Crystal structure of (<i>S</i>)-1-<i>O</i>-<i>tert</i>-butyldiphenylsilylglycerol: eight chiral molecules in a triclinic cell
Doboszewski, Bogdan; Nazarenko, Alexander Y.; Nemykin, Victor N.; e Silva, Maria Joselice; Acta Crystallographica Section E 74 (2018) 1373–1379; doi:10.1107/S2056989018012021

data_2242621
_publ_section_title
;
 Crystal structure of
 (<i>S</i>)-1-<i>O</i>-<i>tert</i>-butyldiphenylsilylglycerol: eight
 chiral molecules in a triclinic cell
;
_journal_coeditor_code           ZL2734
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1373
_journal_page_last               1379
_journal_paper_doi               10.1107/S2056989018012021
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C19 H26 O3 Si'
_chemical_formula_moiety         'C19 H26 O3 Si'
_chemical_formula_sum            'C19 H26 O3 Si'
_chemical_formula_weight         330.49
_chemical_melting_point          334
_chemical_name_common
(<i>S</i>)-1-<i>O</i>-<i>tert</i>-Butyldiphenylsilylglycerol
_chemical_name_systematic
;
3-[(<i>tert</i>-Butyldiphenylsilyl)oxy]propane-1,2-diol
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_cell_angle_alpha                111.053(8)
_cell_angle_beta                 91.616(7)
_cell_angle_gamma                92.898(7)
_cell_formula_units_Z            8
_cell_length_a                   14.7668(2)
_cell_length_b                   15.5936(2)
_cell_length_c                   17.2270(12)
_cell_measurement_reflns_used    124590
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     3692.7(3)
_computing_cell_refinement
;
<i>HKL-2000</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>CrystalClear</i> (Rigaku, 2009)
;
_computing_data_reduction
;
<i>CrystalClear</i> (Rigaku, 2009)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009) and <i>VESTA3</i> (Momma &
Izumi, 2008)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            124586
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.019
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1999)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.229
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 14181 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1839
_refine_ls_number_reflns         33607
_refine_ls_number_restraints     378
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0626P)^2^+0.2573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                31303
_reflns_number_total             33607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2734sup1.cif
_cod_data_source_block           1
_cod_database_code               2242621
_shelx_hkl_checksum              48957
_shelx_res_checksum              96071
_cod_database_fobs_code 2242621