Chiral Synthesis of McGeachin-Type Bisaminals.
Chen, Yang; Li, Siqi; Hou, Shili; Xu, Jiaxi; Yang, Zhanhui; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03362

data_4037926
_publ_section_title
;
 Chiral Synthesis of McGeachin-Type Bisaminals.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03362
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C24 H25 N3'
_chemical_formula_sum            'C24 H25 N3'
_chemical_formula_weight         355.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
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  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
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'A short history of SHELX (Sheldrick, 2007)/Bruker'
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  1 omega  -29.00    9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -57.0000   60.0000 38

  2 omega   18.00   54.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   44.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega   15.00   42.00   1.0000    1.0000
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  5 omega   83.00  108.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 25

  6 omega   92.00  118.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  120.0000 26

  7 omega   73.00  107.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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  8 omega   54.00  121.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 67

  9 omega  100.00  125.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 25

 10 omega   68.00  115.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -150.0000 47

 11 omega   50.00  107.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 57

 12 omega   42.00  142.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000    0.0000 100

 13 omega   67.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   57.0000 -120.0000 37

 14 omega   49.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   77.0000 -180.0000 54

 15 omega   36.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   57.0000 -120.0000 27

 16 omega   22.00  103.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   57.0000    0.0000 81

 17 omega   38.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 38

 18 omega   44.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 27

 19 omega   43.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 28

 20 omega   39.00   89.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 50

 21 omega   44.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 47

 22 omega   56.00   99.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 43

 23 omega   44.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 24 omega    0.00   26.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
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 25 omega  -30.00   -4.00   1.0000    1.0000
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 26 omega   47.00   95.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 48

 27 omega   46.00   72.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
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 28 omega   42.00  175.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000   90.0000 133

 29 omega   58.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  178.0000  -60.0000 51

 30 omega   21.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   57.0000  150.0000 76
;
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_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           'Cu K\a'
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_diffrn_source                   'Enhance (Cu) X-ray Source'
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
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_exptl_crystal_density_diffrn    1.233
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_refine_ls_abs_structure_details
;
 Flack x determined using 1563 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(19)
_refine_ls_extinction_coef       0.0147(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_restraints     1
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_refine_ls_R_factor_all          0.0329
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.1301P] where P=(Fo^2^+2Fc^2^)/3'
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           exp_5470
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_cod_database_code               4037926
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
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_shelx_estimated_absorpt_t_max   0.872
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_shelx_hkl_checksum              72819
_shelx_res_checksum              24861
_shelx_shelxl_version_number     2014/7