#------------------------------------------------------------------------------ #$Date: 2008-03-08 13:25:38 +0000 (Sat, 08 Mar 2008) $ #$Revision: 249 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003263.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_2003263 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 537 _journal_page_last 538 _publ_section_title ; N-[2(R)-Bromopropanoyl]-(2S)-proline Methyl Ester ; _chemical_formula_sum 'C9 H14 Br N O3' _chemical_formula_weight 264.12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _symmetry_space_group_name_H-M 'P 32' _cell_length_a 9.793(1) _cell_length_b 9.793(1) _cell_length_c 9.978(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 828.7(2) _cell_formula_units_Z 3 _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.97 _cell_measurement_theta_max 18.68 _exptl_absorpt_coefficient_mu 3.703 _cell_measurement_temperature 293(10) _exptl_crystal_description Needle _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_colour Colourless _chemical_compound_source ? _diffrn_measurement_device 'Rigaku AFC7R diffractometer' _diffrn_measurement_method '\w2\q scans' _exptl_absorpt_correction_type 'Semi-empirical \y scans' _exptl_absorpt_correction_T_min 0.6662 _exptl_absorpt_correction_T_max 0.9991 _diffrn_reflns_number 1634 _reflns_number_total 1029 _reflns_number_observed 940 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0343 _refine_ls_wR_factor_obs 0.0909 _refine_ls_wR_factor_all 0.0944 _refine_ls_goodness_of_fit_obs 1.140 _refine_ls_goodness_of_fit_all 1.124 _refine_ls_number_reflns 1029 _refine_ls_number_parameters 129 _refine_ls_hydrogen_treatment riding _refine_ls_weighting_scheme ; calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.4771P] where P=(Fo^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.343 _refine_diff_density_min -0.258 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 '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)' _refine_ls_abs_structure_Flack -0.01(2) ##;PROCESS TEXSAN (Molecular Structure Corporation, 1985) ##; 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 Br 1 -0.21052(10) 0.19080(9) -0.00055(8) 0.0712(3) O1 1 -0.0925(5) -0.0922(5) 0.0758(5) 0.0479(10) O2 1 -0.4777(7) -0.3416(6) 0.0274(6) 0.0642(15) O3 1 -0.3892(5) -0.4940(5) 0.1089(5) 0.0474(10) N 1 -0.2783(5) -0.1059(5) 0.2138(5) 0.0361(10) C1 1 0.0882(9) 0.2359(9) 0.0767(10) 0.066(2) H1A 1 0.1273(21) 0.3474(10) 0.0751(52) 0.079 H1B 1 0.0931(12) 0.2003(47) -0.0118(24) 0.079 H1C 1 0.1515(15) 0.2136(52) 0.1364(32) 0.079 C2 1 -0.0779(7) 0.1528(7) 0.1240(6) 0.0438(13) H2 1 -0.0820(7) 0.1949(7) 0.2121(6) 0.053 C3 1 -0.1501(7) -0.0258(7) 0.1358(6) 0.0359(12) C4 1 -0.3553(7) -0.0435(8) 0.2990(7) 0.0435(14) H4A 1 -0.3909(7) 0.0168(8) 0.2474(7) 0.052 H4B 1 -0.2857(7) 0.0223(8) 0.3699(7) 0.052 C5 1 -0.4918(11) -0.1912(11) 0.3543(10) 0.081(3) H5A 1 -0.5127(11) -0.1739(11) 0.4459(10) 0.097 H5B 1 -0.5856(11) -0.2209(11) 0.3012(10) 0.097 C6 1 -0.4526(10) -0.3149(9) 0.3501(8) 0.065(2) H6A 1 -0.5461(10) -0.4161(9) 0.3335(8) 0.078 H6B 1 -0.4061(10) -0.3204(9) 0.4343(8) 0.078 C7 1 -0.3353(7) -0.2725(7) 0.2363(6) 0.0379(13) H7 1 -0.2479(7) -0.2871(7) 0.2653(6) 0.045 C8 1 -0.4105(6) -0.3697(6) 0.1108(6) 0.0386(13) C9 1 -0.4633(9) -0.6029(8) 0.0014(8) 0.061(2) H9A 1 -0.4520(56) -0.6937(29) 0.0152(29) 0.073 H9B 1 -0.4146(43) -0.5533(22) -0.0818(10) 0.073 H9C 1 -0.5733(16) -0.6348(50) -0.0013(35) 0.073 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 Br 0.0843(6) 0.0475(5) -0.0154(5) 0.0699(5) 0.0042(4) 0.0713(5) O1 0.054(2) 0.033(2) 0.010(2) 0.051(2) -0.003(2) 0.048(2) O2 0.076(3) 0.043(3) -0.037(3) 0.061(3) -0.022(3) 0.068(3) O3 0.052(2) 0.023(2) -0.004(2) 0.034(2) -0.008(2) 0.057(3) N 0.041(2) 0.022(2) 0.001(2) 0.035(2) -0.003(2) 0.036(2) C1 0.051(4) 0.018(3) 0.007(4) 0.055(4) 0.022(4) 0.080(5) C2 0.048(3) 0.021(3) -0.008(3) 0.040(3) 0.001(3) 0.042(3) C3 0.036(3) 0.022(2) -0.004(2) 0.042(3) -0.001(2) 0.032(3) C4 0.039(3) 0.026(3) -0.001(3) 0.052(4) -0.010(3) 0.044(4) C5 0.086(6) 0.048(5) 0.050(5) 0.078(6) 0.021(5) 0.087(6) C6 0.073(5) 0.023(4) 0.021(4) 0.054(4) 0.001(3) 0.057(4) C7 0.037(3) 0.018(2) 0.001(3) 0.035(3) 0.000(2) 0.042(3) C8 0.034(3) 0.015(2) 0.004(3) 0.034(3) -0.001(2) 0.045(3) C9 0.068(5) 0.021(3) 0.007(4) 0.039(3) -0.011(3) 0.068(5)