Isolation of an inclusion complex of naphthol and its benzoate as an intermediate in the solvent-free benzoylation reaction of naphthol
Nakamatsu, Seiken; Yoshizawa, Kazuhiro; Toyota, Sinji; Toda, Fumio; Matijasic, Ivanka; Organic & Biomolecular Chemistry 1 (2003) 2231–; doi:10.1039/b303060c

data_7151435
_publ_section_title
;
 Isolation of an inclusion complex of naphthol and its benzoate as an
 intermediate in the solvent-free benzoylation reaction of naphthol
;
_journal_issue                   13
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              2231
_journal_paper_doi               10.1039/b303060c
_journal_volume                  1
_journal_year                    2003
_chemical_formula_moiety         'C26 H20 O4, 2(C10 H8 O2)'
_chemical_formula_sum            'C46 H36 O8'
_chemical_formula_weight         716.75
_chemical_name_systematic
; 
bisnaphthalene-2,3-diol 2,3-di(p-methylbenzoyloxy)naphthalene complex 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2b 2ac'
_symmetry_space_group_name_H-M   'P c n b'
_atom_sites_solution_hydrogens   'geom & dmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.448(1)
_cell_length_b                   15.243(1)
_cell_length_c                   31.849(1)
_cell_measurement_reflns_used    3157
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.089
_cell_measurement_theta_min      2.209
_cell_volume                     3615.8(6)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997-2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'graded mirror'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0347
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            5596
_diffrn_reflns_theta_full        65.10
_diffrn_reflns_theta_max         65.10
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.211
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                2383
_reflns_number_total             3062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303060c.txt
_cod_data_source_block           compound(15)
_cod_database_code               7151435