Bimetallic PdII complexes with NHC/Py/PCy3 donor set ligands: applications in α-arylation, Suzuki–Miyaura and Sonogashira coupling reactions
Majumder, Adhir; Naskar, Rajat; Phukan, Shankab J.; Maity, Ramananda; New Journal of Chemistry 46 (2022) 13075–13081; doi:10.1039/D2NJ01852G

data_7061592
_publ_section_title
;
 Bimetallic PdII complexes with NHC/Py/PCy3 donor set ligands:
 applications in \a-arylation, Suzuki--Miyaura and Sonogashira coupling
 reactions
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13075
_journal_page_last               13081
_journal_paper_doi               10.1039/D2NJ01852G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C28 H32 I4 N6 O2 Pd2'
_chemical_formula_sum            'C28 H32 I4 N6 O2 Pd2'
_chemical_formula_weight         1204.99
_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     dual
_audit_creation_date             2022-01-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-02 deposited with the CCDC.	2022-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.035(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3535(8)
_cell_length_b                   23.046(2)
_cell_length_c                   17.3965(15)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    113.0
_cell_measurement_theta_max      63.63
_cell_measurement_theta_min      3.23
_cell_volume                     3667.6(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'SAINT V8.40B (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50498
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        63.917
_diffrn_reflns_theta_max         63.917
_diffrn_reflns_theta_min         3.229
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    34.615
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.2686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1649 before and 0.1206 after correction. The Ratio of minimum to maximum transmission is 0.3570. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_description       needle
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.618
_refine_diff_density_min         -1.987
_refine_diff_density_rms         0.283
_refine_ls_extinction_coef       0.00028(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0826P)^2^+40.1621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5373
_reflns_number_total             6015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01852g2.cif
_cod_data_source_block           rmadam_pd_0m
_cod_depositor_comments          'Adding full bibliography for 7061592.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7061592
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.103
_shelx_estimated_absorpt_t_min   0.025
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C25(H25), C22(H22), C6(H6), C5(H5), C18(H18), C17(H17), C23(H23),
 C13(H13), C12(H12), C21(H21), C3(H3), C2(H2), C20(H20)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C16(H16A,H16B,
 H16C), C11(H11A,H11B,H11C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              64408
_olex2_submission_special_instructions 'No special instructions were received'