Diverse Cyclization Catalyzed by In(OTf)3for the Convergent Assembly of Substituted Tetrahydrofurans and Tetrahydropyrans
Loh, Teck-Peng; Hu, Qi-Ying; Tan, Kui-Thong; Cheng, Hin-Soon; Organic Letters 3 (2001) 2669–; doi:10.1021/ol016228o

data_1507521
_publ_section_title
;
 Diverse Cyclization Catalyzed by In(OTf)3for the Convergent Assembly of
 Substituted Tetrahydrofurans and Tetrahydropyrans
;
_journal_issue                   17
_journal_name_full               'Organic Letters'
_journal_page_first              2669
_journal_paper_doi               10.1021/ol016228o
_journal_volume                  3
_journal_year                    2001
_chemical_formula_sum            'C15 H20 O2'
_chemical_formula_weight         232.31
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                84.534(2)
_cell_angle_beta                 84.355(2)
_cell_angle_gamma                78.480(2)
_cell_formula_units_Z            4
_cell_length_a                   8.9084(7)
_cell_length_b                   10.0653(8)
_cell_length_c                   14.7694(11)
_cell_measurement_reflns_used    3560
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      2.34
_cell_volume                     1287.45(17)
_computing_cell_refinement       'Bruker AXS, SAINT'
_computing_data_collection       'Bruker AXS, SMART'
_computing_data_reduction        'Bruker AXS, SAINT'
_computing_molecular_graphics    'Bruker AXS, SHELXTL'
_computing_publication_material  'Bruker AXS, SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15389
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_correction_T_min  0.2197
_exptl_absorpt_correction_type   'sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.196
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                4396
_reflns_number_total             7428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol016228o_s1.cif
_cod_data_source_block           1034
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' 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_original_sg_symbol_H-M      P-1
_cod_database_code               1507521