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_7061441
_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         'C26 H24 Cl N P Pd S Se, C H2 Cl2, B F4'
_chemical_formula_sum            'C27 H26 B Cl3 F4 N P Pd S Se'
_chemical_formula_weight         806.04
_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   geom
_audit_creation_date             2022-03-31
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-04-01 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                65.113(5)
_cell_angle_beta                 72.940(4)
_cell_angle_gamma                74.721(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3865(5)
_cell_length_b                   12.8750(7)
_cell_length_c                   12.9927(7)
_cell_measurement_reflns_used    4992
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      28.8900
_cell_measurement_theta_min      3.2980
_cell_volume                     1486.99(15)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(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 0.845
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega -50.00 45.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 -19.0000 -30.0000 95 #__ type_ start__ end____ width___ exp.time_ 2 omega 10.00 44.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 -99.0000 60.0000 34 #__ type_ start__ end____ width___ exp.time_ 3 omega 19.00 54.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 -99.0000 30.0000 35 #__ type_ start__ end____ width___ exp.time_ 4 omega -51.00 -13.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 -77.0000 150.0000 38 #__ type_ start__ end____ width___ exp.time_ 5 omega -1.00 28.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 57.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 6 omega 6.00 83.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 77.0000 -90.0000 77 #__ type_ start__ end____ width___ exp.time_ 7 omega -11.00 66.00 1.0000 28.4000 omega____ theta____ kappa____ phi______ frames - 15.2374 77.0000 -180.0000 77'
_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      0.0089447000
_diffrn_orient_matrix_UB_12      -0.0532107000
_diffrn_orient_matrix_UB_13      -0.0073172000
_diffrn_orient_matrix_UB_21      0.0706516000
_diffrn_orient_matrix_UB_22      0.0022074000
_diffrn_orient_matrix_UB_23      -0.0226246000
_diffrn_orient_matrix_UB_31      0.0129526000
_diffrn_orient_matrix_UB_32      -0.0308348000
_diffrn_orient_matrix_UB_33      0.0567535000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12602
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.213
_diffrn_reflns_theta_min         2.928
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60092
_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.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_description       block
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6826
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0425
_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^)+(0.0253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5427
_reflns_number_total             6826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00924b2.cif
_cod_data_source_block           pdbf4seme
_cod_depositor_comments
'Adding full bibliography for 7061439--7061443.cif.'
_cod_database_code               7061441
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.658
_shelx_estimated_absorpt_t_min   0.547
_reflns_odcompleteness_completeness 99.87
_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. Restrained distances
 C27A-Cl2A = C27A-Cl3A = C27B-Cl2B = C27B-Cl3B
 1.75 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2A \\sim Cl3A \\sim C27A \\sim Cl2B \\sim Cl3B \\sim C27B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 F1A, F2A, F3A, F4A, B1A, F1B, F2B, F3B, F4B, B1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{F1B, F2B, F3B, F4B, B1B} sigma for 1-2: 0.01, 1-3: 0.04
as
{F1A, F2A, F3A, F4A, B1A}
6. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(B1B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=FVAR(1)
 Sof(Cl2B)=Sof(Cl3B)=Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(2)
 Sof(Cl2A)=Sof(Cl3A)=Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(2)
7.a Secondary CH2 refined with riding coordinates:
 C27A(H27A,H27B), C27B(H27C,H27D)
7.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), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26)
7.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              89278
_olex2_submission_special_instructions 'No special instructions were received'