Synthesis, Structure, and Reactivity of a η3-1-Hydroxyallyl Complex: Protonation of an α,β-Unsaturated Carbonyl Compound Bound to Palladium(0) and Platinum(0)
Sensuke Ogoshi; Masaki Morita; Hideo Kurosawa; Journal of the American Chemical Society 125 (2003) 9020–9021; doi:10.1021/ja0361042

data_4113993
_publ_section_title
;
 Synthesis, Structure, and Reactivity of a \h3-1-Hydroxyallyl Complex:
 Protonation of an \a,\b-Unsaturated Carbonyl Compound Bound to
 Palladium(0) and Platinum(0)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9020
_journal_page_last               9021
_journal_paper_doi               10.1021/ja0361042
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C41 H37 F3 O4 P2 Pd S'
_chemical_formula_weight         851.14
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.429(1)
_cell_length_b                   12.8667(8)
_cell_length_c                   14.2909(6)
_cell_measurement_reflns_used    37953
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     3940.3(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.9957
_diffrn_measured_fraction_theta_max 0.9957
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.053
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36628
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.10
_refine_diff_density_min         -0.97
_refine_ls_abs_structure_Flack   0.0(1)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.345
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     469
_refine_ls_number_reflns         2911
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          1.4507
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                2911
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_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ja0361042si20030514_112159.cif
_cod_data_source_block           morita2
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C41 H37 F3 O4 P2 Pd S '
_cod_database_code               4113993