Efficient Synthesis of Symmetrical α,α-Disubstituted β-Amino Acids and α,α-Disubstituted Aldehydes via Dialkylation of Nucleophilic β-Alanine Equivalent
Daizong Lin; Guanghui Deng; Jiang Wang; Xiao Ding; Hualiang Jiang; Hong Liu; Journal of Organic Chemistry 75 (2010) 1717–1722; doi:10.1021/jo902699t

data_4025282
_publ_section_title
;
 Efficient Synthesis of Symmetrical \a,\a-Disubstituted \b-Amino Acids and
 \a,\a-Disubstituted Aldehydes via Dialkylation of Nucleophilic \b-Alanine
 Equivalent
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1717
_journal_page_last               1722
_journal_paper_doi               10.1021/jo902699t
_journal_volume                  75
_journal_year                    2010
_chemical_formula_sum            'C36 H27 N5 Ni O7'
_chemical_formula_weight         700.34
_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                 110.978(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.273(2)
_cell_length_b                   11.4009(15)
_cell_length_c                   17.635(2)
_cell_measurement_reflns_used    1463
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      38.295
_cell_measurement_theta_min      4.375
_cell_volume                     3242.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  '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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1486
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17327
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79564
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.466
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.068
_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   0.786
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.786
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                2999
_reflns_number_total             6360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902699t_si_001.cif
_cod_data_source_block           cd2705
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        3242.7(7)
_cod_database_code               4025282