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_7213023
_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            'C28 H34 Br2 Mn N3 O2'
_chemical_formula_weight         661.39
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 90.518(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2876(5)
_cell_length_b                   9.1876(4)
_cell_length_c                   24.399(1)
_cell_measurement_reflns_used    7416
_cell_measurement_temperature    120
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     2754.4(2)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics
;                                  
      ORTEP-III (Burnett & Johnson, 1996), KRYSTAL 
;
_computing_publication_material  KRYSTAL
_computing_structure_refinement  'modified ORFLS(1962), KRYSTAL'
_computing_structure_solution
;                                  
     SIR97 (Cascarano et al., 1996) KRYSTAL
;
_diffrn_ambient_temperature      120
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation scans with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'x-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.239
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            55917
_diffrn_reflns_reduction_process 55917
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.8
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    3.42
_exptl_absorpt_correction_T_max  0.69
_exptl_absorpt_correction_T_min  0.32
_exptl_absorpt_correction_type   'multi-scan, SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          .88
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .05
_refine_diff_density_max         1.4(2)
_refine_diff_density_min         -1.2(2)
_refine_ls_abs_structure_details
; Rogers (1981) parameter refined to 1.10 (9), reset to 1.0.
  1712 Bijvoet pairs in refinement.                    
;
_refine_ls_abs_structure_Rogers  1.0
_refine_ls_extinction_coef       14(13)
_refine_ls_extinction_method
;                                  
 Type 1 Lorentzian isotropic; Becker and Coppens (1974)
;
_refine_ls_goodness_of_fit_obs   0.745
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    38
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3748
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.060
_refine_ls_shift/esd_max         0.161
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.068
_reflns_number_observed          3748
_reflns_number_total             15788
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            900358dsup1.cif
_cod_data_source_block           2i
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^ ' was changed to 'calc'. New
tag '_refine_ls_weighting_details' was created. The value of the new
tag was set to 'w = 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|}^2^'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'constrained' was replaced with
the value 'constr' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

'_atom_site_thermal_displace_type' value 'Uij' was replaced with the
value 'Uani' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'
(140 times).

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        2754.3(2)
_cod_original_formula_sum        C28H34N3O2Br2Mn
_cod_database_code               7213023