Synthesis of N-methoxy-N-methyl-beta-enaminoketoesters: new synthetic precursors for the regioselective synthesis of heterocyclic compounds.
Persson, Tobias; Nielsen, John; Organic letters 8 (2006) 3219–3222; doi:10.1021/ol0611088

data_1506081
_publ_section_title
;
 Synthesis of N-methoxy-N-methyl-beta-enaminoketoesters: new synthetic
 precursors for the regioselective synthesis of heterocyclic compounds.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3219
_journal_page_last               3222
_journal_paper_doi               10.1021/ol0611088
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C9 H15 N O4'
_chemical_formula_weight         201.22
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.5451(12)
_cell_length_b                   16.2722(11)
_cell_length_c                   7.3076(5)
_cell_measurement_temperature    120(2)
_cell_volume                     2086.3(2)
_computing_cell_refinement       'SAINT (Bruker AXS,1998)'
_computing_data_collection       'SMART (Bruker AXS,1998)'
_computing_data_reduction        'SAINT (Bruker AXS,1998)'
_computing_molecular_graphics    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_refinement  'SHELXTL,ver.6.12 (Sheldrick,2001)'
_computing_structure_solution    'SHELXTL,ver.6.12 (Sheldrick,2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD Platform'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12099
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.32
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  no
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS,ver2.03 (Sheldrick,2001)'
_exptl_crystal_colour            colourles
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.6(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2503
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0518P)^2^+0.6282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0964
_reflns_number_gt                2398
_reflns_number_total             2503
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0611088si20060505_095924.cif
_cod_data_source_block           tp1k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1506081