Synthesis of ferrocenyl imidazolium salts and their novel PEPPSI-type N-heterocyclic carbene (NHC) palladium complexes
Yenisarı, Betül; Fırıncı, Rukiye; Özdemir, Namık; Günay, M. Emin; Inorganica Chimica Acta 511 (2020) 119792–; doi:10.1016/j.ica.2020.119792

data_1564161
_publ_section_title
;
 Synthesis of ferrocenyl imidazolium salts and their novel PEPPSI-type
 N-heterocyclic carbene (NHC) palladium complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119792
_journal_paper_doi               10.1016/j.ica.2020.119792
_journal_volume                  511
_journal_year                    2020
_chemical_formula_moiety         'C36 H40 Cl2 Fe N4 Pd'
_chemical_formula_sum            'C36 H40 Cl2 Fe N4 Pd'
_chemical_formula_weight         761.87
_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
_cell_angle_alpha                90
_cell_angle_beta                 100.266(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6604(11)
_cell_length_b                   8.7608(3)
_cell_length_c                   20.8479(11)
_cell_measurement_reflns_used    13406
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      1.57
_cell_volume                     3533.4(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 2012)'
_computing_publication_material
'WinGX (Farrugia, 2012) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.8 mm diameter, multiple pinhole'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1278
_diffrn_reflns_av_unetI/netI     0.1572
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22832
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.247
_diffrn_reflns_theta_min         1.985
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.6943
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED32 (Stoe & Cie, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.526
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6408
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0132P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0825
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2564
_reflns_number_total             6408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-511-119792.cif
_cod_data_source_block           namikoz31
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1564161
_shelx_estimated_absorpt_t_min   0.595
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              67790
_shelx_hkl_checksum              7866