#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 12 _journal_issue 2 _journal_year 2021 _journal_page_first 187 _journal_page_last 191 #============================================================================== data_shelx _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ; 5-Bromospiro[indoline-3,7'-pyrano[3,2-c:5,6-c']dichromene]-2,6',8'-trione ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H12 Br N O6, C2 H6 O S, O' _chemical_formula_sum 'C108 H60 Br4 N4 O29 S2' _chemical_formula_weight 2261.36 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' '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 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 11.8333(6) _cell_length_b 12.8151(6) _cell_length_c 17.1798(8) _cell_angle_alpha 77.317(4) _cell_angle_beta 74.147(4) _cell_angle_gamma 66.493(5) _cell_volume 2280.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 149.99(10) _cell_measurement_reflns_used 4443 _cell_measurement_theta_min 2.0060 _cell_measurement_theta_max 28.0140 _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.647 _exptl_crystal_F_000 1140 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_absorpt_coefficient_mu 1.902 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.62740 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Crys Alis Red' _exptl_special_details ; CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 149.99(10) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9974 _diffrn_reflns_number 11545 _diffrn_reflns_av_unetI/netI 0.0875 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.918 _diffrn_reflns_theta_max 25.499 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.978 _diffrn_reflns_point_group_measured_fraction_full 0.979 _reflns_number_total 8310 _reflns_number_gt 6264 _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. _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 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2018)' _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 2012)' _computing_publication_material 'PLATON (Spek,2009)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+4.9296P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8310 _refine_ls_number_parameters 734 _refine_ls_number_restraints 217 _refine_ls_R_factor_all 0.0906 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1994 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _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 S1 S 0.7856(3) 0.9405(3) 0.5561(2) 0.0335(7) Uani 0.5 1 d D U P A 1 O1 O 0.8854(10) 0.9546(9) 0.5854(7) 0.037(2) Uani 0.5 1 d . U P A 1 C65 C 0.6393(11) 1.0373(12) 0.6055(9) 0.045(3) Uani 0.5 1 d D U P A 1 H65A H 0.571025 1.031730 0.588721 0.067 Uiso 0.5 1 calc R U P A 1 H65B H 0.629894 1.017730 0.663534 0.067 Uiso 0.5 1 calc R U P A 1 H65C H 0.638338 1.114287 0.590689 0.067 Uiso 0.5 1 calc R U P A 1 C66 C 0.7821(14) 1.0148(12) 0.4548(7) 0.045(3) Uani 0.5 1 d D U P A 1 H66A H 0.718093 1.006660 0.434911 0.068 Uiso 0.5 1 calc R U P A 1 H66B H 0.763658 1.094660 0.455716 0.068 Uiso 0.5 1 calc R U P A 1 H66C H 0.862502 0.982961 0.419712 0.068 Uiso 0.5 1 calc R U P A 1 O1' O 0.9438(11) 0.9702(10) 0.5563(7) 0.045(3) Uani 0.5 1 d . U P B 2 O2' O 0.4763(12) 1.0978(11) 0.4242(6) 0.050(3) Uani 0.5 1 d . U P C 2 O3' O 0.552(3) 1.2908(18) 0.3987(16) 0.056(5) Uani 0.5 1 d . U P D 2 S2 S 0.6034(5) 1.1299(4) 0.4557(2) 0.0606(12) Uani 0.5 1 d D U P E 3 O2 O 0.5621(12) 1.0514(11) 0.4256(5) 0.046(3) Uani 0.5 1 d . U P E 3 C67 C 0.7684(13) 1.0924(17) 0.4086(11) 0.071(5) Uani 0.5 1 d D U P E 3 H67A H 0.801984 1.139213 0.424975 0.106 Uiso 0.5 1 calc R U P E 3 H67B H 0.812866 1.013094 0.425452 0.106 Uiso 0.5 1 calc R U P E 3 H67C H 0.778035 1.105063 0.350384 0.106 Uiso 0.5 1 calc R U P E 3 C68 C 0.547(4) 1.2683(19) 0.397(2) 0.046(6) Uani 0.5 1 d D U P E 3 H68A H 0.570679 1.321687 0.414098 0.069 Uiso 0.5 1 calc R U P E 3 H68B H 0.582510 1.261995 0.340259 0.069 Uiso 0.5 1 calc R U P E 3 H68C H 0.456499 1.295066 0.405749 0.069 Uiso 0.5 1 calc R U P E 3 C1 C 0.9616(5) 0.5321(5) 0.2825(3) 0.0205(11) Uani 1 1 d . . . . . C3 C 1.0510(5) 0.6730(5) 0.2779(3) 0.0248(12) Uani 1 1 d . . . . . C4 C 1.1117(5) 0.6031(5) 0.3439(3) 0.0193(11) Uani 1 1 d . . . . . C5 C 1.1945(5) 0.6439(5) 0.3733(3) 0.0201(11) Uani 1 1 d . . . . . C6 C 1.2435(5) 0.5587(5) 0.4445(3) 0.0196(11) Uani 1 1 d . . . . . C7 C 1.3173(5) 0.5849(5) 0.4869(3) 0.0235(12) Uani 1 1 d . . . . . C9 C 1.3403(5) 0.4054(5) 0.5753(3) 0.0229(12) Uani 1 1 d . . . . . C10 C 1.3895(5) 0.3353(5) 0.6404(3) 0.0256(12) Uani 1 1 d . . . . . H10 H 1.442048 0.352192 0.663166 0.031 Uiso 1 1 calc R U . . . C11 C 1.3580(6) 0.2384(5) 0.6710(4) 0.0303(14) Uani 1 1 d . . . . . H11 H 1.390535 0.189410 0.714750 0.036 Uiso 1 1 calc R U . . . C12 C 1.2783(5) 0.2136(5) 0.6372(3) 0.0301(14) Uani 1 1 d . . . . . H12 H 1.256232 0.149651 0.659294 0.036 Uiso 1 1 calc R U . . . C13 C 1.2324(5) 0.2842(5) 0.5710(3) 0.0236(12) Uani 1 1 d . . . . . H13 H 1.181215 0.266681 0.547324 0.028 Uiso 1 1 calc R U . . . C14 C 1.2630(5) 0.3822(5) 0.5395(3) 0.0212(11) Uani 1 1 d . . . . . C15 C 1.2176(5) 0.4623(5) 0.4718(3) 0.0194(11) Uani 1 1 d . . . . . C17 C 1.0923(5) 0.5037(5) 0.3765(3) 0.0213(12) Uani 1 1 d . . . . . C18 C 1.0160(5) 0.4638(5) 0.3468(3) 0.0199(11) Uani 1 1 d . . . . . C19 C 0.9947(5) 0.3612(5) 0.3792(3) 0.0250(12) Uani 1 1 d . . . . . H19 H 1.031612 0.314087 0.421909 0.030 Uiso 1 1 calc R U . . . C20 C 0.9193(6) 0.3306(6) 0.3475(4) 0.0306(14) Uani 1 1 d . . . . . H20 H 0.905884 0.262248 0.368494 0.037 Uiso 1 1 calc R U . . . C21 C 0.8633(6) 0.4013(5) 0.2845(4) 0.0304(14) Uani 1 1 d . . . . . H21 H 0.809838 0.381073 0.264899 0.037 Uiso 1 1 calc R U . . . C22 C 0.8853(6) 0.5016(5) 0.2500(3) 0.0287(13) Uani 1 1 d . . . . . H22 H 0.849990 0.547252 0.206297 0.034 Uiso 1 1 calc R U . . . C23 C 1.2991(5) 0.6661(5) 0.3048(3) 0.0188(11) Uani 1 1 d . . . . . C24 C 1.3930(5) 0.5934(5) 0.2540(3) 0.0205(11) Uani 1 1 d . . . . . H24 H 1.403737 0.516415 0.258972 0.025 Uiso 1 1 calc R U . . . C25 C 1.4718(5) 0.6406(5) 0.1942(3) 0.0242(12) Uani 1 1 d . . . . . C26 C 1.4585(5) 0.7535(5) 0.1852(3) 0.0250(12) Uani 1 1 d . . . . . H26 H 1.513608 0.780859 0.144381 0.030 Uiso 1 1 calc R U . . . C27 C 1.3626(5) 0.8272(5) 0.2369(3) 0.0247(12) Uani 1 1 d . . . . . H27 H 1.352094 0.904142 0.231769 0.030 Uiso 1 1 calc R U . . . C28 C 1.2827(5) 0.7812(5) 0.2968(3) 0.0211(11) Uani 1 1 d D . . . . N1 N 1.168(3) 0.8403(17) 0.347(2) 0.017(4) Uani 0.30(10) 1 d D U P F 4 N1' N 1.1811(17) 0.8365(10) 0.3565(12) 0.020(3) Uani 0.70(10) 1 d D U P F 5 C30 C 1.1187(5) 0.7672(5) 0.3995(3) 0.0220(12) Uani 1 1 d D . . . . O3 O 0.9800(4) 0.6332(3) 0.2485(2) 0.0275(9) Uani 1 1 d . . . . . O8 O 1.3680(3) 0.5039(3) 0.5479(2) 0.0259(9) Uani 1 1 d . . . . . O16 O 1.1436(4) 0.4318(3) 0.4393(2) 0.0227(8) Uani 1 1 d . . . . . O31 O 1.0575(4) 0.7647(4) 0.2460(3) 0.0334(10) Uani 1 1 d . . . . . O32 O 1.3382(4) 0.6735(4) 0.4736(2) 0.0296(9) Uani 1 1 d . . . . . O33 O 1.0224(4) 0.7915(3) 0.4518(2) 0.0282(9) Uani 1 1 d . . . . . Br1 Br 1.60031(6) 0.54418(5) 0.11967(4) 0.0382(2) Uani 1 1 d . . . . . H1 H 1.203(12) 0.85(2) 0.379(3) 0.020(4) Uiso 0.30(10) 1 d D U P F 4 H1' H 1.160(6) 0.907(3) 0.359(4) 0.020(4) Uiso 0.70(10) 1 d D U P F 5 C35 C 0.0465(5) 0.7054(5) 0.9433(3) 0.0218(12) Uani 1 1 d . . . . . C37 C 0.2160(5) 0.7531(5) 0.8488(3) 0.0226(12) Uani 1 1 d . . . . . C38 C 0.2217(5) 0.8142(4) 0.9086(3) 0.0186(11) Uani 1 1 d . . . . . C39 C 0.3205(5) 0.8685(4) 0.8853(3) 0.0169(11) Uani 1 1 d . . . . . C40 C 0.2990(5) 0.9376(4) 0.9535(3) 0.0182(11) Uani 1 1 d . . . . . C41 C 0.3744(5) 1.0089(4) 0.9415(3) 0.0196(11) Uani 1 1 d . . . . . C43 C 0.2687(5) 1.0656(5) 1.0745(3) 0.0206(11) Uani 1 1 d . . . . . C44 C 0.2592(5) 1.1319(4) 1.1318(3) 0.0225(12) Uani 1 1 d . . . . . H44 H 0.313463 1.171347 1.123299 0.027 Uiso 1 1 calc R U . . . C45 C 0.1659(5) 1.1373(5) 1.2020(3) 0.0260(13) Uani 1 1 d . . . . . H45 H 0.157230 1.181422 1.241117 0.031 Uiso 1 1 calc R U . . . C46 C 0.0850(5) 1.0777(5) 1.2150(3) 0.0270(13) Uani 1 1 d . . . . . H46 H 0.022689 1.082717 1.262237 0.032 Uiso 1 1 calc R U . . . C47 C 0.0973(5) 1.0117(5) 1.1580(3) 0.0226(12) Uani 1 1 d . . . . . H47 H 0.043764 0.971319 1.166864 0.027 Uiso 1 1 calc R U . . . C48 C 0.1902(5) 1.0050(4) 1.0866(3) 0.0179(11) Uani 1 1 d . . . . . C49 C 0.2109(5) 0.9388(4) 1.0227(3) 0.0177(11) Uani 1 1 d . . . . . C51 C 0.1364(5) 0.8229(5) 0.9798(3) 0.0200(11) Uani 1 1 d . . . . . C52 C 0.0430(5) 0.7696(4) 1.0001(3) 0.0193(11) Uani 1 1 d . . . . . C53 C -0.0510(5) 0.7821(5) 1.0716(3) 0.0258(12) Uani 1 1 d . . . . . H53 H -0.054184 0.824106 1.110440 0.031 Uiso 1 1 calc R U . . . C54 C -0.1380(5) 0.7318(5) 1.0835(4) 0.0288(13) Uani 1 1 d . . . . . H54 H -0.202086 0.741822 1.129941 0.035 Uiso 1 1 calc R U . . . C55 C -0.1314(5) 0.6660(5) 1.0271(4) 0.0299(14) Uani 1 1 d . . . . . H55 H -0.190093 0.630936 1.036812 0.036 Uiso 1 1 calc R U . . . C56 C -0.0387(5) 0.6517(5) 0.9564(4) 0.0300(13) Uani 1 1 d . . . . . H56 H -0.034032 0.607183 0.918733 0.036 Uiso 1 1 calc R U . . . C57 C 0.4533(5) 0.7837(4) 0.8624(3) 0.0179(11) Uani 1 1 d . . . . . C58 C 0.5206(5) 0.6861(4) 0.9062(3) 0.0195(11) Uani 1 1 d . . . . . H58 H 0.487570 0.664509 0.960183 0.023 Uiso 1 1 calc R U . . . C59 C 0.6423(5) 0.6193(5) 0.8662(4) 0.0284(13) Uani 1 1 d . . . . . C60 C 0.6911(5) 0.6535(6) 0.7862(4) 0.0329(14) Uani 1 1 d . . . . . H60 H 0.772094 0.609883 0.761635 0.040 Uiso 1 1 calc R U . . . C61 C 0.6224(5) 0.7508(5) 0.7424(3) 0.0278(13) Uani 1 1 d . . . . . H61 H 0.655161 0.772148 0.688288 0.033 Uiso 1 1 calc R U . . . C62 C 0.5031(5) 0.8159(5) 0.7810(3) 0.0221(12) Uani 1 1 d D . . . . N2 N 0.4157(5) 0.9131(4) 0.7485(3) 0.0243(10) Uani 1 1 d D U . . . C64 C 0.3045(5) 0.9502(5) 0.8027(3) 0.0243(12) Uani 1 1 d D . . . . O36 O 0.1331(3) 0.6955(3) 0.8710(2) 0.0237(8) Uani 1 1 d . . . . . O42 O 0.3591(3) 1.0659(3) 1.0038(2) 0.0218(8) Uani 1 1 d . . . . . O50 O 0.1297(3) 0.8815(3) 1.0386(2) 0.0214(8) Uani 1 1 d . . . . . O65 O 0.2800(4) 0.7467(4) 0.7803(2) 0.0297(9) Uani 1 1 d . . . . . O66 O 0.4478(4) 1.0213(3) 0.8788(2) 0.0272(9) Uani 1 1 d . . . . . O67 O 0.2094(4) 1.0292(3) 0.7921(2) 0.0317(10) Uani 1 1 d . . . . . Br2 Br 0.74106(7) 0.48001(6) 0.91791(4) 0.0452(2) Uani 1 1 d . . . . . H2 H 0.429(2) 0.942(3) 0.6995(16) 0.027(6) Uiso 1 1 d D 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 S1 0.0387(18) 0.0286(16) 0.0335(17) -0.0080(13) -0.0068(13) -0.0106(14) O1 0.038(6) 0.030(5) 0.035(6) -0.007(4) -0.009(4) -0.001(5) C65 0.033(7) 0.055(8) 0.048(8) -0.019(7) -0.001(6) -0.017(6) C66 0.051(8) 0.044(8) 0.036(7) -0.006(6) -0.010(6) -0.012(6) O1' 0.051(7) 0.043(6) 0.036(6) -0.018(5) -0.002(5) -0.009(5) O2' 0.066(7) 0.072(7) 0.023(5) -0.003(5) -0.011(5) -0.037(6) O3' 0.064(7) 0.077(8) 0.042(8) -0.009(7) -0.005(6) -0.045(7) S2 0.101(3) 0.096(3) 0.0192(17) 0.0049(19) -0.0154(18) -0.075(3) O2 0.068(7) 0.076(8) 0.015(4) -0.003(5) -0.006(5) -0.052(6) C67 0.071(10) 0.089(11) 0.067(10) 0.025(9) -0.034(8) -0.050(9) C68 0.056(10) 0.067(12) 0.034(9) -0.034(9) -0.003(8) -0.033(10) C1 0.023(3) 0.022(3) 0.017(3) -0.001(2) -0.001(2) -0.010(2) C3 0.018(3) 0.032(3) 0.020(3) 0.001(2) -0.004(2) -0.007(2) C4 0.019(3) 0.021(3) 0.015(3) -0.002(2) -0.003(2) -0.003(2) C5 0.025(3) 0.023(3) 0.013(3) 0.001(2) -0.002(2) -0.011(2) C6 0.018(3) 0.025(3) 0.011(3) 0.003(2) -0.003(2) -0.006(2) C7 0.024(3) 0.032(3) 0.009(3) 0.006(2) -0.004(2) -0.009(2) C9 0.019(3) 0.029(3) 0.015(3) 0.004(2) -0.002(2) -0.007(2) C10 0.028(3) 0.026(3) 0.021(3) 0.001(2) -0.007(2) -0.008(2) C11 0.032(3) 0.033(3) 0.018(3) 0.007(2) -0.009(2) -0.006(3) C12 0.031(3) 0.031(3) 0.019(3) 0.010(2) -0.004(2) -0.010(3) C13 0.026(3) 0.019(3) 0.023(3) -0.001(2) -0.006(2) -0.005(2) C14 0.024(3) 0.021(3) 0.013(3) 0.001(2) -0.001(2) -0.005(2) C15 0.022(3) 0.023(3) 0.013(3) 0.000(2) -0.003(2) -0.008(2) C17 0.019(3) 0.031(3) 0.009(3) 0.001(2) -0.001(2) -0.006(2) C18 0.021(3) 0.026(3) 0.011(3) -0.004(2) 0.003(2) -0.009(2) C19 0.030(3) 0.027(3) 0.017(3) -0.002(2) 0.000(2) -0.012(3) C20 0.041(4) 0.037(4) 0.020(3) -0.008(3) 0.000(3) -0.022(3) C21 0.035(3) 0.041(4) 0.023(3) -0.016(3) 0.001(2) -0.021(3) C22 0.033(3) 0.037(3) 0.019(3) -0.007(3) -0.007(2) -0.012(3) C23 0.023(3) 0.023(3) 0.011(3) 0.006(2) -0.006(2) -0.012(2) C24 0.021(3) 0.025(3) 0.013(3) 0.000(2) -0.002(2) -0.008(2) C25 0.023(3) 0.032(3) 0.015(3) 0.000(2) -0.004(2) -0.009(2) C26 0.028(3) 0.034(3) 0.016(3) 0.005(2) -0.006(2) -0.017(3) C27 0.033(3) 0.022(3) 0.022(3) 0.005(2) -0.006(2) -0.016(3) C28 0.025(3) 0.023(3) 0.017(3) 0.002(2) -0.005(2) -0.012(2) N1 0.023(5) 0.017(5) 0.017(6) -0.005(4) -0.007(5) -0.008(4) N1' 0.026(4) 0.021(3) 0.016(4) -0.002(3) -0.009(4) -0.008(3) C30 0.030(3) 0.025(3) 0.013(3) -0.001(2) -0.007(2) -0.010(2) O3 0.032(2) 0.033(2) 0.020(2) 0.0019(17) -0.0099(17) -0.0148(19) O8 0.025(2) 0.035(2) 0.019(2) 0.0057(17) -0.0073(16) -0.0142(18) O16 0.032(2) 0.020(2) 0.019(2) 0.0060(16) -0.0125(16) -0.0127(17) O31 0.039(3) 0.032(2) 0.031(2) 0.0134(19) -0.0184(19) -0.016(2) O32 0.037(2) 0.035(2) 0.023(2) 0.0042(18) -0.0098(17) -0.022(2) O33 0.032(2) 0.025(2) 0.019(2) -0.0024(17) 0.0001(17) -0.0057(18) Br1 0.0347(4) 0.0328(4) 0.0361(4) -0.0089(3) 0.0134(3) -0.0121(3) C35 0.021(3) 0.021(3) 0.023(3) 0.000(2) -0.007(2) -0.007(2) C37 0.024(3) 0.019(3) 0.024(3) 0.003(2) -0.009(2) -0.008(2) C38 0.020(3) 0.016(3) 0.018(3) 0.001(2) -0.008(2) -0.004(2) C39 0.019(3) 0.015(3) 0.016(3) 0.000(2) -0.004(2) -0.007(2) C40 0.020(3) 0.018(3) 0.016(3) -0.001(2) -0.005(2) -0.006(2) C41 0.019(3) 0.019(3) 0.018(3) 0.001(2) -0.007(2) -0.004(2) C43 0.018(3) 0.018(3) 0.018(3) 0.002(2) -0.005(2) -0.001(2) C44 0.029(3) 0.013(3) 0.027(3) -0.004(2) -0.009(2) -0.007(2) C45 0.027(3) 0.030(3) 0.019(3) -0.008(2) -0.006(2) -0.005(2) C46 0.025(3) 0.029(3) 0.017(3) -0.003(2) -0.002(2) -0.002(2) C47 0.018(3) 0.024(3) 0.021(3) -0.001(2) -0.003(2) -0.005(2) C48 0.021(3) 0.016(3) 0.014(3) 0.000(2) -0.006(2) -0.003(2) C49 0.019(3) 0.016(3) 0.016(3) 0.004(2) -0.008(2) -0.004(2) C51 0.018(3) 0.020(3) 0.018(3) 0.001(2) -0.008(2) -0.002(2) C52 0.020(3) 0.014(3) 0.022(3) 0.000(2) -0.007(2) -0.004(2) C53 0.021(3) 0.031(3) 0.022(3) 0.002(2) -0.004(2) -0.010(2) C54 0.023(3) 0.035(3) 0.024(3) 0.011(3) -0.007(2) -0.011(3) C55 0.021(3) 0.039(4) 0.031(3) 0.005(3) -0.007(2) -0.016(3) C56 0.024(3) 0.031(3) 0.033(3) 0.000(3) -0.011(3) -0.007(3) C57 0.024(3) 0.017(3) 0.014(3) -0.006(2) 0.000(2) -0.008(2) C58 0.022(3) 0.016(3) 0.018(3) -0.003(2) -0.003(2) -0.005(2) C59 0.030(3) 0.031(3) 0.027(3) -0.014(3) -0.006(2) -0.008(3) C60 0.020(3) 0.046(4) 0.030(3) -0.017(3) 0.002(2) -0.006(3) C61 0.032(3) 0.035(3) 0.019(3) -0.014(3) 0.007(2) -0.018(3) C62 0.024(3) 0.034(3) 0.010(3) -0.003(2) -0.002(2) -0.014(2) N2 0.037(3) 0.024(2) 0.014(2) 0.0011(19) -0.0025(19) -0.017(2) C64 0.034(3) 0.026(3) 0.015(3) 0.001(2) -0.007(2) -0.014(3) O36 0.028(2) 0.0194(19) 0.030(2) -0.0093(17) -0.0026(16) -0.0138(17) O42 0.0201(19) 0.028(2) 0.018(2) -0.0059(16) -0.0006(15) -0.0097(16) O50 0.025(2) 0.027(2) 0.0154(19) -0.0034(16) -0.0003(15) -0.0148(17) O65 0.038(2) 0.036(2) 0.021(2) -0.0098(18) -0.0012(18) -0.019(2) O66 0.027(2) 0.032(2) 0.020(2) -0.0012(17) 0.0009(16) -0.0135(18) O67 0.040(3) 0.023(2) 0.026(2) 0.0043(17) -0.0159(19) -0.0026(19) Br2 0.0402(4) 0.0376(4) 0.0386(4) -0.0124(3) -0.0121(3) 0.0122(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 S1 O1 1.488(11) . ? S1 C65 1.790(12) . ? S1 C66 1.793(12) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? S2 O2 1.510(10) . ? S2 C68 1.802(19) . ? S2 C67 1.804(14) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C1 O3 1.375(6) . ? C1 C18 1.384(8) . ? C1 C22 1.389(8) . ? C3 O31 1.205(7) . ? C3 O3 1.383(7) . ? C3 C4 1.446(7) . ? C4 C17 1.355(8) . ? C4 C5 1.511(7) . ? C5 C6 1.523(7) . ? C5 C23 1.529(7) . ? C5 C30 1.571(8) . ? C6 C15 1.345(7) . ? C6 C7 1.447(8) . ? C7 O32 1.218(7) . ? C7 O8 1.380(6) . ? C9 C10 1.376(8) . ? C9 O8 1.381(7) . ? C9 C14 1.382(8) . ? C10 C11 1.390(8) . ? C10 H10 0.9300 . ? C11 C12 1.395(9) . ? C11 H11 0.9300 . ? C12 C13 1.379(8) . ? C12 H12 0.9300 . ? C13 C14 1.400(8) . ? C13 H13 0.9300 . ? C14 C15 1.439(7) . ? C15 O16 1.366(6) . ? C17 O16 1.364(6) . ? C17 C18 1.440(8) . ? C18 C19 1.402(8) . ? C19 C20 1.372(8) . ? C19 H19 0.9300 . ? C20 C21 1.384(9) . ? C20 H20 0.9300 . ? C21 C22 1.385(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.366(8) . ? C23 C28 1.389(8) . ? C24 C25 1.395(7) . ? C24 H24 0.9300 . ? C25 C26 1.369(8) . ? C25 Br1 1.900(6) . ? C26 C27 1.390(8) . ? C26 H26 0.9300 . ? C27 C28 1.396(7) . ? C27 H27 0.9300 . ? C28 N1' 1.402(10) . ? C28 N1 1.410(16) . ? N1 C30 1.344(16) . ? N1 H1 0.85(2) . ? N1' C30 1.347(10) . ? N1' H1' 0.84(2) . ? C30 O33 1.218(6) . ? C35 O36 1.372(7) . ? C35 C56 1.379(8) . ? C35 C52 1.389(8) . ? C37 O65 1.213(7) . ? C37 O36 1.379(6) . ? C37 C38 1.452(8) . ? C38 C51 1.350(7) . ? C38 C39 1.512(7) . ? C39 C57 1.514(7) . ? C39 C40 1.527(7) . ? C39 C64 1.575(7) . ? C40 C49 1.349(7) . ? C40 C41 1.462(7) . ? C41 O66 1.210(6) . ? C41 O42 1.359(6) . ? C43 C48 1.381(7) . ? C43 O42 1.383(6) . ? C43 C44 1.390(8) . ? C44 C45 1.389(8) . ? C44 H44 0.9300 . ? C45 C46 1.392(8) . ? C45 H45 0.9300 . ? C46 C47 1.373(8) . ? C46 H46 0.9300 . ? C47 C48 1.399(7) . ? C47 H47 0.9300 . ? C48 C49 1.442(7) . ? C49 O50 1.367(6) . ? C51 O50 1.353(7) . ? C51 C52 1.448(7) . ? C52 C53 1.404(8) . ? C53 C54 1.368(8) . ? C53 H53 0.9300 . ? C54 C55 1.386(9) . ? C54 H54 0.9300 . ? C55 C56 1.387(8) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.372(7) . ? C57 C62 1.402(7) . ? C58 C59 1.419(8) . ? C58 H58 0.9300 . ? C59 C60 1.385(8) . ? C59 Br2 1.884(6) . ? C60 C61 1.377(9) . ? C60 H60 0.9300 . ? C61 C62 1.386(8) . ? C61 H61 0.9300 . ? C62 N2 1.384(7) . ? N2 C64 1.361(7) . ? N2 H2 0.84(2) . ? C64 O67 1.203(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 O1 S1 C65 105.9(6) . . ? O1 S1 C66 108.3(7) . . ? C65 S1 C66 96.9(7) . . ? S1 C65 H65A 109.5 . . ? S1 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? S1 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? S1 C66 H66A 109.5 . . ? S1 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? S1 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? O2 S2 C68 106.3(14) . . ? O2 S2 C67 104.4(8) . . ? C68 S2 C67 97.7(17) . . ? S2 C67 H67A 109.5 . . ? S2 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? S2 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? S2 C68 H68A 109.5 . . ? S2 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? S2 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O3 C1 C18 121.4(5) . . ? O3 C1 C22 117.3(5) . . ? C18 C1 C22 121.3(5) . . ? O31 C3 O3 116.8(5) . . ? O31 C3 C4 124.7(5) . . ? O3 C3 C4 118.4(5) . . ? C17 C4 C3 118.7(5) . . ? C17 C4 C5 122.9(5) . . ? C3 C4 C5 118.4(5) . . ? C4 C5 C6 108.7(4) . . ? C4 C5 C23 112.6(4) . . ? C6 C5 C23 113.3(4) . . ? C4 C5 C30 110.5(4) . . ? C6 C5 C30 110.8(4) . . ? C23 C5 C30 100.8(4) . . ? C15 C6 C7 118.3(5) . . ? C15 C6 C5 123.1(5) . . ? C7 C6 C5 118.5(5) . . ? O32 C7 O8 116.6(5) . . ? O32 C7 C6 125.3(5) . . ? O8 C7 C6 118.1(5) . . ? C10 C9 O8 117.1(5) . . ? C10 C9 C14 122.5(5) . . ? O8 C9 C14 120.3(5) . . ? C9 C10 C11 117.9(5) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? C10 C11 C12 121.0(5) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 119.9(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 119.8(5) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 118.9(5) . . ? C9 C14 C15 117.2(5) . . ? C13 C14 C15 123.9(5) . . ? C6 C15 O16 123.5(5) . . ? C6 C15 C14 123.2(5) . . ? O16 C15 C14 113.3(4) . . ? C4 C17 O16 123.7(5) . . ? C4 C17 C18 122.6(5) . . ? O16 C17 C18 113.6(5) . . ? C1 C18 C19 119.3(5) . . ? C1 C18 C17 116.9(5) . . ? C19 C18 C17 123.8(5) . . ? C20 C19 C18 119.8(6) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 120.2(6) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 121.2(5) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C1 118.3(6) . . ? C21 C22 H22 120.9 . . ? C1 C22 H22 120.9 . . ? C24 C23 C28 121.6(5) . . ? C24 C23 C5 129.8(5) . . ? C28 C23 C5 108.5(5) . . ? C23 C24 C25 116.5(5) . . ? C23 C24 H24 121.7 . . ? C25 C24 H24 121.7 . . ? C26 C25 C24 123.2(5) . . ? C26 C25 Br1 118.7(4) . . ? C24 C25 Br1 118.1(4) . . ? C25 C26 C27 120.1(5) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 117.3(5) . . ? C26 C27 H27 121.4 . . ? C28 C27 H27 121.4 . . ? C23 C28 C27 121.3(5) . . ? C23 C28 N1' 110.4(5) . . ? C27 C28 N1' 128.3(6) . . ? C23 C28 N1 110.0(9) . . ? C27 C28 N1 128.0(8) . . ? C30 N1 C28 111.4(13) . . ? C30 N1 H1 99(10) . . ? C28 N1 H1 94(10) . . ? C30 N1' C28 111.7(8) . . ? C30 N1' H1' 126.7(16) . . ? C28 N1' H1' 121.2(16) . . ? O33 C30 N1 127.2(9) . . ? O33 C30 N1' 127.7(6) . . ? O33 C30 C5 124.0(5) . . ? N1 C30 C5 108.2(9) . . ? N1' C30 C5 108.2(6) . . ? C1 O3 C3 121.9(4) . . ? C7 O8 C9 122.5(4) . . ? C17 O16 C15 118.0(4) . . ? O36 C35 C56 117.3(5) . . ? O36 C35 C52 121.1(5) . . ? C56 C35 C52 121.6(5) . . ? O65 C37 O36 116.4(5) . . ? O65 C37 C38 125.3(5) . . ? O36 C37 C38 118.2(5) . . ? C51 C38 C37 118.6(5) . . ? C51 C38 C39 124.0(5) . . ? C37 C38 C39 117.3(5) . . ? C38 C39 C57 113.3(4) . . ? C38 C39 C40 107.6(4) . . ? C57 C39 C40 115.2(4) . . ? C38 C39 C64 108.9(4) . . ? C57 C39 C64 101.6(4) . . ? C40 C39 C64 110.1(4) . . ? C49 C40 C41 118.8(5) . . ? C49 C40 C39 122.9(5) . . ? C41 C40 C39 118.2(4) . . ? O66 C41 O42 118.4(5) . . ? O66 C41 C40 123.7(5) . . ? O42 C41 C40 117.9(4) . . ? C48 C43 O42 121.7(5) . . ? C48 C43 C44 122.0(5) . . ? O42 C43 C44 116.3(5) . . ? C45 C44 C43 117.7(5) . . ? C45 C44 H44 121.1 . . ? C43 C44 H44 121.1 . . ? C44 C45 C46 121.2(5) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C47 C46 C45 120.0(5) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0(5) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 119.1(5) . . ? C43 C48 C49 116.4(5) . . ? C47 C48 C49 124.5(5) . . ? C40 C49 O50 124.1(5) . . ? C40 C49 C48 122.7(5) . . ? O50 C49 C48 113.2(4) . . ? C38 C51 O50 123.7(5) . . ? C38 C51 C52 122.5(5) . . ? O50 C51 C52 113.8(5) . . ? C35 C52 C53 119.3(5) . . ? C35 C52 C51 116.9(5) . . ? C53 C52 C51 123.8(5) . . ? C54 C53 C52 119.3(6) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C53 C54 C55 120.6(6) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C54 C55 C56 121.0(5) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C35 C56 C55 118.2(6) . . ? C35 C56 H56 120.9 . . ? C55 C56 H56 120.9 . . ? C58 C57 C62 121.1(5) . . ? C58 C57 C39 130.6(5) . . ? C62 C57 C39 108.2(4) . . ? C57 C58 C59 117.6(5) . . ? C57 C58 H58 121.2 . . ? C59 C58 H58 121.2 . . ? C60 C59 C58 120.6(6) . . ? C60 C59 Br2 117.6(4) . . ? C58 C59 Br2 121.8(4) . . ? C61 C60 C59 121.4(5) . . ? C61 C60 H60 119.3 . . ? C59 C60 H60 119.3 . . ? C60 C61 C62 118.2(5) . . ? C60 C61 H61 120.9 . . ? C62 C61 H61 120.9 . . ? N2 C62 C61 128.4(5) . . ? N2 C62 C57 110.5(5) . . ? C61 C62 C57 121.0(5) . . ? C64 N2 C62 112.4(5) . . ? C64 N2 H2 124.7(14) . . ? C62 N2 H2 122.8(14) . . ? O67 C64 N2 128.3(5) . . ? O67 C64 C39 124.5(5) . . ? N2 C64 C39 107.2(5) . . ? C35 O36 C37 122.2(4) . . ? C41 O42 C43 122.2(4) . . ? C51 O50 C49 117.5(4) . . ? 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 O31 C3 C4 C17 177.3(5) . . . . ? O3 C3 C4 C17 -2.8(8) . . . . ? O31 C3 C4 C5 -2.9(8) . . . . ? O3 C3 C4 C5 177.1(4) . . . . ? C17 C4 C5 C6 -2.2(7) . . . . ? C3 C4 C5 C6 177.9(4) . . . . ? C17 C4 C5 C23 124.1(5) . . . . ? C3 C4 C5 C23 -55.7(6) . . . . ? C17 C4 C5 C30 -124.0(5) . . . . ? C3 C4 C5 C30 56.2(6) . . . . ? C4 C5 C6 C15 2.3(7) . . . . ? C23 C5 C6 C15 -123.7(6) . . . . ? C30 C5 C6 C15 123.9(5) . . . . ? C4 C5 C6 C7 -175.3(5) . . . . ? C23 C5 C6 C7 58.8(6) . . . . ? C30 C5 C6 C7 -53.7(6) . . . . ? C15 C6 C7 O32 -173.1(5) . . . . ? C5 C6 C7 O32 4.5(8) . . . . ? C15 C6 C7 O8 6.4(7) . . . . ? C5 C6 C7 O8 -175.9(4) . . . . ? O8 C9 C10 C11 177.2(5) . . . . ? C14 C9 C10 C11 -0.7(8) . . . . ? C9 C10 C11 C12 -0.5(9) . . . . ? C10 C11 C12 C13 1.8(9) . . . . ? C11 C12 C13 C14 -1.8(9) . . . . ? C10 C9 C14 C13 0.6(8) . . . . ? O8 C9 C14 C13 -177.2(5) . . . . ? C10 C9 C14 C15 179.9(5) . . . . ? O8 C9 C14 C15 2.1(8) . . . . ? C12 C13 C14 C9 0.7(8) . . . . ? C12 C13 C14 C15 -178.6(5) . . . . ? C7 C6 C15 O16 176.6(5) . . . . ? C5 C6 C15 O16 -1.0(8) . . . . ? C7 C6 C15 C14 -2.0(8) . . . . ? C5 C6 C15 C14 -179.5(5) . . . . ? C9 C14 C15 C6 -2.3(8) . . . . ? C13 C14 C15 C6 177.0(5) . . . . ? C9 C14 C15 O16 179.0(5) . . . . ? C13 C14 C15 O16 -1.7(7) . . . . ? C3 C4 C17 O16 -179.3(5) . . . . ? C5 C4 C17 O16 0.9(8) . . . . ? C3 C4 C17 C18 1.5(8) . . . . ? C5 C4 C17 C18 -178.4(5) . . . . ? O3 C1 C18 C19 -179.8(5) . . . . ? C22 C1 C18 C19 0.7(8) . . . . ? O3 C1 C18 C17 0.1(7) . . . . ? C22 C1 C18 C17 -179.4(5) . . . . ? C4 C17 C18 C1 -0.2(8) . . . . ? O16 C17 C18 C1 -179.5(4) . . . . ? C4 C17 C18 C19 179.7(5) . . . . ? O16 C17 C18 C19 0.4(7) . . . . ? C1 C18 C19 C20 -0.8(8) . . . . ? C17 C18 C19 C20 179.3(5) . . . . ? C18 C19 C20 C21 -0.7(9) . . . . ? C19 C20 C21 C22 2.4(9) . . . . ? C20 C21 C22 C1 -2.5(9) . . . . ? O3 C1 C22 C21 -178.6(5) . . . . ? C18 C1 C22 C21 0.9(8) . . . . ? C4 C5 C23 C24 -58.5(7) . . . . ? C6 C5 C23 C24 65.3(7) . . . . ? C30 C5 C23 C24 -176.3(5) . . . . ? C4 C5 C23 C28 118.5(5) . . . . ? C6 C5 C23 C28 -117.7(5) . . . . ? C30 C5 C23 C28 0.7(5) . . . . ? C28 C23 C24 C25 0.5(8) . . . . ? C5 C23 C24 C25 177.1(5) . . . . ? C23 C24 C25 C26 0.0(8) . . . . ? C23 C24 C25 Br1 -177.9(4) . . . . ? C24 C25 C26 C27 -0.1(9) . . . . ? Br1 C25 C26 C27 177.7(4) . . . . ? C25 C26 C27 C28 -0.1(8) . . . . ? C24 C23 C28 C27 -0.7(8) . . . . ? C5 C23 C28 C27 -178.0(5) . . . . ? C24 C23 C28 N1' -179.4(13) . . . . ? C5 C23 C28 N1' 3.3(14) . . . . ? C24 C23 C28 N1 170(3) . . . . ? C5 C23 C28 N1 -7(3) . . . . ? C26 C27 C28 C23 0.5(8) . . . . ? C26 C27 C28 N1' 179.0(16) . . . . ? C26 C27 C28 N1 -169(3) . . . . ? C23 C28 N1 C30 11(4) . . . . ? C27 C28 N1 C30 -178.3(18) . . . . ? C23 C28 N1' C30 -7(2) . . . . ? C27 C28 N1' C30 174.7(10) . . . . ? C28 N1 C30 O33 178.3(17) . . . . ? C28 N1 C30 C5 -10(4) . . . . ? C28 N1' C30 O33 -175.1(10) . . . . ? C28 N1' C30 C5 7(2) . . . . ? C4 C5 C30 O33 58.1(7) . . . . ? C6 C5 C30 O33 -62.4(7) . . . . ? C23 C5 C30 O33 177.4(5) . . . . ? C4 C5 C30 N1 -113(3) . . . . ? C6 C5 C30 N1 126(3) . . . . ? C23 C5 C30 N1 6(3) . . . . ? C4 C5 C30 N1' -123.9(13) . . . . ? C6 C5 C30 N1' 115.6(13) . . . . ? C23 C5 C30 N1' -4.6(14) . . . . ? C18 C1 O3 C3 -1.5(8) . . . . ? C22 C1 O3 C3 178.0(5) . . . . ? O31 C3 O3 C1 -177.2(5) . . . . ? C4 C3 O3 C1 2.8(7) . . . . ? O32 C7 O8 C9 172.7(5) . . . . ? C6 C7 O8 C9 -6.9(7) . . . . ? C10 C9 O8 C7 -175.4(5) . . . . ? C14 C9 O8 C7 2.6(8) . . . . ? C4 C17 O16 C15 0.8(7) . . . . ? C18 C17 O16 C15 -179.9(4) . . . . ? C6 C15 O16 C17 -0.7(7) . . . . ? C14 C15 O16 C17 178.0(4) . . . . ? O65 C37 C38 C51 173.8(5) . . . . ? O36 C37 C38 C51 -7.3(7) . . . . ? O65 C37 C38 C39 -3.7(8) . . . . ? O36 C37 C38 C39 175.2(4) . . . . ? C51 C38 C39 C57 125.2(5) . . . . ? C37 C38 C39 C57 -57.4(6) . . . . ? C51 C38 C39 C40 -3.2(7) . . . . ? C37 C38 C39 C40 174.1(4) . . . . ? C51 C38 C39 C64 -122.5(5) . . . . ? C37 C38 C39 C64 54.8(6) . . . . ? C38 C39 C40 C49 4.1(7) . . . . ? C57 C39 C40 C49 -123.2(5) . . . . ? C64 C39 C40 C49 122.6(5) . . . . ? C38 C39 C40 C41 -173.6(4) . . . . ? C57 C39 C40 C41 59.1(6) . . . . ? C64 C39 C40 C41 -55.1(6) . . . . ? C49 C40 C41 O66 -173.4(5) . . . . ? C39 C40 C41 O66 4.4(8) . . . . ? C49 C40 C41 O42 5.3(7) . . . . ? C39 C40 C41 O42 -176.9(4) . . . . ? C48 C43 C44 C45 -1.0(8) . . . . ? O42 C43 C44 C45 177.4(5) . . . . ? C43 C44 C45 C46 0.4(8) . . . . ? C44 C45 C46 C47 0.4(9) . . . . ? C45 C46 C47 C48 -0.6(8) . . . . ? O42 C43 C48 C47 -177.5(5) . . . . ? C44 C43 C48 C47 0.8(8) . . . . ? O42 C43 C48 C49 2.2(7) . . . . ? C44 C43 C48 C49 -179.4(5) . . . . ? C46 C47 C48 C43 0.0(8) . . . . ? C46 C47 C48 C49 -179.7(5) . . . . ? C41 C40 C49 O50 175.8(4) . . . . ? C39 C40 C49 O50 -1.8(8) . . . . ? C41 C40 C49 C48 -1.8(8) . . . . ? C39 C40 C49 C48 -179.4(5) . . . . ? C43 C48 C49 C40 -2.0(7) . . . . ? C47 C48 C49 C40 177.8(5) . . . . ? C43 C48 C49 O50 -179.8(4) . . . . ? C47 C48 C49 O50 -0.1(7) . . . . ? C37 C38 C51 O50 -177.4(5) . . . . ? C39 C38 C51 O50 -0.1(8) . . . . ? C37 C38 C51 C52 2.7(8) . . . . ? C39 C38 C51 C52 180.0(5) . . . . ? O36 C35 C52 C53 176.9(5) . . . . ? C56 C35 C52 C53 -1.3(8) . . . . ? O36 C35 C52 C51 -1.3(7) . . . . ? C56 C35 C52 C51 -179.5(5) . . . . ? C38 C51 C52 C35 1.6(8) . . . . ? O50 C51 C52 C35 -178.3(4) . . . . ? C38 C51 C52 C53 -176.6(5) . . . . ? O50 C51 C52 C53 3.5(7) . . . . ? C35 C52 C53 C54 -0.7(8) . . . . ? C51 C52 C53 C54 177.4(5) . . . . ? C52 C53 C54 C55 2.1(9) . . . . ? C53 C54 C55 C56 -1.5(9) . . . . ? O36 C35 C56 C55 -176.5(5) . . . . ? C52 C35 C56 C55 1.9(8) . . . . ? C54 C55 C56 C35 -0.4(9) . . . . ? C38 C39 C57 C58 -58.4(7) . . . . ? C40 C39 C57 C58 66.0(7) . . . . ? C64 C39 C57 C58 -175.0(5) . . . . ? C38 C39 C57 C62 118.1(5) . . . . ? C40 C39 C57 C62 -117.5(5) . . . . ? C64 C39 C57 C62 1.5(5) . . . . ? C62 C57 C58 C59 0.1(8) . . . . ? C39 C57 C58 C59 176.3(5) . . . . ? C57 C58 C59 C60 1.1(8) . . . . ? C57 C58 C59 Br2 -177.1(4) . . . . ? C58 C59 C60 C61 -2.0(9) . . . . ? Br2 C59 C60 C61 176.3(5) . . . . ? C59 C60 C61 C62 1.5(9) . . . . ? C60 C61 C62 N2 -176.9(6) . . . . ? C60 C61 C62 C57 -0.3(8) . . . . ? C58 C57 C62 N2 176.6(5) . . . . ? C39 C57 C62 N2 -0.3(6) . . . . ? C58 C57 C62 C61 -0.6(8) . . . . ? C39 C57 C62 C61 -177.5(5) . . . . ? C61 C62 N2 C64 175.6(6) . . . . ? C57 C62 N2 C64 -1.3(6) . . . . ? C62 N2 C64 O67 -177.1(6) . . . . ? C62 N2 C64 C39 2.3(6) . . . . ? C38 C39 C64 O67 57.4(7) . . . . ? C57 C39 C64 O67 177.1(5) . . . . ? C40 C39 C64 O67 -60.3(7) . . . . ? C38 C39 C64 N2 -122.0(5) . . . . ? C57 C39 C64 N2 -2.3(5) . . . . ? C40 C39 C64 N2 120.3(5) . . . . ? C56 C35 O36 C37 174.7(5) . . . . ? C52 C35 O36 C37 -3.6(8) . . . . ? O65 C37 O36 C35 -173.1(5) . . . . ? C38 C37 O36 C35 7.9(7) . . . . ? O66 C41 O42 C43 173.6(5) . . . . ? C40 C41 O42 C43 -5.2(7) . . . . ? C48 C43 O42 C41 1.4(7) . . . . ? C44 C43 O42 C41 -177.0(5) . . . . ? C38 C51 O50 C49 3.0(7) . . . . ? C52 C51 O50 C49 -177.1(4) . . . . ? C40 C49 O50 C51 -2.0(7) . . . . ? C48 C49 O50 C51 175.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C66^a H66C^a O33 0.96 2.48 3.126(15) 124.1 . yes C67^c H67C^c O65 0.96 2.65 3.499(18) 147.0 2_676 yes C68^c H68A^c O32 0.96 2.48 3.25(4) 137.1 2_776 yes C68^c H68B^c O65 0.96 2.25 3.17(4) 160.6 2_676 yes N2 H2 O2'^b 0.84(2) 2.18(3) 2.902(11) 143(3) 2_676 yes N2 H2 O2^c 0.84(2) 2.11(3) 2.879(10) 152(5) 2_676 yes _refine_diff_density_max 0.867 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.128 _shelx_res_file ; TITL bb_s3_3_lt_mo_a.res in P-1 shelx.res created by SHELXL-2018/3 at 16:08:01 on 14-May-2020 CELL 0.71073 11.8333 12.8151 17.1798 77.317 74.147 66.493 ZERR 1.00 0.0006 0.0006 0.0008 0.004 0.004 0.005 LATT 1 SFAC C H N O S BR UNIT 108 60 4 29 2 4 MERG 2 OMIT -3.00 51.00 SIMU 0.01 0.02 N1 N1' H1 H1' SIMU 0.01 0.02 N2 H2 SIMU 0.02 0.04 3.5 O2' > C68 SIMU 0.02 0.04 3.5 S1 > O1' DFIX 1.80 0.02 S1 C65 S1 C66 S2 C67 S2 C68 SADI 0.02 C28 N1 C28 N1' SADI 0.02 C30 N1 C30 N1' DFIX 0.85 0.02 N1 H1 N1' H1' N2 H2 ISOR 0.01 N1 N1' N2 SADI 0.02 C62 H2 C64 H2 SADI 0.02 C28 H1 C30 H1 SADI 0.02 C28 H1' C30 H1' HTAB C66 O33 EQIV $1 -x+1, -y+2, -z+1 HTAB C67 O65_$1 EQIV $2 -x+2, -y+2, -z+1 HTAB C68 O32_$2 HTAB C68 O65_$1 HTAB N2 O2'_$1 HTAB N2 O2_$1 FMAP 2 PLAN 25 ACTA HTAB 2.00000 BOND $H CONF L.S. 11 WGHT 0.094000 4.929600 FVAR 0.37330 0.29631 PART 1 S1 5 0.785597 0.940465 0.556111 10.50000 0.03870 0.02856 = 0.03349 -0.00798 -0.00685 -0.01058 O1 4 0.885388 0.954594 0.585360 10.50000 0.03816 0.02976 = 0.03473 -0.00742 -0.00893 -0.00141 C65 1 0.639251 1.037273 0.605486 10.50000 0.03264 0.05518 = 0.04826 -0.01894 -0.00082 -0.01652 AFIX 33 H65A 2 0.571025 1.031730 0.588721 10.50000 -1.50000 H65B 2 0.629894 1.017730 0.663534 10.50000 -1.50000 H65C 2 0.638338 1.114287 0.590689 10.50000 -1.50000 AFIX 0 C66 1 0.782050 1.014826 0.454848 10.50000 0.05118 0.04407 = 0.03602 -0.00632 -0.01033 -0.01168 AFIX 33 H66A 2 0.718093 1.006660 0.434911 10.50000 -1.50000 H66B 2 0.763658 1.094660 0.455716 10.50000 -1.50000 H66C 2 0.862502 0.982961 0.419712 10.50000 -1.50000 AFIX 0 PART 2 O1' 4 0.943793 0.970211 0.556267 10.50000 0.05062 0.04335 = 0.03621 -0.01798 -0.00192 -0.00876 O2' 4 0.476276 1.097777 0.424167 10.50000 0.06647 0.07167 = 0.02269 -0.00332 -0.01107 -0.03703 O3' 4 0.551545 1.290779 0.398657 10.50000 0.06407 0.07699 = 0.04162 -0.00880 -0.00453 -0.04502 PART 3 S2 5 0.603418 1.129901 0.455743 10.50000 0.10097 0.09557 = 0.01921 0.00486 -0.01536 -0.07465 O2 4 0.562091 1.051360 0.425614 10.50000 0.06835 0.07616 = 0.01526 -0.00303 -0.00593 -0.05223 C67 1 0.768374 1.092435 0.408626 10.50000 0.07094 0.08924 = 0.06743 0.02464 -0.03383 -0.05026 AFIX 33 H67A 2 0.801984 1.139213 0.424975 10.50000 -1.50000 H67B 2 0.812866 1.013094 0.425452 10.50000 -1.50000 H67C 2 0.778035 1.105063 0.350384 10.50000 -1.50000 AFIX 0 C68 1 0.546644 1.268334 0.397113 10.50000 0.05569 0.06719 = 0.03416 -0.03358 -0.00253 -0.03281 AFIX 33 H68A 2 0.570679 1.321687 0.414098 10.50000 -1.50000 H68B 2 0.582510 1.261995 0.340259 10.50000 -1.50000 H68C 2 0.456499 1.295066 0.405749 10.50000 -1.50000 AFIX 0 MOLE 1 PART 0 C1 1 0.961551 0.532069 0.282476 11.00000 0.02318 0.02151 = 0.01657 -0.00053 -0.00149 -0.01044 C3 1 1.051005 0.673036 0.277915 11.00000 0.01779 0.03222 = 0.02009 0.00133 -0.00365 -0.00732 C4 1 1.111739 0.603057 0.343881 11.00000 0.01868 0.02068 = 0.01467 -0.00225 -0.00316 -0.00334 C5 1 1.194456 0.643859 0.373303 11.00000 0.02474 0.02253 = 0.01264 0.00119 -0.00186 -0.01112 C6 1 1.243451 0.558725 0.444511 11.00000 0.01837 0.02537 = 0.01067 0.00256 -0.00290 -0.00584 C7 1 1.317272 0.584859 0.486900 11.00000 0.02390 0.03219 = 0.00942 0.00629 -0.00440 -0.00913 C9 1 1.340331 0.405432 0.575264 11.00000 0.01866 0.02917 = 0.01470 0.00350 -0.00201 -0.00657 C10 1 1.389461 0.335294 0.640393 11.00000 0.02752 0.02578 = 0.02118 0.00085 -0.00686 -0.00804 AFIX 43 H10 2 1.442048 0.352192 0.663166 11.00000 -1.20000 AFIX 0 C11 1 1.357998 0.238445 0.671035 11.00000 0.03177 0.03267 = 0.01849 0.00730 -0.00925 -0.00622 AFIX 43 H11 2 1.390535 0.189410 0.714750 11.00000 -1.20000 AFIX 0 C12 1 1.278318 0.213641 0.637208 11.00000 0.03081 0.03101 = 0.01936 0.01038 -0.00390 -0.00971 AFIX 43 H12 2 1.256232 0.149651 0.659294 11.00000 -1.20000 AFIX 0 C13 1 1.232391 0.284171 0.570982 11.00000 0.02625 0.01886 = 0.02264 -0.00114 -0.00576 -0.00532 AFIX 43 H13 2 1.181215 0.266681 0.547324 11.00000 -1.20000 AFIX 0 C14 1 1.263031 0.382194 0.539462 11.00000 0.02392 0.02080 = 0.01253 0.00065 -0.00142 -0.00465 C15 1 1.217576 0.462307 0.471786 11.00000 0.02177 0.02257 = 0.01289 -0.00049 -0.00320 -0.00817 C17 1 1.092338 0.503744 0.376484 11.00000 0.01857 0.03126 = 0.00873 0.00056 -0.00095 -0.00620 C18 1 1.015962 0.463802 0.346792 11.00000 0.02132 0.02555 = 0.01062 -0.00422 0.00294 -0.00923 C19 1 0.994724 0.361217 0.379154 11.00000 0.02989 0.02672 = 0.01651 -0.00176 -0.00041 -0.01164 AFIX 43 H19 2 1.031612 0.314087 0.421909 11.00000 -1.20000 AFIX 0 C20 1 0.919350 0.330647 0.347519 11.00000 0.04075 0.03672 = 0.02039 -0.00837 -0.00014 -0.02182 AFIX 43 H20 2 0.905884 0.262248 0.368494 11.00000 -1.20000 AFIX 0 C21 1 0.863264 0.401291 0.284470 11.00000 0.03529 0.04128 = 0.02285 -0.01570 0.00100 -0.02064 AFIX 43 H21 2 0.809838 0.381073 0.264899 11.00000 -1.20000 AFIX 0 C22 1 0.885307 0.501552 0.250018 11.00000 0.03265 0.03735 = 0.01880 -0.00706 -0.00719 -0.01228 AFIX 43 H22 2 0.849990 0.547252 0.206297 11.00000 -1.20000 AFIX 0 C23 1 1.299085 0.666070 0.304755 11.00000 0.02350 0.02268 = 0.01125 0.00593 -0.00648 -0.01165 C24 1 1.392962 0.593380 0.253966 11.00000 0.02130 0.02479 = 0.01299 0.00004 -0.00177 -0.00826 AFIX 43 H24 2 1.403737 0.516415 0.258972 11.00000 -1.20000 AFIX 0 C25 1 1.471840 0.640575 0.194196 11.00000 0.02322 0.03194 = 0.01482 0.00033 -0.00372 -0.00912 C26 1 1.458462 0.753474 0.185169 11.00000 0.02815 0.03357 = 0.01603 0.00451 -0.00557 -0.01713 AFIX 43 H26 2 1.513608 0.780859 0.144381 11.00000 -1.20000 AFIX 0 C27 1 1.362576 0.827235 0.236878 11.00000 0.03290 0.02162 = 0.02225 0.00463 -0.00628 -0.01617 AFIX 43 H27 2 1.352094 0.904142 0.231769 11.00000 -1.20000 AFIX 0 C28 1 1.282660 0.781166 0.296787 11.00000 0.02454 0.02325 = 0.01673 0.00206 -0.00528 -0.01167 PART 4 N1 3 1.168272 0.840266 0.347311 21.00000 0.02278 0.01689 = 0.01651 -0.00546 -0.00718 -0.00771 PART 5 N1' 3 1.181098 0.836464 0.356533 -21.00000 0.02607 0.02071 = 0.01649 -0.00236 -0.00859 -0.00791 PART 0 C30 1 1.118736 0.767239 0.399496 11.00000 0.02972 0.02480 = 0.01273 -0.00132 -0.00672 -0.01001 O3 4 0.979961 0.633161 0.248499 11.00000 0.03214 0.03332 = 0.02014 0.00186 -0.00993 -0.01477 O8 4 1.368044 0.503894 0.547919 11.00000 0.02489 0.03452 = 0.01905 0.00567 -0.00732 -0.01423 O16 4 1.143612 0.431752 0.439349 11.00000 0.03211 0.02030 = 0.01915 0.00600 -0.01255 -0.01273 O31 4 1.057525 0.764674 0.246048 11.00000 0.03933 0.03169 = 0.03063 0.01339 -0.01835 -0.01609 O32 4 1.338246 0.673499 0.473603 11.00000 0.03719 0.03489 = 0.02328 0.00422 -0.00984 -0.02151 O33 4 1.022413 0.791545 0.451803 11.00000 0.03186 0.02504 = 0.01948 -0.00239 0.00010 -0.00567 BR1 6 1.600311 0.544183 0.119670 11.00000 0.03469 0.03281 = 0.03606 -0.00886 0.01342 -0.01206 PART 4 H1 2 1.203307 0.854153 0.378604 21.00000 0.01991 PART 5 H1' 2 1.159640 0.906984 0.359222 -21.00000 0.01967 MOLE 2 PART 0 C35 1 0.046491 0.705430 0.943346 11.00000 0.02070 0.02057 = 0.02325 -0.00037 -0.00658 -0.00656 C37 1 0.216039 0.753062 0.848775 11.00000 0.02397 0.01923 = 0.02444 0.00253 -0.00899 -0.00772 C38 1 0.221718 0.814161 0.908629 11.00000 0.02016 0.01590 = 0.01792 0.00120 -0.00775 -0.00377 C39 1 0.320524 0.868541 0.885319 11.00000 0.01891 0.01519 = 0.01647 -0.00041 -0.00401 -0.00653 C40 1 0.299047 0.937643 0.953472 11.00000 0.01984 0.01826 = 0.01588 -0.00109 -0.00546 -0.00575 C41 1 0.374418 1.008860 0.941453 11.00000 0.01933 0.01874 = 0.01790 0.00075 -0.00659 -0.00389 C43 1 0.268685 1.065572 1.074545 11.00000 0.01837 0.01844 = 0.01841 0.00210 -0.00538 -0.00106 C44 1 0.259180 1.131905 1.131771 11.00000 0.02923 0.01303 = 0.02719 -0.00447 -0.00874 -0.00661 AFIX 43 H44 2 0.313463 1.171347 1.123299 11.00000 -1.20000 AFIX 0 C45 1 0.165866 1.137271 1.202024 11.00000 0.02652 0.03002 = 0.01929 -0.00802 -0.00562 -0.00496 AFIX 43 H45 2 0.157230 1.181422 1.241117 11.00000 -1.20000 AFIX 0 C46 1 0.084995 1.077731 1.214984 11.00000 0.02541 0.02937 = 0.01672 -0.00280 -0.00188 -0.00184 AFIX 43 H46 2 0.022689 1.082717 1.262237 11.00000 -1.20000 AFIX 0 C47 1 0.097258 1.011659 1.157987 11.00000 0.01841 0.02431 = 0.02147 -0.00122 -0.00344 -0.00538 AFIX 43 H47 2 0.043764 0.971319 1.166864 11.00000 -1.20000 AFIX 0 C48 1 0.190226 1.005032 1.086564 11.00000 0.02083 0.01623 = 0.01416 0.00005 -0.00616 -0.00339 C49 1 0.210917 0.938791 1.022729 11.00000 0.01866 0.01599 = 0.01596 0.00411 -0.00774 -0.00415 C51 1 0.136369 0.822940 0.979797 11.00000 0.01781 0.02049 = 0.01791 0.00139 -0.00770 -0.00239 C52 1 0.042993 0.769614 1.000064 11.00000 0.02001 0.01423 = 0.02185 0.00027 -0.00694 -0.00386 C53 1 -0.051029 0.782096 1.071588 11.00000 0.02117 0.03150 = 0.02195 0.00250 -0.00380 -0.01008 AFIX 43 H53 2 -0.054184 0.824106 1.110440 11.00000 -1.20000 AFIX 0 C54 1 -0.137963 0.731794 1.083520 11.00000 0.02289 0.03469 = 0.02392 0.01056 -0.00714 -0.01112 AFIX 43 H54 2 -0.202086 0.741822 1.129941 11.00000 -1.20000 AFIX 0 C55 1 -0.131412 0.666018 1.027090 11.00000 0.02092 0.03949 = 0.03128 0.00482 -0.00736 -0.01637 AFIX 43 H55 2 -0.190093 0.630936 1.036812 11.00000 -1.20000 AFIX 0 C56 1 -0.038663 0.651750 0.956362 11.00000 0.02428 0.03068 = 0.03339 0.00004 -0.01106 -0.00709 AFIX 43 H56 2 -0.034032 0.607183 0.918733 11.00000 -1.20000 AFIX 0 C57 1 0.453308 0.783660 0.862412 11.00000 0.02370 0.01657 = 0.01430 -0.00594 -0.00031 -0.00836 C58 1 0.520581 0.686097 0.906198 11.00000 0.02203 0.01581 = 0.01843 -0.00302 -0.00336 -0.00453 AFIX 43 H58 2 0.487570 0.664509 0.960183 11.00000 -1.20000 AFIX 0 C59 1 0.642261 0.619333 0.866203 11.00000 0.03002 0.03052 = 0.02661 -0.01361 -0.00603 -0.00769 C60 1 0.691110 0.653534 0.786247 11.00000 0.01993 0.04550 = 0.02972 -0.01738 0.00196 -0.00619 AFIX 43 H60 2 0.772094 0.609883 0.761635 11.00000 -1.20000 AFIX 0 C61 1 0.622398 0.750773 0.742375 11.00000 0.03240 0.03529 = 0.01924 -0.01437 0.00681 -0.01797 AFIX 43 H61 2 0.655161 0.772148 0.688288 11.00000 -1.20000 AFIX 0 C62 1 0.503110 0.815943 0.780970 11.00000 0.02448 0.03431 = 0.01015 -0.00321 -0.00183 -0.01437 N2 3 0.415681 0.913097 0.748495 11.00000 0.03721 0.02423 = 0.01396 0.00108 -0.00252 -0.01712 C64 1 0.304502 0.950175 0.802745 11.00000 0.03434 0.02568 = 0.01530 0.00149 -0.00714 -0.01412 O36 4 0.133083 0.695497 0.870979 11.00000 0.02784 0.01939 = 0.02989 -0.00930 -0.00256 -0.01380 O42 4 0.359103 1.065866 1.003836 11.00000 0.02011 0.02784 = 0.01780 -0.00591 -0.00061 -0.00970 O50 4 0.129701 0.881507 1.038581 11.00000 0.02548 0.02659 = 0.01537 -0.00342 -0.00027 -0.01478 O65 4 0.280032 0.746689 0.780253 11.00000 0.03765 0.03594 = 0.02108 -0.00979 -0.00116 -0.01888 O66 4 0.447777 1.021273 0.878752 11.00000 0.02708 0.03235 = 0.02017 -0.00120 0.00087 -0.01352 O67 4 0.209375 1.029164 0.792080 11.00000 0.03960 0.02325 = 0.02594 0.00427 -0.01593 -0.00265 BR2 6 0.741058 0.480014 0.917909 11.00000 0.04022 0.03757 = 0.03861 -0.01236 -0.01212 0.01217 H2 2 0.429389 0.942500 0.699486 11.00000 0.02690 HKLF 4 REM bb_s3_3_lt_mo_a.res in P-1 REM wR2 = 0.1994, GooF = S = 1.044, Restrained GooF = 1.033 for all data REM R1 = 0.0622 for 6264 Fo > 4sig(Fo) and 0.0906 for all 8310 data REM 734 parameters refined using 217 restraints END WGHT 0.0940 4.9295 REM Instructions for potential hydrogen bonds HTAB C66 O33 HTAB C67 O65_$1 HTAB C68 O32_$2 HTAB C68 O65_$1 HTAB N2 O2'_$1 HTAB N2 O2_$1 REM Highest difference peak 0.867, deepest hole -0.949, 1-sigma level 0.128 Q1 1 1.7172 0.5437 0.1227 11.00000 0.05 0.87 Q2 1 1.4946 0.6173 0.1390 11.00000 0.05 0.86 Q3 1 0.8368 0.4173 0.8826 11.00000 0.05 0.85 Q4 1 1.4936 0.5397 0.1232 11.00000 0.05 0.83 Q5 1 0.8971 0.3813 0.9115 11.00000 0.05 0.80 Q6 1 0.8583 0.4840 0.9168 11.00000 0.05 0.79 Q7 1 1.6970 0.4770 0.0946 11.00000 0.05 0.78 Q8 1 0.8646 0.4002 0.8980 11.00000 0.05 0.76 Q9 1 1.7165 0.4584 0.1094 11.00000 0.05 0.74 Q10 1 1.4578 0.6391 0.1246 11.00000 0.05 0.69 Q11 1 0.6971 0.4965 0.9710 11.00000 0.05 0.68 Q12 1 0.6359 0.4779 0.9166 11.00000 0.05 0.64 Q13 1 1.4072 0.6595 0.1247 11.00000 0.05 0.63 Q14 1 0.6536 0.4637 0.9349 11.00000 0.05 0.63 Q15 1 1.7457 0.4427 0.1245 11.00000 0.05 0.61 Q16 1 0.6450 0.5387 0.9476 11.00000 0.05 0.61 Q17 1 0.1119 0.5555 0.9457 11.00000 0.05 0.56 Q18 1 0.1545 0.5991 0.8670 11.00000 0.05 0.54 Q19 1 1.3193 0.6966 0.1074 11.00000 0.05 0.53 Q20 1 0.6372 0.5589 0.9286 11.00000 0.05 0.52 Q21 1 0.6844 1.0872 0.4309 11.00000 0.05 0.50 Q22 1 0.4372 1.0805 1.1036 11.00000 0.05 0.49 Q23 1 0.2604 1.2154 1.1317 11.00000 0.05 0.48 Q24 1 0.1702 0.5389 0.9315 11.00000 0.05 0.47 Q25 1 -0.1372 0.7967 1.0235 11.00000 0.05 0.47 ; _shelx_res_checksum 45264 _shelx_hkl_file ; 0 0 -2 728.55 13.92 0 0 2 753.60 13.75 0 0 -3 454.76 13.44 0 0 3 453.88 13.17 0 0 -4 369.63 14.13 0 0 -5 175.01 10.74 0 0 -6 2769.58 47.79 0 0 -7 17.95 4.85 0 0 -8 95.56 10.58 0 0 -9 1475.93 43.35 0 0 -10 171.98 16.01 0 0 -11 249.87 20.11 0 0 -12 206.10 19.50 0 0 -13 3.35 3.29 0 0 -14 44.70 9.74 0 0 -15 58.18 12.20 0 0 -16 52.11 12.35 0 0 -17 23.76 9.33 0 0 -18 58.95 14.46 0 0 -19 80.43 17.37 0 0 -20 27.16 11.26 0 1 -20 75.30 17.05 0 1 -19 59.14 15.22 0 1 -18 7.59 6.89 0 1 -17 72.17 15.64 0 1 -16 16.20 7.31 0 1 -15 17.06 7.57 0 1 -14 6.58 5.30 0 1 -13 49.76 11.03 0 1 -12 35.71 8.83 0 1 -11 112.38 13.79 0 1 -10 154.93 15.41 0 1 -9 26.63 6.32 0 1 -8 101.74 10.92 0 1 -7 7.83 3.20 0 1 -6 359.82 17.86 0 -1 5 2246.90 16.87 0 1 -5 2239.06 40.40 0 1 -4 82.54 7.29 0 -1 4 97.65 3.62 0 1 -3 64.04 5.54 0 -1 3 57.08 2.74 0 1 -2 1562.99 23.05 0 -1 2 1593.75 15.78 0 -1 1 76.26 4.11 0 1 -1 95.66 4.73 0 -1 -1 202.51 7.06 0 1 1 420.17 9.03 0 -1 -2 898.77 13.68 0 1 2 1020.51 16.72 0 -1 -2 1012.80 17.54 0 1 3 18.88 2.75 0 -1 -3 31.54 2.15 0 -1 -3 30.42 3.62 0 1 4 1780.74 30.37 0 -1 -4 1772.62 31.31 0 -1 -4 1897.41 15.73 0 -1 -5 3245.41 47.59 0 1 5 3180.65 45.25 0 -1 -6 157.13 4.55 0 1 6 152.95 10.93 0 -1 -6 142.33 10.84 0 1 7 321.87 17.12 0 -1 -7 317.39 17.50 0 -1 -8 465.65 22.66 0 1 8 474.23 22.18 0 -1 -9 6.05 3.13 0 -1 -10 173.81 15.68 0 -1 -11 225.28 18.74 0 -1 -12 39.52 8.67 0 -1 -13 94.44 13.58 0 -1 -14 11.96 5.82 0 -1 -15 25.77 7.20 0 -1 -16 102.48 16.10 0 -1 -17 26.76 9.12 0 -1 -18 74.75 15.51 0 -1 -19 39.13 12.29 0 -1 -20 52.65 14.50 0 2 -19 6.87 6.44 0 2 -18 2.42 3.13 0 2 -17 30.91 10.20 0 2 -16 74.58 15.09 0 2 -15 6.62 5.76 0 2 -14 6.10 6.08 0 2 -13 1.78 3.75 0 2 -12 15.70 5.91 0 2 -11 199.07 19.13 0 2 -10 38.24 8.42 0 2 -9 131.78 13.93 0 2 -8 391.58 22.62 0 -2 8 368.72 9.94 0 2 -7 27.08 6.13 0 -2 7 18.12 2.28 0 -2 6 2664.41 28.36 0 2 -6 2276.54 47.44 0 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13.21 4.32 0 3 10 62.75 9.20 0 -3 -10 55.59 8.97 0 -3 -10 65.89 5.41 0 -3 -11 -0.15 2.22 0 3 11 -0.40 2.18 0 -3 -12 45.27 9.18 0 3 12 40.10 8.89 0 -3 -13 7.12 4.49 0 3 13 6.39 4.83 0 -3 -14 45.23 10.19 0 -3 -15 27.39 8.35 0 -3 -16 9.69 7.07 0 -3 -17 6.86 4.83 0 -3 -18 1.03 3.64 0 -3 -19 143.12 21.60 0 -3 -20 29.90 10.46 0 -3 -21 18.91 8.93 0 4 -19 8.40 6.85 0 4 -18 27.03 10.03 0 4 -17 3.24 3.51 0 4 -16 4.62 4.69 0 4 -15 18.47 7.69 0 4 -14 0.97 4.01 0 4 -13 38.93 10.33 0 4 -12 124.14 17.06 0 4 -11 5.95 4.24 0 4 -10 143.88 16.69 0 4 -9 6.73 4.31 0 -4 8 291.80 13.21 0 4 -8 259.32 20.11 0 -4 7 608.37 19.71 0 4 -7 456.40 25.47 0 4 -6 843.22 32.56 0 -4 6 882.41 22.29 0 4 -5 125.91 12.03 0 -4 5 102.01 7.21 0 -4 4 275.53 11.99 0 4 -4 282.42 17.15 0 4 -3 314.11 16.95 0 -4 3 332.10 13.35 0 4 -2 470.73 19.71 0 -4 2 466.83 16.46 0 -4 1 3462.89 45.99 0 4 -1 3365.78 49.83 0 4 -1 3480.52 49.88 0 4 0 1408.95 31.45 0 -4 0 1404.50 29.25 0 4 0 1421.42 31.37 0 -4 -1 138.74 9.57 0 4 1 136.41 9.47 0 4 2 54.56 6.05 0 -4 -2 46.19 5.48 0 -4 -3 2633.64 40.16 0 4 3 2442.48 42.79 0 4 4 794.69 24.49 0 -4 -4 883.08 22.54 0 4 5 712.89 24.82 0 -4 -5 792.66 20.93 0 -4 -6 175.36 13.21 0 4 6 165.19 12.34 0 -4 -6 195.84 10.37 0 -4 -7 315.28 13.48 0 -4 -7 274.70 17.65 0 4 7 268.37 16.43 0 -4 -8 21.79 5.62 0 4 8 9.07 3.41 0 -4 -8 13.90 2.63 0 -4 -9 76.58 7.29 0 -4 -9 55.49 9.22 0 4 9 51.50 8.22 0 -4 -10 20.42 5.90 0 4 10 13.84 4.26 0 -4 -10 18.16 3.63 0 -4 -11 237.64 19.87 0 4 11 228.36 18.65 0 -4 -12 104.85 13.57 0 4 12 108.68 13.40 0 -4 -13 342.47 26.10 0 4 13 344.87 25.28 0 4 14 132.77 16.36 0 -4 -14 122.89 16.67 0 -4 -15 169.35 19.70 0 -4 -16 12.05 6.24 0 -4 -17 26.05 8.88 0 -4 -18 25.63 9.16 0 -4 -19 58.26 14.45 0 -4 -20 19.99 8.11 0 -4 -21 26.56 10.89 0 5 -18 11.98 7.20 0 5 -17 4.59 6.09 0 5 -16 2.04 3.64 0 5 -15 8.67 4.42 0 5 -14 37.97 11.10 0 5 -13 0.28 3.12 0 5 -12 19.00 6.73 0 5 -11 256.45 24.29 0 5 -10 114.87 15.09 0 5 -9 71.98 11.68 0 -5 8 165.07 11.66 0 5 -8 123.39 14.88 0 5 -7 611.12 31.18 0 -5 7 768.22 24.57 0 5 -6 665.95 31.05 0 -5 6 677.29 22.24 0 -5 5 439.12 17.46 0 5 -5 430.15 23.73 0 5 -4 85.98 10.06 0 -5 4 76.21 7.24 0 5 -3 808.79 29.78 0 -5 3 768.30 22.78 0 5 -2 3169.78 56.62 0 -5 2 3052.60 45.96 0 5 -2 3119.86 56.82 0 -5 1 663.05 21.98 0 5 -1 674.41 25.08 0 5 -1 683.48 25.09 0 5 0 97.35 9.25 0 5 0 85.45 8.78 0 -5 0 91.79 8.45 0 5 1 7.39 2.82 0 -5 -1 6.64 2.82 0 5 2 658.68 23.38 0 -5 -2 698.58 22.64 0 5 3 407.07 18.97 0 -5 -3 406.31 17.22 0 -5 -4 581.23 20.20 0 5 4 555.48 22.63 0 5 5 19.16 4.10 0 -5 -5 -4.91 7.32 0 -5 -6 3.98 2.32 0 5 6 4.06 1.88 0 -5 -7 225.29 16.87 0 5 7 253.49 16.66 0 -5 -7 278.98 14.03 0 -5 -8 39.54 7.30 0 5 8 43.88 7.43 0 -5 -8 46.31 5.98 0 5 9 43.22 7.65 0 -5 -9 68.45 7.68 0 -5 -9 55.15 8.96 0 5 10 11.19 4.17 0 -5 -10 11.71 5.46 0 -5 -10 16.12 4.14 0 -5 -11 134.47 10.50 0 5 11 120.68 13.97 0 -5 -11 122.23 14.46 0 -5 -12 2.15 3.48 0 5 12 3.65 2.78 0 -5 -13 3.34 2.35 0 5 13 7.50 4.92 0 -5 -14 12.73 6.05 0 5 14 21.01 6.45 0 5 15 31.60 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6.31 5.03 -13 -12 -6 21.52 9.01 -13 -12 -7 15.07 6.90 -13 -12 -8 15.90 7.85 -13 -12 -9 111.48 17.04 -13 -12 -10 2.07 4.38 -13 -12 -11 77.60 14.18 -13 -12 -12 18.87 7.84 -13 -12 -13 43.73 10.65 -14 0 -3 58.80 15.44 -14 0 -4 95.96 19.58 -14 0 -5 49.38 14.15 -14 0 -6 18.92 7.19 -14 -1 1 37.26 11.24 -14 -1 0 55.74 14.42 -14 -1 -1 20.52 9.84 -14 -1 -2 29.36 10.92 -14 -1 -3 6.80 5.76 -14 -1 -4 4.29 3.14 -14 -1 -5 4.39 4.73 -14 -1 -6 18.87 9.03 -14 -1 -7 -1.27 4.11 -14 -1 -8 6.74 5.80 -14 -1 -9 -0.28 2.85 -14 -1 -10 37.99 11.71 -14 -2 3 2.19 3.43 -14 -2 2 2.65 3.98 -14 -2 1 71.45 15.74 -14 -2 0 22.17 9.10 -14 -2 -1 -2.16 3.95 -14 -2 -2 35.38 11.07 -14 -2 -3 40.87 13.01 -14 -2 -4 35.79 13.01 -14 -2 -5 82.39 17.06 -14 -2 -6 -0.07 2.90 -14 -2 -7 -5.87 6.33 -14 -2 -8 27.19 10.15 -14 -2 -9 10.36 6.38 -14 -2 -10 25.15 9.66 -14 -2 -11 0.76 4.59 -14 -2 -12 -1.97 4.34 -14 -2 -13 9.36 6.93 -14 -3 4 23.23 9.58 -14 -3 3 -0.45 3.06 -14 -3 3 -9.54 8.37 -14 -3 2 14.65 7.53 -14 -3 2 19.31 8.99 -14 -3 1 13.33 7.33 -14 -3 1 12.73 6.19 -14 -3 0 23.67 8.83 -14 -3 0 23.88 9.43 -14 -3 -1 6.79 5.94 -14 -3 -1 -7.37 7.80 -14 -3 -2 3.30 4.81 -14 -3 -2 12.56 8.00 -14 -3 -3 13.82 6.06 -14 -3 -3 12.08 6.39 -14 -3 -4 46.18 12.53 -14 -3 -4 38.57 10.10 -14 -3 -5 28.60 10.03 -14 -3 -5 32.42 9.92 -14 -3 -6 -2.10 5.22 -14 -3 -6 5.35 3.16 -14 -3 -7 23.86 9.06 -14 -3 -8 9.97 5.11 -14 -3 -9 12.82 7.07 -14 -3 -10 2.11 4.22 -14 -3 -11 5.63 5.52 -14 -3 -12 -3.18 3.59 -14 -3 -13 -6.63 6.97 -14 -3 -14 4.33 4.10 -14 -4 3 5.78 5.13 -14 -4 2 18.60 7.18 -14 -4 1 42.94 12.21 -14 -4 0 12.27 6.44 -14 -4 -1 -2.40 5.16 -14 -4 -2 11.04 5.04 -14 -4 -3 104.41 18.49 -14 -4 -4 14.40 7.75 -14 -4 -5 81.83 16.60 -14 -4 -6 -1.77 5.37 -14 -4 -7 18.76 7.60 -14 -4 -8 35.04 10.48 -14 -4 -9 27.98 9.55 -14 -4 -10 -1.73 5.70 -14 -4 -11 5.10 4.85 -14 -4 -12 -3.30 4.36 -14 -4 -13 0.61 4.07 -14 -4 -14 -2.94 3.96 -14 -5 3 14.04 7.73 -14 -5 2 10.65 4.33 -14 -5 1 15.78 7.34 -14 -5 0 13.55 6.30 -14 -5 -1 1.21 3.07 -14 -5 -2 34.22 10.70 -14 -5 -3 126.14 20.21 -14 -5 -4 -4.52 5.38 -14 -5 -5 66.49 14.25 -14 -5 -6 7.09 6.14 -14 -5 -7 13.32 6.73 -14 -5 -8 -2.00 4.34 -14 -5 -9 4.43 3.50 -14 -5 -10 12.89 6.76 -14 -5 -11 6.88 5.08 -14 -5 -12 50.86 13.20 -14 -5 -13 -3.23 5.27 -14 -5 -14 9.38 7.00 -14 -6 3 11.71 6.68 -14 -6 2 0.34 3.64 -14 -6 1 54.46 13.11 -14 -6 0 0.95 2.70 -14 -6 -1 2.81 4.63 -14 -6 -2 55.15 12.95 -14 -6 -3 5.29 4.37 -14 -6 -4 28.15 8.79 -14 -6 -5 5.05 4.98 -14 -6 -6 37.22 11.36 -14 -6 -7 44.16 12.07 -14 -6 -8 100.74 17.26 -14 -6 -9 4.56 4.62 -14 -6 -10 22.69 8.37 -14 -6 -11 5.96 5.66 -14 -6 -12 2.87 4.07 -14 -6 -13 3.34 4.43 -14 -6 -14 -4.42 4.02 -14 -6 -15 32.00 9.86 -14 -7 3 62.46 13.85 -14 -7 2 5.69 5.81 -14 -7 1 41.16 11.19 -14 -7 0 3.42 5.54 -14 -7 -1 6.76 5.12 -14 -7 -2 58.98 13.51 -14 -7 -3 38.36 10.34 -14 -7 -4 6.98 5.61 -14 -7 -5 4.74 4.05 -14 -7 -6 1.18 3.53 -14 -7 -7 8.55 6.07 -14 -7 -8 6.07 5.49 -14 -7 -9 1.65 5.64 -14 -7 -10 13.77 7.67 -14 -7 -11 4.23 5.00 -14 -7 -12 1.98 3.82 -14 -7 -13 10.20 7.87 -14 -7 -14 5.85 5.73 -14 -7 -15 17.30 8.07 -14 -8 3 56.36 12.21 -14 -8 2 74.98 14.63 -14 -8 1 77.53 15.13 -14 -8 0 33.89 10.80 -14 -8 -1 6.50 5.88 -14 -8 -2 16.63 7.80 -14 -8 -3 46.53 12.01 -14 -8 -4 4.86 3.21 -14 -8 -5 3.42 3.69 -14 -8 -6 8.68 5.69 -14 -8 -7 88.22 16.33 -14 -8 -8 3.62 4.87 -14 -8 -9 17.37 8.30 -14 -8 -10 9.08 6.64 -14 -8 -11 11.57 7.37 -14 -8 -12 1.29 4.49 -14 -8 -13 4.36 4.06 -14 -8 -14 -11.95 8.60 -14 -8 -15 -10.44 7.19 -14 -9 2 1.13 3.08 -14 -9 1 4.00 2.89 -14 -9 0 81.05 15.34 -14 -9 -1 32.91 9.89 -14 -9 -2 31.95 8.61 -14 -9 -3 -8.75 7.51 -14 -9 -4 0.57 4.17 -14 -9 -5 -4.48 6.57 -14 -9 -6 21.14 6.92 -14 -9 -7 -3.97 5.40 -14 -9 -8 -9.90 8.03 -14 -9 -9 -13.24 8.21 -14 -9 -10 -5.51 5.96 -14 -9 -11 -9.38 7.20 -14 -9 -12 -10.71 6.84 -14 -9 -13 -7.31 6.18 -14 -9 -14 7.76 2.69 -14 -9 -15 -2.04 4.75 -14 -10 0 -5.08 6.11 -14 -10 -1 43.62 10.32 -14 -10 -2 10.11 5.08 -14 -10 -3 -1.28 5.07 -14 -10 -4 -3.78 4.43 -14 -10 -5 4.51 2.78 -14 -10 -6 15.64 6.77 -14 -10 -7 -7.94 6.92 -14 -10 -8 11.29 4.71 -14 -10 -9 -5.67 5.31 -14 -10 -10 30.02 8.62 -14 -10 -11 31.79 8.57 -14 -10 -12 -6.55 5.36 -15 -2 -3 3.96 3.39 -15 -2 -4 1.05 4.46 -15 -2 -5 25.33 9.60 -15 -2 -6 40.28 11.88 -15 -2 -7 -6.91 7.27 -15 -2 -8 -5.29 6.62 0 0 0 0.00 0.00 TITL BB_S3_3_Lt_Mo in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 11.833288 12.815064 17.179850 77.3166 74.1473 66.4933 ZERR 1.00 0.000582 0.000629 0.000819 0.0042 0.0042 0.0047 LATT 1 SFAC C H N O Br UNIT 110.00 66.00 4.00 30.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 1149