Crystal structure of a dicationic Pd^II^ dimer containing a 2-[(diisopropylphosphanyl)methyl]quinoline-8-thiolate pincer ligand
Clerc, Arnaud; Saffon-Merceron, Nathalie; Monot, Julien; Martin Vaca, Blanca; Bourissou, Didier; Acta Crystallographica Section E 78 (2022) 18–22; doi:10.1107/S2056989021012561

data_2243966
_publ_section_title
;
 Crystal structure of a dicationic Pd^II^ dimer containing a
 2-[(diisopropylphosphanyl)methyl]quinoline-8-thiolate pincer ligand
;
_journal_coeditor_code           ZQ2270
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              18
_journal_page_last               22
_journal_paper_doi               10.1107/S2056989021012561
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
'[Pd2 (C32 H42 N2 P2 S2)] (Sb F6)2 , C H2 Cl2'
_chemical_formula_moiety
'C32 H42 N2 P2 Pd2 S2 2+, 2(F6 Sb -), C H2 Cl2'
_chemical_formula_sum            'C33 H44 Cl2 F12 N2 P2 Pd2 S2 Sb2'
_chemical_formula_weight         1349.96
_chemical_name_systematic
;
Bis{2-[(diisopropylphosphanyl)methyl]quinoline-8-thiolato}palladium(II)
bis(hexafluoridoantimonate) dichloromethane monosolvate)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.5167(19)
_cell_length_b                   16.1492(14)
_cell_length_c                   24.0414(18)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.97
_cell_volume                     9130.3(13)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al</i>,
2020)
;
_computing_publication_material
;
PLATON (Spek, 2020) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD Quazar'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1223
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            152552
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.899
_diffrn_reflns_theta_min         1.903
_diffrn_source                   'Incoatec microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.301
_exptl_absorpt_correction_T_max  0.7283
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_description       plate
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         9812
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0384P)^2^+45.7164P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                6263
_reflns_number_total             9812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zq2270sup1.cif
_cod_data_source_block           I
_cod_database_code               2243966
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.914
_shelx_hkl_checksum              43003
_shelx_res_checksum              23459
_cod_database_fobs_code 2243966