Pd and Pt Catalyst Poisoning in the Study of Reaction Mechanisms: What Does the Mercury Test Mean for Catalysis?
Chernyshev, Victor M.; Astakhov, Alexander V.; Chikunov, Ilya E.; Tyurin, Roman V.; Eremin, Dmitry B.; Ranny, Gleb S.; Khrustalev, Victor N.; Ananikov, Valentine P.; ACS Catalysis 9 (2019) 2984–; doi:10.1021/acscatal.8b03683

data_4514730
_publ_section_title
;
 Pd and Pt Catalyst Poisoning in the Study of Reaction Mechanisms: What
 Does the Mercury Test Mean for Catalysis?
;
_journal_issue                   4
_journal_name_full               'ACS Catalysis'
_journal_page_first              2984
_journal_paper_doi               10.1021/acscatal.8b03683
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C18 H20 I2 N4 Pd'
_chemical_formula_sum            'C18 H20 I2 N4 Pd'
_chemical_formula_weight         652.58
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 99.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.3065(17)
_cell_length_b                   16.337(3)
_cell_length_c                   7.6187(15)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.8
_cell_volume                     1020.8(4)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.1164
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9763
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.410
_diffrn_reflns_theta_min         3.794
_exptl_absorpt_coefficient_mu    8.980
_exptl_absorpt_correction_T_max  0.400
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.123
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.595
_refine_diff_density_rms         0.280
_refine_ls_extinction_coef       0.0026(2)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1278
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1643
_reflns_number_total             2055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03683_si_002.cif
_cod_data_source_block           TR056
_cod_database_code               4514730
_shelx_estimated_absorpt_t_min   0.395
_shelx_estimated_absorpt_t_max   0.450
_shelxl_version_number           2014/6
_shelx_res_checksum              28243
_shelx_hkl_checksum              76912