Crystal structure and absolute configuration of (3a<i>S</i>,4<i>S</i>,5<i>R</i>,7a<i>R</i>)-2,2,7-trimethyl-3a,4,5,7a-tetrahydro-1,3-benzodioxole-4,5-diol
Macías, Mario A.; Suescun, Leopoldo; Pandolfi, Enrique; Schapiro, Valeria; Tibhe, Gaurao D.; Mombrú, Álvaro W.; Acta Crystallographica Section E 71 (2015) 1013–1016; doi:10.1107/S2056989015014590

data_2240988
_publ_section_title
;
 Crystal structure and absolute configuration of
 (3a<i>S</i>,4<i>S</i>,5<i>R</i>,7a<i>R</i>)-2,2,7-trimethyl-3a,4,5,7a-tetrahydro-1,3-benzodioxole-4,5-diol
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1013
_journal_page_last               1016
_journal_paper_doi               10.1107/S2056989015014590
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C10 H16 O4'
_chemical_formula_moiety         'C10 H16 O4'
_chemical_formula_sum            'C10 H16 O4'
_chemical_formula_weight         200.23
_chemical_name_systematic
(3a<i>S</i>,4<i>S</i>,5<i>R</i>,7a<i>R</i>)-2,2,7-Trimethyl-3a,4,5,7a-tetrahydro-1,3-benzodioxole-4,5-diol
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1230(13)
_cell_length_b                   7.5163(17)
_cell_length_c                   23.347(5)
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      66.732
_cell_measurement_theta_min      3.786
_cell_volume                     1074.5(4)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100 CMOS'
_diffrn_measurement_method       '\p and \w scans'
_diffrn_radiation_monochromator
;
Helios X-ray optical focusing and monochromatization module
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29451
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.444
_diffrn_reflns_theta_min         3.786
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.136
_refine_diff_density_min         -0.113
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 782 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.0063(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+0.2133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                1951
_reflns_number_total             1967
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2644sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     ' P 2ac 2ab'
_cod_database_code               2240988
_cod_database_fobs_code          2240988
_shelx_hkl_checksum              72972
_shelx_res_checksum              27606
_shelxl_version_number           2.014