Highly stereoselective, cobalt(III)-directed Mannich additions in water yielding α-methylamino acid products.
Oerum, Stephanie; Krabbe, Peter; Schau-Magnussen, Magnus; Furbo, Søren; Bendix, Jesper; Hammershøi, Anders; Dalton transactions (Cambridge, England : 2003) 42 (2013) 292–298; doi:10.1039/c2dt32250a

data_7022280
_publ_section_title
;
 Highly stereoselective, cobalt(III)-directed Mannich additions in water
 yielding \a-methylamino acid products.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              292
_journal_page_last               298
_journal_paper_doi               10.1039/c2dt32250a
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C8 H23 Co N6 O4, Cl4 Zn'
_chemical_formula_sum            'C8 H23 Cl4 Co N6 O4 Zn'
_chemical_formula_weight         533.42
_chemical_name_common
;
rac-cdelta*-bis(ethane-1,2-diamine)((S*)-N-methyl-3-nitro-
(R*)-alaninato-kappa$2!N,O$1!)cobalt(iii) tetrachloridozincate
;
_chemical_name_systematic
;
rac-\D*-bis(ethane-1,2-diamine)[(<i>S</i>*)-<i>N</i>-methyl-3-nitro-(<i>R</i>*)-
alaninato-\k^2^<i>N,O</i>^1^]cobalt(III) tetrachloridozincate

;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 103.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.739(2)
_cell_length_b                   17.035(3)
_cell_length_c                   11.652(6)
_cell_measurement_reflns_used    25110
_cell_measurement_temperature    122(1)
_cell_measurement_theta_max      33.00
_cell_measurement_theta_min      2.39
_cell_volume                     1877.0(11)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Mercury (Macrae et. al., 2006)
;
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\w and \f 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  0.1036
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62337
_diffrn_reflns_theta_full        33.00
_diffrn_reflns_theta_max         33.00
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    2.757
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.215
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.904
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         6997
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+6.0734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                6573
_reflns_number_total             6997
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32250a.txt
_cod_data_source_block           kcd129
_cod_original_cell_volume        1876.9(11)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7022280