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_4087194
_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         'C14 H15 I2 N3 Pd'
_chemical_formula_sum            'C14 H15 I2 N3 Pd'
_chemical_formula_weight         585.49
_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
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.98(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1410(16)
_cell_length_b                   12.504(3)
_cell_length_c                   17.364(4)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      2.8
_cell_volume                     1763.3(7)
_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)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.959
_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  0.0566
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       9
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_diffrn_reflns_limit_k_max       15
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_diffrn_reflns_limit_l_min       -22
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_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.959
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_diffrn_reflns_theta_max         38.309
_diffrn_reflns_theta_min         2.742
_exptl_absorpt_coefficient_mu    10.366
_exptl_absorpt_correction_T_max  0.345
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            yellow
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_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.12
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_refine_diff_density_min         -0.871
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       0.00015(2)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3699
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.036P)^2^+6.66P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0764
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3429
_reflns_number_total             3699
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00184_si_003.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 4087193--4087194.cif.'
_cod_database_code               4087194
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.251
_shelx_estimated_absorpt_t_max   0.355
_shelx_res_checksum              27229
_shelx_hkl_checksum              19239