Palladium complexes with an annellated mesoionic carbene (MIC) ligand: catalytic sequential Sonogashira coupling/cyclization reaction for one-pot synthesis of benzofuran, indole, isocoumarin and isoquinolone derivatives.
Tyagi, Akshi; Reshi, Noor U Din; Daw, Prosenjit; Bera, Jitendra K.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15238–15248; doi:10.1039/d0dt02918a

data_7705604
_publ_section_title
;
 Palladium complexes with an annellated mesoionic carbene (MIC) ligand:
 catalytic sequential Sonogashira coupling/cyclization reaction for
 one-pot synthesis of benzofuran, indole, isocoumarin and isoquinolone
 derivatives.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15238
_journal_page_last               15248
_journal_paper_doi               10.1039/d0dt02918a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'C53 H43 I2 N3 P2 Pd'
_chemical_formula_weight         1144.04
_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-2017/1
_audit_update_record
;
2020-07-06 deposited with the CCDC.	2020-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.5670(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   16.9889(14)
_cell_measurement_reflns_used    9515
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.46
_cell_volume                     4806.5(7)
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.977
_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  0.0930
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30117
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.402
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.776
_exptl_absorpt_correction_T_max  0.665
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       needle
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         11790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1455
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0587P)^2^+2.4075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6510
_reflns_number_total             11790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02918a2.cif
_cod_data_source_block           Pd1
_cod_depositor_comments
'Adding full bibliography for 7705604--7705605.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7705604
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.655
_shelx_estimated_absorpt_t_max   0.686
_exptl_absorpt_special_details   SADABS
_shelx_res_checksum              18759