Direct catalytic asymmetric Mannich-type reaction of beta-keto phosphonate using a dinuclear Ni2-Schiff base complex.
Chen, Zhihua; Yakura, Kenichiro; Matsunaga, Shigeki; Shibasaki, Masakatsu; Organic letters 10 (2008) 3239–3242; doi:10.1021/ol800965t

data_1504731
_publ_section_title
;
 Direct catalytic asymmetric Mannich-type reaction of beta-keto
 phosphonate using a dinuclear Ni2-Schiff base complex.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3239
_journal_page_last               3242
_journal_paper_doi               10.1021/ol800965t
_journal_volume                  10
_journal_year                    2008
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C21 H31 Cl N O6 P '
_chemical_formula_sum            'C21 H31 Cl N O6 P'
_chemical_formula_weight         459.91
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 95.391(2)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   10.4863(4)
_cell_length_b                   10.1556(4)
_cell_length_c                   10.9469(5)
_cell_measurement_reflns_used    7769
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.1
_cell_volume                     1160.63(8)
_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    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13228
_diffrn_reflns_theta_full        68.22
_diffrn_reflns_theta_max         68.22
_exptl_absorpt_coefficient_mu    2.419
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.512
_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    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             488.00
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.37
_refine_diff_density_min         -0.78
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1858 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4081
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.0015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0002Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                3258
_reflns_number_total             4081
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol800965t-file005.cif
_cod_data_source_block           '_080403chenparachloro'
_cod_original_cell_volume        1160.64(8)
_cod_original_formula_sum        'C21 H31 Cl N O6 P '
_cod_database_code               1504731