Electronic influence of β-diketonato-type ligands on the coordination of 1,5-cyclooctadiene to palladium(II) as defined by `Venus fly trap' geometric parameters
Hill, Tania N.; Roodt, Andreas; Steyl, Gideon; Acta Crystallographica Section B 69 (2013) 36–42; doi:10.1107/S0108768112046733

data_2105310
_publ_section_title
;
 Electronic influence of \b-diketonato-type ligands on the coordination of
 1,5-cyclooctadiene to palladium(II) as defined by `Venus fly trap'
 geometric parameters
;
_journal_coeditor_code           EB5019
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              36
_journal_page_last               42
_journal_paper_doi               10.1107/S0108768112046733
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C13 H19 O2 Pd, B F4'
_chemical_formula_structural     '(Pd (C8 H12) (O2 C5 H7)) (B F4)'
_chemical_formula_sum            'C13 H19 B F4 O2 Pd'
_chemical_formula_weight         400.49
_chemical_name_systematic
;
(acetylacetonato)(\h^4^-cyclo-octa-1,5-dienyl)palladium(II) tetrafluoroborate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.2908(11)
_cell_length_b                   7.1684(3)
_cell_length_c                   7.7782(3)
_cell_measurement_reflns_used    8277
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.84
_cell_volume                     1465.90(10)
_computing_cell_refinement       'Bruker SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2005)'
_computing_data_reduction        'Bruker SAINT-Plus and XPREP (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND 3.0c (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEX-II 4K Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15654
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.9139
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.61
_refine_ls_abs_structure_details
;
Flack H D (1983), Acta Cryst. A39, 876-881, 1143 Friedel pairs
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3117
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.7363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                2960
_reflns_number_total             3117
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            eb5019.cif
_cod_data_source_block           10rth5_0ma
_cod_database_code               2105310
_cod_database_fobs_code          2105310