A Facile Cu(I)/TF-Bipham Phos-Catalyzed Asymmetric Approach to Unnatural α-Amino Acid Derivatives Containinggem-Bisphosphonates
Zhi-Yong Xue; Qing-Hua Li; Hai-Yan Tao; Chun-Jiang Wang; Journal of the American Chemical Society 133 (2011) 11757–11765; doi:10.1021/ja2043563

data_4106478
_publ_section_title
;
 A Facile Cu(I)/TF-Bipham Phos-Catalyzed Asymmetric Approach to Unnatural
 \a-Amino Acid Derivatives Containinggem-Bisphosphonates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11757
_journal_page_last               11765
_journal_paper_doi               10.1021/ja2043563
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration 7R,8S
_chemical_formula_sum            'C19 H33.5 N O8 P2'
_chemical_formula_weight         465.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.902(2)
_cell_length_b                   11.717(3)
_cell_length_c                   23.448(6)
_cell_measurement_temperature    293(2)
_cell_volume                     2445.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14364
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.219
_exptl_absorpt_correction_T_max  0.9493
_exptl_absorpt_correction_T_min  0.9332
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_coef       0.0011(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+1.9722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1860
_reflns_number_gt                3374
_reflns_number_total             4805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2043563_si_002.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C19 H33.50 N O8 P2'
_cod_database_code               4106478