[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_4107083
_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            'C34 H49 B N9 O6 P S W'
_chemical_formula_weight         937.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.591(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1701(2)
_cell_length_b                   22.4204(3)
_cell_length_c                   16.2299(2)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.20
_cell_volume                     3933.50(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44159
_diffrn_reflns_theta_full        30.42
_diffrn_reflns_theta_max         30.42
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_T_max  0.7904
_exptl_absorpt_correction_T_min  0.3948
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      0
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.37
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_refine_diff_density_max         1.000
_refine_diff_density_min         -0.487
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_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         11818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.700
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_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          0.0809
_refine_ls_wR_factor_ref         0.0970
_reflns_number_gt                9392
_reflns_number_total             11818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2075086_si_001.cif
_cod_data_source_block           C34H49BN9O6PSW
_cod_original_cell_volume        3933.4(1)
_cod_database_code               4107083