Trinuclear complexes of palladium(II) with chalcogenated N-heterocyclic carbenes: catalysis of selective nitrile-primary amide interconversion and Sonogashira coupling
Singh, Ajai kumar; Dubey, Pooja; Gupta, Sonu; Dalton Trans.  (2017) –; doi:10.1039/C7DT02592K

data_7044141
_publ_section_title
;
 Trinuclear complexes of palladium(II) with chalcogenated N-heterocyclic
 carbenes: catalysis of selective nitrile-primary amide interconversion
 and Sonogashira coupling
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02592K
_journal_year                    2017
_chemical_formula_moiety         'C36 H38 Cl6 N6 Pd3 Se2, 4(C2 H3 N)'
_chemical_formula_sum            'C44 H50 Cl6 N10 Pd3 Se2'
_chemical_formula_weight         1408.76
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc1pppy0
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-08-19 deposited with the CCDC.
2017-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                67.79(2)
_cell_angle_beta                 81.88(3)
_cell_angle_gamma                82.02(2)
_cell_formula_units_Z            1
_cell_length_a                   8.380(2)
_cell_length_b                   11.721(3)
_cell_length_c                   14.883(4)
_cell_measurement_reflns_used    3764
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.47
_cell_volume                     1334.0(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      298(2)
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1111
_diffrn_reflns_av_unetI/netI     0.0950
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12922
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.979
_diffrn_reflns_theta_max         24.979
_diffrn_reflns_theta_min         1.485
_exptl_absorpt_coefficient_mu    2.706
_exptl_absorpt_correction_T_max  0.495
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2016/6)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_density_meas      1.754
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4632
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.911
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0159P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0764
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3693
_reflns_number_total             4672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02592k2.cif
_cod_data_source_block           complex2
_cod_database_code               7044141
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.469
_shelx_estimated_absorpt_t_max   0.529
_shelx_res_checksum              24370