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_7061439
_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 N P S Se'
_chemical_formula_sum            'C31 H26 N P S Se'
_chemical_formula_weight         554.52
_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             2022-01-04
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-04 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                62.093(5)
_cell_angle_beta                 74.683(4)
_cell_angle_gamma                87.704(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3859(4)
_cell_length_b                   12.4127(5)
_cell_length_c                   12.8167(6)
_cell_measurement_reflns_used    9700
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      72.5950
_cell_measurement_theta_min      4.0200
_cell_volume                     1266.55(12)
_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      101(2)
_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 0.979
_diffrn_measurement_details
;
 #__ type_ start__ end____ width___ exp.time_ 1 omega -27.00 48.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 36.8926 -57.0000 60.0000 75 #__ type_ start__ end____ width___ exp.time_ 2 omega 6.00 73.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 36.8926 -99.0000 150.0000 67 #__ type_ start__ end____ width___ exp.time_ 3 omega 58.00 89.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 36.8926 -125.0000 30.0000 31 #__ type_ start__ end____ width___ exp.time_ 4 omega 57.00 82.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 36.8926 -125.0000 -60.0000 25 #__ type_ start__ end____ width___ exp.time_ 5 omega 40.00 110.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 -95.0000 0.0000 70 #__ type_ start__ end____ width___ exp.time_ 6 omega 63.00 124.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 -61.0000 -30.0000 61 #__ type_ start__ end____ width___ exp.time_ 7 omega 41.00 107.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 -95.0000 -90.0000 66 #__ type_ start__ end____ width___ exp.time_ 8 omega 40.00 109.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 -95.0000 -180.0000 69 #__ type_ start__ end____ width___ exp.time_ 9 omega 41.00 97.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 -45.0000 -120.0000 56 #__ type_ start__ end____ width___ exp.time_ 10 omega 92.00 122.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 61.0000 -150.0000 30 #__ type_ start__ end____ width___ exp.time_ 11 omega 127.00 168.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 61.0000 -150.0000 41 #__ type_ start__ end____ width___ exp.time_ 12 omega 126.00 159.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 77.0000 -60.0000 33 #__ type_ start__ end____ width___ exp.time_ 13 omega 129.00 169.00 1.0000 1.4800 omega____ theta____ kappa____ phi______ frames - 108.0000 61.0
;
_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      0.1062777000
_diffrn_orient_matrix_UB_12      -0.0917149000
_diffrn_orient_matrix_UB_13      -0.0176692000
_diffrn_orient_matrix_UB_21      0.0557659000
_diffrn_orient_matrix_UB_22      -0.0148182000
_diffrn_orient_matrix_UB_23      0.1083469000
_diffrn_orient_matrix_UB_31      -0.1218100000
_diffrn_orient_matrix_UB_32      -0.1062304000
_diffrn_orient_matrix_UB_33      0.0894333000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18864
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.028
_diffrn_reflns_theta_min         4.050
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85079
_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            colorless
_exptl_crystal_colour_modifier   light
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       plate
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.575
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0955P)^2^+1.2594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1446
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4625
_reflns_number_total             4957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00924b2.cif
_cod_data_source_block           l-seph
_cod_depositor_comments
'Adding full bibliography for 7061439--7061443.cif.'
_cod_original_cell_volume        1266.55(11)
_cod_database_code               7061439
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O S Se P'
_shelx_estimated_absorpt_t_max   0.843
_shelx_estimated_absorpt_t_min   0.719
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a 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.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'