Ni<sup>II</sup>, Pd<sup>II</sup> and Pt<sup>II</sup> pincer complexes of 2-(diphenylphosphanyl)-<i>N</i>-(2-(diphenyl-phosphanyl)benzyl)benzamide: synthesis, reactivity and catalytic studies.
Dwivedi, Khilesh C.; Sabharwal, Gazal; Kote, Basvaraj S.; Balakrishna, Maravanji S.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18321–18329; doi:10.1039/d4dt02611j

data_7717247
_publ_section_title
;
 Ni<sup>II</sup>, Pd<sup>II</sup> and Pt<sup>II</sup> pincer complexes of
 2-(diphenylphosphanyl)-<i>N</i>-(2-(diphenyl-phosphanyl)benzyl)benzamide:
 synthesis, reactivity and catalytic studies.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18321
_journal_page_last               18329
_journal_paper_doi               10.1039/d4dt02611j
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C38 H30 Cl N O P2 Pd, C H2 Cl2'
_chemical_formula_sum            'C40 H34 Cl5 N O P2 Pd'
_chemical_formula_weight         890.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-04-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                77.550(2)
_cell_angle_beta                 76.927(2)
_cell_angle_gamma                60.683(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6618(7)
_cell_length_b                   12.8044(7)
_cell_length_c                   13.8971(7)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.92
_cell_measurement_theta_min      2.23
_cell_volume                     1898.98(18)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            69406
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.917
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0741 after correction.
The Ratio of minimum to maximum transmission is 0.8039.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0283
_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^)+(0.0288P)^2^+2.1125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5893
_reflns_number_total             6677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02611j2.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
'Adding full bibliography for 7717241--7717247.cif.'
_cod_database_code               7717247
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C6(H6), C5(H5), C4(H4), C3(H3),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 76 electrons were 
found in a volume of 190\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_shelx_res_checksum              98669
_shelx_hkl_checksum              96909
_shelx_fab_checksum              33788
_olex2_submission_special_instructions 'No special instructions were received'