(2<i>R</i>,3<i>R</i>)-1,4-Dioxaspiro[4.4]nonane-2,3-dicarboxylic and (2<i>R</i>,3<i>R</i>)-1,4-dioxaspiro[4.5]decane-2,3-dicarboxylic acids
Minyaev, Mikhail E.; Roitershtein, Dmitrii M.; Vinogradov, Alexey A.; Ananyev, Ivan V.; Nifant'ev, Ilya E.; Acta Crystallographica Section E 74 (2018) 1058–1062; doi:10.1107/S2056989018009593

data_2242549
_publ_section_title
;
 (2<i>R</i>,3<i>R</i>)-1,4-Dioxaspiro[4.4]nonane-2,3-dicarboxylic and
 (2<i>R</i>,3<i>R</i>)-1,4-dioxaspiro[4.5]decane-2,3-dicarboxylic acids
;
_journal_coeditor_code           EB2009
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1058
_journal_page_last               1062
_journal_paper_doi               10.1107/S2056989018009593
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C10 H14 O6'
_chemical_formula_moiety         'C10 H14 O6'
_chemical_formula_sum            'C10 H14 O6'
_chemical_formula_weight         230.21
_chemical_melting_point          413.0(10)
_chemical_name_common
'(2R,3R)-1,4-dioxaspiro[4.5]decane-2,3-dicarboxylic acid'
_chemical_name_systematic
'(2<i>R</i>,3<i>R</i>)-1,4-Dioxaspiro[4.5]decane-2,3-dicarboxylic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 94.469(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.4272(8)
_cell_length_b                   5.2976(6)
_cell_length_c                   15.5678(19)
_cell_measurement_reflns_used    361
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      3
_cell_volume                     528.45(11)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2017 (Sheldrick, 2015) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4329
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.996
_diffrn_reflns_theta_min         2.625
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.9947
_exptl_absorpt_correction_T_min  0.9171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             244
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2612
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0411P)^2^+0.0783P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0717
_reflns_number_gt                2503
_reflns_number_total             2612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eb2009sup1.cif
_cod_data_source_block           II
_cod_database_code               2242549
_cod_database_fobs_code          2242549
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              43106
_shelx_res_checksum              9877