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_4113440
_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                 107.892(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9307(14)
_cell_length_b                   15.139(2)
_cell_length_c                   13.712(2)
_cell_measurement_temperature    173(2)
_cell_volume                     1961.8(5)
_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 0.863
_diffrn_measured_fraction_theta_max 0.863
_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  0.1049
_diffrn_reflns_av_sigmaI/netI    0.2043
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9833
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_type   'empirical from SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6403
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.957
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1389
_reflns_number_gt                3935
_reflns_number_total             6403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029404c_s2_1.cif
_cod_data_source_block           C42H46BOP3Pd
_cod_original_cell_volume        1961.7(5)
_cod_database_code               4113440