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_4070046
_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         'C7 H17 N O2 Si'
_chemical_formula_sum            'C7 H17 N O2 Si'
_chemical_formula_weight         175.31
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.236(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6265(5)
_cell_length_b                   5.8852(5)
_cell_length_c                   12.9436(11)
_cell_measurement_reflns_used    5282
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      65.992
_cell_measurement_theta_min      6.418
_cell_volume                     495.10(7)
_computing_cell_refinement       Bruker-SAINT
_computing_data_collection       Bruker-SAINT
_computing_data_reduction        Bruker-SAINT
_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      99(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Bruker-Nonius_Kappa-Apex2_CCD
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  MONTEL_multi_layer_optics
_diffrn_radiation_source         rotating_anode
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20813
_diffrn_reflns_theta_full        33.19
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  .7465
_exptl_absorpt_correction_T_min  .6350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-Sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flat_needle
_exptl_crystal_F_000             192
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .02
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.053
_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   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0337P)^2^+0.0578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0773
_reflns_number_gt                3374
_reflns_number_total             3711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900583d_si_004.cif
_cod_data_source_block           fal19d
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi_scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4070046