Palladium(II)-Catalyzed Cycloisomerization of Substituted 1,5-Hexadienes: A Combined Experimental and Computational Study on an Open and an Interrupted Hydropalladation/Carbopalladation/β-Hydride Elimination (HCHe) Catalytic Cycle
Björn Nelson; Sonja Herres-Pawlis; Wolf Hiller; Hans Preut; Carsten Strohmann; Martin Hiersemann; Journal of Organic Chemistry 77 (2012) 4980–4995; doi:10.1021/jo3004088

data_4027217
_publ_section_title
;
 Palladium(II)-Catalyzed Cycloisomerization of Substituted 1,5-Hexadienes:
 A Combined Experimental and Computational Study on an Open and an
 Interrupted Hydropalladation/Carbopalladation/\b-Hydride Elimination
 (HCHe) Catalytic Cycle
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4980
_journal_page_last               4995
_journal_paper_doi               10.1021/jo3004088
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C22 H36 O6'
_chemical_formula_weight         396.51
_space_group_IT_number           2
_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                87.965(7)
_cell_angle_beta                 72.478(10)
_cell_angle_gamma                77.756(7)
_cell_formula_units_Z            2
_cell_length_a                   9.0823(9)
_cell_length_b                   11.2934(7)
_cell_length_c                   11.7674(16)
_cell_measurement_temperature    173(2)
_cell_volume                     1124.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.845
_diffrn_measured_fraction_theta_max 0.845
_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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.1066
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10014
_diffrn_reflns_theta_full        28.98
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.084
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_F_000             432
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5044
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.0674
_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^)+(0.1126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2580
_reflns_number_gt                2578
_reflns_number_total             5044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo3004088_si_004.cif
_cod_data_source_block           preu
_cod_depositor_comments
;

2022-01-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum        'C44 H72 O12'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     793.02
_cod_database_code               4027217