A functionalized enol lactone containing a protected α-amino acid
Bruno, Giuseppe; Nicoló, Francesco; Cordaro, Massimiliano; Grassi, Giovanni; Risitano, Francesco; Acta Crystallographica Section E 66 (2010) o3356–; doi:10.1107/S1600536810043709

data_2228427
_publ_section_title
;
 A functionalized enol lactone containing a protected \a-amino acid
;
_journal_coeditor_code           JH2217
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3356
_journal_paper_doi               10.1107/S1600536810043709
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C28 H23 N O5, C H4 O'
_chemical_formula_sum            'C29 H27 N O6'
_chemical_formula_weight         485.52
_chemical_name_systematic
;
<i>N</i>-(3,9-dimethyl-4-phenyl-2,5-dioxo-3,4-dihydro-
2<i>H</i>,5<i>H</i>-pyrano[3,2-<i>c</i>]chromen-3-yl)-<i>N</i>-methylbenzamide
methanol monosolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.817(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7435(14)
_cell_length_b                   9.9056(17)
_cell_length_c                   23.298(3)
_cell_measurement_reflns_used    59
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.49
_cell_measurement_theta_min      7.74
_cell_volume                     2470.6(6)
_computing_cell_refinement       'XSCANS (Bruker, 1999)'
_computing_data_collection       'XSCANS (Bruker, 1999)'
_computing_data_reduction        'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material
;
PARST97 (Nardelli, 1995) and SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9535
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(Kopfmann & Huber, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.309
_refine_ls_extinction_coef       0.0036(8)
_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   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0533P)^2^+0.7913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                2843
_reflns_number_total             4347
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jh2217.cif
_cod_data_source_block           I
_cod_original_cell_volume        2470.7(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2228427
_cod_database_fobs_code          2228427