Inclusion Complex of (<i>S</i>)-1,3-Butanediol with (<i>S</i>,<i>S</i>)-(+)-<i>trans</i>-2,3-Bis(hydroxydiphenylmethyl)-1,4-dioxaspiro[4.4]nonane
Nishikawa, K.; Matsumoto, A.; Tsukada, H.; Shiro, M.; Toda, F.; Acta Crystallographica Section C 53 (1997) 351–353; doi:10.1107/S0108270196014175

data_2006020
_publ_contact_author
;
    Mr KAZUYOSHI NISHIKAWA
    Research Center
    Daicel Chemical Industries, Ltd.
    Himeji
    Hyogo
    Japan    671-12
;
_publ_section_title
;Inclusion Complex of (<i>S</i>)-1,3-Butanediol with
 (<i>S</i>,<i>S</i>)-(+)-<i>trans</i>-2,3-Bis(hydroxydiphenylmethyl)-1,4-dioxaspiro[4.4]nonane
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              351
_journal_page_last               353
_journal_paper_doi               10.1107/S0108270196014175
_journal_volume                  53
_journal_year                    1997
_chemical_formula_analytical     'C80.78 H6.67'
_chemical_formula_moiety         'C33 H32 O4, C4 H10 O2'
_chemical_formula_sum            'C37 H42 O6'
_chemical_formula_weight         582.74
_chemical_melting_point          445.0(3)
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 100.21(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.447(1)
_cell_length_b                   10.037(2)
_cell_length_c                   17.040(2)
_cell_measurement_reflns_used    16
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      27.6
_cell_volume                     1590.1(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation,
 1992)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1993)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.049
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            2696
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        -0.92
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             624.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.17
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       0.080(10)
_refine_ls_extinction_method     'Zachariasen (1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_obs   1.260
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     388
_refine_ls_number_reflns         2086
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.0010
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0553
_reflns_number_observed          2086
_reflns_number_total             2526
_reflns_observed_criterion       >3.0sigma(I)
_cod_data_source_file            ta1108.cif
_cod_data_source_block           RAS227
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '444.6-445.3' was changed to
'445.0(3)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 'w = 1/[\s^2^(Fo) +
0.00090|Fo|^2^]' 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) + 0.00090|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C37 H42 O6 '
_cod_database_code               2006020