Experimental and theoretical insights into the trans influence of organo-sulfur and -selenium ligands in 5,6-membered palladium(ii) cationic pincer complexes based on iminophosphoranes
Rodríguez-Álvarez, Aurora; González-Espinoza, Cristina E.; Martínez-De-León, Carla Gabriela; Carrillo-Tripp, Mauricio; Hô, Minhhuy; Grévy, Jean-Michel; New Journal of Chemistry 46 (2022) 9344–9356; doi:10.1039/D2NJ00924B

data_7061443
_publ_section_title
;
 Experimental and theoretical insights into the trans influence of
 organo-sulfur and -selenium ligands in 5,6-membered palladium(ii)
 cationic pincer complexes based on iminophosphoranes
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9344
_journal_page_last               9356
_journal_paper_doi               10.1039/D2NJ00924B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C31 H26 Cl N P Pd S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C32 H30 B Cl3 F4 N O P Pd S2'
_chemical_formula_weight         839.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-01-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-05 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.705(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5136(7)
_cell_length_b                   15.1765(5)
_cell_length_c                   19.8095(6)
_cell_measurement_reflns_used    13590
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      28.7650
_cell_measurement_theta_min      3.1500
_cell_volume                     6760.9(4)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 4.00 82.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - 15.2374 57.0000 0.0000 78 #__ type_ start__ end____ width___ exp.time_ 2 omega -10.00 82.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - 15.2374 77.0000 90.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -35.00 50.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - -16.1749 19.0000 -90.0000 85 #__ type_ start__ end____ width___ exp.time_ 4 omega -14.00 52.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - 15.2374 -99.0000 -180.0000 66 #__ type_ start__ end____ width___ exp.time_ 5 omega -52.00 2.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - 15.2374 -57.0000 -60.0000 54 #__ type_ start__ end____ width___ exp.time_ 6 omega -74.00 -39.00 1.0000 11.3300 omega____ theta____ kappa____ phi______ frames - -16.1749 132.0000 161.0000 35'
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0187337000
_diffrn_orient_matrix_UB_12      -0.0059899000
_diffrn_orient_matrix_UB_13      0.0274036000
_diffrn_orient_matrix_UB_21      0.0253425000
_diffrn_orient_matrix_UB_22      -0.0032375000
_diffrn_orient_matrix_UB_23      0.0225444000
_diffrn_orient_matrix_UB_31      -0.0006769000
_diffrn_orient_matrix_UB_32      0.0462573000
_diffrn_orient_matrix_UB_33      0.0051403000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29675
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.157
_diffrn_reflns_theta_min         2.585
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.008
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.883
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         8127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0341P)^2^+15.7707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6926
_reflns_number_total             8127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00924b2.cif
_cod_data_source_block           pdbf4-sph
_cod_depositor_comments
'Adding full bibliography for 7061439--7061443.cif.'
_cod_original_cell_volume        6760.9(3)
_cod_database_code               7061443
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N P S Pd Cl F B'
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.726
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'