#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 3 _journal_year 2020 _journal_page_first 255 _journal_page_last 260 #=============================================================================== data_20dab1_oa _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2.5(C6 Cl2 O4), 5(C7 H11 N2), 11(H2 O), C7 H10 N2' _chemical_formula_sum 'C57 H87 Cl5 N12 O21' _chemical_formula_weight 1453.64 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _space_group_IT_number '2' _symmetry_space_group_name_H-M 'P-1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3824(15) _cell_length_b 13.4515(17) _cell_length_c 19.048(2) _cell_angle_alpha 86.014(4) _cell_angle_beta 88.821(4) _cell_angle_gamma 86.367(4) _cell_volume 3413.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9943 _cell_measurement_theta_min 4.07 _cell_measurement_theta_max 28.16 _exptl_crystal_description 'Cuboid' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.252 _exptl_crystal_size_mid 0.173 _exptl_crystal_size_min 0.130 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 0.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7053 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59413 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.00 _reflns_number_total 16405 _reflns_number_gt 10907 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _computing_structure_refinement 'ShelXT (Sheldrick, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+1.6111P] 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 16405 _refine_ls_number_parameters 852 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1271 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1A Cl 0.71876(4) 0.03923(4) 0.28363(3) 0.02468(13) Uani 1 1 d . . . Cl2A Cl 0.41734(4) 0.34222(5) 0.43327(3) 0.03511(16) Uani 1 1 d . . . O1A O 0.73407(10) 0.11447(11) 0.42696(7) 0.0209(3) Uani 1 1 d . . . O2A O 0.61023(11) 0.24600(12) 0.48755(8) 0.0240(4) Uani 1 1 d . . . O3A O 0.39574(10) 0.25678(11) 0.29381(7) 0.0221(3) Uani 1 1 d . . . O4A O 0.52804(10) 0.13631(11) 0.22943(7) 0.0209(3) Uani 1 1 d . . . C1A C 0.63639(14) 0.12229(15) 0.32518(11) 0.0165(4) Uani 1 1 d . . . C2A C 0.65833(14) 0.14795(15) 0.39207(10) 0.0157(4) Uani 1 1 d . . . C3A C 0.58612(14) 0.22334(16) 0.42814(11) 0.0166(4) Uani 1 1 d . . . C4A C 0.49984(15) 0.25939(16) 0.39225(11) 0.0182(4) Uani 1 1 d . . . C5A C 0.47460(14) 0.22945(15) 0.32604(11) 0.0165(4) Uani 1 1 d . . . C6A C 0.54925(14) 0.15839(15) 0.28934(10) 0.0156(4) Uani 1 1 d . . . Cl3A Cl 0.91767(4) 0.42230(4) 0.10032(3) 0.02120(12) Uani 1 1 d . . . Cl4A Cl 0.65551(4) 0.77169(4) 0.23509(3) 0.02278(13) Uani 1 1 d . . . O5A O 0.94244(11) 0.50755(11) 0.24145(8) 0.0230(3) Uani 1 1 d . . . O6A O 0.83101(11) 0.65346(12) 0.29567(8) 0.0244(4) Uani 1 1 d . . . O7A O 0.62091(10) 0.67722(11) 0.10012(8) 0.0229(3) Uani 1 1 d . . . O8A O 0.73384(11) 0.53253(12) 0.04366(8) 0.0247(4) Uani 1 1 d . . . C7A C 0.84439(14) 0.51603(15) 0.13893(11) 0.0166(4) Uani 1 1 d . . . C8A C 0.87029(14) 0.54376(15) 0.20514(11) 0.0167(4) Uani 1 1 d . . . C9A C 0.80542(14) 0.62866(15) 0.23667(10) 0.0163(4) Uani 1 1 d . . . C10A C 0.72330(14) 0.67279(15) 0.19915(11) 0.0167(4) Uani 1 1 d . . . C11A C 0.69493(14) 0.64147(15) 0.13479(11) 0.0163(4) Uani 1 1 d . . . C12A C 0.75977(14) 0.55736(15) 0.10178(11) 0.0165(4) Uani 1 1 d . . . Cl5A Cl 0.15637(4) 0.86280(4) -0.08237(3) 0.02272(13) Uani 1 1 d . . . O9A O 0.17548(10) 0.93908(11) 0.06182(7) 0.0207(3) Uani 1 1 d . . . O10A O -0.04017(10) 0.95052(11) -0.13061(7) 0.0220(3) Uani 1 1 d . . . C13A C 0.09507(14) 0.96321(15) 0.03090(10) 0.0144(4) Uani 1 1 d . . . C14A C 0.07037(14) 0.93618(15) -0.03604(10) 0.0157(4) Uani 1 1 d . . . C15A C -0.01831(14) 0.97012(15) -0.06984(10) 0.0145(4) Uani 1 1 d . . . O11W O 0.36440(6) 0.88433(6) 0.00399(4) 0.0300(4) Uani 1 1 d G . . H11C H 0.3067 0.8952 0.0223 0.045 Uiso 1 1 d G . . H11D H 0.4085 0.8833 0.0356 0.045 Uiso 1 1 d G . . O7W O 1.06847(4) 0.33790(4) 0.23090(2) 0.0272(4) Uani 1 1 d G . . H7WA H 1.1077 0.3351 0.2657 0.041 Uiso 1 1 d G . . H7WB H 1.0290 0.3899 0.2320 0.041 Uiso 1 1 d G . . O5W O 0.93541(4) 0.10944(3) 0.37618(3) 0.0292(4) Uani 1 1 d G . . H5WA H 0.8732 0.1110 0.3866 0.044 Uiso 1 1 d G . . H5WB H 0.9431 0.1244 0.3324 0.044 Uiso 1 1 d G . . O4W O 1.10773(4) 0.17879(4) 0.43012(3) 0.0315(4) Uani 1 1 d G . . H4WA H 1.1291 0.1516 0.4691 0.047 Uiso 1 1 d G . . H4WB H 1.0551 0.1518 0.4191 0.047 Uiso 1 1 d G . . O1 O 0.49598(5) 0.85265(5) 0.11102(4) 0.0283(4) Uani 1 1 d G . . H1A H 0.5325 0.9022 0.1090 0.042 Uiso 1 1 d G . . H1B H 0.5329 0.7989 0.1102 0.042 Uiso 1 1 d G . . O6W O 0.95789(5) 0.17362(4) 0.23925(3) 0.0322(4) Uani 1 1 d G . . H6WA H 0.9619 0.1427 0.2017 0.048 Uiso 1 1 d G . . H6WB H 0.9899 0.2263 0.2335 0.048 Uiso 1 1 d G . . O1W O 1.47742(4) 0.34334(6) 0.59838(4) 0.0378(5) Uani 1 1 d G . . H1WA H 1.5147 0.3681 0.6273 0.057 Uiso 1 1 d G . . H1WB H 1.5114 0.3298 0.5617 0.057 Uiso 1 1 d G . . O8W O 1.19921(3) 0.31945(4) 0.34143(3) 0.0270(4) Uani 1 1 d G . . H8WA H 1.1759 0.2763 0.3710 0.041 Uiso 1 1 d G . . H8WB H 1.2604 0.3034 0.3327 0.041 Uiso 1 1 d G . . O2W O 1.28492(4) 0.26071(5) 0.59489(3) 0.0286(4) Uani 1 1 d G . . H2WA H 1.2559 0.2771 0.6328 0.043 Uiso 1 1 d G . . H2WB H 1.3436 0.2816 0.5929 0.043 Uiso 1 1 d G . . O3W O 1.19515(4) 0.09874(4) 0.55279(3) 0.0338(4) Uani 1 1 d G . . H3WA H 1.2154 0.0427 0.5726 0.051 Uiso 1 1 d G . . H3WB H 1.2285 0.1445 0.5678 0.051 Uiso 1 1 d G . . O10W O 0.60535(6) 1.01240(4) 0.12114(4) 0.0335(4) Uani 1 1 d G . . H10A H 0.5998 1.0460 0.1574 0.050 Uiso 1 1 d G . . H10B H 0.6112 1.0519 0.0847 0.050 Uiso 1 1 d G . . N1B N 0.97670(5) 0.17133(6) 0.72553(3) 0.0227(4) Uani 1 1 d G . . N2B N 0.78685(4) 0.17494(5) 0.55780(3) 0.0221(4) Uani 1 1 d G . . C1B C 1.07181(5) 0.11072(6) 0.72900(3) 0.0273(5) Uani 1 1 d G . . H1BA H 1.0613 0.0471 0.7532 0.041 Uiso 1 1 calc R . . H1BB H 1.1197 0.1444 0.7539 0.041 Uiso 1 1 calc R . . H1BC H 1.0966 0.1010 0.6822 0.041 Uiso 1 1 calc R . . C2B C 0.95095(18) 0.2294(2) 0.78558(12) 0.0347(6) Uani 1 1 d . . . H2BA H 0.9368 0.2980 0.7697 0.052 Uiso 1 1 calc R . . H2BB H 1.0061 0.2244 0.8174 0.052 Uiso 1 1 calc R . . H2BC H 0.8929 0.2040 0.8094 0.052 Uiso 1 1 calc R . . C3B C 0.76231(15) 0.22981(17) 0.61250(11) 0.0218(5) Uani 1 1 d . . . H3B H 0.7022 0.2686 0.6118 0.026 Uiso 1 1 calc R . . C4B C 0.82284(15) 0.23022(16) 0.66883(11) 0.0201(5) Uani 1 1 d . . . H4B H 0.8040 0.2689 0.7061 0.024 Uiso 1 1 calc R . . C5B C 0.91510(15) 0.17148(16) 0.67089(11) 0.0168(4) Uani 1 1 d . . . C6B C 0.93813(15) 0.11383(16) 0.61233(11) 0.0199(5) Uani 1 1 d . . . H6BA H 0.9973 0.0738 0.6111 0.024 Uiso 1 1 calc R . . C7B C 0.87347(16) 0.11751(17) 0.55826(11) 0.0221(5) Uani 1 1 d . . . H7B H 0.8892 0.0793 0.5202 0.026 Uiso 1 1 calc R . . N9B N 1.60829(13) 0.39516(15) 0.70769(10) 0.0255(4) Uani 1 1 d . . . N10B N 1.79004(13) 0.39251(13) 0.88547(9) 0.0195(4) Uani 1 1 d . . . C29B C 1.78355(17) 0.31622(17) 0.94251(11) 0.0249(5) Uani 1 1 d . . . H29A H 1.7148 0.3110 0.9569 0.037 Uiso 1 1 calc R . . H29B H 1.8215 0.3337 0.9816 0.037 Uiso 1 1 calc R . . H29C H 1.8101 0.2533 0.9270 0.037 Uiso 1 1 calc R . . C30B C 1.86789(16) 0.46193(17) 0.88885(12) 0.0249(5) Uani 1 1 d . . . H30A H 1.9220 0.4438 0.8574 0.037 Uiso 1 1 calc R . . H30B H 1.8921 0.4597 0.9361 0.037 Uiso 1 1 calc R . . H30C H 1.8412 0.5283 0.8753 0.037 Uiso 1 1 calc R . . C31B C 1.67811(15) 0.46115(17) 0.71346(12) 0.0234(5) Uani 1 1 d . . . H31B H 1.6846 0.5095 0.6766 0.028 Uiso 1 1 calc R . . C32B C 1.74107(15) 0.46311(16) 0.76964(11) 0.0193(4) Uani 1 1 d . . . H32B H 1.7884 0.5109 0.7696 0.023 Uiso 1 1 calc R . . C33B C 1.73304(14) 0.39204(15) 0.82705(11) 0.0166(4) Uani 1 1 d . . . C34B C 1.66031(15) 0.32204(16) 0.82140(11) 0.0201(5) Uani 1 1 d . . . H34B H 1.6517 0.2725 0.8572 0.024 Uiso 1 1 calc R . . C35B C 1.60196(16) 0.32760(17) 0.76225(12) 0.0249(5) Uani 1 1 d . . . H35B H 1.5543 0.2805 0.7601 0.030 Uiso 1 1 calc R . . N7B N 0.56190(13) 0.61019(14) -0.02896(10) 0.0209(4) Uani 1 1 d . . . N8B N 0.37270(13) 0.62613(14) -0.19777(9) 0.0218(4) Uani 1 1 d . . . C22B C 0.39351(18) 0.56486(19) -0.25705(12) 0.0278(5) Uani 1 1 d . . . H22A H 0.4579 0.5786 -0.2772 0.042 Uiso 1 1 calc R . . H22B H 0.3430 0.5800 -0.2919 0.042 Uiso 1 1 calc R . . H22C H 0.3934 0.4956 -0.2411 0.042 Uiso 1 1 calc R . . C23B C 0.28273(16) 0.69357(18) -0.19932(12) 0.0273(5) Uani 1 1 d . . . H23A H 0.2436 0.6809 -0.1572 0.041 Uiso 1 1 calc R . . H23B H 0.2439 0.6827 -0.2396 0.041 Uiso 1 1 calc R . . H23C H 0.3016 0.7614 -0.2022 0.041 Uiso 1 1 calc R . . C24B C 0.58063(16) 0.55017(17) -0.08167(11) 0.0225(5) Uani 1 1 d . . . H24B H 0.6366 0.5054 -0.0794 0.027 Uiso 1 1 calc R . . C25B C 0.52011(15) 0.55299(17) -0.13821(11) 0.0211(5) Uani 1 1 d . . . H25B H 0.5349 0.5105 -0.1740 0.025 Uiso 1 1 calc R . . C26B C 0.43436(14) 0.62064(16) -0.14276(11) 0.0178(4) Uani 1 1 d . . . C27B C 0.41716(15) 0.68248(16) -0.08593(11) 0.0209(5) Uani 1 1 d . . . H27B H 0.3619 0.7280 -0.0861 0.025 Uiso 1 1 calc R . . C28B C 0.48150(15) 0.67537(17) -0.03115(11) 0.0215(5) Uani 1 1 d . . . H28B H 0.4695 0.7166 0.0057 0.026 Uiso 1 1 calc R . . N3B N 0.35541(13) 0.19654(14) 0.15431(10) 0.0226(4) Uani 1 1 d . . . N4B N 0.16624(13) 0.20346(14) -0.01375(9) 0.0214(4) Uani 1 1 d . . . C8B C 0.07459(16) 0.26879(18) -0.01544(13) 0.0281(5) Uani 1 1 d . . . H8BA H 0.0309 0.2483 0.0227 0.042 Uiso 1 1 calc R . . H8BB H 0.0416 0.2645 -0.0593 0.042 Uiso 1 1 calc R . . H8BC H 0.0911 0.3364 -0.0108 0.042 Uiso 1 1 calc R . . C9B C 0.19274(18) 0.14786(18) -0.07519(12) 0.0293(5) Uani 1 1 d . . . H9BA H 0.2454 0.1794 -0.1015 0.044 Uiso 1 1 calc R . . H9BB H 0.1352 0.1469 -0.1043 0.044 Uiso 1 1 calc R . . H9BC H 0.2151 0.0807 -0.0602 0.044 Uiso 1 1 calc R . . C10B C 0.22755(15) 0.20064(15) 0.04148(11) 0.0172(4) Uani 1 1 d . . . C11B C 0.20201(15) 0.25263(16) 0.10184(11) 0.0195(5) Uani 1 1 d . . . H11A H 0.1409 0.2893 0.1044 0.023 Uiso 1 1 calc R . . C12B C 0.26659(16) 0.24910(16) 0.15618(12) 0.0222(5) Uani 1 1 d . . . H12B H 0.2490 0.2838 0.1956 0.027 Uiso 1 1 calc R . . C13B C 0.38154(16) 0.14463(17) 0.09843(12) 0.0228(5) Uani 1 1 d . . . H13B H 0.4428 0.1078 0.0982 0.027 Uiso 1 1 calc R . . C14B C 0.32100(15) 0.14443(16) 0.04219(11) 0.0199(5) Uani 1 1 d . . . H14B H 0.3407 0.1075 0.0042 0.024 Uiso 1 1 calc R . . N5B N 1.18349(14) 0.57999(14) 0.54309(10) 0.0273(4) Uani 1 1 d . . . N6B N 0.98992(14) 0.58622(15) 0.37764(10) 0.0250(4) Uani 1 1 d . . . C15B C 1.27788(19) 0.5178(2) 0.54321(16) 0.0447(7) Uani 1 1 d . . . H15A H 1.2635 0.4486 0.5447 0.067 Uiso 1 1 calc R . . H15B H 1.3158 0.5296 0.5838 0.067 Uiso 1 1 calc R . . H15C H 1.3160 0.5346 0.5013 0.067 Uiso 1 1 calc R . . C16B C 1.1637(2) 0.6390(2) 0.60330(13) 0.0373(6) Uani 1 1 d . . . H16A H 1.1231 0.6981 0.5892 0.056 Uiso 1 1 calc R . . H16B H 1.2259 0.6575 0.6213 0.056 Uiso 1 1 calc R . . H16C H 1.1291 0.6004 0.6393 0.056 Uiso 1 1 calc R . . C17B C 0.96865(16) 0.64438(17) 0.43101(12) 0.0253(5) Uani 1 1 d . . . H17B H 0.9105 0.6861 0.4298 0.030 Uiso 1 1 calc R . . C18B C 1.03017(15) 0.64372(16) 0.48671(12) 0.0216(5) Uani 1 1 d . . . H18B H 1.0135 0.6845 0.5232 0.026 Uiso 1 1 calc R . . C19B C 1.11975(15) 0.58148(16) 0.48980(11) 0.0182(4) Uani 1 1 d . . . C20B C 1.13853(16) 0.52061(16) 0.43279(11) 0.0215(5) Uani 1 1 d . . . H20B H 1.1955 0.4773 0.4324 0.026 Uiso 1 1 calc R . . C21B C 1.07355(16) 0.52507(17) 0.37851(11) 0.0232(5) Uani 1 1 d . . . H21B H 1.0872 0.4850 0.3412 0.028 Uiso 1 1 calc R . . N11B N -0.21590(13) 0.99966(14) -0.20162(10) 0.0216(4) Uani 1 1 d . . . N12B N -0.41023(13) 1.01433(14) -0.36717(9) 0.0227(4) Uani 1 1 d . . . C36B C -0.38351(19) 0.9687(2) -0.43246(12) 0.0318(6) Uani 1 1 d . . . H36A H -0.3428 1.0120 -0.4612 0.048 Uiso 1 1 calc R . . H36B H -0.4433 0.9579 -0.4571 0.048 Uiso 1 1 calc R . . H36C H -0.3468 0.9059 -0.4221 0.048 Uiso 1 1 calc R . . C37B C -0.50022(17) 1.08224(19) -0.36744(14) 0.0344(6) Uani 1 1 d . . . H37A H -0.5407 1.0664 -0.3265 0.052 Uiso 1 1 calc R . . H37B H -0.5378 1.0751 -0.4090 0.052 Uiso 1 1 calc R . . H37C H -0.4812 1.1498 -0.3670 0.052 Uiso 1 1 calc R . . C38B C -0.19006(15) 0.95246(16) -0.25956(12) 0.0216(5) Uani 1 1 d . . . H38B H -0.1280 0.9175 -0.2618 0.026 Uiso 1 1 calc R . . C39B C -0.25251(15) 0.95453(16) -0.31522(11) 0.0184(4) Uani 1 1 d . . . H39B H -0.2331 0.9209 -0.3548 0.022 Uiso 1 1 calc R . . C40B C -0.34724(14) 1.00799(15) -0.31292(11) 0.0160(4) Uani 1 1 d . . . C41B C -0.37174(15) 1.05479(16) -0.24995(11) 0.0194(4) Uani 1 1 d . . . H41B H -0.4336 1.0895 -0.2451 0.023 Uiso 1 1 calc R . . C42B C -0.30545(16) 1.04937(16) -0.19649(11) 0.0216(5) Uani 1 1 d . . . H42B H -0.3226 1.0808 -0.1556 0.026 Uiso 1 1 calc R . . H2B H 0.743(2) 0.182(2) 0.5195(16) 0.067(10) Uiso 1 1 d . . . H7BA H 0.603(2) 0.607(2) 0.0103(15) 0.051(9) Uiso 1 1 d . . . H3BA H 0.398(2) 0.193(2) 0.1917(18) 0.075(11) Uiso 1 1 d . . . H6B H 0.948(2) 0.589(2) 0.3448(14) 0.042(8) Uiso 1 1 d . . . H11B H -0.176(2) 0.996(2) -0.1648(16) 0.056(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1A 0.0195(2) 0.0323(3) 0.0222(3) -0.0113(2) -0.0033(2) 0.0104(2) Cl2A 0.0315(3) 0.0500(4) 0.0229(3) -0.0183(3) -0.0102(2) 0.0249(3) O1A 0.0168(7) 0.0278(9) 0.0180(8) -0.0050(6) -0.0063(6) 0.0048(6) O2A 0.0227(8) 0.0325(9) 0.0172(8) -0.0098(7) -0.0088(6) 0.0072(7) O3A 0.0163(7) 0.0314(9) 0.0184(8) -0.0066(7) -0.0054(6) 0.0065(6) O4A 0.0185(7) 0.0277(9) 0.0171(8) -0.0086(6) -0.0044(6) 0.0032(6) C1A 0.0138(9) 0.0186(11) 0.0170(11) -0.0041(9) -0.0004(8) 0.0037(8) C2A 0.0134(9) 0.0184(11) 0.0155(10) -0.0008(8) -0.0009(8) -0.0016(8) C3A 0.0165(10) 0.0183(11) 0.0151(10) -0.0033(8) -0.0006(8) 0.0001(8) C4A 0.0167(10) 0.0207(12) 0.0170(11) -0.0054(9) 0.0002(8) 0.0052(8) C5A 0.0148(9) 0.0187(11) 0.0158(10) 0.0000(8) -0.0020(8) -0.0001(8) C6A 0.0152(9) 0.0165(11) 0.0154(10) -0.0030(8) -0.0012(8) -0.0017(8) Cl3A 0.0180(2) 0.0237(3) 0.0225(3) -0.0101(2) -0.0019(2) 0.0038(2) Cl4A 0.0202(2) 0.0268(3) 0.0213(3) -0.0096(2) -0.0043(2) 0.0095(2) O5A 0.0211(7) 0.0272(9) 0.0206(8) -0.0070(7) -0.0071(6) 0.0081(6) O6A 0.0212(8) 0.0323(9) 0.0200(8) -0.0106(7) -0.0058(6) 0.0087(7) O7A 0.0196(7) 0.0254(9) 0.0241(8) -0.0079(7) -0.0083(6) 0.0057(6) O8A 0.0237(8) 0.0301(9) 0.0208(8) -0.0105(7) -0.0075(6) 0.0054(7) C7A 0.0153(9) 0.0163(11) 0.0184(11) -0.0050(8) -0.0001(8) 0.0010(8) C8A 0.0166(10) 0.0170(11) 0.0165(11) -0.0022(8) -0.0004(8) 0.0001(8) C9A 0.0161(10) 0.0181(11) 0.0148(10) -0.0030(8) -0.0001(8) -0.0010(8) C10A 0.0151(9) 0.0170(11) 0.0179(11) -0.0034(9) 0.0000(8) 0.0016(8) C11A 0.0152(9) 0.0165(11) 0.0172(11) -0.0013(8) -0.0022(8) -0.0001(8) C12A 0.0166(10) 0.0171(11) 0.0163(11) -0.0029(8) -0.0010(8) -0.0025(8) Cl5A 0.0175(2) 0.0303(3) 0.0207(3) -0.0125(2) -0.0031(2) 0.0082(2) O9A 0.0162(7) 0.0273(9) 0.0185(8) -0.0066(6) -0.0056(6) 0.0061(6) O10A 0.0198(7) 0.0312(9) 0.0156(8) -0.0101(7) -0.0047(6) 0.0048(6) C13A 0.0134(9) 0.0143(10) 0.0156(10) -0.0023(8) -0.0024(8) 0.0000(8) C14A 0.0146(9) 0.0171(11) 0.0159(10) -0.0075(8) 0.0004(8) 0.0014(8) C15A 0.0143(9) 0.0158(11) 0.0139(10) -0.0044(8) -0.0003(8) -0.0021(8) O11W 0.0170(7) 0.0371(10) 0.0363(10) -0.0106(8) -0.0029(7) 0.0050(7) O7W 0.0249(8) 0.0264(9) 0.0293(9) -0.0029(7) -0.0054(7) 0.0096(7) O5W 0.0181(8) 0.0415(11) 0.0274(9) 0.0005(8) -0.0005(7) 0.0000(7) O4W 0.0322(9) 0.0381(10) 0.0246(9) -0.0032(8) -0.0032(7) -0.0035(8) O1 0.0245(8) 0.0263(9) 0.0328(9) -0.0017(7) 0.0002(7) 0.0075(7) O6W 0.0382(10) 0.0359(10) 0.0241(9) -0.0109(8) 0.0022(7) -0.0067(8) O1W 0.0289(9) 0.0634(13) 0.0237(9) -0.0143(9) -0.0016(7) -0.0105(9) O8W 0.0182(7) 0.0289(9) 0.0333(9) -0.0038(7) -0.0012(7) 0.0060(7) O2W 0.0269(8) 0.0373(10) 0.0224(9) -0.0101(7) 0.0016(7) -0.0008(7) O3W 0.0362(9) 0.0285(10) 0.0368(10) -0.0012(8) -0.0134(8) 0.0013(8) O10W 0.0340(9) 0.0407(11) 0.0267(9) -0.0134(8) -0.0010(7) 0.0035(8) N1B 0.0187(9) 0.0309(11) 0.0184(10) -0.0090(8) -0.0057(7) 0.0080(8) N2B 0.0209(9) 0.0269(11) 0.0189(10) -0.0005(8) -0.0070(8) -0.0034(8) C1B 0.0197(11) 0.0344(14) 0.0273(13) -0.0080(11) -0.0078(9) 0.0096(10) C2B 0.0304(13) 0.0506(17) 0.0238(13) -0.0182(12) -0.0093(10) 0.0122(12) C3B 0.0174(10) 0.0232(12) 0.0245(12) -0.0011(10) -0.0034(9) 0.0023(9) C4B 0.0169(10) 0.0219(12) 0.0215(11) -0.0055(9) -0.0011(8) 0.0029(9) C5B 0.0159(10) 0.0189(11) 0.0156(10) -0.0010(8) -0.0006(8) -0.0021(8) C6B 0.0189(10) 0.0202(12) 0.0204(11) -0.0045(9) -0.0008(8) 0.0040(9) C7B 0.0257(11) 0.0248(12) 0.0162(11) -0.0061(9) -0.0013(9) -0.0005(9) N9B 0.0217(9) 0.0321(12) 0.0234(10) -0.0110(9) -0.0033(8) 0.0046(8) N10B 0.0205(9) 0.0210(10) 0.0174(9) -0.0011(8) -0.0020(7) -0.0044(7) C29B 0.0296(12) 0.0245(13) 0.0206(12) 0.0001(10) 0.0003(9) -0.0016(10) C30B 0.0229(11) 0.0268(13) 0.0260(12) -0.0044(10) -0.0034(9) -0.0052(9) C31B 0.0220(11) 0.0278(13) 0.0197(12) -0.0019(10) 0.0021(9) 0.0043(9) C32B 0.0172(10) 0.0193(11) 0.0216(11) -0.0029(9) 0.0018(8) -0.0007(8) C33B 0.0152(10) 0.0151(11) 0.0195(11) -0.0064(9) 0.0032(8) 0.0035(8) C34B 0.0194(10) 0.0189(11) 0.0222(11) -0.0039(9) 0.0029(9) -0.0007(9) C35B 0.0190(11) 0.0240(13) 0.0331(13) -0.0130(10) 0.0004(9) -0.0014(9) N7B 0.0184(9) 0.0246(11) 0.0201(10) -0.0040(8) -0.0039(8) -0.0003(8) N8B 0.0179(9) 0.0282(11) 0.0195(10) -0.0066(8) -0.0041(7) 0.0033(8) C22B 0.0308(12) 0.0353(14) 0.0183(12) -0.0055(10) -0.0035(9) -0.0045(10) C23B 0.0181(11) 0.0353(14) 0.0279(13) 0.0001(11) -0.0051(9) 0.0027(10) C24B 0.0196(10) 0.0247(12) 0.0228(12) -0.0064(10) -0.0010(9) 0.0057(9) C25B 0.0208(10) 0.0241(12) 0.0189(11) -0.0082(9) 0.0005(8) 0.0020(9) C26B 0.0148(10) 0.0207(12) 0.0182(11) -0.0034(9) -0.0003(8) -0.0019(8) C27B 0.0179(10) 0.0221(12) 0.0229(12) -0.0067(9) -0.0001(9) 0.0029(9) C28B 0.0221(11) 0.0225(12) 0.0208(11) -0.0083(9) 0.0003(9) -0.0009(9) N3B 0.0206(9) 0.0252(11) 0.0226(10) -0.0004(8) -0.0080(8) -0.0049(8) N4B 0.0203(9) 0.0258(11) 0.0185(9) -0.0052(8) -0.0053(7) 0.0025(8) C8B 0.0211(11) 0.0333(14) 0.0296(13) -0.0017(11) -0.0100(10) 0.0029(10) C9B 0.0381(13) 0.0333(14) 0.0185(12) -0.0086(10) 0.0000(10) -0.0108(11) C10B 0.0169(10) 0.0175(11) 0.0172(11) -0.0003(9) -0.0016(8) -0.0016(8) C11B 0.0192(10) 0.0190(11) 0.0205(11) -0.0055(9) -0.0012(8) 0.0026(8) C12B 0.0253(11) 0.0224(12) 0.0196(11) -0.0043(9) -0.0012(9) -0.0036(9) C13B 0.0160(10) 0.0215(12) 0.0303(13) 0.0015(10) -0.0023(9) 0.0016(9) C14B 0.0186(10) 0.0204(12) 0.0207(11) -0.0038(9) 0.0020(8) 0.0010(9) N5B 0.0314(10) 0.0258(11) 0.0251(11) -0.0071(9) -0.0122(8) 0.0047(8) N6B 0.0226(10) 0.0312(12) 0.0214(10) 0.0009(9) -0.0080(8) -0.0048(8) C15B 0.0387(15) 0.0415(17) 0.0538(18) -0.0088(14) -0.0258(13) 0.0123(13) C16B 0.0505(16) 0.0364(16) 0.0262(14) -0.0096(12) -0.0137(12) 0.0000(12) C17B 0.0186(11) 0.0273(13) 0.0290(13) 0.0014(10) -0.0008(9) 0.0017(9) C18B 0.0229(11) 0.0204(12) 0.0219(12) -0.0055(9) 0.0019(9) 0.0000(9) C19B 0.0196(10) 0.0163(11) 0.0187(11) -0.0005(9) -0.0006(8) -0.0019(8) C20B 0.0211(11) 0.0212(12) 0.0223(12) -0.0036(9) 0.0010(9) 0.0001(9) C21B 0.0265(11) 0.0255(13) 0.0182(11) -0.0048(9) 0.0007(9) -0.0037(10) N11B 0.0218(9) 0.0234(11) 0.0202(10) -0.0004(8) -0.0070(8) -0.0043(8) N12B 0.0200(9) 0.0302(11) 0.0181(10) -0.0034(8) -0.0043(7) 0.0010(8) C36B 0.0386(14) 0.0432(16) 0.0152(12) -0.0045(11) -0.0032(10) -0.0105(12) C37B 0.0246(12) 0.0349(15) 0.0430(16) 0.0011(12) -0.0159(11) 0.0037(11) C38B 0.0154(10) 0.0224(12) 0.0265(12) 0.0000(10) -0.0018(9) 0.0021(9) C39B 0.0176(10) 0.0200(11) 0.0179(11) -0.0059(9) 0.0012(8) 0.0007(8) C40B 0.0159(9) 0.0159(11) 0.0161(10) 0.0003(8) -0.0017(8) -0.0020(8) C41B 0.0189(10) 0.0196(12) 0.0195(11) -0.0032(9) 0.0005(8) 0.0024(9) C42B 0.0272(11) 0.0212(12) 0.0171(11) -0.0056(9) 0.0007(9) -0.0029(9) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cl1A C1A 1.738(2) . ? Cl2A C4A 1.732(2) . ? O1A C2A 1.265(2) . ? O2A C3A 1.246(2) . ? O3A C5A 1.254(2) . ? O4A C6A 1.242(2) . ? C1A C2A 1.385(3) . ? C1A C6A 1.406(3) . ? C2A C3A 1.543(3) . ? C3A C4A 1.397(3) . ? C4A C5A 1.404(3) . ? C5A C6A 1.531(3) . ? Cl3A C7A 1.742(2) . ? Cl4A C10A 1.735(2) . ? O5A C8A 1.253(2) . ? O6A C9A 1.255(2) . ? O7A C11A 1.253(2) . ? O8A C12A 1.241(2) . ? C7A C8A 1.396(3) . ? C7A C12A 1.411(3) . ? C8A C9A 1.538(3) . ? C9A C10A 1.400(3) . ? C10A C11A 1.391(3) . ? C11A C12A 1.543(3) . ? Cl5A C14A 1.736(2) . ? O9A C13A 1.251(2) . ? O10A C15A 1.249(2) . ? C13A C14A 1.401(3) . ? C13A C15A 1.534(3) 2_575 ? C14A C15A 1.398(3) . ? C15A C13A 1.534(3) 2_575 ? O11W H11C 0.8501 . ? O11W H11D 0.8498 . ? O7W H7WA 0.8512 . ? O7W H7WB 0.8503 . ? O5W H5WA 0.8513 . ? O5W H5WB 0.8503 . ? O4W H4WA 0.8513 . ? O4W H4WB 0.8488 . ? O1 H1A 0.8496 . ? O1 H1B 0.8507 . ? O6W H6WA 0.8507 . ? O6W H6WB 0.8497 . ? O1W H1WA 0.8499 . ? O1W H1WB 0.8503 . ? O8W H8WA 0.8501 . ? O8W H8WB 0.8496 . ? O2W H2WA 0.8496 . ? O2W H2WB 0.8502 . ? O3W H3WA 0.8498 . ? O3W H3WB 0.8500 . ? O10W H10A 0.8503 . ? O10W H10B 0.8499 . ? N1B C5B 1.341(2) . ? N1B C2B 1.453(2) . ? N1B C1B 1.4675 . ? N2B C3B 1.342(2) . ? N2B C7B 1.352(2) . ? N2B H2B 0.94(3) . ? C1B H1BA 0.9600 . ? C1B H1BB 0.9600 . ? C1B H1BC 0.9600 . ? C2B H2BA 0.9600 . ? C2B H2BB 0.9600 . ? C2B H2BC 0.9600 . ? C3B C4B 1.358(3) . ? C3B H3B 0.9300 . ? C4B C5B 1.423(3) . ? C4B H4B 0.9300 . ? C5B C6B 1.420(3) . ? C6B C7B 1.355(3) . ? C6B H6BA 0.9300 . ? C7B H7B 0.9300 . ? N9B C35B 1.337(3) . ? N9B C31B 1.340(3) . ? N10B C33B 1.363(3) . ? N10B C29B 1.447(3) . ? N10B C30B 1.448(3) . ? C29B H29A 0.9600 . ? C29B H29B 0.9600 . ? C29B H29C 0.9600 . ? C30B H30A 0.9600 . ? C30B H30B 0.9600 . ? C30B H30C 0.9600 . ? C31B C32B 1.378(3) . ? C31B H31B 0.9300 . ? C32B C33B 1.409(3) . ? C32B H32B 0.9300 . ? C33B C34B 1.407(3) . ? C34B C35B 1.379(3) . ? C34B H34B 0.9300 . ? C35B H35B 0.9300 . ? N7B C24B 1.341(3) . ? N7B C28B 1.344(3) . ? N7B H7BA 0.94(3) . ? N8B C26B 1.342(3) . ? N8B C22B 1.456(3) . ? N8B C23B 1.460(3) . ? C22B H22A 0.9600 . ? C22B H22B 0.9600 . ? C22B H22C 0.9600 . ? C23B H23A 0.9600 . ? C23B H23B 0.9600 . ? C23B H23C 0.9600 . ? C24B C25B 1.358(3) . ? C24B H24B 0.9300 . ? C25B C26B 1.419(3) . ? C25B H25B 0.9300 . ? C26B C27B 1.417(3) . ? C27B C28B 1.361(3) . ? C27B H27B 0.9300 . ? C28B H28B 0.9300 . ? N3B C13B 1.342(3) . ? N3B C12B 1.345(3) . ? N3B H3BA 0.92(3) . ? N4B C10B 1.344(2) . ? N4B C9B 1.458(3) . ? N4B C8B 1.462(3) . ? C8B H8BA 0.9600 . ? C8B H8BB 0.9600 . ? C8B H8BC 0.9600 . ? C9B H9BA 0.9600 . ? C9B H9BB 0.9600 . ? C9B H9BC 0.9600 . ? C10B C11B 1.412(3) . ? C10B C14B 1.420(3) . ? C11B C12B 1.358(3) . ? C11B H11A 0.9300 . ? C12B H12B 0.9300 . ? C13B C14B 1.357(3) . ? C13B H13B 0.9300 . ? C14B H14B 0.9300 . ? N5B C19B 1.337(3) . ? N5B C16B 1.450(3) . ? N5B C15B 1.470(3) . ? N6B C17B 1.341(3) . ? N6B C21B 1.346(3) . ? N6B H6B 0.85(3) . ? C15B H15A 0.9600 . ? C15B H15B 0.9600 . ? C15B H15C 0.9600 . ? C16B H16A 0.9600 . ? C16B H16B 0.9600 . ? C16B H16C 0.9600 . ? C17B C18B 1.355(3) . ? C17B H17B 0.9300 . ? C18B C19B 1.418(3) . ? C18B H18B 0.9300 . ? C19B C20B 1.414(3) . ? C20B C21B 1.360(3) . ? C20B H20B 0.9300 . ? C21B H21B 0.9300 . ? N11B C38B 1.340(3) . ? N11B C42B 1.340(3) . ? N11B H11B 0.89(3) . ? N12B C40B 1.342(2) . ? N12B C36B 1.453(3) . ? N12B C37B 1.465(3) . ? C36B H36A 0.9600 . ? C36B H36B 0.9600 . ? C36B H36C 0.9600 . ? C37B H37A 0.9600 . ? C37B H37B 0.9600 . ? C37B H37C 0.9600 . ? C38B C39B 1.361(3) . ? C38B H38B 0.9300 . ? C39B C40B 1.419(3) . ? C39B H39B 0.9300 . ? C40B C41B 1.416(3) . ? C41B C42B 1.359(3) . ? C41B H41B 0.9300 . ? C42B H42B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2A C1A C6A 123.30(18) . . ? C2A C1A Cl1A 118.83(15) . . ? C6A C1A Cl1A 117.85(15) . . ? O1A C2A C1A 125.18(19) . . ? O1A C2A C3A 116.17(17) . . ? C1A C2A C3A 118.65(17) . . ? O2A C3A C4A 125.82(19) . . ? O2A C3A C2A 116.35(17) . . ? C4A C3A C2A 117.84(17) . . ? C3A C4A C5A 123.66(19) . . ? C3A C4A Cl2A 118.00(16) . . ? C5A C4A Cl2A 118.30(15) . . ? O3A C5A C4A 125.33(19) . . ? O3A C5A C6A 116.75(17) . . ? C4A C5A C6A 117.91(17) . . ? O4A C6A C1A 124.38(19) . . ? O4A C6A C5A 117.14(17) . . ? C1A C6A C5A 118.47(17) . . ? C8A C7A C12A 123.81(19) . . ? C8A C7A Cl3A 118.80(15) . . ? C12A C7A Cl3A 117.36(15) . . ? O5A C8A C7A 126.59(19) . . ? O5A C8A C9A 116.12(17) . . ? C7A C8A C9A 117.28(17) . . ? O6A C9A C10A 124.39(19) . . ? O6A C9A C8A 116.20(17) . . ? C10A C9A C8A 119.41(17) . . ? C11A C10A C9A 123.02(19) . . ? C11A C10A Cl4A 119.24(15) . . ? C9A C10A Cl4A 117.74(15) . . ? O7A C11A C10A 125.24(19) . . ? O7A C11A C12A 116.37(17) . . ? C10A C11A C12A 118.37(17) . . ? O8A C12A C7A 125.11(19) . . ? O8A C12A C11A 116.89(17) . . ? C7A C12A C11A 117.99(17) . . ? O9A C13A C14A 125.77(18) . . ? O9A C13A C15A 116.39(17) . 2_575 ? C14A C13A C15A 117.83(16) . 2_575 ? C15A C14A C13A 123.34(18) . . ? C15A C14A Cl5A 117.44(15) . . ? C13A C14A Cl5A 119.11(15) . . ? O10A C15A C14A 124.57(18) . . ? O10A C15A C13A 116.65(17) . 2_575 ? C14A C15A C13A 118.78(17) . 2_575 ? H11C O11W H11D 109.5 . . ? H7WA O7W H7WB 109.3 . . ? H5WA O5W H5WB 109.4 . . ? H4WA O4W H4WB 109.4 . . ? H1A O1 H1B 109.5 . . ? H6WA O6W H6WB 109.4 . . ? H1WA O1W H1WB 109.5 . . ? H8WA O8W H8WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.3 . . ? H10A O10W H10B 109.4 . . ? C5B N1B C2B 121.37(14) . . ? C5B N1B C1B 122.12(9) . . ? C2B N1B C1B 116.48(10) . . ? C3B N2B C7B 119.83(13) . . ? C3B N2B H2B 116.6(19) . . ? C7B N2B H2B 123.5(19) . . ? N1B C1B H1BA 109.5 . . ? N1B C1B H1BB 109.5 . . ? H1BA C1B H1BB 109.5 . . ? N1B C1B H1BC 109.5 . . ? H1BA C1B H1BC 109.5 . . ? H1BB C1B H1BC 109.5 . . ? N1B C2B H2BA 109.5 . . ? N1B C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? N1B C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? N2B C3B C4B 121.77(18) . . ? N2B C3B H3B 119.1 . . ? C4B C3B H3B 119.1 . . ? C3B C4B C5B 120.0(2) . . ? C3B C4B H4B 120.0 . . ? C5B C4B H4B 120.0 . . ? N1B C5B C6B 122.19(17) . . ? N1B C5B C4B 121.22(18) . . ? C6B C5B C4B 116.60(18) . . ? C7B C6B C5B 119.66(19) . . ? C7B C6B H6BA 120.2 . . ? C5B C6B H6BA 120.2 . . ? N2B C7B C6B 122.13(19) . . ? N2B C7B H7B 118.9 . . ? C6B C7B H7B 118.9 . . ? C35B N9B C31B 114.86(18) . . ? C33B N10B C29B 121.26(17) . . ? C33B N10B C30B 120.96(18) . . ? C29B N10B C30B 117.36(17) . . ? N10B C29B H29A 109.5 . . ? N10B C29B H29B 109.5 . . ? H29A C29B H29B 109.5 . . ? N10B C29B H29C 109.5 . . ? H29A C29B H29C 109.5 . . ? H29B C29B H29C 109.5 . . ? N10B C30B H30A 109.5 . . ? N10B C30B H30B 109.5 . . ? H30A C30B H30B 109.5 . . ? N10B C30B H30C 109.5 . . ? H30A C30B H30C 109.5 . . ? H30B C30B H30C 109.5 . . ? N9B C31B C32B 125.2(2) . . ? N9B C31B H31B 117.4 . . ? C32B C31B H31B 117.4 . . ? C31B C32B C33B 119.3(2) . . ? C31B C32B H32B 120.3 . . ? C33B C32B H32B 120.3 . . ? N10B C33B C34B 121.81(19) . . ? N10B C33B C32B 122.24(18) . . ? C34B C33B C32B 115.92(18) . . ? C35B C34B C33B 119.3(2) . . ? C35B C34B H34B 120.3 . . ? C33B C34B H34B 120.3 . . ? N9B C35B C34B 125.3(2) . . ? N9B C35B H35B 117.3 . . ? C34B C35B H35B 117.3 . . ? C24B N7B C28B 120.09(19) . . ? C24B N7B H7BA 121.5(18) . . ? C28B N7B H7BA 118.4(17) . . ? C26B N8B C22B 120.93(18) . . ? C26B N8B C23B 120.63(18) . . ? C22B N8B C23B 118.44(17) . . ? N8B C22B H22A 109.5 . . ? N8B C22B H22B 109.5 . . ? H22A C22B H22B 109.5 . . ? N8B C22B H22C 109.5 . . ? H22A C22B H22C 109.5 . . ? H22B C22B H22C 109.5 . . ? N8B C23B H23A 109.5 . . ? N8B C23B H23B 109.5 . . ? H23A C23B H23B 109.5 . . ? N8B C23B H23C 109.5 . . ? H23A C23B H23C 109.5 . . ? H23B C23B H23C 109.5 . . ? N7B C24B C25B 121.8(2) . . ? N7B C24B H24B 119.1 . . ? C25B C24B H24B 119.1 . . ? C24B C25B C26B 120.1(2) . . ? C24B C25B H25B 119.9 . . ? C26B C25B H25B 119.9 . . ? N8B C26B C27B 121.59(19) . . ? N8B C26B C25B 122.09(19) . . ? C27B C26B C25B 116.33(18) . . ? C28B C27B C26B 120.1(2) . . ? C28B C27B H27B 120.0 . . ? C26B C27B H27B 120.0 . . ? N7B C28B C27B 121.6(2) . . ? N7B C28B H28B 119.2 . . ? C27B C28B H28B 119.2 . . ? C13B N3B C12B 120.17(19) . . ? C13B N3B H3BA 119(2) . . ? C12B N3B H3BA 121(2) . . ? C10B N4B C9B 121.20(18) . . ? C10B N4B C8B 120.16(18) . . ? C9B N4B C8B 118.49(18) . . ? N4B C8B H8BA 109.5 . . ? N4B C8B H8BB 109.5 . . ? H8BA C8B H8BB 109.5 . . ? N4B C8B H8BC 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? N4B C9B H9BA 109.5 . . ? N4B C9B H9BB 109.5 . . ? H9BA C9B H9BB 109.5 . . ? N4B C9B H9BC 109.5 . . ? H9BA C9B H9BC 109.5 . . ? H9BB C9B H9BC 109.5 . . ? N4B C10B C11B 121.79(19) . . ? N4B C10B C14B 121.55(19) . . ? C11B C10B C14B 116.66(18) . . ? C12B C11B C10B 120.1(2) . . ? C12B C11B H11A 120.0 . . ? C10B C11B H11A 120.0 . . ? N3B C12B C11B 121.5(2) . . ? N3B C12B H12B 119.2 . . ? C11B C12B H12B 119.2 . . ? N3B C13B C14B 121.7(2) . . ? N3B C13B H13B 119.1 . . ? C14B C13B H13B 119.1 . . ? C13B C14B C10B 119.8(2) . . ? C13B C14B H14B 120.1 . . ? C10B C14B H14B 120.1 . . ? C19B N5B C16B 122.24(19) . . ? C19B N5B C15B 121.2(2) . . ? C16B N5B C15B 116.61(19) . . ? C17B N6B C21B 120.24(19) . . ? C17B N6B H6B 116.9(19) . . ? C21B N6B H6B 122.8(19) . . ? N5B C15B H15A 109.5 . . ? N5B C15B H15B 109.5 . . ? H15A C15B H15B 109.5 . . ? N5B C15B H15C 109.5 . . ? H15A C15B H15C 109.5 . . ? H15B C15B H15C 109.5 . . ? N5B C16B H16A 109.5 . . ? N5B C16B H16B 109.5 . . ? H16A C16B H16B 109.5 . . ? N5B C16B H16C 109.5 . . ? H16A C16B H16C 109.5 . . ? H16B C16B H16C 109.5 . . ? N6B C17B C18B 121.4(2) . . ? N6B C17B H17B 119.3 . . ? C18B C17B H17B 119.3 . . ? C17B C18B C19B 120.6(2) . . ? C17B C18B H18B 119.7 . . ? C19B C18B H18B 119.7 . . ? N5B C19B C20B 121.43(19) . . ? N5B C19B C18B 122.5(2) . . ? C20B C19B C18B 116.06(19) . . ? C21B C20B C19B 120.3(2) . . ? C21B C20B H20B 119.9 . . ? C19B C20B H20B 119.9 . . ? N6B C21B C20B 121.4(2) . . ? N6B C21B H21B 119.3 . . ? C20B C21B H21B 119.3 . . ? C38B N11B C42B 120.52(19) . . ? C38B N11B H11B 121.3(19) . . ? C42B N11B H11B 118.1(19) . . ? C40B N12B C36B 121.43(19) . . ? C40B N12B C37B 120.69(19) . . ? C36B N12B C37B 116.99(18) . . ? N12B C36B H36A 109.5 . . ? N12B C36B H36B 109.5 . . ? H36A C36B H36B 109.5 . . ? N12B C36B H36C 109.5 . . ? H36A C36B H36C 109.5 . . ? H36B C36B H36C 109.5 . . ? N12B C37B H37A 109.5 . . ? N12B C37B H37B 109.5 . . ? H37A C37B H37B 109.5 . . ? N12B C37B H37C 109.5 . . ? H37A C37B H37C 109.5 . . ? H37B C37B H37C 109.5 . . ? N11B C38B C39B 121.5(2) . . ? N11B C38B H38B 119.2 . . ? C39B C38B H38B 119.2 . . ? C38B C39B C40B 120.05(19) . . ? C38B C39B H39B 120.0 . . ? C40B C39B H39B 120.0 . . ? N12B C40B C41B 121.65(19) . . ? N12B C40B C39B 122.20(19) . . ? C41B C40B C39B 116.16(18) . . ? C42B C41B C40B 120.44(19) . . ? C42B C41B H41B 119.8 . . ? C40B C41B H41B 119.8 . . ? N11B C42B C41B 121.3(2) . . ? N11B C42B H42B 119.4 . . ? C41B C42B H42B 119.4 . . ? 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 C6A C1A C2A O1A 177.5(2) . . . . ? Cl1A C1A C2A O1A -1.1(3) . . . . ? C6A C1A C2A C3A -2.7(3) . . . . ? Cl1A C1A C2A C3A 178.77(15) . . . . ? O1A C2A C3A O2A 1.6(3) . . . . ? C1A C2A C3A O2A -178.29(19) . . . . ? O1A C2A C3A C4A -177.86(19) . . . . ? C1A C2A C3A C4A 2.3(3) . . . . ? O2A C3A C4A C5A -178.2(2) . . . . ? C2A C3A C4A C5A 1.2(3) . . . . ? O2A C3A C4A Cl2A -0.6(3) . . . . ? C2A C3A C4A Cl2A 178.79(15) . . . . ? C3A C4A C5A O3A 176.6(2) . . . . ? Cl2A C4A C5A O3A -1.0(3) . . . . ? C3A C4A C5A C6A -4.0(3) . . . . ? Cl2A C4A C5A C6A 178.42(15) . . . . ? C2A C1A C6A O4A -179.9(2) . . . . ? Cl1A C1A C6A O4A -1.4(3) . . . . ? C2A C1A C6A C5A -0.1(3) . . . . ? Cl1A C1A C6A C5A 178.41(15) . . . . ? O3A C5A C6A O4A 2.7(3) . . . . ? C4A C5A C6A O4A -176.71(19) . . . . ? O3A C5A C6A C1A -177.04(19) . . . . ? C4A C5A C6A C1A 3.5(3) . . . . ? C12A C7A C8A O5A 177.6(2) . . . . ? Cl3A C7A C8A O5A -0.3(3) . . . . ? C12A C7A C8A C9A -3.7(3) . . . . ? Cl3A C7A C8A C9A 178.45(14) . . . . ? O5A C8A C9A O6A 0.0(3) . . . . ? C7A C8A C9A O6A -178.87(19) . . . . ? O5A C8A C9A C10A -179.92(19) . . . . ? C7A C8A C9A C10A 1.2(3) . . . . ? O6A C9A C10A C11A -177.9(2) . . . . ? C8A C9A C10A C11A 2.0(3) . . . . ? O6A C9A C10A Cl4A 2.7(3) . . . . ? C8A C9A C10A Cl4A -177.37(15) . . . . ? C9A C10A C11A O7A 178.4(2) . . . . ? Cl4A C10A C11A O7A -2.2(3) . . . . ? C9A C10A C11A C12A -2.8(3) . . . . ? Cl4A C10A C11A C12A 176.59(15) . . . . ? C8A C7A C12A O8A -178.3(2) . . . . ? Cl3A C7A C12A O8A -0.4(3) . . . . ? C8A C7A C12A C11A 2.9(3) . . . . ? Cl3A C7A C12A C11A -179.17(14) . . . . ? O7A C11A C12A O8A 0.4(3) . . . . ? C10A C11A C12A O8A -178.49(19) . . . . ? O7A C11A C12A C7A 179.33(18) . . . . ? C10A C11A C12A C7A 0.4(3) . . . . ? O9A C13A C14A C15A -176.1(2) . . . . ? C15A C13A C14A C15A 2.7(3) 2_575 . . . ? O9A C13A C14A Cl5A 0.0(3) . . . . ? C15A C13A C14A Cl5A 178.77(14) 2_575 . . . ? C13A C14A C15A O10A 176.9(2) . . . . ? Cl5A C14A C15A O10A 0.7(3) . . . . ? C13A C14A C15A C13A -2.7(3) . . . 2_575 ? Cl5A C14A C15A C13A -178.86(14) . . . 2_575 ? C7B N2B C3B C4B 0.6(3) . . . . ? N2B C3B C4B C5B 0.0(3) . . . . ? C2B N1B C5B C6B -178.8(2) . . . . ? C1B N1B C5B C6B -0.7(2) . . . . ? C2B N1B C5B C4B 1.3(3) . . . . ? C1B N1B C5B C4B 179.51(14) . . . . ? C3B C4B C5B N1B 179.31(18) . . . . ? C3B C4B C5B C6B -0.5(3) . . . . ? N1B C5B C6B C7B -179.44(18) . . . . ? C4B C5B C6B C7B 0.4(3) . . . . ? C3B N2B C7B C6B -0.7(3) . . . . ? C5B C6B C7B N2B 0.2(3) . . . . ? C35B N9B C31B C32B 0.2(3) . . . . ? N9B C31B C32B C33B -0.8(3) . . . . ? C29B N10B C33B C34B 4.6(3) . . . . ? C30B N10B C33B C34B 176.88(19) . . . . ? C29B N10B C33B C32B -177.32(19) . . . . ? C30B N10B C33B C32B -5.0(3) . . . . ? C31B C32B C33B N10B -177.15(19) . . . . ? C31B C32B C33B C34B 1.0(3) . . . . ? N10B C33B C34B C35B 177.36(19) . . . . ? C32B C33B C34B C35B -0.8(3) . . . . ? C31B N9B C35B C34B 0.0(3) . . . . ? C33B C34B C35B N9B 0.3(3) . . . . ? C28B N7B C24B C25B 0.0(3) . . . . ? N7B C24B C25B C26B 0.0(3) . . . . ? C22B N8B C26B C27B 177.6(2) . . . . ? C23B N8B C26B C27B -2.7(3) . . . . ? C22B N8B C26B C25B -2.4(3) . . . . ? C23B N8B C26B C25B 177.3(2) . . . . ? C24B C25B C26B N8B 179.8(2) . . . . ? C24B C25B C26B C27B -0.2(3) . . . . ? N8B C26B C27B C28B -179.6(2) . . . . ? C25B C26B C27B C28B 0.3(3) . . . . ? C24B N7B C28B C27B 0.2(3) . . . . ? C26B C27B C28B N7B -0.3(3) . . . . ? C9B N4B C10B C11B -178.8(2) . . . . ? C8B N4B C10B C11B 5.8(3) . . . . ? C9B N4B C10B C14B 0.7(3) . . . . ? C8B N4B C10B C14B -174.7(2) . . . . ? N4B C10B C11B C12B -179.1(2) . . . . ? C14B C10B C11B C12B 1.4(3) . . . . ? C13B N3B C12B C11B -1.1(3) . . . . ? C10B C11B C12B N3B -0.2(3) . . . . ? C12B N3B C13B C14B 1.0(3) . . . . ? N3B C13B C14B C10B 0.3(3) . . . . ? N4B C10B C14B C13B 179.0(2) . . . . ? C11B C10B C14B C13B -1.5(3) . . . . ? C21B N6B C17B C18B 0.3(3) . . . . ? N6B C17B C18B C19B 0.4(3) . . . . ? C16B N5B C19B C20B -177.6(2) . . . . ? C15B N5B C19B C20B 2.5(3) . . . . ? C16B N5B C19B C18B 2.6(3) . . . . ? C15B N5B C19B C18B -177.3(2) . . . . ? C17B C18B C19B N5B 178.7(2) . . . . ? C17B C18B C19B C20B -1.1(3) . . . . ? N5B C19B C20B C21B -178.6(2) . . . . ? C18B C19B C20B C21B 1.2(3) . . . . ? C17B N6B C21B C20B -0.2(3) . . . . ? C19B C20B C21B N6B -0.6(3) . . . . ? C42B N11B C38B C39B 1.0(3) . . . . ? N11B C38B C39B C40B 0.4(3) . . . . ? C36B N12B C40B C41B 178.1(2) . . . . ? C37B N12B C40B C41B 9.2(3) . . . . ? C36B N12B C40B C39B -1.7(3) . . . . ? C37B N12B C40B C39B -170.6(2) . . . . ? C38B C39B C40B N12B 178.2(2) . . . . ? C38B C39B C40B C41B -1.6(3) . . . . ? N12B C40B C41B C42B -178.3(2) . . . . ? C39B C40B C41B C42B 1.6(3) . . . . ? C38B N11B C42B C41B -1.1(3) . . . . ? C40B C41B C42B N11B -0.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.381 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.065 _iucr_refine_instructions_details ; TITL 20dab1_0m_a.res in P-1 REM Old TITL 17DAb1_0m in P-1 REM SHELXT solution in P-1 REM R1 0.165, Rweak 0.003, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C58 O21 Cl5 N11 CELL 0.71073 13.3824 13.4515 19.0479 86.014 88.821 86.367 ZERR 2 0.0015 0.0017 0.0022 0.004 0.004 0.004 LATT 1 SFAC C H Cl N O UNIT 114 174 10 24 42 RIGU O11W H11c H11d L.S. 24 PLAN 50 BOND $H LIST 4 MORE -1 CONF FMAP 2 ACTA OMIT -4 56 OMIT -1 -1 1 OMIT -1 0 2 OMIT -1 -2 1 OMIT 1 2 1 OMIT 2 0 0 OMIT 1 -1 2 OMIT -1 1 3 OMIT -1 2 1 OMIT -1 -2 2 OMIT 2 -1 1 OMIT 1 1 1 OMIT -2 0 1 OMIT 0 1 2 OMIT 0 1 3 OMIT 0 -2 1 OMIT 1 2 0 OMIT -2 -1 1 OMIT -1 -1 2 OMIT -1 1 1 OMIT 1 0 2 OMIT 0 -1 3 OMIT 1 1 2 OMIT -1 2 0 OMIT 0 0 1 OMIT 0 2 2 OMIT 2 1 1 OMIT 0 2 1 OMIT -2 1 0 OMIT 0 0 2 OMIT 1 -1 1 OMIT -2 -1 2 OMIT 1 1 3 OMIT -1 1 0 OMIT 1 0 0 OMIT 1 -2 1 OMIT 2 1 0 OMIT 2 1 3 OMIT 0 1 1 OMIT 0 2 0 OMIT 2 2 0 OMIT 0 -1 1 OMIT 0 1 0 OMIT 1 0 4 OMIT -1 1 2 OMIT 0 0 4 OMIT -1 0 1 OMIT -2 0 2 OMIT -2 1 1 OMIT -1 1 4 OMIT 2 2 1 OMIT 0 0 3 OMIT 2 -1 2 OMIT 3 0 1 OMIT 3 1 1 OMIT 1 0 3 OMIT -3 0 1 OMIT 2 -1 3 OMIT 1 1 0 REM REM REM WGHT 0.056500 1.580800 FVAR 0.12100 CL1A 3 0.718736 0.039206 0.283647 11.00000 0.01940 0.03219 = 0.02228 -0.01136 -0.00332 0.01034 CL2A 3 0.417304 0.342201 0.433256 11.00000 0.03148 0.04996 = 0.02302 -0.01838 -0.01025 0.02492 O1A 5 0.734027 0.114362 0.426940 11.00000 0.01680 0.02796 = 0.01790 -0.00497 -0.00626 0.00491 O2A 5 0.610267 0.245895 0.487568 11.00000 0.02274 0.03232 = 0.01734 -0.00991 -0.00876 0.00711 O3A 5 0.395737 0.256841 0.293820 11.00000 0.01621 0.03141 = 0.01841 -0.00664 -0.00538 0.00664 O4A 5 0.527951 0.136205 0.229468 11.00000 0.01870 0.02783 = 0.01746 -0.00843 -0.00439 0.00329 C1A 1 0.636523 0.122186 0.325256 11.00000 0.01376 0.01855 = 0.01666 -0.00427 -0.00050 0.00355 C2A 1 0.658416 0.147773 0.392078 11.00000 0.01330 0.01855 = 0.01511 -0.00077 -0.00076 -0.00171 C3A 1 0.586199 0.223183 0.428080 11.00000 0.01656 0.01842 = 0.01526 -0.00312 -0.00064 -0.00016 C4A 1 0.499770 0.259405 0.392191 11.00000 0.01685 0.02101 = 0.01668 -0.00541 0.00012 0.00500 C5A 1 0.474534 0.229446 0.326060 11.00000 0.01492 0.01879 = 0.01558 -0.00008 -0.00207 -0.00018 C6A 1 0.549255 0.158415 0.289456 11.00000 0.01510 0.01648 = 0.01553 -0.00316 -0.00125 -0.00180 CL3A 3 0.917638 0.422312 0.100315 11.00000 0.01800 0.02370 = 0.02252 -0.01013 -0.00191 0.00380 CL4A 3 0.655499 0.771706 0.235095 11.00000 0.02024 0.02674 = 0.02124 -0.00966 -0.00435 0.00949 O5A 5 0.942439 0.507638 0.241482 11.00000 0.02107 0.02680 = 0.02070 -0.00705 -0.00700 0.00818 O6A 5 0.831015 0.653401 0.295666 11.00000 0.02124 0.03226 = 0.01966 -0.01057 -0.00578 0.00853 O7A 5 0.620910 0.677207 0.100108 11.00000 0.01999 0.02532 = 0.02420 -0.00782 -0.00846 0.00557 O8A 5 0.733950 0.532443 0.043615 11.00000 0.02390 0.03008 = 0.02056 -0.01059 -0.00752 0.00552 N5B 4 1.183504 0.579928 0.543087 11.00000 0.03153 0.02578 = 0.02529 -0.00712 -0.01201 0.00451 N6B 4 0.989932 0.586269 0.377573 11.00000 0.02262 0.03134 = 0.02100 0.00101 -0.00797 -0.00478 C7A 1 0.844402 0.515980 0.138838 11.00000 0.01518 0.01663 = 0.01839 -0.00501 -0.00013 0.00104 C8A 1 0.870326 0.543726 0.205148 11.00000 0.01666 0.01658 = 0.01672 -0.00244 -0.00057 0.00012 C9A 1 0.805487 0.628630 0.236729 11.00000 0.01597 0.01817 = 0.01493 -0.00327 -0.00014 -0.00064 C10A 1 0.723367 0.672771 0.199207 11.00000 0.01514 0.01720 = 0.01786 -0.00322 0.00021 0.00149 C11A 1 0.695064 0.641357 0.134692 11.00000 0.01521 0.01660 = 0.01721 -0.00122 -0.00233 -0.00035 C12A 1 0.759942 0.557319 0.101746 11.00000 0.01630 0.01732 = 0.01642 -0.00291 -0.00115 -0.00238 C15B 1 1.277909 0.517568 0.543338 11.00000 0.03798 0.04154 = 0.05460 -0.00856 -0.02572 0.01189 AFIX 137 H15A 2 1.263504 0.448537 0.543530 11.00000 -1.50000 H15B 2 1.314877 0.527986 0.584580 11.00000 -1.50000 H15C 2 1.316937 0.535496 0.502069 11.00000 -1.50000 AFIX 0 C16B 1 1.163661 0.638676 0.603395 11.00000 0.05068 0.03621 = 0.02617 -0.00947 -0.01335 -0.00046 AFIX 137 H16A 2 1.122188 0.697330 0.589559 11.00000 -1.50000 H16B 2 1.225770 0.657971 0.621003 11.00000 -1.50000 H16C 2 1.129887 0.599631 0.639558 11.00000 -1.50000 AFIX 0 C17B 1 0.968743 0.644356 0.430929 11.00000 0.01838 0.02720 = 0.02923 0.00150 -0.00097 0.00162 AFIX 43 H17B 2 0.910583 0.686080 0.429688 11.00000 -1.20000 AFIX 0 C18B 1 1.030144 0.643696 0.486678 11.00000 0.02305 0.02025 = 0.02219 -0.00565 0.00174 0.00002 AFIX 43 H18B 2 1.013351 0.684333 0.523227 11.00000 -1.20000 AFIX 0 C19B 1 1.119738 0.581575 0.489724 11.00000 0.01963 0.01617 = 0.01872 -0.00055 -0.00062 -0.00193 C20B 1 1.138479 0.520581 0.432787 11.00000 0.02121 0.02109 = 0.02271 -0.00367 0.00098 0.00013 AFIX 43 H20B 2 1.195389 0.477176 0.432458 11.00000 -1.20000 AFIX 0 C21B 1 1.073536 0.525180 0.378482 11.00000 0.02628 0.02572 = 0.01796 -0.00511 0.00083 -0.00401 AFIX 43 H21B 2 1.087248 0.485174 0.341127 11.00000 -1.20000 AFIX 0 H6B 2 0.948974 0.589569 0.343153 11.00000 0.04138 CL5A 3 0.156383 0.862797 -0.082367 11.00000 0.01746 0.03030 = 0.02079 -0.01247 -0.00311 0.00822 O9A 5 0.175439 0.939162 0.061788 11.00000 0.01604 0.02756 = 0.01853 -0.00674 -0.00552 0.00594 O10A 5 -0.040187 0.950500 -0.130634 11.00000 0.01971 0.03106 = 0.01605 -0.01000 -0.00466 0.00505 C13A 1 0.095081 0.963268 0.030822 11.00000 0.01331 0.01441 = 0.01556 -0.00215 -0.00241 0.00025 C14A 1 0.070392 0.936256 -0.036044 11.00000 0.01462 0.01690 = 0.01597 -0.00752 0.00054 0.00137 C15A 1 -0.018310 0.970114 -0.069809 11.00000 0.01449 0.01581 = 0.01394 -0.00426 -0.00047 -0.00198 AFIX 6 O4W 5 1.107773 0.178852 0.430138 11.00000 0.03231 0.03740 = 0.02502 -0.00326 -0.00304 -0.00351 H4WA 2 1.130122 0.151799 0.468919 11.00000 -1.50000 H4WB 2 1.055597 0.150830 0.419424 11.00000 -1.50000 AFIX 6 O10W 5 0.605883 1.013757 0.121665 11.00000 0.03087 0.03898 = 0.03095 -0.01007 -0.00209 0.00013 H10A 2 0.566783 0.966246 0.122309 11.00000 -1.50000 H10B 2 0.603182 1.046211 0.081746 11.00000 -1.50000 AFIX 6 O7W 5 1.068535 0.337944 0.230862 11.00000 0.02484 0.02577 = 0.02994 -0.00293 -0.00566 0.00920 H7WA 2 1.108574 0.334568 0.265196 11.00000 -1.50000 H7WB 2 1.030844 0.391151 0.231698 11.00000 -1.50000 AFIX 6 O5W 5 0.935428 0.109446 0.376140 11.00000 0.01819 0.04099 = 0.02790 0.00013 -0.00049 -0.00012 H5WA 2 0.872946 0.109904 0.385367 11.00000 -1.50000 H5WB 2 0.944593 0.123180 0.332315 11.00000 -1.50000 AFIX 6 O1W 5 1.477334 0.343342 0.598412 11.00000 0.02888 0.06342 = 0.02345 -0.01415 -0.00128 -0.01058 H1WA 2 1.513886 0.368772 0.627547 11.00000 -1.50000 H1WB 2 1.511823 0.330410 0.561809 11.00000 -1.50000 AFIX 6 O8W 5 1.199186 0.319422 0.341408 11.00000 0.01808 0.02873 = 0.03334 -0.00370 -0.00115 0.00581 H8WA 2 1.175696 0.276997 0.371528 11.00000 -1.50000 H8WB 2 1.260210 0.302709 0.332632 11.00000 -1.50000 AFIX 6 O2W 5 1.284940 0.260659 0.594881 11.00000 0.02710 0.03730 = 0.02228 -0.01009 0.00171 -0.00123 H2WA 2 1.257061 0.276761 0.633274 11.00000 -1.50000 H2WB 2 1.343391 0.282093 0.591877 11.00000 -1.50000 AFIX 6 O11W 5 0.364407 0.884291 0.004057 11.00000 0.01692 0.03741 = 0.03638 -0.01086 -0.00292 0.00502 H11C 2 0.307096 0.896660 0.022697 11.00000 -1.50000 H11D 2 0.409214 0.885262 0.034898 11.00000 -1.50000 AFIX 6 O3W 5 1.195254 0.098690 0.552792 11.00000 0.03571 0.02843 = 0.03739 -0.00173 -0.01338 0.00128 H3WA 2 1.218007 0.041548 0.569186 11.00000 -1.50000 H3WB 2 1.230140 0.143300 0.567600 11.00000 -1.50000 AFIX 6 O6W 5 0.957878 0.173656 0.239309 11.00000 0.03806 0.03619 = 0.02393 -0.01126 0.00234 -0.00678 H6WA 2 0.964359 0.139932 0.203166 11.00000 -1.50000 H6WB 2 0.993103 0.224144 0.233699 11.00000 -1.50000 AFIX 0 N1B 4 0.976674 0.171376 0.725530 11.00000 0.01859 0.03096 = 0.01826 -0.00910 -0.00549 0.00815 N2B 4 0.786836 0.174873 0.557824 11.00000 0.02086 0.02714 = 0.01877 -0.00067 -0.00680 -0.00338 C1B 1 1.071755 0.110780 0.729020 11.00000 0.01973 0.03470 = 0.02702 -0.00782 -0.00776 0.00938 AFIX 137 H1BA 2 1.061247 0.047141 0.753141 11.00000 -1.50000 H1BB 2 1.119631 0.144460 0.754008 11.00000 -1.50000 H1BC 2 1.096605 0.101086 0.682194 11.00000 -1.50000 AFIX 0 C2B 1 0.951097 0.229714 0.785353 11.00000 0.03031 0.05068 = 0.02365 -0.01816 -0.00913 0.01177 AFIX 137 H2BA 2 0.936833 0.298271 0.769265 11.00000 -1.50000 H2BB 2 1.006325 0.225027 0.817036 11.00000 -1.50000 H2BC 2 0.893210 0.204437 0.809335 11.00000 -1.50000 AFIX 0 C3B 1 0.762349 0.229749 0.612460 11.00000 0.01754 0.02329 = 0.02434 -0.00105 -0.00347 0.00220 AFIX 43 H3B 2 0.702263 0.268506 0.611805 11.00000 -1.20000 AFIX 0 C4B 1 0.823004 0.230245 0.668781 11.00000 0.01702 0.02242 = 0.02125 -0.00578 -0.00118 0.00314 AFIX 43 H4B 2 0.804204 0.269064 0.705959 11.00000 -1.20000 AFIX 0 C5B 1 0.915148 0.171496 0.670924 11.00000 0.01597 0.01893 = 0.01547 -0.00112 -0.00057 -0.00205 C6B 1 0.938052 0.113855 0.612421 11.00000 0.01874 0.02038 = 0.02038 -0.00459 -0.00097 0.00405 AFIX 43 H6BA 2 0.997197 0.073753 0.611194 11.00000 -1.20000 AFIX 0 C7B 1 0.873360 0.117462 0.558294 11.00000 0.02581 0.02518 = 0.01617 -0.00619 -0.00140 -0.00044 AFIX 43 H7B 2 0.889087 0.079187 0.520301 11.00000 -1.20000 AFIX 0 H2B 2 0.741405 0.175603 0.519329 11.00000 0.06400 N11B 4 -0.215815 0.999606 -0.201607 11.00000 0.02177 0.02299 = 0.02040 -0.00027 -0.00679 -0.00433 N12B 4 -0.410216 1.014435 -0.367162 11.00000 0.02011 0.03013 = 0.01789 -0.00323 -0.00441 0.00106 C36B 1 -0.383327 0.968892 -0.432433 11.00000 0.03858 0.04309 = 0.01527 -0.00419 -0.00336 -0.01052 AFIX 137 H36A 2 -0.342768 1.012445 -0.461205 11.00000 -1.50000 H36B 2 -0.443045 0.957907 -0.457114 11.00000 -1.50000 H36C 2 -0.346397 0.906226 -0.422117 11.00000 -1.50000 AFIX 0 C37B 1 -0.500339 1.082307 -0.367356 11.00000 0.02500 0.03460 = 0.04271 0.00121 -0.01582 0.00391 AFIX 137 H37A 2 -0.541033 1.066000 -0.326594 11.00000 -1.50000 H37B 2 -0.537636 1.075522 -0.409091 11.00000 -1.50000 H37C 2 -0.481378 1.149852 -0.366511 11.00000 -1.50000 AFIX 0 C38B 1 -0.189905 0.952439 -0.259617 11.00000 0.01547 0.02259 = 0.02624 -0.00016 -0.00190 0.00216 AFIX 43 H38B 2 -0.127828 0.917491 -0.261908 11.00000 -1.20000 AFIX 0 C39B 1 -0.252464 0.954572 -0.315248 11.00000 0.01783 0.01987 = 0.01799 -0.00598 0.00117 0.00046 AFIX 43 H39B 2 -0.233045 0.920940 -0.354823 11.00000 -1.20000 AFIX 0 C40B 1 -0.347332 1.008067 -0.312961 11.00000 0.01588 0.01571 = 0.01636 0.00021 -0.00194 -0.00211 C41B 1 -0.371928 1.054809 -0.249961 11.00000 0.01892 0.01959 = 0.01982 -0.00309 0.00038 0.00236 AFIX 43 H41B 2 -0.433797 1.089446 -0.245152 11.00000 -1.20000 AFIX 0 C42B 1 -0.305638 1.049356 -0.196462 11.00000 0.02741 0.02113 = 0.01708 -0.00571 0.00049 -0.00307 AFIX 43 H42B 2 -0.322824 1.080680 -0.155512 11.00000 -1.20000 AFIX 0 H11B 2 -0.172925 0.994578 -0.164411 11.00000 0.06240 N9B 4 1.608238 0.395200 0.707748 11.00000 0.02154 0.03236 = 0.02372 -0.01138 -0.00341 0.00451 N10B 4 1.789971 0.392570 0.885517 11.00000 0.02035 0.02090 = 0.01780 -0.00104 -0.00203 -0.00427 C29B 1 1.783436 0.316429 0.942675 11.00000 0.02962 0.02454 = 0.02041 0.00005 0.00014 -0.00157 AFIX 137 H29A 2 1.714647 0.311184 0.956949 11.00000 -1.50000 H29B 2 1.821275 0.334093 0.981729 11.00000 -1.50000 H29C 2 1.810050 0.253501 0.927262 11.00000 -1.50000 AFIX 0 C30B 1 1.867911 0.461982 0.888861 11.00000 0.02278 0.02670 = 0.02608 -0.00426 -0.00332 -0.00504 AFIX 137 H30A 2 1.921841 0.444025 0.857268 11.00000 -1.50000 H30B 2 1.892383 0.459567 0.936011 11.00000 -1.50000 H30C 2 1.841165 0.528359 0.875520 11.00000 -1.50000 AFIX 0 C31B 1 1.678057 0.461256 0.713383 11.00000 0.02216 0.02755 = 0.01998 -0.00209 0.00212 0.00450 AFIX 43 H31B 2 1.684544 0.509619 0.676522 11.00000 -1.20000 AFIX 0 C32B 1 1.741040 0.463013 0.769668 11.00000 0.01721 0.01910 = 0.02185 -0.00308 0.00157 -0.00058 AFIX 43 H32B 2 1.788434 0.510679 0.769655 11.00000 -1.20000 AFIX 0 C33B 1 1.733017 0.392092 0.827127 11.00000 0.01508 0.01511 = 0.01957 -0.00630 0.00318 0.00365 C34B 1 1.660176 0.322090 0.821456 11.00000 0.01968 0.01909 = 0.02198 -0.00403 0.00306 -0.00068 AFIX 43 H34B 2 1.651529 0.272634 0.857277 11.00000 -1.20000 AFIX 0 C35B 1 1.601819 0.327498 0.762375 11.00000 0.01894 0.02374 = 0.03287 -0.01263 0.00028 -0.00154 AFIX 43 H35B 2 1.554199 0.280397 0.760269 11.00000 -1.20000 AFIX 0 N3B 4 0.355396 0.196582 0.154249 11.00000 0.02069 0.02542 = 0.02277 -0.00032 -0.00830 -0.00513 N4B 4 0.166306 0.203407 -0.013806 11.00000 0.02019 0.02614 = 0.01856 -0.00526 -0.00556 0.00277 C8B 1 0.074778 0.268801 -0.015477 11.00000 0.02132 0.03389 = 0.02924 -0.00201 -0.00983 0.00340 AFIX 137 H8BA 2 0.031040 0.248355 0.022680 11.00000 -1.50000 H8BB 2 0.041793 0.264600 -0.059358 11.00000 -1.50000 H8BC 2 0.091385 0.336402 -0.010849 11.00000 -1.50000 AFIX 0 C9B 1 0.192859 0.147681 -0.075044 11.00000 0.03784 0.03338 = 0.01822 -0.00867 0.00012 -0.01075 AFIX 137 H9BA 2 0.245849 0.178883 -0.101214 11.00000 -1.50000 H9BB 2 0.135451 0.147010 -0.104371 11.00000 -1.50000 H9BC 2 0.214785 0.080404 -0.059926 11.00000 -1.50000 AFIX 0 C10B 1 0.227530 0.200596 0.041411 11.00000 0.01682 0.01747 = 0.01703 -0.00025 -0.00157 -0.00157 C11B 1 0.202025 0.252619 0.101711 11.00000 0.01895 0.01893 = 0.02087 -0.00544 -0.00123 0.00257 AFIX 43 H11A 2 0.140960 0.289364 0.104227 11.00000 -1.20000 AFIX 0 C12B 1 0.266638 0.249112 0.156188 11.00000 0.02516 0.02248 = 0.01958 -0.00436 -0.00104 -0.00383 AFIX 43 H12B 2 0.249010 0.283806 0.195614 11.00000 -1.20000 AFIX 0 C13B 1 0.381572 0.144607 0.098385 11.00000 0.01580 0.02157 = 0.03018 0.00162 -0.00212 0.00145 AFIX 43 H13B 2 0.442792 0.107815 0.098198 11.00000 -1.20000 AFIX 0 C14B 1 0.320951 0.144383 0.042155 11.00000 0.01867 0.02010 = 0.02064 -0.00354 0.00230 0.00056 AFIX 43 H14B 2 0.340592 0.107454 0.004172 11.00000 -1.20000 AFIX 0 H3BA 2 0.395385 0.195529 0.190616 11.00000 0.07075 N7B 4 0.561836 0.610226 -0.028987 11.00000 0.01834 0.02470 = 0.02019 -0.00402 -0.00377 -0.00014 N8B 4 0.372685 0.626029 -0.197829 11.00000 0.01813 0.02784 = 0.01983 -0.00653 -0.00407 0.00332 C22B 1 0.393548 0.564677 -0.257182 11.00000 0.03139 0.03500 = 0.01825 -0.00563 -0.00324 -0.00432 AFIX 137 H22A 2 0.457714 0.578811 -0.277613 11.00000 -1.50000 H22B 2 0.342709 0.579424 -0.291856 11.00000 -1.50000 H22C 2 0.393962 0.495391 -0.241169 11.00000 -1.50000 AFIX 0 C23B 1 0.282627 0.693364 -0.199295 11.00000 0.01787 0.03551 = 0.02832 0.00010 -0.00529 0.00292 AFIX 137 H23A 2 0.243394 0.680448 -0.157268 11.00000 -1.50000 H23B 2 0.243937 0.682642 -0.239670 11.00000 -1.50000 H23C 2 0.301356 0.761260 -0.201910 11.00000 -1.50000 AFIX 0 C24B 1 0.580633 0.550136 -0.081709 11.00000 0.01959 0.02507 = 0.02293 -0.00668 -0.00097 0.00566 AFIX 43 H24B 2 0.636557 0.505388 -0.079434 11.00000 -1.20000 AFIX 0 C25B 1 0.520209 0.552956 -0.138220 11.00000 0.02063 0.02448 = 0.01896 -0.00790 0.00054 0.00208 AFIX 43 H25B 2 0.535009 0.510523 -0.174043 11.00000 -1.20000 AFIX 0 C26B 1 0.434377 0.620650 -0.142721 11.00000 0.01498 0.02067 = 0.01839 -0.00329 -0.00047 -0.00182 C27B 1 0.417144 0.682460 -0.085871 11.00000 0.01810 0.02189 = 0.02265 -0.00664 -0.00015 0.00277 AFIX 43 H27B 2 0.361809 0.727927 -0.085976 11.00000 -1.20000 AFIX 0 C28B 1 0.481493 0.675328 -0.031144 11.00000 0.02242 0.02241 = 0.02073 -0.00819 0.00014 -0.00075 AFIX 43 H28B 2 0.469529 0.716595 0.005712 11.00000 -1.20000 AFIX 0 H7BA 2 0.603513 0.607030 0.009788 11.00000 0.05599 AFIX 6 O1 5 0.496675 0.853278 0.110347 11.00000 0.02648 0.03244 = 0.02563 -0.00317 0.00138 0.01220 H1A 2 0.483595 0.864901 0.152975 11.00000 -1.50000 H1B 2 0.537038 0.802008 0.108963 11.00000 -1.50000 AFIX 0 HKLF 4 REM 17dab1_0m_a.res in P-1 REM R1 = 0.0471 for 10900 Fo > 4sig(Fo) and 0.0857 for all 16396 data REM 921 parameters refined using 0 restraints END WGHT 0.0562 1.5869 REM Highest difference peak 0.618, deepest hole -0.573, 1-sigma level 0.066 Q1 1 0.5985 1.0543 0.1579 11.00000 0.05 0.62 Q2 1 0.8627 0.1992 0.6686 11.00000 0.05 0.38 Q3 1 0.6223 0.1941 0.4040 11.00000 0.05 0.38 Q4 1 -0.3023 0.9781 -0.3079 11.00000 0.05 0.37 Q5 1 0.0742 0.9406 0.0014 11.00000 0.05 0.35 Q6 1 0.6369 0.1205 0.3609 11.00000 0.05 0.34 Q7 1 1.0719 0.0470 0.7092 11.00000 0.05 0.33 Q8 1 0.5414 0.9041 0.1120 11.00000 0.05 0.33 Q9 1 0.2791 0.1778 0.0378 11.00000 0.05 0.33 Q10 1 0.8032 0.5398 0.1247 11.00000 0.05 0.33 Q11 1 0.6981 0.6452 0.1797 11.00000 0.05 0.32 Q12 1 0.5938 0.1392 0.3137 11.00000 0.05 0.32 Q13 1 1.1032 0.6550 0.6078 11.00000 0.05 0.32 Q14 1 0.5007 0.2632 0.3515 11.00000 0.05 0.31 Q15 1 1.0017 0.6326 0.4608 11.00000 0.05 0.31 Q16 1 1.0790 0.0807 0.7757 11.00000 0.05 0.31 Q17 1 0.0347 0.9572 -0.0544 11.00000 0.05 0.30 Q18 1 0.8495 0.5221 0.1760 11.00000 0.05 0.30 Q19 1 0.8632 0.5418 0.1638 11.00000 0.05 0.30 Q20 1 0.0542 0.9947 0.0495 11.00000 0.05 0.30 Q21 1 -0.3480 1.0421 -0.2858 11.00000 0.05 0.30 Q22 1 0.5534 0.2645 0.4027 11.00000 0.05 0.30 Q23 1 0.5386 0.5373 -0.0996 11.00000 0.05 0.29 Q24 1 0.4444 0.8577 0.0807 11.00000 0.05 0.29 Q25 1 0.7693 0.6555 0.2146 11.00000 0.05 0.29 Q26 1 -0.3017 0.9609 -0.4486 11.00000 0.05 0.28 Q27 1 0.6033 0.2375 0.4508 11.00000 0.05 0.28 Q28 1 0.7376 0.6146 0.1129 11.00000 0.05 0.28 Q29 1 -0.2234 0.9656 -0.2891 11.00000 0.05 0.28 Q30 1 1.2261 -0.0393 0.6107 11.00000 0.05 0.27 Q31 1 0.3945 0.6006 -0.1634 11.00000 0.05 0.27 Q32 1 0.5173 0.1976 0.3078 11.00000 0.05 0.27 Q33 1 1.1861 0.6031 0.6412 11.00000 0.05 0.27 Q34 1 -0.3344 1.0591 -0.2335 11.00000 0.05 0.27 Q35 1 0.8418 0.5979 0.2133 11.00000 0.05 0.27 Q36 1 1.4960 0.3901 0.5438 11.00000 0.05 0.27 Q37 1 0.5383 0.2357 0.4130 11.00000 0.05 0.27 Q38 1 0.3292 0.5128 -0.2518 11.00000 0.05 0.27 Q39 1 0.3623 0.1649 0.0489 11.00000 0.05 0.26 Q40 1 0.7960 0.2187 0.6441 11.00000 0.05 0.26 Q41 1 1.1363 0.1444 0.7072 11.00000 0.05 0.26 Q42 1 0.7434 0.1349 0.4608 11.00000 0.05 0.26 Q43 1 1.0959 0.5031 0.4212 11.00000 0.05 0.26 Q44 1 -0.3790 1.0064 -0.3406 11.00000 0.05 0.26 Q45 1 0.1991 0.2165 -0.1223 11.00000 0.05 0.25 Q46 1 1.1209 0.1717 0.7221 11.00000 0.05 0.25 Q47 1 0.9333 0.1576 0.6386 11.00000 0.05 0.25 Q48 1 0.3752 0.9324 -0.0317 11.00000 0.05 0.25 Q49 1 0.1657 0.1821 -0.1211 11.00000 0.05 0.25 Q50 1 0.3896 0.6072 -0.2957 11.00000 0.05 0.24 REM The information below was added by Olex2. REM REM R1 = 0.0471 for 10900 Fo > 4sig(Fo) and 0.0857 for all 60979 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.62, deepest hole -0.57 REM Mean Shift 0.001, Max Shift 0.074. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0857 REM R1_gt = 0.0471 REM wR_ref = 0.1315 REM GOOF = 1.006 REM Shift_max = 0.074 REM Shift_mean = 0.001 REM Reflections_all = 60979 REM Reflections_gt = 10900 REM Parameters = n/a REM Hole = -0.57 REM Peak = 0.62 REM Flack = n/a ; _publcif_info_exptl_table_max_cols 4 loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max ; ;