Development of a New Building Block for the Synthesis of Silicon-Based Drugs and Odorants: Alternative Synthesis of the Retinoid Agonist Disila-bexarotene
Büttner, Matthias W.; Nätscher, Jennifer B.; Burschka, Christian; Tacke, Reinhold; Organometallics 26 (2007) 4835–; doi:10.1021/om700570f

data_4073711
_publ_section_title
;
 Development of a New Building Block for the Synthesis of Silicon-Based
 Drugs and Odorants:&#x00A0; Alternative Synthesis of the Retinoid Agonist
 Disila-bexarotene
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4835
_journal_paper_doi               10.1021/om700570f
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C13 H22 O Si2'
_chemical_formula_sum            'C13 H22 O Si2'
_chemical_formula_weight         250.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.22(3)
_cell_angle_beta                 102.27(3)
_cell_angle_gamma                100.55(3)
_cell_formula_units_Z            4
_cell_length_a                   9.2211(18)
_cell_length_b                   10.489(2)
_cell_length_c                   16.445(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      7.?
_cell_volume                     1523.0(6)
_computing_cell_refinement       Stoe-IPDS
_computing_data_collection       Stoe-IPDS
_computing_data_reduction        Stoe-IPDS
_computing_molecular_graphics    Bruker-SHELXTL
_computing_publication_material  Bruker-SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  Stoe-IPDS
_diffrn_measurement_method       Stoe-IPDS
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22192
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             544
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         6771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0413
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.5354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                4867
_reflns_number_total             6771
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700570f-file004.cif
_cod_data_source_block           mbu11b
_cod_original_cell_volume        1522.9(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4073711