Doubly diastereoselective [3,3]-sigmatropic aza-Claisen rearrangements
Davies, Stephen G.; Garner, A. Christopher; Nicholson, Rebecca L.; Osborne, James; Roberts, Paul M.; Savory, Edward D.; Smith, Andrew D.; Thomson, James E.; Organic & Biomolecular Chemistry 7 (2009) 2604–2611; doi:10.1039/b902753j

data_7150660
_publ_section_title
;
 Doubly diastereoselective [3,3]-sigmatropic aza-Claisen rearrangements
;
_journal_issue                   12
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              2604
_journal_page_last               2611
_journal_paper_doi               10.1039/b902753j
_journal_volume                  7
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C17 H23 N1 O1'
_chemical_formula_sum            'C17 H23 N O'
_chemical_formula_weight         257.38
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.207(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3683(17)
_cell_length_b                   4.9903(8)
_cell_length_c                   12.8281(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    190
_cell_measurement_theta_max      43
_cell_measurement_theta_min      21
_cell_volume                     790.5(2)
_computing_cell_refinement       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_collection       'CAD4 EXPRESS, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin et al., 1994)'
_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      190
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1796
_diffrn_reflns_theta_full        74.060
_diffrn_reflns_theta_max         74.060
_diffrn_reflns_theta_min         3.451
_diffrn_standards_decay_%        2.87
_diffrn_standards_interval_time  600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_T_max  0.8151
_exptl_absorpt_correction_T_min  0.8151
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.36
_refine_diff_density_min         -0.32
_refine_ls_extinction_coef       99(15)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0335
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         1692
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000772
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
5.24 3.84 4.28
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0611
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0557
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1706
_reflns_number_total             1796
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0508
_oxford_refine_ls_scale          5.73(2)
_oxford_reflns_number_all        1796
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b902753j.txt
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C17 H23 N1 O1'
_cod_database_code               7150660