Crystal structure of ({-})-(2<i>R</i>,3<i>S</i>,4<i>R</i>,5<i>R</i>)-5-(1,3-dithian-2-yl)-3-methyl-1-(triisopropylsilyloxy)hexane-2,4-diol
Cruz-Montanez, Alejandra; Piñero Cruz, Dalice M.; Prieto, Jose A.; Acta Crystallographica Section E 70 (2014) o1285–o1286; doi:10.1107/S160053681402443X

data_2240248
_publ_section_title
;
 Crystal structure of
 ({-})-(2<i>R</i>,3<i>S</i>,4<i>R</i>,5<i>R</i>)-5-(1,3-dithian-2-yl)-3-methyl-1-(triisopropylsilyloxy)hexane-2,4-diol
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1285
_journal_page_last               o1286
_journal_paper_doi               10.1107/S160053681402443X
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C20 H42 O3 S2 Si'
_chemical_formula_moiety         'C20 H42 O3 S2 Si'
_chemical_formula_sum            'C20 H42 O3 S2 Si'
_chemical_formula_weight         422.74
_chemical_name_systematic
(-)-(2<i>R</i>,3<i>S</i>,4<i>R</i>,5<i>R</i>)-5-(1,3-Dithian-2-yl)-3-methyl-1-(triisopropylsilyloxy)hexane-2,4-diol
_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-2014
_cell_angle_alpha                90
_cell_angle_beta                 101.253(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9691(4)
_cell_length_b                   8.3420(2)
_cell_length_c                   19.1245(5)
_cell_measurement_reflns_used    8415
_cell_measurement_temperature    124(2)
_cell_measurement_theta_max      70.90
_cell_measurement_theta_min      2.82
_cell_volume                     2498.68(11)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      124(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38635
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.747
_diffrn_reflns_theta_min         2.355
_exptl_absorpt_coefficient_mu    2.505
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.179
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 3771 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.035(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         9653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                8808
_reflns_number_total             9653
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5013sup1.cif
_cod_data_source_block           I
_cod_database_code               2240248
_cod_database_fobs_code          2240248
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.885
_shelx_hkl_checksum              14501
_shelx_res_checksum              49803
_shelxl_version_number           2.014