Ferrocenyl palladacycles derived from unsymmetrical pincer-type ligands: Evidences of Pd(0) nanoparticles generation during Suzuki-Miyaura reaction and applications in direct arylation of thiazole and isoxazole
Maji, Ankur; Singh, Anshu; Mohanty, Aurobinda; Maji, Pradip K.; Ghosh, Kaushik; Dalton Transactions  (2019) –; doi:10.1039/C9DT03465J

data_7701387
_publ_section_title
;
 Ferrocenyl palladacycles derived from unsymmetrical pincer-type ligands:
 Evidences of Pd(0) nanoparticles generation during Suzuki-Miyaura
 reaction and applications in direct arylation of thiazole and isoxazole
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03465J
_journal_year                    2019
_chemical_formula_moiety         'C22 H18 Cl Fe N3 Pd'
_chemical_formula_sum            'C22 H18 Cl Fe N3 Pd'
_chemical_formula_weight         522.09
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-07-08 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.272(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4053(7)
_cell_length_b                   12.1239(8)
_cell_length_c                   15.8095(11)
_cell_measurement_reflns_used    111
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.43
_cell_volume                     1973.7(2)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'Apex2 (Bruker, 2013)'
_computing_data_reduction        'SAINT (Bruker, 2013)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5599
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.043
_diffrn_reflns_theta_min         2.125
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_description       squar
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0768P)^2^+3.3038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5110
_reflns_number_total             5599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03465j2.cif
_cod_data_source_block           am22tw
_cod_database_code               7701387
_shelx_shelxl_version_number     2018/3