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_2105311
_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         'C16 H16 F3 O2 Pd S, F6 P'
_chemical_formula_structural     '(Pd (C8 H12) (O2 S F3 C8 H7)) (P F6)'
_chemical_formula_sum            'C16 H16 F9 O2 P Pd S'
_chemical_formula_weight         580.72
_chemical_name_systematic
;
(thenoyltrifluoroacetonato)(\h^4^-cyclo-octa-1,5-dienyl)palladium(II)
 hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_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           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 124.4390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9691(2)
_cell_length_b                   17.0294(3)
_cell_length_c                   13.6427(3)
_cell_measurement_reflns_used    10209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0099
_cell_measurement_theta_min      2.1649
_cell_volume                     1910.15(7)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'DIAMOND 3.0c (Brandenburg & Putz, 2004)'
_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 16.1829
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15058
_diffrn_reflns_theta_full        28
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.8842
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.019
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.707
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.033
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.059
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                3596
_reflns_number_total             4606
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            eb5019.cif
_cod_data_source_block           9Tth12_L
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105311