Naphthyl and biphenyl para-substituted POCOP-Ni(ii) pincer complexes as efficient catalysts in C–S cross-coupling reactions
López-Robledo, Luis E.; Ortiz-Fuentes, Evelin E.; Rufino-Felipe, Ernesto; Serrano-García, Juan S.; Arenaza-Corona, Antonino; Hernandez-Ortega, Simón; Valdés, Hugo; Gonzalez-Sebastian, Lucero; Reyes-Márquez, Viviana; Morales-Morales, David; New Journal of Chemistry 49 (2025) 3426–3435; doi:10.1039/D4NJ03776F

data_7063512
_publ_section_title
;
 Naphthyl and biphenyl para-substituted POCOP-Ni(ii) pincer complexes as
 efficient catalysts in C--S cross-coupling reactions
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3426
_journal_page_last               3435
_journal_paper_doi               10.1039/D4NJ03776F
_journal_volume                  49
_journal_year                    2025
_chemical_formula_sum            'C73 H98 Cl2 Ni2 O8 P4'
_chemical_formula_weight         1415.71
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-02-14 deposited with the CCDC.	2024-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.7660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0438(2)
_cell_length_b                   28.5592(10)
_cell_length_c                   16.4261(5)
_cell_measurement_reflns_used    9750
_cell_measurement_temperature    199(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      2.49
_cell_volume                     3680.20(19)
_computing_cell_refinement       'APEX3 v2018.2 (Bruker, 2018)'
_computing_data_collection       'APEX3 v2018.2 (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.37A  (Bruker, 2018)'
_computing_molecular_graphics
'Ortep-3 Ver 2.02 L.J. Farrugia (1997) J. Appl. Cryst. 30, 565'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2018 (Bruker, 2015)'
_diffrn_ambient_temperature      199(2)
_diffrn_detector_area_resol_mean 52.0833
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker D8 Venture \k-geometry diffractometer 208039-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45956
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.401
_diffrn_reflns_theta_min         2.489
_diffrn_source                   'micro-focus X-ray source'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         6769
_refine_ls_number_restraints     235
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+4.9014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4955
_reflns_number_total             6769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03776f2.cif
_cod_data_source_block           compound2b
_cod_depositor_comments
'Adding full bibliography for 7063510--7063512.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7063512
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.757
_shelx_estimated_absorpt_t_max   0.929
_exptl_absorpt_special_details
; 
 The following wavelength and cell were deduced by SADABS from the 
 direction cosines etc. They are given here for emergency use only: 
 CELL 0.71104    8.051   28.568   16.440   90.029  102.748   89.983 
;
_shelx_res_checksum              62205
_shelx_hkl_checksum              29607