Stereoselective Cyclization and Pyramidal Inversion Strategies for P-Chirogenic Phospholane Synthesis
Garrett Hoge; Journal of the American Chemical Society 126 (2004) 9920–9921; doi:10.1021/ja048079l

data_4112857
_publ_section_title
;
 Stereoselective Cyclization and Pyramidal Inversion Strategies for
 P-Chirogenic Phospholane Synthesis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9920
_journal_page_last               9921
_journal_paper_doi               10.1021/ja048079l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C17 H19 B P'
_chemical_formula_weight         265.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                61.938(3)
_cell_angle_beta                 76.230(3)
_cell_angle_gamma                63.747(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6803(17)
_cell_length_b                   10.1882(18)
_cell_length_c                   10.5467(18)
_cell_measurement_temperature    299(2)
_cell_volume                     822.6(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      299(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  '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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7249
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.9573
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_meas      0
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6399
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1472
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1765
_reflns_number_gt                3345
_reflns_number_total             6399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048079lsi20040402_050027.cif
_cod_data_source_block           sad1
_cod_original_cell_volume        822.6(2)
_cod_database_code               4112857