Chiral Silver Amide-Catalyzed Enantioselective [3 + 2] Cycloaddition of α-Aminophosphonates with Olefins
Yasuhiro Yamashita; Xun-Xiang Guo; Ryuta Takashita; Shū Kobayashi; Journal of the American Chemical Society 132 (2010) 3262–3263; doi:10.1021/ja100101n

data_4102030
_publ_section_title
;
 Chiral Silver Amide-Catalyzed Enantioselective [3 + 2] Cycloaddition of
 \a-Aminophosphonates with Olefins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3262
_journal_page_last               3263
_journal_paper_doi               10.1021/ja100101n
_journal_volume                  132
_journal_year                    2010
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C19 H29 F N O5 P '
_chemical_formula_sum            'C19 H29 F N O5 P'
_chemical_formula_weight         401.41
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.2992(5)
_cell_length_b                   9.2248(13)
_cell_length_c                   27.3952(5)
_cell_measurement_reflns_used    16810
_cell_measurement_temperature    88.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.1
_cell_volume                     2097.3(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR2002
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            19892
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856.00
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.79
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2038 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.05(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3899
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0019Fo^2^ + 1.0000\s(Fo^2^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0730
_reflns_number_gt                3877
_reflns_number_total             4776
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja100101n_si_002.cif
_cod_data_source_block           '_090804XGuo'
_cod_original_formula_sum        'C19 H29 F N O5 P '
_cod_database_code               4102030