#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003628.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_2003628 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1411 _journal_page_last 1412 _publ_section_title ; Homochiral Methyl (S)-2-Benzenesulfonyloxy-4-bromo-4-methylpentanoate ; _chemical_formula_sum 'C13 H17 Br O5 S' _chemical_formula_weight 365.24 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _symmetry_space_group_name_H-M 'P 21' _cell_length_a 10.352(2) _cell_length_b 7.1190(10) _cell_length_c 10.652(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.89(3) _cell_angle_gamma 90.00 _cell_volume 758.6(2) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 12 _cell_measurement_theta_max 17 _exptl_absorpt_coefficient_mu 2.862 _cell_measurement_temperature 130(2) _exptl_crystal_description block _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.3 _exptl_crystal_colour colourless _chemical_compound_source 'evaporation from hexane/dichloromethane' _diffrn_measurement_device 'Nicolet R3M diffractometer' _diffrn_measurement_method '\w scans' _exptl_absorpt_correction_type 'empirical \y scans' _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.907 _diffrn_reflns_number 1520 _reflns_number_total 1438 _reflns_number_observed 1214 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0400 _refine_ls_wR_factor_obs 0.0829 _refine_ls_wR_factor_all 0.0898 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_number_reflns 1438 _refine_ls_number_parameters 184 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.0000P] wh _refine_ls_shift/esd_max -0.002 _refine_diff_density_max 0.615 _refine_diff_density_min -0.504 _refine_ls_extinction_method none _refine_ls_extinction_coef 0 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.123 'Br' 'Br' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.2901 2. _refine_ls_abs_structure_details 'Flack (1983), \c = 0.01(2)' _refine_ls_abs_structure_Flack 0.01(2) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Br1 1 0.89489(7) 0.15280(14) 0.55164(6) 0.0430(3) S1 1 0.5895(2) -0.0750(2) 0.8244(2) 0.0229(4) O1 1 0.7964(4) 0.2711(7) 1.0333(4) 0.0222(11) O2 1 0.9771(4) 0.1211(7) 1.0025(4) 0.0251(12) O3 1 0.6447(4) 0.1306(7) 0.8099(4) 0.0198(10) O4 1 0.4485(4) -0.0553(8) 0.7762(5) 0.0307(13) O5 1 0.6600(5) -0.2061(8) 0.7659(5) 0.0343(13) C1 1 0.7813(8) 0.5164(13) 0.5454(7) 0.040(2) H1A 1 0.7829(51) 0.5041(16) 0.4560(15) 0.060 H1B 1 0.8641(25) 0.5697(32) 0.5943(31) 0.060 H1C 1 0.7087(28) 0.5970(25) 0.5513(45) 0.060 C2 1 0.7624(7) 0.3239(12) 0.6000(6) 0.028(2) C3 1 0.6267(6) 0.2451(12) 0.5387(6) 0.034(2) H3A 1 0.6105(22) 0.2491(66) 0.4459(6) 0.051 H3B 1 0.5601(7) 0.3184(44) 0.5647(40) 0.051 H3C 1 0.6224(17) 0.1174(25) 0.5662(38) 0.051 C4 1 0.7995(7) 0.3369(11) 0.7479(6) 0.024(2) H4A 1 0.8912(7) 0.3805(11) 0.7764(6) 0.029 H4B 1 0.7435(7) 0.4322(11) 0.7723(6) 0.029 C5 1 0.7873(5) 0.1597(13) 0.8217(5) 0.0212(13) H5 1 0.8227(5) 0.0534(13) 0.7824(5) 0.025 C6 1 0.8659(6) 0.1800(11) 0.9635(5) 0.0189(14) C7 1 0.8637(7) 0.2963(12) 1.1696(6) 0.027(2) H7A 1 0.8039(16) 0.3552(54) 1.2132(10) 0.040 H7B 1 0.9411(25) 0.3742(49) 1.1774(6) 0.040 H7C 1 0.8908(36) 0.1762(13) 1.2085(11) 0.040 C8 1 0.6309(6) -0.1103(9) 0.9921(6) 0.021(2) C9 1 0.7515(6) -0.1997(10) 1.0527(7) 0.024(2) H9 1 0.8071(6) -0.2488(10) 1.0048(7) 0.029 C10 1 0.7843(7) -0.2118(12) 1.1874(7) 0.037(2) H10 1 0.8639(7) -0.2692(12) 1.2310(7) 0.044 C11 1 0.7013(8) -0.1408(11) 1.2567(7) 0.036(2) H11 1 0.7257(8) -0.1499(11) 1.3468(7) 0.043 C12 1 0.5830(8) -0.0564(12) 1.1960(7) 0.035(2) H12 1 0.5274(8) -0.0094(12) 1.2447(7) 0.042 C13 1 0.5467(7) -0.0415(10) 1.0631(6) 0.026(2) H13 1 0.4660(7) 0.0145(10) 1.0211(6) 0.032 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Br1 0.0348(4) 0.0116(6) 0.0046(3) 0.0679(6) -0.0110(5) 0.0247(3) S1 0.0204(9) -0.0018(8) 0.0005(7) 0.0189(9) -0.0046(8) 0.0265(8) O1 0.020(2) -0.001(2) 0.000(2) 0.025(3) -0.002(2) 0.019(2) O2 0.015(2) 0.006(2) 0.003(2) 0.029(3) 0.005(2) 0.030(2) O3 0.016(2) 0.000(2) 0.001(2) 0.018(3) 0.000(2) 0.023(2) O4 0.019(3) -0.006(3) -0.007(2) 0.032(3) 0.003(3) 0.034(3) O5 0.041(3) -0.004(3) 0.010(2) 0.026(3) -0.008(3) 0.036(3) C1 0.052(5) -0.002(5) 0.012(4) 0.044(5) 0.007(4) 0.025(4) C2 0.028(4) -0.002(4) 0.001(3) 0.038(5) 0.003(3) 0.016(3) C3 0.025(4) 0.001(4) -0.001(3) 0.049(5) -0.005(3) 0.024(3) C4 0.023(4) -0.004(3) 0.004(3) 0.027(4) -0.003(3) 0.022(3) C5 0.018(3) -0.001(4) 0.003(2) 0.023(4) -0.001(4) 0.022(3) C6 0.020(3) 0.000(3) 0.010(2) 0.014(4) 0.007(3) 0.025(3) C7 0.034(4) -0.005(4) 0.005(3) 0.026(4) -0.001(3) 0.020(3) C8 0.018(3) -0.003(3) 0.001(3) 0.012(4) 0.002(3) 0.030(3) C9 0.018(3) -0.006(3) 0.004(3) 0.013(4) 0.002(3) 0.039(4) C10 0.027(4) -0.009(4) -0.012(3) 0.024(4) 0.013(4) 0.046(5) C11 0.051(5) -0.012(4) 0.005(4) 0.031(5) 0.002(4) 0.024(4) C12 0.047(5) -0.008(4) 0.015(4) 0.025(5) 0.003(4) 0.037(4) C13 0.029(4) 0.000(3) 0.007(3) 0.018(4) 0.008(3) 0.032(4)