The Role of Trinuclear Species in Palladium Acetate/Trifluoroacetic Acid Catalytic System
Váňa, Jiří; Lang, Jan; Šoltésová, Mária; Hanusek, Jiri; Růžička, Aleš; Sedlák, Miloš; Roithova, Jana; Dalton Transactions  (2017) –; doi:10.1039/C7DT03832A

data_7044613
_publ_section_title
;
 The Role of Trinuclear Species in Palladium Acetate/Trifluoroacetic Acid
 Catalytic System
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03832A
_journal_year                    2017
_chemical_formula_moiety
'C24 H12 Br2 F12 N2 O10 Pd3, 2(C2 O2 H4),2(H2 O)'
_chemical_formula_sum            'C28 H24 Br2 F12 N2 O16 Pd3'
_chemical_formula_weight         1351.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-10 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                112.321(6)
_cell_angle_beta                 96.629(6)
_cell_angle_gamma                105.443(5)
_cell_formula_units_Z            3
_cell_length_a                   11.5323(14)
_cell_length_b                   17.832(2)
_cell_length_c                   18.105(2)
_cell_measurement_reflns_used    43887
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.2
_cell_volume                     3220.4(7)
_computing_cell_refinement       'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_collection       'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_data_reduction        'XT-version 2014/5'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SAINT'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43856
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.780
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.223
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.091
_exptl_crystal_description       block
_exptl_crystal_F_000             1950
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.132
_refine_diff_density_max         2.223
_refine_diff_density_min         -1.847
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         13330
_refine_ls_number_restraints     792
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1185P)^2^+35.2433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1942
_refine_ls_wR_factor_ref         0.2414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8562
_reflns_number_total             13330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03832a2.cif
_cod_data_source_block           shelx
_cod_database_code               7044613
_shelx_shelxl_version_number     2014/7
_shelxl_version_number           2013-4
_shelx_res_checksum              34438
_shelx_fab_checksum              96230