Enantioselective α-amination of ketones mediated by chiral nitridomanganese(V) complexes using ammonia as the terminal nitrogen source
Svenstrup, Niels; Bøgevig, Anders; Hazell, Rita G.; Jørgensen, Karl Anker; Journal of the Chemical Society, Perkin Transactions 1  (1999) 1559–; doi:10.1039/a900358d

data_7213022
_publ_section_title
;
 Enantioselective \a-amination of ketones mediated by chiral
 nitridomanganese(V) complexes using ammonia as the terminal nitrogen
 source
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1559
_journal_paper_doi               10.1039/a900358d
_journal_year                    1999
_chemical_formula_sum            'C36 H52 Mn N3 O2'
_chemical_formula_weight         613.75
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.1440(10)
_cell_angle_beta                 78.5960(10)
_cell_angle_gamma                71.5410(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9795(4)
_cell_length_b                   13.4234(6)
_cell_length_c                   14.6685(6)
_cell_measurement_reflns_used    16219
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      1.8
_cell_volume                     1659.37(12)
_computing_cell_refinement       'SAINT,  Siemens, 1995'
_computing_data_collection       'SMART, Siemens, 1995'
_computing_data_reduction        'SAINT,  Siemens, 1995'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      122(2)
_diffrn_measured_fraction_theta_full 0.805
_diffrn_measured_fraction_theta_max 0.805
_diffrn_measurement_device_type  'area detector'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9514
_diffrn_reflns_theta_full        25.92
_diffrn_reflns_theta_max         25.92
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         9514
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.628
_refine_ls_shift/su_mean         0.042
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+3.1889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                8212
_reflns_number_total             9514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900358dsup1.cif
_cod_data_source_block           2f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7213022