Palladium(ii)-complexes of bi- and tri-dentate phosphine ligands: precursor for palladium–phosphorous nanoparticles and activity towards Suzuki–Miyaura coupling
Rao, Gyandshwar Kumar; Dutta, Anirban; Yadav, Nisha; Oswal, Preeti; Kumar, Arun; Singh, Ajai K.; New Journal of Chemistry 47 (2023) 4218–4227; doi:10.1039/D2NJ05357H

data_7062188
_publ_section_title
;
 Palladium(ii)-complexes of bi- and tri-dentate phosphine ligands:
 precursor for palladium--phosphorous nanoparticles and activity towards
 Suzuki--Miyaura coupling
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4218
_journal_page_last               4227
_journal_paper_doi               10.1039/D2NJ05357H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C28 H25 Cl N O P Pd'
_chemical_formula_sum            'C28 H25 Cl N O P Pd'
_chemical_formula_weight         564.36
_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_Int_Tables_number      14
_audit_creation_date             2022-11-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-08 deposited with the CCDC.	2022-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.878(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.606(3)
_cell_length_b                   8.4228(19)
_cell_length_c                   22.777(5)
_cell_measurement_reflns_used    1758
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.91
_cell_volume                     2401.0(9)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9976
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.1113
_diffrn_reflns_Laue_measured_fraction_full 0.9976
_diffrn_reflns_Laue_measured_fraction_max 0.9976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14940
_diffrn_reflns_point_group_measured_fraction_full 0.9976
_diffrn_reflns_point_group_measured_fraction_max 0.9976
_diffrn_reflns_theta_full        24.9992
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1141.567
_refine_diff_density_max         1.2679
_refine_diff_density_min         -1.0694
_refine_diff_density_rms         0.1780
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.5517
_refine_ls_goodness_of_fit_ref   0.9431
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    47
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9431
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.0006
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -14
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -11
_reflns_number_gt                3275
_reflns_number_total             4196
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj05357h2.cif
_cod_data_source_block           anirbanm_CCDC1
_cod_depositor_comments
;
Adding full bibliography for 7062187--7062188.cif.

2025-03-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum
'C6.588 H5.882 Cl0.235 N0.235 O0.235 P0.235 Pd0.235'
_cod_original_formula_weight         132.790
_cod_original_formula_moiety         '0.235(C28 H25 Cl N O P Pd)'
_cod_original_formula_units_Z            17
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7062188
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b)
1.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C25(H25), C28(H28), C22(H22), C26(H26), C4(H4), C27(H27), C1(H1),
 C5(H5), C8(H8), C18(H18), C9(H9), C10(H10), C19(H19), C20(H20), C11(H11),
 C3(H3), C21(H21), C2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'