(2<i>S</i>,3<i>S</i>)-2,6-Dimethylheptane-1,3-diol, the oxygenated side chain of 22(<i>S</i>)-hydroxycholestrol, and its synthetic precursor (<i>R</i>)-4-benzyl-3-[(2<i>R</i>,3<i>S</i>)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one
Høgmoen Åstrand, Ove Alexander; Iqbal, Zeshan; Sandberg, Marcel; Kase, Eili T.; Görbitz, Carl Henrik; Rongved, Pål; Acta Crystallographica Section C 69 (2013) 647–650; doi:10.1107/S0108270113011852

data_2018960
_publ_section_title
;
 (2<i>S</i>,3<i>S</i>)-2,6-Dimethylheptane-1,3-diol, the oxygenated side
 chain of 22(<i>S</i>)-hydroxycholestrol, and its synthetic precursor
 (<i>R</i>)-4-benzyl-3-[(2<i>R</i>,3<i>S</i>)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one
;
_journal_coeditor_code           GZ3232
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              647
_journal_page_last               650
_journal_paper_doi               10.1107/S0108270113011852
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C19 H27 N O4'
_chemical_formula_moiety         'C19 H27 N O4'
_chemical_formula_sum            'C19 H27 N O4'
_chemical_formula_weight         333.42
_chemical_name_systematic
(<i>R</i>)-4-Benzyl-3-[(2<i>R</i>,3<i>S</i>)-3-hydroxy-2,6-dimethylheptanoyl]-1,3-oxazolidin-2-one
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.827(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.459(3)
_cell_length_b                   5.7077(13)
_cell_length_c                   15.247(3)
_cell_measurement_reflns_used    2875
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      24.73
_cell_measurement_theta_min      2.75
_cell_volume                     968.3(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method
'Sets of exposures each taken over 0.5\% \w rotation'
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7434
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.83
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.8367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'flat needle'
_exptl_crystal_F_000             360
_exptl_crystal_size_max          1.54
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.132
_refine_diff_density_min         -0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2047
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.1669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                1823
_reflns_number_total             2047
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3232.cif
_cod_data_source_block           II
_cod_original_cell_volume        968.4(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018960
_cod_database_fobs_code          2018960