Asymmetric Synthesis of the Nonproteinogenic Silicon-Containing α-Amino Acids (R)- and (S)-α-[(Trimethylsilyl)methyl]alanine
Falgner, Steffen; Burschka, Christian; Wagner, Stephan; Böhm, Andreas; Daiss, Jürgen O.; Tacke, Reinhold; Organometallics 28 (2009) 6059–6066; doi:10.1021/om900583d

data_4070045
_publ_section_title
;
 Asymmetric Synthesis of the Nonproteinogenic Silicon-Containing \a-Amino
 Acids (R)- and (S)-\a-[(Trimethylsilyl)methyl]alanine
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              6059
_journal_page_last               6066
_journal_paper_doi               10.1021/om900583d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C9 H18 O4 Si'
_chemical_formula_sum            'C9 H18 O4 Si'
_chemical_formula_weight         218.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 91.65(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.3149(11)
_cell_length_b                   15.034(2)
_cell_length_c                   13.090(3)
_cell_measurement_reflns_used    2963
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      6.15
_cell_volume                     1242.2(4)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Ortep/Povray
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  Stoe-IPDS_image_plate
_diffrn_measurement_method       omega_scan
_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  0.0967
_diffrn_reflns_av_sigmaI/netI    0.0567
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12930
_diffrn_reflns_theta_full        27.91
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  1.4494
_exptl_absorpt_correction_T_min  0.7760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .4
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         2760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0819P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                2000
_reflns_number_total             2760
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900583d_si_003.cif
_cod_data_source_block           fal04g
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4070045