Preparation of α-Alkyl-β-Amino Acids via β-Alanine Ni(II) Complex
Daizong Lin; Li Lv; Jiang Wang; Xiao Ding; Hualiang Jiang; Hong Liu; Journal of Organic Chemistry 76 (2011) 6649–6656; doi:10.1021/jo200971k

data_4026518
_publ_section_title
;
 Preparation of \a-Alkyl-\b-Amino Acids via \b-Alanine Ni(II) Complex
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6649
_journal_page_last               6656
_journal_paper_doi               10.1021/jo200971k
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C29 H21 N3 Ni O3'
_chemical_formula_weight         518.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.322(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8486(13)
_cell_length_b                   9.5964(14)
_cell_length_c                   27.377(4)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      54.195
_cell_measurement_theta_min      4.501
_cell_volume                     2310.6(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0188
_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       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            16116
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      1.49
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0017(4)
_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   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         4487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0516P)^2^+0.6549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                4126
_reflns_number_total             4487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200971k_si_001.cif
_cod_data_source_block           mo_dm1013_0m
_cod_database_code               4026518