Syntheses, Structures, and Reactivities of Novel Palladium β-Diiminato-Acetate Complexes
Alen Hadzovic; Datong Song; Inorganic Chemistry 47 (2008) 12010–12017; doi:10.1021/ic801557c

data_4306742
_publ_section_title
;
Syntheses, Structures, and Reactivities of Novel Palladium
\b-Diiminato-Acetate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12010
_journal_page_last               12017
_journal_paper_doi               10.1021/ic801557c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C31 H44 N2 O2 Pd'
_chemical_formula_weight         583.08
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.165(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.692(6)
_cell_length_b                   16.787(6)
_cell_length_c                   21.497(7)
_cell_measurement_reflns_used    46538
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.44
_cell_volume                     6348(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1233
_diffrn_reflns_av_sigmaI/netI    0.1466
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46538
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.44
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker Apex 2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         11094
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1617
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.3034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1296
_reflns_number_gt                5071
_reflns_number_total             11094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801557c_si_001_2.cif
_cod_data_source_block           Complex_1b
_cod_database_code               4306742