Germanium(II)-Mediated Reductive Cross-Aldol Reaction of Bromoaldehydes with Aldehydes: NMR Studies and ab Initio Calculations
Shin-ya Tanaka; Nobuo Tagashira; Kouji Chiba; Makoto Yasuda; Akio Baba; Journal of Organic Chemistry 73 (2008) 6312–6320; doi:10.1021/jo800904u

data_4023610
_publ_section_title
;
 Germanium(II)-Mediated Reductive Cross-Aldol Reaction
 of Bromoaldehydes with Aldehydes: NMR Studies
 and ab Initio Calculations
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6312
_journal_page_last               6320
_journal_paper_doi               10.1021/jo800904u
_journal_volume                  73
_journal_year                    2008
_chemical_formula_moiety         'C52 H52 O2 Si2 '
_chemical_formula_sum            'C52 H52 O2 Si2'
_chemical_formula_weight         765.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             2008-05-26
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.30(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   15.985(4)
_cell_length_b                   27.737(5)
_cell_length_c                   10.073(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      10.2
_cell_volume                     4466(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.692
_diffrn_measured_fraction_theta_max 0.692
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9471
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_standards_decay_%        0.36
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1632.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     563
_refine_ls_number_reflns         3157
_refine_ls_R_factor_gt           0.0963
_refine_ls_shift/su_max          0.0025
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
    Chebychev polynomial with 3 parameters (Carruthers & Watkin, 1979)
    5.2187    5.0005    3.7318
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                3146
_reflns_number_total             9033
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo800904u-file006.cif
_cod_data_source_block           '_m2086'
_cod_original_formula_sum        'C52 H52 O2 Si2 '
_cod_database_code               4023610