#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000007.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000007 _journal_name_full 'Chemistry of Materials' _journal_year 2000 _publ_section_title ; Macroscopic Helical and Cylindrical Morphologies from Achiral 1,3-Diynes ; loop_ _publ_author_name 'Lindsell, W. Edward' 'Preston, Peter N.' 'Seddon, John M.' 'Rosair, Georgina M.' 'Woodman, Thomas A.' _chemical_formula_sum 'C30 H46 O3 S' _chemical_formula_weight 486.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.9730(10) _cell_length_b 8.0690(10) _cell_length_c 29.524(3) _cell_angle_alpha 95.020(10) _cell_angle_beta 93.260(10) _cell_angle_gamma 97.480(10) _cell_volume 1402.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 9.757 _cell_measurement_theta_max 24.956 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.143 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.544 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_process_details 'North, Phillips & Matthews 1968' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6446 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4917 _reflns_number_gt 3774 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.4511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4917 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.75097(8) 1.20141(6) 0.388055(17) 0.03378(15) Uani 1 1 d . . . O1 O -0.7231(2) 1.22443(17) 0.33626(4) 0.0365(3) Uani 1 1 d . . . O2 O -0.9883(2) 1.19507(19) 0.39218(5) 0.0506(4) Uani 1 1 d . . . O3 O -0.6380(3) 1.06541(17) 0.40037(5) 0.0474(4) Uani 1 1 d . . . C1 C -0.4984(3) 1.2223(2) 0.31867(7) 0.0349(4) Uani 1 1 d . . . H1A H -0.3870 1.2161 0.3435 0.042 Uiso 1 1 calc R . . H1B H -0.4549 1.3243 0.3044 0.042 Uiso 1 1 calc R . . C2 C -0.5076(3) 1.0718(2) 0.28438(6) 0.0312(4) Uani 1 1 d . . . H2B H -0.6397 1.0671 0.2634 0.037 Uiso 1 1 calc R . . H2C H -0.5244 0.9708 0.3001 0.037 Uiso 1 1 calc R . . C3 C -0.2969(3) 1.0755(2) 0.25739(6) 0.0302(4) Uani 1 1 d . . . H3B H -0.1645 1.0797 0.2783 0.036 Uiso 1 1 calc R . . H3C H -0.2798 1.1763 0.2415 0.036 Uiso 1 1 calc R . . C4 C -0.3101(3) 0.9216(2) 0.22273(6) 0.0296(4) Uani 1 1 d . . . H4A H -0.3173 0.8219 0.2390 0.036 Uiso 1 1 calc R . . H4B H -0.4493 0.9132 0.2036 0.036 Uiso 1 1 calc R . . C5 C -0.1125(3) 0.9243(2) 0.19240(6) 0.0292(4) Uani 1 1 d . . . H5A H 0.0273 0.9343 0.2115 0.035 Uiso 1 1 calc R . . H5B H -0.1068 1.0225 0.1756 0.035 Uiso 1 1 calc R . . C6 C -0.1275(3) 0.7678(2) 0.15868(6) 0.0304(4) Uani 1 1 d . . . H6A H -0.1280 0.6701 0.1756 0.036 Uiso 1 1 calc R . . H6B H -0.2699 0.7557 0.1404 0.036 Uiso 1 1 calc R . . C7 C 0.0652(3) 0.7716(2) 0.12699(6) 0.0316(4) Uani 1 1 d . . . H7A H 0.2082 0.7895 0.1452 0.038 Uiso 1 1 calc R . . H7B H 0.0609 0.8657 0.1088 0.038 Uiso 1 1 calc R . . C8 C 0.0541(3) 0.6107(2) 0.09533(6) 0.0318(4) Uani 1 1 d . . . H8A H -0.0915 0.5899 0.0781 0.038 Uiso 1 1 calc R . . H8B H 0.0660 0.5172 0.1135 0.038 Uiso 1 1 calc R . . C9 C 0.2426(4) 0.6198(2) 0.06222(7) 0.0376(5) Uani 1 1 d . . . H9A H 0.2223 0.7067 0.0422 0.045 Uiso 1 1 calc R . . H9B H 0.3875 0.6513 0.0794 0.045 Uiso 1 1 calc R . . C10 C 0.2463(3) 0.4603(3) 0.03448(6) 0.0367(5) Uani 1 1 d . . . C11 C 0.2478(3) 0.3274(3) 0.01286(6) 0.0345(4) Uani 1 1 d . . . C12 C 0.2510(3) 0.1755(3) -0.01228(6) 0.0353(4) Uani 1 1 d . . . C13 C 0.2519(3) 0.0423(3) -0.03381(6) 0.0371(5) Uani 1 1 d . . . C14 C 0.2565(4) -0.1171(3) -0.06144(7) 0.0385(5) Uani 1 1 d . . . H14A H 0.1119 -0.1491 -0.0787 0.046 Uiso 1 1 calc R . . H14B H 0.2774 -0.2037 -0.0414 0.046 Uiso 1 1 calc R . . C15 C 0.4449(3) -0.1075(2) -0.09444(6) 0.0326(4) Uani 1 1 d . . . H15A H 0.4325 -0.0141 -0.1126 0.039 Uiso 1 1 calc R . . H15B H 0.5903 -0.0860 -0.0771 0.039 Uiso 1 1 calc R . . C16 C 0.4357(3) -0.2681(2) -0.12614(6) 0.0325(4) Uani 1 1 d . . . H16A H 0.4401 -0.3622 -0.1079 0.039 Uiso 1 1 calc R . . H16B H 0.2930 -0.2865 -0.1445 0.039 Uiso 1 1 calc R . . C17 C 0.6285(3) -0.2640(2) -0.15760(6) 0.0313(4) Uani 1 1 d . . . H17A H 0.7706 -0.2515 -0.1392 0.038 Uiso 1 1 calc R . . H17B H 0.6291 -0.1661 -0.1745 0.038 Uiso 1 1 calc R . . C18 C 0.6156(3) -0.4199(2) -0.19144(6) 0.0318(4) Uani 1 1 d . . . H18A H 0.6095 -0.5182 -0.1746 0.038 Uiso 1 1 calc R . . H18B H 0.4761 -0.4301 -0.2106 0.038 Uiso 1 1 calc R . . C19 C 0.8127(3) -0.4185(2) -0.22174(6) 0.0309(4) Uani 1 1 d . . . H19A H 0.9522 -0.4090 -0.2026 0.037 Uiso 1 1 calc R . . H19B H 0.8193 -0.3200 -0.2385 0.037 Uiso 1 1 calc R . . C20 C 0.7977(3) -0.5741(2) -0.25555(6) 0.0315(4) Uani 1 1 d . . . H20A H 0.7888 -0.6725 -0.2387 0.038 Uiso 1 1 calc R . . H20B H 0.6588 -0.5826 -0.2748 0.038 Uiso 1 1 calc R . . C21 C 0.9950(3) -0.5756(2) -0.28574(6) 0.0313(4) Uani 1 1 d . . . H21A H 1.1348 -0.5616 -0.2665 0.038 Uiso 1 1 calc R . . H21B H 0.9994 -0.4805 -0.3038 0.038 Uiso 1 1 calc R . . C22 C 0.9834(3) -0.7357(2) -0.31769(6) 0.0323(4) Uani 1 1 d . . . H22A H 0.9746 -0.8311 -0.2997 0.039 Uiso 1 1 calc R . . H22B H 0.8461 -0.7479 -0.3376 0.039 Uiso 1 1 calc R . . C23 C 1.1850(4) -0.7380(3) -0.34670(7) 0.0419(5) Uani 1 1 d . . . H23A H 1.1682 -0.8415 -0.3660 0.063 Uiso 1 1 calc R . . H23B H 1.3214 -0.7287 -0.3273 0.063 Uiso 1 1 calc R . . H23C H 1.1929 -0.6454 -0.3651 0.063 Uiso 1 1 calc R . . C24 C -0.6077(3) 1.3892(2) 0.41632(6) 0.0272(4) Uani 1 1 d . . . C25 C -0.7081(3) 1.5352(2) 0.41493(6) 0.0317(4) Uani 1 1 d . . . H25A H -0.8514 1.5318 0.4005 0.038 Uiso 1 1 calc R . . C26 C -0.5929(4) 1.6848(2) 0.43513(7) 0.0364(5) Uani 1 1 d . . . H26A H -0.6591 1.7827 0.4341 0.044 Uiso 1 1 calc R . . C27 C -0.3792(3) 1.6919(2) 0.45707(6) 0.0358(5) Uani 1 1 d . . . C28 C -0.2847(3) 1.5445(3) 0.45855(6) 0.0366(5) Uani 1 1 d . . . H28A H -0.1426 1.5476 0.4735 0.044 Uiso 1 1 calc R . . C29 C -0.3965(3) 1.3925(2) 0.43831(6) 0.0326(4) Uani 1 1 d . . . H29A H -0.3306 1.2946 0.4395 0.039 Uiso 1 1 calc R . . C30 C -0.2502(4) 1.8575(3) 0.47745(8) 0.0565(6) Uani 1 1 d . . . H30A H -0.3409 1.9456 0.4734 0.085 Uiso 1 1 calc R . . H30B H -0.1123 1.8798 0.4625 0.085 Uiso 1 1 calc R . . H30C H -0.2155 1.8522 0.5094 0.085 Uiso 1 1 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0344(3) 0.0295(2) 0.0363(3) -0.00302(19) 0.0084(2) 0.00155(19) O1 0.0317(7) 0.0448(8) 0.0313(7) -0.0073(6) 0.0002(6) 0.0069(6) O2 0.0365(8) 0.0491(9) 0.0606(10) -0.0154(7) 0.0163(7) -0.0067(7) O3 0.0645(10) 0.0276(7) 0.0509(9) 0.0037(6) 0.0092(8) 0.0074(7) C1 0.0310(10) 0.0396(11) 0.0311(10) -0.0047(8) 0.0041(8) -0.0011(8) C2 0.0321(10) 0.0285(9) 0.0319(10) -0.0002(8) 0.0026(8) 0.0018(8) C3 0.0321(10) 0.0288(9) 0.0279(9) -0.0007(7) 0.0017(8) 0.0004(8) C4 0.0320(10) 0.0282(9) 0.0269(9) -0.0007(7) 0.0012(8) 0.0003(8) C5 0.0300(10) 0.0294(9) 0.0263(9) -0.0002(7) 0.0008(8) -0.0002(8) C6 0.0335(10) 0.0287(9) 0.0273(9) -0.0004(7) 0.0007(8) 0.0011(8) C7 0.0355(11) 0.0309(10) 0.0270(10) -0.0004(8) 0.0020(8) 0.0007(8) C8 0.0365(11) 0.0296(10) 0.0273(10) -0.0009(8) 0.0010(8) 0.0005(8) C9 0.0395(11) 0.0386(11) 0.0323(10) -0.0049(8) 0.0048(9) 0.0009(9) C10 0.0363(11) 0.0441(12) 0.0292(10) 0.0003(9) 0.0049(8) 0.0038(9) C11 0.0331(11) 0.0433(11) 0.0267(10) -0.0005(8) 0.0047(8) 0.0054(9) C12 0.0323(11) 0.0450(12) 0.0280(10) -0.0009(9) 0.0039(8) 0.0048(9) C13 0.0367(11) 0.0436(12) 0.0299(10) -0.0008(9) 0.0039(8) 0.0036(9) C14 0.0404(12) 0.0380(11) 0.0349(11) -0.0037(8) 0.0044(9) 0.0011(9) C15 0.0377(11) 0.0299(10) 0.0287(10) 0.0002(8) -0.0002(8) 0.0017(8) C16 0.0352(11) 0.0311(10) 0.0293(10) -0.0014(8) -0.0008(8) 0.0016(8) C17 0.0346(10) 0.0295(9) 0.0284(10) 0.0006(8) -0.0004(8) 0.0013(8) C18 0.0343(10) 0.0309(10) 0.0284(10) 0.0005(8) -0.0008(8) 0.0000(8) C19 0.0315(10) 0.0297(9) 0.0301(10) 0.0015(8) -0.0010(8) 0.0012(8) C20 0.0324(10) 0.0289(9) 0.0312(10) -0.0003(8) 0.0005(8) -0.0006(8) C21 0.0327(10) 0.0304(10) 0.0296(10) 0.0020(8) 0.0016(8) 0.0001(8) C22 0.0369(11) 0.0320(10) 0.0271(9) 0.0021(8) 0.0015(8) 0.0021(8) C23 0.0470(13) 0.0448(12) 0.0339(11) -0.0004(9) 0.0062(9) 0.0073(10) C24 0.0317(10) 0.0278(9) 0.0226(9) 0.0013(7) 0.0071(7) 0.0038(8) C25 0.0322(10) 0.0334(10) 0.0303(10) 0.0028(8) 0.0004(8) 0.0089(8) C26 0.0483(12) 0.0259(9) 0.0362(11) 0.0026(8) 0.0075(9) 0.0082(9) C27 0.0433(12) 0.0385(11) 0.0238(9) -0.0007(8) 0.0093(8) -0.0021(9) C28 0.0303(10) 0.0515(12) 0.0270(10) 0.0044(9) 0.0000(8) 0.0018(9) C29 0.0333(11) 0.0367(10) 0.0302(10) 0.0063(8) 0.0041(8) 0.0103(8) C30 0.0695(17) 0.0461(13) 0.0462(14) -0.0093(10) 0.0074(12) -0.0135(12) _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.306 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.042 _cod_database_code 4000007