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_7062187
_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         'C15 H17 Cl2 N P Pd'
_chemical_formula_sum            'C15 H17 Cl2 N P Pd'
_chemical_formula_weight         419.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                 107.457(5)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   34.786(10)
_cell_length_b                   12.983(4)
_cell_length_c                   17.594(5)
_cell_measurement_reflns_used    1758
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.26
_cell_measurement_theta_min      2.91
_cell_volume                     7580(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34521
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.684
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3344
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0557P)^2^+14.0716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5337
_reflns_number_total             6660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05357h2.cif
_cod_data_source_block           anirbanm
_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_weight         83.91
_cod_original_formula_moiety         '0.2(C15 H17 Cl2 N P Pd)'
_cod_original_formula_units_Z            80
_cod_original_formula_sum        'C3 H3.40 Cl0.40 N0.20 P0.20 Pd0.20'
_cod_database_code               7062187
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C16(H16A,H16B), C17(H17A,H17B), C1(H1C,H1D), C2(H2C,
 H2D)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C18(H18), C5(H5), C23(H23), C24(H24), C14(H14), C12(H12),
 C26(H26), C9(H9), C7(H7), C22(H22), C30(H30), C15(H15), C8(H8), C13(H13),
 C29(H29), C28(H28), C21(H21), C27(H27), C11(H11), C20(H20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3740
_shelx_fab_checksum              51062
_olex2_submission_special_instructions 'No special instructions were received'