Synthesis, characterization and evaluation of bulky bis(pyrazolyl)palladium complexes in Suzuki‒Miyaura cross-coupling reactions
Ocansey, Edward; Darkwa, James; Makhubela, Banothile C. E.; RSC Advances 8 (2018) 13826–; doi:10.1039/C8RA01430B

data_7230470
_publ_section_title
;
 Synthesis, characterization and evaluation of bulky
 bis(pyrazolyl)palladium complexes in Suzuki--Miyaura cross-coupling
 reactions
;
_journal_issue                   25
_journal_name_full               'RSC Advances'
_journal_page_first              13826
_journal_paper_doi               10.1039/C8RA01430B
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C22 H18 Cl N2 Pd0.5'
_chemical_formula_sum            'C22 H18 Cl N2 Pd0.5'
_chemical_formula_weight         399.03
_chemical_name_systematic
'bis(2-benzyl-3,5-diphenyl-2,3-dihydro-1H-pyrazol-1-yl)palladium(IV) chloride'
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-06-13 deposited with the CCDC.
2018-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                102.123(2)
_cell_angle_beta                 98.442(2)
_cell_angle_gamma                94.970(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7767(6)
_cell_length_b                   10.2586(9)
_cell_length_c                   13.5319(13)
_cell_measurement_reflns_used    6135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.28
_cell_volume                     903.05(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12765
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         2.046
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0500 before and 0.0442 after correction.
The Ratio of minimum to maximum transmission is 0.9245.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0280P)^2^+0.4300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4175
_reflns_number_total             4497
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra01430b2.cif
_cod_data_source_block           eo18a
_cod_original_formula_sum        'C22 H18 Cl N2 Pd0.50'
_cod_database_code               7230470
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.785
_olex2_refinement_description
;
;
_shelx_res_checksum              62554
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'mounted on a MiTeGen DualThickness Micro-Mount, coated in a layer of Paratone oil'
_olex2_submission_original_sample_id EOI8A
_olex2_submission_special_instructions 'No special instructions were received'