Mechanistic Insights on Pd/Cu-Catalyzed Dehydrogenative Coupling of Dimethyl Phthalate
Hirano, Masafumi; Sano, Kosuke; Kanazawa, Yuki; Komine, Nobuyuki; Maeno, Zen; Mitsudome, Takato; Takaya, Hikaru; ACS Catalysis 8 (2018) 5827–; doi:10.1021/acscatal.8b01095

data_4515704
_publ_section_title
;
 Mechanistic Insights on Pd/Cu-Catalyzed Dehydrogenative Coupling of
 Dimethyl Phthalate
;
_journal_issue                   7
_journal_name_full               'ACS Catalysis'
_journal_page_first              5827
_journal_paper_doi               10.1021/acscatal.8b01095
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C22 H17 I N2 O4 Pd'
_chemical_formula_sum            'C22 H17 I N2 O4 Pd'
_chemical_formula_weight         606.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 93.262(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   7.939(2)
_cell_length_b                   16.611(4)
_cell_length_c                   16.219(4)
_cell_measurement_reflns_used    5732
_cell_measurement_temperature    298
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.05
_cell_volume                     2135.4(9)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.000
_diffrn_reflns_Laue_measured_fraction_max 0.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16368
_diffrn_reflns_point_group_measured_fraction_full 0.000
_diffrn_reflns_point_group_measured_fraction_max 0.000
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.054
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.347
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            paleYellow
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1176.00
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.173
_refine_diff_density_max         1.21
_refine_diff_density_min         -0.93
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4880
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                4143
_reflns_number_total             4880
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            cs8b01095_si_002.cif
_cod_data_source_block           Compound_1e
_cod_original_cell_volume        2135.2(9)
_cod_database_code               4515704