Crystal structures of six complexes of phosphane chalcogenides <i>R</i> <sup>1</sup> <i>R</i> <sup>2</sup> <i>R</i> <sup>3</sup>P<i>E</i> (<i>R</i> = <i>tert</i>-butyl or isopropyl, <i>E</i> = S or Se) with the metal halides <i>MX</i> <sub>2</sub> (<i>M</i> = Pd or Pt, <i>X</i> = Cl or Br), two halochalcogenyl-phospho-nium derivatives ( <sup><i>t</i></sup> Bu<sub>2</sub> <sup>i</sup>PrP<i>E</i>Br)<sub>2</sub>[Pd<sub>2</sub>Br<sub>6</sub>] and one hydrolysis product.
Upmann, Daniel; Jones, Peter G.; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 183–194; doi:10.1107/S2056989025000805

data_2023375
_publ_section_title
;
 Crystal structures of six complexes of phosphane chalcogenides <i>R</i>
 <sup>1</sup> <i>R</i> <sup>2</sup> <i>R</i> <sup>3</sup>P<i>E</i>
 (<i>R</i> = <i>tert</i>-butyl or isopropyl, <i>E</i> = S or Se) with the
 metal halides <i>MX</i> <sub>2</sub> (<i>M</i> = Pd or Pt, <i>X</i> = Cl
 or Br), two halochalcogenyl-phospho-nium derivatives (
 <sup><i>t</i></sup> Bu<sub>2</sub>
 <sup>i</sup>PrP<i>E</i>Br)<sub>2</sub>[Pd<sub>2</sub>Br<sub>6</sub>] and
 one hydrolysis product.
;
_journal_coeditor_code           YZ2063
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              183
_journal_page_last               194
_journal_paper_doi               10.1107/S2056989025000805
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '[Pd Br2 (C11 H25 P1 S1)2]'
_chemical_formula_moiety         'C22 H50 Br2 P2 Pd S2'
_chemical_formula_sum            'C22 H50 Br2 P2 Pd S2'
_chemical_formula_weight         706.90
_chemical_name_systematic
;
Dibromido(di-<i>tert</i>-butylisopropylphosphine
sulfide-\k<i>S</i>)palladium(II)
;
_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           SHELXL2019/3
_cell_angle_alpha                90
_cell_angle_beta                 94.551(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8595(3)
_cell_length_b                   17.5019(6)
_cell_length_c                   10.6740(3)
_cell_measurement_reflns_used    9329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7809
_cell_measurement_theta_min      2.2355
_cell_volume                     1463.65(9)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_computing_data_reduction
;
CrysAlisPro, Version 1.171.35.21 (Rigaku OD, 2012)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45160
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.850
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2012)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.023
_refine_diff_density_min         -0.700
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.219
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0106P)^2^+2.7056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                3832
_reflns_number_total             4422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yz2063.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 2023372--2023380.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2023375
_shelx_estimated_absorpt_t_min   0.531
_shelx_estimated_absorpt_t_max   0.840
_shelx_hkl_checksum              55445
_shelx_res_checksum              72643