Catalytic enantio- and diastereoselective Mannich reaction of α-substituted isocyanoacetates and ketimines.
de la Campa, Raquel; Gammack Yamagata, Adam D.; Ortín, Irene; Franchino, Allegra; Thompson, Amber L.; Odell, Barbara; Dixon, Darren J.; Chemical communications (Cambridge, England) 52 (2016) 10632–10635; doi:10.1039/c6cc04132a

data_7124717
_publ_section_title
;
 Catalytic enantio- and diastereoselective Mannich reaction of
 \a-substituted isocyanoacetates and ketimines.
;
_journal_issue                   70
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10632
_journal_page_last               10635
_journal_paper_doi               10.1039/c6cc04132a
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H43 Ag N3 O4 P, 1.98(C H2 Cl2)'
_chemical_formula_sum            'C42.98 H46.96 Ag Cl3.96 N3 O4 P'
_chemical_formula_weight         948.89
_chemical_melting_point          ?
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-27
_audit_creation_method           CRYSTALS_ver_14.61_build_5555
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0180(1)
_cell_length_b                   17.0222(1)
_cell_length_c                   19.3743(1)
_cell_measurement_reflns_used    63422
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     4623.04(5)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            124114
_diffrn_reflns_theta_full        76.352
_diffrn_reflns_theta_max         76.352
_diffrn_reflns_theta_min         3.456
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.267
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1948.787
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.48
_refine_ls_abs_structure_details 'Flack (1983), 4324 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.017(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9636
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.0035348
_refine_ls_shift/su_mean         0.0000709
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 3.14P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0715
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0715
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                9450
_reflns_number_total             9674
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.23
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0276
_oxford_refine_ls_scale          3.189(17)
_oxford_reflns_number_all        9636
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 6531
_cod_data_source_file            c6cc04132a2.cif
_cod_data_source_block           1a-AgOAc
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C42.98 H46.96 Ag1 Cl3.96 N3 O4 P1'
_cod_database_code               7124717