# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sc0942 #TrackingRef '1_DTT-8.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C36 H44 S3' _chemical_formula_moiety 'C36 H44 S3' _chemical_formula_weight 572.92 _chemical_melting_point ? _chemical_absolute_configuration ad #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,+Z 3 +X,-Y,1/2+Z 4 -X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,+Z 7 1/2+X,1/2-Y,1/2+Z 8 1/2-X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 70.25(3) _cell_length_b 7.333(3) _cell_length_c 5.822(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 2999(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3491 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 25.30 _cell_measurement_temperature 93 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.269 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232.00 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.720 _exptl_absorpt_correction_T_max 0.995 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 93 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.111 _diffrn_reflns_number 5010 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 84 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 6 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2435 _reflns_number_gt 2315 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1050 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2435 _refine_ls_number_parameters 179 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.002 _refine_diff_density_max 0.370 _refine_diff_density_min -0.330 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 921 Friedel Pairs' _refine_ls_abs_structure_Flack 0.07(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.0000 0.65344(11) 1.13933(15) 0.0133(3) Uani 1.0 4 d . . . S2 S 0.971763(7) 0.82756(7) 0.54713(13) 0.01317(19) Uani 1.0 8 d . . . C1 C 0.98989(3) 0.7816(3) 0.7394(5) 0.0112(5) Uani 1.0 8 d . . . C2 C 0.98259(3) 0.7120(3) 0.9426(5) 0.0115(6) Uani 1.0 8 d . . . C3 C 0.96248(3) 0.6918(4) 0.9433(5) 0.0128(6) Uani 1.0 8 d . . . C4 C 0.95451(3) 0.7485(4) 0.7417(5) 0.0121(6) Uani 1.0 8 d . . . C5 C 0.93432(3) 0.7484(4) 0.6752(5) 0.0122(6) Uani 1.0 8 d . . . C6 C 0.92059(3) 0.6724(3) 0.8226(6) 0.0134(6) Uani 1.0 8 d . . . C7 C 0.90133(4) 0.6835(4) 0.7714(6) 0.0163(6) Uani 1.0 8 d . . . C8 C 0.89501(3) 0.7709(4) 0.5722(5) 0.0156(6) Uani 1.0 8 d . . . C9 C 0.90855(3) 0.8367(3) 0.4206(6) 0.0156(6) Uani 1.0 8 d . . . C10 C 0.92791(4) 0.8270(3) 0.4705(5) 0.0138(6) Uani 1.0 8 d . . . C11 C 0.87395(3) 0.8063(4) 0.5356(7) 0.0179(6) Uani 1.0 8 d . . . C12 C 0.86450(3) 0.7172(4) 0.3273(6) 0.0182(6) Uani 1.0 8 d . . . C13 C 0.84399(3) 0.7850(4) 0.2985(6) 0.0180(6) Uani 1.0 8 d . . . C14 C 0.83324(3) 0.7053(4) 0.0964(5) 0.0198(7) Uani 1.0 8 d . . . C15 C 0.81325(3) 0.7847(4) 0.0731(6) 0.0194(6) Uani 1.0 8 d . . . C16 C 0.80175(3) 0.7062(4) -0.1264(6) 0.0223(7) Uani 1.0 8 d . . . C17 C 0.78193(4) 0.7907(4) -0.1431(6) 0.0281(8) Uani 1.0 8 d . . . C18 C 0.76997(4) 0.7097(5) -0.3378(7) 0.0387(9) Uani 1.0 8 d . . . H3 H 0.9554 0.6444 1.0690 0.0153 Uiso 1.0 8 calc R . . H6 H 0.9246 0.6127 0.9592 0.0160 Uiso 1.0 8 calc R . . H7 H 0.8923 0.6310 0.8733 0.0196 Uiso 1.0 8 calc R . . H9 H 0.9045 0.8894 0.2796 0.0187 Uiso 1.0 8 calc R . . H10 H 0.9369 0.8744 0.3640 0.0165 Uiso 1.0 8 calc R . . H11A H 0.8721 0.9397 0.5233 0.0215 Uiso 1.0 8 calc R . . H11B H 0.8671 0.7652 0.6748 0.0215 Uiso 1.0 8 calc R . . H12A H 0.8645 0.5831 0.3469 0.0218 Uiso 1.0 8 calc R . . H12B H 0.8719 0.7463 0.1873 0.0218 Uiso 1.0 8 calc R . . H13A H 0.8368 0.7566 0.4407 0.0215 Uiso 1.0 8 calc R . . H13B H 0.8442 0.9193 0.2817 0.0215 Uiso 1.0 8 calc R . . H14A H 0.8323 0.5714 0.1155 0.0238 Uiso 1.0 8 calc R . . H14B H 0.8405 0.7296 -0.0465 0.0238 Uiso 1.0 8 calc R . . H15A H 0.8143 0.9183 0.0527 0.0233 Uiso 1.0 8 calc R . . H15B H 0.8062 0.7623 0.2178 0.0233 Uiso 1.0 8 calc R . . H16A H 0.8087 0.7282 -0.2718 0.0267 Uiso 1.0 8 calc R . . H16B H 0.8005 0.5727 -0.1061 0.0267 Uiso 1.0 8 calc R . . H17A H 0.7832 0.9237 -0.1677 0.0337 Uiso 1.0 8 calc R . . H17B H 0.7752 0.7721 0.0043 0.0337 Uiso 1.0 8 calc R . . H18A H 0.7681 0.5790 -0.3106 0.0464 Uiso 1.0 8 calc R . . H18B H 0.7766 0.7273 -0.4844 0.0464 Uiso 1.0 8 calc R . . H18C H 0.7576 0.7709 -0.3432 0.0464 Uiso 1.0 8 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0117(4) 0.0173(5) 0.0109(5) 0.0000 0.0000 0.0019(4) S2 0.0108(3) 0.0166(4) 0.0121(4) -0.0000(2) 0.0003(3) 0.0021(4) C1 0.0117(12) 0.0121(12) 0.0100(14) 0.0017(9) -0.0019(11) -0.0026(13) C2 0.0127(12) 0.0098(12) 0.0121(14) 0.0007(10) -0.0012(12) -0.0031(11) C3 0.0145(13) 0.0141(12) 0.0096(14) -0.0012(9) 0.0041(11) 0.0004(11) C4 0.0143(12) 0.0105(13) 0.0117(14) -0.0008(9) -0.0001(11) -0.0010(12) C5 0.0108(11) 0.0114(13) 0.0144(14) 0.0000(9) 0.0025(11) -0.0025(11) C6 0.0138(12) 0.0139(14) 0.0123(14) -0.0006(9) -0.0017(11) 0.0017(11) C7 0.0144(13) 0.0164(14) 0.0181(16) -0.0025(9) 0.0031(12) -0.0005(12) C8 0.0129(12) 0.0172(13) 0.0165(14) 0.0014(9) 0.0002(11) -0.0040(13) C9 0.0155(13) 0.0178(14) 0.0136(16) 0.0027(10) -0.0013(12) -0.0021(12) C10 0.0127(12) 0.0150(14) 0.0135(16) -0.0010(10) 0.0012(11) -0.0002(10) C11 0.0110(11) 0.0239(13) 0.0188(14) 0.0006(9) 0.0008(13) 0.0000(14) C12 0.0125(12) 0.0216(14) 0.0204(16) -0.0001(11) -0.0010(12) -0.0001(13) C13 0.0144(12) 0.0173(13) 0.0222(16) -0.0001(10) 0.0023(12) -0.0013(13) C14 0.0133(12) 0.0237(14) 0.0225(19) 0.0016(10) -0.0007(12) -0.0025(13) C15 0.0135(12) 0.0221(13) 0.0227(16) -0.0007(10) 0.0026(13) -0.0005(14) C16 0.0166(13) 0.0266(15) 0.0237(18) -0.0018(11) -0.0022(12) 0.0010(14) C17 0.0172(13) 0.0369(17) 0.030(2) 0.0010(12) -0.0012(13) -0.0023(16) C18 0.0194(14) 0.054(2) 0.042(3) 0.0020(14) -0.0106(15) -0.0030(19) #============================================================================== _computing_data_collection 'CrystalClear-SM Expert 2.0 r10 (Rigaku, 2011)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r10' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r10' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 C2 1.730(3) yes . . S1 C2 1.730(3) yes . 2_755 S2 C1 1.729(3) yes . . S2 C4 1.757(3) yes . . C1 C1 1.420(3) yes . 2_755 C1 C2 1.387(4) yes . . C2 C3 1.421(3) yes . . C3 C4 1.365(4) yes . . C4 C5 1.470(4) yes . . C5 C6 1.406(4) yes . . C5 C10 1.398(4) yes . . C6 C7 1.388(4) yes . . C7 C8 1.397(4) yes . . C8 C9 1.384(4) yes . . C8 C11 1.517(3) yes . . C9 C10 1.393(4) yes . . C11 C12 1.529(5) yes . . C12 C13 1.533(4) yes . . C13 C14 1.515(4) yes . . C14 C15 1.526(4) yes . . C15 C16 1.528(4) yes . . C16 C17 1.527(4) yes . . C17 C18 1.531(5) yes . . C3 H3 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C9 H9 0.950 no . . C10 H10 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C13 H13A 0.990 no . . C13 H13B 0.990 no . . C14 H14A 0.990 no . . C14 H14B 0.990 no . . C15 H15A 0.990 no . . C15 H15B 0.990 no . . C16 H16A 0.990 no . . C16 H16B 0.990 no . . C17 H17A 0.990 no . . C17 H17B 0.990 no . . C18 H18A 0.980 no . . C18 H18B 0.980 no . . C18 H18C 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C2 S1 C2 89.99(13) yes . . 2_755 C1 S2 C4 91.52(12) yes . . . S2 C1 C1 137.5(2) yes . . 2_755 S2 C1 C2 110.59(17) yes . . . C1 C1 C2 111.7(3) yes 2_755 . . S1 C2 C1 113.26(17) yes . . . S1 C2 C3 132.5(2) yes . . . C1 C2 C3 114.1(3) yes . . . C2 C3 C4 111.9(3) yes . . . S2 C4 C3 111.82(17) yes . . . S2 C4 C5 119.7(2) yes . . . C3 C4 C5 128.4(3) yes . . . C4 C5 C6 120.1(3) yes . . . C4 C5 C10 122.3(3) yes . . . C6 C5 C10 117.6(3) yes . . . C5 C6 C7 121.0(3) yes . . . C6 C7 C8 121.0(3) yes . . . C7 C8 C9 118.1(3) yes . . . C7 C8 C11 120.3(3) yes . . . C9 C8 C11 121.4(3) yes . . . C8 C9 C10 121.4(3) yes . . . C5 C10 C9 120.9(3) yes . . . C8 C11 C12 117.5(3) yes . . . C11 C12 C13 110.9(3) yes . . . C12 C13 C14 115.4(3) yes . . . C13 C14 C15 112.4(3) yes . . . C14 C15 C16 114.2(3) yes . . . C15 C16 C17 112.2(3) yes . . . C16 C17 C18 112.9(3) yes . . . C2 C3 H3 124.020 no . . . C4 C3 H3 124.035 no . . . C5 C6 H6 119.498 no . . . C7 C6 H6 119.542 no . . . C6 C7 H7 119.494 no . . . C8 C7 H7 119.516 no . . . C8 C9 H9 119.311 no . . . C10 C9 H9 119.330 no . . . C5 C10 H10 119.567 no . . . C9 C10 H10 119.552 no . . . C8 C11 H11A 107.927 no . . . C8 C11 H11B 107.916 no . . . C12 C11 H11A 107.925 no . . . C12 C11 H11B 107.930 no . . . H11A C11 H11B 107.209 no . . . C11 C12 H12A 109.449 no . . . C11 C12 H12B 109.449 no . . . C13 C12 H12A 109.496 no . . . C13 C12 H12B 109.473 no . . . H12A C12 H12B 108.033 no . . . C12 C13 H13A 108.447 no . . . C12 C13 H13B 108.446 no . . . C14 C13 H13A 108.416 no . . . C14 C13 H13B 108.427 no . . . H13A C13 H13B 107.469 no . . . C13 C14 H14A 109.137 no . . . C13 C14 H14B 109.137 no . . . C15 C14 H14A 109.108 no . . . C15 C14 H14B 109.126 no . . . H14A C14 H14B 107.873 no . . . C14 C15 H15A 108.681 no . . . C14 C15 H15B 108.696 no . . . C16 C15 H15A 108.704 no . . . C16 C15 H15B 108.711 no . . . H15A C15 H15B 107.626 no . . . C15 C16 H16A 109.171 no . . . C15 C16 H16B 109.174 no . . . C17 C16 H16A 109.173 no . . . C17 C16 H16B 109.154 no . . . H16A C16 H16B 107.885 no . . . C16 C17 H17A 109.004 no . . . C16 C17 H17B 108.994 no . . . C18 C17 H17A 108.993 no . . . C18 C17 H17B 108.994 no . . . H17A C17 H17B 107.780 no . . . C17 C18 H18A 109.470 no . . . C17 C18 H18B 109.475 no . . . C17 C18 H18C 109.466 no . . . H18A C18 H18B 109.472 no . . . H18A C18 H18C 109.487 no . . . H18B C18 H18C 109.456 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C2 S1 C2 C1 2.81(17) no . . 2_755 2_755 C2 S1 C2 C3 -172.4(3) no . . 2_755 2_755 C2 S1 C2 C1 -2.81(17) no 2_755 . . . C2 S1 C2 C3 172.4(3) no 2_755 . . . C1 S2 C4 C3 0.48(17) no . . . . C1 S2 C4 C5 -179.05(17) no . . . . C4 S2 C1 C1 172.5(3) no . . . 2_755 C4 S2 C1 C2 -0.95(16) no . . . . S2 C1 C1 S2 0.0(5) no . . 2_755 2_755 S2 C1 C1 C2 -173.40(19) no . . 2_755 2_755 S2 C1 C2 S1 177.38(12) no . . . . S2 C1 C2 C3 1.2(3) no . . . . C1 C1 C2 S1 2.1(3) no 2_755 . . . C1 C1 C2 C3 -174.03(18) no 2_755 . . . C2 C1 C1 S2 173.4(2) no . . 2_755 2_755 C2 C1 C1 C2 0.0(3) no . . 2_755 2_755 S1 C2 C3 C4 -176.09(17) no . . . . C1 C2 C3 C4 -0.9(3) no . . . . C2 C3 C4 S2 0.1(3) no . . . . C2 C3 C4 C5 179.6(2) no . . . . S2 C4 C5 C6 175.08(16) no . . . . S2 C4 C5 C10 -6.9(4) no . . . . C3 C4 C5 C6 -4.4(4) no . . . . C3 C4 C5 C10 173.7(3) no . . . . C4 C5 C6 C7 175.0(2) no . . . . C4 C5 C10 C9 -175.2(2) no . . . . C6 C5 C10 C9 2.9(4) no . . . . C10 C5 C6 C7 -3.2(4) no . . . . C5 C6 C7 C8 -0.1(4) no . . . . C6 C7 C8 C9 3.7(4) no . . . . C6 C7 C8 C11 -171.1(2) no . . . . C7 C8 C9 C10 -4.0(4) no . . . . C7 C8 C11 C12 -118.7(3) no . . . . C9 C8 C11 C12 66.7(3) no . . . . C11 C8 C9 C10 170.7(2) no . . . . C8 C9 C10 C5 0.7(4) no . . . . C8 C11 C12 C13 -173.0(2) no . . . . C11 C12 C13 C14 180.0(2) no . . . . C12 C13 C14 C15 -177.70(19) no . . . . C13 C14 C15 C16 -179.12(19) no . . . . C14 C15 C16 C17 -179.7(2) no . . . . C15 C16 C17 C18 -178.3(2) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 C1 2.610(3) no . 2_755 S1 C3 2.886(3) no . 2_755 S2 C10 3.113(4) no . . C3 C6 3.029(4) no . . C5 C8 2.831(4) no . . C6 C9 2.765(4) no . . C7 C10 2.768(4) no . . C9 C12 3.262(4) no . . S1 S2 3.3469(13) no . 1_556 S1 S2 3.3469(13) no . 2_756 S1 C1 3.320(3) no . 3_565 S1 C1 3.320(3) no . 4_765 S1 C2 3.434(3) no . 3_565 S1 C2 3.434(3) no . 4_765 S2 S1 3.3469(13) no . 1_554 S2 C2 3.514(3) no . 3_574 C1 S1 3.320(3) no . 3_564 C2 S1 3.434(3) no . 3_564 C2 S2 3.514(3) no . 3_575 C5 C10 3.585(4) no . 3_575 C10 C5 3.585(4) no . 3_574 S1 H3 3.1591 no . . S1 H3 3.1591 no . 2_755 S2 H3 3.5147 no . . S2 H10 2.6944 no . . C1 H3 3.2495 no . . C3 H6 2.7279 no . . C4 H6 2.6501 no . . C4 H10 2.6871 no . . C5 H3 2.8345 no . . C5 H7 3.2836 no . . C5 H9 3.2785 no . . C6 H3 2.8437 no . . C6 H10 3.2606 no . . C7 H9 3.2449 no . . C7 H11A 3.1361 no . . C7 H11B 2.5417 no . . C8 H6 3.2762 no . . C8 H10 3.2706 no . . C8 H12A 2.8658 no . . C8 H12B 2.7731 no . . C9 H7 3.2442 no . . C9 H11A 2.7367 no . . C9 H11B 3.3088 no . . C9 H12B 2.9854 no . . C10 H6 3.2592 no . . C11 H7 2.6802 no . . C11 H9 2.6859 no . . C11 H13A 2.6890 no . . C11 H13B 2.6883 no . . C12 H9 3.0964 no . . C12 H14A 2.7889 no . . C12 H14B 2.7565 no . . C13 H11A 2.6266 no . . C13 H11B 2.7303 no . . C13 H15A 2.7123 no . . C13 H15B 2.6997 no . . C14 H12A 2.7839 no . . C14 H12B 2.7833 no . . C14 H16A 2.7562 no . . C14 H16B 2.7613 no . . C15 H13A 2.7148 no . . C15 H13B 2.6813 no . . C15 H17A 2.7306 no . . C15 H17B 2.7058 no . . C16 H14A 2.7511 no . . C16 H14B 2.7636 no . . C16 H18A 2.7583 no . . C16 H18B 2.7375 no . . C16 H18C 3.3831 no . . C17 H15A 2.7098 no . . C17 H15B 2.7147 no . . C18 H16A 2.7505 no . . C18 H16B 2.7258 no . . H3 H6 2.2721 no . . H6 H7 2.3240 no . . H7 H11A 3.3612 no . . H7 H11B 2.3332 no . . H9 H10 2.3264 no . . H9 H11A 2.7110 no . . H9 H12B 2.5789 no . . H11A H12A 2.8597 no . . H11A H12B 2.4165 no . . H11A H13A 2.8572 no . . H11A H13B 2.4142 no . . H11B H12A 2.3363 no . . H11B H12B 2.8617 no . . H11B H13A 2.5248 no . . H11B H13B 3.0151 no . . H12A H13A 2.3846 no . . H12A H13B 2.8713 no . . H12A H14A 2.6332 no . . H12A H14B 3.0417 no . . H12B H13A 2.8714 no . . H12B H13B 2.3847 no . . H12B H14A 3.0911 no . . H12B H14B 2.5978 no . . H13A H14A 2.3517 no . . H13A H14B 2.8544 no . . H13A H15A 3.0034 no . . H13A H15B 2.5132 no . . H13B H14A 2.8542 no . . H13B H14B 2.3784 no . . H13B H15A 2.4910 no . . H13B H15B 2.9321 no . . H14A H15A 2.8647 no . . H14A H15B 2.3819 no . . H14A H16A 3.0263 no . . H14A H16B 2.5802 no . . H14B H15A 2.3718 no . . H14B H15B 2.8647 no . . H14B H16A 2.5883 no . . H14B H16B 3.0531 no . . H15A H16A 2.3808 no . . H15A H16B 2.8666 no . . H15A H17A 2.5322 no . . H15A H17B 2.9628 no . . H15B H16A 2.8666 no . . H15B H16B 2.3770 no . . H15B H17A 3.0080 no . . H15B H17B 2.5109 no . . H16A H17A 2.3717 no . . H16A H17B 2.8687 no . . H16A H18A 3.0624 no . . H16A H18B 2.5730 no . . H16B H17A 2.8686 no . . H16B H17B 2.3905 no . . H16B H18A 2.5693 no . . H16B H18B 2.9935 no . . H17A H18A 2.8653 no . . H17A H18B 2.3855 no . . H17A H18C 2.3547 no . . H17B H18A 2.3693 no . . H17B H18B 2.8657 no . . H17B H18C 2.3709 no . . S2 H3 3.2972 no . 1_554 C3 H3 3.3273 no . 3_564 C3 H10 3.3211 no . 1_556 C4 H3 3.0519 no . 3_564 C4 H10 3.1126 no . 3_575 C5 H3 3.2982 no . 3_564 C5 H6 3.0105 no . 3_564 C5 H9 3.4342 no . 3_575 C5 H10 2.9814 no . 3_575 C6 H6 2.9874 no . 3_564 C6 H9 3.2986 no . 1_556 C6 H9 3.4137 no . 3_575 C6 H10 3.5225 no . 3_575 C7 H6 3.2687 no . 3_564 C7 H7 3.3305 no . 3_564 C7 H9 3.3294 no . 1_556 C7 H9 3.1397 no . 3_575 C7 H12A 3.2735 no . 3_565 C7 H12B 3.2169 no . 1_556 C8 H6 3.5572 no . 3_564 C8 H7 3.1720 no . 3_564 C8 H9 2.8478 no . 3_575 C9 H6 3.3435 no . 1_554 C9 H6 3.4887 no . 3_564 C9 H9 2.9123 no . 3_575 C10 H3 3.3154 no . 1_554 C10 H6 3.3744 no . 1_554 C10 H6 3.2333 no . 3_564 C10 H9 3.2023 no . 3_575 C10 H10 3.2311 no . 3_575 C11 H7 3.5828 no . 3_564 C11 H9 3.4085 no . 3_575 C11 H11A 3.5185 no . 3_574 C11 H11A 3.3984 no . 3_575 C11 H12A 3.4471 no . 3_565 C11 H12B 3.4004 no . 3_575 C11 H13B 3.2341 no . 3_575 C11 H14B 3.4315 no . 1_556 C12 H7 3.3470 no . 1_554 C12 H7 3.2262 no . 3_564 C12 H11A 3.1214 no . 3_574 C12 H12A 3.5600 no . 3_564 C12 H14A 3.5227 no . 3_565 C13 H11A 3.2462 no . 3_574 C13 H13B 3.5524 no . 3_575 C13 H14A 3.3031 no . 3_565 C13 H15A 3.3582 no . 3_575 C13 H16A 3.5472 no . 1_556 C14 H11B 3.4455 no . 1_554 C14 H12A 3.3767 no . 3_564 C14 H13A 3.5155 no . 3_564 C14 H13B 3.3956 no . 3_574 C14 H14A 3.4584 no . 3_564 C14 H16B 3.5280 no . 3_565 C15 H13B 3.5114 no . 3_574 C15 H15A 3.5418 no . 3_575 C15 H16B 3.3403 no . 3_565 C15 H17A 3.3615 no . 3_575 C16 H13A 3.5453 no . 1_554 C16 H14A 3.3184 no . 3_564 C16 H15A 3.4420 no . 3_574 C16 H15B 3.5672 no . 3_564 C16 H16B 3.4623 no . 3_564 C17 H15A 3.5856 no . 3_574 C17 H17A 3.4718 no . 3_575 C17 H18A 3.4702 no . 3_565 C17 H18C 3.3102 no . 8_665 C18 H16B 3.3654 no . 3_564 C18 H17A 3.4323 no . 3_574 C18 H17B 3.3049 no . 8_664 C18 H18A 3.4752 no . 3_564 C18 H18C 3.5243 no . 8_664 C18 H18C 3.4729 no . 8_665 H3 S2 3.2972 no . 1_556 H3 C3 3.3273 no . 3_565 H3 C4 3.0519 no . 3_565 H3 C5 3.2982 no . 3_565 H3 C10 3.3154 no . 1_556 H3 H3 3.5998 no . 3_564 H3 H3 3.5998 no . 3_565 H3 H10 2.7372 no . 1_556 H6 C5 3.0105 no . 3_565 H6 C6 2.9874 no . 3_565 H6 C7 3.2687 no . 3_565 H6 C8 3.5572 no . 3_565 H6 C9 3.3435 no . 1_556 H6 C9 3.4887 no . 3_565 H6 C10 3.3744 no . 1_556 H6 C10 3.2333 no . 3_565 H6 H6 3.3472 no . 3_564 H6 H6 3.3472 no . 3_565 H6 H9 3.0944 no . 1_556 H6 H10 3.1605 no . 1_556 H7 C7 3.3305 no . 3_565 H7 C8 3.1720 no . 3_565 H7 C11 3.5828 no . 3_565 H7 C12 3.3470 no . 1_556 H7 C12 3.2262 no . 3_565 H7 H7 3.4876 no . 3_564 H7 H7 3.4876 no . 3_565 H7 H9 3.1506 no . 1_556 H7 H11A 3.5622 no . 3_575 H7 H12A 3.3978 no . 1_556 H7 H12A 2.5116 no . 3_565 H7 H12B 2.4723 no . 1_556 H7 H12B 3.2992 no . 3_565 H9 C5 3.4342 no . 3_574 H9 C6 3.2986 no . 1_554 H9 C6 3.4137 no . 3_574 H9 C7 3.3294 no . 1_554 H9 C7 3.1397 no . 3_574 H9 C8 2.8478 no . 3_574 H9 C9 2.9123 no . 3_574 H9 C10 3.2023 no . 3_574 H9 C11 3.4085 no . 3_574 H9 H6 3.0944 no . 1_554 H9 H7 3.1506 no . 1_554 H9 H9 3.3321 no . 3_574 H9 H9 3.3321 no . 3_575 H9 H11A 2.9991 no . 3_574 H10 C3 3.3211 no . 1_554 H10 C4 3.1126 no . 3_574 H10 C5 2.9814 no . 3_574 H10 C6 3.5225 no . 3_574 H10 C10 3.2311 no . 3_574 H10 H3 2.7372 no . 1_554 H10 H6 3.1605 no . 1_554 H10 H10 3.4446 no . 3_574 H10 H10 3.4446 no . 3_575 H11A C11 3.3984 no . 3_574 H11A C11 3.5185 no . 3_575 H11A C12 3.1214 no . 3_575 H11A C13 3.2462 no . 3_575 H11A H7 3.5622 no . 3_574 H11A H9 2.9991 no . 3_575 H11A H11A 3.0422 no . 3_574 H11A H11A 3.0422 no . 3_575 H11A H11B 2.9872 no . 3_574 H11A H12B 2.4919 no . 3_575 H11A H13B 2.6757 no . 3_575 H11A H14B 3.3141 no . 3_575 H11B C14 3.4455 no . 1_556 H11B H11A 2.9872 no . 3_575 H11B H12A 2.7498 no . 3_565 H11B H12B 3.0060 no . 1_556 H11B H12B 3.5987 no . 3_575 H11B H13B 2.8842 no . 3_575 H11B H14A 3.4902 no . 3_565 H11B H14B 2.4907 no . 1_556 H12A C7 3.2735 no . 3_564 H12A C11 3.4471 no . 3_564 H12A C12 3.5600 no . 3_565 H12A C14 3.3767 no . 3_565 H12A H7 3.3978 no . 1_554 H12A H7 2.5116 no . 3_564 H12A H11B 2.7498 no . 3_564 H12A H12A 3.1561 no . 3_564 H12A H12A 3.1561 no . 3_565 H12A H12B 3.1678 no . 3_565 H12A H14A 2.9732 no . 3_565 H12A H14B 2.9150 no . 3_565 H12B C7 3.2169 no . 1_554 H12B C11 3.4004 no . 3_574 H12B H7 2.4723 no . 1_554 H12B H7 3.2992 no . 3_564 H12B H11A 2.4919 no . 3_574 H12B H11B 3.0060 no . 1_554 H12B H11B 3.5987 no . 3_574 H12B H12A 3.1678 no . 3_564 H13A C14 3.5155 no . 3_565 H13A C16 3.5453 no . 1_556 H13A H13B 3.1401 no . 3_575 H13A H14A 2.6314 no . 3_565 H13A H14B 3.0030 no . 1_556 H13A H14B 3.5753 no . 3_565 H13A H15A 2.9358 no . 3_575 H13A H16A 2.5998 no . 1_556 H13A H16B 3.5250 no . 3_565 H13B C11 3.2341 no . 3_574 H13B C13 3.5524 no . 3_574 H13B C14 3.3956 no . 3_575 H13B C15 3.5114 no . 3_575 H13B H11A 2.6757 no . 3_574 H13B H11B 2.8842 no . 3_574 H13B H13A 3.1401 no . 3_574 H13B H13B 3.1424 no . 3_574 H13B H13B 3.1424 no . 3_575 H13B H14B 2.7746 no . 3_575 H13B H15A 2.8867 no . 3_575 H14A C12 3.5227 no . 3_564 H14A C13 3.3031 no . 3_564 H14A C14 3.4584 no . 3_565 H14A C16 3.3184 no . 3_565 H14A H11B 3.4902 no . 3_564 H14A H12A 2.9732 no . 3_564 H14A H13A 2.6314 no . 3_564 H14A H14A 3.0938 no . 3_564 H14A H14A 3.0938 no . 3_565 H14A H14B 3.0124 no . 3_565 H14A H16A 2.8305 no . 3_565 H14A H16B 2.9562 no . 3_565 H14B C11 3.4315 no . 1_554 H14B H11A 3.3141 no . 3_574 H14B H11B 2.4907 no . 1_554 H14B H12A 2.9151 no . 3_564 H14B H13A 3.0030 no . 1_554 H14B H13A 3.5753 no . 3_564 H14B H13B 2.7746 no . 3_574 H14B H14A 3.0124 no . 3_564 H15A C13 3.3582 no . 3_574 H15A C15 3.5418 no . 3_574 H15A C16 3.4420 no . 3_575 H15A C17 3.5856 no . 3_575 H15A H13A 2.9358 no . 3_574 H15A H13B 2.8867 no . 3_574 H15A H15A 3.1478 no . 3_574 H15A H15A 3.1478 no . 3_575 H15A H15B 3.0996 no . 3_574 H15A H16A 2.8138 no . 3_575 H15A H17A 2.9589 no . 3_575 H15B C16 3.5672 no . 3_565 H15B H15A 3.0996 no . 3_575 H15B H16A 2.9872 no . 1_556 H15B H16B 2.6923 no . 3_565 H15B H17A 2.8905 no . 3_575 H15B H18B 2.7218 no . 1_556 H16A C13 3.5472 no . 1_554 H16A H13A 2.5998 no . 1_554 H16A H14A 2.8305 no . 3_564 H16A H15A 2.8138 no . 3_574 H16A H15B 2.9872 no . 1_554 H16A H16B 2.9976 no . 3_564 H16B C14 3.5280 no . 3_564 H16B C15 3.3403 no . 3_564 H16B C16 3.4623 no . 3_565 H16B C18 3.3654 no . 3_565 H16B H13A 3.5250 no . 3_564 H16B H14A 2.9562 no . 3_564 H16B H15B 2.6923 no . 3_564 H16B H16A 2.9976 no . 3_565 H16B H16B 3.1000 no . 3_564 H16B H16B 3.1000 no . 3_565 H16B H18A 3.0621 no . 3_565 H16B H18B 2.8576 no . 3_565 H17A C15 3.3615 no . 3_574 H17A C17 3.4718 no . 3_574 H17A C18 3.4323 no . 3_575 H17A H15A 2.9589 no . 3_574 H17A H15B 2.8905 no . 3_574 H17A H17A 3.1185 no . 3_574 H17A H17A 3.1185 no . 3_575 H17A H17B 2.9902 no . 3_574 H17A H18B 2.8113 no . 3_575 H17A H18C 3.4396 no . 3_575 H17B C18 3.3049 no . 8_665 H17B H17A 2.9902 no . 3_575 H17B H18A 2.8349 no . 3_565 H17B H18A 3.4054 no . 8_665 H17B H18B 2.9965 no . 1_556 H17B H18C 2.4868 no . 8_665 H18A C17 3.4702 no . 3_564 H18A C18 3.4752 no . 3_565 H18A H16B 3.0621 no . 3_564 H18A H17B 2.8349 no . 3_564 H18A H17B 3.4054 no . 8_664 H18A H18A 3.1333 no . 3_564 H18A H18A 3.1333 no . 3_565 H18A H18B 3.0017 no . 3_565 H18A H18C 2.8978 no . 6_645 H18A H18C 3.4459 no . 8_665 H18B H15B 2.7218 no . 1_554 H18B H16B 2.8576 no . 3_564 H18B H17A 2.8113 no . 3_574 H18B H17B 2.9965 no . 1_554 H18B H18A 3.0017 no . 3_564 H18B H18C 3.1815 no . 8_664 H18C C17 3.3102 no . 8_664 H18C C18 3.4729 no . 8_664 H18C C18 3.5243 no . 8_665 H18C H17A 3.4396 no . 3_574 H18C H17B 2.4868 no . 8_664 H18C H18A 2.8978 no . 6_655 H18C H18A 3.4459 no . 8_664 H18C H18B 3.1815 no . 8_665 H18C H18C 3.1147 no . 8_664 H18C H18C 3.1147 no . 8_665 _database_code_depnum_ccdc_archive 'CCDC 922123' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_opera1209c #TrackingRef '2_DTT-12.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C44 H60 S3' _chemical_formula_moiety 'C44 H60 S3' _chemical_formula_weight 685.14 _chemical_melting_point ? _chemical_absolute_configuration ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21' _symmetry_space_group_name_Hall 'C 2c -2' _symmetry_Int_Tables_number 36 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,+Z 3 +X,-Y,1/2+Z 4 -X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,+Z 7 1/2+X,1/2-Y,1/2+Z 8 1/2-X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 88.90(8) _cell_length_b 7.391(7) _cell_length_c 5.846(5) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 3842(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3112 _cell_measurement_theta_min 6.56 _cell_measurement_theta_max 27.50 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488.00 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.996 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 123 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_reflns_number 14012 _diffrn_reflns_av_R_equivalents 0.0652 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measured_fraction_theta_full 0.965 _diffrn_reflns_limit_h_min -100 _diffrn_reflns_limit_h_max 114 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4032 _reflns_number_gt 3730 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1857 _refine_ls_number_restraints 1 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 4032 _refine_ls_number_parameters 215 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0994P)^2^+6.9433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.790 _refine_diff_density_min -0.380 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1664 Friedel Pairs' _refine_ls_abs_structure_Flack 0.01(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 1.0000 0.65298(16) 1.6606(2) 0.0242(3) Uani 1.0 4 d . . . S2 S 0.977465(8) 0.82799(11) 1.06679(18) 0.0238(3) Uani 1.0 8 d . . . C1 C 0.99197(4) 0.7817(5) 1.2614(7) 0.0223(7) Uani 1.0 8 d . . . C2 C 0.98606(4) 0.7124(5) 1.4645(7) 0.0224(7) Uani 1.0 8 d . . . C3 C 0.97020(4) 0.6929(5) 1.4660(7) 0.0247(7) Uani 1.0 8 d . . . C4 C 0.96374(4) 0.7473(5) 1.2611(7) 0.0241(8) Uani 1.0 8 d . . . C5 C 0.94763(3) 0.7482(5) 1.1973(7) 0.0238(7) Uani 1.0 8 d . . . C6 C 0.94243(4) 0.8270(5) 0.9877(7) 0.0245(8) Uani 1.0 8 d . . . C7 C 0.92702(4) 0.8377(5) 0.9403(7) 0.0255(8) Uani 1.0 8 d . . . C8 C 0.91622(4) 0.7703(5) 1.0940(7) 0.0267(8) Uani 1.0 8 d . . . C9 C 0.92138(4) 0.6829(5) 1.2940(7) 0.0263(8) Uani 1.0 8 d . . . C10 C 0.93674(4) 0.6718(5) 1.3442(7) 0.0248(8) Uani 1.0 8 d . . . C11 C 0.89942(3) 0.8064(5) 1.0590(9) 0.0302(8) Uani 1.0 8 d . . . C12 C 0.89179(4) 0.7182(6) 0.8481(8) 0.0300(8) Uani 1.0 8 d . . . C13 C 0.87542(4) 0.7853(6) 0.8202(8) 0.0292(8) Uani 1.0 8 d . . . C14 C 0.86689(4) 0.7063(5) 0.6169(7) 0.0309(9) Uani 1.0 8 d . . . C15 C 0.85095(4) 0.7838(5) 0.5934(8) 0.0308(8) Uani 1.0 8 d . . . C16 C 0.84190(4) 0.7068(6) 0.3927(8) 0.0314(9) Uani 1.0 8 d . . . C17 C 0.82604(4) 0.7867(6) 0.3721(8) 0.0318(9) Uani 1.0 8 d . . . C18 C 0.81679(4) 0.7089(6) 0.1741(8) 0.0326(8) Uani 1.0 8 d . . . C19 C 0.80084(4) 0.7901(6) 0.1572(8) 0.0354(9) Uani 1.0 8 d . . . C20 C 0.79133(4) 0.7107(6) -0.0397(9) 0.0372(9) Uani 1.0 8 d . . . C21 C 0.77560(4) 0.7940(7) -0.0582(10) 0.0451(11) Uani 1.0 8 d . . . C22 C 0.76595(5) 0.7115(8) -0.2475(10) 0.0504(12) Uani 1.0 8 d . . . H3 H 0.9646 0.6480 1.5925 0.0297 Uiso 1.0 8 calc R . . H6 H 0.9495 0.8723 0.8801 0.0294 Uiso 1.0 8 calc R . . H7 H 0.9238 0.8918 0.8013 0.0305 Uiso 1.0 8 calc R . . H9 H 0.9143 0.6308 1.3963 0.0315 Uiso 1.0 8 calc R . . H10 H 0.9399 0.6118 1.4796 0.0298 Uiso 1.0 8 calc R . . H11A H 0.8980 0.9390 1.0481 0.0362 Uiso 1.0 8 calc R . . H11B H 0.8940 0.7649 1.1975 0.0362 Uiso 1.0 8 calc R . . H12A H 0.8976 0.7481 0.7087 0.0360 Uiso 1.0 8 calc R . . H12B H 0.8918 0.5850 0.8663 0.0360 Uiso 1.0 8 calc R . . H13A H 0.8698 0.7561 0.9617 0.0351 Uiso 1.0 8 calc R . . H13B H 0.8756 0.9187 0.8047 0.0351 Uiso 1.0 8 calc R . . H14A H 0.8662 0.5733 0.6349 0.0370 Uiso 1.0 8 calc R . . H14B H 0.8726 0.7316 0.4750 0.0370 Uiso 1.0 8 calc R . . H15A H 0.8454 0.7599 0.7368 0.0369 Uiso 1.0 8 calc R . . H15B H 0.8517 0.9167 0.5750 0.0369 Uiso 1.0 8 calc R . . H16A H 0.8411 0.5740 0.4111 0.0376 Uiso 1.0 8 calc R . . H16B H 0.8474 0.7305 0.2489 0.0376 Uiso 1.0 8 calc R . . H17A H 0.8206 0.7646 0.5169 0.0381 Uiso 1.0 8 calc R . . H17B H 0.8269 0.9192 0.3517 0.0381 Uiso 1.0 8 calc R . . H18A H 0.8160 0.5763 0.1938 0.0391 Uiso 1.0 8 calc R . . H18B H 0.8222 0.7318 0.0288 0.0391 Uiso 1.0 8 calc R . . H19A H 0.8017 0.9225 0.1355 0.0424 Uiso 1.0 8 calc R . . H19B H 0.7955 0.7689 0.3035 0.0424 Uiso 1.0 8 calc R . . H20A H 0.7967 0.7301 -0.1858 0.0446 Uiso 1.0 8 calc R . . H20B H 0.7903 0.5786 -0.0167 0.0446 Uiso 1.0 8 calc R . . H21A H 0.7704 0.7784 0.0899 0.0541 Uiso 1.0 8 calc R . . H21B H 0.7766 0.9254 -0.0865 0.0541 Uiso 1.0 8 calc R . . H22A H 0.7713 0.7201 -0.3937 0.0604 Uiso 1.0 8 calc R . . H22B H 0.7564 0.7773 -0.2579 0.0604 Uiso 1.0 8 calc R . . H22C H 0.7640 0.5841 -0.2123 0.0604 Uiso 1.0 8 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0247(6) 0.0274(6) 0.0204(6) 0.0000 0.0000 0.0026(5) S2 0.0248(4) 0.0245(4) 0.0221(5) 0.0003(3) 0.0003(4) 0.0033(4) C1 0.0244(16) 0.0194(18) 0.0230(18) -0.0014(13) -0.0040(13) -0.0026(16) C2 0.0300(17) 0.0173(16) 0.0200(18) 0.0037(13) -0.0034(14) -0.0028(14) C3 0.0299(18) 0.0228(17) 0.0215(18) -0.0006(13) -0.0001(14) 0.0008(15) C4 0.0289(17) 0.0205(17) 0.0228(19) -0.0009(12) 0.0020(13) -0.0044(15) C5 0.0248(16) 0.0194(16) 0.0271(19) 0.0013(12) -0.0009(13) -0.0032(14) C6 0.0291(17) 0.0220(16) 0.0224(19) -0.0004(13) 0.0024(14) -0.0002(13) C7 0.0299(17) 0.0237(18) 0.023(2) 0.0018(13) 0.0001(14) -0.0001(14) C8 0.0262(16) 0.0233(16) 0.031(2) 0.0009(12) -0.0027(14) -0.0022(16) C9 0.0293(16) 0.0225(17) 0.027(2) -0.0037(13) 0.0033(15) 0.0006(15) C10 0.0277(16) 0.0252(18) 0.022(2) 0.0001(12) -0.0011(14) 0.0012(14) C11 0.0240(15) 0.0353(18) 0.031(2) 0.0015(13) -0.0021(17) 0.0008(19) C12 0.0277(17) 0.0301(19) 0.032(3) -0.0012(14) -0.0004(15) -0.0027(17) C13 0.0278(16) 0.0293(19) 0.031(2) 0.0011(14) -0.0011(15) -0.0012(16) C14 0.0278(17) 0.0338(19) 0.031(3) -0.0005(14) 0.0005(14) -0.0014(16) C15 0.0271(16) 0.0315(18) 0.034(3) 0.0010(13) -0.0019(15) -0.0044(18) C16 0.0264(17) 0.033(2) 0.034(2) 0.0030(14) -0.0050(15) -0.0032(17) C17 0.0279(17) 0.034(2) 0.033(3) 0.0007(15) -0.0018(16) 0.0005(17) C18 0.0256(17) 0.037(2) 0.036(3) 0.0008(14) -0.0052(16) -0.001(2) C19 0.0297(18) 0.040(3) 0.037(3) 0.0029(15) -0.0028(17) 0.001(2) C20 0.0308(18) 0.042(3) 0.039(3) -0.0012(16) -0.0019(17) -0.003(2) C21 0.031(2) 0.056(3) 0.049(3) 0.0023(18) -0.0096(19) -0.004(3) C22 0.032(2) 0.071(4) 0.049(3) 0.001(2) -0.0126(19) -0.006(3) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 C2 1.744(4) yes . . S1 C2 1.744(4) yes . 2_755 S2 C1 1.753(4) yes . . S2 C4 1.771(4) yes . . C1 C1 1.428(6) yes . 2_755 C1 C2 1.396(6) yes . . C2 C3 1.417(6) yes . . C3 C4 1.388(6) yes . . C4 C5 1.480(5) yes . . C5 C6 1.433(6) yes . . C5 C10 1.412(5) yes . . C6 C7 1.400(6) yes . . C7 C8 1.406(6) yes . . C8 C9 1.412(6) yes . . C8 C11 1.531(5) yes . . C9 C10 1.399(6) yes . . C11 C12 1.551(6) yes . . C12 C13 1.546(6) yes . . C13 C14 1.526(6) yes . . C14 C15 1.535(6) yes . . C15 C16 1.532(6) yes . . C16 C17 1.533(6) yes . . C17 C18 1.532(6) yes . . C18 C19 1.543(6) yes . . C19 C20 1.544(7) yes . . C20 C21 1.532(6) yes . . C21 C22 1.527(8) yes . . C3 H3 0.950 no . . C6 H6 0.950 no . . C7 H7 0.950 no . . C9 H9 0.950 no . . C10 H10 0.950 no . . C11 H11A 0.990 no . . C11 H11B 0.990 no . . C12 H12A 0.990 no . . C12 H12B 0.990 no . . C13 H13A 0.990 no . . C13 H13B 0.990 no . . C14 H14A 0.990 no . . C14 H14B 0.990 no . . C15 H15A 0.990 no . . C15 H15B 0.990 no . . C16 H16A 0.990 no . . C16 H16B 0.990 no . . C17 H17A 0.990 no . . C17 H17B 0.990 no . . C18 H18A 0.990 no . . C18 H18B 0.990 no . . C19 H19A 0.990 no . . C19 H19B 0.990 no . . C20 H20A 0.990 no . . C20 H20B 0.990 no . . C21 H21A 0.990 no . . C21 H21B 0.990 no . . C22 H22A 0.980 no . . C22 H22B 0.981 no . . C22 H22C 0.980 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C2 S1 C2 90.55(19) yes . . 2_755 C1 S2 C4 91.43(19) yes . . . S2 C1 C1 137.4(3) yes . . 2_755 S2 C1 C2 110.3(3) yes . . . C1 C1 C2 112.1(4) yes 2_755 . . S1 C2 C1 112.6(3) yes . . . S1 C2 C3 132.6(3) yes . . . C1 C2 C3 114.6(4) yes . . . C2 C3 C4 112.2(4) yes . . . S2 C4 C3 111.5(3) yes . . . S2 C4 C5 120.2(3) yes . . . C3 C4 C5 128.3(4) yes . . . C4 C5 C6 122.0(3) yes . . . C4 C5 C10 120.6(4) yes . . . C6 C5 C10 117.5(3) yes . . . C5 C6 C7 120.5(4) yes . . . C6 C7 C8 121.4(4) yes . . . C7 C8 C9 118.0(4) yes . . . C7 C8 C11 121.2(4) yes . . . C9 C8 C11 120.5(4) yes . . . C8 C9 C10 121.2(4) yes . . . C5 C10 C9 121.2(4) yes . . . C8 C11 C12 117.4(4) yes . . . C11 C12 C13 111.1(3) yes . . . C12 C13 C14 115.3(4) yes . . . C13 C14 C15 112.7(4) yes . . . C14 C15 C16 114.5(4) yes . . . C15 C16 C17 113.6(4) yes . . . C16 C17 C18 114.1(4) yes . . . C17 C18 C19 113.3(4) yes . . . C18 C19 C20 113.8(4) yes . . . C19 C20 C21 113.6(4) yes . . . C20 C21 C22 113.8(4) yes . . . C2 C3 H3 123.906 no . . . C4 C3 H3 123.932 no . . . C5 C6 H6 119.722 no . . . C7 C6 H6 119.767 no . . . C6 C7 H7 119.262 no . . . C8 C7 H7 119.294 no . . . C8 C9 H9 119.393 no . . . C10 C9 H9 119.453 no . . . C5 C10 H10 119.394 no . . . C9 C10 H10 119.381 no . . . C8 C11 H11A 107.964 no . . . C8 C11 H11B 107.963 no . . . C12 C11 H11A 107.953 no . . . C12 C11 H11B 107.956 no . . . H11A C11 H11B 107.225 no . . . C11 C12 H12A 109.404 no . . . C11 C12 H12B 109.407 no . . . C13 C12 H12A 109.414 no . . . C13 C12 H12B 109.393 no . . . H12A C12 H12B 108.018 no . . . C12 C13 H13A 108.426 no . . . C12 C13 H13B 108.400 no . . . C14 C13 H13A 108.482 no . . . C14 C13 H13B 108.475 no . . . H13A C13 H13B 107.510 no . . . C13 C14 H14A 109.032 no . . . C13 C14 H14B 109.034 no . . . C15 C14 H14A 109.093 no . . . C15 C14 H14B 109.075 no . . . H14A C14 H14B 107.794 no . . . C14 C15 H15A 108.616 no . . . C14 C15 H15B 108.639 no . . . C16 C15 H15A 108.657 no . . . C16 C15 H15B 108.628 no . . . H15A C15 H15B 107.576 no . . . C15 C16 H16A 108.861 no . . . C15 C16 H16B 108.872 no . . . C17 C16 H16A 108.804 no . . . C17 C16 H16B 108.835 no . . . H16A C16 H16B 107.719 no . . . C16 C17 H17A 108.692 no . . . C16 C17 H17B 108.672 no . . . C18 C17 H17A 108.756 no . . . C18 C17 H17B 108.746 no . . . H17A C17 H17B 107.655 no . . . C17 C18 H18A 108.903 no . . . C17 C18 H18B 108.897 no . . . C19 C18 H18A 108.911 no . . . C19 C18 H18B 108.920 no . . . H18A C18 H18B 107.727 no . . . C18 C19 H19A 108.768 no . . . C18 C19 H19B 108.793 no . . . C20 C19 H19A 108.818 no . . . C20 C19 H19B 108.811 no . . . H19A C19 H19B 107.696 no . . . C19 C20 H20A 108.821 no . . . C19 C20 H20B 108.854 no . . . C21 C20 H20A 108.888 no . . . C21 C20 H20B 108.847 no . . . H20A C20 H20B 107.705 no . . . C20 C21 H21A 108.758 no . . . C20 C21 H21B 108.760 no . . . C22 C21 H21A 108.846 no . . . C22 C21 H21B 108.813 no . . . H21A C21 H21B 107.689 no . . . C21 C22 H22A 109.515 no . . . C21 C22 H22B 109.461 no . . . C21 C22 H22C 109.471 no . . . H22A C22 H22B 109.457 no . . . H22A C22 H22C 109.473 no . . . H22B C22 H22C 109.450 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C2 S1 C2 C1 2.4(3) no . . 2_755 2_755 C2 S1 C2 C3 -172.8(4) no . . 2_755 2_755 C2 S1 C2 C1 -2.4(3) no 2_755 . . . C2 S1 C2 C3 172.8(4) no 2_755 . . . C1 S2 C4 C3 1.6(3) no . . . . C1 S2 C4 C5 -179.9(3) no . . . . C4 S2 C1 C1 172.1(4) no . . . 2_755 C4 S2 C1 C2 -1.4(3) no . . . . S2 C1 C1 S2 0.0(7) no . . 2_755 2_755 S2 C1 C1 C2 -173.4(3) no . . 2_755 2_755 S2 C1 C2 S1 177.05(18) no . . . . S2 C1 C2 C3 1.0(4) no . . . . C1 C1 C2 S1 1.8(4) no 2_755 . . . C1 C1 C2 C3 -174.3(3) no 2_755 . . . C2 C1 C1 S2 173.4(3) no . . 2_755 2_755 C2 C1 C1 C2 0.0(4) no . . 2_755 2_755 S1 C2 C3 C4 -174.9(3) no . . . . C1 C2 C3 C4 0.2(5) no . . . . C2 C3 C4 S2 -1.3(4) no . . . . C2 C3 C4 C5 -179.7(3) no . . . . S2 C4 C5 C6 -5.3(5) no . . . . S2 C4 C5 C10 175.3(3) no . . . . C3 C4 C5 C6 173.0(4) no . . . . C3 C4 C5 C10 -6.4(6) no . . . . C4 C5 C6 C7 -175.2(3) no . . . . C4 C5 C10 C9 175.5(3) no . . . . C6 C5 C10 C9 -4.0(5) no . . . . C10 C5 C6 C7 4.2(5) no . . . . C5 C6 C7 C8 -0.8(5) no . . . . C6 C7 C8 C9 -3.0(5) no . . . . C6 C7 C8 C11 171.0(3) no . . . . C7 C8 C9 C10 3.3(5) no . . . . C7 C8 C11 C12 66.9(5) no . . . . C9 C8 C11 C12 -119.3(4) no . . . . C11 C8 C9 C10 -170.8(3) no . . . . C8 C9 C10 C5 0.3(6) no . . . . C8 C11 C12 C13 -173.2(3) no . . . . C11 C12 C13 C14 180.0(3) no . . . . C12 C13 C14 C15 -177.8(3) no . . . . C13 C14 C15 C16 -179.4(3) no . . . . C14 C15 C16 C17 -179.8(3) no . . . . C15 C16 C17 C18 -179.2(3) no . . . . C16 C17 C18 C19 179.6(3) no . . . . C17 C18 C19 C20 -179.2(3) no . . . . C18 C19 C20 C21 -179.1(3) no . . . . C19 C20 C21 C22 -178.0(4) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 S1 C1 2.620(5) no . 2_755 S1 C3 2.898(5) no . 2_755 S2 C6 3.149(5) no . . C3 C10 3.063(6) no . . C5 C8 2.862(5) no . . C6 C9 2.801(6) no . . C7 C10 2.797(6) no . . C7 C12 3.299(6) no . . S1 S2 3.366(3) no . 1_556 S1 S2 3.366(3) no . 2_756 S1 C1 3.343(5) no . 3_565 S1 C1 3.343(5) no . 4_765 S1 C2 3.462(5) no . 3_565 S1 C2 3.462(5) no . 4_765 S2 S1 3.366(3) no . 1_554 S2 C2 3.533(5) no . 3_574 C1 S1 3.343(5) no . 3_564 C2 S1 3.462(5) no . 3_564 C2 S2 3.533(5) no . 3_575 C5 C6 3.599(6) no . 3_575 C6 C5 3.599(6) no . 3_574 S1 H3 3.1690 no . . S1 H3 3.1690 no . 2_755 S2 H3 3.5380 no . . S2 H6 2.7350 no . . C1 H3 3.2603 no . . C3 H10 2.7609 no . . C4 H6 2.7236 no . . C4 H10 2.6696 no . . C5 H3 2.8593 no . . C5 H7 3.3131 no . . C5 H9 3.3005 no . . C6 H10 3.2941 no . . C7 H9 3.2753 no . . C7 H11A 2.7617 no . . C7 H11B 3.3396 no . . C7 H12A 3.0189 no . . C8 H6 3.2997 no . . C8 H10 3.2992 no . . C8 H12A 2.8004 no . . C8 H12B 2.8909 no . . C9 H7 3.2751 no . . C9 H11A 3.1592 no . . C9 H11B 2.5687 no . . C10 H3 2.8795 no . . C10 H6 3.2931 no . . C11 H7 2.7130 no . . C11 H9 2.7062 no . . C11 H13A 2.7187 no . . C11 H13B 2.7186 no . . C12 H7 3.1328 no . . C12 H14A 2.8030 no . . C12 H14B 2.7719 no . . C13 H11A 2.6616 no . . C13 H11B 2.7616 no . . C13 H15A 2.7213 no . . C13 H15B 2.7300 no . . C14 H12A 2.7996 no . . C14 H12B 2.7995 no . . C14 H16A 2.7692 no . . C14 H16B 2.7663 no . . C15 H13A 2.7368 no . . C15 H13B 2.7045 no . . C15 H17A 2.7405 no . . C15 H17B 2.7521 no . . C16 H14A 2.7687 no . . C16 H14B 2.7766 no . . C16 H18A 2.7573 no . . C16 H18B 2.7622 no . . C17 H15A 2.7466 no . . C17 H15B 2.7435 no . . C17 H19A 2.7576 no . . C17 H19B 2.7460 no . . C18 H16A 2.7527 no . . C18 H16B 2.7644 no . . C18 H20A 2.7629 no . . C18 H20B 2.7768 no . . C19 H17A 2.7457 no . . C19 H17B 2.7510 no . . C19 H21A 2.7396 no . . C19 H21B 2.7682 no . . C20 H18A 2.7651 no . . C20 H18B 2.7771 no . . C20 H22A 2.7316 no . . C20 H22B 3.3932 no . . C20 H22C 2.7964 no . . C21 H19A 2.7513 no . . C21 H19B 2.7643 no . . C22 H20A 2.7636 no . . C22 H20B 2.7350 no . . H3 H10 2.3120 no . . H6 H7 2.3361 no . . H7 H11A 2.7336 no . . H7 H12A 2.6158 no . . H9 H10 2.3325 no . . H9 H11A 3.3821 no . . H9 H11B 2.3618 no . . H11A H12A 2.4347 no . . H11A H12B 2.8764 no . . H11A H13A 2.8895 no . . H11A H13B 2.4516 no . . H11B H12A 2.8780 no . . H11B H12B 2.3574 no . . H11B H13A 2.5577 no . . H11B H13B 3.0426 no . . H12A H13A 2.8801 no . . H12A H13B 2.3952 no . . H12A H14A 3.1022 no . . H12A H14B 2.6127 no . . H12B H13A 2.3951 no . . H12B H13B 2.8800 no . . H12B H14A 2.6461 no . . H12B H14B 3.0541 no . . H13A H14A 2.3615 no . . H13A H14B 2.8620 no . . H13A H15A 2.5389 no . . H13A H15B 3.0196 no . . H13B H14A 2.8617 no . . H13B H14B 2.3872 no . . H13B H15A 2.9569 no . . H13B H15B 2.5137 no . . H14A H15A 2.3875 no . . H14A H15B 2.8707 no . . H14A H16A 2.5920 no . . H14A H16B 3.0395 no . . H14B H15A 2.8705 no . . H14B H15B 2.3810 no . . H14B H16A 3.0566 no . . H14B H16B 2.5974 no . . H15A H16A 2.3789 no . . H15A H16B 2.8669 no . . H15A H17A 2.5526 no . . H15A H17B 3.0265 no . . H15B H16A 2.8668 no . . H15B H16B 2.3811 no . . H15B H17A 3.0038 no . . H15B H17B 2.5616 no . . H16A H17A 2.3850 no . . H16A H17B 2.8674 no . . H16A H18A 2.5696 no . . H16A H18B 3.0290 no . . H16B H17A 2.8673 no . . H16B H17B 2.3760 no . . H16B H18A 3.0391 no . . H16B H18B 2.5874 no . . H17A H18A 2.3826 no . . H17A H18B 2.8675 no . . H17A H19A 3.0253 no . . H17A H19B 2.5538 no . . H17B H18A 2.8676 no . . H17B H18B 2.3785 no . . H17B H19A 2.5717 no . . H17B H19B 3.0153 no . . H18A H19A 2.8765 no . . H18A H19B 2.3961 no . . H18A H20A 3.0234 no . . H18A H20B 2.5904 no . . H18B H19A 2.3866 no . . H18B H19B 2.8768 no . . H18B H20A 2.5882 no . . H18B H20B 3.0629 no . . H19A H20A 2.3974 no . . H19A H20B 2.8774 no . . H19A H21A 2.9949 no . . H19A H21B 2.5793 no . . H19B H20A 2.8771 no . . H19B H20B 2.3868 no . . H19B H21A 2.5628 no . . H19B H21B 3.0590 no . . H20A H21A 2.8674 no . . H20A H21B 2.3695 no . . H20A H22A 2.5686 no . . H20A H22C 3.1116 no . . H20B H21A 2.3914 no . . H20B H21B 2.8672 no . . H20B H22A 2.9689 no . . H20B H22C 2.6089 no . . H21A H22A 2.8609 no . . H21A H22B 2.3822 no . . H21A H22C 2.3471 no . . H21B H22A 2.3988 no . . H21B H22B 2.3317 no . . H21B H22C 2.8596 no . . S2 H3 3.2802 no . 1_554 C3 H3 3.3706 no . 3_564 C3 H6 3.3175 no . 1_556 C4 H3 3.0841 no . 3_564 C4 H6 3.1609 no . 3_575 C5 H3 3.3521 no . 3_564 C5 H6 3.0059 no . 3_575 C5 H7 3.4558 no . 3_575 C5 H10 3.0287 no . 3_564 C6 H3 3.3149 no . 1_554 C6 H6 3.2552 no . 3_575 C6 H7 3.2294 no . 3_575 C6 H10 3.3772 no . 1_554 C6 H10 3.2515 no . 3_564 C7 H7 2.9214 no . 3_575 C7 H10 3.3698 no . 1_554 C7 H10 3.5218 no . 3_564 C8 H7 2.8569 no . 3_575 C8 H9 3.1862 no . 3_564 C8 H10 3.5853 no . 3_564 C9 H7 3.3504 no . 1_556 C9 H7 3.1511 no . 3_575 C9 H9 3.3436 no . 3_564 C9 H10 3.2918 no . 3_564 C9 H12A 3.2527 no . 1_556 C9 H12B 3.3183 no . 3_565 C10 H6 3.5612 no . 3_575 C10 H7 3.3333 no . 1_556 C10 H7 3.4339 no . 3_575 C10 H10 3.0030 no . 3_564 C11 H7 3.4173 no . 3_575 C11 H11A 3.5325 no . 3_574 C11 H11A 3.4257 no . 3_575 C11 H12A 3.4108 no . 3_575 C11 H12B 3.4723 no . 3_565 C11 H13B 3.2686 no . 3_575 C11 H14B 3.4514 no . 1_556 C12 H9 3.3760 no . 1_554 C12 H9 3.2761 no . 3_564 C12 H11A 3.1306 no . 3_574 C12 H12B 3.5996 no . 3_564 C12 H14A 3.5507 no . 3_565 C13 H11A 3.2716 no . 3_574 C13 H13B 3.5790 no . 3_575 C13 H14A 3.3279 no . 3_565 C13 H15B 3.3948 no . 3_575 C13 H16B 3.5545 no . 1_556 C14 H11B 3.4674 no . 1_554 C14 H12B 3.4191 no . 3_564 C14 H13A 3.5456 no . 3_564 C14 H13B 3.4079 no . 3_574 C14 H14A 3.4952 no . 3_564 C14 H16A 3.5378 no . 3_565 C15 H13B 3.5326 no . 3_574 C15 H15B 3.5822 no . 3_575 C15 H16A 3.3491 no . 3_565 C15 H17B 3.4166 no . 3_575 C16 H13A 3.5552 no . 1_554 C16 H14A 3.3534 no . 3_564 C16 H15A 3.5814 no . 3_564 C16 H15B 3.4569 no . 3_574 C16 H16A 3.4987 no . 3_564 C16 H18A 3.5769 no . 3_565 C17 H17B 3.5487 no . 3_575 C17 H18A 3.3963 no . 3_565 C17 H19A 3.4167 no . 3_575 C18 H16A 3.3766 no . 3_564 C18 H17B 3.4515 no . 3_574 C18 H18A 3.5121 no . 3_564 C19 H19A 3.5124 no . 3_575 C19 H20B 3.4547 no . 3_565 C19 H21B 3.3614 no . 3_575 C20 H18A 3.4236 no . 3_564 C20 H19A 3.4355 no . 3_574 C20 H20B 3.5150 no . 3_564 C21 H21B 3.4518 no . 3_575 C21 H22B 3.3843 no . 8_665 C22 H20B 3.4302 no . 3_564 C22 H21A 3.3661 no . 8_664 C22 H21B 3.4687 no . 3_574 C22 H22B 3.5861 no . 8_664 C22 H22B 3.4854 no . 8_665 C22 H22C 3.4912 no . 3_564 H3 S2 3.2802 no . 1_556 H3 C3 3.3706 no . 3_565 H3 C4 3.0841 no . 3_565 H3 C5 3.3521 no . 3_565 H3 C6 3.3149 no . 1_556 H3 H6 2.7182 no . 1_556 H6 C3 3.3175 no . 1_554 H6 C4 3.1609 no . 3_574 H6 C5 3.0059 no . 3_574 H6 C6 3.2552 no . 3_574 H6 C10 3.5612 no . 3_574 H6 H3 2.7182 no . 1_554 H6 H6 3.4796 no . 3_574 H6 H6 3.4796 no . 3_575 H6 H10 3.1494 no . 1_554 H7 C5 3.4558 no . 3_574 H7 C6 3.2294 no . 3_574 H7 C7 2.9214 no . 3_574 H7 C8 2.8569 no . 3_574 H7 C9 3.3504 no . 1_554 H7 C9 3.1511 no . 3_574 H7 C10 3.3333 no . 1_554 H7 C10 3.4339 no . 3_574 H7 C11 3.4173 no . 3_574 H7 H7 3.3325 no . 3_574 H7 H7 3.3325 no . 3_575 H7 H9 3.1688 no . 1_554 H7 H10 3.1418 no . 1_554 H7 H11A 3.0045 no . 3_574 H9 C8 3.1862 no . 3_565 H9 C9 3.3436 no . 3_565 H9 C12 3.3760 no . 1_556 H9 C12 3.2761 no . 3_565 H9 H7 3.1688 no . 1_556 H9 H9 3.5047 no . 3_564 H9 H9 3.5047 no . 3_565 H9 H12A 2.5079 no . 1_556 H9 H12A 3.3535 no . 3_565 H9 H12B 3.4146 no . 1_556 H9 H12B 2.5629 no . 3_565 H10 C5 3.0287 no . 3_565 H10 C6 3.3772 no . 1_556 H10 C6 3.2515 no . 3_565 H10 C7 3.3698 no . 1_556 H10 C7 3.5218 no . 3_565 H10 C8 3.5853 no . 3_565 H10 C9 3.2918 no . 3_565 H10 C10 3.0030 no . 3_565 H10 H6 3.1494 no . 1_556 H10 H7 3.1418 no . 1_556 H10 H10 3.3581 no . 3_564 H10 H10 3.3581 no . 3_565 H11A C11 3.4257 no . 3_574 H11A C11 3.5325 no . 3_575 H11A C12 3.1306 no . 3_575 H11A C13 3.2716 no . 3_575 H11A H7 3.0045 no . 3_575 H11A H11A 3.0593 no . 3_574 H11A H11A 3.0593 no . 3_575 H11A H11B 3.0187 no . 3_574 H11A H12A 2.4966 no . 3_575 H11A H13B 2.7055 no . 3_575 H11A H14B 3.3472 no . 3_575 H11B C14 3.4674 no . 1_556 H11B H11A 3.0187 no . 3_575 H11B H12A 3.0081 no . 1_556 H11B H12B 2.7752 no . 3_565 H11B H13B 2.9243 no . 3_575 H11B H14A 3.5332 no . 3_565 H11B H14B 2.5151 no . 1_556 H12A C9 3.2527 no . 1_554 H12A C11 3.4108 no . 3_574 H12A H9 2.5079 no . 1_554 H12A H9 3.3535 no . 3_564 H12A H11A 2.4966 no . 3_574 H12A H11B 3.0081 no . 1_554 H12A H12B 3.2146 no . 3_564 H12B C9 3.3183 no . 3_564 H12B C11 3.4723 no . 3_564 H12B C12 3.5996 no . 3_565 H12B C14 3.4191 no . 3_565 H12B H9 3.4146 no . 1_554 H12B H9 2.5629 no . 3_564 H12B H11B 2.7752 no . 3_564 H12B H12A 3.2146 no . 3_565 H12B H12B 3.1818 no . 3_564 H12B H12B 3.1818 no . 3_565 H12B H14A 2.9998 no . 3_565 H12B H14B 2.9661 no . 3_565 H13A C14 3.5456 no . 3_565 H13A C16 3.5552 no . 1_556 H13A H13B 3.1719 no . 3_575 H13A H14A 2.6560 no . 3_565 H13A H14B 3.0166 no . 1_556 H13A H15B 2.9808 no . 3_575 H13A H16A 3.5449 no . 3_565 H13A H16B 2.6098 no . 1_556 H13B C11 3.2686 no . 3_574 H13B C13 3.5790 no . 3_574 H13B C14 3.4079 no . 3_575 H13B C15 3.5326 no . 3_575 H13B H11A 2.7055 no . 3_574 H13B H11B 2.9243 no . 3_574 H13B H13A 3.1719 no . 3_574 H13B H13B 3.1608 no . 3_574 H13B H13B 3.1608 no . 3_575 H13B H14B 2.7829 no . 3_575 H13B H15B 2.9143 no . 3_575 H14A C12 3.5507 no . 3_564 H14A C13 3.3279 no . 3_564 H14A C14 3.4952 no . 3_565 H14A C16 3.3534 no . 3_565 H14A H11B 3.5332 no . 3_564 H14A H12B 2.9998 no . 3_564 H14A H13A 2.6560 no . 3_564 H14A H14A 3.1176 no . 3_564 H14A H14A 3.1176 no . 3_565 H14A H14B 3.0576 no . 3_565 H14A H16A 2.9669 no . 3_565 H14A H16B 2.8780 no . 3_565 H14B C11 3.4514 no . 1_554 H14B H11A 3.3472 no . 3_574 H14B H11B 2.5151 no . 1_554 H14B H12B 2.9661 no . 3_564 H14B H13A 3.0166 no . 1_554 H14B H13B 2.7829 no . 3_574 H14B H14A 3.0576 no . 3_564 H15A C16 3.5814 no . 3_565 H15A H15B 3.1521 no . 3_575 H15A H16A 2.6975 no . 3_565 H15A H16B 3.0072 no . 1_556 H15A H17B 2.9625 no . 3_575 H15A H18B 2.6848 no . 1_556 H15B C13 3.3948 no . 3_574 H15B C15 3.5822 no . 3_574 H15B C16 3.4569 no . 3_575 H15B H13A 2.9808 no . 3_574 H15B H13B 2.9143 no . 3_574 H15B H15A 3.1521 no . 3_574 H15B H15B 3.1722 no . 3_574 H15B H15B 3.1722 no . 3_575 H15B H16B 2.8244 no . 3_575 H15B H17B 2.9909 no . 3_575 H16A C14 3.5378 no . 3_564 H16A C15 3.3491 no . 3_564 H16A C16 3.4987 no . 3_565 H16A C18 3.3766 no . 3_565 H16A H13A 3.5449 no . 3_564 H16A H14A 2.9669 no . 3_564 H16A H15A 2.6975 no . 3_564 H16A H16A 3.1214 no . 3_564 H16A H16A 3.1214 no . 3_565 H16A H16B 3.0472 no . 3_565 H16A H18A 2.9919 no . 3_565 H16A H18B 2.8987 no . 3_565 H16B C13 3.5545 no . 1_554 H16B H13A 2.6098 no . 1_554 H16B H14A 2.8780 no . 3_564 H16B H15A 3.0072 no . 1_554 H16B H15B 2.8244 no . 3_574 H16B H16A 3.0472 no . 3_564 H17A H17B 3.0991 no . 3_575 H17A H18A 2.7541 no . 3_565 H17A H18B 3.0062 no . 1_556 H17A H19A 2.9400 no . 3_575 H17A H20A 2.7534 no . 1_556 H17B C15 3.4166 no . 3_574 H17B C17 3.5487 no . 3_574 H17B C18 3.4515 no . 3_575 H17B H15A 2.9625 no . 3_574 H17B H15B 2.9909 no . 3_574 H17B H17A 3.0991 no . 3_574 H17B H17B 3.1576 no . 3_574 H17B H17B 3.1576 no . 3_575 H17B H18B 2.8109 no . 3_575 H17B H19A 3.0226 no . 3_575 H18A C16 3.5769 no . 3_564 H18A C17 3.3963 no . 3_564 H18A C18 3.5121 no . 3_565 H18A C20 3.4236 no . 3_565 H18A H16A 2.9919 no . 3_564 H18A H17A 2.7541 no . 3_564 H18A H18A 3.1330 no . 3_564 H18A H18A 3.1330 no . 3_565 H18A H18B 3.0540 no . 3_565 H18A H20A 2.9233 no . 3_565 H18A H20B 3.0612 no . 3_565 H18B H15A 2.6848 no . 1_554 H18B H16A 2.8987 no . 3_564 H18B H17A 3.0062 no . 1_554 H18B H17B 2.8109 no . 3_574 H18B H18A 3.0540 no . 3_564 H19A C17 3.4167 no . 3_574 H19A C19 3.5124 no . 3_574 H19A C20 3.4355 no . 3_575 H19A H17A 2.9400 no . 3_574 H19A H17B 3.0226 no . 3_574 H19A H19A 3.1394 no . 3_574 H19A H19A 3.1394 no . 3_575 H19A H19B 3.0447 no . 3_574 H19A H20A 2.8066 no . 3_575 H19A H21B 2.9786 no . 3_575 H19B H19A 3.0447 no . 3_575 H19B H20A 3.0014 no . 1_556 H19B H20B 2.8133 no . 3_565 H19B H21B 2.8875 no . 3_575 H19B H22A 2.8117 no . 1_556 H20A H17A 2.7534 no . 1_554 H20A H18A 2.9233 no . 3_564 H20A H19A 2.8066 no . 3_574 H20A H19B 3.0014 no . 1_554 H20A H20B 3.0449 no . 3_564 H20B C19 3.4547 no . 3_564 H20B C20 3.5150 no . 3_565 H20B C22 3.4302 no . 3_565 H20B H18A 3.0612 no . 3_564 H20B H19B 2.8133 no . 3_564 H20B H20A 3.0449 no . 3_565 H20B H20B 3.1455 no . 3_564 H20B H20B 3.1455 no . 3_565 H20B H22A 2.8726 no . 3_565 H20B H22C 3.1793 no . 3_565 H21A C22 3.3661 no . 8_665 H21A H21B 2.9466 no . 3_575 H21A H22A 3.0512 no . 1_556 H21A H22B 2.5733 no . 8_665 H21A H22C 2.9732 no . 3_565 H21A H22C 3.4169 no . 8_665 H21B C19 3.3614 no . 3_574 H21B C21 3.4518 no . 3_574 H21B C22 3.4687 no . 3_575 H21B H19A 2.9786 no . 3_574 H21B H19B 2.8875 no . 3_574 H21B H21A 2.9466 no . 3_574 H21B H21B 3.1242 no . 3_574 H21B H21B 3.1242 no . 3_575 H21B H22A 2.8915 no . 3_575 H21B H22B 3.4280 no . 3_575 H22A H19B 2.8117 no . 1_554 H22A H20B 2.8726 no . 3_564 H22A H21A 3.0512 no . 1_554 H22A H21B 2.8915 no . 3_574 H22A H22B 3.2551 no . 8_664 H22A H22C 2.9917 no . 3_564 H22B C21 3.3843 no . 8_664 H22B C22 3.4854 no . 8_664 H22B C22 3.5861 no . 8_665 H22B H21A 2.5733 no . 8_664 H22B H21B 3.4280 no . 3_574 H22B H22A 3.2551 no . 8_665 H22B H22B 3.1629 no . 8_664 H22B H22B 3.1629 no . 8_665 H22B H22C 2.9127 no . 6_655 H22B H22C 3.3735 no . 8_664 H22C C22 3.4912 no . 3_565 H22C H20B 3.1793 no . 3_564 H22C H21A 2.9732 no . 3_564 H22C H21A 3.4169 no . 8_664 H22C H22A 2.9917 no . 3_565 H22C H22B 2.9127 no . 6_645 H22C H22B 3.3735 no . 8_665 H22C H22C 3.1765 no . 3_564 H22C H22C 3.1765 no . 3_565 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 922124'