Synthesis and absolute configuration of methyl (–)-(3<i>R</i>)-8-(4-bromophenyl)-7-(naphthalen-1-ylmethyl)-5-oxo-2,3-dihydro-5<i>H</i>-thiazolo[3,2-<i>a</i>]pyridine-3-carboxylate
Veronica Åberg; Dan Boström; Andreas Fischer; Fredrik Almqvist; Acta Crystallographica Section E 58 (2002) o812–o814; doi:10.1107/S1600536802011480

data_2201548
_publ_section_title
;Synthesis and absolute configuration of methyl
 (--)-(3<i>R</i>)-8-(4-bromophenyl)-7-(naphthalen-1-ylmethyl)-5-oxo-2,3-dihydro-5<i>H</i>-thiazolo[3,2-<i>a</i>]pyridine-3-carboxylate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o812
_journal_page_last               o814
_journal_paper_doi               10.1107/S1600536802011480
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C26 H20 Br N O3 S'
_chemical_formula_sum            'C26 H20 Br N O3 S'
_chemical_formula_weight         506.40
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 91.028(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5502(5)
_cell_length_b                   8.6443(5)
_cell_length_c                   13.1213(6)
_cell_measurement_reflns_used    8301
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      4.52
_cell_volume                     1083.05(10)
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8301
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         4.52
_exptl_absorpt_coefficient_mu    2.020
_exptl_absorpt_correction_T_max  0.8151
_exptl_absorpt_correction_T_min  0.5656
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Herrendorf et al., 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.521
_refine_ls_abs_structure_details '(Flack, 1983), 1582 Friedel pairs'
_refine_ls_abs_structure_Flack   0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0225P)^2^+1.1354P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                3754
_reflns_number_total             4234
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6142.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2201548
_cod_database_fobs_code          2201548