Methyl 2-acetamido-2-(4-hydroxy-2-methyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-4-yl)-4-methylpentanoate
Fun, Hoong-Kun; Quah, Ching Kheng; Xu, Kai; Zhang, Yan; Acta Crystallographica Section E 67 (2011) o1710–o1711; doi:10.1107/S1600536811022999

data_2230784
_publ_section_title
;
 Methyl
 2-acetamido-2-(4-hydroxy-2-methyl-1,3-dioxo-1,2,3,4-tetrahydroisoquinolin-4-yl)-4-methylpentanoate
;
_journal_coeditor_code           LH5262
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1710
_journal_page_last               o1711
_journal_paper_doi               10.1107/S1600536811022999
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C19 H24 N2 O6'
_chemical_formula_moiety         'C19 H24 N2 O6'
_chemical_formula_sum            'C19 H24 N2 O6'
_chemical_formula_weight         376.40
_chemical_name_systematic
;
Methyl 2-acetamido-2-(4-hydroxy-2-methyl-1,3-dioxo-
1,2,3,4-tetrahydroisoquinolin-4-yl)-4-methylpentanoate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.404(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8256(15)
_cell_length_b                   8.7584(6)
_cell_length_c                   11.9182(8)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      64.17
_cell_measurement_theta_min      5.05
_cell_volume                     1830.1(2)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            18268
_diffrn_reflns_theta_full        64.68
_diffrn_reflns_theta_max         64.68
_diffrn_reflns_theta_min         5.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  0.8830
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.112
_refine_diff_density_min         -0.140
_refine_ls_abs_structure_details 'Flack (1983), 1204 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2713
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.7184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0590
_reflns_number_gt                2673
_reflns_number_total             2713
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5262.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2230784
_cod_database_fobs_code          2230784