A New Mode of Operation of Pd-NHC Systems Studied in a Catalytic Mizoroki‒Heck Reaction
Astakhov, Alexander V.; Khazipov, Oleg V.; Chernenko, Andrey Yu.; Pasyukov, Dmitry V.; Kashin, Alexey S.; Gordeev, Evgeniy G.; Khrustalev, Victor N.; Chernyshev, Victor M.; Ananikov, Valentine P.; Organometallics 36 (2017) 1981–; doi:10.1021/acs.organomet.7b00184

data_4087193
_publ_section_title
;
 A New Mode of Operation of Pd-NHC Systems Studied in a Catalytic
 Mizoroki--Heck Reaction
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1981
_journal_paper_doi               10.1021/acs.organomet.7b00184
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C13 H19 Cl2 N3 Pd'
_chemical_formula_sum            'C13 H19 Cl2 N3 Pd'
_chemical_formula_weight         394.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.480(3)
_cell_length_b                   7.9200(16)
_cell_length_c                   29.400(6)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      4.4
_cell_volume                     3138.8(11)
_computing_cell_refinement       'iMosflm (Battye <i>et al.</i>, 2011)'
_computing_data_collection       'Automar (MarXperts, 2015)'
_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 0.978
_diffrn_measured_fraction_theta_max 0.941
_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  0.0701
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            45431
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.119
_diffrn_reflns_theta_min         4.181
_exptl_absorpt_coefficient_mu    3.498
_exptl_absorpt_correction_T_max  0.606
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.689
_refine_diff_density_min         -1.990
_refine_diff_density_rms         0.329
_refine_ls_extinction_coef       0.0051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0674
_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^)+(0.06P)^2^+18P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2825
_reflns_number_total             3182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00184_si_005.cif
_cod_data_source_block           5b
_cod_depositor_comments
'Adding full bibliography for 4087193--4087194.cif.'
_cod_database_code               4087193
_shelx_estimated_absorpt_t_min   0.456
_shelx_estimated_absorpt_t_max   0.605
_shelxl_version_number           2014/6
_shelx_res_checksum              87726
_shelx_hkl_checksum              63978