Preventing Pd‒NHC bond cleavage and switching from nano-scale to molecular catalytic systems: amines and temperature as catalyst activators
Khazipov, Oleg V.; Shevchenko, Maxim A.; Pasyukov, Dmitry V.; Chernenko, Andrey Yu.; Astakhov, Alexander V.; Tafeenko, Victor A.; Chernyshev, Victor M.; Ananikov, Valentine P.; Catalysis Science & Technology 10 (2020) 1228–1247; doi:10.1039/C9CY02041A

data_1556928
_publ_section_title
;
 Preventing Pd--NHC bond cleavage and switching from nano-scale to
 molecular catalytic systems: amines and temperature as catalyst
 activators
;
_journal_issue                   5
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1228
_journal_page_last               1247
_journal_paper_doi               10.1039/C9CY02041A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C13 H21 I2 N3 Pd'
_chemical_formula_sum            'C13 H21 I2 N3 Pd'
_chemical_formula_weight         579.53
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-09-14 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.550(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5721(7)
_cell_length_b                   12.5994(8)
_cell_length_c                   8.4655(4)
_cell_measurement_reflns_used    2334
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      70.5
_cell_measurement_theta_min      4.5
_cell_volume                     1848.27(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295
_diffrn_detector                 Pilatus100K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  STOE
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  none
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.097
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_number            3573
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.259
_diffrn_reflns_theta_min         4.339
_diffrn_source                   'Cu GeniX 3D'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    34.259
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          .17
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .13
_refine_diff_density_max         0.955
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0626
_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^)+(0.1309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1764
_refine_ls_wR_factor_ref         0.1857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2389
_reflns_number_total             3573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cy02041a2.cif
_cod_data_source_block           p2c23016
_cod_depositor_comments
;Adding full bibliography for 1556927--1556930.cif.

 Adding full bibliography for 1556927--1556930.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556928
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              35257