data_C35H31BO3 _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H31 B O3' _chemical_formula_sum 'C35 H31 B O3' _chemical_formula_weight 510.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 1 _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' _cell_length_a 10.1118(3) _cell_length_b 11.8308(4) _cell_length_c 12.5795(4) _cell_angle_alpha 83.3770(10) _cell_angle_beta 70.4740(10) _cell_angle_gamma 72.0230(10) _cell_volume 1348.98(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9808 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 66.69 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.257 _exptl_crystal_F_000 540 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.560 _exptl_crystal_size_min 0.480 _exptl_absorpt_coefficient_mu 0.611 _shelx_estimated_absorpt_T_min 0.711 _shelx_estimated_absorpt_T_max 0.758 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6878 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_process_details ; Sheldrick, G.M. (2016). SADABS. Bruker AXS Inc. Madison, WI USA. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\uS' _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type 'Bruker Kappa DUO CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25450 _diffrn_reflns_av_unetI/netI 0.0457 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.728 _diffrn_reflns_theta_max 66.684 _diffrn_reflns_theta_full 66.684 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_point_group_measured_fraction_full 0.951 _reflns_number_total 9064 _reflns_number_gt 9021 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.930 _reflns_Friedel_fraction_max 0.916 _reflns_Friedel_fraction_full 0.916 _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 'APEX2 (Bruker, 2014)' _computing_cell_refinement 'SAINT (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_structure_solution 'SHELXT 2016/6 (Sheldrick, 2016)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _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^)+(0.0885P)^2^+0.2292P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 4277 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). Flack x = -0.002(171) by classical fit to all intensities ; _refine_ls_abs_structure_Flack -0.16(14) _chemical_absolute_configuration ad _refine_ls_number_reflns 9064 _refine_ls_number_parameters 709 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 O1 O 0.4672(2) 0.8507(2) 0.60179(17) 0.0279(5) Uani 1 1 d . . . . . O2 O 0.40738(19) 0.32146(16) 0.84065(15) 0.0163(4) Uani 1 1 d . . . . . O3 O 0.52153(19) 0.29948(16) 0.64976(15) 0.0164(4) Uani 1 1 d . . . . . B1 B 0.3926(3) 0.3316(2) 0.7359(2) 0.0154(6) Uani 1 1 d . . . . . C1 C 0.4580(4) 0.9395(3) 0.6731(3) 0.0290(6) Uani 1 1 d . . . . . H1A H 0.356376 0.989585 0.700673 0.043 Uiso 1 1 calc R U . . . H1B H 0.521115 0.988560 0.630532 0.043 Uiso 1 1 calc R U . . . H1C H 0.490061 0.901513 0.737278 0.043 Uiso 1 1 calc R U . . . C2 C 0.3893(3) 0.7698(3) 0.6483(2) 0.0220(6) Uani 1 1 d . . . . . C3 C 0.4155(3) 0.6776(3) 0.5788(2) 0.0242(6) Uani 1 1 d . . . . . H3 H 0.483166 0.673350 0.504755 0.029 Uiso 1 1 calc R U . . . C4 C 0.3429(3) 0.5910(2) 0.6171(2) 0.0202(5) Uani 1 1 d . . . . . H4 H 0.361987 0.528265 0.568317 0.024 Uiso 1 1 calc R U . . . C5 C 0.2434(3) 0.5938(2) 0.7248(2) 0.0168(5) Uani 1 1 d . . . . . C6 C 0.2195(3) 0.6869(3) 0.7936(2) 0.0242(6) Uani 1 1 d . . . . . H6 H 0.152990 0.690738 0.868151 0.029 Uiso 1 1 calc R U . . . C7 C 0.2915(3) 0.7755(3) 0.7556(3) 0.0247(6) Uani 1 1 d . . . . . H7 H 0.272679 0.838749 0.803644 0.030 Uiso 1 1 calc R U . . . C8 C 0.1550(3) 0.5039(2) 0.7672(2) 0.0150(5) Uani 1 1 d . . . . . H8 H 0.137185 0.494277 0.850415 0.018 Uiso 1 1 calc R U . . . C9 C 0.2394(3) 0.3790(2) 0.7145(2) 0.0151(5) Uani 1 1 d . . . . . H9 H 0.258481 0.387957 0.631113 0.018 Uiso 1 1 calc R U . . . C10 C 0.1524(3) 0.2892(2) 0.7575(2) 0.0164(5) Uani 1 1 d . . . . . C11 C 0.1382(4) 0.2187(3) 0.6836(3) 0.0269(6) Uani 1 1 d . . . . . H11 H 0.179881 0.228921 0.604618 0.032 Uiso 1 1 calc R U . . . C12 C 0.0639(4) 0.1334(3) 0.7230(3) 0.0349(7) Uani 1 1 d . . . . . H12 H 0.056077 0.085717 0.670923 0.042 Uiso 1 1 calc R U . . . C13 C 0.0016(3) 0.1175(3) 0.8371(3) 0.0304(7) Uani 1 1 d . . . . . H13 H -0.048855 0.058971 0.863814 0.037 Uiso 1 1 calc R U . . . C14 C 0.0133(3) 0.1874(3) 0.9120(3) 0.0273(6) Uani 1 1 d . . . . . H14 H -0.030074 0.177675 0.990802 0.033 Uiso 1 1 calc R U . . . C15 C 0.0886(3) 0.2723(3) 0.8725(2) 0.0230(6) Uani 1 1 d . . . . . H15 H 0.096594 0.319532 0.924908 0.028 Uiso 1 1 calc R U . . . C16 C 0.0056(3) 0.5519(2) 0.7494(2) 0.0143(5) Uani 1 1 d . . . . . C17 C -0.0068(3) 0.5735(2) 0.6408(2) 0.0174(5) Uani 1 1 d . . . . . H17 H 0.078733 0.556724 0.576733 0.021 Uiso 1 1 calc R U . . . C18 C -0.1439(3) 0.6192(2) 0.6266(2) 0.0219(6) Uani 1 1 d . . . . . H18 H -0.151609 0.633795 0.552764 0.026 Uiso 1 1 calc R U . . . C19 C -0.2694(3) 0.6438(2) 0.7193(3) 0.0241(6) Uani 1 1 d . . . . . H19 H -0.362917 0.675024 0.708946 0.029 Uiso 1 1 calc R U . . . C20 C -0.2586(3) 0.6229(2) 0.8266(3) 0.0233(6) Uani 1 1 d . . . . . H20 H -0.344593 0.639422 0.890356 0.028 Uiso 1 1 calc R U . . . C21 C -0.1214(3) 0.5775(2) 0.8411(2) 0.0195(5) Uani 1 1 d . . . . . H21 H -0.114570 0.563791 0.915262 0.023 Uiso 1 1 calc R U . . . C22 C 0.5634(3) 0.2852(2) 0.8288(2) 0.0146(5) Uani 1 1 d . . . . . C23 C 0.6414(3) 0.2646(2) 0.6972(2) 0.0148(5) Uani 1 1 d . . . . . C24 C 0.6085(3) 0.1633(2) 0.8817(2) 0.0139(5) Uani 1 1 d . . . . . C25 C 0.5863(3) 0.1260(2) 0.9918(2) 0.0168(5) Uani 1 1 d . . . . . H25 H 0.529846 0.180272 1.051592 0.020 Uiso 1 1 calc R U . . . C26 C 0.6493(3) 0.0046(3) 1.0149(2) 0.0226(6) Uani 1 1 d . . . . . H26 H 0.634148 -0.021549 1.091173 0.027 Uiso 1 1 calc R U . . . C27 C 0.7314(3) -0.0762(2) 0.9304(2) 0.0208(5) Uani 1 1 d . . . . . H27 H 0.770631 -0.157031 0.949027 0.025 Uiso 1 1 calc R U . . . C28 C 0.7579(3) -0.0398(2) 0.8157(2) 0.0170(5) Uani 1 1 d . . . . . C29 C 0.8460(3) -0.1100(2) 0.7193(2) 0.0199(5) Uani 1 1 d . . . . . H29 H 0.893055 -0.191847 0.728173 0.024 Uiso 1 1 calc R U . . . C30 C 0.8637(3) -0.0601(2) 0.6125(2) 0.0207(5) Uani 1 1 d . . . . . H30 H 0.921546 -0.109236 0.549033 0.025 Uiso 1 1 calc R U . . . C31 C 0.7984(3) 0.0620(2) 0.5944(2) 0.0183(5) Uani 1 1 d . . . . . H31 H 0.812198 0.094619 0.520203 0.022 Uiso 1 1 calc R U . . . C32 C 0.7149(3) 0.1316(2) 0.6867(2) 0.0146(5) Uani 1 1 d . . . . . C33 C 0.6940(3) 0.0809(2) 0.7950(2) 0.0146(5) Uani 1 1 d . . . . . C34 C 0.5932(3) 0.3813(2) 0.8795(2) 0.0206(5) Uani 1 1 d . . . . . H34A H 0.560665 0.457794 0.842876 0.031 Uiso 1 1 calc R U . . . H34B H 0.698507 0.361948 0.867780 0.031 Uiso 1 1 calc R U . . . H34C H 0.539726 0.386319 0.960480 0.031 Uiso 1 1 calc R U . . . C35 C 0.7470(3) 0.3368(2) 0.6381(2) 0.0222(6) Uani 1 1 d . . . . . H35A H 0.789885 0.316416 0.558015 0.033 Uiso 1 1 calc R U . . . H35B H 0.825094 0.318749 0.672538 0.033 Uiso 1 1 calc R U . . . H35C H 0.694100 0.421660 0.645602 0.033 Uiso 1 1 calc R U . . . O4 O 0.5748(2) 0.14251(19) 0.26067(18) 0.0246(4) Uani 1 1 d . . . . . O5 O 0.4948(2) 0.69669(17) 0.30359(15) 0.0188(4) Uani 1 1 d . . . . . O6 O 0.56745(19) 0.68224(16) 0.11097(15) 0.0171(4) Uani 1 1 d . . . . . B2 B 0.6079(3) 0.6697(3) 0.2057(2) 0.0168(6) Uani 1 1 d . . . . . C36 C 0.4884(3) 0.0968(3) 0.3601(3) 0.0300(7) Uani 1 1 d . . . . . H36A H 0.543584 0.070732 0.413786 0.045 Uiso 1 1 calc R U . . . H36B H 0.464559 0.029230 0.340740 0.045 Uiso 1 1 calc R U . . . H36C H 0.397724 0.159059 0.394145 0.045 Uiso 1 1 calc R U . . . C37 C 0.6230(3) 0.2349(2) 0.2721(2) 0.0188(5) Uani 1 1 d . . . . . C38 C 0.7034(3) 0.2789(3) 0.1721(2) 0.0237(6) Uani 1 1 d . . . . . H38 H 0.719928 0.244965 0.102289 0.028 Uiso 1 1 calc R U . . . C39 C 0.7596(3) 0.3714(3) 0.1735(2) 0.0232(6) Uani 1 1 d . . . . . H39 H 0.814457 0.400123 0.104504 0.028 Uiso 1 1 calc R U . . . C40 C 0.7367(3) 0.4231(2) 0.2749(2) 0.0168(5) Uani 1 1 d . . . . . C41 C 0.6527(3) 0.3804(3) 0.3732(2) 0.0206(5) Uani 1 1 d . . . . . H41 H 0.633381 0.415821 0.442878 0.025 Uiso 1 1 calc R U . . . C42 C 0.5957(3) 0.2872(3) 0.3730(2) 0.0207(6) Uani 1 1 d . . . . . H42 H 0.538567 0.259840 0.441700 0.025 Uiso 1 1 calc R U . . . C43 C 0.8049(3) 0.5195(2) 0.2813(2) 0.0167(5) Uani 1 1 d . . . . . H43 H 0.758003 0.551344 0.359625 0.020 Uiso 1 1 calc R U . . . C44 C 0.7745(3) 0.6263(2) 0.1996(2) 0.0166(5) Uani 1 1 d . . . . . H44 H 0.833831 0.598520 0.121134 0.020 Uiso 1 1 calc R U . . . C45 C 0.8232(3) 0.7286(2) 0.2220(2) 0.0193(5) Uani 1 1 d . . . . . C46 C 0.9251(3) 0.7727(3) 0.1373(3) 0.0266(6) Uani 1 1 d . . . . . H46 H 0.965755 0.737932 0.064770 0.032 Uiso 1 1 calc R U . . . C47 C 0.9685(4) 0.8673(3) 0.1573(3) 0.0376(8) Uani 1 1 d . . . . . H47 H 1.036748 0.897277 0.098143 0.045 Uiso 1 1 calc R U . . . C48 C 0.9124(4) 0.9174(3) 0.2632(3) 0.0365(8) Uani 1 1 d . . . . . H48 H 0.943095 0.980683 0.277527 0.044 Uiso 1 1 calc R U . . . C49 C 0.8112(4) 0.8743(3) 0.3478(3) 0.0320(7) Uani 1 1 d . . . . . H49 H 0.772078 0.908322 0.420646 0.038 Uiso 1 1 calc R U . . . C50 C 0.7662(3) 0.7816(3) 0.3271(3) 0.0249(6) Uani 1 1 d . . . . . H50 H 0.695247 0.753980 0.385775 0.030 Uiso 1 1 calc R U . . . C51 C 0.9681(3) 0.4669(2) 0.2649(2) 0.0165(5) Uani 1 1 d . . . . . C52 C 1.0185(3) 0.4415(2) 0.3574(2) 0.0187(5) Uani 1 1 d . . . . . H52 H 0.950997 0.458772 0.431110 0.022 Uiso 1 1 calc R U . . . C53 C 1.1670(3) 0.3911(2) 0.3431(3) 0.0229(6) Uani 1 1 d . . . . . H53 H 1.200080 0.374333 0.407203 0.027 Uiso 1 1 calc R U . . . C54 C 1.2669(3) 0.3652(2) 0.2366(3) 0.0238(6) Uani 1 1 d . . . . . H54 H 1.368323 0.331129 0.227251 0.029 Uiso 1 1 calc R U . . . C55 C 1.2182(3) 0.3892(2) 0.1432(2) 0.0211(6) Uani 1 1 d . . . . . H55 H 1.285908 0.370625 0.069684 0.025 Uiso 1 1 calc R U . . . C56 C 1.0707(3) 0.4401(2) 0.1575(2) 0.0180(5) Uani 1 1 d . . . . . H56 H 1.038302 0.457235 0.093112 0.022 Uiso 1 1 calc R U . . . C57 C 0.3578(3) 0.7328(2) 0.2778(2) 0.0156(5) Uani 1 1 d . . . . . C58 C 0.4083(3) 0.7232(2) 0.1441(2) 0.0149(5) Uani 1 1 d . . . . . C59 C 0.2813(3) 0.8640(2) 0.3005(2) 0.0157(5) Uani 1 1 d . . . . . C60 C 0.2130(3) 0.9262(3) 0.3986(2) 0.0203(6) Uani 1 1 d . . . . . H60 H 0.211262 0.887613 0.469428 0.024 Uiso 1 1 calc R U . . . C61 C 0.1443(3) 1.0503(3) 0.3918(2) 0.0234(6) Uani 1 1 d . . . . . H61 H 0.095629 1.094061 0.459686 0.028 Uiso 1 1 calc R U . . . C62 C 0.1459(3) 1.1091(2) 0.2912(3) 0.0220(6) Uani 1 1 d . . . . . H62 H 0.097198 1.191795 0.290448 0.026 Uiso 1 1 calc R U . . . C63 C 0.2201(3) 1.0468(2) 0.1879(2) 0.0188(5) Uani 1 1 d . . . . . C64 C 0.2337(3) 1.0928(2) 0.0769(3) 0.0231(6) Uani 1 1 d . . . . . H64 H 0.191017 1.174986 0.065637 0.028 Uiso 1 1 calc R U . . . C65 C 0.3079(3) 1.0200(3) -0.0144(2) 0.0245(6) Uani 1 1 d . . . . . H65 H 0.317858 1.053693 -0.087947 0.029 Uiso 1 1 calc R U . . . C66 C 0.3703(3) 0.8962(2) -0.0029(2) 0.0197(5) Uani 1 1 d . . . . . H66 H 0.419731 0.847123 -0.067354 0.024 Uiso 1 1 calc R U . . . C67 C 0.3573(3) 0.8492(2) 0.1035(2) 0.0153(5) Uani 1 1 d . . . . . C68 C 0.2848(3) 0.9244(2) 0.1970(2) 0.0152(5) Uani 1 1 d . . . . . C69 C 0.2639(3) 0.6545(3) 0.3455(2) 0.0246(6) Uani 1 1 d . . . . . H69A H 0.318150 0.570871 0.328491 0.037 Uiso 1 1 calc R U . . . H69B H 0.173535 0.674464 0.325569 0.037 Uiso 1 1 calc R U . . . H69C H 0.239440 0.667506 0.426245 0.037 Uiso 1 1 calc R U . . . C70 C 0.3580(3) 0.6360(2) 0.0979(2) 0.0209(5) Uani 1 1 d . . . . . H70A H 0.396725 0.636388 0.015371 0.031 Uiso 1 1 calc R U . . . H70B H 0.250652 0.659590 0.121753 0.031 Uiso 1 1 calc R U . . . H70C H 0.394180 0.555954 0.127008 0.031 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0332(11) 0.0344(11) 0.0219(10) 0.0041(8) -0.0085(9) -0.0199(9) O2 0.0115(9) 0.0184(9) 0.0160(8) -0.0007(7) -0.0042(7) -0.0003(7) O3 0.0134(9) 0.0190(9) 0.0147(8) 0.0000(7) -0.0048(7) -0.0015(7) B1 0.0154(14) 0.0119(12) 0.0171(13) 0.0005(10) -0.0026(11) -0.0044(11) C1 0.0310(16) 0.0289(15) 0.0331(16) 0.0021(12) -0.0118(13) -0.0162(13) C2 0.0205(13) 0.0256(14) 0.0258(13) 0.0064(11) -0.0144(11) -0.0095(11) C3 0.0249(14) 0.0296(15) 0.0187(13) 0.0020(11) -0.0065(11) -0.0099(12) C4 0.0218(13) 0.0210(13) 0.0184(12) 0.0011(10) -0.0078(11) -0.0061(11) C5 0.0155(12) 0.0166(12) 0.0199(12) 0.0005(10) -0.0105(10) -0.0016(10) C6 0.0203(13) 0.0286(15) 0.0226(13) -0.0060(11) -0.0015(11) -0.0089(12) C7 0.0250(14) 0.0236(14) 0.0286(14) -0.0065(11) -0.0093(12) -0.0083(12) C8 0.0142(12) 0.0168(12) 0.0129(11) -0.0010(9) -0.0044(9) -0.0024(10) C9 0.0143(12) 0.0158(12) 0.0133(11) -0.0003(9) -0.0046(9) -0.0016(10) C10 0.0111(11) 0.0130(12) 0.0240(13) 0.0016(10) -0.0094(10) 0.0016(9) C11 0.0311(16) 0.0286(15) 0.0250(14) 0.0010(11) -0.0143(12) -0.0090(13) C12 0.0424(19) 0.0345(17) 0.0438(18) 0.0044(14) -0.0282(16) -0.0193(15) C13 0.0227(15) 0.0289(15) 0.0470(18) 0.0108(13) -0.0196(14) -0.0122(12) C14 0.0179(13) 0.0260(14) 0.0330(15) 0.0046(12) -0.0039(12) -0.0056(11) C15 0.0220(13) 0.0194(13) 0.0244(14) -0.0015(10) -0.0049(11) -0.0037(11) C16 0.0153(12) 0.0091(11) 0.0183(12) -0.0005(9) -0.0063(10) -0.0021(9) C17 0.0182(12) 0.0134(12) 0.0181(12) -0.0035(9) -0.0049(10) -0.0010(10) C18 0.0269(15) 0.0146(12) 0.0283(14) -0.0040(10) -0.0166(12) -0.0015(11) C19 0.0157(13) 0.0143(12) 0.0462(17) -0.0037(12) -0.0165(13) -0.0013(10) C20 0.0135(13) 0.0174(13) 0.0360(16) -0.0026(11) -0.0030(12) -0.0050(10) C21 0.0202(14) 0.0155(12) 0.0211(13) 0.0000(10) -0.0044(11) -0.0053(10) C22 0.0107(12) 0.0145(12) 0.0176(12) 0.0003(9) -0.0046(9) -0.0025(9) C23 0.0109(11) 0.0156(12) 0.0170(12) -0.0010(9) -0.0040(10) -0.0026(10) C24 0.0114(11) 0.0126(12) 0.0188(12) 0.0001(9) -0.0064(10) -0.0033(9) C25 0.0149(12) 0.0185(12) 0.0180(12) -0.0017(10) -0.0058(10) -0.0051(10) C26 0.0242(14) 0.0230(14) 0.0230(13) 0.0075(11) -0.0115(11) -0.0087(11) C27 0.0215(13) 0.0167(12) 0.0271(14) 0.0046(10) -0.0124(11) -0.0062(11) C28 0.0149(12) 0.0127(12) 0.0268(14) 0.0005(10) -0.0102(11) -0.0052(10) C29 0.0170(12) 0.0127(12) 0.0307(14) -0.0046(10) -0.0097(11) -0.0017(10) C30 0.0165(12) 0.0182(13) 0.0266(13) -0.0097(10) -0.0047(10) -0.0025(10) C31 0.0143(12) 0.0225(13) 0.0178(12) -0.0047(10) -0.0030(10) -0.0054(10) C32 0.0110(11) 0.0154(12) 0.0193(12) -0.0009(9) -0.0057(10) -0.0052(9) C33 0.0130(11) 0.0144(12) 0.0200(13) -0.0016(10) -0.0077(10) -0.0057(10) C34 0.0236(13) 0.0169(12) 0.0230(13) -0.0041(10) -0.0075(11) -0.0066(11) C35 0.0177(13) 0.0196(13) 0.0272(14) 0.0019(10) -0.0034(11) -0.0074(11) O4 0.0207(10) 0.0259(10) 0.0297(10) -0.0020(8) -0.0068(8) -0.0108(8) O5 0.0158(9) 0.0234(9) 0.0158(9) 0.0003(7) -0.0066(7) -0.0022(7) O6 0.0128(9) 0.0192(9) 0.0173(9) -0.0026(7) -0.0052(7) -0.0006(7) B2 0.0181(14) 0.0157(13) 0.0164(13) -0.0008(10) -0.0054(11) -0.0046(11) C36 0.0240(15) 0.0272(15) 0.0382(17) 0.0039(13) -0.0072(13) -0.0111(12) C37 0.0113(11) 0.0223(13) 0.0231(13) -0.0001(10) -0.0075(10) -0.0031(10) C38 0.0203(13) 0.0352(16) 0.0184(13) -0.0068(11) -0.0039(11) -0.0118(12) C39 0.0200(14) 0.0333(15) 0.0165(12) -0.0028(11) -0.0014(11) -0.0119(12) C40 0.0102(11) 0.0203(12) 0.0173(12) -0.0016(10) -0.0055(10) 0.0009(10) C41 0.0198(12) 0.0244(14) 0.0154(12) -0.0029(10) -0.0058(10) -0.0020(11) C42 0.0191(13) 0.0233(13) 0.0179(12) 0.0042(10) -0.0056(10) -0.0055(11) C43 0.0167(13) 0.0180(12) 0.0135(11) -0.0032(9) -0.0048(10) -0.0015(10) C44 0.0139(12) 0.0200(13) 0.0128(11) 0.0000(9) -0.0051(9) 0.0001(10) C45 0.0119(12) 0.0204(13) 0.0242(13) 0.0018(10) -0.0093(10) 0.0005(10) C46 0.0174(13) 0.0277(15) 0.0318(15) 0.0063(12) -0.0092(12) -0.0033(11) C47 0.0206(15) 0.0335(17) 0.059(2) 0.0147(16) -0.0151(15) -0.0113(13) C48 0.0258(16) 0.0250(15) 0.066(2) -0.0040(15) -0.0221(16) -0.0076(13) C49 0.0269(15) 0.0279(16) 0.0457(18) -0.0100(13) -0.0182(14) -0.0033(12) C50 0.0206(14) 0.0259(14) 0.0284(15) -0.0032(11) -0.0088(12) -0.0049(12) C51 0.0165(12) 0.0124(11) 0.0212(12) -0.0026(9) -0.0065(10) -0.0038(10) C52 0.0243(14) 0.0130(11) 0.0212(12) -0.0029(9) -0.0103(11) -0.0042(10) C53 0.0254(14) 0.0156(12) 0.0347(15) 0.0008(11) -0.0191(12) -0.0057(11) C54 0.0151(12) 0.0140(12) 0.0441(17) -0.0028(11) -0.0118(12) -0.0032(10) C55 0.0169(13) 0.0140(12) 0.0298(15) -0.0032(10) -0.0030(11) -0.0048(10) C56 0.0187(13) 0.0153(12) 0.0201(13) -0.0023(9) -0.0064(10) -0.0040(10) C57 0.0133(12) 0.0161(12) 0.0174(12) 0.0001(9) -0.0043(10) -0.0050(10) C58 0.0115(12) 0.0165(12) 0.0171(12) -0.0019(9) -0.0056(9) -0.0028(9) C59 0.0100(11) 0.0184(13) 0.0207(13) -0.0001(10) -0.0050(10) -0.0067(10) C60 0.0165(12) 0.0255(14) 0.0193(13) -0.0020(10) -0.0027(10) -0.0091(11) C61 0.0200(13) 0.0234(14) 0.0251(14) -0.0107(11) -0.0015(11) -0.0063(11) C62 0.0160(13) 0.0170(13) 0.0334(15) -0.0058(11) -0.0052(11) -0.0060(10) C63 0.0150(12) 0.0160(12) 0.0281(14) -0.0023(10) -0.0071(11) -0.0070(10) C64 0.0254(14) 0.0149(12) 0.0314(15) 0.0024(11) -0.0113(12) -0.0074(11) C65 0.0266(15) 0.0229(14) 0.0247(14) 0.0063(11) -0.0107(12) -0.0079(12) C66 0.0196(13) 0.0202(13) 0.0190(13) -0.0019(10) -0.0060(10) -0.0050(11) C67 0.0099(11) 0.0171(12) 0.0208(12) -0.0012(10) -0.0055(10) -0.0057(10) C68 0.0116(12) 0.0171(12) 0.0194(12) -0.0002(10) -0.0047(10) -0.0079(10) C69 0.0264(14) 0.0238(14) 0.0226(13) 0.0043(11) -0.0036(11) -0.0122(12) C70 0.0226(13) 0.0160(12) 0.0273(14) -0.0038(10) -0.0106(11) -0.0060(11) _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 O1 C2 1.380(3) . ? O1 C1 1.421(4) . ? O2 B1 1.364(3) . ? O2 C22 1.461(3) . ? O3 B1 1.365(3) . ? O3 C23 1.454(3) . ? B1 C9 1.579(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C7 1.376(4) . ? C2 C3 1.383(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.388(4) . ? C4 H4 0.9500 . ? C5 C6 1.393(4) . ? C5 C8 1.533(4) . ? C6 C7 1.407(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C16 1.525(3) . ? C8 C9 1.556(3) . ? C8 H8 1.0000 . ? C9 C10 1.524(4) . ? C9 H9 1.0000 . ? C10 C11 1.387(4) . ? C10 C15 1.391(4) . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 C13 1.377(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.386(4) . ? C16 C17 1.400(4) . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.378(5) . ? C19 H19 0.9500 . ? C20 C21 1.391(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C34 1.516(3) . ? C22 C24 1.518(3) . ? C22 C23 1.588(3) . ? C23 C32 1.518(3) . ? C23 C35 1.519(3) . ? C24 C25 1.370(4) . ? C24 C33 1.407(4) . ? C25 C26 1.419(4) . ? C25 H25 0.9500 . ? C26 C27 1.374(4) . ? C26 H26 0.9500 . ? C27 C28 1.418(4) . ? C27 H27 0.9500 . ? C28 C33 1.407(4) . ? C28 C29 1.417(4) . ? C29 C30 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.418(4) . ? C30 H30 0.9500 . ? C31 C32 1.370(4) . ? C31 H31 0.9500 . ? C32 C33 1.399(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O4 C37 1.366(3) . ? O4 C36 1.422(4) . ? O5 B2 1.360(3) . ? O5 C57 1.452(3) . ? O6 B2 1.362(4) . ? O6 C58 1.455(3) . ? B2 C44 1.581(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.383(4) . ? C37 C38 1.392(4) . ? C38 C39 1.384(4) . ? C38 H38 0.9500 . ? C39 C40 1.397(4) . ? C39 H39 0.9500 . ? C40 C41 1.387(4) . ? C40 C43 1.526(4) . ? C41 C42 1.393(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C51 1.523(4) . ? C43 C44 1.555(3) . ? C43 H43 1.0000 . ? C44 C45 1.524(4) . ? C44 H44 1.0000 . ? C45 C50 1.390(4) . ? C45 C46 1.392(4) . ? C46 C47 1.396(5) . ? C46 H46 0.9500 . ? C47 C48 1.385(6) . ? C47 H47 0.9500 . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 C50 1.390(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C52 1.388(4) . ? C51 C56 1.401(4) . ? C52 C53 1.391(4) . ? C52 H52 0.9500 . ? C53 C54 1.382(4) . ? C53 H53 0.9500 . ? C54 C55 1.389(4) . ? C54 H54 0.9500 . ? C55 C56 1.382(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C59 1.517(4) . ? C57 C69 1.519(3) . ? C57 C58 1.593(3) . ? C58 C67 1.508(4) . ? C58 C70 1.523(3) . ? C59 C60 1.367(4) . ? C59 C68 1.406(4) . ? C60 C61 1.424(4) . ? C60 H60 0.9500 . ? C61 C62 1.370(4) . ? C61 H61 0.9500 . ? C62 C63 1.423(4) . ? C62 H62 0.9500 . ? C63 C68 1.401(4) . ? C63 C64 1.416(4) . ? C64 C65 1.370(4) . ? C64 H64 0.9500 . ? C65 C66 1.416(4) . ? C65 H65 0.9500 . ? C66 C67 1.369(4) . ? C66 H66 0.9500 . ? C67 C68 1.406(4) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 C1 117.9(2) . . ? B1 O2 C22 108.67(19) . . ? B1 O3 C23 108.5(2) . . ? O2 B1 O3 114.6(2) . . ? O2 B1 C9 123.2(2) . . ? O3 B1 C9 122.2(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 O1 125.0(3) . . ? C7 C2 C3 119.7(3) . . ? O1 C2 C3 115.3(3) . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 121.7(3) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 117.2(3) . . ? C4 C5 C8 123.1(2) . . ? C6 C5 C8 119.7(2) . . ? C5 C6 C7 121.6(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C2 C7 C6 119.6(3) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C16 C8 C5 110.7(2) . . ? C16 C8 C9 111.64(19) . . ? C5 C8 C9 112.7(2) . . ? C16 C8 H8 107.1 . . ? C5 C8 H8 107.1 . . ? C9 C8 H8 107.1 . . ? C10 C9 C8 112.8(2) . . ? C10 C9 B1 110.5(2) . . ? C8 C9 B1 110.2(2) . . ? C10 C9 H9 107.7 . . ? C8 C9 H9 107.7 . . ? B1 C9 H9 107.7 . . ? C11 C10 C15 117.7(3) . . ? C11 C10 C9 121.1(2) . . ? C15 C10 C9 121.2(2) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C10 C15 C14 121.2(3) . . ? C10 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C21 C16 C17 118.5(2) . . ? C21 C16 C8 120.4(2) . . ? C17 C16 C8 121.1(2) . . ? C18 C17 C16 120.1(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C20 C19 C18 119.9(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 119.7(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 121.2(3) . . ? C16 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? O2 C22 C34 107.8(2) . . ? O2 C22 C24 111.05(19) . . ? C34 C22 C24 113.2(2) . . ? O2 C22 C23 103.62(19) . . ? C34 C22 C23 116.5(2) . . ? C24 C22 C23 104.3(2) . . ? O3 C23 C32 110.7(2) . . ? O3 C23 C35 108.1(2) . . ? C32 C23 C35 112.6(2) . . ? O3 C23 C22 104.40(18) . . ? C32 C23 C22 104.6(2) . . ? C35 C23 C22 116.2(2) . . ? C25 C24 C33 119.3(2) . . ? C25 C24 C22 131.9(2) . . ? C33 C24 C22 108.7(2) . . ? C24 C25 C26 118.7(2) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C27 C26 C25 122.1(2) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C28 120.4(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C33 C28 C29 116.2(2) . . ? C33 C28 C27 116.4(2) . . ? C29 C28 C27 127.4(2) . . ? C30 C29 C28 120.3(2) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 122.2(2) . . ? C29 C30 H30 118.9 . . ? C31 C30 H30 118.9 . . ? C32 C31 C30 118.2(2) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C31 C32 C33 119.8(2) . . ? C31 C32 C23 131.4(2) . . ? C33 C32 C23 108.7(2) . . ? C32 C33 C28 123.3(2) . . ? C32 C33 C24 113.5(2) . . ? C28 C33 C24 123.1(2) . . ? C22 C34 H34A 109.5 . . ? C22 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C22 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C23 C35 H35A 109.5 . . ? C23 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C23 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 O4 C36 117.7(2) . . ? B2 O5 C57 108.8(2) . . ? B2 O6 C58 108.3(2) . . ? O5 B2 O6 115.0(2) . . ? O5 B2 C44 123.6(2) . . ? O6 B2 C44 121.4(2) . . ? O4 C36 H36A 109.5 . . ? O4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O4 C37 C42 125.2(3) . . ? O4 C37 C38 115.6(2) . . ? C42 C37 C38 119.2(3) . . ? C39 C38 C37 120.7(3) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 120.9(3) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 117.5(3) . . ? C41 C40 C43 119.7(2) . . ? C39 C40 C43 122.7(2) . . ? C40 C41 C42 122.2(3) . . ? C40 C41 H41 118.9 . . ? C42 C41 H41 118.9 . . ? C37 C42 C41 119.5(2) . . ? C37 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C51 C43 C40 110.7(2) . . ? C51 C43 C44 111.8(2) . . ? C40 C43 C44 113.3(2) . . ? C51 C43 H43 106.9 . . ? C40 C43 H43 106.9 . . ? C44 C43 H43 106.9 . . ? C45 C44 C43 111.4(2) . . ? C45 C44 B2 110.8(2) . . ? C43 C44 B2 111.6(2) . . ? C45 C44 H44 107.6 . . ? C43 C44 H44 107.6 . . ? B2 C44 H44 107.6 . . ? C50 C45 C46 117.9(3) . . ? C50 C45 C44 121.1(2) . . ? C46 C45 C44 121.0(3) . . ? C45 C46 C47 121.1(3) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C48 C47 C46 120.1(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 119.3(3) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C50 120.4(3) . . ? C48 C49 H49 119.8 . . ? C50 C49 H49 119.8 . . ? C49 C50 C45 121.2(3) . . ? C49 C50 H50 119.4 . . ? C45 C50 H50 119.4 . . ? C52 C51 C56 118.1(2) . . ? C52 C51 C43 120.3(2) . . ? C56 C51 C43 121.6(2) . . ? C51 C52 C53 120.6(3) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C53 C54 C55 119.6(3) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C56 C55 C54 119.8(3) . . ? C56 C55 H55 120.1 . . ? C54 C55 H55 120.1 . . ? C55 C56 C51 121.4(3) . . ? C55 C56 H56 119.3 . . ? C51 C56 H56 119.3 . . ? O5 C57 C59 110.9(2) . . ? O5 C57 C69 108.5(2) . . ? C59 C57 C69 112.6(2) . . ? O5 C57 C58 103.77(19) . . ? C59 C57 C58 104.4(2) . . ? C69 C57 C58 116.4(2) . . ? O6 C58 C67 110.5(2) . . ? O6 C58 C70 107.7(2) . . ? C67 C58 C70 113.1(2) . . ? O6 C58 C57 104.19(19) . . ? C67 C58 C57 104.5(2) . . ? C70 C58 C57 116.6(2) . . ? C60 C59 C68 119.4(2) . . ? C60 C59 C57 131.8(2) . . ? C68 C59 C57 108.8(2) . . ? C59 C60 C61 118.2(2) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? C62 C61 C60 122.5(2) . . ? C62 C61 H61 118.7 . . ? C60 C61 H61 118.7 . . ? C61 C62 C63 120.2(3) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C68 C63 C64 116.0(2) . . ? C68 C63 C62 116.1(3) . . ? C64 C63 C62 127.9(3) . . ? C65 C64 C63 120.7(3) . . ? C65 C64 H64 119.6 . . ? C63 C64 H64 119.6 . . ? C64 C65 C66 122.3(3) . . ? C64 C65 H65 118.9 . . ? C66 C65 H65 118.9 . . ? C67 C66 C65 118.2(2) . . ? C67 C66 H66 120.9 . . ? C65 C66 H66 120.9 . . ? C66 C67 C68 119.5(2) . . ? C66 C67 C58 131.3(2) . . ? C68 C67 C58 109.2(2) . . ? C63 C68 C59 123.6(2) . . ? C63 C68 C67 123.2(2) . . ? C59 C68 C67 113.2(2) . . ? C57 C69 H69A 109.5 . . ? C57 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C57 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C58 C70 H70A 109.5 . . ? C58 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C58 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 O2 B1 O3 3.8(3) . . . . ? C22 O2 B1 C9 -175.0(2) . . . . ? C23 O3 B1 O2 -1.0(3) . . . . ? C23 O3 B1 C9 177.7(2) . . . . ? C1 O1 C2 C7 7.0(4) . . . . ? C1 O1 C2 C3 -172.9(3) . . . . ? C7 C2 C3 C4 0.2(4) . . . . ? O1 C2 C3 C4 180.0(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C3 C4 C5 C8 176.3(3) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C8 C5 C6 C7 -176.0(3) . . . . ? O1 C2 C7 C6 -179.5(3) . . . . ? C3 C2 C7 C6 0.3(4) . . . . ? C5 C6 C7 C2 -0.8(4) . . . . ? C4 C5 C8 C16 -94.0(3) . . . . ? C6 C5 C8 C16 82.7(3) . . . . ? C4 C5 C8 C9 31.9(3) . . . . ? C6 C5 C8 C9 -151.5(2) . . . . ? C16 C8 C9 C10 -55.2(3) . . . . ? C5 C8 C9 C10 179.4(2) . . . . ? C16 C8 C9 B1 -179.3(2) . . . . ? C5 C8 C9 B1 55.3(3) . . . . ? O2 B1 C9 C10 -69.9(3) . . . . ? O3 B1 C9 C10 111.5(3) . . . . ? O2 B1 C9 C8 55.5(3) . . . . ? O3 B1 C9 C8 -123.1(2) . . . . ? C8 C9 C10 C11 131.5(3) . . . . ? B1 C9 C10 C11 -104.6(3) . . . . ? C8 C9 C10 C15 -50.6(3) . . . . ? B1 C9 C10 C15 73.3(3) . . . . ? C15 C10 C11 C12 -0.6(4) . . . . ? C9 C10 C11 C12 177.3(3) . . . . ? C10 C11 C12 C13 0.4(5) . . . . ? C11 C12 C13 C14 0.2(5) . . . . ? C12 C13 C14 C15 -0.6(5) . . . . ? C11 C10 C15 C14 0.1(4) . . . . ? C9 C10 C15 C14 -177.8(2) . . . . ? C13 C14 C15 C10 0.5(4) . . . . ? C5 C8 C16 C21 -114.2(3) . . . . ? C9 C8 C16 C21 119.3(2) . . . . ? C5 C8 C16 C17 64.5(3) . . . . ? C9 C8 C16 C17 -62.0(3) . . . . ? C21 C16 C17 C18 -0.1(4) . . . . ? C8 C16 C17 C18 -178.8(2) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C17 C16 C21 C20 0.4(4) . . . . ? C8 C16 C21 C20 179.1(2) . . . . ? C19 C20 C21 C16 -0.4(4) . . . . ? B1 O2 C22 C34 119.5(2) . . . . ? B1 O2 C22 C24 -116.0(2) . . . . ? B1 O2 C22 C23 -4.5(2) . . . . ? B1 O3 C23 C32 110.1(2) . . . . ? B1 O3 C23 C35 -126.2(2) . . . . ? B1 O3 C23 C22 -1.9(2) . . . . ? O2 C22 C23 O3 3.9(2) . . . . ? C34 C22 C23 O3 -114.3(2) . . . . ? C24 C22 C23 O3 120.2(2) . . . . ? O2 C22 C23 C32 -112.5(2) . . . . ? C34 C22 C23 C32 129.4(2) . . . . ? C24 C22 C23 C32 3.8(2) . . . . ? O2 C22 C23 C35 122.8(2) . . . . ? C34 C22 C23 C35 4.7(3) . . . . ? C24 C22 C23 C35 -120.9(2) . . . . ? O2 C22 C24 C25 -75.1(3) . . . . ? C34 C22 C24 C25 46.3(4) . . . . ? C23 C22 C24 C25 173.9(3) . . . . ? O2 C22 C24 C33 108.3(2) . . . . ? C34 C22 C24 C33 -130.3(2) . . . . ? C23 C22 C24 C33 -2.7(3) . . . . ? C33 C24 C25 C26 -0.6(4) . . . . ? C22 C24 C25 C26 -176.9(2) . . . . ? C24 C25 C26 C27 -0.1(4) . . . . ? C25 C26 C27 C28 1.0(4) . . . . ? C26 C27 C28 C33 -1.1(4) . . . . ? C26 C27 C28 C29 176.4(3) . . . . ? C33 C28 C29 C30 -0.9(4) . . . . ? C27 C28 C29 C30 -178.4(3) . . . . ? C28 C29 C30 C31 1.3(4) . . . . ? C29 C30 C31 C32 -0.2(4) . . . . ? C30 C31 C32 C33 -1.2(4) . . . . ? C30 C31 C32 C23 174.4(2) . . . . ? O3 C23 C32 C31 68.4(3) . . . . ? C35 C23 C32 C31 -52.7(4) . . . . ? C22 C23 C32 C31 -179.7(3) . . . . ? O3 C23 C32 C33 -115.6(2) . . . . ? C35 C23 C32 C33 123.2(2) . . . . ? C22 C23 C32 C33 -3.7(3) . . . . ? C31 C32 C33 C28 1.6(4) . . . . ? C23 C32 C33 C28 -174.9(2) . . . . ? C31 C32 C33 C24 178.7(2) . . . . ? C23 C32 C33 C24 2.2(3) . . . . ? C29 C28 C33 C32 -0.6(4) . . . . ? C27 C28 C33 C32 177.2(2) . . . . ? C29 C28 C33 C24 -177.4(2) . . . . ? C27 C28 C33 C24 0.4(4) . . . . ? C25 C24 C33 C32 -176.6(2) . . . . ? C22 C24 C33 C32 0.4(3) . . . . ? C25 C24 C33 C28 0.5(4) . . . . ? C22 C24 C33 C28 177.5(2) . . . . ? C57 O5 B2 O6 -0.1(3) . . . . ? C57 O5 B2 C44 -179.8(2) . . . . ? C58 O6 B2 O5 0.3(3) . . . . ? C58 O6 B2 C44 -180.0(2) . . . . ? C36 O4 C37 C42 0.6(4) . . . . ? C36 O4 C37 C38 -178.2(3) . . . . ? O4 C37 C38 C39 -179.1(3) . . . . ? C42 C37 C38 C39 2.0(4) . . . . ? C37 C38 C39 C40 -0.2(4) . . . . ? C38 C39 C40 C41 -1.7(4) . . . . ? C38 C39 C40 C43 175.8(3) . . . . ? C39 C40 C41 C42 1.8(4) . . . . ? C43 C40 C41 C42 -175.8(2) . . . . ? O4 C37 C42 C41 179.4(3) . . . . ? C38 C37 C42 C41 -1.9(4) . . . . ? C40 C41 C42 C37 0.0(4) . . . . ? C41 C40 C43 C51 103.6(3) . . . . ? C39 C40 C43 C51 -73.9(3) . . . . ? C41 C40 C43 C44 -129.9(3) . . . . ? C39 C40 C43 C44 52.7(3) . . . . ? C51 C43 C44 C45 -63.1(3) . . . . ? C40 C43 C44 C45 170.9(2) . . . . ? C51 C43 C44 B2 172.5(2) . . . . ? C40 C43 C44 B2 46.5(3) . . . . ? O5 B2 C44 C45 -72.9(3) . . . . ? O6 B2 C44 C45 107.5(3) . . . . ? O5 B2 C44 C43 51.9(3) . . . . ? O6 B2 C44 C43 -127.7(3) . . . . ? C43 C44 C45 C50 -58.4(3) . . . . ? B2 C44 C45 C50 66.4(3) . . . . ? C43 C44 C45 C46 122.2(3) . . . . ? B2 C44 C45 C46 -113.0(3) . . . . ? C50 C45 C46 C47 -0.1(4) . . . . ? C44 C45 C46 C47 179.3(3) . . . . ? C45 C46 C47 C48 1.3(5) . . . . ? C46 C47 C48 C49 -1.2(5) . . . . ? C47 C48 C49 C50 0.1(5) . . . . ? C48 C49 C50 C45 1.1(5) . . . . ? C46 C45 C50 C49 -1.1(4) . . . . ? C44 C45 C50 C49 179.5(3) . . . . ? C40 C43 C51 C52 -99.2(3) . . . . ? C44 C43 C51 C52 133.4(2) . . . . ? C40 C43 C51 C56 79.3(3) . . . . ? C44 C43 C51 C56 -48.1(3) . . . . ? C56 C51 C52 C53 0.1(4) . . . . ? C43 C51 C52 C53 178.6(2) . . . . ? C51 C52 C53 C54 -0.1(4) . . . . ? C52 C53 C54 C55 -0.4(4) . . . . ? C53 C54 C55 C56 0.8(4) . . . . ? C54 C55 C56 C51 -0.9(4) . . . . ? C52 C51 C56 C55 0.4(4) . . . . ? C43 C51 C56 C55 -178.1(2) . . . . ? B2 O5 C57 C59 -111.6(2) . . . . ? B2 O5 C57 C69 124.3(2) . . . . ? B2 O5 C57 C58 -0.1(3) . . . . ? B2 O6 C58 C67 111.3(2) . . . . ? B2 O6 C58 C70 -124.7(2) . . . . ? B2 O6 C58 C57 -0.4(3) . . . . ? O5 C57 C58 O6 0.3(2) . . . . ? C59 C57 C58 O6 116.5(2) . . . . ? C69 C57 C58 O6 -118.8(2) . . . . ? O5 C57 C58 C67 -115.7(2) . . . . ? C59 C57 C58 C67 0.5(2) . . . . ? C69 C57 C58 C67 125.2(2) . . . . ? O5 C57 C58 C70 118.7(2) . . . . ? C59 C57 C58 C70 -125.1(2) . . . . ? C69 C57 C58 C70 -0.3(3) . . . . ? O5 C57 C59 C60 -70.2(3) . . . . ? C69 C57 C59 C60 51.5(4) . . . . ? C58 C57 C59 C60 178.6(3) . . . . ? O5 C57 C59 C68 111.2(2) . . . . ? C69 C57 C59 C68 -127.1(2) . . . . ? C58 C57 C59 C68 0.0(3) . . . . ? C68 C59 C60 C61 1.5(4) . . . . ? C57 C59 C60 C61 -177.0(2) . . . . ? C59 C60 C61 C62 -0.7(4) . . . . ? C60 C61 C62 C63 -1.1(4) . . . . ? C61 C62 C63 C68 2.0(4) . . . . ? C61 C62 C63 C64 -179.6(3) . . . . ? C68 C63 C64 C65 -0.7(4) . . . . ? C62 C63 C64 C65 -179.2(3) . . . . ? C63 C64 C65 C66 1.9(4) . . . . ? C64 C65 C66 C67 -1.1(4) . . . . ? C65 C66 C67 C68 -0.7(4) . . . . ? C65 C66 C67 C58 178.9(2) . . . . ? O6 C58 C67 C66 68.0(3) . . . . ? C70 C58 C67 C66 -52.8(4) . . . . ? C57 C58 C67 C66 179.5(3) . . . . ? O6 C58 C67 C68 -112.4(2) . . . . ? C70 C58 C67 C68 126.8(2) . . . . ? C57 C58 C67 C68 -0.9(3) . . . . ? C64 C63 C68 C59 -179.8(2) . . . . ? C62 C63 C68 C59 -1.2(4) . . . . ? C64 C63 C68 C67 -1.1(4) . . . . ? C62 C63 C68 C67 177.5(2) . . . . ? C60 C59 C68 C63 -0.6(4) . . . . ? C57 C59 C68 C63 178.2(2) . . . . ? C60 C59 C68 C67 -179.4(2) . . . . ? C57 C59 C68 C67 -0.6(3) . . . . ? C66 C67 C68 C63 1.8(4) . . . . ? C58 C67 C68 C63 -177.9(2) . . . . ? C66 C67 C68 C59 -179.4(2) . . . . ? C58 C67 C68 C59 1.0(3) . . . . ? _refine_diff_density_max 0.242 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.043 _shelx_res_file ; TITL sad_a.res in P1 sad_a.res created by SHELXL-2016/6 at 13:50:23 on 11-Jan-2018 REM Old TITL sad in P1 REM SHELXT solution in P1 REM R1 0.088, Rweak 0.030, Alpha 0.000, Orientation as input REM Flack x = -0.029 ( 0.107 ) from Parsons' quotients REM Formula found by SHELXT: C72 O6 CELL 1.54178 10.1118 11.8308 12.5795 83.377 70.474 72.023 ZERR 2.000 0.0003 0.0004 0.0004 0.001 0.001 0.001 LATT -1 SFAC C H B O UNIT 70 62 2 6 L.S. 10 BOND $H FMAP 2 PLAN 20 SIZE 0.60 0.56 0.48 TEMP -173 CONF ACTA WGHT 0.088500 0.229200 FVAR 1.44872 O1 4 0.467159 0.850686 0.601790 11.00000 0.03315 0.03444 = 0.02193 0.00410 -0.00849 -0.01988 O2 4 0.407378 0.321458 0.840652 11.00000 0.01147 0.01840 = 0.01603 -0.00072 -0.00417 -0.00030 O3 4 0.521533 0.299482 0.649762 11.00000 0.01342 0.01895 = 0.01469 0.00003 -0.00481 -0.00145 B1 3 0.392555 0.331571 0.735853 11.00000 0.01536 0.01188 = 0.01714 0.00050 -0.00257 -0.00438 C1 1 0.457965 0.939469 0.673096 11.00000 0.03105 0.02889 = 0.03308 0.00213 -0.01185 -0.01620 AFIX 137 H1A 2 0.356376 0.989585 0.700673 11.00000 -1.50000 H1B 2 0.521115 0.988560 0.630532 11.00000 -1.50000 H1C 2 0.490061 0.901513 0.737278 11.00000 -1.50000 AFIX 0 C2 1 0.389342 0.769849 0.648261 11.00000 0.02052 0.02564 = 0.02581 0.00639 -0.01439 -0.00951 C3 1 0.415470 0.677590 0.578825 11.00000 0.02493 0.02961 = 0.01867 0.00199 -0.00650 -0.00995 AFIX 43 H3 2 0.483166 0.673350 0.504755 11.00000 -1.20000 AFIX 0 C4 1 0.342920 0.590990 0.617125 11.00000 0.02177 0.02103 = 0.01841 0.00111 -0.00779 -0.00610 AFIX 43 H4 2 0.361987 0.528265 0.568317 11.00000 -1.20000 AFIX 0 C5 1 0.243386 0.593769 0.724774 11.00000 0.01551 0.01655 = 0.01992 0.00050 -0.01048 -0.00160 C6 1 0.219509 0.686905 0.793644 11.00000 0.02027 0.02855 = 0.02256 -0.00604 -0.00150 -0.00893 AFIX 43 H6 2 0.152990 0.690738 0.868151 11.00000 -1.20000 AFIX 0 C7 1 0.291509 0.775452 0.755553 11.00000 0.02504 0.02360 = 0.02856 -0.00648 -0.00931 -0.00833 AFIX 43 H7 2 0.272679 0.838749 0.803644 11.00000 -1.20000 AFIX 0 C8 1 0.155013 0.503925 0.767213 11.00000 0.01416 0.01677 = 0.01289 -0.00104 -0.00438 -0.00235 AFIX 13 H8 2 0.137185 0.494277 0.850415 11.00000 -1.20000 AFIX 0 C9 1 0.239412 0.379037 0.714481 11.00000 0.01432 0.01582 = 0.01332 -0.00030 -0.00459 -0.00163 AFIX 13 H9 2 0.258481 0.387957 0.631113 11.00000 -1.20000 AFIX 0 C10 1 0.152367 0.289201 0.757547 11.00000 0.01112 0.01296 = 0.02398 0.00155 -0.00941 0.00158 C11 1 0.138167 0.218717 0.683564 11.00000 0.03110 0.02864 = 0.02501 0.00103 -0.01426 -0.00900 AFIX 43 H11 2 0.179881 0.228921 0.604618 11.00000 -1.20000 AFIX 0 C12 1 0.063925 0.133432 0.723036 11.00000 0.04244 0.03454 = 0.04377 0.00443 -0.02817 -0.01932 AFIX 43 H12 2 0.056077 0.085717 0.670923 11.00000 -1.20000 AFIX 0 C13 1 0.001618 0.117486 0.837074 11.00000 0.02269 0.02888 = 0.04703 0.01076 -0.01965 -0.01220 AFIX 43 H13 2 -0.048855 0.058971 0.863814 11.00000 -1.20000 AFIX 0 C14 1 0.013333 0.187431 0.912008 11.00000 0.01788 0.02598 = 0.03295 0.00465 -0.00387 -0.00563 AFIX 43 H14 2 -0.030074 0.177675 0.990802 11.00000 -1.20000 AFIX 0 C15 1 0.088618 0.272303 0.872458 11.00000 0.02197 0.01943 = 0.02439 -0.00154 -0.00491 -0.00374 AFIX 43 H15 2 0.096594 0.319532 0.924908 11.00000 -1.20000 AFIX 0 C16 1 0.005553 0.551892 0.749376 11.00000 0.01529 0.00914 = 0.01833 -0.00054 -0.00629 -0.00214 C17 1 -0.006845 0.573456 0.640807 11.00000 0.01818 0.01336 = 0.01814 -0.00352 -0.00485 -0.00098 AFIX 43 H17 2 0.078733 0.556724 0.576733 11.00000 -1.20000 AFIX 0 C18 1 -0.143883 0.619217 0.626630 11.00000 0.02692 0.01459 = 0.02826 -0.00396 -0.01661 -0.00151 AFIX 43 H18 2 -0.151609 0.633795 0.552764 11.00000 -1.20000 AFIX 0 C19 1 -0.269438 0.643793 0.719292 11.00000 0.01574 0.01432 = 0.04618 -0.00374 -0.01652 -0.00125 AFIX 43 H19 2 -0.362917 0.675024 0.708946 11.00000 -1.20000 AFIX 0 C20 1 -0.258636 0.622889 0.826579 11.00000 0.01355 0.01738 = 0.03598 -0.00260 -0.00299 -0.00500 AFIX 43 H20 2 -0.344593 0.639422 0.890356 11.00000 -1.20000 AFIX 0 C21 1 -0.121423 0.577501 0.841114 11.00000 0.02024 0.01545 = 0.02111 0.00000 -0.00438 -0.00533 AFIX 43 H21 2 -0.114570 0.563791 0.915262 11.00000 -1.20000 AFIX 0 C22 1 0.563406 0.285177 0.828812 11.00000 0.01070 0.01451 = 0.01757 0.00030 -0.00456 -0.00249 C23 1 0.641419 0.264612 0.697224 11.00000 0.01092 0.01556 = 0.01698 -0.00097 -0.00401 -0.00256 C24 1 0.608534 0.163276 0.881680 11.00000 0.01141 0.01261 = 0.01880 0.00014 -0.00644 -0.00334 C25 1 0.586321 0.125952 0.991812 11.00000 0.01495 0.01845 = 0.01795 -0.00168 -0.00575 -0.00507 AFIX 43 H25 2 0.529846 0.180272 1.051592 11.00000 -1.20000 AFIX 0 C26 1 0.649270 0.004616 1.014897 11.00000 0.02424 0.02304 = 0.02304 0.00751 -0.01151 -0.00874 AFIX 43 H26 2 0.634148 -0.021549 1.091173 11.00000 -1.20000 AFIX 0 C27 1 0.731389 -0.076219 0.930437 11.00000 0.02148 0.01673 = 0.02715 0.00464 -0.01236 -0.00620 AFIX 43 H27 2 0.770631 -0.157031 0.949027 11.00000 -1.20000 AFIX 0 C28 1 0.757940 -0.039759 0.815653 11.00000 0.01487 0.01272 = 0.02681 0.00050 -0.01016 -0.00518 C29 1 0.845978 -0.110017 0.719284 11.00000 0.01701 0.01272 = 0.03071 -0.00456 -0.00968 -0.00166 AFIX 43 H29 2 0.893055 -0.191847 0.728173 11.00000 -1.20000 AFIX 0 C30 1 0.863674 -0.060108 0.612503 11.00000 0.01648 0.01817 = 0.02656 -0.00965 -0.00475 -0.00247 AFIX 43 H30 2 0.921546 -0.109236 0.549033 11.00000 -1.20000 AFIX 0 C31 1 0.798391 0.061979 0.594385 11.00000 0.01427 0.02250 = 0.01784 -0.00473 -0.00302 -0.00543 AFIX 43 H31 2 0.812198 0.094619 0.520203 11.00000 -1.20000 AFIX 0 C32 1 0.714854 0.131628 0.686735 11.00000 0.01104 0.01537 = 0.01932 -0.00094 -0.00575 -0.00524 C33 1 0.693960 0.080900 0.794988 11.00000 0.01303 0.01439 = 0.02003 -0.00157 -0.00765 -0.00570 C34 1 0.593209 0.381303 0.879462 11.00000 0.02357 0.01689 = 0.02300 -0.00411 -0.00746 -0.00662 AFIX 137 H34A 2 0.560665 0.457794 0.842876 11.00000 -1.50000 H34B 2 0.698507 0.361948 0.867780 11.00000 -1.50000 H34C 2 0.539726 0.386319 0.960480 11.00000 -1.50000 AFIX 0 C35 1 0.746986 0.336757 0.638102 11.00000 0.01769 0.01963 = 0.02723 0.00186 -0.00343 -0.00738 AFIX 137 H35A 2 0.789885 0.316416 0.558015 11.00000 -1.50000 H35B 2 0.825094 0.318749 0.672538 11.00000 -1.50000 H35C 2 0.694100 0.421660 0.645602 11.00000 -1.50000 AFIX 0 O4 4 0.574760 0.142505 0.260673 11.00000 0.02066 0.02590 = 0.02966 -0.00196 -0.00685 -0.01081 O5 4 0.494820 0.696686 0.303593 11.00000 0.01583 0.02339 = 0.01582 0.00027 -0.00657 -0.00220 O6 4 0.567446 0.682243 0.110969 11.00000 0.01281 0.01917 = 0.01729 -0.00256 -0.00518 -0.00064 B2 3 0.607850 0.669743 0.205686 11.00000 0.01814 0.01570 = 0.01642 -0.00075 -0.00540 -0.00459 C36 1 0.488447 0.096831 0.360062 11.00000 0.02403 0.02721 = 0.03824 0.00393 -0.00718 -0.01110 AFIX 137 H36A 2 0.543584 0.070732 0.413786 11.00000 -1.50000 H36B 2 0.464559 0.029230 0.340740 11.00000 -1.50000 H36C 2 0.397724 0.159059 0.394145 11.00000 -1.50000 AFIX 0 C37 1 0.622996 0.234905 0.272068 11.00000 0.01133 0.02225 = 0.02308 -0.00013 -0.00748 -0.00314 C38 1 0.703429 0.278853 0.172133 11.00000 0.02034 0.03516 = 0.01836 -0.00683 -0.00385 -0.01180 AFIX 43 H38 2 0.719928 0.244965 0.102289 11.00000 -1.20000 AFIX 0 C39 1 0.759608 0.371403 0.173476 11.00000 0.01997 0.03327 = 0.01649 -0.00281 -0.00144 -0.01187 AFIX 43 H39 2 0.814457 0.400123 0.104504 11.00000 -1.20000 AFIX 0 C40 1 0.736706 0.423105 0.274898 11.00000 0.01016 0.02027 = 0.01730 -0.00157 -0.00552 0.00090 C41 1 0.652684 0.380376 0.373183 11.00000 0.01977 0.02435 = 0.01536 -0.00292 -0.00576 -0.00204 AFIX 43 H41 2 0.633381 0.415821 0.442878 11.00000 -1.20000 AFIX 0 C42 1 0.595712 0.287231 0.373028 11.00000 0.01908 0.02334 = 0.01786 0.00421 -0.00561 -0.00555 AFIX 43 H42 2 0.538567 0.259840 0.441700 11.00000 -1.20000 AFIX 0 C43 1 0.804903 0.519527 0.281318 11.00000 0.01675 0.01796 = 0.01354 -0.00324 -0.00480 -0.00154 AFIX 13 H43 2 0.758003 0.551344 0.359625 11.00000 -1.20000 AFIX 0 C44 1 0.774549 0.626321 0.199626 11.00000 0.01390 0.02004 = 0.01279 -0.00003 -0.00506 0.00012 AFIX 13 H44 2 0.833831 0.598520 0.121134 11.00000 -1.20000 AFIX 0 C45 1 0.823162 0.728619 0.221955 11.00000 0.01187 0.02041 = 0.02424 0.00177 -0.00933 0.00048 C46 1 0.925104 0.772733 0.137304 11.00000 0.01744 0.02771 = 0.03184 0.00629 -0.00916 -0.00330 AFIX 43 H46 2 0.965755 0.737932 0.064770 11.00000 -1.20000 AFIX 0 C47 1 0.968542 0.867269 0.157293 11.00000 0.02062 0.03352 = 0.05920 0.01471 -0.01514 -0.01129 AFIX 43 H47 2 1.036748 0.897277 0.098143 11.00000 -1.20000 AFIX 0 C48 1 0.912358 0.917364 0.263206 11.00000 0.02578 0.02501 = 0.06573 -0.00399 -0.02207 -0.00762 AFIX 43 H48 2 0.943095 0.980683 0.277527 11.00000 -1.20000 AFIX 0 C49 1 0.811186 0.874330 0.347796 11.00000 0.02691 0.02786 = 0.04566 -0.01001 -0.01820 -0.00332 AFIX 43 H49 2 0.772078 0.908322 0.420646 11.00000 -1.20000 AFIX 0 C50 1 0.766215 0.781633 0.327052 11.00000 0.02059 0.02592 = 0.02838 -0.00320 -0.00877 -0.00489 AFIX 43 H50 2 0.695247 0.753980 0.385775 11.00000 -1.20000 AFIX 0 C51 1 0.968056 0.466893 0.264862 11.00000 0.01654 0.01243 = 0.02115 -0.00258 -0.00651 -0.00380 C52 1 1.018522 0.441526 0.357374 11.00000 0.02435 0.01295 = 0.02119 -0.00288 -0.01032 -0.00418 AFIX 43 H52 2 0.950997 0.458772 0.431110 11.00000 -1.20000 AFIX 0 C53 1 1.167048 0.391087 0.343141 11.00000 0.02543 0.01558 = 0.03472 0.00079 -0.01907 -0.00569 AFIX 43 H53 2 1.200080 0.374333 0.407203 11.00000 -1.20000 AFIX 0 C54 1 1.266947 0.365151 0.236555 11.00000 0.01512 0.01402 = 0.04408 -0.00283 -0.01184 -0.00320 AFIX 43 H54 2 1.368323 0.331129 0.227251 11.00000 -1.20000 AFIX 0 C55 1 1.218152 0.389150 0.143161 11.00000 0.01695 0.01402 = 0.02981 -0.00320 -0.00304 -0.00477 AFIX 43 H55 2 1.285908 0.370625 0.069684 11.00000 -1.20000 AFIX 0 C56 1 1.070716 0.440066 0.157471 11.00000 0.01873 0.01529 = 0.02008 -0.00226 -0.00639 -0.00402 AFIX 43 H56 2 1.038302 0.457235 0.093112 11.00000 -1.20000 AFIX 0 C57 1 0.357821 0.732829 0.277818 11.00000 0.01333 0.01614 = 0.01745 0.00005 -0.00428 -0.00503 C58 1 0.408281 0.723207 0.144086 11.00000 0.01153 0.01650 = 0.01709 -0.00192 -0.00556 -0.00276 C59 1 0.281347 0.864040 0.300482 11.00000 0.00996 0.01837 = 0.02074 -0.00012 -0.00501 -0.00669 C60 1 0.212966 0.926177 0.398629 11.00000 0.01649 0.02553 = 0.01931 -0.00203 -0.00273 -0.00914 AFIX 43 H60 2 0.211262 0.887613 0.469428 11.00000 -1.20000 AFIX 0 C61 1 0.144342 1.050327 0.391827 11.00000 0.02002 0.02338 = 0.02506 -0.01069 -0.00151 -0.00631 AFIX 43 H61 2 0.095629 1.094061 0.459686 11.00000 -1.20000 AFIX 0 C62 1 0.145853 1.109136 0.291219 11.00000 0.01600 0.01696 = 0.03336 -0.00581 -0.00520 -0.00603 AFIX 43 H62 2 0.097198 1.191795 0.290448 11.00000 -1.20000 AFIX 0 C63 1 0.220076 1.046795 0.187855 11.00000 0.01498 0.01596 = 0.02806 -0.00229 -0.00706 -0.00698 C64 1 0.233745 1.092771 0.076887 11.00000 0.02537 0.01491 = 0.03137 0.00236 -0.01129 -0.00736 AFIX 43 H64 2 0.191017 1.174986 0.065637 11.00000 -1.20000 AFIX 0 C65 1 0.307919 1.019968 -0.014410 11.00000 0.02659 0.02291 = 0.02472 0.00635 -0.01070 -0.00789 AFIX 43 H65 2 0.317858 1.053693 -0.087947 11.00000 -1.20000 AFIX 0 C66 1 0.370257 0.896227 -0.002943 11.00000 0.01962 0.02022 = 0.01899 -0.00188 -0.00601 -0.00505 AFIX 43 H66 2 0.419731 0.847123 -0.067354 11.00000 -1.20000 AFIX 0 C67 1 0.357336 0.849211 0.103472 11.00000 0.00990 0.01713 = 0.02082 -0.00124 -0.00547 -0.00566 C68 1 0.284760 0.924446 0.197047 11.00000 0.01164 0.01715 = 0.01941 -0.00015 -0.00467 -0.00792 C69 1 0.263904 0.654465 0.345539 11.00000 0.02637 0.02382 = 0.02261 0.00427 -0.00365 -0.01217 AFIX 137 H69A 2 0.318150 0.570871 0.328491 11.00000 -1.50000 H69B 2 0.173535 0.674464 0.325569 11.00000 -1.50000 H69C 2 0.239440 0.667506 0.426245 11.00000 -1.50000 AFIX 0 C70 1 0.357976 0.636014 0.097942 11.00000 0.02264 0.01603 = 0.02728 -0.00383 -0.01062 -0.00601 AFIX 137 H70A 2 0.396725 0.636388 0.015371 11.00000 -1.50000 H70B 2 0.250652 0.659590 0.121753 11.00000 -1.50000 H70C 2 0.394180 0.555954 0.127008 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in P1 REM R1 = 0.0449 for 9021 Fo > 4sig(Fo) and 0.0450 for all 9064 data REM 709 parameters refined using 3 restraints END WGHT 0.0889 0.2261 REM Highest difference peak 0.242, deepest hole -0.207, 1-sigma level 0.043 Q1 1 0.6156 0.2838 0.7666 11.00000 0.05 0.24 Q2 1 0.3040 0.6989 0.3094 11.00000 0.05 0.22 Q3 1 0.6931 0.3024 0.6767 11.00000 0.05 0.20 Q4 1 1.0165 0.4637 0.2130 11.00000 0.05 0.19 Q5 1 0.3643 0.7198 0.2120 11.00000 0.05 0.19 Q6 1 0.0929 0.7632 0.3276 11.00000 0.05 0.19 Q7 1 0.3950 0.8690 0.7048 11.00000 0.05 0.18 Q8 1 0.3799 0.6838 0.1234 11.00000 0.05 0.18 Q9 1 0.3850 0.7021 0.6419 11.00000 0.05 0.18 Q10 1 0.2801 0.8820 0.1562 11.00000 0.05 0.17 Q11 1 0.0648 0.3110 0.8206 11.00000 0.05 0.17 Q12 1 0.3559 0.6378 0.6186 11.00000 0.05 0.17 Q13 1 0.2029 0.4384 0.7360 11.00000 0.05 0.17 Q14 1 0.3046 0.5955 0.6643 11.00000 0.05 0.17 Q15 1 0.0011 0.1776 0.8540 11.00000 0.05 0.17 Q16 1 0.6234 0.2230 0.6701 11.00000 0.05 0.16 Q17 1 0.5982 0.3125 0.8547 11.00000 0.05 0.16 Q18 1 -0.0670 0.5367 0.8017 11.00000 0.05 0.16 Q19 1 0.6987 0.0396 0.8024 11.00000 0.05 0.16 Q20 1 0.2470 0.8986 0.2333 11.00000 0.05 0.16 ; _shelx_res_checksum 4468 _shelx_hkl_file ; -3 0 0 10.00 3.50 -3 0 0 9.20 4.80 -3 0 0 10.70 4.50 3 0 0 15.20 3.00 3 0 0 12.80 2.90 3 0 0 15.20 4.00 -4 0 0 630.64 47.60 -4 0 0 534.35 42.80 -4 0 0 535.05 39.20 -4 0 0 591.54 39.50 4 0 0 675.23 41.80 4 0 0 601.04 39.00 4 0 0 695.13 43.10 4 0 0 598.14 43.00 -5 0 0 1877.71 99.19 -5 0 0 1814.72 110.79 -5 0 0 1829.22 117.79 5 0 0 1911.21 114.19 5 0 0 2095.09 118.49 5 0 0 1890.61 115.79 -6 0 0 406.66 40.40 -6 0 0 334.07 22.00 -6 0 0 408.26 35.30 6 0 0 378.96 33.20 6 0 0 392.66 32.00 -7 0 0 170.38 26.80 -7 0 0 159.98 9.20 -7 0 0 149.88 21.80 -7 0 0 172.68 11.50 7 0 0 142.69 18.50 -8 0 0 786.52 42.70 -8 0 0 804.22 45.40 8 0 0 937.51 51.89 8 0 0 989.00 51.79 8 0 0 1025.70 52.39 8 0 0 916.21 51.99 8 0 0 1012.70 52.69 8 0 0 944.81 51.89 -9 0 0 188.78 13.20 -9 0 0 185.88 10.20 -9 0 0 188.88 10.60 9 0 0 236.88 12.70 9 0 0 215.38 12.90 9 0 0 222.58 12.50 9 0 0 223.68 13.20 9 0 0 221.38 12.50 9 0 0 239.48 12.50 -10 0 0 10.70 0.90 -10 0 0 10.20 1.30 10 0 0 14.70 1.30 10 0 0 12.90 1.60 10 0 0 13.10 1.40 10 0 0 12.00 1.70 10 -1 0 203.48 10.70 10 -1 0 182.08 10.70 10 -1 0 200.78 11.00 10 -1 0 195.08 10.80 -10 1 0 161.78 8.70 -10 1 0 160.38 9.00 9 -1 0 79.09 5.30 9 -1 0 78.09 5.00 9 -1 0 88.49 4.90 9 -1 0 85.99 4.90 -9 1 0 70.79 3.90 -9 1 0 68.69 4.30 -9 1 0 62.79 6.20 8 -1 0 40.50 3.30 8 -1 0 49.50 3.00 8 -1 0 39.70 3.00 8 -1 0 42.00 2.80 8 -1 0 44.60 3.60 -8 1 0 35.20 2.60 -8 1 0 36.70 4.60 7 -1 0 56.99 12.30 -7 1 0 50.49 5.10 -7 1 0 47.70 12.90 -7 1 0 48.80 3.20 -7 1 0 49.99 15.50 6 -1 0 130.19 16.80 -6 1 0 119.09 8.10 -6 1 0 114.29 21.30 -6 1 0 108.19 17.00 5 -1 0 456.55 35.00 5 -1 0 463.35 34.80 -5 1 0 415.06 34.70 -5 1 0 440.16 40.10 -5 1 0 422.16 23.90 4 -1 0 143.19 14.50 4 -1 0 155.08 15.20 -4 1 0 132.59 17.70 -4 1 0 153.68 15.90 -4 1 0 132.69 9.60 3 -1 0 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314.27 17.60 -8 -7 0 580.94 29.50 -8 -7 0 520.35 28.80 -8 -7 0 500.45 29.00 8 7 0 539.95 27.10 8 7 0 497.55 27.40 8 7 0 465.15 29.70 -9 -7 0 188.78 11.20 -9 -7 0 191.18 10.90 -9 -7 0 190.58 10.70 9 7 0 187.58 10.50 9 7 0 196.38 10.90 9 7 0 187.28 10.60 9 7 0 184.98 12.90 -10 -7 0 19.90 1.70 -10 -7 0 18.90 2.00 -10 -7 0 20.50 1.90 10 7 0 21.30 1.70 10 7 0 22.10 2.00 10 7 0 22.40 3.20 10 7 0 21.00 1.80 -11 -7 0 44.30 2.80 -11 -7 0 43.80 2.90 11 7 0 44.60 2.90 7 -8 0 49.20 2.90 7 -8 0 49.90 2.90 7 -8 0 48.30 3.00 -7 8 0 36.80 2.10 6 -8 0 15.20 1.50 6 -8 0 18.30 1.50 6 -8 0 17.70 1.60 6 -8 0 19.90 1.70 -6 8 0 17.80 1.40 -6 8 0 14.50 1.10 5 -8 0 45.60 3.10 5 -8 0 43.60 3.00 5 -8 0 46.60 3.10 5 -8 0 49.80 3.20 -5 8 0 38.20 2.60 -5 8 0 39.90 4.40 4 -8 0 141.79 7.90 4 -8 0 133.89 8.00 4 -8 0 152.98 8.00 4 -8 0 143.79 8.10 4 -8 0 127.29 8.00 4 -8 0 136.79 7.90 -4 8 0 106.29 11.50 -4 8 0 116.39 8.90 -4 8 0 120.99 6.70 3 -8 0 81.49 4.70 3 -8 0 78.99 4.80 3 -8 0 74.39 4.70 3 -8 0 80.99 4.90 3 -8 0 76.59 4.70 3 -8 0 73.89 4.70 -3 8 0 67.19 6.10 -3 8 0 67.09 8.70 -3 8 0 69.29 4.20 2 -8 0 155.08 22.40 2 -8 0 182.68 21.20 -2 8 0 172.38 10.90 -2 8 0 146.09 13.20 -2 8 0 135.99 17.00 -2 8 0 155.88 8.70 -2 8 0 157.78 18.10 1 -8 0 115.99 17.60 -1 8 0 131.99 7.20 -1 8 0 135.29 15.60 -1 8 0 120.29 11.30 -1 8 0 125.19 9.00 -1 8 0 121.89 15.20 0 -8 0 393.26 36.70 0 8 0 308.07 26.30 0 8 0 307.37 26.60 0 8 0 350.16 19.60 -1 -8 0 190.88 22.60 1 8 0 198.48 12.20 1 8 0 182.18 18.40 1 8 0 220.58 20.20 1 8 0 216.48 13.50 1 8 0 201.88 15.00 -2 -8 0 3628.64 207.58 -2 -8 0 3546.75 215.18 2 8 0 2849.22 192.98 2 8 0 3782.32 180.88 2 8 0 2996.00 185.38 2 8 0 3609.84 176.68 -3 -8 0 977.00 75.09 -3 -8 0 1295.67 85.29 3 8 0 1066.89 61.29 3 8 0 1013.00 57.49 3 8 0 1090.29 66.59 -4 -8 0 719.53 59.79 -4 -8 0 725.53 54.49 4 8 0 833.12 47.70 4 8 0 906.51 51.79 -5 -8 0 88.59 16.00 -5 -8 0 80.89 18.00 5 8 0 86.99 6.20 5 8 0 90.29 9.30 5 8 0 66.39 11.80 5 8 0 71.49 15.50 -6 -8 0 973.20 77.79 -6 -8 0 1003.60 71.89 6 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10 0 84.29 9.70 -1 10 0 92.79 5.00 0 -10 0 113.69 6.60 0 -10 0 115.49 6.60 0 -10 0 115.69 6.70 0 -10 0 112.89 6.70 0 10 0 77.99 7.40 0 10 0 95.89 4.90 0 10 0 97.69 9.80 0 10 0 80.59 5.50 -1 -10 0 60.59 3.70 -1 -10 0 56.19 3.70 1 10 0 51.89 3.10 1 10 0 50.69 3.70 1 10 0 55.49 3.70 -2 -10 0 199.08 13.40 2 10 0 173.08 10.20 2 10 0 198.88 15.30 2 10 0 173.38 10.30 2 10 0 165.18 9.60 -3 -10 0 3125.39 161.18 -3 -10 0 2838.62 158.18 3 10 0 2822.92 151.48 3 10 0 2911.21 145.59 3 10 0 2582.24 144.79 3 10 0 2620.74 145.39 -4 -10 0 200.78 11.40 -4 -10 0 207.38 14.30 4 10 0 159.68 10.00 4 10 0 166.38 9.80 4 10 0 172.68 15.00 4 10 0 176.68 9.60 -5 -10 0 82.49 7.60 -5 -10 0 76.69 4.90 5 10 0 70.59 9.10 5 10 0 78.29 4.80 5 10 0 71.39 4.50 -6 -10 0 72.69 4.40 -6 -10 0 69.19 4.20 -6 -10 0 63.59 6.70 6 10 0 71.99 9.00 6 10 0 61.39 4.40 6 10 0 65.29 4.20 6 10 0 70.69 4.70 -7 -10 0 165.58 9.30 -7 -10 0 155.38 12.00 -7 -10 0 174.68 9.40 7 10 0 154.58 8.70 7 10 0 144.09 11.10 7 10 0 161.88 9.00 -8 -10 0 56.29 4.10 -8 -10 0 58.39 3.70 -8 -10 0 61.59 3.70 8 10 0 59.79 3.80 8 10 0 62.89 6.10 8 10 0 60.09 4.00 -9 -10 0 54.29 3.30 -9 -10 0 51.89 3.60 9 10 0 55.59 3.80 9 10 0 62.49 5.50 4 -11 0 15.10 1.30 4 -11 0 15.20 1.30 4 -11 0 18.00 1.30 4 -11 0 16.10 1.30 3 -11 0 42.30 2.80 3 -11 0 43.10 2.80 3 -11 0 43.70 2.80 3 -11 0 43.00 2.80 -3 11 0 30.20 1.80 2 -11 0 78.99 4.70 2 -11 0 74.39 4.70 2 -11 0 78.49 4.70 2 -11 0 78.29 4.60 1 -11 0 696.93 37.00 1 -11 0 720.43 37.00 1 -11 0 709.03 36.90 1 -11 0 628.24 36.80 -1 11 0 515.45 30.40 0 -11 0 281.87 16.60 0 -11 0 310.27 16.70 0 -11 0 306.27 16.70 0 -11 0 320.07 16.60 0 11 0 275.57 15.50 0 11 0 270.47 14.90 0 11 0 284.87 15.50 -1 -11 0 197.38 10.70 -1 -11 0 194.28 10.70 -1 -11 0 180.38 12.40 1 11 0 172.88 9.20 1 11 0 161.78 9.70 1 11 0 170.58 9.90 -2 -11 0 221.88 14.60 2 11 0 180.78 11.00 2 11 0 199.78 11.00 2 11 0 191.08 10.30 -3 -11 0 1246.78 71.49 -3 -11 0 1338.07 68.99 3 11 0 1079.09 59.69 3 11 0 1146.39 59.59 3 11 0 1117.89 58.99 3 11 0 1097.89 65.19 -4 -11 0 221.38 12.80 -4 -11 0 239.78 15.60 4 11 0 218.58 12.50 4 11 0 214.38 12.20 4 11 0 208.28 11.90 -5 -11 0 39.60 5.00 -5 -11 0 40.10 2.90 5 11 0 38.20 3.20 5 11 0 40.20 2.70 5 11 0 37.60 3.00 -6 -11 0 148.09 11.20 -6 -11 0 151.98 8.60 6 11 0 137.19 8.80 6 11 0 154.78 8.40 6 11 0 149.88 8.60 -7 -11 0 173.38 12.50 -7 -11 0 187.78 10.10 -7 -11 0 174.08 9.90 7 11 0 181.88 12.20 7 11 0 163.98 9.90 7 11 0 173.78 9.70 -8 -11 0 92.29 5.20 -8 -11 0 87.19 5.10 -8 -11 0 84.69 7.20 8 11 0 83.59 6.90 8 11 0 80.79 5.00 -9 -11 0 86.69 4.80 -9 -11 0 81.99 4.80 9 11 0 82.19 4.90 9 11 0 83.69 6.30 2 -12 0 39.10 2.50 2 -12 0 38.60 2.40 2 -12 0 36.00 2.50 -2 12 0 33.10 2.30 -2 12 0 30.10 1.80 1 -12 0 17.90 1.60 1 -12 0 17.70 1.50 1 -12 0 18.60 1.70 -1 12 0 15.40 1.10 -1 12 0 14.20 1.60 0 -12 0 312.47 16.70 0 -12 0 304.67 16.70 0 -12 0 298.67 16.70 0 12 0 274.27 15.60 0 12 0 290.47 15.70 0 12 0 282.27 15.10 -1 -12 0 218.68 12.30 -1 -12 0 226.58 12.30 1 12 0 201.68 11.00 1 12 0 206.38 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204.68 13.50 6 12 -1 149.79 8.10 6 12 -1 140.99 8.20 6 12 -1 142.39 8.40 -6 -12 1 183.28 12.30 -6 -12 1 177.58 10.10 5 12 -1 61.99 3.80 5 12 -1 56.89 3.90 5 12 -1 62.09 4.20 -5 -12 1 76.29 6.60 -5 -12 1 68.59 4.50 4 12 -1 81.49 4.70 4 12 -1 78.89 4.90 4 12 -1 74.09 5.10 -4 -12 1 90.99 7.30 -4 -12 1 83.79 5.30 3 12 -1 103.79 6.10 3 12 -1 114.99 6.30 3 12 -1 91.49 6.30 -3 -12 1 114.09 6.60 -3 -12 1 110.99 8.40 2 12 -1 33.30 2.70 2 12 -1 30.00 2.30 2 12 -1 30.70 2.50 2 12 -1 31.50 1.90 -2 -12 1 34.20 3.80 1 12 -1 55.89 3.90 1 12 -1 64.39 4.00 1 12 -1 56.19 3.30 -1 -12 1 71.89 4.30 -1 -12 1 68.79 4.30 0 12 -1 58.99 3.10 0 12 -1 50.89 3.60 0 12 -1 52.29 3.60 0 -12 1 86.59 4.60 0 -12 1 63.99 4.50 -1 12 -1 391.06 20.20 -1 12 -1 365.86 20.60 1 -12 1 470.95 24.10 1 -12 1 423.46 24.10 -2 12 -1 72.69 3.90 -2 12 -1 69.39 4.30 2 -12 1 94.39 5.30 2 -12 1 88.49 5.30 8 11 -1 96.49 5.70 8 11 -1 103.69 5.60 8 11 -1 91.39 7.30 -8 -11 1 95.49 7.70 -8 -11 1 109.99 5.90 -8 -11 1 101.49 5.80 7 11 -1 138.79 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4 -3 77.29 4.80 -9 -4 3 73.19 4.80 -9 -4 3 78.99 5.00 8 4 -3 1430.76 72.89 8 4 -3 1231.98 69.79 8 4 -3 1263.27 69.79 -8 -4 3 1044.90 55.69 -8 -4 3 1030.30 55.99 7 4 -3 695.33 36.00 7 4 -3 667.33 36.10 7 4 -3 696.93 36.10 7 4 -3 621.94 38.80 -7 -4 3 603.54 35.10 -7 -4 3 685.23 35.00 6 4 -3 104.69 17.00 6 4 -3 115.69 15.70 -6 -4 3 109.89 21.60 5 4 -3 48.20 9.90 5 4 -3 66.89 12.50 -5 -4 3 55.49 11.60 -5 -4 3 55.89 14.50 4 4 -3 1157.08 74.19 4 4 -3 1244.68 76.49 -4 -4 3 1466.65 90.09 -4 -4 3 1410.66 96.09 3 4 -3 887.91 46.00 3 4 -3 843.72 48.10 3 4 -3 857.91 54.69 3 4 -3 806.42 54.39 -3 -4 3 745.13 46.80 -3 -4 3 844.62 60.39 -3 -4 3 898.11 56.09 2 4 -3 837.82 51.09 2 4 -3 759.82 50.19 2 4 -3 810.02 45.70 2 4 -3 890.21 43.70 2 4 -3 737.13 47.60 -2 -4 3 862.31 56.99 -2 -4 3 943.31 49.90 -2 -4 3 827.02 59.59 1 4 -3 592.14 35.90 1 4 -3 514.15 36.60 1 4 -3 616.04 31.10 1 4 -3 558.04 32.90 -1 -4 3 501.65 34.20 -1 -4 3 617.74 32.50 -1 -4 3 602.44 42.00 -1 -4 3 586.34 44.80 -1 -4 3 519.25 38.10 -1 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30.20 6 -3 9 571.44 29.80 7 -3 9 592.04 32.30 7 -3 9 598.04 31.90 8 -3 9 948.71 47.50 8 -3 9 819.32 47.10 9 -3 9 75.19 4.60 6 2 -9 51.79 3.30 6 2 -9 58.69 3.50 6 2 -9 56.89 5.20 -6 -2 9 45.60 3.00 5 2 -9 487.75 28.90 5 2 -9 480.95 26.30 5 2 -9 499.55 26.40 -5 -2 9 391.06 22.90 -5 -2 9 449.06 25.10 4 2 -9 61.79 3.40 4 2 -9 53.29 3.90 4 2 -9 48.60 5.90 4 2 -9 49.99 3.50 -4 -2 9 54.59 5.60 -4 -2 9 51.99 3.70 3 2 -9 1380.86 72.89 3 2 -9 1401.76 72.79 3 2 -9 1321.87 73.29 -3 -2 9 1263.27 75.09 -3 -2 9 1336.27 68.59 -3 -2 9 1242.38 70.99 2 2 -9 6.00 0.90 2 2 -9 6.10 1.00 2 2 -9 9.70 2.00 -2 -2 9 8.00 1.50 -2 -2 9 5.10 2.30 -2 -2 9 5.30 3.40 1 2 -9 760.42 59.39 1 2 -9 763.82 55.39 -1 -2 9 780.82 50.19 -1 -2 9 824.22 58.59 -1 -2 9 869.11 66.19 0 2 -9 314.97 29.30 0 2 -9 288.77 16.00 0 2 -9 247.88 29.30 0 2 -9 313.47 19.50 0 -2 9 340.47 34.60 0 -2 9 363.66 24.20 0 -2 9 283.07 28.80 -1 2 -9 968.40 49.50 -1 2 -9 1061.79 52.19 -1 2 -9 847.72 50.49 -1 2 -9 841.02 62.79 -1 2 -9 902.51 66.79 1 -2 9 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32.20 2.40 5 4 14 34.10 2.20 5 4 14 34.70 2.30 -6 -4 -14 17.00 1.10 -6 -4 -14 16.90 1.60 6 4 14 18.90 1.40 6 4 14 19.20 1.50 6 4 14 17.20 1.50 -7 -4 -14 120.39 6.50 7 4 14 149.88 8.30 -2 -5 -14 143.39 8.40 -2 -5 -14 154.68 8.20 2 5 14 150.28 9.10 2 5 14 144.69 8.10 -3 -5 -14 98.89 5.80 -3 -5 -14 111.09 6.20 3 5 14 94.59 6.40 3 5 14 100.39 5.50 -4 -5 -14 56.29 3.60 4 5 14 51.69 3.90 4 5 14 56.79 3.30 -5 -5 -14 152.98 8.70 5 5 14 166.78 9.20 -6 -5 -14 104.89 6.10 6 5 14 121.59 6.80 -7 -5 -14 45.90 2.90 7 5 14 59.59 3.50 -4 -6 -14 11.60 1.30 4 6 14 11.30 1.00 4 6 14 11.20 1.60 -5 -6 -14 58.59 3.70 5 6 14 60.69 3.60 -6 -6 -14 26.40 2.00 6 6 14 28.10 1.90 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 82275