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_4023608
_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         'C22 H23 N O5 '
_chemical_formula_sum            'C22 H23 N O5'
_chemical_formula_weight         381.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2007-02-19
_audit_creation_method           'by CrystalStructure 3.8'
_cell_angle_alpha                102.699(13)
_cell_angle_beta                 97.108(14)
_cell_angle_gamma                109.078(12)
_cell_formula_units_Z            2
_cell_length_a                   10.3715(15)
_cell_length_b                   14.020(2)
_cell_length_c                   7.6066(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     996.6(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.020
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6034
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             404.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     276
_refine_ls_number_reflns         3049
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.0061
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                3043
_reflns_number_total             5813
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo800904u-file004.cif
_cod_data_source_block           '_m2313____________________'
_cod_original_formula_sum        'C22 H23 N O5 '
_cod_database_code               4023608