Crystal structure of (±)-(7<i>RS</i>,8<i>SR</i>)-7-methyl-1,4-dioxaspiro[4.5]decane-7,8-diol
Oishi, Takeshi; Yamamoto, Hiroaki; Sugai, Tomoya; Fukaya, Keisuke; Yamaguchi, Yu; Watanabe, Ami; Sato, Takaaki; Chida, Noritaka; Acta Crystallographica Section E 71 (2015) 1181–1184; doi:10.1107/S2056989015016783

data_2241125
_publ_section_title
;
 Crystal structure of
 (+-)-(7<i>RS</i>,8<i>SR</i>)-7-methyl-1,4-dioxaspiro[4.5]decane-7,8-diol
;
_journal_coeditor_code           IS5419
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1181
_journal_page_last               1184
_journal_paper_doi               10.1107/S2056989015016783
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C9 H16 O4'
_chemical_formula_moiety         'C9 H16 O4'
_chemical_formula_sum            'C9 H16 O4'
_chemical_formula_weight         188.22
_chemical_melting_point          360.2
_chemical_name_systematic
;
(+-)-(7<i>RS</i>,8<i>SR</i>)-7-Methyl-1,4-dioxaspiro[4.5]decane-7,8-diol
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 103.281(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7403(5)
_cell_length_b                   18.1498(11)
_cell_length_c                   6.7335(5)
_cell_measurement_reflns_used    2733
_cell_measurement_temperature    90.0
_cell_measurement_theta_max      24.66
_cell_measurement_theta_min      2.70
_cell_volume                     920.66(11)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>Mercury</i> (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010) and <i>PLATON</i> (Spek, 2009)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2013</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      90.0
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8165
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.4103P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0916
_reflns_number_gt                1205
_reflns_number_total             1612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5419sup1.cif
_cod_data_source_block           I
_cod_database_code               2241125
_cod_database_fobs_code          2241125
_shelx_res_checksum              46280