data_6051 _audit_creation_date 2019-09-19 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelxl_version_number 2013-2 _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _audit_update_record ; ???? ; _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H30 O3,C2 H6 O S' _chemical_formula_sum 'C26 H36 O4 S' _chemical_formula_weight 444.61 _chemical_absolute_configuration ad _chemical_melting_point ? 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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.3541(3) _cell_length_b 11.5712(3) _cell_length_c 32.2251(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2369.34(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 71.5 _cell_measurement_theta_min 26.6 _shelx_estimated_absorpt_T_max 0.772 _shelx_estimated_absorpt_T_min 0.595 _exptl_absorpt_coefficient_mu 1.443 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.548 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ? _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.402 _exptl_crystal_size_mid 0.352 _exptl_crystal_size_min 0.189 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_unetI/netI 0.0409 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 15032 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.115 _diffrn_reflns_theta_min 4.059 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 0 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'MicroMax 002+' _diffrn_measurement_method \f\k _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_source 'fine-focus sealed tube' _reflns_Friedel_coverage 0.698 _reflns_Friedel_fraction_full 0.976 _reflns_Friedel_fraction_max 0.947 _reflns_number_gt 3823 _reflns_number_total 4521 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'ORTEPII(Johnson,1976)andPLUTON(Spek,1990)' _computing_publication_material ' SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement ' SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution ' SHELXL-2018/3 (Sheldrick, 2018)' _refine_diff_density_max 0.263 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Flack x determined using 1358 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.003(12) _refine_ls_extinction_coef 0.0053(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 295 _refine_ls_number_reflns 4521 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0406 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1073 _refine_ls_wR_factor_ref 0.1114 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances S1A-O1D 1.4 with sigma of 0.02 S1A-C2D 1.7 with sigma of 0.02 3. Others Sof(H2DD)=Sof(H2DE)=Sof(H2DF)=Sof(H1DD)=Sof(H1DE)=Sof(H1DF)=Sof(S1A)=1-FVAR(1) Sof(S1B)=Sof(H2DA)=Sof(H2DB)=Sof(H2DC)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=FVAR(1) 4.a Ternary CH refined with riding coordinates: C004(H004), C005(H005), C006(H006), C008(H008), C009(H009), C00A(H00A), C00G(H00G) 4.b Secondary CH2 refined with riding coordinates: C00D(H00B,H00C), C00I(H00H,H00I), C00K(H00J,H00K), C00M(H00L,H00M), C00N(H00N, H00O), C00P(H00S,H00T), C00R(H00V,H00W), C00T(H00X,H00Y) 4.c Aromatic/amide H refined with riding coordinates: C00Q(H00U) 4.d Idealised Me refined as rotating group: C00F(H00D,H00E,H00F), C00O(H00P,H00Q,H00R), C2D(H2DA,H2DB,H2DC), C2D(H2DD, H2DE,H2DF), C1D(H1DA,H1DB,H1DC), C1D(H1DD,H1DE,H1DF) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 S1B S 1.14787(16) 0.57834(9) 0.42248(4) 0.0805(4) Uani 0.868(4) 1 d . . P A 1 O002 O 0.9034(3) 0.08404(16) 0.46501(5) 0.0550(5) Uani 1 1 d . . . . . O003 O 1.0074(5) -0.0898(2) 0.48434(8) 0.0877(8) Uani 1 1 d . . . . . C004 C 0.7525(4) 0.34579(19) 0.34748(6) 0.0403(5) Uani 1 1 d . . . . . H004 H 0.8917 0.3781 0.3536 0.048 Uiso 1 1 calc R . . . . C005 C 0.6798(3) 0.2753(2) 0.38473(6) 0.0406(5) Uani 1 1 d . . . . . H005 H 0.5539 0.2345 0.3751 0.049 Uiso 1 1 calc R . . . . C006 C 0.7716(4) 0.2635(2) 0.30992(6) 0.0417(5) Uani 1 1 d . . . . . H006 H 0.6286 0.2366 0.3039 0.050 Uiso 1 1 calc R . . . . C007 C 0.6880(4) 0.4219(2) 0.26001(7) 0.0473(5) Uani 1 1 d . . . . . C008 C 0.5804(4) 0.4833(2) 0.29355(8) 0.0507(6) Uani 1 1 d . . . . . H008 H 0.4388 0.5100 0.2862 0.061 Uiso 1 1 calc R . . . . C009 C 0.6019(4) 0.4447(2) 0.33820(7) 0.0477(5) Uani 1 1 d . . . . . H009 H 0.4733 0.4473 0.3550 0.057 Uiso 1 1 calc R . . . . C00A C 0.6134(4) 0.3327(2) 0.42484(7) 0.0489(5) Uani 1 1 d . . . . . H00A H 0.4798 0.3749 0.4253 0.059 Uiso 1 1 calc R . . . . C00B C 0.8370(4) 0.17836(19) 0.39656(6) 0.0413(5) Uani 1 1 d . . . . . C00C C 0.8477(4) 0.3277(2) 0.27010(7) 0.0461(5) Uani 1 1 d . . . . . C00D C 0.8342(5) 0.0930(2) 0.36016(7) 0.0499(6) Uani 1 1 d . . . . . H00B H 0.6938 0.0614 0.3569 0.060 Uiso 1 1 calc R . . . . H00C H 0.9299 0.0296 0.3658 0.060 Uiso 1 1 calc R . . . . O00E O 0.6783(6) 0.4210(3) 0.14891(6) 0.1062(10) Uani 1 1 d . . . . . C00F C 1.0683(4) 0.2165(3) 0.40288(8) 0.0531(6) Uani 1 1 d . . . . . H00D H 1.0919 0.2885 0.3889 0.080 Uiso 1 1 calc GR . . . . H00E H 1.1608 0.1587 0.3917 0.080 Uiso 1 1 calc GR . . . . H00F H 1.0958 0.2258 0.4320 0.080 Uiso 1 1 calc GR . . . . C00G C 0.6558(5) 0.2462(2) 0.45904(7) 0.0536(6) Uani 1 1 d . . . . . H00G H 0.5477 0.2368 0.4805 0.064 Uiso 1 1 calc R . . . . C00H C 0.7402(4) 0.1380(2) 0.43879(7) 0.0462(5) Uani 1 1 d . . . . . C00I C 0.7721(5) 0.3587(2) 0.45775(7) 0.0557(6) Uani 1 1 d . . . . . H00H H 0.7360 0.4166 0.4783 0.067 Uiso 1 1 calc R . . . . H00I H 0.9196 0.3569 0.4500 0.067 Uiso 1 1 calc R . . . . C00J C 0.8822(6) -0.0302(2) 0.46647(8) 0.0628(7) Uani 1 1 d . . . . . C00K C 0.6906(5) 0.5588(2) 0.32534(8) 0.0593(7) Uani 1 1 d . . . . . H00J H 0.8424 0.5657 0.3235 0.071 Uiso 1 1 calc R . . . . H00K H 0.6184 0.6280 0.3346 0.071 Uiso 1 1 calc R . . . . O1D O 1.1653(5) 0.5453(3) 0.37882(11) 0.1175(11) Uani 1 1 d D . . . . C00M C 0.5717(4) 0.0444(3) 0.43609(8) 0.0571(7) Uani 1 1 d . . . . . H00L H 0.4663 0.0544 0.4576 0.068 Uiso 1 1 calc R . . . . H00M H 0.5030 0.0453 0.4092 0.068 Uiso 1 1 calc R . . . . C00N C 0.9010(5) 0.1548(2) 0.31985(7) 0.0530(6) Uani 1 1 d . . . . . H00N H 1.0481 0.1763 0.3221 0.064 Uiso 1 1 calc R . . . . H00O H 0.8880 0.1010 0.2969 0.064 Uiso 1 1 calc R . . . . C00O C 1.0680(4) 0.3817(3) 0.27629(9) 0.0583(6) Uani 1 1 d . . . . . H00P H 1.0653 0.4325 0.2999 0.087 Uiso 1 1 calc GR . . . . H00Q H 1.1062 0.4248 0.2520 0.087 Uiso 1 1 calc GR . . . . H00R H 1.1693 0.3215 0.2809 0.087 Uiso 1 1 calc GR . . . . C00P C 0.8569(6) 0.2413(3) 0.23369(7) 0.0610(7) Uani 1 1 d . . . . . H00S H 0.9728 0.1882 0.2382 0.073 Uiso 1 1 calc R . . . . H00T H 0.7279 0.1965 0.2333 0.073 Uiso 1 1 calc R . . . . C00Q C 0.6334(5) 0.4461(3) 0.22043(8) 0.0629(7) Uani 1 1 d . . . . . H00U H 0.5292 0.5012 0.2161 0.075 Uiso 1 1 calc R . . . . C00R C 0.8855(7) 0.2998(3) 0.19151(8) 0.0748(9) Uani 1 1 d . . . . . H00V H 1.0252 0.3334 0.1901 0.090 Uiso 1 1 calc R . . . . H00W H 0.8746 0.2421 0.1698 0.090 Uiso 1 1 calc R . . . . C00S C 0.7266(6) 0.3916(3) 0.18412(8) 0.0718(9) Uani 1 1 d . . . . . C00T C 0.6922(6) -0.0655(3) 0.44232(11) 0.0752(9) Uani 1 1 d . . . . . H00X H 0.6092 -0.1214 0.4577 0.090 Uiso 1 1 calc R . . . . H00Y H 0.7322 -0.0991 0.4159 0.090 Uiso 1 1 calc R . . . . C2D C 0.8959(7) 0.6428(4) 0.42744(17) 0.1046(14) Uani 1 1 d D . . . . H2DA H 0.8886 0.7103 0.4101 0.157 Uiso 0.868(4) 1 calc GR . P A 1 H2DB H 0.8729 0.6645 0.4558 0.157 Uiso 0.868(4) 1 calc GR . P A 1 H2DC H 0.7898 0.5886 0.4190 0.157 Uiso 0.868(4) 1 calc GR . P A 1 H2DD H 0.8081 0.5871 0.4137 0.157 Uiso 0.132(4) 1 calc GR . P A 2 H2DE H 0.8264 0.7165 0.4277 0.157 Uiso 0.132(4) 1 calc GR . P A 2 H2DF H 0.9220 0.6183 0.4554 0.157 Uiso 0.132(4) 1 calc GR . P A 2 C1D C 1.3026(7) 0.7073(4) 0.42890(14) 0.0965(12) Uani 1 1 d . . . . . H1DA H 1.4492 0.6885 0.4265 0.145 Uiso 0.868(4) 1 calc GR . P A 1 H1DB H 1.2758 0.7399 0.4558 0.145 Uiso 0.868(4) 1 calc GR . P A 1 H1DC H 1.2652 0.7622 0.4078 0.145 Uiso 0.868(4) 1 calc GR . P A 1 H1DD H 1.3802 0.6462 0.4420 0.145 Uiso 0.132(4) 1 calc GR . P A 2 H1DE H 1.2620 0.7633 0.4494 0.145 Uiso 0.132(4) 1 calc GR . P A 2 H1DF H 1.3891 0.7437 0.4083 0.145 Uiso 0.132(4) 1 calc GR . P A 2 S1A S 1.0864(10) 0.6525(7) 0.4063(2) 0.075(3) Uani 0.132(4) 1 d D . P A 2 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 S1B 0.0596(6) 0.0541(6) 0.1276(9) -0.0078(6) -0.0119(5) 0.0010(4) O002 0.0635(11) 0.0493(10) 0.0522(8) 0.0066(7) -0.0150(8) -0.0037(9) O003 0.109(2) 0.0612(13) 0.0933(15) 0.0087(12) -0.0242(14) 0.0194(14) C004 0.0351(10) 0.0389(11) 0.0468(10) -0.0012(9) -0.0024(8) 0.0013(9) C005 0.0346(10) 0.0405(11) 0.0467(10) -0.0022(9) -0.0021(8) 0.0010(9) C006 0.0416(11) 0.0395(11) 0.0440(10) -0.0003(9) -0.0026(8) 0.0003(9) C007 0.0440(12) 0.0452(12) 0.0527(11) 0.0049(10) -0.0062(9) -0.0056(10) C008 0.0450(13) 0.0444(13) 0.0627(14) 0.0059(11) -0.0079(10) 0.0062(10) C009 0.0454(12) 0.0422(12) 0.0556(12) 0.0002(10) 0.0002(10) 0.0067(10) C00A 0.0496(13) 0.0471(12) 0.0500(11) -0.0042(10) 0.0051(10) 0.0049(11) C00B 0.0405(11) 0.0394(11) 0.0440(10) 0.0014(9) -0.0013(9) 0.0018(9) C00C 0.0454(13) 0.0485(12) 0.0445(10) 0.0022(9) -0.0015(9) 0.0026(10) C00D 0.0607(15) 0.0402(12) 0.0489(11) 0.0008(9) -0.0006(10) 0.0070(11) O00E 0.144(3) 0.121(2) 0.0531(11) 0.0177(12) -0.0173(13) 0.027(2) C00F 0.0386(12) 0.0581(15) 0.0627(13) 0.0082(12) -0.0034(10) 0.0035(11) C00G 0.0594(15) 0.0535(14) 0.0479(11) -0.0004(10) 0.0075(10) -0.0015(12) C00H 0.0482(13) 0.0453(13) 0.0450(10) 0.0028(9) -0.0048(9) -0.0030(10) C00I 0.0680(17) 0.0512(15) 0.0481(11) -0.0091(10) -0.0014(11) 0.0001(12) C00J 0.082(2) 0.0472(14) 0.0597(14) 0.0012(12) -0.0072(13) 0.0059(15) C00K 0.0667(17) 0.0413(13) 0.0699(15) -0.0043(11) -0.0062(13) 0.0026(12) O1D 0.0753(17) 0.115(2) 0.162(3) -0.074(2) 0.0054(17) 0.0098(17) C00M 0.0566(16) 0.0588(16) 0.0559(13) 0.0022(11) 0.0011(11) -0.0144(13) C00N 0.0662(16) 0.0451(13) 0.0477(11) 0.0001(10) 0.0054(11) 0.0128(12) C00O 0.0410(13) 0.0702(17) 0.0636(14) 0.0101(13) 0.0028(11) -0.0016(12) C00P 0.081(2) 0.0561(15) 0.0458(12) -0.0009(11) 0.0014(12) 0.0097(15) C00Q 0.0638(17) 0.0666(17) 0.0583(13) 0.0114(12) -0.0105(12) 0.0074(14) C00R 0.095(2) 0.082(2) 0.0469(13) 0.0052(13) 0.0020(13) 0.013(2) C00S 0.084(2) 0.080(2) 0.0511(13) 0.0097(14) -0.0103(13) 0.0022(17) C00T 0.092(2) 0.0505(16) 0.0830(19) 0.0047(15) -0.0143(17) -0.0156(17) C2D 0.085(3) 0.080(3) 0.149(4) -0.023(3) 0.023(3) 0.006(2) C1D 0.088(3) 0.091(3) 0.110(3) -0.001(2) -0.024(2) -0.023(2) S1A 0.062(4) 0.090(6) 0.073(4) -0.005(3) -0.006(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1B O1D 1.462(3) . ? S1B C2D 1.774(5) . ? S1B C1D 1.798(4) . ? O002 C00H 1.476(3) . ? O002 C00J 1.329(4) . ? O003 C00J 1.201(4) . ? C004 C005 1.523(3) . ? C004 C006 1.545(3) . ? C004 C009 1.521(3) . ? C005 C00A 1.513(3) . ? C005 C00B 1.550(3) . ? C006 C00C 1.560(3) . ? C006 C00N 1.536(3) . ? C007 C008 1.463(4) . ? C007 C00C 1.525(3) . ? C007 C00Q 1.351(3) . ? C008 C009 1.513(3) . ? C008 C00K 1.517(4) . ? C009 C00K 1.494(4) . ? C00A C00G 1.513(4) . ? C00A C00I 1.494(4) . ? C00B C00D 1.534(3) . ? C00B C00F 1.548(4) . ? C00B C00H 1.565(3) . ? C00C C00O 1.546(4) . ? C00C C00P 1.543(3) . ? C00D C00N 1.543(3) . ? O00E C00S 1.224(3) . ? C00G C00H 1.510(4) . ? C00G C00I 1.498(4) . ? C00H C00M 1.526(4) . ? C00J C00T 1.493(5) . ? O1D S1A 1.604(8) . ? C00M C00T 1.498(5) . ? C00P C00R 1.530(4) . ? C00Q C00S 1.455(4) . ? C00R C00S 1.485(5) . ? C2D S1A 1.394(8) . ? C1D S1A 1.679(8) . ? 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 O1D S1B C2D 105.4(2) . . ? O1D S1B C1D 106.6(2) . . ? C2D S1B C1D 97.7(2) . . ? C00J O002 C00H 111.7(2) . . ? C005 C004 C006 108.12(18) . . ? C009 C004 C005 111.54(18) . . ? C009 C004 C006 111.05(17) . . ? C004 C005 C00B 112.72(17) . . ? C00A C005 C004 121.53(19) . . ? C00A C005 C00B 106.69(18) . . ? C004 C006 C00C 112.05(19) . . ? C00N C006 C004 112.57(17) . . ? C00N C006 C00C 113.29(19) . . ? C008 C007 C00C 120.0(2) . . ? C00Q C007 C008 118.5(2) . . ? C00Q C007 C00C 121.3(2) . . ? C007 C008 C009 121.2(2) . . ? C007 C008 C00K 124.2(2) . . ? C009 C008 C00K 59.08(17) . . ? C008 C009 C004 117.8(2) . . ? C00K C009 C004 118.8(2) . . ? C00K C009 C008 60.61(17) . . ? C00G C00A C005 106.42(19) . . ? C00I C00A C005 120.4(2) . . ? C00I C00A C00G 59.73(17) . . ? C005 C00B C00H 100.18(17) . . ? C00D C00B C005 105.71(18) . . ? C00D C00B C00F 107.2(2) . . ? C00D C00B C00H 117.92(19) . . ? C00F C00B C005 115.99(19) . . ? C00F C00B C00H 110.11(18) . . ? C007 C00C C006 108.04(19) . . ? C007 C00C C00O 109.9(2) . . ? C007 C00C C00P 109.1(2) . . ? C00O C00C C006 111.54(19) . . ? C00P C00C C006 109.2(2) . . ? C00P C00C C00O 109.0(2) . . ? C00B C00D C00N 110.0(2) . . ? C00H C00G C00A 107.25(18) . . ? C00I C00G C00A 59.52(17) . . ? C00I C00G C00H 122.2(2) . . ? O002 C00H C00B 110.4(2) . . ? O002 C00H C00G 110.65(19) . . ? O002 C00H C00M 103.02(19) . . ? C00G C00H C00B 105.55(19) . . ? C00G C00H C00M 111.4(2) . . ? C00M C00H C00B 115.99(19) . . ? C00A C00I C00G 60.75(17) . . ? O002 C00J C00T 109.6(2) . . ? O003 C00J O002 121.4(3) . . ? O003 C00J C00T 128.9(3) . . ? C009 C00K C008 60.31(17) . . ? C00T C00M C00H 103.7(2) . . ? C006 C00N C00D 114.1(2) . . ? C00R C00P C00C 113.2(2) . . ? C007 C00Q C00S 124.4(3) . . ? C00S C00R C00P 112.3(3) . . ? O00E C00S C00Q 121.5(3) . . ? O00E C00S C00R 121.2(3) . . ? C00Q C00S C00R 117.2(2) . . ? C00J C00T C00M 104.5(2) . . ? O1D S1A C1D 106.0(4) . . ? C2D S1A O1D 118.7(6) . . ? C2D S1A C1D 121.9(5) . . ? _shelx_res_file ; TITL shelxl_a.res in P2(1)2(1)2(1) REM Old TITL shelxl_a.res in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.172, Rweak 0.047, Alpha 0.005 REM 0.839 for 28 systematic absences, Orientation as input REM Flack x = 0.104 ( 0.013 ) from 1372 Parsons' quotients REM Formula found by SHELXT: C26 O4 S CELL 1.54178 6.3541 11.5712 32.2251 90 90 90 ZERR 4 0.0003 0.0003 0.0004 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H O S UNIT 104 144 16 4 DFIX 1.4 S1A O1D DFIX 1.7 S1A C2D L.S. 15 PLAN 5 SIZE 0.189 0.402 0.352 list 4 fmap 2 ACTA OMIT 0 0 2 REM REM REM WGHT 0.071200 EXTI 0.005326 FVAR 0.76801 0.86829 PART 1 S1B 4 1.147869 0.578343 0.422476 21.00000 0.05959 0.05414 = 0.12763 -0.00775 -0.01191 0.00103 PART 0 O002 3 0.903396 0.084039 0.465010 11.00000 0.06353 0.04935 = 0.05219 0.00661 -0.01503 -0.00367 O003 3 1.007420 -0.089848 0.484344 11.00000 0.10859 0.06116 = 0.09326 0.00868 -0.02421 0.01938 C004 1 0.752478 0.345793 0.347483 11.00000 0.03509 0.03885 = 0.04682 -0.00119 -0.00238 0.00126 AFIX 13 H004 2 0.891708 0.378060 0.353559 11.00000 -1.20000 AFIX 0 C005 1 0.679808 0.275297 0.384728 11.00000 0.03456 0.04050 = 0.04667 -0.00225 -0.00208 0.00100 AFIX 13 H005 2 0.553896 0.234460 0.375062 11.00000 -1.20000 AFIX 0 C006 1 0.771616 0.263484 0.309925 11.00000 0.04156 0.03951 = 0.04402 -0.00031 -0.00261 0.00034 AFIX 13 H006 2 0.628564 0.236568 0.303941 11.00000 -1.20000 AFIX 0 C007 1 0.688006 0.421944 0.260013 11.00000 0.04404 0.04525 = 0.05266 0.00489 -0.00616 -0.00555 C008 1 0.580435 0.483287 0.293553 11.00000 0.04500 0.04442 = 0.06272 0.00589 -0.00792 0.00620 AFIX 13 H008 2 0.438823 0.509964 0.286246 11.00000 -1.20000 AFIX 0 C009 1 0.601933 0.444690 0.338203 11.00000 0.04543 0.04216 = 0.05564 0.00016 0.00024 0.00670 AFIX 13 H009 2 0.473329 0.447349 0.354963 11.00000 -1.20000 AFIX 0 C00A 1 0.613387 0.332656 0.424836 11.00000 0.04960 0.04713 = 0.05005 -0.00415 0.00515 0.00490 AFIX 13 H00A 2 0.479754 0.374921 0.425292 11.00000 -1.20000 AFIX 0 C00B 1 0.836975 0.178355 0.396560 11.00000 0.04047 0.03939 = 0.04402 0.00140 -0.00134 0.00176 C00C 1 0.847728 0.327696 0.270096 11.00000 0.04539 0.04850 = 0.04452 0.00222 -0.00148 0.00258 C00D 1 0.834181 0.092959 0.360164 11.00000 0.06066 0.04018 = 0.04889 0.00076 -0.00059 0.00696 AFIX 23 H00B 2 0.693757 0.061363 0.356898 11.00000 -1.20000 H00C 2 0.929850 0.029558 0.365815 11.00000 -1.20000 AFIX 0 O00E 3 0.678311 0.421018 0.148909 11.00000 0.14425 0.12134 = 0.05312 0.01767 -0.01725 0.02747 C00F 1 1.068316 0.216456 0.402885 11.00000 0.03856 0.05808 = 0.06270 0.00816 -0.00342 0.00352 AFIX 137 H00D 2 1.091865 0.288503 0.388862 11.00000 -1.50000 H00E 2 1.160767 0.158659 0.391729 11.00000 -1.50000 H00F 2 1.095773 0.225833 0.431985 11.00000 -1.50000 AFIX 0 C00G 1 0.655796 0.246183 0.459045 11.00000 0.05943 0.05346 = 0.04792 -0.00041 0.00754 -0.00146 AFIX 13 H00G 2 0.547681 0.236811 0.480470 11.00000 -1.20000 AFIX 0 C00H 1 0.740174 0.138000 0.438789 11.00000 0.04821 0.04529 = 0.04496 0.00278 -0.00476 -0.00296 C00I 1 0.772109 0.358705 0.457754 11.00000 0.06795 0.05117 = 0.04807 -0.00908 -0.00135 0.00012 AFIX 23 H00H 2 0.736000 0.416606 0.478324 11.00000 -1.20000 H00I 2 0.919582 0.356864 0.450004 11.00000 -1.20000 AFIX 0 C00J 1 0.882187 -0.030192 0.466474 11.00000 0.08161 0.04718 = 0.05972 0.00121 -0.00718 0.00594 C00K 1 0.690588 0.558777 0.325336 11.00000 0.06667 0.04132 = 0.06986 -0.00432 -0.00616 0.00263 AFIX 23 H00J 2 0.842431 0.565744 0.323496 11.00000 -1.20000 H00K 2 0.618423 0.627970 0.334625 11.00000 -1.20000 AFIX 0 O1D 3 1.165348 0.545330 0.378823 11.00000 0.07527 0.11509 = 0.16201 -0.07367 0.00539 0.00977 C00M 1 0.571659 0.044359 0.436090 11.00000 0.05662 0.05878 = 0.05585 0.00218 0.00111 -0.01440 AFIX 23 H00L 2 0.466293 0.054378 0.457572 11.00000 -1.20000 H00M 2 0.503019 0.045263 0.409205 11.00000 -1.20000 AFIX 0 C00N 1 0.900972 0.154794 0.319847 11.00000 0.06619 0.04514 = 0.04765 0.00010 0.00544 0.01278 AFIX 23 H00N 2 1.048084 0.176291 0.322092 11.00000 -1.20000 H00O 2 0.888037 0.101016 0.296898 11.00000 -1.20000 AFIX 0 C00O 1 1.067971 0.381737 0.276290 11.00000 0.04100 0.07020 = 0.06357 0.01007 0.00279 -0.00162 AFIX 137 H00P 2 1.065277 0.432457 0.299859 11.00000 -1.50000 H00Q 2 1.106161 0.424788 0.251963 11.00000 -1.50000 H00R 2 1.169258 0.321528 0.280894 11.00000 -1.50000 AFIX 0 C00P 1 0.856925 0.241270 0.233692 11.00000 0.08099 0.05612 = 0.04585 -0.00089 0.00143 0.00972 AFIX 23 H00S 2 0.972759 0.188155 0.238235 11.00000 -1.20000 H00T 2 0.727890 0.196491 0.233279 11.00000 -1.20000 AFIX 0 C00Q 1 0.633377 0.446067 0.220433 11.00000 0.06379 0.06658 = 0.05833 0.01141 -0.01052 0.00742 AFIX 43 H00U 2 0.529168 0.501201 0.216104 11.00000 -1.20000 AFIX 0 C00R 1 0.885494 0.299820 0.191513 11.00000 0.09533 0.08206 = 0.04689 0.00521 0.00202 0.01256 AFIX 23 H00V 2 1.025177 0.333406 0.190089 11.00000 -1.20000 H00W 2 0.874610 0.242114 0.169785 11.00000 -1.20000 AFIX 0 C00S 1 0.726586 0.391605 0.184119 11.00000 0.08397 0.08034 = 0.05112 0.00971 -0.01029 0.00215 C00T 1 0.692220 -0.065516 0.442319 11.00000 0.09210 0.05046 = 0.08300 0.00469 -0.01430 -0.01558 AFIX 23 H00X 2 0.609217 -0.121368 0.457681 11.00000 -1.20000 H00Y 2 0.732165 -0.099067 0.415882 11.00000 -1.20000 AFIX 0 C2D 1 0.895910 0.642834 0.427440 11.00000 0.08474 0.08043 = 0.14870 -0.02344 0.02275 0.00620 PART 1 AFIX 137 H2DA 2 0.888603 0.710275 0.410150 21.00000 -1.50000 H2DB 2 0.872919 0.664524 0.455835 21.00000 -1.50000 H2DC 2 0.789827 0.588610 0.419023 21.00000 -1.50000 AFIX 137 PART 0 PART 2 H2DD 2 0.808145 0.587119 0.413738 -21.00000 -1.50000 H2DE 2 0.826389 0.716489 0.427728 -21.00000 -1.50000 H2DF 2 0.921971 0.618253 0.455425 -21.00000 -1.50000 AFIX 0 PART 0 C1D 1 1.302570 0.707256 0.428901 11.00000 0.08848 0.09093 = 0.11019 -0.00108 -0.02417 -0.02281 PART 1 AFIX 137 H1DA 2 1.449222 0.688453 0.426511 21.00000 -1.50000 H1DB 2 1.275825 0.739887 0.455778 21.00000 -1.50000 H1DC 2 1.265242 0.762244 0.407843 21.00000 -1.50000 AFIX 137 PART 0 PART 2 H1DD 2 1.380240 0.646158 0.442001 -21.00000 -1.50000 H1DE 2 1.261981 0.763279 0.449364 -21.00000 -1.50000 H1DF 2 1.389070 0.743655 0.408267 -21.00000 -1.50000 AFIX 0 S1A 4 1.086430 0.652474 0.406287 -21.00000 0.06165 0.08988 = 0.07347 -0.00533 -0.00610 0.00188 HKLF 4 REM shelxl_a.res in P2(1)2(1)2(1) REM R1 = 0.0406 for 3823 Fo > 4sig(Fo) and 0.0450 for all 4521 data REM 295 parameters refined using 2 restraints END WGHT 0.0712 0.0000 REM Highest difference peak 0.263, deepest hole -0.172, 1-sigma level 0.036 Q1 1 0.9973 0.6140 0.4566 11.00000 0.05 0.26 Q2 1 0.5594 0.3708 0.1546 11.00000 0.05 0.21 Q3 1 0.6426 -0.0570 0.4726 11.00000 0.05 0.20 Q4 1 1.1380 0.2313 0.3722 11.00000 0.05 0.13 Q5 1 0.9433 0.6980 0.4596 11.00000 0.05 0.13 ; _shelx_res_checksum 15172 _shelx_hkl_file ; 0 0 -1 0.02 0.06 0 0 1 0.04 0.07 0 0 1 0.00 0.07 0 0 -2 17.19 1.12 0 0 -3 4.01 0.60 0 0 3 0.11 0.21 0 0 -4 363.13 5.96 0 0 4 350.75 7.03 0 0 -5 0.66 0.85 0 0 5 1.33 1.82 0 0 -6 3273.54 28.29 0 0 6 3220.56 31.51 0 0 -7 2.95 0.95 0 0 7 0.27 1.49 0 0 -8 7306.64 474.75 0 0 8 7498.65 488.14 0 0 -9 0.09 1.07 0 0 9 0.24 1.53 0 0 -10 1673.86 22.19 0 0 10 1585.49 24.55 0 0 -11 1.29 0.93 0 0 11 0.46 1.15 0 0 -12 3.02 1.30 0 0 12 3.33 1.60 0 0 -13 0.10 1.21 0 0 13 2.25 3.60 0 0 -14 2.66 3.31 0 0 14 5.13 2.23 0 0 -15 0.36 0.46 0 0 15 1.59 2.57 0 0 -16 103.40 7.60 0 0 16 120.75 10.18 0 0 -17 0.62 0.84 0 0 17 -0.19 2.70 0 0 -18 91.35 8.66 0 0 18 112.37 11.85 0 0 -19 1.21 1.02 0 0 19 3.81 3.80 0 0 20 220.06 16.77 0 0 -20 204.69 11.81 0 0 20 210.04 11.90 0 0 21 0.38 2.02 0 0 -21 0.40 0.55 0 0 -21 0.27 1.98 0 0 21 0.94 0.99 0 0 22 53.02 8.89 0 0 -22 47.25 3.86 0 0 -22 53.42 4.83 0 0 22 55.01 5.16 0 0 23 -0.25 2.55 0 0 -23 0.26 0.82 0 0 -23 4.07 3.27 0 0 23 1.51 1.24 0 0 24 511.30 31.97 0 0 24 434.42 21.59 0 0 -24 446.31 21.44 0 0 -24 497.79 24.96 0 0 24 530.57 26.37 0 0 25 1.23 2.13 0 0 25 0.93 1.05 0 0 -25 0.78 0.67 0 0 -25 -0.17 1.86 0 0 25 -0.90 2.88 0 0 26 658.96 37.00 0 0 26 602.08 26.01 0 0 -26 593.12 25.08 0 0 -26 651.94 31.14 0 0 26 708.36 50.98 0 0 27 0.18 2.27 0 0 27 0.41 1.35 0 0 -27 0.11 0.87 0 0 -27 0.80 1.35 0 0 27 -0.02 2.40 0 0 28 131.38 16.20 0 0 28 118.15 10.61 0 0 -28 134.37 12.67 0 0 28 154.65 18.44 0 0 29 0.72 2.90 0 0 29 -0.22 1.46 0 0 -29 0.33 1.10 0 0 29 0.37 1.64 0 0 30 4.65 1.63 0 0 -30 6.50 5.52 0 0 30 7.31 6.40 0 0 31 0.01 1.01 0 0 -31 0.24 1.09 0 0 31 0.24 0.75 0 0 32 5.33 2.72 0 0 -32 4.24 1.89 0 0 32 6.77 4.92 0 0 33 0.07 0.97 0 0 -33 0.53 1.70 0 0 33 0.26 0.73 0 0 34 0.31 1.34 0 0 -34 0.54 1.39 0 0 34 0.46 1.35 0 0 35 0.22 0.45 0 0 -35 0.30 1.52 0 0 35 1.22 1.45 0 0 36 46.56 2.95 0 0 -36 51.33 4.05 0 0 36 54.14 6.51 0 0 -37 0.57 1.13 0 0 37 0.16 0.59 0 0 -38 4.34 1.24 0 0 -39 0.14 0.54 0 1 1 2210.28 18.39 0 -1 2 320.80 5.30 0 1 2 337.03 6.14 0 -1 3 661.09 9.04 0 1 -4 577.69 7.17 0 -1 -4 648.89 10.70 0 -1 4 631.66 9.66 0 1 4 633.57 10.51 0 1 -5 109.35 5.58 0 -1 -5 109.44 6.39 0 -1 5 111.21 6.32 0 1 5 109.53 6.55 0 1 -6 757.63 9.87 0 -1 -6 773.91 13.03 0 -1 6 788.11 12.97 0 1 6 794.04 14.01 0 1 -7 54.61 3.53 0 -1 -7 53.29 4.13 0 -1 7 79.78 5.56 0 1 7 54.22 4.47 0 1 -8 5087.41 40.56 0 -1 -8 5241.17 46.55 0 -1 8 5432.49 49.65 0 1 8 5144.90 48.61 0 1 -9 148.25 8.03 0 -1 -9 155.31 9.29 0 -1 9 156.11 9.56 0 1 9 148.86 9.51 0 1 -10 1151.89 16.35 0 -1 -10 1203.68 20.18 0 -1 10 1217.71 21.55 0 1 10 1187.57 22.37 0 1 -11 1105.42 17.21 0 -1 -11 1128.78 20.09 0 -1 11 1162.59 22.03 0 1 11 1193.93 23.55 0 1 -12 664.09 13.18 0 -1 -12 675.13 16.29 0 -1 12 696.75 17.59 0 1 12 681.33 18.46 0 1 -13 1456.70 21.52 0 -1 -13 1433.35 26.21 0 -1 13 1412.23 27.33 0 1 13 1270.31 26.78 0 1 -14 618.66 13.70 0 -1 -14 613.64 19.90 0 -1 14 615.94 18.08 0 1 14 610.27 18.21 0 1 -15 787.08 16.41 0 -1 -15 822.78 20.08 0 -1 15 832.16 22.71 0 1 15 798.42 22.12 0 1 -16 42.66 4.22 0 -1 -16 44.33 5.21 0 -1 16 42.71 5.70 0 1 16 45.33 6.24 0 1 -17 5.26 1.52 0 -1 -17 5.46 2.36 0 -1 17 9.70 7.77 0 1 17 6.37 2.71 0 -1 -18 149.60 11.18 0 -1 18 163.74 13.12 0 1 18 161.11 13.27 0 -1 -19 323.26 19.93 0 -1 19 393.75 25.74 0 1 19 392.90 24.91 0 -1 -19 240.36 13.30 0 -1 19 366.81 19.26 0 1 19 369.40 18.92 0 -1 -20 35.90 4.88 0 -1 20 43.47 15.67 0 1 20 42.78 6.81 0 -1 20 33.32 3.04 0 1 -20 34.55 3.10 0 1 -20 35.16 3.44 0 -1 -20 34.41 3.77 0 -1 20 38.29 3.91 0 1 20 35.86 3.66 0 -1 -21 48.51 5.73 0 -1 21 55.74 7.68 0 1 21 56.42 9.94 0 -1 21 47.58 4.39 0 1 -21 49.13 3.98 0 -1 -21 52.86 4.00 0 1 -21 50.57 4.54 0 -1 -21 52.58 4.82 0 -1 21 54.91 4.81 0 1 21 50.35 4.51 0 -1 22 480.47 29.57 0 1 22 494.85 29.04 0 -1 22 416.14 18.00 0 1 -22 427.82 18.41 0 -1 -22 397.29 17.18 0 1 -22 453.04 20.00 0 -1 -22 445.21 20.38 0 -1 22 487.54 22.10 0 1 22 449.77 20.00 0 -1 23 0.43 2.47 0 1 23 0.14 2.41 0 -1 23 0.57 1.05 0 1 -23 3.61 2.76 0 -1 -23 0.45 0.59 0 1 -23 1.57 1.23 0 -1 -23 -0.36 2.06 0 -1 23 0.20 1.41 0 1 23 -0.18 1.95 0 1 24 238.39 19.27 0 -1 24 243.28 19.32 0 -1 24 200.54 12.53 0 -1 -24 189.58 11.39 0 1 -24 215.06 11.80 0 -1 -24 220.91 13.57 0 1 -24 216.94 15.73 0 -1 24 260.96 15.04 0 1 24 226.92 14.71 0 1 25 0.18 2.47 0 -1 25 0.47 2.02 0 -1 25 0.20 1.44 0 -1 -25 0.19 0.87 0 1 -25 0.27 1.07 0 -1 -25 -0.44 2.27 0 -1 25 -0.06 2.19 0 1 25 1.59 1.60 0 -1 26 687.13 52.92 0 1 26 688.71 53.85 0 -1 26 606.22 27.89 0 -1 -26 572.86 24.17 0 -1 -26 676.54 30.03 0 1 -26 671.91 30.53 0 -1 26 736.57 50.81 0 1 26 719.70 50.81 0 -1 27 99.83 13.17 0 1 27 100.62 13.26 0 -1 27 90.79 8.00 0 -1 -27 85.07 8.01 0 1 -27 88.11 8.45 0 -1 -27 96.30 9.32 0 -1 27 107.03 9.84 0 1 27 101.36 9.53 0 -1 28 8.63 12.19 0 1 28 12.29 8.77 0 -1 28 13.03 7.42 0 1 28 14.33 3.37 0 -1 -28 12.81 8.07 0 1 -28 16.45 8.64 0 -1 -28 14.44 4.16 0 1 28 17.85 11.12 0 -1 28 17.27 10.88 0 -1 29 17.66 19.77 0 1 29 19.09 17.15 0 -1 29 25.54 3.64 0 1 29 23.03 3.64 0 1 -29 25.12 7.72 0 -1 -29 25.28 4.63 0 -1 29 25.49 5.26 0 1 29 25.80 4.15 0 -1 30 36.38 4.06 0 1 30 38.05 4.58 0 1 -30 41.41 9.62 0 -1 -30 39.58 7.07 0 -1 30 40.62 5.15 0 1 30 50.42 6.44 0 -1 31 8.94 5.36 0 1 31 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18.08 2.90 -4 -7 -23 16.05 2.68 -4 7 -23 17.98 2.18 4 -7 -23 21.33 3.32 -4 7 -23 14.90 1.47 -4 -7 24 4.68 2.86 -4 -7 -24 4.56 4.09 -4 -7 -24 4.63 1.63 -4 7 -24 2.79 2.18 4 -7 -24 4.35 5.38 -4 -7 25 1.42 1.14 -4 -7 -25 1.23 1.12 -4 -7 -25 0.75 0.84 -4 7 -25 0.56 1.01 4 -7 -25 0.79 2.13 -4 -7 26 10.91 7.78 -4 -7 -26 10.58 2.02 -4 -7 -26 7.34 3.60 4 -7 -26 10.56 3.09 -4 -7 27 2.10 3.47 -4 -7 -27 2.30 2.90 -4 -7 -27 1.32 3.46 4 -7 -27 1.62 3.42 -4 -7 28 12.26 2.12 -4 -7 -28 9.57 2.54 4 -7 -28 10.81 1.95 -4 -8 0 161.62 14.08 -4 -8 0 163.74 12.99 -4 8 0 155.58 12.37 -4 8 0 171.70 16.00 -4 -8 -1 23.06 3.48 -4 -8 1 20.69 12.68 -4 -8 1 20.10 3.29 -4 -8 -1 22.16 3.43 -4 8 1 27.17 7.60 -4 8 -1 20.39 3.10 -4 8 -1 20.64 3.40 -4 8 1 23.77 3.44 -4 -8 -2 34.13 3.81 -4 -8 2 29.53 3.82 -4 -8 2 29.47 3.65 -4 -8 -2 34.49 4.21 -4 8 2 38.03 4.69 -4 8 -2 30.48 3.82 -4 8 2 35.65 5.17 -4 8 -2 30.28 3.30 -4 -8 -3 16.13 2.95 -4 -8 3 16.98 3.03 -4 -8 -3 17.75 3.31 -4 -8 3 15.24 2.87 -4 8 3 19.85 12.16 -4 8 -3 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193.50 13.71 -5 6 -8 202.90 13.20 -5 -6 -8 156.66 10.56 -5 6 8 219.52 16.46 -5 6 -8 201.01 13.19 -5 -6 9 8.80 5.83 -5 -6 -9 10.98 6.16 -5 6 9 10.17 6.45 -5 6 -9 13.58 6.91 -5 -6 -9 7.73 6.77 -5 6 9 14.38 10.14 -5 6 -9 13.13 7.76 -5 -6 10 34.54 4.04 -5 -6 -10 35.00 4.47 -5 6 10 34.50 3.83 -5 6 -10 43.80 5.62 -5 -6 -10 32.25 3.97 -5 6 10 40.31 4.95 -5 6 -10 40.88 4.67 -5 -6 11 18.47 2.81 -5 -6 -11 19.89 9.85 -5 6 -11 22.42 3.30 -5 -6 -11 18.21 2.97 -5 6 11 19.36 3.32 -5 6 -11 21.47 3.12 -5 -6 12 17.08 3.82 -5 -6 -12 16.88 11.21 -5 6 -12 21.25 2.67 -5 -6 -12 14.55 2.24 -5 6 -12 20.11 2.89 -5 6 12 20.25 10.00 -5 6 -12 19.44 2.66 -5 -6 13 1.64 1.44 -5 -6 -13 2.10 2.35 -5 6 -13 2.35 1.58 -5 -6 -13 1.62 1.54 -5 6 -13 1.20 1.40 -5 6 13 1.98 1.49 -5 6 -13 1.37 1.84 5 -6 -13 1.02 1.36 -5 -6 -14 33.01 3.76 -5 6 -14 34.84 3.41 -5 -6 -14 32.34 4.04 -5 6 -14 33.21 3.26 -5 6 14 41.51 4.32 -5 6 -14 29.40 2.83 -5 -6 15 4.96 3.40 -5 -6 -15 4.56 4.34 -5 6 -15 6.02 3.68 -5 -6 -15 4.22 4.43 -5 6 -15 4.70 3.07 -5 6 15 10.81 8.45 -5 6 -15 4.11 1.30 -5 -6 16 20.99 2.67 -5 -6 -16 17.33 2.92 -5 6 -16 24.71 4.90 -5 -6 -16 16.02 2.60 -5 6 -16 24.36 2.86 -5 6 16 19.57 3.69 -5 6 -16 20.97 2.32 -5 -6 17 5.19 2.97 -5 -6 -17 4.71 3.14 -5 6 -17 5.15 3.31 -5 -6 -17 3.97 4.69 -5 6 -17 4.40 3.66 -5 6 17 5.09 4.31 -5 -6 18 39.48 3.38 -5 -6 -18 39.31 3.83 -5 6 -18 40.37 3.00 -5 -6 -18 37.62 4.22 -5 6 -18 41.69 3.51 -5 6 18 38.51 3.57 -5 6 -18 36.38 2.86 -5 -6 19 8.44 4.38 -5 -6 -19 9.52 7.31 -5 6 -19 8.63 4.78 -5 -6 -19 10.27 1.92 -5 6 -19 9.51 5.68 -5 6 -19 8.76 1.53 -5 -6 20 4.39 2.45 -5 -6 -20 3.90 5.10 -5 6 -20 4.82 1.17 -5 -6 -20 4.17 1.50 -5 6 -20 4.11 3.41 -5 6 -20 4.23 1.85 -5 -6 21 2.63 2.46 -5 -6 -21 2.97 2.20 -5 6 -21 2.11 2.51 -5 -6 -21 2.56 1.77 -5 6 -21 2.77 2.76 5 -6 -21 2.65 3.06 -5 6 -21 2.40 2.15 -5 -6 22 2.59 2.77 -5 -6 -22 2.33 2.48 -5 6 -22 1.85 3.16 -5 -6 -22 1.97 2.36 -5 6 -22 3.16 3.35 5 -6 -22 3.47 5.20 -5 6 -22 2.61 3.06 -5 -6 23 23.79 3.58 -5 -6 -23 23.51 3.46 -5 6 -23 23.30 2.55 -5 -6 -23 23.12 3.25 -5 6 -23 25.30 2.98 5 -6 -23 25.00 3.59 -5 6 -23 24.66 2.81 -5 -6 24 1.36 3.26 -5 -6 -24 2.33 2.24 -5 -6 -24 2.24 1.02 5 -6 -24 2.05 3.52 -5 6 -24 3.14 0.79 -5 -6 -25 25.01 3.35 -5 -6 -25 20.57 2.72 5 -6 -25 23.39 3.22 -5 -7 0 40.01 4.65 -5 7 0 39.35 4.42 -5 7 0 43.11 4.82 -5 -7 1 1.41 1.02 -5 -7 -1 1.53 1.89 -5 7 -1 1.75 1.75 -5 7 1 2.23 1.31 -5 7 -1 2.90 2.15 -5 7 1 2.65 2.00 -5 -7 -2 79.26 7.56 -5 7 -2 88.54 7.97 -5 7 2 73.65 6.82 -5 7 -2 92.74 8.71 -5 7 2 84.96 8.74 -5 -7 3 6.32 8.00 -5 -7 -3 8.77 7.61 -5 7 3 10.86 6.41 -5 7 -3 10.69 6.24 -5 7 -3 14.44 8.59 -5 7 3 11.46 8.53 -5 -7 -4 32.03 4.13 -5 7 4 35.26 4.37 -5 7 -4 31.64 5.09 -5 7 4 34.86 4.41 -5 7 -4 30.12 4.00 -5 -7 -5 11.14 6.50 -5 7 5 10.75 5.43 -5 7 -5 10.88 4.54 -5 7 5 11.65 7.24 -5 7 -5 10.11 5.81 -5 -7 6 93.15 5.22 -5 -7 -6 104.55 6.01 -5 7 6 117.65 7.34 -5 7 -6 121.08 5.98 -5 7 6 128.01 8.19 -5 7 -6 109.32 5.47 -5 -7 7 10.86 2.05 -5 -7 -7 13.00 2.75 -5 7 7 13.17 2.48 -5 7 -7 14.07 7.98 -5 7 7 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0.99 -7 6 -6 0.19 0.38 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 1549 _olex2_submission_special_instructions 'No special instructions were received'