Facile Domino Access to Chiral Mono-, Bi-, and Tricyclic 2,3-Dihydrofurans
Li-Ping Fan; Ping Li; Xin-Sheng Li; Dong-Cheng Xu; Meng-Meng Ge; Wei-Dong Zhu; Jian-Wu Xie; Journal of Organic Chemistry 75 (2010) 8716–8719; doi:10.1021/jo101935k

data_4025905
_publ_contact_author_address
;
Department of Chemistry and Life Science, Zhejiang Normal University, 
321004 Jinhua,, P. R. of China
;
_publ_contact_author_email       freexjw@yahoo.com.cn
_publ_contact_author_fax         0579-82282610
_publ_contact_author_name        'Jian-Wu Xie'
_publ_contact_author_phone       0579-82282610
_publ_section_title
;
 Facile Domino Access to Chiral Mono-, Bi-, and Tricyclic
 2,3-Dihydrofurans
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8716
_journal_page_last               8719
_journal_paper_doi               10.1021/jo101935k
_journal_volume                  75
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C16 H16 Cl N O4'
_chemical_formula_sum            'C16 H16 Cl N O4'
_chemical_formula_weight         321.75
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-07-17 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5771(2)
_cell_length_b                   7.3843(2)
_cell_length_c                   32.6590(8)
_cell_measurement_reflns_used    6836
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.49
_cell_volume                     1586.16(8)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEXII (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\w 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  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            25743
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  .97
_exptl_absorpt_correction_T_min  .93
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          .37
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .13
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3683
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0584P)^2^+0.2065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1104
_reflns_number_gt                3069
_reflns_number_total             3683
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo101935k_si_002.cif
_cod_data_source_block           a
_cod_database_code               4025905
_refine_ls_r_factor_ref          0.0505