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_2023374
_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 Se1)2]'
_chemical_formula_moiety         'C22 H50 Br2 P2 Pd Se2'
_chemical_formula_sum            'C22 H50 Br2 P2 Pd Se2'
_chemical_formula_weight         800.70
_chemical_name_systematic
;
Dibromido(di-<i>tert</i>-butylisopropylphosphine
selenide-\k<i>Se</i>)palladium(II)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 116.558(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3561(6)
_cell_length_b                   13.4695(4)
_cell_length_c                   16.1371(6)
_cell_measurement_reflns_used    11858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8204
_cell_measurement_theta_min      2.1134
_cell_volume                     2985.6(2)
_computing_cell_refinement
;
CrysAlisPro, Version 1.171.35.11 (Rigaku OD, 2012)
;
_computing_data_collection
;
CrysAlisPro, Version 1.171.35.11 (Rigaku OD, 2012)
;
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CrysAlisPro, Version 1.171.35.11 (Rigaku OD, 2012)
;
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;
Bruker XP, Version 5.1 (Bruker, 1998)
;
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;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2012)
;
_exptl_crystal_colour            'dichroic orange yellow'
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
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_refine_diff_density_min         -1.318
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         7402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0262P)^2^+9.8278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                5854
_reflns_number_total             7402
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2023372--2023380.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2023374
_shelx_estimated_absorpt_t_min   0.419
_shelx_estimated_absorpt_t_max   0.892
_shelx_hkl_checksum              8155
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