#------------------------------------------------------------------------------
#$Date: 2017-08-23 06:06:12 +0300 (Wed, 23 Aug 2017) $
#$Revision: 199887 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/40/7044012.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7044012
loop_
_publ_author_name
'Krisyuk, Vladislav'
'Baidina, Iraida'
'Kryuchkova, Natalia'
'Logvinenko, Vladimir A.'
'Plyusnin, Pavel'
'Korolkov, Ilya V.'
'Zharkova, G. I.'
'Turgambaeva, Asiya'
'Igumenov, Igor K.'
_publ_section_title
;
 Volatile heterometallics: structural diversity of palladium-lead
 β-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       'φ and ω 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/[σ²(Fo²)+(0.0104P)²+0.9812P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.655795(7) 0.172864(5) 0.267802(4) 0.02031(2) Uani 1 1 d .
Pd1 Pd 0.5000 0.0000 0.5000 0.01482(3) Uani 1 2 d S
Pd2 Pd 0.871283(14) -0.065526(11) 0.435429(9) 0.01893(3) Uani 1 1 d .
O1 O 0.43868(14) 0.15981(10) 0.44474(9) 0.0196(2) Uani 1 1 d .
O2 O 0.53829(14) -0.02062(11) 0.36346(9) 0.0192(2) Uani 1 1 d .
C1 C 0.38338(19) 0.23409(15) 0.49810(13) 0.0200(3) Uani 1 1 d .
C2 C 0.3724(2) 0.21640(15) 0.59822(14) 0.0224(3) Uani 1 1 d .
H2 H 0.3327 0.2798 0.6276 0.029 Uiso 1 1 calc R
C3 C 0.58687(19) -0.11585(15) 0.33964(13) 0.0196(3) Uani 1 1 d .
C4 C 0.3268(2) 0.34852(17) 0.44458(16) 0.0303(4) Uani 1 1 d .
H4A H 0.4075 0.3675 0.3923 0.039 Uiso 1 1 calc R
H4B H 0.2901 0.4001 0.4900 0.039 Uiso 1 1 calc R
H4C H 0.2458 0.3526 0.4166 0.039 Uiso 1 1 calc R
C5 C 0.5991(3) -0.11677(18) 0.23492(14) 0.0286(4) Uani 1 1 d .
H5A H 0.5111 -0.1306 0.2290 0.037 Uiso 1 1 calc R
H5B H 0.6882 -0.1747 0.2121 0.037 Uiso 1 1 calc R
H5C H 0.6061 -0.0457 0.1953 0.037 Uiso 1 1 calc R
O3 O 0.80225(15) 0.09470(11) 0.43827(10) 0.0229(2) Uani 1 1 d .
O4 O 0.85470(16) -0.11277(13) 0.57754(10) 0.0265(3) Uani 1 1 d .
O5 O 0.89202(15) -0.02268(11) 0.29083(9) 0.0226(2) Uani 1 1 d .
O6 O 0.94665(15) -0.22535(12) 0.43468(10) 0.0249(3) Uani 1 1 d .
C6 C 0.8187(2) -0.04611(19) 0.63540(14) 0.0269(4) Uani 1 1 d .
C7 C 0.7853(2) 0.06826(18) 0.60996(14) 0.0265(4) Uani 1 1 d .
H7 H 0.7649 0.1069 0.6611 0.034 Uiso 1 1 calc R
C8 C 0.77882(19) 0.13106(17) 0.51748(14) 0.0236(3) Uani 1 1 d .
C9 C 0.7450(2) 0.25314(18) 0.50383(17) 0.0313(4) Uani 1 1 d .
H9A H 0.8353 0.2740 0.4689 0.041 Uiso 1 1 calc R
H9B H 0.7093 0.2757 0.5677 0.041 Uiso 1 1 calc R
H9C H 0.6684 0.2894 0.4660 0.041 Uiso 1 1 calc R
C10 C 0.8161(3) -0.0998(2) 0.74063(16) 0.0414(6) Uani 1 1 d .
H10A H 0.7487 -0.1452 0.7623 0.054 Uiso 1 1 calc R
H10B H 0.7816 -0.0432 0.7810 0.054 Uiso 1 1 calc R
H10C H 0.9164 -0.1459 0.7469 0.054 Uiso 1 1 calc R
C11 C 0.9578(2) -0.09276(16) 0.23272(13) 0.0234(3) Uani 1 1 d .
C12 C 1.0138(2) -0.20537(17) 0.26078(15) 0.0284(4) Uani 1 1 d .
H12 H 1.0636 -0.2466 0.2098 0.037 Uiso 1 1 calc R
C13 C 1.0045(2) -0.26484(17) 0.35651(15) 0.0261(4) Uani 1 1 d .
C14 C 0.9705(3) -0.04417(19) 0.12661(14) 0.0311(4) Uani 1 1 d .
H14A H 0.8712 -0.0133 0.1128 0.040 Uiso 1 1 calc R
H14B H 1.0304 -0.1013 0.0876 0.040 Uiso 1 1 calc R
H14C H 1.0181 0.0139 0.1100 0.040 Uiso 1 1 calc R
C15 C 1.0659(3) -0.38781(19) 0.37207(19) 0.0404(5) Uani 1 1 d .
H15A H 1.0564 -0.4171 0.4420 0.053 Uiso 1 1 calc R
H15B H 1.1709 -0.4087 0.3385 0.053 Uiso 1 1 calc R
H15C H 1.0104 -0.4178 0.3459 0.053 Uiso 1 1 calc R
O7 O 0.4581(2) 0.32335(15) 0.20999(12) 0.0391(4) Uani 1 1 d .
O8 O 0.62202(18) 0.13314(13) 0.12021(11) 0.0311(3) Uani 1 1 d .
O9 O 0.67224(19) 0.34651(13) 0.29040(11) 0.0332(3) Uani 1 1 d .
O10 O 0.84903(18) 0.22379(13) 0.13610(11) 0.0320(3) Uani 1 1 d .
C16 C 0.4231(3) 0.3564(2) 0.12942(16) 0.0331(4) Uani 1 1 d .
C17 C 0.4678(3) 0.3022(2) 0.05121(17) 0.0401(5) Uani 1 1 d .
H17 H 0.4341 0.3399 -0.0067 0.052 Uiso 1 1 calc R
C18 C 0.5603(2) 0.19441(18) 0.05442(14) 0.0261(4) Uani 1 1 d .
C19 C 0.3100(4) 0.4710(3) 0.1211(2) 0.0563(8) Uani 1 1 d .
C20 C 0.5868(3) 0.1442(2) -0.03557(16) 0.0363(5) Uani 1 1 d .
C21 C 0.7477(3) 0.40791(18) 0.24012(15) 0.0308(4) Uani 1 1 d .
C22 C 0.8622(3) 0.39252(18) 0.15672(16) 0.0328(4) Uani 1 1 d .
H22 H 0.9137 0.4460 0.1290 0.043 Uiso 1 1 calc R
C23 C 0.9029(2) 0.30192(17) 0.11313(14) 0.0253(4) Uani 1 1 d .
C24 C 0.7064(4) 0.5165(2) 0.2764(2) 0.0531(8) Uani 1 1 d .
C25 C 1.0322(3) 0.29202(19) 0.02208(16) 0.0340(5) Uani 1 1 d .
F1 F 0.3459(3) 0.53956(15) 0.15385(16) 0.0703(6) Uani 1 1 d .
F2 F 0.3006(3) 0.51683(18) 0.02858(15) 0.0939(10) Uani 1 1 d .
F3 F 0.1772(2) 0.4678(2) 0.17292(19) 0.0809(7) Uani 1 1 d .
F4 F 0.4611(2) 0.1376(2) -0.04504(16) 0.0740(7) Uani 1 1 d .
F5 F 0.6792(2) 0.04339(16) -0.02996(14) 0.0636(5) Uani 1 1 d .
F6 F 0.6442(3) 0.20153(19) -0.11678(13) 0.0802(7) Uani 1 1 d .
F7 F 0.6017(14) 0.5916(5) 0.2360(11) 0.126(3) Uani 0.50 1 d P
F8 F 0.6560(17) 0.5100(6) 0.3659(4) 0.112(5) Uani 0.50 1 d P
F9 F 0.8134(9) 0.5620(7) 0.2497(8) 0.102(4) Uani 0.50 1 d P
F7A F 0.7802(16) 0.4948(7) 0.3499(8) 0.131(4) Uani 0.50 1 d P
F8A F 0.5717(11) 0.5478(8) 0.3217(11) 0.126(4) Uani 0.50 1 d P
F9A F 0.7429(17) 0.5932(6) 0.2186(6) 0.126(5) Uani 0.50 1 d P
F10 F 0.9855(2) 0.29701(17) -0.05568(11) 0.0602(5) Uani 1 1 d .
F11 F 1.0983(3) 0.36923(17) 0.00030(15) 0.0748(7) Uani 1 1 d .
F12 F 1.13458(18) 0.19638(15) 0.03322(13) 0.0598(5) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O10 Pb1 O7 94.05(6) . .
O10 Pb1 O9 72.57(5) . .
O7 Pb1 O9 70.93(6) . .
O10 Pb1 O8 74.78(6) . .
O7 Pb1 O8 71.97(5) . .
O9 Pb1 O8 127.76(5) . .
O2 Pd1 O2 180.0 2_656 .
O2 Pd1 O1 84.93(5) 2_656 2_656
O2 Pd1 O1 95.07(5) . 2_656
O2 Pd1 O1 95.07(5) 2_656 .
O2 Pd1 O1 84.93(5) . .
O1 Pd1 O1 179.999(1) 2_656 .
O4 Pd2 O6 83.60(6) . .
O4 Pd2 O3 95.34(6) . .
O6 Pd2 O3 177.74(5) . .
O4 Pd2 O5 178.12(6) . .
O6 Pd2 O5 94.57(6) . .
O3 Pd2 O5 86.48(6) . .
C1 O1 Pd1 122.74(12) . .
C3 O2 Pd1 122.49(11) . .
O1 C1 C2 125.69(17) . .
O1 C1 C4 114.82(16) . .
C2 C1 C4 119.48(16) . .
C1 C2 C3 127.42(17) . 2_656
O2 C3 C2 126.20(16) . 2_656
O2 C3 C5 115.52(16) . .
C2 C3 C5 118.28(16) 2_656 .
C8 O3 Pd2 121.64(13) . .
C6 O4 Pd2 123.06(13) . .
C11 O5 Pd2 122.55(12) . .
C13 O6 Pd2 122.84(13) . .
O4 C6 C7 126.41(18) . .
O4 C6 C10 114.4(2) . .
C7 C6 C10 119.2(2) . .
C8 C7 C6 126.79(19) . .
O3 C8 C7 126.41(19) . .
O3 C8 C9 114.45(17) . .
C7 C8 C9 119.13(18) . .
O5 C11 C12 125.77(18) . .
O5 C11 C14 114.75(17) . .
C12 C11 C14 119.48(18) . .
C11 C12 C13 126.94(19) . .
O6 C13 C12 126.51(19) . .
O6 C13 C15 114.48(19) . .
C12 C13 C15 119.0(2) . .
C16 O7 Pb1 132.72(15) . .
C18 O8 Pb1 130.88(14) . .
C21 O9 Pb1 132.11(14) . .
C23 O10 Pb1 134.01(13) . .
O7 C16 C17 128.8(2) . .
O7 C16 C19 113.1(2) . .
C17 C16 C19 118.0(2) . .
C16 C17 C18 122.5(2) . .
O8 C18 C17 129.00(19) . .
O8 C18 C20 115.7(2) . .
C17 C18 C20 115.27(19) . .
F3 C19 F1 106.6(3) . .
F3 C19 F2 108.6(3) . .
F1 C19 F2 105.9(3) . .
F3 C19 C16 111.2(3) . .
F1 C19 C16 111.8(2) . .
F2 C19 C16 112.5(2) . .
F6 C20 F4 108.2(2) . .
F6 C20 F5 106.3(2) . .
F4 C20 F5 106.4(2) . .
F6 C20 C18 112.3(2) . .
F4 C20 C18 110.83(18) . .
F5 C20 C18 112.6(2) . .
O9 C21 C22 129.4(2) . .
O9 C21 C24 113.9(2) . .
C22 C21 C24 116.6(2) . .
C23 C22 C21 122.18(19) . .
O10 C23 C22 129.41(19) . .
O10 C23 C25 112.55(18) . .
C22 C23 C25 118.04(18) . .
F9A C24 F8 127.4(5) . .
F9A C24 F8A 110.7(7) . .
F8 C24 F8A 52.0(6) . .
F9A C24 F9 39.8(7) . .
F8 C24 F9 109.5(7) . .
F8A C24 F9 132.3(5) . .
F9A C24 F7 64.0(6) . .
F8 C24 F7 105.6(7) . .
F8A C24 F7 56.6(6) . .
F9 C24 F7 102.6(6) . .
F9A C24 F7A 104.6(7) . .
F8 C24 F7A 50.6(5) . .
F8A C24 F7A 101.5(7) . .
F9 C24 F7A 68.0(6) . .
F7 C24 F7A 142.3(5) . .
F9A C24 C21 117.9(4) . .
F8 C24 C21 114.0(4) . .
F8A C24 C21 113.4(4) . .
F9 C24 C21 114.2(4) . .
F7 C24 C21 110.1(4) . .
F7A C24 C21 106.9(4) . .
F12 C25 F11 107.6(2) . .
F12 C25 F10 106.1(2) . .
F11 C25 F10 107.0(2) . .
F12 C25 C23 110.95(18) . .
F11 C25 C23 113.8(2) . .
F10 C25 C23 111.0(2) . .
F8A F7 C24 59.8(5) . .
F8A F7 F9A 105.5(8) . .
C24 F7 F9A 54.6(4) . .
F8A F8 F7A 134.2(10) . .
F8A F8 C24 65.2(5) . .
F7A F8 C24 71.2(6) . .
F9A F9 C24 64.9(6) . .
F9A F9 F7A 118.7(10) . .
C24 F9 F7A 58.5(5) . .
F8 F7A C24 58.2(5) . .
F8 F7A F9 103.3(8) . .
C24 F7A F9 53.5(4) . .
F8 F8A F7 122.2(10) . .
F8 F8A C24 62.8(6) . .
F7 F8A C24 63.6(5) . .
F9 F9A C24 75.4(7) . .
F9 F9A F7 134.4(10) . .
C24 F9A F7 61.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O10 2.4160(14) .
Pb1 O7 2.4192(16) .
Pb1 O9 2.4737(15) .
Pb1 O8 2.4860(15) .
Pd1 O2 1.9900(12) 2_656
Pd1 O2 1.9900(12) .
Pd1 O1 1.9961(13) 2_656
Pd1 O1 1.9961(13) .
Pd2 O4 1.9769(14) .
Pd2 O6 1.9839(15) .
Pd2 O3 1.9958(14) .
Pd2 O5 2.0033(13) .
O1 C1 1.284(2) .
O2 C3 1.285(2) .
C1 C2 1.395(3) .
C1 C4 1.503(3) .
C2 C3 1.400(3) 2_656
C3 C2 1.400(3) 2_656
C3 C5 1.501(3) .
O3 C8 1.296(2) .
O4 C6 1.271(3) .
O5 C11 1.292(2) .
O6 C13 1.273(2) .
C6 C7 1.402(3) .
C6 C10 1.510(3) .
C7 C8 1.393(3) .
C8 C9 1.502(3) .
C11 C12 1.389(3) .
C11 C14 1.498(3) .
C12 C13 1.405(3) .
C13 C15 1.505(3) .
O7 C16 1.248(3) .
O8 C18 1.241(3) .
O9 C21 1.242(3) .
O10 C23 1.251(2) .
C16 C17 1.388(3) .
C16 C19 1.535(4) .
C17 C18 1.396(3) .
C18 C20 1.541(3) .
C19 F3 1.315(4) .
C19 F1 1.317(4) .
C19 F2 1.343(3) .
C20 F6 1.316(3) .
C20 F4 1.323(3) .
C20 F5 1.324(3) .
C21 C22 1.398(3) .
C21 C24 1.542(3) .
C22 C23 1.385(3) .
C23 C25 1.543(3) .
C24 F9A 1.223(6) .
C24 F8 1.244(6) .
C24 F8A 1.271(8) .
C24 F9 1.307(7) .
C24 F7 1.318(7) .
C24 F7A 1.386(8) .
C25 F12 1.320(3) .
C25 F11 1.322(3) .
C25 F10 1.325(3) .
F7 F8A 1.228(12) .
F7 F9A 1.348(12) .
F8 F8A 1.102(12) .
F8 F7A 1.132(12) .
F9 F9A 0.864(14) .
F9 F7A 1.508(12) .
