Simple and easy functionalization of <i>para</i>-hydroxy POCOP-M (M = Ni(II), Pd(II)) pincer complexes: synthesis of multimetallic species.
Serrano-García, Juan S; García-Eleno, Marco Antonio; Arenaza-Corona, Antonino; Rufino-Felipe, Ernesto; Valdés, Hugo; Hernandez-Ortega, Simon; Morales-Morales, David; Dalton transactions (Cambridge, England : 2003) 54 (2025) 694–699; doi:10.1039/d4dt02841d

data_7717499
_publ_section_title
;
 Simple and easy functionalization of <i>para</i>-hydroxy POCOP-M (M =
 Ni(II), Pd(II)) pincer complexes: synthesis of multimetallic species.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              694
_journal_page_last               699
_journal_paper_doi               10.1039/d4dt02841d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C25 H38 Cl3 N3 O3 P2 Pd'
_chemical_formula_sum            'C25 H38 Cl3 N3 O3 P2 Pd'
_chemical_formula_weight         703.27
_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-2019/3
_audit_update_record
;
2024-08-27 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.542(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1646(10)
_cell_length_b                   28.713(4)
_cell_length_c                   13.7242(17)
_cell_measurement_reflns_used    3292
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.64
_cell_measurement_theta_min      2.60
_cell_volume                     3202.3(7)
_computing_cell_refinement       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_collection       'APEX2 v2012.10.0(Bruker, 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker, 2012)'
_computing_molecular_graphics    'SHELXLe (H\"ubschle et al, 2011)'
_computing_publication_material  'CIFTAB V 2013/2 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'Bruker Smart Apex CCD diffractometer 01-670-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.1110
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15756
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.569
_diffrn_reflns_theta_min         2.058
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       lamina
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.684
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5932
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0901P)^2^+0.5485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3407
_reflns_number_total             5932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02841d2.cif
_cod_data_source_block           Compoun_2-Pd
_cod_depositor_comments
'Adding full bibliography for 7717499--7717502.cif.'
_cod_original_cell_volume        3202.4(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717499
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              63863
_shelx_hkl_checksum              53522