Facile Diels-Alder Reactions with Pyridines Promoted by Tungsten
Peter M. Graham; David A. Delafuente; Weijun Liu; William H. Myers; Michal Sabat; W. D. Harman; Journal of the American Chemical Society 127 (2005) 10568–10572; doi:10.1021/ja050143r

data_4111844
_publ_section_title
;
 Facile Diels-Alder Reactions with Pyridines Promoted by Tungsten
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10568
_journal_page_last               10572
_journal_paper_doi               10.1021/ja050143r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C22 H32 B N10 O P W'
_chemical_formula_weight         678.21
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.808(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.4866(7)
_cell_length_b                   15.1344(12)
_cell_length_c                   10.3639(9)
_cell_measurement_reflns_used    6345
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      32.607
_cell_measurement_theta_min      2.382
_cell_volume                     1326.45(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.1527
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18587
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.57
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    4.451
_exptl_absorpt_correction_T_max  0.801927
_exptl_absorpt_correction_T_min  0.655941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS '
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.855
_refine_diff_density_min         -1.731
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.023(8)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.733
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         9499
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.733
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0088P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                6244
_reflns_number_total             9499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050143rsi20050110_110438.cif
_cod_data_source_block           c22h32bn10opw
_cod_database_code               4111844