#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2010386.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2010386 loop_ _publ_author_name 'Urtiaga, M. K.' 'Bad\'ia, D.' 'Dom\'inguez, E.' 'Gonz\'alez-Cameno, A. M.' 'Amig\'o, J. M.' 'Revent\'os, M. M.' 'Debaerdemaeker, T.' _publ_section_title ; Methyl (3R*,4R*)-4-Hydroxy-3-phenyl-2-(p-toluenesulfonyl)-1,2,3,4-tetrahydro-4-isoquinolinylacetate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 112 _journal_page_last 114 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C25 H25 N1 O5 S1' _chemical_formula_sum 'C25 H25 N O5 S' _chemical_formula_weight 451.536 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90. _cell_angle_beta 98.890(10) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 15.606(2) _cell_length_b 10.624(2) _cell_length_c 13.499(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 25 _cell_measurement_theta_min 1 _cell_volume 2211.2(6) _diffrn_measurement_device 'Philips PW1100' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.023 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3428 _diffrn_reflns_theta_max 25 _diffrn_standards_decay_% 1.0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type none _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.356 _exptl_crystal_description prismatic _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.286 _refine_diff_density_min -0.24 _refine_ls_goodness_of_fit_obs 0.873 _refine_ls_number_parameters 390 _refine_ls_number_reflns 2591 _refine_ls_R_factor_obs 0.037 _refine_ls_shift/esd_max 0.20 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme unit _refine_ls_wR_factor_obs 0.037 _reflns_number_observed 2595 _reflns_number_total 3072 _reflns_observed_criterion I>2\s(I) _[local]_cod_data_source_file li1101.cif _[local]_cod_data_source_block li1101a _[local]_cod_chemical_formula_sum_orig 'C25 H25 N1 O5 S1' _cod_database_code 2010386 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z S1 .14190(8) .05830(10) .86850(10) O11 .08130(10) -.0075(2) .91860(10) O12 .19010(10) .1618(2) .91590(10) C2 .0852(2) .1107(2) .7532(2) C3 .0146(2) .0446(3) .7069(2) C4 -.0263(2) .0830(3) .6134(2) C5 .0017(2) .1877(3) .5666(2) C51 -.0434(2) .2291(4) .4647(2) C6 .0717(2) .2540(3) .6153(2) C7 .1135(2) .2161(3) .7075(2) N8 .21230(10) -.0460(2) .84390(10) C9 .2983(2) -.0054(2) .8237(2) C10 .36260(10) -.1103(2) .8645(2) O10 .44610(10) -.0818(2) .84200(10) C11 .3347(2) -.2343(2) .8149(2) C12 .3944(2) -.3223(3) .7915(2) C13 .3672(2) -.4342(3) .7450(2) C14 .2800(2) -.4597(3) .7212(2) C15 .2195(2) -.3733(3) .7433(2) C16 .2470(2) -.2605(2) .7910(2) C17 .1779(2) -.1697(3) .8104(2) C18 .3018(2) .0375(2) .7173(2) C19 .2661(2) -.0284(3) .6328(2) C20 .2691(2) .0192(4) .5378(2) C21 .3087(2) .1327(4) .5263(2) C22 .3454(2) .1982(3) .6092(3) C23 .3423(2) .1515(3) .7046(2) C24 .3656(2) -.1151(3) .9798(2) C25 .4392(2) -.1914(3) 1.0331(2) O251 .41870(10) -.3111(2) 1.03920(10) O252 .50910(10) -.1493(2) 1.06820(10) C26 .4833(2) -.3895(3) 1.0978(2) H3 -.0038(15) -.023(2) .73870(10) H4 -.0734(15) .035(2) .5842(17) H6 .0959(18) .329(3) .587(2) H7 .1600(14) .260(2) .7377(16) H511 -.102(3) .173(5) .439(3) H512 -.067(3) .302(4) .457(3) H513 -.013(3) .210(4) .409(3) H9 .3137(12) .0642(18) .8659(14) H101 .4623(13) -.024(2) .8687(15) H12 .4535(13) -.3042(19) .8061(15) H13 .4116(15) -.495(2) .7299(17) H14 .2550(17) -.538(3) .6847(19) H15 .1523(15) -.391(2) .7214(18) H171 .1489(16) -.203(2) .8588(19) H172 .1277(18) -.161(3) .743(2) H19 .2389(15) -.104(2) .6372(17) H20 .2433(16) -.029(2) .4816(18) H21 .3089(18) .166(3) .457(2) H22 .3780(19) .276(3) .601(2) H23 .3710(16) .196(3) .7700(19) H241 .3097(15) -.149(2) .9953(17) H242 .3713(14) -.027(2) 1.0037(16) H261 .4967(18) -.356(3) 1.168(2) H262 .5388(17) -.392(3) 1.072(2) H263 .459(2) -.472(3) 1.095(2) 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 C2 S1 N8 107.30(10) yes O12 S1 N8 106.90(10) yes O12 S1 C2 108.10(10) yes O11 S1 N8 106.30(10) yes O11 S1 C2 107.20(10) yes O11 S1 O12 120.50(10) yes S1 C2 C7 120.0(2) yes S1 C2 C3 120.0(2) yes C3 C2 C7 120.0(3) yes C2 C3 C4 119.2(3) yes C3 C4 C5 121.3(3) yes C4 C5 C6 118.4(3) yes C4 C5 C51 121.0(3) yes C51 C5 C6 120.6(3) yes C5 C6 C7 120.9(3) yes S1 N8 C17 116.5(2) yes S1 N8 C9 120.0(2) yes C9 N8 C17 120.4(2) yes C2 C7 C6 120.1(3) yes N8 C9 C18 115.5(2) yes N8 C9 C10 106.4(2) yes C10 C9 C18 116.0(2) yes C9 C10 C24 107.4(2) yes C9 C10 C11 110.2(2) yes C9 C10 O10 109.8(2) yes C11 C10 C24 112.2(2) yes O10 C10 C24 109.6(2) yes O10 C10 C11 107.6(2) yes C10 C11 C16 119.0(2) yes C10 C11 C12 122.0(2) yes C11 C12 C13 120.8(3) yes C12 C11 C16 119.0(2) yes C12 C13 C14 120.0(3) yes C13 C14 C15 120.2(3) yes C14 C15 C16 119.9(3) yes C11 C16 C15 120.1(3) yes C15 C16 C17 117.0(2) yes C11 C16 C17 122.8(2) yes N8 C17 C16 113.1(2) yes C9 C18 C23 117.6(2) yes C9 C18 C19 124.2(2) yes C19 C18 C23 118.3(2) yes C18 C19 C20 120.8(3) yes C19 C20 C21 120.3(3) yes C20 C21 C22 119.6(3) yes C21 C22 C23 120.5(3) yes C18 C23 C22 120.5(3) yes C10 C24 C25 113.7(2) yes C24 C25 O252 124.6(3) yes C24 C25 O251 112.2(2) yes O251 C25 O252 123.2(3) yes C25 O251 C26 115.8(2) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag S1 O11 1.428(2) yes S1 O12 1.427(2) yes S1 C2 1.758(3) yes S1 N8 1.630(2) yes C2 C3 1.373(4) yes C2 C7 1.383(4) yes C3 C4 1.385(4) yes C4 C5 1.383(4) yes C5 C51 1.510(4) yes C5 C6 1.378(4) yes C6 C7 1.373(4) yes N8 C9 1.475(4) yes N8 C17 1.464(4) yes C9 C10 1.543(3) yes C9 C18 1.516(4) yes C10 O10 1.416(2) yes C10 C11 1.511(3) yes C10 C24 1.551(4) yes C11 C12 1.390(4) yes C11 C16 1.385(4) yes C12 C13 1.380(4) yes C13 C14 1.376(4) yes C14 C15 1.382(4) yes C15 C16 1.396(4) yes C16 C17 1.500(4) yes C18 C19 1.380(4) yes C18 C23 1.389(4) yes C19 C20 1.386(4) yes C20 C21 1.375(6) yes C21 C22 1.366(5) yes C22 C23 1.388(5) yes C24 C25 1.496(4) yes C25 O251 1.317(4) yes C25 O252 1.206(3) yes O251 C26 1.446(3) yes C3 H3 .91(2) no C4 H4 .93(2) no C51 H511 1.11(5) no C51 H512 .86(4) no C51 H513 .98(4) no C6 H6 .99(3) no C7 H7 .90(2) no C9 H9 .942(19) no O10 H101 .74(2) no C12 H12 .93(2) no C13 H13 .99(3) no C14 H14 1.01(3) no C15 H15 1.06(2) no C17 H171 .92(3) no C17 H172 1.11(3) no C19 H19 .92(3) no C20 H20 .95(2) no C21 H21 1.00(3) no C22 H22 .99(3) no C23 H23 1.04(3) no C24 H241 1.00(3) no C24 H242 .99(2) no C26 H261 1.00(3) no C26 H262 .98(3) no C26 H263 .96(3) 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 C9 N8 C17 C16 20.8(3) yes C17 N8 C9 C10 -53.3(3) yes N8 C9 C10 C11 57.9(2) yes C9 C10 C11 C16 -35.3(3) yes C10 C11 C16 C17 1.2(4) yes C11 C16 C17 N8 7.8(4) yes C18 C9 C10 O10 46.2(3) yes C18 C9 C10 C24 165.4(2) yes