All-Metal Aromatic Cationic Palladium Triangles Can Mimic Aromatic Donor Ligands towards Lewis Acidic Cations
Maestri, Giovanni; WANG, Yanlan; Monfredini, Anna; Deyris, Pierre-Alexandre; Derat, Etienne; Malacria, Max; Blanchard, Florent; Chem. Sci.  (2017) –; doi:10.1039/C7SC03475J

data_1546909
_publ_section_title
;
 All-Metal Aromatic Cationic Palladium Triangles Can Mimic Aromatic Donor
 Ligands towards Lewis Acidic Cations
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03475J
_journal_year                    2017
_chemical_formula_moiety         'C72 H48 Cl3 F9 P3 Pd3 S3, C F3 O3 S'
_chemical_formula_sum            'C73 H48 Cl3 F12 O3 P3 Pd3 S4'
_chemical_formula_weight         1847.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-08 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.151(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4508(5)
_cell_length_b                   24.6808(11)
_cell_length_c                   29.1391(13)
_cell_measurement_reflns_used    15365
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3670
_cell_measurement_theta_min      2.5670
_cell_volume                     7496.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.32a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -103.00  77.00   0.25   20.00    --  -13.00 -15.00 108.00  720
  2  \w    -61.00  30.00   0.25   20.00    --  -13.00 -44.00 144.00  364
  3  \w    -76.25   8.00   0.25   20.00    --  -13.00 -72.00 108.00  337
  4  \w    -40.00   5.00   0.25   20.00    --  -13.00  72.00   0.00  180
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_XtaLabPro
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0613140000
_diffrn_orient_matrix_UB_12      0.0073881000
_diffrn_orient_matrix_UB_13      -0.0069231000
_diffrn_orient_matrix_UB_21      0.0218756000
_diffrn_orient_matrix_UB_22      0.0041968000
_diffrn_orient_matrix_UB_23      0.0233324000
_diffrn_orient_matrix_UB_31      0.0198736000
_diffrn_orient_matrix_UB_32      -0.0274566000
_diffrn_orient_matrix_UB_33      0.0017056000
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            62641
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.189
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.32a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         16722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0344P)^2^+2.2209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12961
_reflns_number_total             16722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03475j2.cif
_cod_data_source_block           wyl-230415_mo
_cod_database_code               1546909
_chemical_oxdiff_formula         C73H48Cl3F12O3P3Pd3S4
_reflns_odcompleteness_completeness 97.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(S5)=Sof(C74)=Sof(F13)=Sof(F14)=Sof(F15)=Sof(O4)=Sof(O5)=Sof(O6)=1-FVAR(1)
 Sof(S4)=Sof(C73)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(O1)=Sof(O2)=Sof(O3)=FVAR(1)
3.a Free rotating group:
 S4(C73,F10,F11,F12,O1,O2,O3), S5(C74,F13,F14,F15,O4,O5,O6)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C13(H13), C14(H14),
 C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C25(H25), C26(H26),
  C28(H28), C29(H29), C31(H31), C32(H32), C34(H34), C35(H35), C37(H37),
 C38(H38), C40(H40), C41(H41), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C51(H51), C52(H52), C55(H55), C56(H56), C58(H58), C59(H59),
 C61(H61), C62(H62), C64(H64), C65(H65), C67(H67), C68(H68), C70(H70), C71(H71),
  C72(H72)
;
_shelx_res_checksum              69072
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.243
_oxdiff_exptl_absorpt_empirical_full_min 0.779