Polarization of the Pyridine Ring: Highly Functionalized Piperidines from Tungsten-Pyridine Complex
Daniel P. Harrison; Michal Sabat; William H. Myers; W. Dean Harman; Journal of the American Chemical Society 132 (2010) 17282–17295; doi:10.1021/ja107536w

data_4103623
_publ_section_title
;
 Polarization of the Pyridine Ring: Highly Functionalized Piperidines from
 Tungsten-Pyridine Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17282
_journal_page_last               17295
_journal_paper_doi               10.1021/ja107536w
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C25 H37 B N9 O4 P W'
_chemical_formula_weight         753.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 94.488(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.5913(6)
_cell_length_b                   23.5880(9)
_cell_length_c                   16.1339(6)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.42
_cell_volume                     6294.7(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0458
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            48644
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    3.766
_exptl_absorpt_correction_T_max  0.6607
_exptl_absorpt_correction_T_min  0.3787
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.334
_refine_diff_density_min         -1.401
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.836
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     777
_refine_ls_number_reflns         11460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.836
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0364
_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^)+(0.1000P)^2^+0.9254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1130
_reflns_number_gt                9428
_reflns_number_total             11460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja107536w_si_003.cif
_cod_data_source_block           C25H37BN9O4PW
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4103623