Preparative and mechanistic studies of solvent-free Rap–Stoermer reactions
Kazuhiro Yoshizawa; Shinji Toyota; Fumio Toda; Ingeborg Csöregh; Green Chem. 5 (2003) 353–356; doi:10.1039/b303802p

data_7204653
_publ_section_title
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 Preparative and mechanistic studies of solvent-free Rap--Stoermer
 reactions
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_journal_issue                   3
_journal_name_full               'Green Chem.'
_journal_page_first              353
_journal_page_last               356
_journal_paper_doi               10.1039/b303802p
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C15 H12 O3'
_chemical_formula_weight         240.25
_chemical_name_common
'cis-2-benzoyl-3-hydroxy-2,3-dihydrobenzofuran (8a)'
_chemical_name_systematic
; 
cis-2-benzoyl-3-hydroxy-2,3-dihydrobenzofuran (8a) 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9120(10)
_cell_length_b                   8.0430(10)
_cell_length_c                   25.070(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1192.1(3)
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7807
_diffrn_reflns_theta_max         25.85
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         'data collection without standards'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_type   'no abs. correction'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         .186
_refine_diff_density_min         -.178
_refine_diff_density_rms         .038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.1(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.274
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_obs          0.0411
_refine_ls_shift/esd_max         0.025
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1043
_refine_ls_wR_factor_obs         0.1020
_reflns_number_observed          1994
_reflns_number_total             2204
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b303802p.txt
_cod_data_source_block           8a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0730P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'.
New tag '_refine_ls_weighting_details' was created. The value of the
new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0730P)^2^+0.0000P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      Pbc21
_cod_database_code               7204653