Concomitant polymorphism in the stereoselective synthesis of a β-benzyl-β-hydroxyaspartate analogue
Mekki, Sofiane; Rolland, Valérie; Bellahouel, Salima; van der Lee, Arie; Rolland, Marc; Acta Crystallographica Section C 67 (2011) o301–o305; doi:10.1107/S0108270111024632

data_2018189
_publ_section_title
;
 Concomitant polymorphism in the stereoselective synthesis of a
 \b-benzyl-\b-hydroxyaspartate analogue
;
_journal_coeditor_code           GZ3195
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o301
_journal_page_last               o305
_journal_paper_doi               10.1107/S0108270111024632
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C32 H31 N O7 S'
_chemical_formula_moiety         'C32 H31 N O7 S'
_chemical_formula_sum            'C32 H31 N O7 S'
_chemical_formula_weight         573.64
_chemical_name_systematic
;
dibenzyl 2-benzyl-2-hydroxy-3-(4-methylphenylsulfonamido)succinate
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.156(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8712(4)
_cell_length_b                   19.8539(6)
_cell_length_c                   13.8180(4)
_cell_measurement_reflns_used    2973
_cell_measurement_temperature    173
_cell_measurement_theta_max      51.4978
_cell_measurement_theta_min      4.2178
_cell_volume                     2878.68(17)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material
;
PLATON (Spek, 2009) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0143
_diffrn_measured_fraction_theta_full 0.667
_diffrn_measured_fraction_theta_max 0.662
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3 Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.062
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5477
_diffrn_reflns_theta_full        50.38
_diffrn_reflns_theta_max         51.81
_diffrn_reflns_theta_min         4.21
_exptl_absorpt_coefficient_mu    1.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2010)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.398
_refine_ls_extinction_coef       0.0007(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1412P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2339
_reflns_number_gt                2878
_reflns_number_total             5477
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3195.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018189
_cod_database_fobs_code          2018189