Oxidative rearrangements of isobenzofurans: studies toward the synthesis of the ajudazols.
Hobson, Stephen J.; Parkin, Andrew; Marquez, Rodolfo; Organic letters 10 (2008) 2813–2816; doi:10.1021/ol8009336

data_1504727
_publ_section_title
;
 Oxidative rearrangements of isobenzofurans: studies toward the synthesis
 of the ajudazols.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              2813
_journal_page_last               2816
_journal_paper_doi               10.1021/ol8009336
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C15 H18 O3'
_chemical_formula_sum            'C15 H18 O3'
_chemical_formula_weight         246.31
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             08-01-29
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 97.09(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.150(13)
_cell_length_b                   5.058(3)
_cell_length_c                   12.838(10)
_cell_measurement_reflns_used    3637
_cell_measurement_temperature    100
_cell_measurement_theta_max      24
_cell_measurement_theta_min      2
_cell_volume                     1234.0(15)
_computing_cell_refinement       'CrystalClear v1.4.0'
_computing_data_collection       'CrystalClear v1.4.0'
_computing_data_reduction        'CrystalClear v1.4.0'
_computing_molecular_graphics    Mercury
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
'Rigaku R-AXIS RAPID IP Area Detector Diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.207
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7318
_diffrn_reflns_theta_full        22.790
_diffrn_reflns_theta_max         23.255
_diffrn_reflns_theta_min         3.198
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       needle
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.00
_refine_diff_density_min         -1.12
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         1765
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1909
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.000069
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1766
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1766
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                718
_reflns_number_total             1765
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.68
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_scale          2.87(7)
_oxford_structure_analysis_title 'sx158 in P1 P21/c'
_cod_data_source_file            ol8009336-file005.cif
_cod_data_source_block           compound39
_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_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               1504727