.0024(6) O3 0.0224(7) 0.0289(7) 0.0316(8) 0.0003(6) 0.0148(6) 0.0068(6) O4 0.0314(8) 0.0221(7) 0.0282(7) 0.0027(6) 0.0145(6) 0.0056(6) O5 0.0297(8) 0.0506(10) 0.0248(8) 0.0012(7) 0.0090(6) -0.0045(7) N1 0.0183(8) 0.0188(8) 0.0201(8) -0.0008(6) 0.0095(6) 0.0007(6) B1 0.0164(10) 0.0269(11) 0.0129(9) -0.0033(8) 0.0029(8) -0.0014(8) C1 0.0154(9) 0.0202(9) 0.0160(8) -0.0019(7) 0.0045(7) -0.0020(7) C2 0.0188(9) 0.0274(10) 0.0245(10) -0.0009(8) 0.0123(8) -0.0009(8) C3 0.0219(10) 0.0301(10) 0.0264(10) 0.0011(8) 0.0137(8) -0.0047(8) C4 0.0251(10) 0.0187(9) 0.0232(10) 0.0010(8) 0.0089(8) -0.0049(8) C5 0.0189(9) 0.0206(9) 0.0207(9) -0.0021(7) 0.0073(8) 0.0003(7) C6 0.0144(8) 0.0222(9) 0.0144(8) -0.0022(7) 0.0047(7) -0.0005(7) C7 0.0149(9) 0.0218(9) 0.0134(8) -0.0023(7) 0.0041(7) -0.0033(7) C8 0.0143(8) 0.0234(9) 0.0149(8) -0.0019(7) 0.0054(7) -0.0015(7) C9 0.0202(9) 0.0212(9) 0.0212(9) -0.0025(7) 0.0104(8) -0.0038(7) C10 0.0273(10) 0.0222(10) 0.0231(10) 0.0033(8) 0.0108(8) -0.0018(8) C11 0.0348(12) 0.0287(11) 0.0220(10) 0.0018(8) 0.0110(9) -0.0025(9) C12 0.0553(16) 0.0349(13) 0.0251(11) 0.0034(10) 0.0076(11) -0.0101(11) C13 0.0192(10) 0.0365(12) 0.0342(11) -0.0071(9) 0.0147(9) 0.0038(8) C14 0.0229(10) 0.0379(12) 0.0353(12) -0.0097(9) 0.0195(9) -0.0007(9) C15 0.0338(13) 0.0677(19) 0.0496(16) 0.0121(13) 0.0143(12) 0.0247(13) C16 0.0462(15) 0.0463(15) 0.0700(18) -0.0255(13) 0.0407(14) -0.0053(12) C17 0.0260(12) 0.0541(15) 0.0731(18) -0.0227(14) 0.0315(13) -0.0087(11) C18 0.0451(14) 0.0646(17) 0.0391(14) 0.0036(12) 0.0301(12) 0.0079(13) C19 0.0271(10) 0.0218(10) 0.0221(10) -0.0033(8) 0.0131(8) 0.0021(8) C20 0.0277(11) 0.0334(11) 0.0282(11) -0.0012(9) 0.0153(9) -0.0028(9) C21 0.0330(12) 0.0434(13) 0.0273(11) 0.0041(10) 0.0174(10) -0.0025(10) C22 0.0273(11) 0.0322(11) 0.0247(10) -0.0019(9) 0.0108(9) 0.0015(9) C23 0.0249(10) 0.0286(11) 0.0305(11) -0.0040(9) 0.0141(9) -0.0038(8) C24 0.0326(11) 0.0228(10) 0.0255(10) -0.0012(8) 0.0175(9) 0.0009(8) C25 0.0295(12) 0.0439(13) 0.0316(12) -0.0033(10) 0.0091(10) -0.0022(10) Br2 0.03254(12) 0.03714(12) 0.02852(11) -0.00602(9) 0.01613(9) -0.00711(9) S2 0.0224(2) 0.0260(3) 0.0322(3) -0.0010(2) 0.0072(2) 0.0023(2) O6 0.0302(8) 0.0297(8) 0.0407(9) 0.0099(7) -0.0062(7) 0.0051(7) O7 0.0328(8) 0.0580(11) 0.0230(8) 0.0043(7) 0.0021(7) 0.0222(8) O8 0.0217(7) 0.0325(8) 0.0459(9) 0.0001(7) 0.0066(7) 0.0039(6) O9 0.0371(9) 0.0376(9) 0.0363(9) -0.0053(7) 0.0160(7) 0.0029(7) O10 0.0325(9) 0.0667(12) 0.0404(10) 0.0108(9) 0.0061(8) -0.0146(8) N2 0.0195(8) 0.0248(9) 0.0249(9) 0.0019(7) 0.0036(7) -0.0007(7) B2 0.0184(11) 0.0375(13) 0.0275(12) 0.0115(10) 0.0086(9) 0.0012(10) C26 0.0178(9) 0.0222(9) 0.0259(10) 0.0049(8) 0.0083(8) -0.0024(7) C27 0.0185(9) 0.0235(10) 0.0282(10) 0.0066(8) 0.0047(8) 0.0004(8) C28 0.0200(10) 0.0325(11) 0.0218(10) 0.0081(8) 0.0051(8) -0.0020(8) C29 0.0239(10) 0.0293(10) 0.0234(10) -0.0013(8) 0.0133(8) -0.0077(8) C30 0.0207(9) 0.0258(10) 0.0265(10) 0.0076(8) 0.0132(8) 0.0021(8) C31 0.0158(9) 0.0270(10) 0.0214(9) 0.0078(8) 0.0072(8) 0.0001(8) C32 0.0170(9) 0.0309(11) 0.0226(10) 0.0062(8) 0.0067(8) -0.0025(8) C33 0.0163(9) 0.0324(11) 0.0234(10) 0.0057(8) 0.0050(8) -0.0030(8) C34 0.0225(10) 0.0349(12) 0.0261(11) 0.0020(9) 0.0048(9) -0.0050(9) C35 0.0349(12) 0.0530(15) 0.0286(12) -0.0019(11) 0.0114(10) -0.0151(11) C36 0.0539(16) 0.0571(17) 0.0343(13) -0.0127(12) 0.0199(12) -0.0220(13) C37 0.048(3) 0.054(3) 0.026(2) 0.000(2) 0.007(2) -0.022(2) C37B 0.066(4) 0.058(4) 0.033(3) -0.007(3) 0.012(3) -0.021(3) C38 0.0252(11) 0.0393(13) 0.0451(14) 0.0236(11) 0.0006(10) 0.0066(10) C39 0.0269(11) 0.0489(14) 0.0281(11) 0.0095(10) 0.0045(9) 0.0171(10) C40 0.0553(17) 0.0401(15) 0.0510(16) 0.0055(12) -0.0018(13) 0.0190(13) C42 0.0255(12) 0.0476(15) 0.077(2) 0.0039(14) 0.0128(13) 0.0046(11) C43 0.048(5) 0.048(5) 0.024(3) 0.010(3) 0.010(3) 0.019(3) C43B 0.051(6) 0.051(6) 0.043(5) 0.024(5) 0.003(4) 0.014(4) C44 0.0245(10) 0.0186(9) 0.0278(10) -0.0003(8) 0.0050(8) 0.0018(8) C45 0.0236(10) 0.0303(11) 0.0267(11) -0.0007(9) -0.0017(9) -0.0012(9) C46 0.0344(12) 0.0407(13) 0.0220(11) 0.0012(9) 0.0019(9) -0.0034(10) C47 0.0311(12) 0.0346(12) 0.0306(11) 0.0035(9) 0.0073(10) -0.0047(9) C48 0.0256(11) 0.0296(11) 0.0268(11) -0.0011(9) -0.0017(9) -0.0051(9) C49 0.0287(11) 0.0239(10) 0.0241(10) -0.0004(8) 0.0012(9) -0.0018(8) C50 0.0515(18) 0.082(2) 0.063(2) 0.0017(17) 0.0155(16) -0.0231(17) _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 Br1 C4 1.8976(19) . ? S1 O4 1.4251(14) . ? S1 O3 1.4252(14) . ? S1 N1 1.6869(15) . ? S1 C19 1.750(2) . ? O1 B1 1.364(3) . ? O1 C13 1.467(2) . ? O2 B1 1.360(3) . ? O2 C14 1.471(2) . ? O5 C22 1.357(2) . ? O5 C25 1.429(3) . ? N1 C1 1.417(2) . ? N1 C8 1.420(2) . ? B1 C7 1.546(3) . ? C1 C2 1.393(3) . ? C1 C6 1.403(2) . ? C2 C3 1.381(3) . ? C3 C4 1.394(3) . ? C4 C5 1.373(3) . ? C5 C6 1.401(3) . ? C6 C7 1.451(2) . ? C7 C8 1.369(3) . ? C8 C9 1.496(3) . ? C9 C10 1.541(3) . ? C10 C11 1.513(3) . ? C11 C12 1.525(3) . ? C13 C15 1.514(3) . ? C13 C16 1.515(3) . ? C13 C14 1.546(3) . ? C14 C17 1.519(3) . ? C14 C18 1.522(3) . ? C19 C24 1.392(3) . ? C19 C20 1.396(3) . ? C20 C21 1.378(3) . ? C21 C22 1.392(3) . ? C22 C23 1.390(3) . ? C23 C24 1.379(3) . ? Br2 C29 1.901(2) . ? S2 O9 1.4203(16) . ? S2 O8 1.4257(15) . ? S2 N2 1.6910(17) . ? S2 C44 1.747(2) . ? O6 B2 1.359(3) . ? O6 C38 1.475(2) . ? O7 B2 1.357(3) . ? O7 C39 1.466(3) . ? O10 C47 1.352(3) . ? O10 C50 1.424(3) . ? N2 C26 1.416(3) . ? N2 C33 1.417(2) . ? B2 C32 1.551(3) . ? C26 C27 1.396(3) . ? C26 C31 1.407(3) . ? C27 C28 1.382(3) . ? C28 C29 1.397(3) . ? C29 C30 1.376(3) . ? C30 C31 1.395(3) . ? C31 C32 1.445(3) . ? C32 C33 1.367(3) . ? C33 C34 1.494(3) . ? C34 C35 1.534(3) . ? C35 C36 1.529(3) . ? C36 C37B 1.529(7) . ? C36 C37 1.627(6) . ? C38 C41 1.500(5) . ? C38 C40 1.509(4) . ? C38 C39 1.546(4) . ? C38 C41C 1.55(2) . ? C38 C41B 1.631(7) . ? C39 C43B 1.510(14) . ? C39 C42 1.512(3) . ? C39 C43 1.558(9) . ? C44 C49 1.391(3) . ? C44 C45 1.392(3) . ? C45 C46 1.371(3) . ? C46 C47 1.397(3) . ? C47 C48 1.387(3) . ? C48 C49 1.387(3) . ? 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 O4 S1 O3 120.67(8) . . ? O4 S1 N1 106.98(8) . . ? O3 S1 N1 104.97(8) . . ? O4 S1 C19 109.34(9) . . ? O3 S1 C19 109.42(9) . . ? N1 S1 C19 104.11(8) . . ? B1 O1 C13 107.08(15) . . ? B1 O2 C14 106.88(15) . . ? C22 O5 C25 118.29(17) . . ? C1 N1 C8 108.13(14) . . ? C1 N1 S1 121.34(12) . . ? C8 N1 S1 126.12(12) . . ? O2 B1 O1 113.94(17) . . ? O2 B1 C7 125.06(18) . . ? O1 B1 C7 120.97(17) . . ? C2 C1 C6 121.75(17) . . ? C2 C1 N1 131.34(17) . . ? C6 C1 N1 106.89(15) . . ? C3 C2 C1 117.63(17) . . ? C2 C3 C4 120.66(17) . . ? C5 C4 C3 122.37(18) . . ? C5 C4 Br1 119.50(15) . . ? C3 C4 Br1 118.10(14) . . ? C4 C5 C6 117.69(17) . . ? C5 C6 C1 119.89(16) . . ? C5 C6 C7 131.52(17) . . ? C1 C6 C7 108.58(16) . . ? C8 C7 C6 106.95(15) . . ? C8 C7 B1 128.21(17) . . ? C6 C7 B1 124.83(17) . . ? C7 C8 N1 109.40(15) . . ? C7 C8 C9 127.98(16) . . ? N1 C8 C9 122.25(16) . . ? C8 C9 C10 113.01(15) . . ? C11 C10 C9 112.74(16) . . ? C10 C11 C12 112.91(18) . . ? O1 C13 C15 106.12(17) . . ? O1 C13 C16 107.79(17) . . ? C15 C13 C16 111.5(2) . . ? O1 C13 C14 102.96(15) . . ? C15 C13 C14 113.05(19) . . ? C16 C13 C14 114.52(19) . . ? O2 C14 C17 107.77(17) . . ? O2 C14 C18 105.68(17) . . ? C17 C14 C18 110.4(2) . . ? O2 C14 C13 102.74(15) . . ? C17 C14 C13 114.99(19) . . ? C18 C14 C13 114.29(19) . . ? C24 C19 C20 120.13(18) . . ? C24 C19 S1 119.93(15) . . ? C20 C19 S1 119.94(15) . . ? C21 C20 C19 119.50(19) . . ? C20 C21 C22 120.35(19) . . ? O5 C22 C23 124.52(19) . . ? O5 C22 C21 115.41(18) . . ? C23 C22 C21 120.07(19) . . ? C24 C23 C22 119.80(19) . . ? C23 C24 C19 120.13(18) . . ? O9 S2 O8 120.68(10) . . ? O9 S2 N2 106.89(9) . . ? O8 S2 N2 105.07(9) . . ? O9 S2 C44 109.28(10) . . ? O8 S2 C44 109.08(10) . . ? N2 S2 C44 104.60(9) . . ? B2 O6 C38 107.17(18) . . ? B2 O7 C39 107.06(18) . . ? C47 O10 C50 119.8(2) . . ? C26 N2 C33 108.27(16) . . ? C26 N2 S2 122.93(13) . . ? C33 N2 S2 126.00(14) . . ? O7 B2 O6 113.76(19) . . ? O7 B2 C32 124.3(2) . . ? O6 B2 C32 121.87(19) . . ? C27 C26 C31 121.83(18) . . ? C27 C26 N2 131.36(18) . . ? C31 C26 N2 106.72(16) . . ? C28 C27 C26 117.48(18) . . ? C27 C28 C29 120.63(18) . . ? C30 C29 C28 122.38(19) . . ? C30 C29 Br2 119.19(15) . . ? C28 C29 Br2 118.41(15) . . ? C29 C30 C31 117.79(18) . . ? C30 C31 C26 119.86(17) . . ? C30 C31 C32 131.74(18) . . ? C26 C31 C32 108.35(17) . . ? C33 C32 C31 107.34(17) . . ? C33 C32 B2 127.52(19) . . ? C31 C32 B2 125.13(19) . . ? C32 C33 N2 109.26(17) . . ? C32 C33 C34 126.68(18) . . ? N2 C33 C34 123.72(18) . . ? C33 C34 C35 112.79(17) . . ? C36 C35 C34 112.27(19) . . ? C37B C36 C35 110.8(3) . . ? C35 C36 C37 112.9(3) . . ? O6 C38 C41 104.8(3) . . ? O6 C38 C40 108.2(2) . . ? C41 C38 C40 105.5(3) . . ? O6 C38 C39 101.90(17) . . ? C41 C38 C39 119.9(3) . . ? C40 C38 C39 115.6(2) . . ? O6 C38 C41C 102.6(8) . . ? C40 C38 C41C 86.9(9) . . ? C39 C38 C41C 139.1(9) . . ? O6 C38 C41B 108.1(3) . . ? C40 C38 C41B 122.8(3) . . ? C39 C38 C41B 98.2(3) . . ? O7 C39 C43B 104.5(6) . . ? O7 C39 C42 106.1(2) . . ? C43B C39 C42 100.6(5) . . ? O7 C39 C38 103.14(17) . . ? C43B C39 C38 128.1(4) . . ? C42 C39 C38 112.7(2) . . ? O7 C39 C43 110.4(4) . . ? C42 C39 C43 117.1(4) . . ? C38 C39 C43 106.5(3) . . ? C49 C44 C45 120.4(2) . . ? C49 C44 S2 119.59(16) . . ? C45 C44 S2 120.00(16) . . ? C46 C45 C44 119.83(19) . . ? C45 C46 C47 120.2(2) . . ? O10 C47 C48 123.8(2) . . ? O10 C47 C46 116.3(2) . . ? C48 C47 C46 119.9(2) . . ? C49 C48 C47 120.06(19) . . ? C48 C49 C44 119.54(19) . . ? _refine_diff_density_max 0.842 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.055 _shelx_res_file ; sab14.res created by SHELXL-2014/7 TITL sab14 in P2(1)/n CELL 0.71073 18.13080 19.24580 18.65330 90.0000 115.2273 90.0000 ZERR 8.00 0.00090 0.00100 0.00100 0.0000 0.0006 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H B N O S BR UNIT 200 248 8 8 40 8 8 TEMP -140.000 SIZE 0.40 0.465 0.557 shel 100 0.78 L.S. 12 acta 51 ABIN WGHT 0.042800 2.543600 FVAR 0.06654 BR1 7 0.652999 0.989120 0.718500 11.00000 0.04574 0.02162 = 0.04714 0.00433 0.02695 -0.00419 S1 6 0.674458 0.614998 0.763664 11.00000 0.02212 0.02079 = 0.02332 -0.00030 0.01151 0.00428 O1 5 0.489332 0.855565 0.859821 11.00000 0.02221 0.02657 = 0.02950 -0.00507 0.01565 0.00074 O2 5 0.440191 0.747157 0.864234 11.00000 0.02349 0.02939 = 0.03838 -0.00649 0.02056 -0.00240 O3 5 0.750566 0.632757 0.763198 11.00000 0.02242 0.02893 = 0.03165 0.00034 0.01480 0.00675 O4 5 0.668398 0.557640 0.809176 11.00000 0.03138 0.02210 = 0.02819 0.00269 0.01451 0.00563 O5 5 0.427309 0.593350 0.434572 11.00000 0.02973 0.05057 = 0.02483 0.00120 0.00905 -0.00446 N1 4 0.646229 0.686468 0.798068 11.00000 0.01835 0.01880 = 0.02005 -0.00083 0.00950 0.00072 B1 3 0.495347 0.785892 0.850072 11.00000 0.01643 0.02694 = 0.01294 -0.00326 0.00288 -0.00142 C1 1 0.655552 0.753891 0.772567 11.00000 0.01536 0.02017 = 0.01595 -0.00195 0.00446 -0.00196 C2 1 0.706068 0.778829 0.739275 11.00000 0.01880 0.02742 = 0.02449 -0.00087 0.01234 -0.00094 AFIX 43 H2A 2 0.741522 0.748656 0.728413 11.00000 -1.20000 AFIX 0 C3 1 0.702786 0.848959 0.722621 11.00000 0.02191 0.03011 = 0.02635 0.00114 0.01367 -0.00473 AFIX 43 H3A 2 0.736358 0.867554 0.699728 11.00000 -1.20000 AFIX 0 C4 1 0.650685 0.892774 0.739067 11.00000 0.02513 0.01871 = 0.02324 0.00105 0.00885 -0.00495 C5 1 0.600360 0.868915 0.771635 11.00000 0.01890 0.02059 = 0.02065 -0.00212 0.00725 0.00035 AFIX 43 H5A 2 0.565264 0.899573 0.782412 11.00000 -1.20000 AFIX 0 C6 1 0.602558 0.797801 0.788423 11.00000 0.01441 0.02220 = 0.01440 -0.00218 0.00473 -0.00053 C7 1 0.558482 0.756653 0.822572 11.00000 0.01489 0.02176 = 0.01344 -0.00228 0.00411 -0.00332 C8 1 0.585317 0.689609 0.826859 11.00000 0.01432 0.02339 = 0.01489 -0.00191 0.00545 -0.00146 C9 1 0.564276 0.628335 0.863937 11.00000 0.02023 0.02121 = 0.02119 -0.00245 0.01036 -0.00381 AFIX 23 H9A 2 0.555528 0.587388 0.829122 11.00000 -1.20000 H9B 2 0.512508 0.637883 0.867943 11.00000 -1.20000 AFIX 0 C10 1 0.630794 0.611004 0.947000 11.00000 0.02731 0.02219 = 0.02314 0.00334 0.01084 -0.00184 AFIX 23 H10A 2 0.623297 0.562569 0.960508 11.00000 -1.20000 H10B 2 0.684892 0.614117 0.946090 11.00000 -1.20000 AFIX 0 C11 1 0.629169 0.659088 1.010462 11.00000 0.03484 0.02866 = 0.02201 0.00177 0.01098 -0.00246 AFIX 23 H11A 2 0.576563 0.653409 1.014022 11.00000 -1.20000 H11B 2 0.632541 0.707757 0.994933 11.00000 -1.20000 AFIX 0 C12 1 0.698635 0.645469 1.091711 11.00000 0.05529 0.03491 = 0.02511 0.00342 0.00764 -0.01011 AFIX 137 H12A 2 0.694946 0.678212 1.130287 11.00000 -1.50000 H12B 2 0.750954 0.651622 1.088816 11.00000 -1.50000 H12C 2 0.694654 0.597819 1.108251 11.00000 -1.50000 AFIX 0 C13 1 0.416231 0.866504 0.873465 11.00000 0.01924 0.03654 = 0.03424 -0.00706 0.01465 0.00378 C14 1 0.400918 0.793918 0.899950 11.00000 0.02288 0.03793 = 0.03528 -0.00966 0.01948 -0.00069 C15 1 0.349667 0.889026 0.794652 11.00000 0.03385 0.06773 = 0.04961 0.01214 0.01431 0.02467 AFIX 137 H15A 2 0.300443 0.900787 0.801456 11.00000 -1.50000 H15B 2 0.337530 0.851047 0.756294 11.00000 -1.50000 H15C 2 0.367951 0.929818 0.775201 11.00000 -1.50000 AFIX 0 C16 1 0.435451 0.922767 0.935676 11.00000 0.04625 0.04626 = 0.07004 -0.02554 0.04074 -0.00529 AFIX 137 H16A 2 0.389341 0.928108 0.949529 11.00000 -1.50000 H16B 2 0.445150 0.966772 0.914674 11.00000 -1.50000 H16C 2 0.484292 0.909809 0.983060 11.00000 -1.50000 AFIX 0 C17 1 0.311828 0.773063 0.868683 11.00000 0.02598 0.05414 = 0.07305 -0.02269 0.03155 -0.00873 AFIX 137 H17A 2 0.282352 0.807561 0.885136 11.00000 -1.50000 H17B 2 0.307715 0.727450 0.890051 11.00000 -1.50000 H17C 2 0.287939 0.770723 0.810692 11.00000 -1.50000 AFIX 0 C18 1 0.444423 0.781373 0.988857 11.00000 0.04515 0.06462 = 0.03908 0.00357 0.03013 0.00791 AFIX 137 H18A 2 0.418103 0.808719 1.015750 11.00000 -1.50000 H18B 2 0.501643 0.795415 1.008211 11.00000 -1.50000 H18C 2 0.441540 0.731906 0.999867 11.00000 -1.50000 AFIX 0 C19 1 0.600174 0.607002 0.666036 11.00000 0.02709 0.02184 = 0.02211 -0.00328 0.01313 0.00212 C20 1 0.613497 0.636036 0.604005 11.00000 0.02772 0.03339 = 0.02822 -0.00121 0.01528 -0.00281 AFIX 43 H20A 2 0.663016 0.659726 0.614495 11.00000 -1.20000 AFIX 0 C21 1 0.554265 0.630081 0.527399 11.00000 0.03296 0.04342 = 0.02726 0.00409 0.01740 -0.00246 AFIX 43 H21A 2 0.563117 0.649624 0.484950 11.00000 -1.20000 AFIX 0 C22 1 0.481565 0.595589 0.511914 11.00000 0.02726 0.03222 = 0.02470 -0.00189 0.01081 0.00151 C23 1 0.468613 0.566297 0.573720 11.00000 0.02489 0.02861 = 0.03049 -0.00401 0.01413 -0.00378 AFIX 43 H23A 2 0.419104 0.542555 0.563146 11.00000 -1.20000 AFIX 0 C24 1 0.527851 0.571809 0.650430 11.00000 0.03255 0.02285 = 0.02552 -0.00116 0.01751 0.00087 AFIX 43 H24A 2 0.519277 0.551545 0.692702 11.00000 -1.20000 AFIX 0 C25 1 0.353284 0.555436 0.414018 11.00000 0.02954 0.04390 = 0.03163 -0.00327 0.00906 -0.00221 AFIX 137 H25A 2 0.322079 0.555220 0.356287 11.00000 -1.50000 H25B 2 0.320944 0.577534 0.438458 11.00000 -1.50000 H25C 2 0.366065 0.507553 0.433212 11.00000 -1.50000 AFIX 0 BR2 7 0.845580 0.653086 0.641601 11.00000 0.03254 0.03714 = 0.02852 -0.00602 0.01613 -0.00711 S2 6 0.770512 0.344156 0.394560 11.00000 0.02239 0.02596 = 0.03218 -0.00101 0.00717 0.00229 O6 5 0.601711 0.644771 0.347215 11.00000 0.03017 0.02974 = 0.04072 0.00987 -0.00623 0.00515 O7 5 0.543702 0.573376 0.240429 11.00000 0.03280 0.05801 = 0.02301 0.00429 0.00208 0.02223 O8 5 0.851972 0.337950 0.454201 11.00000 0.02175 0.03255 = 0.04589 0.00012 0.00660 0.00388 O9 5 0.750369 0.323561 0.315273 11.00000 0.03713 0.03757 = 0.03634 -0.00531 0.01603 0.00286 O10 5 0.551627 0.208632 0.509371 11.00000 0.03246 0.06668 = 0.04036 0.01085 0.00608 -0.01459 N2 4 0.748101 0.429666 0.392038 11.00000 0.01945 0.02483 = 0.02494 0.00185 0.00362 -0.00070 B2 3 0.604074 0.582258 0.314329 11.00000 0.01844 0.03746 = 0.02749 0.01146 0.00863 0.00115 C26 1 0.777807 0.472250 0.460482 11.00000 0.01777 0.02222 = 0.02593 0.00487 0.00833 -0.00243 C27 1 0.843002 0.463536 0.534719 11.00000 0.01854 0.02350 = 0.02819 0.00655 0.00473 0.00036 AFIX 43 H27A 2 0.874312 0.422009 0.547983 11.00000 -1.20000 AFIX 0 C28 1 0.860288 0.517593 0.588198 11.00000 0.01998 0.03253 = 0.02184 0.00810 0.00509 -0.00195 AFIX 43 H28A 2 0.903772 0.513136 0.639540 11.00000 -1.20000 AFIX 0 C29 1 0.814433 0.578734 0.567490 11.00000 0.02392 0.02927 = 0.02344 -0.00130 0.01326 -0.00767 C30 1 0.749282 0.587509 0.494893 11.00000 0.02065 0.02577 = 0.02650 0.00765 0.01315 0.00207 AFIX 43 H30A 2 0.718218 0.629170 0.482303 11.00000 -1.20000 AFIX 0 C31 1 0.730369 0.533182 0.440391 11.00000 0.01578 0.02698 = 0.02138 0.00784 0.00725 0.00007 C32 1 0.669210 0.526602 0.359693 11.00000 0.01703 0.03093 = 0.02263 0.00622 0.00674 -0.00253 C33 1 0.680804 0.463723 0.331978 11.00000 0.01630 0.03235 = 0.02337 0.00565 0.00500 -0.00302 C34 1 0.637088 0.436855 0.249272 11.00000 0.02251 0.03491 = 0.02605 0.00196 0.00482 -0.00498 AFIX 23 H34A 2 0.582704 0.459003 0.223928 11.00000 -1.20000 H34B 2 0.628791 0.386166 0.251157 11.00000 -1.20000 AFIX 0 C35 1 0.683436 0.450814 0.198533 11.00000 0.03487 0.05298 = 0.02861 -0.00194 0.01145 -0.01509 AFIX 23 H35A 2 0.698350 0.500612 0.202466 11.00000 -1.20000 H35B 2 0.734505 0.423394 0.219562 11.00000 -1.20000 AFIX 0 C36 1 0.633166 0.432012 0.111433 11.00000 0.05385 0.05714 = 0.03434 -0.01274 0.01987 -0.02203 AFIX 23 PART 1 H36A 2 0.613678 0.383541 0.108054 10.55000 -1.20000 H36B 2 0.668608 0.434434 0.083227 10.55000 -1.20000 AFIX 23 PART 2 H36C 2 0.607288 0.386060 0.107867 10.45000 -1.20000 H36D 2 0.589363 0.466799 0.086569 10.45000 -1.20000 AFIX 0 PART 1 C37 1 0.555099 0.482956 0.067419 10.55000 0.04799 0.05401 = 0.02586 -0.00045 0.00750 -0.02178 AFIX 137 H37A 2 0.526584 0.469888 0.011450 10.55000 -1.50000 H37B 2 0.573829 0.531176 0.071472 10.55000 -1.50000 H37C 2 0.517870 0.478483 0.092830 10.55000 -1.50000 AFIX 0 PART 2 C37B 1 0.686962 0.429888 0.066808 10.45000 0.06610 0.05753 = 0.03260 -0.00742 0.01205 -0.02055 AFIX 137 H37D 2 0.654026 0.416096 0.011703 10.45000 -1.50000 H37E 2 0.731017 0.396178 0.092129 10.45000 -1.50000 H37F 2 0.710322 0.476026 0.067992 10.45000 -1.50000 AFIX 0 PART 0 C38 1 0.541746 0.688155 0.284094 11.00000 0.02516 0.03929 = 0.04514 0.02356 0.00057 0.00660 C39 1 0.488357 0.632786 0.224542 11.00000 0.02691 0.04891 = 0.02808 0.00952 0.00450 0.01713 C40 1 0.498498 0.732970 0.320581 11.00000 0.05528 0.04009 = 0.05097 0.00549 -0.00182 0.01898 AFIX 137 H40A 2 0.456431 0.760613 0.279099 11.00000 -1.50000 H40B 2 0.537921 0.764073 0.359907 11.00000 -1.50000 H40C 2 0.473053 0.703331 0.346433 11.00000 -1.50000 AFIX 0 PART 1 C41 1 0.592050 0.737258 0.260892 10.50000 0.03193 AFIX 137 H41A 2 0.631988 0.760483 0.308305 10.50000 -1.50000 H41B 2 0.556430 0.772093 0.224058 10.50000 -1.50000 H41C 2 0.620608 0.711287 0.235151 10.50000 -1.50000 AFIX 0 PART 2 C41B 1 0.585948 0.719969 0.231309 10.40000 0.04584 AFIX 137 H41D 2 0.606748 0.681875 0.210244 10.40000 -1.50000 H41E 2 0.631288 0.749983 0.264648 10.40000 -1.50000 H41F 2 0.546373 0.747166 0.187312 10.40000 -1.50000 AFIX 0 PART 3 C41C 1 0.592263 0.753522 0.285387 10.10000 0.01892 AFIX 137 H41G 2 0.618684 0.771794 0.339519 10.10000 -1.50000 H41H 2 0.556115 0.789028 0.250213 10.10000 -1.50000 H41I 2 0.633924 0.741066 0.267246 10.10000 -1.50000 AFIX 0 PART 0 C42 1 0.418496 0.608258 0.242064 11.00000 0.02549 0.04763 = 0.07694 0.00393 0.01278 0.00461 AFIX 137 H42A 2 0.378728 0.645890 0.231065 11.00000 -1.50000 H42B 2 0.439344 0.594834 0.297948 11.00000 -1.50000 H42C 2 0.392144 0.568156 0.208534 11.00000 -1.50000 AFIX 0 PART 1 C43 1 0.466351 0.662527 0.140198 10.55000 0.04763 0.04850 = 0.02368 0.01046 0.00984 0.01876 AFIX 137 H43A 2 0.429681 0.702360 0.130622 10.55000 -1.50000 H43B 2 0.439272 0.626495 0.100498 10.55000 -1.50000 H43C 2 0.516257 0.677434 0.136417 10.55000 -1.50000 AFIX 0 PART 2 C43B 1 0.446472 0.637590 0.135286 10.45000 0.05061 0.05108 = 0.04289 0.02363 0.00343 0.01376 AFIX 137 H43D 2 0.410157 0.678023 0.119760 10.45000 -1.50000 H43E 2 0.414563 0.595306 0.113718 10.45000 -1.50000 H43F 2 0.487509 0.642558 0.114446 10.45000 -1.50000 AFIX 0 PART 0 C44 1 0.704344 0.303576 0.427397 11.00000 0.02450 0.01864 = 0.02776 -0.00027 0.00504 0.00180 C45 1 0.726937 0.295604 0.508207 11.00000 0.02363 0.03033 = 0.02669 -0.00066 -0.00169 -0.00117 AFIX 43 H45A 2 0.778271 0.312315 0.545570 11.00000 -1.20000 AFIX 0 C46 1 0.674899 0.263563 0.533754 11.00000 0.03443 0.04069 = 0.02198 0.00124 0.00191 -0.00340 AFIX 43 H46A 2 0.690396 0.257887 0.588896 11.00000 -1.20000 AFIX 0 C47 1 0.599190 0.239240 0.479000 11.00000 0.03111 0.03459 = 0.03057 0.00346 0.00727 -0.00474 C48 1 0.577008 0.246616 0.398446 11.00000 0.02560 0.02958 = 0.02680 -0.00114 -0.00167 -0.00508 AFIX 43 H48A 2 0.525864 0.229493 0.361153 11.00000 -1.20000 AFIX 0 C49 1 0.629410 0.278955 0.372316 11.00000 0.02865 0.02385 = 0.02412 -0.00036 0.00124 -0.00184 AFIX 43 H49A 2 0.614260 0.284266 0.317190 11.00000 -1.20000 AFIX 0 C50 1 0.474171 0.181268 0.457444 11.00000 0.05150 0.08194 = 0.06285 0.00173 0.01546 -0.02314 AFIX 137 H50A 2 0.447053 0.162190 0.488685 11.00000 -1.50000 H50B 2 0.481588 0.144388 0.424883 11.00000 -1.50000 H50C 2 0.440573 0.218396 0.423032 11.00000 -1.50000 AFIX 0 HKLF 4 REM sab14 in P2(1)/n REM R1 = 0.0344 for 10471 Fo > 4sig(Fo) and 0.0480 for all 12992 data REM 650 parameters refined using 0 restraints END WGHT 0.0428 2.5421 REM Highest difference peak 0.842, deepest hole -0.443, 1-sigma level 0.055 Q1 1 0.5850 0.1776 0.5797 11.00000 0.05 0.84 Q2 1 0.6074 0.9878 0.6754 11.00000 0.05 0.51 Q3 1 0.8192 0.6912 0.6287 11.00000 0.05 0.46 Q4 1 0.7344 0.3177 0.4098 11.00000 0.05 0.43 Q5 1 0.6272 0.6410 0.3209 11.00000 0.05 0.42 Q6 1 0.6873 0.9718 0.6972 11.00000 0.05 0.41 Q7 1 0.8067 0.6266 0.6101 11.00000 0.05 0.35 Q8 1 0.6325 0.6102 0.7096 11.00000 0.05 0.35 Q9 1 0.3802 0.8767 0.8350 11.00000 0.05 0.32 Q10 1 0.6519 0.6542 0.7811 11.00000 0.05 0.32 Q11 1 0.7478 0.4985 0.4579 11.00000 0.05 0.31 Q12 1 0.5558 0.6821 0.2477 11.00000 0.05 0.31 Q13 1 0.5967 0.6169 0.9079 11.00000 0.05 0.31 Q14 1 0.6647 0.4454 0.2922 11.00000 0.05 0.30 Q15 1 0.5995 0.8289 0.7812 11.00000 0.05 0.30 Q16 1 0.6638 0.4420 0.2254 11.00000 0.05 0.29 Q17 1 0.6328 0.5510 0.3374 11.00000 0.05 0.29 Q18 1 0.6991 0.5380 0.3997 11.00000 0.05 0.29 Q19 1 0.8118 0.4623 0.4948 11.00000 0.05 0.29 Q20 1 0.6363 0.7786 0.7947 11.00000 0.05 0.28 ; _shelx_res_checksum 430 _shelx_hkl_file ; 1 0 0 -0.02 0.02 1 0 0 -0.05 0.02 -1 0 0 -0.02 0.02 2 0 0 33.08 0.84 -2 0 0 33.06 0.82 -2 0 0 33.01 0.86 3 0 0 -0.02 0.05 -3 0 0 -0.03 0.03 3 0 0 -0.11 0.04 -3 0 0 -0.08 0.05 -4 0 0 409.21 9.58 4 0 0 393.91 9.64 4 0 0 396.93 9.62 -4 0 0 397.93 9.65 5 0 0 -0.14 0.08 -5 0 0 -0.30 0.08 -5 0 0 -0.12 0.05 5 0 0 -0.26 0.08 -6 0 0 52.46 1.47 -6 0 0 55.62 1.37 6 0 0 56.42 1.43 6 0 0 54.42 1.45 -7 0 0 0.02 0.06 7 0 0 0.27 0.10 -7 0 0 0.11 0.13 7 0 0 0.10 0.11 -8 0 0 0.09 0.07 8 0 0 0.12 0.11 8 0 0 0.12 0.14 -8 0 0 0.08 0.15 9 0 0 -0.05 0.12 -9 0 0 0.12 0.18 9 0 0 0.08 0.16 10 0 0 175.51 4.48 10 0 0 175.02 4.44 -10 0 0 174.14 4.51 10 0 0 184.10 4.33 11 0 0 0.08 0.19 -11 0 0 0.13 0.21 11 0 0 0.12 0.15 12 0 0 83.20 2.17 12 0 0 78.90 2.22 -12 0 0 79.29 2.27 13 0 0 0.09 0.20 -13 0 0 0.44 0.28 13 0 0 0.41 0.24 14 0 0 6.26 0.53 -14 0 0 6.05 0.59 14 0 0 6.81 0.47 -15 0 0 -0.58 0.31 15 0 0 -0.13 0.30 15 0 0 0.02 0.22 16 0 0 17.73 0.84 -16 0 0 18.43 0.89 -17 0 0 0.26 0.41 17 0 0 0.49 0.36 -18 0 0 1.23 0.44 18 0 0 -0.23 0.32 -19 0 0 0.29 0.47 19 0 0 -0.09 0.40 -20 0 0 10.40 0.93 20 0 0 8.80 0.81 21 0 0 0.22 0.44 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17 -1 0 15.20 0.81 -17 1 0 16.46 0.93 17 1 0 15.88 0.87 -18 -1 0 0.56 0.43 18 -1 0 0.09 0.34 18 1 0 0.97 0.41 -18 1 0 0.36 0.44 19 -1 0 10.50 0.77 -19 -1 0 12.22 0.92 19 1 0 13.14 0.87 -19 1 0 11.14 0.91 -20 -1 0 0.29 0.50 20 -1 0 1.25 0.47 -20 1 0 -0.08 0.50 20 1 0 0.63 0.46 -21 -1 0 0.93 0.63 21 -1 0 0.58 0.49 21 1 0 1.12 0.55 0 -2 0 0.81 0.06 0 2 0 0.71 0.05 1 -2 0 34.08 0.88 -1 -2 0 35.48 0.86 -1 -2 0 34.99 0.89 1 -2 0 35.70 0.88 -1 2 0 34.87 0.87 1 2 0 35.52 0.88 1 2 0 35.60 0.88 -1 2 0 35.92 0.89 -2 -2 0 86.05 2.05 2 -2 0 83.47 2.05 2 -2 0 83.49 2.06 -2 -2 0 85.15 2.07 2 2 0 84.73 2.04 -2 2 0 81.81 2.06 -2 2 0 83.82 2.06 2 2 0 80.93 2.06 3 -2 0 141.49 3.38 -3 -2 0 140.63 3.40 3 -2 0 137.76 3.40 -3 -2 0 140.81 3.39 3 2 0 135.53 3.39 -3 2 0 137.86 3.40 -3 2 0 138.56 3.38 3 2 0 137.37 3.35 4 -2 0 92.59 2.30 -4 -2 0 91.48 2.33 4 -2 0 91.35 2.33 4 2 0 93.00 2.32 -4 2 0 95.31 2.30 4 2 0 93.92 2.26 4 2 0 93.58 2.33 -4 2 0 94.10 2.34 5 -2 0 68.14 1.72 -5 -2 0 68.55 1.76 -5 2 0 69.71 1.71 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8.49 0.47 13 -2 0 6.94 0.53 -13 -2 0 7.60 0.53 -13 -2 0 8.06 0.50 13 2 0 7.27 0.52 13 2 0 8.48 0.49 -13 2 0 8.72 0.59 -14 -2 0 0.53 0.25 14 -2 0 0.39 0.27 14 -2 0 0.51 0.22 -14 -2 0 0.08 0.30 -14 2 0 0.11 0.28 14 2 0 0.80 0.31 -15 -2 0 3.29 0.46 -15 -2 0 3.07 0.39 15 -2 0 3.05 0.43 15 2 0 4.24 0.46 -15 2 0 3.56 0.48 -16 -2 0 1.81 0.43 -16 -2 0 1.48 0.34 16 -2 0 1.46 0.38 16 2 0 2.26 0.40 -16 2 0 0.92 0.35 17 -2 0 3.04 0.47 -17 -2 0 2.95 0.51 -17 2 0 2.95 0.51 17 2 0 2.64 0.43 18 -2 0 1.68 0.45 -18 -2 0 1.19 0.48 18 2 0 1.09 0.43 -18 2 0 1.71 0.47 19 -2 0 -0.03 0.40 -19 -2 0 -0.01 0.42 19 2 0 -0.32 0.38 -19 2 0 1.03 0.51 20 -2 0 2.10 0.51 -20 -2 0 1.86 0.57 20 2 0 2.06 0.51 -20 2 0 1.53 0.55 21 -2 0 2.10 0.56 -21 -2 0 1.24 0.58 0 -3 0 0.00 0.04 0 3 0 0.20 0.05 0 3 0 0.02 0.04 -1 -3 0 19.09 0.53 1 -3 0 19.08 0.52 -1 -3 0 19.25 0.48 1 -3 0 19.23 0.52 -1 3 0 18.38 0.53 -1 3 0 18.74 0.49 1 3 0 18.64 0.52 1 3 0 19.53 0.52 2 -3 0 50.66 1.30 -2 -3 0 51.09 1.27 2 -3 0 51.81 1.29 2 3 0 49.83 1.29 -2 3 0 52.27 1.31 2 3 0 50.78 1.28 -2 3 0 52.11 1.29 3 -3 0 3.31 0.16 -3 -3 0 3.34 0.16 -3 -3 0 3.47 0.18 -3 3 0 3.29 0.18 -3 3 0 3.47 0.17 3 3 0 3.24 0.16 3 3 0 3.35 0.14 -4 -3 0 1.01 0.12 4 -3 0 1.03 0.12 4 -3 0 1.28 0.14 -4 -3 0 1.17 0.13 -4 3 0 1.32 0.14 4 3 0 1.24 0.09 -4 3 0 0.91 0.11 4 3 0 1.41 0.14 5 -3 0 71.42 1.80 5 -3 0 69.82 1.84 -5 -3 0 72.26 1.83 -5 -3 0 72.37 1.84 5 3 0 70.54 1.82 5 3 0 71.52 1.75 -5 3 0 70.12 1.84 -5 3 0 70.37 1.80 6 -3 0 13.93 0.51 -6 -3 0 14.60 0.50 -6 -3 0 14.03 0.50 6 -3 0 14.34 0.46 -6 3 0 15.09 0.46 6 3 0 14.87 0.40 -6 3 0 14.17 0.51 6 3 0 13.70 0.48 7 -3 0 0.76 0.16 -7 -3 0 0.89 0.16 7 -3 0 0.81 0.13 -7 -3 0 1.02 0.17 -7 3 0 0.90 0.13 7 3 0 0.87 0.16 7 3 0 0.84 0.08 -7 3 0 0.93 0.17 -8 -3 0 3.98 0.30 -8 -3 0 3.46 0.28 8 -3 0 3.79 0.25 8 3 0 4.08 0.17 8 3 0 3.63 0.29 -8 3 0 4.17 0.24 -8 3 0 4.09 0.32 9 -3 0 0.04 0.12 9 -3 0 0.23 0.17 -9 -3 0 0.12 0.16 -9 -3 0 0.35 0.16 9 3 0 0.15 0.14 -9 3 0 0.10 0.11 9 3 0 0.13 0.07 -9 3 0 0.20 0.18 -10 -3 0 0.55 0.19 10 -3 0 0.59 0.16 10 -3 0 0.90 0.22 -10 -3 0 0.62 0.21 -10 3 0 0.50 0.20 -10 3 0 0.57 0.14 10 3 0 0.43 0.20 10 3 0 0.61 0.09 -11 -3 0 0.30 0.20 11 -3 0 0.46 0.22 11 -3 0 0.22 0.16 -11 -3 0 0.26 0.22 11 3 0 0.08 0.18 -11 3 0 0.34 0.23 -11 3 0 0.35 0.14 12 -3 0 0.74 0.24 -12 -3 0 0.88 0.28 12 -3 0 0.82 0.20 -12 -3 0 0.65 0.23 12 3 0 0.45 0.22 -12 3 0 1.00 0.29 -13 -3 0 6.35 0.54 13 -3 0 5.91 0.40 13 -3 0 4.79 0.44 -13 -3 0 5.95 0.46 -13 3 0 5.07 0.52 13 3 0 5.36 0.48 -14 -3 0 0.01 0.23 -14 -3 0 0.17 0.31 14 -3 0 -0.02 0.26 14 3 0 -0.50 0.25 -14 3 0 0.01 0.30 -15 -3 0 7.32 0.54 -15 -3 0 6.26 0.61 15 -3 0 6.01 0.57 15 3 0 6.55 0.58 -15 3 0 6.63 0.64 -16 -3 0 19.16 0.86 16 -3 0 19.84 0.92 -16 -3 0 20.45 0.97 -16 3 0 17.52 0.91 16 3 0 21.53 0.93 -17 -3 0 0.32 0.38 17 -3 0 0.17 0.36 -17 -3 0 0.01 0.32 17 3 0 0.22 0.31 -17 3 0 0.75 0.42 18 -3 0 -0.09 0.38 -18 -3 0 -0.12 0.42 -18 3 0 0.33 0.42 18 3 0 -0.05 0.31 -19 -3 0 0.49 0.45 19 -3 0 0.49 0.43 -19 3 0 -0.16 0.45 19 3 0 -0.21 0.39 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0.40 7 -4 0 9.00 0.41 7 -4 0 8.85 0.35 -7 -4 0 9.11 0.39 7 4 0 8.81 0.29 -7 4 0 8.78 0.41 -7 4 0 8.54 0.35 7 4 0 7.97 0.37 8 -4 0 17.26 0.57 -8 -4 0 18.33 0.63 -8 -4 0 17.12 0.61 8 -4 0 16.93 0.63 8 4 0 17.54 0.48 -8 4 0 16.22 0.63 -8 4 0 17.32 0.56 8 4 0 16.16 0.60 -9 -4 0 1.36 0.21 -9 -4 0 1.28 0.21 9 -4 0 1.39 0.22 9 -4 0 1.21 0.17 -9 4 0 1.35 0.17 9 4 0 1.55 0.22 9 4 0 1.30 0.13 -9 4 0 1.45 0.23 10 -4 0 1.14 0.22 -10 -4 0 0.49 0.19 10 -4 0 0.43 0.16 -10 -4 0 0.87 0.23 -10 4 0 0.75 0.16 10 4 0 0.59 0.18 -10 4 0 0.73 0.22 11 -4 0 23.27 0.78 11 -4 0 24.10 0.87 -11 -4 0 23.90 0.85 -11 -4 0 24.28 0.88 11 4 0 23.51 0.85 -11 4 0 24.90 0.75 -11 4 0 22.92 0.87 12 -4 0 5.33 0.42 -12 -4 0 5.30 0.43 -12 -4 0 4.61 0.46 12 -4 0 5.24 0.37 12 4 0 5.07 0.44 -12 4 0 4.67 0.48 13 -4 0 -0.11 0.24 -13 -4 0 0.10 0.26 -13 -4 0 0.17 0.24 13 -4 0 0.19 0.19 -13 4 0 0.43 0.30 13 4 0 0.33 0.23 -14 -4 0 3.70 0.41 -14 -4 0 3.56 0.43 14 -4 0 4.00 0.44 -14 4 0 2.76 0.43 14 4 0 3.50 0.39 -15 -4 0 8.57 0.61 -15 -4 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0 13.63 0.42 4 -5 0 13.07 0.43 4 -5 0 12.99 0.45 4 5 0 14.08 0.45 -4 5 0 13.47 0.44 4 5 0 13.07 0.41 -4 5 0 13.52 0.46 5 -5 0 0.81 0.15 -5 -5 0 0.66 0.12 5 -5 0 0.79 0.12 -5 -5 0 0.79 0.14 -5 5 0 1.65 0.18 5 5 0 0.67 0.09 5 5 0 0.49 0.12 -5 5 0 0.63 0.13 6 -5 0 10.09 0.42 6 -5 0 9.77 0.37 -6 -5 0 9.60 0.42 -6 -5 0 9.74 0.38 -6 5 0 10.58 0.40 6 5 0 9.30 0.40 6 5 0 9.48 0.32 -6 5 0 9.84 0.41 -7 -5 0 10.03 0.42 7 -5 0 10.78 0.45 -7 -5 0 10.07 0.45 7 -5 0 10.29 0.40 7 5 0 10.70 0.43 7 5 0 10.29 0.34 -7 5 0 10.76 0.41 -7 5 0 10.24 0.45 8 -5 0 91.49 2.38 8 -5 0 94.08 2.46 -8 -5 0 93.38 2.44 -8 -5 0 94.52 2.46 8 5 0 95.57 2.31 8 5 0 92.24 2.43 -8 5 0 91.19 2.39 -8 5 0 93.06 2.46 -9 -5 0 13.00 0.56 -9 -5 0 14.08 0.57 9 -5 0 12.68 0.49 9 -5 0 13.02 0.58 9 5 0 13.83 0.55 -9 5 0 13.04 0.58 -9 5 0 13.27 0.51 9 5 0 14.06 0.42 -10 -5 0 3.70 0.36 10 -5 0 3.86 0.30 -10 -5 0 3.80 0.36 10 -5 0 4.40 0.36 10 5 0 4.11 0.34 -10 5 0 4.09 0.30 -10 5 0 4.46 0.40 -11 -5 0 -0.16 0.20 -11 -5 0 0.11 0.21 11 -5 0 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5.84 1 6 0 238.61 5.82 -1 6 0 235.80 5.82 -1 6 0 232.79 5.85 2 -6 0 147.21 3.58 -2 -6 0 144.27 3.60 2 -6 0 147.27 3.58 -2 -6 0 146.08 3.49 -2 6 0 146.62 3.53 2 6 0 141.57 3.58 -2 6 0 142.30 3.60 2 6 0 143.18 3.58 -3 -6 0 8.30 0.35 -3 -6 0 8.62 0.27 3 -6 0 8.69 0.34 3 -6 0 8.51 0.34 -3 6 0 8.13 0.35 3 6 0 8.85 0.34 3 6 0 8.36 0.32 -3 6 0 8.65 0.30 4 -6 0 19.76 0.60 -4 -6 0 20.51 0.56 -4 -6 0 19.42 0.64 4 -6 0 18.64 0.61 4 6 0 19.87 0.58 -4 6 0 19.62 0.59 -4 6 0 18.96 0.62 5 -6 0 79.55 2.05 5 -6 0 80.13 2.02 -5 -6 0 81.59 2.00 -5 -6 0 76.92 2.06 5 6 0 78.52 1.99 5 6 0 78.17 2.04 -5 6 0 76.56 2.04 -5 6 0 76.59 2.03 -6 -6 0 61.71 1.71 -6 -6 0 65.26 1.66 6 -6 0 62.79 1.70 6 -6 0 62.43 1.65 6 6 0 62.35 1.68 -6 6 0 62.76 1.68 6 6 0 64.19 1.61 -6 6 0 61.53 1.68 -7 -6 0 3.23 0.26 -7 -6 0 3.15 0.30 7 -6 0 3.47 0.30 7 -6 0 3.90 0.25 7 6 0 3.21 0.28 -7 6 0 2.98 0.25 -7 6 0 3.26 0.28 7 6 0 3.30 0.20 -8 -6 0 51.36 1.45 -8 -6 0 52.60 1.49 8 -6 0 51.32 1.41 8 -6 0 51.30 1.48 -8 6 0 50.44 1.47 8 6 0 52.24 1.46 -8 6 0 52.12 1.44 8 6 0 53.94 1.35 -9 -6 0 5.73 0.42 9 -6 0 6.42 0.43 -9 -6 0 6.05 0.38 9 -6 0 6.66 0.34 -9 6 0 6.99 0.42 9 6 0 6.81 0.27 9 6 0 6.31 0.41 -9 6 0 6.76 0.37 -10 -6 0 34.00 1.09 -10 -6 0 33.52 1.08 10 -6 0 33.72 1.01 10 -6 0 32.78 1.09 10 6 0 32.38 1.07 -10 6 0 34.63 1.02 -10 6 0 34.90 1.11 11 -6 0 10.24 0.56 -11 -6 0 8.69 0.53 11 -6 0 9.64 0.45 -11 -6 0 9.97 0.56 -11 6 0 10.53 0.48 11 6 0 9.25 0.51 -11 6 0 9.15 0.55 12 -6 0 4.55 0.45 -12 -6 0 3.99 0.43 -12 -6 0 3.07 0.38 12 -6 0 3.77 0.35 12 6 0 4.12 0.40 -12 6 0 3.45 0.43 -12 6 0 3.52 0.40 -13 -6 0 0.25 0.27 -13 -6 0 1.31 0.31 13 -6 0 0.65 0.26 13 6 0 0.23 0.27 -13 6 0 0.11 0.30 -14 -6 0 14.92 0.77 14 -6 0 13.66 0.75 -14 -6 0 13.78 0.74 14 6 0 15.78 0.76 -14 6 0 15.22 0.81 15 -6 0 0.36 0.32 -15 -6 0 -0.19 0.30 -15 -6 0 -0.15 0.29 15 6 0 -0.55 0.27 -15 6 0 0.22 0.35 16 -6 0 34.26 1.28 -16 -6 0 34.76 1.31 -16 -6 0 34.81 1.29 -16 6 0 31.64 1.31 16 6 0 35.23 1.28 -17 -6 0 0.09 0.39 17 -6 0 0.29 0.36 -17 -6 0 -0.11 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0.72 -5 7 0 23.50 0.74 5 7 0 22.93 0.68 6 -7 0 6.56 0.31 -6 -7 0 6.58 0.36 -6 -7 0 6.04 0.29 6 -7 0 5.86 0.33 6 7 0 6.02 0.28 -6 7 0 5.23 0.34 -6 7 0 6.22 0.33 6 7 0 5.45 0.33 7 -7 0 129.00 3.32 -7 -7 0 133.80 3.34 7 -7 0 128.74 3.25 -7 -7 0 129.61 3.26 7 7 0 128.07 3.21 -7 7 0 129.28 3.29 -7 7 0 128.63 3.29 7 7 0 125.31 3.29 -8 -7 0 1.07 0.21 -8 -7 0 1.80 0.22 8 -7 0 1.61 0.25 8 -7 0 2.12 0.23 8 7 0 1.78 0.22 8 7 0 2.02 0.19 -8 7 0 1.81 0.23 -8 7 0 1.82 0.25 -9 -7 0 10.60 0.55 9 -7 0 10.99 0.46 -9 -7 0 11.37 0.49 9 -7 0 11.03 0.55 9 7 0 10.66 0.52 -9 7 0 10.68 0.49 -9 7 0 10.31 0.52 9 7 0 11.04 0.40 -10 -7 0 3.13 0.31 -10 -7 0 3.69 0.40 10 -7 0 3.47 0.30 10 -7 0 4.11 0.41 -10 7 0 3.43 0.31 -10 7 0 3.13 0.34 10 7 0 2.84 0.30 11 -7 0 33.03 1.00 -11 -7 0 30.05 1.09 11 -7 0 32.54 1.10 -11 -7 0 33.25 1.08 11 7 0 32.51 1.09 -11 7 0 32.39 1.02 -11 7 0 31.98 1.11 -12 -7 0 6.67 0.52 12 -7 0 7.13 0.53 -12 -7 0 7.50 0.51 -12 7 0 5.64 0.42 12 7 0 6.58 0.47 -12 7 0 6.01 0.52 13 -7 0 75.30 2.19 -13 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13.20 0.51 3 -8 0 14.06 0.48 -3 -8 0 13.44 0.37 3 -8 0 12.98 0.47 3 8 0 13.10 0.48 -3 8 0 12.72 0.41 3 8 0 12.74 0.47 -3 8 0 12.14 0.49 -4 -8 0 51.69 1.32 4 -8 0 53.68 1.43 -4 -8 0 52.26 1.45 4 -8 0 52.40 1.41 4 8 0 51.49 1.40 4 8 0 50.79 1.41 -4 8 0 51.50 1.45 -4 8 0 52.08 1.37 -5 -8 0 18.70 0.67 5 -8 0 19.85 0.66 -5 -8 0 19.41 0.57 5 -8 0 18.56 0.63 5 8 0 18.17 0.60 -5 8 0 18.55 0.66 5 8 0 18.73 0.64 -5 8 0 18.56 0.60 6 -8 0 9.25 0.45 -6 -8 0 9.91 0.38 -6 -8 0 9.70 0.48 6 -8 0 10.08 0.42 -6 8 0 9.31 0.45 6 8 0 10.01 0.44 -6 8 0 9.45 0.41 6 8 0 9.54 0.39 7 -8 0 0.28 0.17 -7 -8 0 0.35 0.14 7 -8 0 0.43 0.15 -7 -8 0 0.29 0.18 7 8 0 0.26 0.12 -7 8 0 0.28 0.16 7 8 0 0.35 0.18 -7 8 0 0.26 0.17 -8 -8 0 1.71 0.28 8 -8 0 2.58 0.30 -8 -8 0 2.72 0.27 8 -8 0 2.13 0.24 -8 8 0 2.33 0.26 8 8 0 2.42 0.27 8 8 0 1.97 0.22 -8 8 0 2.36 0.27 9 -8 0 1.16 0.26 -9 -8 0 1.59 0.28 -9 -8 0 1.40 0.23 9 -8 0 1.50 0.22 -9 8 0 1.50 0.24 9 8 0 1.30 0.23 9 8 0 1.38 0.17 -9 8 0 1.38 0.24 -10 -8 0 3.15 0.36 -10 -8 0 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4 22 0.03 0.00 -1 4 22 -0.59 0.00 -17 5 22 0.24 0.00 -2 5 22 0.31 0.00 -1 5 22 0.33 0.00 -16 6 22 0.04 0.00 -2 6 22 -0.41 0.00 -16 7 22 -0.29 0.00 -15 7 22 -0.38 0.00 -3 7 22 0.44 0.00 -15 8 22 0.25 0.00 -14 8 22 -0.33 0.00 -4 8 22 -0.62 0.00 -3 8 22 0.51 0.00 -14 9 22 -0.39 0.00 -13 9 22 0.43 0.00 -6 9 22 1.41 0.00 -5 9 22 1.40 0.00 -4 9 22 0.00 0.00 -12 10 22 -0.69 0.00 -11 10 22 0.51 0.00 -10 10 22 0.00 0.00 -9 10 22 0.17 0.00 -8 10 22 0.29 0.00 -7 10 22 -0.61 0.00 -6 10 22 -1.90 0.00 -3 0 23 1.37 0.00 -16 1 23 -0.51 0.00 -3 1 23 -0.17 0.00 -16 2 23 0.22 0.00 -4 2 23 -0.03 0.00 -3 2 23 0.94 0.00 -16 3 23 0.27 0.00 -15 3 23 0.51 0.00 -4 3 23 -1.51 0.00 -3 3 23 0.01 0.00 -15 4 23 -0.40 0.00 -4 4 23 -0.23 0.00 -15 5 23 0.53 0.00 -14 5 23 -0.31 0.00 -5 5 23 -0.01 0.00 -4 5 23 -0.24 0.00 -14 6 23 -0.18 0.00 -13 6 23 -0.39 0.00 -6 6 23 -0.47 0.00 -5 6 23 -0.18 0.00 -13 7 23 0.27 0.00 -12 7 23 0.58 0.00 -11 7 23 -0.63 0.00 -10 7 23 -0.17 0.00 -9 7 23 -0.31 0.00 -8 7 23 -0.67 0.00 -7 7 23 0.04 0.00 -6 7 23 0.14 0.00 -11 8 23 0.03 0.00 -10 8 23 0.36 0.00 -9 8 23 0.72 0.00 -8 8 23 0.48 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 301214) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 506 95 ' ' 2 0.500 0.000 0.500 506 95 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL sab14 in P2(1)/n CELL 18.1308 19.2458 18.6533 90.00 115.23 90.00 SPGR P21/n # Solvent Accessible Volume = 1043.6 # Electrons Found in S.A.V. = 188.7 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.580 0.973 0.294 ! 3.27 eA-3 C102 0.892 0.532 0.066 ! 3.16 eA-3 C103 0.907 0.466 0.112 ! 3.08 eA-3 C104 0.925 0.404 0.238 ! 2.75 eA-3 C105 0.926 0.406 0.319 ! 2.61 eA-3 C106 0.871 0.442 0.064 ! 2.47 eA-3 C107 0.633 0.033 0.488 ! 2.24 eA-3 C108 0.376 0.974 0.476 ! 2.20 eA-3 C109 0.634 0.957 0.356 ! 2.00 eA-3 C110 0.200 0.580 0.011 ! 1.95 eA-3 C111 0.222 0.653 0.015 ! 1.75 eA-3 Q112 0.417 0.812 0.426 ! 0.79 eA-3 Q113 0.111 0.510 0.187 ! 0.69 eA-3 Q114 0.362 0.997 0.332 ! 0.58 eA-3 Q115 0.870 0.149 0.172 ! 0.54 eA-3 Q116 0.175 0.312 0.373 ! 0.53 eA-3 ) ; _shelx_fab_checksum 44798