data_C8OBTBTOC8rtHB _publ_section_title ; DFT-assisted polymorph identification from lattice Raman fingerprinting ; _publ_contact_author_name 'Nicola Demitri' _publ_contact_author_address ; Elettra-Sincrotrone Trieste, S.S. 14 Km 163.5 in Area Science Park, 34149 Basovizza - Trieste, Italy. ; _publ_contact_author_email nicola.demitri@elettra.eu _publ_contact_author_phone '+39 040 375 8084' loop_ _publ_author_name _publ_author_address 'Bedoya-Martinez, Natalia' ; Institute of Solid State Physics Graz University of Technology Petersgasse 16, 8010 Graz, Austria. ; 'Schrode, Benedikt' ; Institute of Solid State Physics Graz University of Technology Petersgasse 16, 8010 Graz, Austria. ; 'Jones, Andrew O.F.' ; Institute of Solid State Physics Graz University of Technology Petersgasse 16, 8010 Graz, Austria. ; 'Salzillo, Tommaso' ; Department of Industrial Chemistry Toso Montanari, University of Bologna, Viale Risorgimento 4, I-40136 Bologna, Italy. ; 'Ruzie, Christian' ; Laboratoire de Chimie des Polymeres, Faculte des Sciences, Universite Libre de Bruxelles, CP206/01, Campus de la Plaine, 1050 Brussels, Belgium. ; 'Demitri, Nicola' ; Elettra-Sincrotrone Trieste, S.S. 14 Km 163.5 in Area Science Park, 34149 Basovizza - Trieste, Italy. ; 'Geerts, Yves H.' ; Laboratoire de Chimie des Polymeres, Faculte des Sciences, Universite Libre de Bruxelles, CP206/01, Campus de la Plaine, 1050 Brussels, Belgium. ; 'Venuti, Elisabetta' ; Department of Industrial Chemistry Toso Montanari, University of Bologna, Viale Risorgimento 4, I-40136 Bologna, Italy. ; 'Della Valle, Raffaele Guido' ; Department of Industrial Chemistry Toso Montanari, University of Bologna, Viale Risorgimento 4, I-40136 Bologna, Italy. ; 'Zojer, Egbert' ; Institute of Solid State Physics Graz University of Technology Petersgasse 16, 8010 Graz, Austria. ; 'Resel, Roland' ; Institute of Solid State Physics Graz University of Technology Petersgasse 16, 8010 Graz, Austria. ; _publ_contact_letter ; Please consider this CIF for publication. I certify that this contibution is the original work of those listed as authors; that it has not been published before (in any language or medium) and is not being considered for publication elsewhere; that all authors concur with and are aware of the submission; that all workers involved in the study are listed as authors or given proper credit in the acknowledgements; that I have obtained permission for and acknowledged the source of any excerpts from other copyright works; and that to the best of my knowledge the paper contains no statements which are libellous, unlawful or in any way actionable. All coauthors have made significant scientific contributions to the work reported, including the ideas and their execution, and share responsibility and accountability for the results. ; _publ_section_abstract ; The structure of C8OBTBTOC8, C~60~H~80~O~4~S~4~, at 298 K has monoclinic (P2~1~(/c) symmetry. Crystals showed significant radiation damage and poor diffraction limit. ; _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H80 O4 S4' _chemical_formula_sum 'C60 H80 O4 S4' _chemical_formula_weight 993.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0030 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1218 0.1208 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 31.056(6) _cell_length_b 7.663(2) _cell_length_c 5.996(1) _cell_angle_alpha 90 _cell_angle_beta 94.18(3) _cell_angle_gamma 90 _cell_volume 1423.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 321 _cell_measurement_theta_min 1.295 _cell_measurement_theta_max 16.664 _exptl_crystal_description 'Thin plates' _exptl_crystal_colour 'Colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_F_000 536 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 0.200 _shelx_estimated_absorpt_T_min 0.984 _shelx_estimated_absorpt_T_max 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4747 _exptl_absorpt_correction_T_max 0.7442 _exptl_absorpt_process_details 'SADABS v2012/1 (Bruker, 2012)' _exptl_special_details ; SADABS was used to perform the Absorption correction. Parameters refinement is based on 3334 reflections. Ratio of minimum to maximum apparent transmission: 0.63787 The given Tmin and Tmax were generated using the SHELX SIZE command ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.700 _diffrn_measurement_method 'Rotating crystal' _diffrn_radiation_type Synchrotron _diffrn_source 'Elettra Synchrotron - XRD1 BL' _diffrn_measurement_device_type ; 'Huber 4-circles Kappa Goniometer, Pilatus 2M detector' ; _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2641 _diffrn_reflns_av_unetI/netI 0.1679 _diffrn_reflns_av_R_equivalents 0.1461 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.295 _diffrn_reflns_theta_max 16.664 _diffrn_reflns_theta_full 16.664 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measured_fraction_theta_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_point_group_measured_fraction_full 0.984 _reflns_number_total 806 _reflns_number_gt 473 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _computing_data_collection 'Elettra XRD1 Data Collection SW' _computing_cell_refinement 'XDS (Kabsch, 2010)' _computing_data_reduction 'XDS (Kabsch, 2010)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2016 (Sheldrick, 2015)' _computing_molecular_graphics 'Ortep3 for Windows - Coot' _computing_publication_material 'enCIFer - publCIF' _refine_special_details ; Hydrogen atoms were included at calculated positions with isotropic Ufactors=1.2Ueq (Ufactors=1.5Ueq for methyl). Anisotropic thermal motion modeling as then been applied only to S and O atoms. ; _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^)+(0.1440P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 806 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0951 _refine_ls_wR_factor_ref 0.2835 _refine_ls_wR_factor_gt 0.2388 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 C22_1 C 0.9524(9) 0.512(4) 0.221(5) 0.294(15) Uiso 1 1 d . . . . . H22A_1 H 0.965768 0.463868 0.095120 0.441 Uiso 1 1 calc R U . . . H22B_1 H 0.953582 0.636972 0.214830 0.441 Uiso 1 1 calc R U . . . H22C_1 H 0.967347 0.471761 0.356847 0.441 Uiso 1 1 calc R U . . . C21_1 C 0.9078(7) 0.456(3) 0.214(4) 0.217(10) Uiso 1 1 d . . . . . H21A_1 H 0.906627 0.329861 0.217410 0.261 Uiso 1 1 calc R U . . . H21B_1 H 0.892844 0.495289 0.075207 0.261 Uiso 1 1 calc R U . . . C20_1 C 0.8853(6) 0.530(3) 0.411(3) 0.162(7) Uiso 1 1 d . . . . . H20A_1 H 0.900822 0.494200 0.550097 0.195 Uiso 1 1 calc R U . . . H20B_1 H 0.885665 0.656591 0.405149 0.195 Uiso 1 1 calc R U . . . C19_1 C 0.8395(5) 0.467(2) 0.407(3) 0.141(6) Uiso 1 1 d . . . . . H19A_1 H 0.839539 0.340269 0.407972 0.169 Uiso 1 1 calc R U . . . H19B_1 H 0.824289 0.504366 0.267899 0.169 Uiso 1 1 calc R U . . . C18_1 C 0.8153(5) 0.531(2) 0.600(3) 0.127(6) Uiso 1 1 d . . . . . H18A_1 H 0.830889 0.495056 0.738100 0.152 Uiso 1 1 calc R U . . . H18B_1 H 0.815317 0.658067 0.597446 0.152 Uiso 1 1 calc R U . . . C17_1 C 0.7692(5) 0.470(2) 0.603(2) 0.123(5) Uiso 1 1 d . . . . . H17A_1 H 0.752505 0.518205 0.474205 0.147 Uiso 1 1 calc R U . . . H17B_1 H 0.768576 0.343682 0.587980 0.147 Uiso 1 1 calc R U . . . C16_1 C 0.7482(5) 0.519(2) 0.809(2) 0.113(5) Uiso 1 1 d . . . . . H16A_1 H 0.764585 0.469250 0.937618 0.136 Uiso 1 1 calc R U . . . H16B_1 H 0.749185 0.645170 0.825323 0.136 Uiso 1 1 calc R U . . . C15_1 C 0.7025(4) 0.461(2) 0.812(2) 0.106(5) Uiso 1 1 d . . . . . H15A_1 H 0.685153 0.516618 0.690622 0.127 Uiso 1 1 calc R U . . . H15B_1 H 0.700745 0.335775 0.790984 0.127 Uiso 1 1 calc R U . . . S1_1 S 0.52753(11) 0.3905(5) 0.7247(5) 0.0854(19) Uani 1 1 d . . . . . O1_1 O 0.6869(3) 0.5082(13) 1.0216(13) 0.107(3) Uani 1 1 d . . . . . C6_1 C 0.6435(5) 0.5079(19) 1.038(2) 0.088(4) Uiso 1 1 d . . . . . C5_1 C 0.6128(4) 0.4387(16) 0.876(2) 0.085(4) Uiso 1 1 d . . . . . H5_1 H 0.621399 0.385734 0.747412 0.102 Uiso 1 1 calc R U . . . C7_1 C 0.6299(4) 0.5828(16) 1.2354(19) 0.083(4) Uiso 1 1 d . . . . . H7_1 H 0.650297 0.626568 1.342426 0.099 Uiso 1 1 calc R U . . . C8_1 C 0.5879(4) 0.5914(16) 1.2700(19) 0.079(4) Uiso 1 1 d . . . . . H8_1 H 0.579510 0.635846 1.404554 0.095 Uiso 1 1 calc R U . . . C3_1 C 0.5559(4) 0.5345(15) 1.1062(18) 0.070(4) Uiso 1 1 d . . . . . C4_1 C 0.5700(4) 0.4518(16) 0.9145(18) 0.073(4) Uiso 1 1 d . . . . . C2_1 C 0.5105(4) 0.5331(15) 1.0950(16) 0.074(4) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1_1 0.114(3) 0.076(3) 0.066(2) -0.0046(19) 0.0030(17) 0.003(2) O1_1 0.108(8) 0.133(9) 0.079(6) -0.009(5) 0.000(5) 0.000(6) _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 C22_1 C21_1 1.44(3) . ? C22_1 H22A_1 0.9600 . ? C22_1 H22B_1 0.9600 . ? C22_1 H22C_1 0.9600 . ? C21_1 C20_1 1.53(2) . ? C21_1 H21A_1 0.9700 . ? C21_1 H21B_1 0.9700 . ? C20_1 C19_1 1.50(2) . ? C20_1 H20A_1 0.9700 . ? C20_1 H20B_1 0.9700 . ? C19_1 C18_1 1.510(18) . ? C19_1 H19A_1 0.9700 . ? C19_1 H19B_1 0.9700 . ? C18_1 C17_1 1.510(19) . ? C18_1 H18A_1 0.9700 . ? C18_1 H18B_1 0.9700 . ? C17_1 C16_1 1.491(16) . ? C17_1 H17A_1 0.9700 . ? C17_1 H17B_1 0.9700 . ? C16_1 C15_1 1.486(17) . ? C16_1 H16A_1 0.9700 . ? C16_1 H16B_1 0.9700 . ? C15_1 O1_1 1.429(14) . ? C15_1 H15A_1 0.9700 . ? C15_1 H15B_1 0.9700 . ? S1_1 C4_1 1.741(12) . ? S1_1 C2_1 1.759(12) 3_667 ? O1_1 C6_1 1.359(15) . ? C6_1 C7_1 1.407(15) . ? C6_1 C5_1 1.413(17) . ? C5_1 C4_1 1.369(15) . ? C5_1 H5_1 0.9300 . ? C7_1 C8_1 1.339(14) . ? C7_1 H7_1 0.9300 . ? C8_1 C3_1 1.413(15) . ? C8_1 H8_1 0.9300 . ? C3_1 C2_1 1.407(14) . ? C3_1 C4_1 1.409(14) . ? C2_1 C2_1 1.37(2) 3_667 ? 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 C21_1 C22_1 H22A_1 109.5 . . ? C21_1 C22_1 H22B_1 109.5 . . ? H22A_1 C22_1 H22B_1 109.5 . . ? C21_1 C22_1 H22C_1 109.5 . . ? H22A_1 C22_1 H22C_1 109.5 . . ? H22B_1 C22_1 H22C_1 109.5 . . ? C22_1 C21_1 C20_1 111(2) . . ? C22_1 C21_1 H21A_1 109.4 . . ? C20_1 C21_1 H21A_1 109.4 . . ? C22_1 C21_1 H21B_1 109.4 . . ? C20_1 C21_1 H21B_1 109.4 . . ? H21A_1 C21_1 H21B_1 108.0 . . ? C19_1 C20_1 C21_1 110.6(17) . . ? C19_1 C20_1 H20A_1 109.5 . . ? C21_1 C20_1 H20A_1 109.5 . . ? C19_1 C20_1 H20B_1 109.5 . . ? C21_1 C20_1 H20B_1 109.5 . . ? H20A_1 C20_1 H20B_1 108.1 . . ? C20_1 C19_1 C18_1 113.8(14) . . ? C20_1 C19_1 H19A_1 108.8 . . ? C18_1 C19_1 H19A_1 108.8 . . ? C20_1 C19_1 H19B_1 108.8 . . ? C18_1 C19_1 H19B_1 108.8 . . ? H19A_1 C19_1 H19B_1 107.7 . . ? C17_1 C18_1 C19_1 115.6(14) . . ? C17_1 C18_1 H18A_1 108.4 . . ? C19_1 C18_1 H18A_1 108.4 . . ? C17_1 C18_1 H18B_1 108.4 . . ? C19_1 C18_1 H18B_1 108.4 . . ? H18A_1 C18_1 H18B_1 107.4 . . ? C16_1 C17_1 C18_1 113.7(13) . . ? C16_1 C17_1 H17A_1 108.8 . . ? C18_1 C17_1 H17A_1 108.8 . . ? C16_1 C17_1 H17B_1 108.8 . . ? C18_1 C17_1 H17B_1 108.8 . . ? H17A_1 C17_1 H17B_1 107.7 . . ? C15_1 C16_1 C17_1 114.0(12) . . ? C15_1 C16_1 H16A_1 108.8 . . ? C17_1 C16_1 H16A_1 108.8 . . ? C15_1 C16_1 H16B_1 108.8 . . ? C17_1 C16_1 H16B_1 108.8 . . ? H16A_1 C16_1 H16B_1 107.7 . . ? O1_1 C15_1 C16_1 108.5(11) . . ? O1_1 C15_1 H15A_1 110.0 . . ? C16_1 C15_1 H15A_1 110.0 . . ? O1_1 C15_1 H15B_1 110.0 . . ? C16_1 C15_1 H15B_1 110.0 . . ? H15A_1 C15_1 H15B_1 108.4 . . ? C4_1 S1_1 C2_1 91.1(5) . 3_667 ? C6_1 O1_1 C15_1 117.8(10) . . ? O1_1 C6_1 C7_1 114.8(12) . . ? O1_1 C6_1 C5_1 125.1(12) . . ? C7_1 C6_1 C5_1 120.1(14) . . ? C4_1 C5_1 C6_1 118.3(12) . . ? C4_1 C5_1 H5_1 120.9 . . ? C6_1 C5_1 H5_1 120.9 . . ? C8_1 C7_1 C6_1 120.3(12) . . ? C8_1 C7_1 H7_1 119.8 . . ? C6_1 C7_1 H7_1 119.8 . . ? C7_1 C8_1 C3_1 121.4(11) . . ? C7_1 C8_1 H8_1 119.3 . . ? C3_1 C8_1 H8_1 119.3 . . ? C2_1 C3_1 C4_1 109.0(10) . . ? C2_1 C3_1 C8_1 133.3(11) . . ? C4_1 C3_1 C8_1 117.6(11) . . ? C5_1 C4_1 C3_1 122.1(11) . . ? C5_1 C4_1 S1_1 124.7(9) . . ? C3_1 C4_1 S1_1 113.0(9) . . ? C2_1 C2_1 C3_1 117.3(13) 3_667 . ? C2_1 C2_1 S1_1 109.5(12) 3_667 3_667 ? C3_1 C2_1 S1_1 133.2(8) . 3_667 ? 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_1 C21_1 C20_1 C19_1 -178(2) . . . . ? C21_1 C20_1 C19_1 C18_1 178.8(17) . . . . ? C20_1 C19_1 C18_1 C17_1 -179.5(14) . . . . ? C19_1 C18_1 C17_1 C16_1 173.2(14) . . . . ? C18_1 C17_1 C16_1 C15_1 179.1(13) . . . . ? C17_1 C16_1 C15_1 O1_1 177.0(12) . . . . ? C16_1 C15_1 O1_1 C6_1 163.6(11) . . . . ? C15_1 O1_1 C6_1 C7_1 -169.9(12) . . . . ? C15_1 O1_1 C6_1 C5_1 10.6(19) . . . . ? O1_1 C6_1 C5_1 C4_1 -178.5(12) . . . . ? C7_1 C6_1 C5_1 C4_1 2.0(19) . . . . ? O1_1 C6_1 C7_1 C8_1 179.4(11) . . . . ? C5_1 C6_1 C7_1 C8_1 -1.0(19) . . . . ? C6_1 C7_1 C8_1 C3_1 -3.3(19) . . . . ? C7_1 C8_1 C3_1 C2_1 -177.8(12) . . . . ? C7_1 C8_1 C3_1 C4_1 6.3(18) . . . . ? C6_1 C5_1 C4_1 C3_1 1.3(18) . . . . ? C6_1 C5_1 C4_1 S1_1 174.5(9) . . . . ? C2_1 C3_1 C4_1 C5_1 177.9(10) . . . . ? C8_1 C3_1 C4_1 C5_1 -5.3(18) . . . . ? C2_1 C3_1 C4_1 S1_1 4.0(13) . . . . ? C8_1 C3_1 C4_1 S1_1 -179.3(9) . . . . ? C2_1 S1_1 C4_1 C5_1 -176.1(11) 3_667 . . . ? C2_1 S1_1 C4_1 C3_1 -2.3(10) 3_667 . . . ? C4_1 C3_1 C2_1 C2_1 -4.2(18) . . . 3_667 ? C8_1 C3_1 C2_1 C2_1 179.7(14) . . . 3_667 ? C4_1 C3_1 C2_1 S1_1 179.0(10) . . . 3_667 ? C8_1 C3_1 C2_1 S1_1 3(2) . . . 3_667 ? _refine_diff_density_max 0.331 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.064 _shelx_res_file ; TITL sxs_a.res in P2(1)/c C8OBTBTOC8RTP21c_4sad.res created by SHELXL-2016/6 at 19:01:10 on 20-Jun-2017 REM Old TITL sxs in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.214, Rweak 0.012, Alpha 0.054, Orientation as input REM Formula found by SHELXT: C15 O S CELL 0.70000 31.05600 7.66300 5.99600 90.0000 94.1780 90.0000 ZERR 1.00 0.00621 0.00153 0.00120 0.0000 0.0300 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O S DISP H 0.00000 0.00000 0.67 DISP C 0.00299 0.00157 10.98 DISP O 0.01046 0.00590 30.82 DISP S 0.12182 0.12075 501.69 UNIT 60 80 4 4 rem simu 0.001 rem simu_$O 0.001 rem simu_$N 0.001 MERG 2 FMAP 2 PLAN 25 L.S. 8 shel 180 1.22 wpdb -2 acta list 4 conf bond $h size 0.08 0.02 0.01 temp 25 rem hfix_drg 33 c22 rem hfix_drg 23 c15 c16 c17 c18 c19 c20 c21 rem hfix_drg 43 c5 c7 c8 REM Omit extracted on Mon Jan 2 19:20:48 2017 omit 1 0 0 WGHT 0.144000 FVAR 0.13110 RESI 1 DRG C22 1 0.952369 0.511890 0.220743 11.00000 0.29376 AFIX 33 H22A 2 0.965768 0.463868 0.095120 11.00000 -1.50000 H22B 2 0.953582 0.636972 0.214830 11.00000 -1.50000 H22C 2 0.967347 0.471761 0.356847 11.00000 -1.50000 AFIX 0 C21 1 0.907839 0.456310 0.213868 11.00000 0.21735 AFIX 23 H21A 2 0.906627 0.329861 0.217410 11.00000 -1.20000 H21B 2 0.892844 0.495289 0.075207 11.00000 -1.20000 AFIX 0 C20 1 0.885345 0.530111 0.411317 11.00000 0.16247 AFIX 23 H20A 2 0.900822 0.494200 0.550097 11.00000 -1.20000 H20B 2 0.885665 0.656591 0.405149 11.00000 -1.20000 AFIX 0 C19 1 0.839506 0.466847 0.406656 11.00000 0.14111 AFIX 23 H19A 2 0.839539 0.340269 0.407972 11.00000 -1.20000 H19B 2 0.824289 0.504366 0.267899 11.00000 -1.20000 AFIX 0 C18 1 0.815291 0.531499 0.599892 11.00000 0.12691 AFIX 23 H18A 2 0.830889 0.495056 0.738100 11.00000 -1.20000 H18B 2 0.815317 0.658067 0.597446 11.00000 -1.20000 AFIX 0 C17 1 0.769159 0.469733 0.602689 11.00000 0.12278 AFIX 23 H17A 2 0.752505 0.518205 0.474205 11.00000 -1.20000 H17B 2 0.768576 0.343682 0.587980 11.00000 -1.20000 AFIX 0 C16 1 0.748157 0.519241 0.809405 11.00000 0.11311 AFIX 23 H16A 2 0.764585 0.469250 0.937618 11.00000 -1.20000 H16B 2 0.749185 0.645170 0.825323 11.00000 -1.20000 AFIX 0 C15 1 0.702548 0.461187 0.811545 11.00000 0.10580 AFIX 23 H15A 2 0.685153 0.516618 0.690622 11.00000 -1.20000 H15B 2 0.700745 0.335775 0.790984 11.00000 -1.20000 AFIX 0 S1 4 0.527530 0.390549 0.724719 11.00000 0.11388 0.07569 = 0.06598 -0.00458 0.00303 0.00310 O1 3 0.686905 0.508241 1.021640 11.00000 0.10842 0.13313 = 0.07930 -0.00857 0.00050 -0.00024 C6 1 0.643482 0.507911 1.038046 11.00000 0.08820 C5 1 0.612764 0.438740 0.876359 11.00000 0.08498 AFIX 43 H5 2 0.621399 0.385734 0.747412 11.00000 -1.20000 AFIX 0 C7 1 0.629934 0.582818 1.235415 11.00000 0.08271 AFIX 43 H7 2 0.650297 0.626568 1.342426 11.00000 -1.20000 AFIX 0 C8 1 0.587875 0.591447 1.269980 11.00000 0.07885 AFIX 43 H8 2 0.579510 0.635846 1.404554 11.00000 -1.20000 AFIX 0 C3 1 0.555936 0.534481 1.106194 11.00000 0.07000 C4 1 0.569952 0.451796 0.914502 11.00000 0.07345 C2 1 0.510525 0.533094 1.095037 11.00000 0.07365 HKLF 4 REM sxs_a.res in P2(1)/c REM R1 = 0.0951 for 473 Fo > 4sig(Fo) and 0.1465 for all 806 data REM 79 parameters refined using 0 restraints END WGHT 0.1440 0.0000 REM Highest difference peak 0.331, deepest hole -0.250, 1-sigma level 0.064 Q1 1 0.4728 0.5398 1.0849 11.00000 0.05 0.33 Q2 1 0.5544 0.6179 1.3183 11.00000 0.05 0.31 Q3 1 0.5000 0.5000 0.5000 10.50000 0.05 0.25 Q4 1 0.5815 0.3911 0.7261 11.00000 0.05 0.24 Q5 1 0.5806 0.5155 1.0216 11.00000 0.05 0.21 Q6 1 0.5063 0.7606 0.9976 11.00000 0.05 0.19 Q7 1 0.6251 0.5082 1.0485 11.00000 0.05 0.18 Q8 1 0.6407 0.4503 0.8483 11.00000 0.05 0.17 Q9 1 0.6928 0.3919 0.5239 11.00000 0.05 0.16 Q10 1 0.8374 0.3158 0.4760 11.00000 0.05 0.15 Q11 1 0.5568 0.2378 0.9456 11.00000 0.05 0.15 Q12 1 0.9560 0.3485 0.2193 11.00000 0.05 0.15 Q13 1 0.8867 0.7307 0.5150 11.00000 0.05 0.14 Q14 1 0.6529 0.6412 1.4597 11.00000 0.05 0.14 Q15 1 0.7599 0.5464 1.0431 11.00000 0.05 0.14 Q16 1 0.9003 0.3315 0.5414 11.00000 0.05 0.13 Q17 1 0.8934 0.3754 0.4953 11.00000 0.05 0.13 Q18 1 0.5285 0.3632 1.2290 11.00000 0.05 0.12 Q19 1 0.6900 0.7417 0.5669 11.00000 0.05 0.12 Q20 1 0.7563 0.4413 0.9413 11.00000 0.05 0.12 Q21 1 0.7093 0.5258 1.2256 11.00000 0.05 0.12 Q22 1 0.9184 0.3606 0.3168 11.00000 0.05 0.12 Q23 1 0.5279 0.6666 0.7041 11.00000 0.05 0.11 Q24 1 0.7715 0.7052 0.9842 11.00000 0.05 0.11 Q25 1 0.7394 0.4985 0.3409 11.00000 0.05 0.11 ; _shelx_res_checksum 73359 _shelx_hkl_file ; 0 0 1 0.86 0.22 0 0 2 23.22 4.86 0 1 0 -0.28 0.36 0 -1 0 -0.18 0.39 0 1 1 31.38 6.58 0 1 1 36.39 7.65 0 1 -1 48.99 10.25 0 -1 1 51.21 10.72 0 1 2 -0.03 0.44 0 1 -2 0.03 0.32 0 1 2 0.77 0.34 0 -1 2 -0.15 0.33 0 1 3 1.22 0.32 0 1 -3 1.05 0.32 0 1 3 1.13 0.30 0 -1 3 0.57 0.35 0 1 -4 1.42 0.51 0 1 -4 2.43 0.56 0 2 0 1000.00 209.09 0 -2 0 825.93 172.65 0 2 1 137.85 28.84 0 2 -1 154.54 32.33 0 -2 1 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0.47 0.62 25 0 0 0.79 0.67 25 0 1 -0.13 0.66 -25 0 -1 -1.11 0.73 -25 1 2 0.06 0.73 25 1 -2 0.25 0.68 25 -1 -2 1.35 0.74 25 1 -1 2.96 0.97 -25 1 1 2.16 0.84 -25 -1 1 2.36 0.87 25 -1 -1 3.98 1.11 25 1 0 0.87 0.64 -25 1 0 1.85 0.72 25 -1 0 0.77 0.76 -25 -1 0 0.71 0.73 25 1 1 2.81 0.88 -25 1 -1 3.66 0.99 25 -1 1 2.98 0.89 -25 -1 -1 3.26 1.00 25 2 -1 0.81 0.71 -25 2 1 0.94 0.63 -25 -2 1 -0.74 0.99 25 -2 -1 1.08 0.80 -25 2 0 0.45 0.68 25 2 0 -0.77 0.64 -25 -2 0 -0.63 0.93 25 -2 0 -0.06 0.66 -26 0 1 -0.04 0.64 26 0 -1 -0.62 0.68 -26 0 0 2.11 0.83 26 0 0 0.15 0.65 -26 1 1 0.97 0.75 26 1 -1 -0.17 0.63 -26 -1 1 -0.88 0.87 26 -1 -1 -0.11 0.63 -26 1 0 2.16 0.81 26 1 0 1.74 0.84 -26 -1 0 1.41 0.88 26 -1 0 0.71 0.67 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 7754 # start Validation Reply Form _vrf_PLAT023_C8OBTBTOC8rtHB ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 16.66 Degree RESPONSE: Crystals diffracted poorly at RT (best ones show reflections at a maximum resolution of ~1.25 Ang). Radiation damage have been found and limited the maximum dose allowed per data collection. ; _vrf_THETM01_C8OBTBTOC8rtHB ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.4097 RESPONSE: Crystals diffracted poorly at RT (best ones show reflections at a maximum resolution of ~1.25 Ang). Radiation damage have been found and limited the maximum dose allowed per data collection. ; _vrf_PLAT201_C8OBTBTOC8rtHB ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 15 RESPONSE: Crystals diffracted poorly at RT (best ones show reflections at a maximum resolution of ~1.25 Ang), so few data were available for refinement. Number of model parameters have been kept low to avoid overrefinement. Anisotropic thermal motion modelling have been applied only to sulphur and oxygen atoms. ; _vrf_PLAT340_C8OBTBTOC8rtHB ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0204 Ang. RESPONSE: Crystals diffracted poorly at RT (best ones show reflections at a maximum resolution of ~1.25 Ang) and were prone to radiation damage. This error is due to high model e.s.d., mainly found on terminal atoms of flexible hydrocarburic tails. ; # end Validation Reply Form