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_7717243
_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 Ni O P2, 2(C2 H4 Cl2)'
_chemical_formula_sum            'C42 H38 Cl5 N Ni O P2'
_chemical_formula_weight         870.63
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                76.582(2)
_cell_angle_beta                 77.268(2)
_cell_angle_gamma                62.127(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6703(4)
_cell_length_b                   12.9622(4)
_cell_length_c                   13.9961(3)
_cell_measurement_reflns_used    13837
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.9050
_cell_measurement_theta_min      1.8270
_cell_volume                     1959.70(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  20.08   0.50    2.00  15.81  -9.84 -59.25    --   720
  2  \w    -65.46   0.04   0.50    2.00    --  -19.34  94.56 145.16  131
  3  \w    -60.89   0.11   0.50    2.00    --  -14.77  94.56 -34.84  122
  4  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25 164.08  233
  5  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25  20.08  233
  6  \w    -65.46   0.04   0.50    2.00    --  -19.34  94.56   1.16  131
  7  \f   -349.73  10.27   0.50    2.00   6.61  -9.84 -31.50    --   720
  8  \w    -65.46   0.04   0.50    2.00    --  -19.34  94.56  73.16  131
  9  \w   -100.81  15.69   0.50    2.00    --   -9.84 -59.25 -51.92  233
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0172878000
_diffrn_orient_matrix_UB_12      -0.0612668000
_diffrn_orient_matrix_UB_13      0.0043718000
_diffrn_orient_matrix_UB_21      -0.0539212000
_diffrn_orient_matrix_UB_22      0.0069598000
_diffrn_orient_matrix_UB_23      0.0321534000
_diffrn_orient_matrix_UB_31      -0.0295506000
_diffrn_orient_matrix_UB_32      0.0108439000
_diffrn_orient_matrix_UB_33      -0.0413313000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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            73706
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.797
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.56
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0489P)^2^+1.7102P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1129
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5752
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02611j2.cif
_cod_data_source_block           Complex_2
_cod_depositor_comments
'Adding full bibliography for 7717241--7717247.cif.'
_cod_database_code               7717243
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.471
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C40(H40A,H40B), C39(H39A,H39B), C41(H41A,H41B), C42(H42A,H42B)
1.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C13(H13), C4(H4), C34(H34), C28(H28), C32(H32), C15(H15),
 C5(H5), C19(H19), C24(H24), C25(H25), C29(H29), C18(H18), C22(H22), C23(H23),
 C38(H38), C17(H17), C12(H12), C30(H30), C35(H35), C16(H16), C31(H31), C11(H11),
  C9(H9), C36(H36), C10(H10), C37(H37)
;
_shelx_res_checksum              43097
_shelx_hkl_checksum              7926
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.214
_oxdiff_exptl_absorpt_empirical_full_min 0.763