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_4088481
_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            'C32 H28 N4 O2 Pd2'
_chemical_formula_weight         713.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.2360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6292(8)
_cell_length_b                   17.6232(8)
_cell_length_c                   17.8101(7)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.31
_cell_volume                     6042.9(4)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2011)'
_computing_data_collection       'APEX2 2012 (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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'XS-SHELXTL-2013 '
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.360
_diffrn_reflns_theta_min         2.116
_diffrn_source                   'high brilliance microfocus sealed tube '
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0202
_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^)+(0.0210P)^2^+9.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6629
_reflns_number_total             7552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00122_si_001.cif
_cod_data_source_block           ivh18_1r_b_sq
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4088481
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              86299
_shelx_hkl_checksum              48316
_shelx_fab_checksum              74211