Sterically enriched bulky 1,3-bis(N,N′-aralkyl)benzimidazolium based Pd-PEPPSI complexes for Buchwald‒Hartwig amination reactions
Reddy, Motakatla Venkata Krishna; Anusha, Gokanapalli; Reddy, Peddiahgari Vasu Govardhana; New Journal of Chemistry 44 (2020) 11694–11703; doi:10.1039/D0NJ01294G

data_7059699
_publ_section_title
;
 Sterically enriched bulky 1,3-bis(N,N&#x2032;-aralkyl)benzimidazolium
 based Pd-PEPPSI complexes for Buchwald--Hartwig amination reactions
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11694
_journal_page_last               11703
_journal_paper_doi               10.1039/D0NJ01294G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C46 H62 Cl3 N3 Pd'
_chemical_formula_sum            'C46 H62 Cl3 N3 Pd'
_chemical_formula_weight         869.73
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-06 deposited with the CCDC.	2020-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.116(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9613(9)
_cell_length_b                   9.3523(4)
_cell_length_c                   26.6508(12)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.38
_cell_measurement_theta_min      2.31
_cell_volume                     4725.1(4)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       '\w and \f scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0764
_diffrn_reflns_av_unetI/netI     0.0498
_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       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            60323
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.149
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.594
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00137(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         8307
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+9.1169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5460
_reflns_number_total             8307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj01294g2.cif
_cod_data_source_block           32902
_cod_depositor_comments
;Adding full bibliography for 7059699.cif.

 Adding full bibliography for 7059699.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7059699
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.916
_shelx_res_checksum              96316