#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:04:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179912 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/07/7020732.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_7020732
loop_
_publ_author_name
'Shishilov, Oleg N.'
'Podobedov, Roman E.'
'Rezinkova, Yaroslavna N.'
'Churakov, Andrei V.'
'Efimenko, Inessa A.'
_publ_section_title
;
 Palladium ketonyl carboxylate complexes - potential models of polynuclear
 intermediates in olefin oxidation: formation and X-ray structure of
 Pd(6)(μ-Cl)(2+x)(μ-CF(3)CO(2))(4)(μ,κ(2)-CH(2)C(O)CMe(3))(6-x) (x =
 0, 2).
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1338
_journal_page_last               1341
_journal_paper_doi               10.1039/c2dt31824e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C32 H44 Cl4 F12 O12 Pd6'
_chemical_formula_sum            'C32 H44 Cl4 F12 O12 Pd6'
_chemical_formula_weight         1628.87
_chemical_name_systematic
;
?
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.500(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1569(14)
_cell_length_b                   14.474(2)
_cell_length_c                   19.072(3)
_cell_measurement_reflns_used    6906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.717
_cell_measurement_theta_min      2.145
_cell_volume                     2516.1(7)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ω
_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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17558
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.407
_exptl_absorpt_correction_T_max  0.7141
_exptl_absorpt_correction_T_min  0.6446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.333
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4932
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0820P)²+7.8764P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                3722
_reflns_number_total             4932
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c2dt31824e.txt
_cod_data_source_block           6b
_cod_original_cell_volume        2516.0(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7020732
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.80776(6) 0.51569(4) 1.01711(3) 0.03237(17) Uani 1 1 d . . .
Pd2 Pd 0.65164(6) 0.68964(4) 0.88758(3) 0.03156(17) Uani 1 1 d . . .
Pd3 Pd 0.33976(6) 0.65427(4) 0.85962(3) 0.03378(18) Uani 1 1 d . . .
Cl1 Cl 0.7134(2) 0.53649(13) 0.90290(9) 0.0379(4) Uani 1 1 d . . .
Cl2 Cl 0.6948(2) 0.37628(13) 1.02468(10) 0.0404(4) Uani 1 1 d . . .
O11 O 0.5906(6) 0.8250(4) 0.8748(3) 0.0411(13) Uani 1 1 d . . .
O12 O 0.3499(7) 0.7996(4) 0.8808(3) 0.0459(14) Uani 1 1 d . . .
C11 C 0.4589(10) 0.8482(5) 0.8775(4) 0.0427(19) Uani 1 1 d . A .
C12 C 0.4344(7) 0.9525(6) 0.8742(3) 0.051(2) Uani 1 1 d D . .
F11 F 0.3153(9) 0.9778(8) 0.9032(6) 0.063(3) Uiso 0.52 1 d PD A 1
F12 F 0.4229(12) 0.9795(8) 0.8069(4) 0.061(3) Uiso 0.52 1 d PD A 1
F13 F 0.5488(10) 0.9985(8) 0.9068(6) 0.068(3) Uiso 0.52 1 d PD A 1
F14 F 0.5055(12) 0.9925(8) 0.9312(5) 0.068(3) Uiso 0.48 1 d PD A 2
F15 F 0.2919(8) 0.9760(8) 0.8747(6) 0.052(3) Uiso 0.48 1 d PD A 2
F16 F 0.4819(12) 0.9921(8) 0.8181(5) 0.064(3) Uiso 0.48 1 d PD A 2
O21 O 0.6232(7) 0.6785(4) 0.7762(3) 0.0436(13) Uani 1 1 d . . .
O22 O 0.3766(6) 0.6846(4) 0.7578(3) 0.0423(13) Uani 1 1 d . . .
C21 C 0.5040(10) 0.6911(5) 0.7400(4) 0.0390(18) Uani 1 1 d . B .
C22 C 0.5156(7) 0.7233(4) 0.6649(4) 0.051(2) Uani 1 1 d D . .
F21 F 0.3975(8) 0.7026(6) 0.6227(5) 0.058(2) Uiso 0.61 1 d PD B 3
F22 F 0.6292(8) 0.6821(6) 0.6379(4) 0.055(2) Uiso 0.61 1 d PD B 3
F23 F 0.5411(10) 0.8125(5) 0.6629(5) 0.063(2) Uiso 0.61 1 d PD B 3
F24 F 0.4627(14) 0.8098(6) 0.6605(7) 0.057(4) Uiso 0.39 1 d PD B 4
F25 F 0.6522(10) 0.7272(11) 0.6485(9) 0.088(6) Uiso 0.39 1 d PD B 4
F26 F 0.4370(14) 0.6753(8) 0.6159(7) 0.060(4) Uiso 0.39 1 d PD B 4
O31 O 0.0986(6) 0.4941(4) 0.8840(3) 0.0396(12) Uani 1 1 d . . .
C30 C 0.3258(9) 0.5167(5) 0.8366(4) 0.0359(16) Uani 1 1 d . . .
H30A H 0.3676 0.5021 0.7919 0.043 Uiso 1 1 calc R . .
H30B H 0.3745 0.4785 0.8751 0.043 Uiso 1 1 calc R . .
C31 C 0.1679(9) 0.5051(5) 0.8305(4) 0.0386(18) Uani 1 1 d . . .
C32 C 0.0714(10) 0.5054(6) 0.7612(4) 0.045(2) Uani 1 1 d . . .
C33 C -0.0182(12) 0.5955(8) 0.7596(5) 0.065(3) Uani 1 1 d . . .
H33A H -0.0810 0.5954 0.7985 0.097 Uiso 1 1 calc R . .
H33B H -0.0794 0.6001 0.7147 0.097 Uiso 1 1 calc R . .
H33C H 0.0487 0.6485 0.7647 0.097 Uiso 1 1 calc R . .
C34 C -0.0292(12) 0.4205(8) 0.7608(5) 0.069(3) Uani 1 1 d . . .
H34A H 0.0305 0.3643 0.7635 0.103 Uiso 1 1 calc R . .
H34B H -0.0953 0.4199 0.7172 0.103 Uiso 1 1 calc R . .
H34C H -0.0871 0.4233 0.8014 0.103 Uiso 1 1 calc R . .
C35 C 0.1614(11) 0.5023(7) 0.6964(4) 0.054(2) Uani 1 1 d . . .
H35A H 0.2235 0.4470 0.6990 0.081 Uiso 1 1 calc R . .
H35B H 0.2233 0.5575 0.6960 0.081 Uiso 1 1 calc R . .
H35C H 0.0944 0.5003 0.6532 0.081 Uiso 1 1 calc R . .
O41 O 0.9111(6) 0.6375(4) 1.0150(3) 0.0402(12) Uani 1 1 d . . .
C40 C 0.6829(9) 0.7120(5) 0.9936(4) 0.0364(17) Uani 1 1 d . . .
H40A H 0.6420 0.7722 1.0068 0.044 Uiso 1 1 calc R . .
H40B H 0.6401 0.6619 1.0204 0.044 Uiso 1 1 calc R . .
C41 C 0.8424(9) 0.7115(5) 1.0035(4) 0.0367(17) Uani 1 1 d . . .
C42 C 0.9346(9) 0.7974(6) 0.9998(4) 0.0431(19) Uani 1 1 d . . .
C43 C 0.8489(12) 0.8877(7) 1.0069(7) 0.069(3) Uani 1 1 d . . .
H43A H 0.7715 0.8927 0.9678 0.104 Uiso 1 1 calc R . .
H43B H 0.9158 0.9404 1.0056 0.104 Uiso 1 1 calc R . .
H43C H 0.8046 0.8877 1.0517 0.104 Uiso 1 1 calc R . .
C44 C 1.0616(12) 0.7932(7) 1.0589(6) 0.066(3) Uani 1 1 d . . .
H44A H 1.0215 0.7899 1.1047 0.099 Uiso 1 1 calc R . .
H44B H 1.1224 0.8487 1.0571 0.099 Uiso 1 1 calc R . .
H44C H 1.1215 0.7383 1.0525 0.099 Uiso 1 1 calc R . .
C45 C 0.9975(11) 0.7959(7) 0.9274(5) 0.058(2) Uani 1 1 d . . .
H45A H 0.9178 0.8051 0.8899 0.087 Uiso 1 1 calc R . .
H45B H 1.0447 0.7362 0.9208 0.087 Uiso 1 1 calc R . .
H45C H 1.0699 0.8455 0.9255 0.087 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 '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'
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
O31 Pd1 O41 85.4(2) 3_667 .
O31 Pd1 Cl2 91.94(16) 3_667 .
O41 Pd1 Cl2 177.39(17) . .
O31 Pd1 Cl1 175.39(16) 3_667 .
O41 Pd1 Cl1 90.06(16) . .
Cl2 Pd1 Cl1 92.55(7) . .
C40 Pd2 O11 88.7(3) . .
C40 Pd2 O21 175.1(3) . .
O11 Pd2 O21 87.0(2) . .
C40 Pd2 Cl1 91.0(2) . .
O11 Pd2 Cl1 178.30(16) . .
O21 Pd2 Cl1 93.37(16) . .
C40 Pd2 Pd3 104.6(2) . .
O11 Pd2 Pd3 83.93(16) . .
O21 Pd2 Pd3 77.20(17) . .
Cl1 Pd2 Pd3 94.53(6) . .
C30 Pd3 O22 91.0(3) . .
C30 Pd3 O12 178.2(3) . .
O22 Pd3 O12 87.7(2) . .
C30 Pd3 Cl2 90.4(2) . 3_667
O22 Pd3 Cl2 177.94(17) . 3_667
O12 Pd3 Cl2 90.90(17) . 3_667
C30 Pd3 Pd2 104.6(2) . .
O22 Pd3 Pd2 83.55(16) . .
O12 Pd3 Pd2 76.59(16) . .
Cl2 Pd3 Pd2 94.65(6) 3_667 .
Pd1 Cl1 Pd2 108.30(8) . .
Pd1 Cl2 Pd3 109.62(8) . 3_667
C11 O11 Pd2 120.1(5) . .
C11 O12 Pd3 125.0(5) . .
O12 C11 O11 129.6(7) . .
O12 C11 C12 116.8(7) . .
O11 C11 C12 113.5(7) . .
F11 C12 F12 109.2(7) . .
F11 C12 F13 107.9(7) . .
F12 C12 F13 106.6(7) . .
F16 C12 F14 107.2(7) . .
F16 C12 F15 106.8(7) . .
F14 C12 F15 106.3(7) . .
F11 C12 C11 112.4(8) . .
F16 C12 C11 113.8(8) . .
F12 C12 C11 109.1(8) . .
F13 C12 C11 111.4(8) . .
F14 C12 C11 109.5(8) . .
F15 C12 C11 112.8(8) . .
C21 O21 Pd2 124.1(5) . .
C21 O22 Pd3 121.2(5) . .
O21 C21 O22 128.8(7) . .
O21 C21 C22 115.5(7) . .
O22 C21 C22 115.6(7) . .
F23 C22 F21 110.0(6) . .
F25 C22 F26 108.6(8) . .
F25 C22 F24 106.8(7) . .
F26 C22 F24 106.1(7) . .
F23 C22 F22 106.1(6) . .
F21 C22 F22 106.5(6) . .
F23 C22 C21 111.0(7) . .
F25 C22 C21 113.0(10) . .
F21 C22 C21 112.3(7) . .
F26 C22 C21 115.1(9) . .
F24 C22 C21 106.7(8) . .
F22 C22 C21 110.7(7) . .
C31 O31 Pd1 124.6(5) . 3_667
C31 C30 Pd3 99.9(5) . .
C31 C30 H30A 111.8 . .
Pd3 C30 H30A 111.8 . .
C31 C30 H30B 111.8 . .
Pd3 C30 H30B 111.8 . .
H30A C30 H30B 109.5 . .
O31 C31 C30 121.6(7) . .
O31 C31 C32 114.1(7) . .
C30 C31 C32 124.3(7) . .
C31 C32 C34 107.5(7) . .
C31 C32 C33 106.5(7) . .
C34 C32 C33 111.1(9) . .
C31 C32 C35 112.6(7) . .
C34 C32 C35 109.7(7) . .
C33 C32 C35 109.4(7) . .
C32 C33 H33A 109.5 . .
C32 C33 H33B 109.5 . .
H33A C33 H33B 109.5 . .
C32 C33 H33C 109.5 . .
H33A C33 H33C 109.5 . .
H33B C33 H33C 109.5 . .
C32 C34 H34A 109.5 . .
C32 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C32 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C32 C35 H35A 109.5 . .
C32 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C32 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 109.5 . .
C41 O41 Pd1 121.8(5) . .
C41 C40 Pd2 99.9(5) . .
C41 C40 H40A 111.8 . .
Pd2 C40 H40A 111.8 . .
C41 C40 H40B 111.8 . .
Pd2 C40 H40B 111.8 . .
H40A C40 H40B 109.5 . .
O41 C41 C40 120.6(7) . .
O41 C41 C42 116.1(7) . .
C40 C41 C42 123.3(7) . .
C41 C42 C43 113.9(7) . .
C41 C42 C44 108.7(7) . .
C43 C42 C44 109.0(8) . .
C41 C42 C45 106.7(7) . .
C43 C42 C45 109.1(8) . .
C44 C42 C45 109.5(8) . .
C42 C43 H43A 109.5 . .
C42 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C42 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C42 C44 H44A 109.5 . .
C42 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C42 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C42 C45 H45A 109.5 . .
C42 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C42 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O31 2.001(5) 3_667
Pd1 O41 2.003(6) .
Pd1 Cl2 2.278(2) .
Pd1 Cl1 2.2851(19) .
Pd2 C40 2.040(7) .
Pd2 O11 2.046(5) .
Pd2 O21 2.121(5) .
Pd2 Cl1 2.2993(19) .
Pd2 Pd3 2.9000(9) .
Pd3 C30 2.041(7) .
Pd3 O22 2.050(5) .
Pd3 O12 2.142(5) .
Pd3 Cl2 2.3017(19) 3_667
Cl2 Pd3 2.3017(19) 3_667
O11 C11 1.258(10) .
O12 C11 1.228(10) .
C11 C12 1.527(12) .
C12 F11 1.321(7) .
C12 F16 1.324(8) .
C12 F12 1.337(7) .
C12 F13 1.342(8) .
C12 F14 1.343(8) .
C12 F15 1.349(8) .
O21 C21 1.249(10) .
O22 C21 1.250(10) .
C21 C22 1.518(11) .
C22 F23 1.313(7) .
C22 F25 1.320(8) .
C22 F21 1.320(7) .
C22 F26 1.322(8) .
C22 F24 1.342(8) .
C22 F22 1.344(7) .
O31 C31 1.262(9) .
O31 Pd1 2.001(5) 3_667
C30 C31 1.448(12) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 C32 1.518(11) .
C32 C34 1.535(13) .
C32 C33 1.540(13) .
C32 C35 1.551(11) .
C33 H33A 0.9800 .
C33 H33B 0.9800 .
C33 H33C 0.9800 .
C34 H34A 0.9800 .
C34 H34B 0.9800 .
C34 H34C 0.9800 .
C35 H35A 0.9800 .
C35 H35B 0.9800 .
C35 H35C 0.9800 .
O41 C41 1.251(9) .
C40 C41 1.455(11) .
C40 H40A 0.9900 .
C40 H40B 0.9900 .
C41 C42 1.508(11) .
C42 C43 1.537(13) .
C42 C44 1.541(13) .
C42 C45 1.548(12) .
C43 H43A 0.9800 .
C43 H43B 0.9800 .
C43 H43C 0.9800 .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
