{α,α′-Bis[(tert-butyl)(6-methoxypyridin-2-yl)phosphino]-o-xylene}(η2-N-methylmaleinimide)palladium(0) toluene hemisolvate
Müller, Stefan; Spannenberg, Anke; Neumann, Helfried; Franke, Robert; Beller, Matthias; IUCrData 10 (2025) x250508–; doi:10.1107/S2414314625005085

data_1574928
_publ_section_title
;
 {\a,\a&#x2032;-Bis[(tert-butyl)(6-methoxypyridin-2-yl)phosphino]-o-xylene}(\h2-N-methylmaleinimide)palladium(0)
 toluene hemisolvate
;
_journal_coeditor_code           HB4516
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x250508
_journal_paper_doi               10.1107/S2414314625005085
_journal_volume                  10
_journal_year                    2025
_chemical_formula_iupac
'[Pd (C5 H5 N O2) (C28 H38 N2 O2 P2)], 0.5C7 H8'
_chemical_formula_moiety         '(C33 H43 N3 O4 P2 Pd), 0.5(C7 H8)'
_chemical_formula_sum            'C36.5 H47 N3 O4 P2 Pd'
_chemical_formula_weight         760.11
_chemical_name_systematic
'(\a,\a'-Bis[(<i>tert</i>-butyl)(6-methoxypyridin-2-yl)phosphino]-<i>o</i>-xylene}(\h^2^-<i>N</i>-methylmaleinimide)palladium(0) toluene hemisolvate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/1
_cell_angle_alpha                74.0508(10)
_cell_angle_beta                 86.9998(10)
_cell_angle_gamma                76.0888(9)
_cell_formula_units_Z            2
_cell_length_a                   9.5548(2)
_cell_length_b                   10.7020(3)
_cell_length_c                   18.4654(5)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      2.49
_cell_volume                     1762.06(8)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2019/1</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         microfocus
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27460
_diffrn_reflns_theta_full        66.675
_diffrn_reflns_theta_max         66.675
_diffrn_reflns_theta_min         2.489
_exptl_absorpt_coefficient_mu    5.449
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       plate
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         6223
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0327P)^2^+0.6517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0568
_reflns_number_gt                5975
_reflns_number_total             6223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4516.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C36.50 H47 N3 O4 P2 Pd'
_cod_database_code               1574928
_shelx_hkl_checksum              35917
_shelx_res_checksum              74772