Volatile heterometallics: structural diversity of palladium-lead β-diketonates and correlation with thermal properties
Krisyuk, Vladislav; Baidina, Iraida; Kryuchkova, Natalia; Logvinenko, Vladimir A.; Plyusnin, Pavel; Korolkov, Ilya V.; Zharkova, G. I.; Turgambaeva, Asiya; Igumenov, Igor K.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02843A

data_7044012
_publ_section_title
;
 Volatile heterometallics: structural diversity of palladium-lead
 \b-diketonates and correlation with thermal properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02843A
_journal_year                    2017
_chemical_formula_moiety         'C12.50 H11.50 F6 O5 Pb0.50 Pd0.75'
_chemical_formula_sum            'C12.5 H11.5 F6 O5 Pb0.5 Pd0.75'
_chemical_formula_weight         539.11
_chemical_melting_point          473
_chemical_name_common            3Pd(aa)2*2Pb(hfa)2
_chemical_name_systematic
'tris-(palladium acetylacetonate)bis-(lead hexafluoroacetylacetonate)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-03-29 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                74.679(2)
_cell_angle_beta                 72.7640(10)
_cell_angle_gamma                69.4460(10)
_cell_formula_units_Z            4
_cell_length_a                   9.8740(3)
_cell_length_b                   13.2443(4)
_cell_length_c                   14.6006(4)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.39
_cell_measurement_theta_min      2.26
_cell_volume                     1679.93(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33793
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         33.41
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    5.915
_exptl_absorpt_correction_T_max  0.4707
_exptl_absorpt_correction_T_min  0.2313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1024
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.351
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         12793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0234
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0104P)^2^+0.9812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0504
_reflns_number_gt                12021
_reflns_number_total             12793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02843a2.cif
_cod_data_source_block           p
_cod_original_formula_sum        'C12.50 H11.50 F6 O5 Pb0.50 Pd0.75'
_cod_database_code               7044012