Trienamines in Asymmetric Organocatalysis: Diels-Alder and Tandem Reactions
Zhi-Jun Jia; Hao Jiang; Jun-Long Li; Björn Gschwend; Qing-Zhu Li; Xiang Yin; Julie Grouleff; Ying-Chun Chen; Karl Anker Jørgensen; Journal of the American Chemical Society 133 (2011) 5053–5061; doi:10.1021/ja1112194

data_4105872
_publ_section_title
;
 Trienamines in Asymmetric Organocatalysis: Diels-Alder and Tandem
 Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5053
_journal_page_last               5061
_journal_paper_doi               10.1021/ja1112194
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C31 H35 N5 O9'
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
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_cell_length_c                   23.3125(4)
_cell_measurement_reflns_used    7715
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      1.8944
_cell_volume                     3172.40(11)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd.)'
_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9149
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Gemini S Ultra, Oxford Diffraction'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
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_diffrn_reflns_av_sigmaI/netI    0.0236
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10260
_diffrn_reflns_theta_full        69.47
_diffrn_reflns_theta_max         69.47
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.7935
_exptl_absorpt_correction_T_min  0.7381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+0.5926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                5105
_reflns_number_total             5550
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1112194_si_002.cif
_cod_data_source_block           5a
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