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_1546911
_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 H52 Ag Cl3 F9 O2 P3 Pd3 S3, 2(B F4), 0.75(C H Cl3)'
_chemical_formula_sum            'C72.75 H52.75 Ag B2 Cl5.25 F17 O2 P3 Pd3 S3'
_chemical_formula_weight         2105.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2017-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.9665(4)
_cell_length_b                   30.9093(6)
_cell_length_c                   32.546(2)
_cell_measurement_reflns_used    21700
_cell_measurement_temperature    200
_cell_measurement_theta_max      69.9
_cell_measurement_theta_min      2.0
_cell_volume                     20085.8(14)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_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      200
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
    Number of images: 33
               Slice: 20.0000 - 187.0000
         Image width: 5.0000
            Exp time: 300.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 90.0000
                 XTD: 127.4000
              2theta: 0.0000
scan:
    Number of images: 28
               Slice: 42.0000 - 185.0000
         Image width: 5.0000
            Exp time: 300.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 180.0000
                 XTD: 127.4000
              2theta: 0.0000
;
_diffrn_measurement_device
;
Crystal Goniometer
;
_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.045779
_diffrn_orient_matrix_UB_12      -0.005303
_diffrn_orient_matrix_UB_13      -0.011408
_diffrn_orient_matrix_UB_21      -0.018783
_diffrn_orient_matrix_UB_22      0.000267
_diffrn_orient_matrix_UB_23      -0.028489
_diffrn_orient_matrix_UB_31      0.007762
_diffrn_orient_matrix_UB_32      0.031920
_diffrn_orient_matrix_UB_33      -0.001657
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70255
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        58.936
_diffrn_reflns_theta_max         58.936
_diffrn_reflns_theta_min         2.635
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    8.716
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'FS_ABSCOR (Rigaku, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             8284
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.582
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         14426
_refine_ls_number_restraints     942
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1369P)^2^+47.0645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2131
_refine_ls_wR_factor_ref         0.2819
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9646
_reflns_number_total             14426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03475j2.cif
_cod_data_source_block           platon_sq
_cod_original_cell_volume        20085.5(15)
_cod_database_code               1546911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: Cl6(0.75) Cl5(0.75) Cl4(0.75) C73(0.75) H73(0.75)
4.a Riding coordinates:
 O2(H2A,H2B)
4.b Free rotating group:
 Cl6(Cl5,Cl4,C73,O2)
4.c Rotating group:
 O1(H1A,H1B)
4.d Ternary CH refined with riding coordinates:
 C73(H73)
4.e Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26),
  C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36),
 C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48),
  C50(H50), C51(H51), C53(H53), C54(H54), C56(H56), C57(H57), C59(H59),
 C60(H60), C62(H62), C63(H63), C65(H65), C66(H66), C68(H68), C69(H69), C71(H71),
  C72(H72)
;
_shelx_res_checksum              11234
_shelx_fab_checksum              54159
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'