The diastereoisomers methyl 5-(<i>S</i>)-[2-(<i>R</i>)/(<i>S</i>)-methoxycarbonyl)-2,3,4,5-tetrahydropyrrol-1-ylcarbonyl]-1-(4-methylphenyl)-4,5-dihydropyrazole-3-carboxylate
Pilati, Tullio; Casalone, Gianluigi; Acta Crystallographica Section C 58 (2002) o178–o180; doi:10.1107/S0108270101021552

data_2012552
_publ_section_title
;The diastereoisomers methyl
 5-(<i>S</i>)-[2-(<i>R</i>)/(<i>S</i>)-methoxycarbonyl)-2,3,4,5-tetrahydropyrrol-1-ylcarbonyl]-1-(4-methylphenyl)-4,5-dihydropyrazole-3-carboxylate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o178
_journal_page_last               o180
_journal_paper_doi               10.1107/S0108270101021552
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C19 H23 N3 O5 , C19 H23 N3 O5'
_chemical_formula_sum            'C38 H46 N6 O10'
_chemical_formula_weight         746.81
_chemical_name_systematic
;
methyl-5-(S)-[2-(S)-methoxycarbonyl)-2,3,4,5-tetrahydropyrrol-1-ylcarbonyl]-
1-(4-methylphenyl)-4,5-dihydropyrazole-3-carboxylate.
methyl-5-(S)-[2-(R)-methoxycarbonyl)-2,3,4,5-tetrahydropyrrol-1-ylcarbonyl]-
1-(4-methylphenyl)-4,5-dihydropyrazole-3-carboxylate co-crystal (1/1)
;
_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
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 117.695(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5056(14)
_cell_length_b                   13.3082(16)
_cell_length_c                   12.9491(14)
_cell_measurement_reflns_used    4420
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.7
_cell_measurement_theta_min      2.3
_cell_volume                     1908.2(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .034
_diffrn_reflns_av_sigmaI/netI    .080
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21406
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    .095
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rhombic prism'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          .42
_exptl_crystal_size_mid          .34
_exptl_crystal_size_min          .12
_refine_diff_density_max         .20
_refine_diff_density_min         -.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         3524
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      .936
_refine_ls_R_factor_all          .050
_refine_ls_R_factor_gt           .039
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/\s^2^(Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .095
_refine_ls_wR_factor_ref         .101
_reflns_number_gt                2789
_reflns_number_total             3524
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1481.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012552
_cod_database_fobs_code          2012552