A comparison between (a/n-NHC)PdX2(pyridine) and (a/n-NHC)2PdX2 (X = I, Cl) type complexes of abnormal fused-bicyclic imidazo[1,2-a]pyridine based N-heterocyclic carbene (a-NHC) and of normal imidazole based N-heterocyclic carbene (n-NHC) ligands in the Suzuki-Miyaura coupling reactions
Modak, Sudipta; Borah, Suchibrata; Prakasham, A.P.; Shaikh, Mobin M.; Butcher, Raymond J.; Gangwar, Manoj; Ghosh, Prasenjit; Inorganica Chimica Acta 498 (2019) 119090–; doi:10.1016/j.ica.2019.119090

data_1565729
_publ_section_title
;
 A comparison between (a/n-NHC)PdX2(pyridine) and (a/n-NHC)2PdX2
 (X&#x202F;=&#x202F;I, Cl) type complexes of abnormal fused-bicyclic
 imidazo[1,2-a]pyridine based N-heterocyclic carbene (a-NHC) and of normal
 imidazole based N-heterocyclic carbene (n-NHC) ligands in the
 Suzuki-Miyaura coupling reactions
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119090
_journal_paper_doi               10.1016/j.ica.2019.119090
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety
;
C35 H37 Cl3 I2 N4 Pd, C34 H36 I2 N4 Pd, 7(C H Cl3)
;
_chemical_formula_sum            'C38 H40 Cl12 I2 N4 Pd'
_chemical_formula_weight         1338.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                76.924(2)
_cell_angle_beta                 89.1810(10)
_cell_angle_gamma                86.8620(10)
_cell_formula_units_Z            4
_cell_length_a                   11.5941(2)
_cell_length_b                   20.2789(4)
_cell_length_c                   22.1269(4)
_cell_measurement_reflns_used    42598
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1600
_cell_measurement_theta_min      2.0300
_cell_volume                     5059.88(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'Rigaku Saturn 724 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.896
_diffrn_reflns_Laue_measured_fraction_max 0.796
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            91494
_diffrn_reflns_point_group_measured_fraction_full 0.896
_diffrn_reflns_point_group_measured_fraction_max 0.796
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.213
_diffrn_reflns_theta_min         1.759
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.240
_refine_diff_density_max         4.448
_refine_diff_density_min         -2.805
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         26180
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0539P)^2^+59.5841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1688
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20146
_reflns_number_total             26180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119090.cif
_cod_data_source_block           2
_cod_database_code               1565729
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.614