A Versatile Method for the Synthesis of 3-Alkoxycarbonyl β-Lactam Derivatives
Lei Jiao; Qianfeng Zhang; Yong Liang; Shiwei Zhang; Jiaxi Xu; Journal of Organic Chemistry 71 (2006) 815–818; doi:10.1021/jo052135z

data_4021417
_publ_contact_author_address
;College of Chemistry and Molecular Engineering
Peking University
Beijing 100871
China
;
_publ_contact_author_email       Jxxu@pku.edu.cn
_publ_contact_author_fax         86-10-62751708
_publ_contact_author_name        'Jiaxi Xu'
_publ_contact_author_phone       86-10-62751497
_publ_section_title
;
 A Versatile Method for the Synthesis of
 3-Alkoxycarbonyl \b-Lactam Derivatives
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              815
_journal_page_last               818
_journal_paper_doi               10.1021/jo052135z
_journal_volume                  71
_journal_year                    2006
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C32 H27 N O3 S2'
_chemical_formula_sum            'C32 H27 N O3 S2'
_chemical_formula_weight         537.67
_chemical_melting_point          449
_chemical_name_common
'[1,5]benzothiazepine-derived beta-lactam derivative'
_chemical_name_systematic
'[1,5]benzothiazepine-derived beta-lactam derivative'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.54(3)
_cell_angle_beta                 85.90(3)
_cell_angle_gamma                73.88(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7629(16)
_cell_length_b                   8.5948(17)
_cell_length_c                   21.728(4)
_cell_measurement_reflns_used    8218
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.49
_cell_volume                     1376.8(5)
_computing_cell_refinement       Rapid-AUTO
_computing_data_collection       'Rapid-AUTO (Rigaku,2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC,2000)'
_computing_molecular_graphics    'Siemens SHELXTL V4.2,(Sheldrick,1990)'
_computing_publication_material  SHELXL-97,(Sheldrick,1997)
_computing_structure_refinement  SHELXL-97,(Sheldrick,1997)
_computing_structure_solution    SHELXS-97,(Sheldrick,1997)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       \W
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8218
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.49
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-Empirical
                                  Absorption Correction based on Fourier
                                  Series Approximation.
                                  Rigaku Corporation,Tokyo,Japan.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_recrystallization_method 'from ethyl acetate - petroleum ether'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1116
_reflns_number_gt                3294
_reflns_number_total             4652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo052135zsi20051012_011550.cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'contr' was replaced with the
value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4021417