Efficient Synthesis of an η2-Pyridine Complex and a Preliminary Investigation of the Bound Heterocycle's Reactivity
Daniel P. Harrison; Kevin D. Welch; Adam C. Nichols-Nielander; Michal Sabat; William H. Myers; W. Dean Harman; Journal of the American Chemical Society 130 (2008) 16844–16845; doi:10.1021/ja807521d

data_4108849
_publ_section_title
;
 Efficient Synthesis of an \h2-Pyridine Complex and a Preliminary
 Investigation of the Bound Heterocycle's Reactivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16844
_journal_page_last               16845
_journal_paper_doi               10.1021/ja807521d
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C22 H32 B N8 O3 P W'
_chemical_formula_weight         682.19
_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                 91.690(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6310(10)
_cell_length_b                   13.9510(10)
_cell_length_c                   16.6470(10)
_cell_measurement_reflns_used    6528
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.68
_cell_measurement_theta_min      2.262
_cell_volume                     2700.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_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     0.71074
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39877
_diffrn_reflns_theta_full        31.68
_diffrn_reflns_theta_max         31.68
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    4.377
_exptl_absorpt_correction_T_max  0.801929
_exptl_absorpt_correction_T_min  0.602151
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS  '
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       needle
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.453
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         16957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                10886
_reflns_number_total             16957
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja807521d_si_004.cif
_cod_data_source_block           C22H32BN8O3PW
_cod_database_code               4108849