Silicon-Containing Dipeptidic Aspartame and Neotame Analogues
Dörrich, Steffen; Falgner, Steffen; Schweeberg, Sarah; Burschka, Christian; Brodin, Peter; Wissing, Britt Marie; Basta, Babro; Schell, Peter; Bauer, Udo; Tacke, Reinhold; Organometallics 31 (2012) 5903–; doi:10.1021/om300442e

data_4078831
_publ_section_title
;
 Silicon-Containing Dipeptidic Aspartame and Neotame Analogues
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              5903
_journal_paper_doi               10.1021/om300442e
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C24 H38 N2 O7 Si'
_chemical_formula_sum            'C24 H38 N2 O7 Si'
_chemical_formula_weight         494.65
_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                 100.233(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8973(11)
_cell_length_b                   11.2852(17)
_cell_length_c                   21.447(2)
_cell_measurement_reflns_used    3863
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.25
_cell_measurement_theta_min      4.5
_cell_volume                     2833.7(6)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  image_plate_Stoe-IPDS
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            41120
_diffrn_reflns_theta_full        29.14
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_correction_T_min  0.9125
_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    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         14687
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                8407
_reflns_number_total             14687
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300442e_si_001.cif
_cod_data_source_block           dor05e
_cod_original_cell_volume        2833.8(6)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4078831