Stereochemistry of Palladium-Mediated Synthesis of PAMP-BH3: Retention of Configuration at P in Formation of Pd-P and P-C Bonds
Jillian R. Moncarz; Tim J. Brunker; David S. Glueck; Roger D. Sommer; Arnold L. Rheingold; Journal of the American Chemical Society 125 (2003) 1180–1181; doi:10.1021/ja029404c

data_4113441
_publ_section_title
;
 Stereochemistry of Palladium-Mediated Synthesis of PAMP-BH3: Retention of
 Configuration at P in Formation of Pd-P and P-C Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1180
_journal_page_last               1181
_journal_paper_doi               10.1021/ja029404c
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C42 H46 B O P3 Pd'
_chemical_formula_weight         776.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.6720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9565(7)
_cell_length_b                   17.8335(13)
_cell_length_c                   11.1574(7)
_cell_measurement_reflns_used    3329
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.232
_cell_measurement_theta_min      4.685
_cell_volume                     1980.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10023
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.8966
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.709
_refine_diff_density_min         -0.787
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6543
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0631P)^2^+1.0196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1260
_reflns_number_gt                5227
_reflns_number_total             6543
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029404c_s2_2.cif
_cod_data_source_block           glu99
_cod_database_code               4113441