A facile synthesis and crystallographic analysis of N-protected β-amino alcohols and short peptaibols.
Jadhav, Sandip V.; Bandyopadhyay, Anupam; Benke, Sushil N.; Mali, Sachitanand M.; Gopi, Hosahudya N.; Organic & biomolecular chemistry 9 (2011) 4182–4187; doi:10.1039/c0ob01226b

data_7151904
_publ_section_title
;
 A facile synthesis and crystallographic analysis of N-protected
 \b-amino alcohols and short peptaibols.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4182
_journal_page_last               4187
_journal_paper_doi               10.1039/c0ob01226b
_journal_volume                  9
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C18 H35 N3 O5'
_chemical_formula_sum            'C19 H36 Cl3 N3 O5'
_chemical_formula_weight         492.86
_chemical_melting_point          410(1)
_chemical_name_common            Boc-Aib-Ala-Leu-CH2OH
_chemical_name_systematic        Boc-Aib-Ala-Leu-CH2OH
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_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                   10.578(4)
_cell_length_b                   11.206(4)
_cell_length_c                   23.306(8)
_cell_measurement_temperature    296(2)
_cell_volume                     2762.6(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_pressure         101.325
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_av_sigmaI/netI    0.3083
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12526
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Graphite monochromator'
_exptl_absorpt_coefficient_mu    0.361
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method CHCl3
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.22(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.715
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.715
_refine_ls_R_factor_all          0.2755
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.087
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1608
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                1573
_reflns_number_total             6526
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ob01226b.txt
_cod_data_source_block           svj15
_cod_original_cell_volume        2762.7(17)
_cod_database_code               7151904