Amino acid motifs in natural products: synthesis of O-acylated derivatives of (2S,3S)-3-hydroxyleucine.
Ries, Oliver; Büschleb, Martin; Granitzka, Markus; Stalke, Dietmar; Ducho, Christian; Beilstein journal of organic chemistry 10 (2014) 1135–1142; doi:10.3762/bjoc.10.113

data_4029596
_publ_section_title
;
 Amino acid motifs in natural products: synthesis of O-acylated
 derivatives of (2S,3S)-3-hydroxyleucine.
;
_journal_name_full               'Beilstein journal of organic chemistry'
_journal_page_first              1135
_journal_page_last               1142
_journal_paper_doi               10.3762/bjoc.10.113
_journal_volume                  10
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H47 N O4 Si'
_chemical_formula_sum            'C31 H47 N O4 Si'
_chemical_formula_weight         525.79
_chemical_name_common            RO_3-061
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7538(17)
_cell_length_b                   11.8065(17)
_cell_length_c                   22.371(3)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.646
_cell_measurement_theta_min      2.445
_cell_volume                     3104.5(8)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2009.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL in SHELXTL Version 2008/3'
_computing_structure_solution    'SHELXS in SHELXTL Version 2008/3'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0184
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86428
_diffrn_reflns_theta_full        25.34
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.89354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.7583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                5404
_reflns_number_total             5682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1860-5397-10-113-S1.cif
_cod_data_source_block           p212121
_cod_depositor_comments          'Adding full bibliography for 4029596.cif.'
_cod_database_code               4029596