Novel Air-Stable and Volatile Bis(pyridylalkenolato)palladium(II) and -platinum(II) Derivatives
Lisa Brückmann; Wieland Tyrra; Stefan Stucky; Sanjay Mathur; Inorganic Chemistry 51 (2012) 536–542; doi:10.1021/ic201996r

data_4327863
_publ_section_title
;
 Novel Air-Stable and Volatile Bis(pyridylalkenolato)palladium(II) and
 -platinum(II) Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              536
_journal_page_last               542
_journal_paper_doi               10.1021/ic201996r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C16 H16 N2 O2 Pd'
_chemical_formula_sum            'C16 H16 N2 O2 Pd'
_chemical_formula_weight         374.71
_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                90.000
_cell_angle_beta                 106.872(14)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   10.1229(19)
_cell_length_b                   5.8527(6)
_cell_length_c                   12.7090(24)
_cell_measurement_reflns_used    10510
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      3.04
_cell_volume                     720.6(2)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9244
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.293
_exptl_absorpt_correction_T_max  0.9128
_exptl_absorpt_correction_T_min  0.6228
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001)
was performed after optimizing the crystal shape
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       needle
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.062(4)
_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   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.0584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0798
_reflns_number_gt                1634
_reflns_number_total             1988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201996r_si_002_3.cif
_cod_data_source_block           shelxl
_cod_database_code               4327863