Synthesis of Aryl-, Benzoyl-, and Iminobenzoyl-Palladium(II) Complexes Derived from N-Phenyl Formamide. Synthesis of a Homoleptic Ball-Shaped Tetranuclear Palladium Complex
Vicente-Hernandez, Inmaculada; Chicote, María-Teresa; Vicente, José; Bautista, Delia; Organometallics 35 (2016) 1107–; doi:10.1021/acs.organomet.6b00122

data_4088482
_publ_section_title
;
 Synthesis of Aryl-, Benzoyl-, and Iminobenzoyl-Palladium(II) Complexes
 Derived from N-Phenyl Formamide. Synthesis of a Homoleptic Ball-Shaped
 Tetranuclear Palladium Complex
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1107
_journal_paper_doi               10.1021/acs.organomet.6b00122
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C26.5 H31 Cl F3 N3 O4 Pd S'
_chemical_formula_weight         686.45
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.758(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.496(2)
_cell_length_b                   21.629(3)
_cell_length_c                   14.2704(18)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.18
_cell_volume                     5689.2(12)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_data_collection       'APEX2 2013.2 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'high brilliance microfocus sealed tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            111104
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.072
_refine_diff_density_min         -2.007
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment
'NH free with DFIX, rigid methyls others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     732
_refine_ls_number_reflns         11609
_refine_ls_number_restraints     221
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+23.1509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1510
_reflns_number_gt                9181
_reflns_number_total             11609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00122_si_001.cif
_cod_data_source_block           ivg39spi
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_original_formula_sum        'C26.50 H31 Cl F3 N3 O4 Pd S'
_cod_database_code               4088482