Sequential rhodium-, silver-, and gold-catalyzed synthesis of fused dihydrofurans.
Wang, Hengbin; Denton, Justin R.; Davies, Huw M. L.; Organic letters 13 (2011) 4316–4319; doi:10.1021/ol2016548

data_1502359
_publ_section_title
;
 Sequential rhodium-, silver-, and gold-catalyzed synthesis of fused
 dihydrofurans.
;
_journal_issue                   16
_journal_name_full               'Organic letters'
_journal_page_first              4316
_journal_page_last               4319
_journal_paper_doi               10.1021/ol2016548
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         '[C28 H24 O4], 0.5[C6 H14]'
_chemical_formula_sum            'C31 H31 O4'
_chemical_formula_weight         467.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.7040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1319(2)
_cell_length_b                   17.6950(2)
_cell_length_c                   13.8306(2)
_cell_measurement_reflns_used    6634
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      69.16
_cell_measurement_theta_min      2.50
_cell_volume                     2494.50(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14475
_diffrn_reflns_theta_full        69.42
_diffrn_reflns_theta_max         69.42
_diffrn_reflns_theta_min         4.29
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.9208
_exptl_absorpt_correction_T_min  0.8451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
 There was approximately i/2 of a badly disordered hexane molecule 
 in the asymmetric unit that could not be modeled properly so the
 programe SQUEEZE was used to remove this solvent material.  A.L Spek, 
 J.Appl.Cryst.2003,36,7-13.
;
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0860P)^2^+0.4650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1313
_reflns_number_gt                3964
_reflns_number_total             4370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol2016548_si_004.cif
_cod_data_source_block           hw_v_022b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2494.50(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1502359