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_1565730
_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         'C21 H20 F I2 N3 Pd'
_chemical_formula_sum            'C21 H20 F I2 N3 Pd'
_chemical_formula_weight         693.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 93.977(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8346(3)
_cell_length_b                   9.3139(2)
_cell_length_c                   22.1383(7)
_cell_measurement_reflns_used    8605
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7583
_cell_measurement_theta_min      3.3501
_cell_volume                     2228.65(11)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23234
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.816
_diffrn_reflns_theta_min         3.355
_exptl_absorpt_coefficient_mu    3.623
_exptl_absorpt_correction_T_max  0.5167
_exptl_absorpt_correction_T_min  0.3811
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.780
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.827
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         7513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.827
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0248P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4726
_reflns_number_total             7513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119090.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565730
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.381
_shelx_estimated_absorpt_t_max   0.517