Crystal structure of a new spiro-polytetrahydrofuran compound with translational pseudosymmetry: <i>rac</i>-(2<i>S</i>,2'<i>S</i>,5'<i>R</i>)-2-methyl-5'-[(1<i>R</i>,2<i>R</i>,5<i>S</i>,5'<i>R</i>)-1,4,4,5'-tetramethyldihydro-3'<i>H</i>-3,8-dioxaspiro[bicyclo[3.2.1]octane-2,2'-furan]-5'-yl]hexahydro[2,2'-bifuran]-5(2<i>H</i>)-one
Piccialli, Vincenzo; Tuzi, Angela; Centore, Roberto; Acta Crystallographica Section E 73 (2017) 780–784; doi:10.1107/S2056989017006065

data_2242250
_publ_section_title
;
 Crystal structure of a new spiro-polytetrahydrofuran compound with
 translational pseudosymmetry:
 <i>rac</i>-(2<i>S</i>,2'<i>S</i>,5'<i>R</i>)-2-methyl-5'-[(1<i>R</i>,2<i>R</i>,5<i>S</i>,5'<i>R</i>)-1,4,4,5'-tetramethyldihydro-3'<i>H</i>-3,8-dioxaspiro[bicyclo[3.2.1]octane-2,2'-furan]-5'-yl]hexahydro[2,2'-bifuran]-5(2<i>H</i>)-one
;
_journal_coeditor_code           RZ5214
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              780
_journal_page_last               784
_journal_paper_doi               10.1107/S2056989017006065
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C22 H34 O6'
_chemical_formula_moiety         'C22 H34 O6'
_chemical_formula_sum            'C22 H34 O6'
_chemical_formula_weight         394.49
_chemical_name_systematic
<i>rac</i>-(2<i>S</i>,2'<i>S</i>,5'<i>R</i>)-2-Methyl-5'-[(1<i>R</i>,2<i>R</i>,5<i>S</i>,5'<i>R</i>)-1,4,4,5'-tetramethyldihydro-3'<i>H</i>-3,8-dioxaspiro[bicyclo[3.2.1]octane-2,2'-furan]-5'-yl]hexahydro[2,2'-bifuran]-5(2<i>H</i>)-one
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                68.622(11)
_cell_angle_beta                 67.780(19)
_cell_angle_gamma                88.557(15)
_cell_formula_units_Z            4
_cell_length_a                   11.750(4)
_cell_length_b                   13.8050(10)
_cell_length_c                   14.737(2)
_cell_measurement_reflns_used    170
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.588
_cell_measurement_theta_min      3.775
_cell_volume                     2043.0(8)
_computing_cell_refinement
;
DIRAX/LSQ (Duisenberg <i>et al.</i>, 2000)
;
_computing_data_collection
;
<i>COLLECT</i> (Nonius, 1999)
;
_computing_data_reduction
;
EvalCCD (Duisenberg <i>et al.</i>, 2003)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method
;
CCD rotation images, thick slices
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.896
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         9260
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1092
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0357P)^2^+1.0216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                5634
_reflns_number_total             9260
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            rz5214sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2043.0(9)
_cod_database_code               2242250
_cod_database_fobs_code          2242250
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.989
_shelx_hkl_checksum              6844
_shelx_res_checksum              60065