Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of 3,4-Dimethyl-1-phenylphosphole
Kent D. Redwine; William L. Wilson; Donald G. Moses; Vincent J. Catalano; John H. Nelson; Inorganic Chemistry 39 (2000) 3392–3402; doi:10.1021/ic990885j

data_4321161
_publ_section_title
;
 Cooperative Diastereoselectivity of Palladium- and Platinum-Promoted
 Intramolecular [4+2] Diels-Alder Cycloaddition Reactions of
 3,4-Dimethyl-1-phenylphosphole
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3392
_journal_page_last               3402
_journal_paper_doi               10.1021/ic990885j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 H26 N2 O6 P2 Pd'
_chemical_formula_weight         606.81
_chemical_name_common            1a
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.4624(17)
_cell_length_b                   13.7194(17)
_cell_length_c                   20.3557(19)
_cell_measurement_temperature    298(2)
_cell_volume                     5156.0(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5582
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.885
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00152(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0362P)^2^+1.8563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                3526
_reflns_number_total             4544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990885j_1.cif
_cod_data_source_block           jhn030b
_cod_database_code               4321161