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_7151903
_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         'C20 H23 N O3'
_chemical_formula_sum            'C20 H23 N O3'
_chemical_formula_weight         325.39
_chemical_melting_point          394(1)
_chemical_name_common            Fmoc-Val-CH2OH
_chemical_name_systematic        Fmoc-Val-CH2OH
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.573(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.942(4)
_cell_length_b                   11.622(11)
_cell_length_c                   15.783(14)
_cell_measurement_temperature    296(2)
_cell_volume                     904.7(14)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9389
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'graphite monochromator'
_exptl_absorpt_coefficient_mu    0.080
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod shape'
_exptl_crystal_F_000             348
_exptl_crystal_recrystallization_method MeOH
_refine_diff_density_max         0.107
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.7(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.456
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4239
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.456
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.097
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0548
_reflns_number_gt                2760
_reflns_number_total             4239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ob01226b.txt
_cod_data_source_block           svj1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7151903