Nucleophile‒Electrophile Interactions in 1,8-Disubstituted Naphthalenes: Structures of Three 1-Naphthaldehydes and a 1-Naphthyl Methyl Ketone
Gallucci, J. C.; Hart, D. J.; Young, D. G. J.; Acta Crystallographica Section B 54 (1998) 73–81; doi:10.1107/S0108768197009440

data_2105538
_publ_section_title
;
 Nucleophile--Electrophile Interactions in 1,8-Disubstituted Naphthalenes:
 Structures of Three 1-Naphthaldehydes and a 1-Naphthyl Methyl Ketone
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              73
_journal_page_last               81
_journal_paper_doi               10.1107/S0108768197009440
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C21 H20 O6 S '
_chemical_formula_sum            'C21 H20 O6 S'
_chemical_formula_weight         400.45
_chemical_melting_point          422.0(10)
_chemical_name_systematic
' 4,8-dimethoxy-5-(tosyloxy)-1-acetonaphthone'
_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'
_cell_angle_alpha                90
_cell_angle_beta                 99.290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.586(2)
_cell_length_b                   7.7270(10)
_cell_length_c                   24.361(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     1966.5(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'TEXSAN (MSC, 1993)'
_computing_molecular_graphics    'ORTEP--II (Johnson, 1976)'
_computing_publication_material  'TEXSAN (MSC, 1993)'
_computing_structure_refinement  'TEXSAN (MSC, 1993)'
_computing_structure_solution    'SHELXS--86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            5102
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0.25
_diffrn_standards_interval_count 150
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular rod'
_exptl_crystal_F_000             840.00
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       '1.0(1) E-06'
_refine_ls_extinction_method     'Zachariasen (1963)'
_refine_ls_goodness_of_fit_obs   1.508
_refine_ls_hydrogen_treatment    'see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/\s^2^(Fo)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0486
_reflns_number_observed          2752
_reflns_number_total             4848
_reflns_observed_criterion       I>1sigma(I)
_cod_data_source_file            bk0045.cif
_cod_data_source_block           Hart4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '421--423 K' was changed to
'422.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

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)' 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)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1966.4(9)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C21 H20 O6 S '
_cod_database_code               2105538