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_2242622
_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_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_moiety         'C19 H26 O3 Si'
_chemical_formula_sum            'C19 H26 O3 Si'
_chemical_formula_weight         330.49
_chemical_melting_point          334
_chemical_name_common            (S)-1-O-t-butyldiphenylsilylglycerol
_chemical_name_systematic        (S)-1-O-t-butyldiphenylsilylpropane-2,3-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                110.901(2)
_cell_angle_beta                 91.705(2)
_cell_angle_gamma                92.851(2)
_cell_formula_units_Z            8
_cell_length_a                   14.7922(10)
_cell_length_b                   15.6306(10)
_cell_length_c                   17.2048(11)
_cell_measurement_reflns_used    9308
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.91
_cell_volume                     3706.8(4)
_computing_cell_refinement
;
SAINT  (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT v8.34A (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_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      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker PHOTON-100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_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            120838
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_min         2.761
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.139
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.252
_refine_ls_abs_structure_details
;
Flack x determined using 11980 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013
;
_refine_ls_abs_structure_Flack   -0.008(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1857
_refine_ls_number_reflns         34177
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0633P)^2^+0.5751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                28468
_reflns_number_total             34177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2734sup1.cif
_cod_data_source_block           2
_cod_database_code               2242622
_cod_database_fobs_code          2242622
_shelx_hkl_checksum              20467
_shelx_res_checksum              80237