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_7150662
_publ_section_title
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 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         'C29 H32.33 N1 O2'
_chemical_formula_sum            'C29 H32.33 N O2'
_chemical_formula_weight         426.91
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9487(2)
_cell_length_b                   5.18510(10)
_cell_length_c                   52.2900(7)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    190
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2426.25(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            4856
_diffrn_reflns_theta_full        25.218
_diffrn_reflns_theta_max         27.411
_diffrn_reflns_theta_min         5.111
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             917.303
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.63
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9860
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         2520
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0777
_refine_ls_shift/su_max          0.023145
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Quasi-Unit weights
W = 1.0 or 1./2F
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1858
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1587
_reflns_limit_h_max              11
_reflns_limit_h_min              0
_reflns_limit_k_max              6
_reflns_limit_k_min              0
_reflns_limit_l_max              67
_reflns_limit_l_min              0
_reflns_number_gt                2375
_reflns_number_total             3067
_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   0.0809
_oxford_refine_ls_scale          0.919(5)
_oxford_reflns_number_all        3066
_oxford_reflns_threshold_expression_ref I>1.5\s(I)
_cod_data_source_file            b902753j.txt
_cod_data_source_block           3
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 21 21 21 '
_cod_original_formula_sum        'C29 H32.33 N1 O2'
_cod_database_code               7150662