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_7061442
_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 S Se, Cl3 Pd, C H Cl3'
_chemical_formula_sum            'C32 H27 Cl7 N P Pd2 S Se'
_chemical_formula_weight         1028.48
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-09
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-04-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.9613(6)
_cell_length_b                   15.9613(6)
_cell_length_c                   25.1755(10)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    99.9(3)
_cell_measurement_theta_max      28.1960
_cell_measurement_theta_min      2.9350
_cell_volume                     5554.5(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details
;      
 #__ type_ start__ end____ width___ exp.time_ 1 omega -51.00 78.00 1.0000 13.2250 omega____ theta____ kappa____ phi______ frames - 15.2374 0.0000 -150.0000 129 
 #__ type_ start__ end____ width___ exp.time_ 2 omega -66.00 2.00 1.0000 13.2250 omega____ theta____ kappa____ phi______ frames - -16.0187 -38.0000 150.0000 68 
 #__ type_ start__ end____ width___ exp.time_ 3 omega -33.00 9.00 1.0000 13.2250 omega____ theta____ kappa____ phi______ frames - -16.0187 57.0000 -60.0000 42
;
_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      0.0229262000
_diffrn_orient_matrix_UB_12      0.0070659000
_diffrn_orient_matrix_UB_13      -0.0251001000
_diffrn_orient_matrix_UB_21      0.0228620000
_diffrn_orient_matrix_UB_22      0.0507818000
_diffrn_orient_matrix_UB_23      0.0035693000
_diffrn_orient_matrix_UB_31      0.0398190000
_diffrn_orient_matrix_UB_32      -0.0001526000
_diffrn_orient_matrix_UB_33      0.0123553000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            28648
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.104
_diffrn_reflns_theta_min         2.677
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57897
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_description       block
_exptl_crystal_F_000             3012
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 2872 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         8831
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0279P)^2^+4.5882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                7587
_reflns_number_total             8831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00924b2.cif
_cod_data_source_block           pbseph
_cod_depositor_comments
'Adding full bibliography for 7061439--7061443.cif.'
_cod_original_cell_volume        5554.5(5)
_cod_database_code               7061442
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H S Se Cl B F P N Pd'
_shelx_estimated_absorpt_t_max   0.698
_shelx_estimated_absorpt_t_min   0.564
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C32A-Cl5A = C32A-Cl6A = C32A-Cl7A = C32-Cl5B = C32-Cl6B = C32-Cl7B
 1.75 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl5A \\sim Cl6A \\sim Cl7A \\sim C32A \\sim Cl5B \\sim Cl6B \\sim Cl7B \\sim
C32: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(Cl5B)=Sof(Cl6B)=Sof(Cl7B)=Sof(C32)=Sof(H32)=1-FVAR(1)
 Sof(Cl5A)=Sof(Cl6A)=Sof(Cl7A)=Sof(C32A)=Sof(H32A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C32A(H32A), C32(H32)
5.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)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'