The Acetyl Derivative of a Novel Fries Rearrangement Product
Jain, S. C.; Talwar, S.; Kumar, R.; Babu, B. R.; Errington, W.; Acta Crystallographica Section C 52 (1996) 2775–2777; doi:10.1107/S0108270196008487

data_2005604
_publ_section_title
;
 The Acetyl Derivative of a Novel Fries Rearrangement Product
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2775
_journal_page_last               2777
_journal_paper_doi               10.1107/S0108270196008487
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C26 H18 O8'
_chemical_formula_weight         458.40
_chemical_name_systematic
;
8,3'-methylene[7-acetoxy-4-methyl-2H-1-benzopyran-2-one] [4''-methyl-2''H-
1''-pyran-2''-one(5',6':6'',5'')-2'H-1'-benzopyran-2'-one]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.630(5)
_cell_length_b                   10.897(4)
_cell_length_c                   14.546(4)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     2160.5(13)
_computing_cell_refinement       'Siemens P3R3 system'
_computing_data_collection       'Siemens P3R3 system'
_computing_data_reduction        'SHELXTL- Plus (Sheldrick, 1990)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    SHELXTL-Plus
_diffrn_ambient_temperature      220(2)
_diffrn_measurement_device       'Siemens P3R3'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3827
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.189
_refine_ls_extinction_coef       0.0060(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    'H atoms riding (see text)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         2592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_obs          0.0475
_refine_ls_shift/esd_max         -0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.4311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1172
_refine_ls_wR_factor_obs         0.0954
_reflns_number_observed          1621
_reflns_number_total             2594
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cf1115.cif
_cod_data_source_block           coumab
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.4311P] 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^)+(0.0485P)^2^+0.4311P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005604