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_7044013
_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         '[Pd(hfa)2*Pb(hfa)2]n'
_chemical_formula_sum            'C20 H4 F24 O8 Pb Pd'
_chemical_formula_weight         1141.82
_chemical_melting_point          ?
_chemical_name_common
palladium(II)hexafluoroacetylacetonate-lead(II)hexafluoroacetylacetonate
_chemical_name_systematic        'heterometallic Pd/Pb complex'
_chemical_properties_physical    'Heat-sensitive, Light-sensitive'
_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
;
2015-11-24 deposited with the CCDC.
2017-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                91.519(5)
_cell_angle_beta                 91.672(5)
_cell_angle_gamma                97.940(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4437(16)
_cell_length_b                   11.538(2)
_cell_length_c                   14.995(3)
_cell_measurement_reflns_used    9628
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      2.18
_cell_volume                     1616.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker X8 Apex'
_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  0.0814
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29916
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.62
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 1
_diffrn_standards_interval_time  1
_diffrn_standards_number         29916
_exptl_absorpt_coefficient_mu    5.937
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_correction_T_min  0.4318
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method Sublimation
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.454
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1667
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1508
_reflns_number_gt                4305
_reflns_number_total             9628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02843a2.cif
_cod_data_source_block           v
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1616.7(5)
_cod_original_sg_symbol_Hall     -P_1
_cod_database_code               7044013