[4 + 2] Cyclocondensation Reactions of Tungsten-Dihydropyridine Complexes and the Generation of Tri- and Tetrasubstituted Piperidines
Daniel P. Harrison; Diana A. Iovan; William H. Myers; Michal Sabat; Sisi Wang; Victor E. Zottig; W. Dean Harman; Journal of the American Chemical Society 133 (2011) 18378–18387; doi:10.1021/ja2075086

data_4107086
_publ_section_title
;
 [4 + 2] Cyclocondensation Reactions of Tungsten-Dihydropyridine Complexes
 and the Generation of Tri- and Tetrasubstituted Piperidines
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18378
_journal_page_last               18387
_journal_paper_doi               10.1021/ja2075086
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C29.5 H40.5 B N9 O3 P W'
_chemical_formula_weight         794.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.337(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.156(1)
_cell_length_b                   23.184(2)
_cell_length_c                   17.542(1)
_cell_measurement_reflns_used    3236
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      21.60
_cell_measurement_theta_min      2.29
_cell_volume                     6695.5(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0822
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30739
_diffrn_reflns_theta_full        21.89
_diffrn_reflns_theta_max         21.89
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    3.543
_exptl_absorpt_correction_T_max  0.7183
_exptl_absorpt_correction_T_min  0.3619
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_meas      0
_exptl_crystal_description       needle
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.440
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         8063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0516
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1515
_reflns_number_gt                5836
_reflns_number_total             8063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2075086_si_004.cif
_cod_data_source_block           dan55_0m
_cod_original_cell_volume        6695.2(9)
_cod_original_formula_sum        'C29.50 H40.50 B N9 O3 P W'
_cod_database_code               4107086