# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
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# Cambridge Crystallographic Data Centre
# CCDC
#
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# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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data_s
_database_code_depnum_ccdc_archive 'CCDC 893512'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1352736740.6a_squeeze.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C44 H66 Cl2 F12 O14 Pd6'
_chemical_formula_sum 'C44 H66 Cl2 F12 O14 Pd6'
_chemical_formula_weight 1756.27
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'
Cl Cl 0.1484 0.1585 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 25.986(4)
_cell_length_b 14.314(2)
_cell_length_c 19.812(3)
_cell_angle_alpha 90.00
_cell_angle_beta 113.231(2)
_cell_angle_gamma 90.00
_cell_volume 6771.9(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 9757
_cell_measurement_theta_min 2.181
_cell_measurement_theta_max 30.156
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.20
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.723
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3440
_exptl_absorpt_coefficient_mu 1.721
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6263
_exptl_absorpt_correction_T_max 0.7247
_exptl_absorpt_process_details 'SADABS (Bruker, 2008)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX II'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 22515
_diffrn_reflns_av_R_equivalents 0.0218
_diffrn_reflns_av_sigmaI/netI 0.0221
_diffrn_reflns_limit_h_min -31
_diffrn_reflns_limit_h_max 32
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 2.18
_diffrn_reflns_theta_max 26.00
_reflns_number_total 6641
_reflns_number_gt 5518
_reflns_threshold_expression I>2\s(I)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 1.000 0.102 0.250 268 93 ' '
2 1.000 -0.102 0.750 268 93 ' '
3 0.500 0.398 0.750 268 93 ' '
4 0.500 0.602 0.250 268 93 ' '
_computing_data_collection 'APEX2 (Bruker, 2008)'
_computing_cell_refinement 'SAINT (Bruker, 2008)'
_computing_data_reduction 'SAINT (Bruker, 2008)'
_computing_structure_solution 'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
One of three crystallographycally independent t-Bu and both -CF3 groups
were found to be rotationally disordered over two or three positions
and were refined isotropically with restrained C-C and C-F distances.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6641
_refine_ls_number_parameters 344
_refine_ls_number_restraints 132
_refine_ls_R_factor_all 0.0682
_refine_ls_R_factor_gt 0.0588
_refine_ls_wR_factor_ref 0.2040
_refine_ls_wR_factor_gt 0.1959
_refine_ls_goodness_of_fit_ref 1.592
_refine_ls_restrained_S_all 1.617
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.35903(2) 0.25728(4) 0.07520(2) 0.0392(2) Uani 1 1 d . . .
Pd2 Pd 0.30489(2) 0.43288(4) 0.17614(3) 0.0424(2) Uani 1 1 d . . .
Pd3 Pd 0.18285(2) 0.46998(4) 0.08332(3) 0.0429(2) Uani 1 1 d . . .
Cl1 Cl 0.32577(9) 0.40485(14) 0.07632(10) 0.0533(5) Uani 1 1 d . . .
O11 O 0.3981(2) 0.2594(3) 0.1899(3) 0.0442(11) Uani 1 1 d . . .
C10 C 0.3140(3) 0.2959(5) 0.2041(3) 0.0401(15) Uani 1 1 d . . .
H10A H 0.2997 0.2828 0.2427 0.048 Uiso 1 1 calc R . .
H10B H 0.2937 0.2560 0.1609 0.048 Uiso 1 1 calc R . .
C11 C 0.3748(3) 0.2791(5) 0.2318(4) 0.0404(14) Uani 1 1 d . . .
C12 C 0.4099(3) 0.2801(7) 0.3134(4) 0.058(2) Uani 1 1 d . . .
C13 C 0.3958(5) 0.1868(9) 0.3427(7) 0.095(3) Uiso 1 1 d . . .
H13A H 0.3551 0.1773 0.3217 0.143 Uiso 1 1 calc R . .
H13B H 0.4093 0.1896 0.3964 0.143 Uiso 1 1 calc R . .
H13C H 0.4139 0.1348 0.3285 0.143 Uiso 1 1 calc R . .
C14 C 0.3992(6) 0.3557(11) 0.3542(8) 0.113(4) Uiso 1 1 d . . .
H14A H 0.3600 0.3538 0.3483 0.170 Uiso 1 1 calc R . .
H14B H 0.4068 0.4154 0.3357 0.170 Uiso 1 1 calc R . .
H14C H 0.4236 0.3493 0.4063 0.170 Uiso 1 1 calc R . .
C15 C 0.4733(5) 0.2763(8) 0.3269(6) 0.084(3) Uiso 1 1 d . . .
H15A H 0.4848 0.3368 0.3145 0.126 Uiso 1 1 calc R . .
H15B H 0.4792 0.2275 0.2961 0.126 Uiso 1 1 calc R . .
H15C H 0.4955 0.2621 0.3788 0.126 Uiso 1 1 calc R . .
O21 O 0.4007(2) 0.1349(4) 0.0824(3) 0.0487(12) Uani 1 1 d . . .
C20 C 0.3242(3) 0.0333(5) 0.0230(4) 0.0442(16) Uani 1 1 d . . .
H20A H 0.3004 0.0831 0.0303 0.053 Uiso 1 1 calc R . .
H20B H 0.3135 -0.0274 0.0376 0.053 Uiso 1 1 calc R . .
C21 C 0.3834(3) 0.0530(5) 0.0644(4) 0.0448(16) Uani 1 1 d . A .
C22 C 0.4284(3) -0.0218(5) 0.0849(4) 0.058(2) Uani 1 1 d D . .
C23 C 0.4039(6) -0.1203(8) 0.0613(7) 0.062(4) Uiso 0.58 1 d PD A 1
H23A H 0.4283 -0.1557 0.0434 0.093 Uiso 0.58 1 calc PR A 1
H23B H 0.3664 -0.1151 0.0220 0.093 Uiso 0.58 1 calc PR A 1
H23C H 0.4014 -0.1528 0.1034 0.093 Uiso 0.58 1 calc PR A 1
C24 C 0.4676(6) 0.0033(11) 0.0456(8) 0.082(5) Uiso 0.58 1 d PD A 1
H24A H 0.4485 -0.0098 -0.0070 0.123 Uiso 0.58 1 calc PR A 1
H24B H 0.5018 -0.0343 0.0662 0.123 Uiso 0.58 1 calc PR A 1
H24C H 0.4772 0.0697 0.0528 0.123 Uiso 0.58 1 calc PR A 1
C25 C 0.4597(6) -0.0160(11) 0.1683(6) 0.076(5) Uiso 0.58 1 d PD A 1
H25A H 0.4746 0.0472 0.1820 0.114 Uiso 0.58 1 calc PR A 1
H25B H 0.4907 -0.0610 0.1843 0.114 Uiso 0.58 1 calc PR A 1
H25C H 0.4340 -0.0305 0.1921 0.114 Uiso 0.58 1 calc PR A 1
C26 C 0.4887(6) 0.0195(13) 0.1103(9) 0.070(6) Uiso 0.42 1 d PD A 2
H26A H 0.4922 0.0539 0.0696 0.105 Uiso 0.42 1 calc PR A 2
H26B H 0.5161 -0.0314 0.1256 0.105 Uiso 0.42 1 calc PR A 2
H26C H 0.4955 0.0620 0.1518 0.105 Uiso 0.42 1 calc PR A 2
C27 C 0.4229(8) -0.0670(12) 0.1534(7) 0.071(6) Uiso 0.42 1 d PD A 2
H27A H 0.3960 -0.1186 0.1376 0.106 Uiso 0.42 1 calc PR A 2
H27B H 0.4098 -0.0200 0.1790 0.106 Uiso 0.42 1 calc PR A 2
H27C H 0.4595 -0.0908 0.1867 0.106 Uiso 0.42 1 calc PR A 2
C28 C 0.4224(7) -0.1006(11) 0.0284(8) 0.063(5) Uiso 0.42 1 d PD A 2
H28A H 0.4283 -0.0746 -0.0137 0.095 Uiso 0.42 1 calc PR A 2
H28B H 0.3848 -0.1277 0.0117 0.095 Uiso 0.42 1 calc PR A 2
H28C H 0.4504 -0.1493 0.0516 0.095 Uiso 0.42 1 calc PR A 2
O31 O 0.3609(2) 0.1421(4) -0.0795(2) 0.0551(13) Uani 1 1 d . . .
C30 C 0.3185(3) 0.2508(7) -0.0387(4) 0.068(3) Uani 1 1 d . . .
H30A H 0.2879 0.2041 -0.0532 0.082 Uiso 1 1 calc R . .
H30B H 0.3022 0.3124 -0.0588 0.082 Uiso 1 1 calc R . .
C31 C 0.3579(3) 0.2258(6) -0.0646(4) 0.0516(18) Uani 1 1 d . . .
C32 C 0.3951(3) 0.2964(6) -0.0828(4) 0.0567(19) Uani 1 1 d . . .
C33 C 0.3646(6) 0.3197(9) -0.1648(6) 0.098(4) Uani 1 1 d . . .
H33A H 0.3283 0.3483 -0.1733 0.147 Uiso 1 1 calc R . .
H33B H 0.3587 0.2622 -0.1938 0.147 Uiso 1 1 calc R . .
H33C H 0.3873 0.3633 -0.1796 0.147 Uiso 1 1 calc R . .
C34 C 0.4071(5) 0.3879(7) -0.0370(6) 0.081(3) Uani 1 1 d . . .
H34A H 0.4224 0.3725 0.0155 0.122 Uiso 1 1 calc R . .
H34B H 0.3722 0.4232 -0.0495 0.122 Uiso 1 1 calc R . .
H34C H 0.4343 0.4259 -0.0479 0.122 Uiso 1 1 calc R . .
C35 C 0.4523(4) 0.2514(7) -0.0707(7) 0.082(3) Uani 1 1 d . . .
H35A H 0.4750 0.2464 -0.0179 0.123 Uiso 1 1 calc R . .
H35B H 0.4719 0.2902 -0.0937 0.123 Uiso 1 1 calc R . .
H35C H 0.4462 0.1889 -0.0927 0.123 Uiso 1 1 calc R . .
O41 O 0.2819(2) 0.4600(4) 0.2622(3) 0.0566(14) Uani 1 1 d . . .
O42 O 0.1900(3) 0.4821(4) 0.1949(3) 0.0609(15) Uani 1 1 d . . .
C41 C 0.2322(3) 0.4772(5) 0.2517(4) 0.0455(17) Uani 1 1 d . B .
C42 C 0.2215(2) 0.4996(4) 0.3202(4) 0.063(2) Uani 1 1 d D . .
F41 F 0.2059(4) 0.5882(4) 0.3210(5) 0.0642(12) Uiso 0.54 1 d PD B 3
F42 F 0.1803(3) 0.4445(6) 0.3236(5) 0.0642(12) Uiso 0.54 1 d PD B 3
F43 F 0.2675(3) 0.4828(6) 0.3811(4) 0.0642(12) Uiso 0.54 1 d PD B 3
F44 F 0.2559(4) 0.4557(8) 0.3812(6) 0.0642(12) Uiso 0.33 1 d PD B 4
F45 F 0.2321(5) 0.5918(5) 0.3308(7) 0.0642(12) Uiso 0.33 1 d PD B 4
F46 F 0.1687(3) 0.4844(9) 0.3133(7) 0.0642(12) Uiso 0.33 1 d PD B 4
F47 F 0.2110(12) 0.4230(13) 0.3519(15) 0.0642(12) Uiso 0.13 1 d PD B 7
F48 F 0.1763(8) 0.5560(17) 0.3024(16) 0.0642(12) Uiso 0.13 1 d PD B 7
F49 F 0.2649(8) 0.5446(19) 0.3710(12) 0.0642(12) Uiso 0.13 1 d PD B 7
O51 O 0.3019(3) 0.5795(4) 0.1554(4) 0.0648(15) Uani 1 1 d . . .
O52 O 0.2116(3) 0.6011(4) 0.0883(3) 0.0608(14) Uani 1 1 d . . .
C51 C 0.2602(4) 0.6247(6) 0.1211(4) 0.0522(18) Uani 1 1 d . C .
C52 C 0.2688(3) 0.7315(6) 0.1208(3) 0.065(2) Uani 1 1 d D . .
F51 F 0.2238(4) 0.7719(8) 0.0671(4) 0.091(3) Uiso 0.57 1 d PD C 5
F52 F 0.3131(4) 0.7582(8) 0.1083(6) 0.093(3) Uiso 0.57 1 d PD C 5
F53 F 0.2722(4) 0.7684(6) 0.1841(4) 0.062(2) Uiso 0.57 1 d PD C 5
F54 F 0.2460(5) 0.7764(9) 0.0573(5) 0.085(4) Uiso 0.43 1 d PD C 6
F55 F 0.3243(3) 0.7504(10) 0.1482(7) 0.090(4) Uiso 0.43 1 d PD C 6
F56 F 0.2492(5) 0.7702(8) 0.1678(5) 0.058(3) Uiso 0.43 1 d PD C 6
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0391(3) 0.0461(4) 0.0333(3) -0.0053(2) 0.0153(2) 0.0018(2)
Pd2 0.0461(3) 0.0343(3) 0.0505(3) -0.0046(2) 0.0230(3) -0.0020(2)
Pd3 0.0496(4) 0.0452(4) 0.0376(3) -0.0023(2) 0.0210(2) -0.0024(2)
Cl1 0.0673(12) 0.0462(10) 0.0571(10) 0.0063(8) 0.0358(9) 0.0094(9)
O11 0.049(3) 0.043(3) 0.041(2) -0.006(2) 0.019(2) 0.002(2)
C10 0.050(4) 0.036(4) 0.035(3) 0.000(3) 0.018(3) -0.005(3)
C11 0.053(4) 0.030(3) 0.042(3) -0.005(3) 0.022(3) -0.001(3)
C12 0.059(5) 0.072(6) 0.039(4) -0.006(4) 0.016(3) 0.009(4)
O21 0.049(3) 0.047(3) 0.050(3) -0.016(2) 0.020(2) 0.000(2)
C20 0.053(4) 0.045(4) 0.042(4) -0.008(3) 0.026(3) -0.005(3)
C21 0.050(4) 0.055(5) 0.032(3) -0.007(3) 0.019(3) 0.005(3)
C22 0.064(5) 0.049(5) 0.066(5) -0.001(4) 0.031(4) 0.010(4)
O31 0.070(3) 0.062(4) 0.034(2) -0.004(2) 0.022(2) 0.015(3)
C30 0.044(4) 0.124(8) 0.029(3) 0.024(4) 0.005(3) -0.025(5)
C31 0.060(5) 0.045(4) 0.039(4) -0.009(3) 0.009(3) 0.012(4)
C32 0.057(5) 0.055(5) 0.057(4) 0.003(4) 0.022(4) -0.004(4)
C33 0.127(10) 0.106(10) 0.059(6) 0.021(6) 0.035(6) 0.012(8)
C34 0.100(8) 0.059(6) 0.099(7) 0.003(5) 0.055(6) -0.006(5)
C35 0.069(6) 0.072(7) 0.113(9) 0.012(6) 0.045(6) 0.001(5)
O41 0.067(4) 0.057(3) 0.055(3) -0.022(3) 0.033(3) -0.001(3)
O42 0.073(4) 0.076(4) 0.046(3) -0.007(3) 0.036(3) 0.007(3)
C41 0.064(5) 0.036(4) 0.040(4) 0.001(3) 0.024(3) -0.002(3)
C42 0.092(6) 0.041(4) 0.055(4) -0.005(4) 0.031(4) 0.006(4)
O51 0.070(4) 0.034(3) 0.090(4) -0.003(3) 0.031(3) -0.008(3)
O52 0.086(4) 0.033(3) 0.063(3) -0.006(2) 0.028(3) 0.001(3)
C51 0.067(5) 0.044(4) 0.048(4) -0.005(3) 0.026(4) 0.003(4)
C52 0.087(7) 0.049(5) 0.056(5) -0.012(4) 0.026(5) 0.003(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 O21 2.035(5) . ?
Pd1 C30 2.082(7) . ?
Pd1 O11 2.091(5) . ?
Pd1 Cl1 2.286(2) . ?
Pd2 C10 2.027(7) . ?
Pd2 O41 2.054(5) . ?
Pd2 O51 2.134(6) . ?
Pd2 Cl1 2.2830(18) . ?
Pd2 Pd3 3.0201(8) . ?
Pd3 O31 1.949(6) 7 ?
Pd3 O52 2.009(6) . ?
Pd3 C20 2.041(6) 7 ?
Pd3 O42 2.152(5) . ?
O11 C11 1.237(8) . ?
C10 C11 1.474(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.510(10) . ?
C12 C14 1.442(15) . ?
C12 C13 1.556(15) . ?
C12 C15 1.562(14) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O21 C21 1.257(9) . ?
C20 C21 1.458(10) . ?
C20 Pd3 2.041(6) 7 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.516(11) . ?
C22 C25 1.529(9) . ?
C22 C23 1.543(9) . ?
C22 C24 1.548(9) . ?
C22 C28 1.554(9) . ?
C22 C26 1.561(9) . ?
C22 C27 1.560(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O31 C31 1.243(9) . ?
O31 Pd3 1.949(6) 7 ?
C30 C31 1.362(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.539(12) . ?
C32 C34 1.554(13) . ?
C32 C35 1.548(13) . ?
C32 C33 1.536(12) . ?
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 1.250(9) . ?
O42 C41 1.224(9) . ?
C41 C42 1.524(11) . ?
C42 F41 1.334(6) . ?
C42 F46 1.342(6) . ?
C42 F47 1.343(7) . ?
C42 F44 1.342(6) . ?
C42 F43 1.344(6) . ?
C42 F49 1.345(7) . ?
C42 F45 1.348(6) . ?
C42 F48 1.352(7) . ?
C42 F42 1.352(6) . ?
O51 C51 1.215(10) . ?
O52 C51 1.216(10) . ?
C51 C52 1.545(12) . ?
C52 F54 1.326(7) . ?
C52 F52 1.327(6) . ?
C52 F53 1.331(6) . ?
C52 F56 1.344(6) . ?
C52 F55 1.353(7) . ?
C52 F51 1.360(6) . ?
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
_geom_angle_publ_flag
O21 Pd1 C30 93.8(3) . . ?
O21 Pd1 O11 85.38(19) . . ?
C30 Pd1 O11 177.9(3) . . ?
O21 Pd1 Cl1 171.01(15) . . ?
C30 Pd1 Cl1 91.1(3) . . ?
O11 Pd1 Cl1 89.94(14) . . ?
C10 Pd2 O41 89.8(2) . . ?
C10 Pd2 O51 174.8(3) . . ?
O41 Pd2 O51 88.5(2) . . ?
C10 Pd2 Cl1 91.43(19) . . ?
O41 Pd2 Cl1 176.96(17) . . ?
O51 Pd2 Cl1 90.51(18) . . ?
C10 Pd2 Pd3 108.56(19) . . ?
O41 Pd2 Pd3 83.84(17) . . ?
O51 Pd2 Pd3 76.12(17) . . ?
Cl1 Pd2 Pd3 93.14(5) . . ?
O31 Pd3 O52 166.1(2) 7 . ?
O31 Pd3 C20 97.3(2) 7 7 ?
O52 Pd3 C20 87.3(3) . 7 ?
O31 Pd3 O42 85.4(2) 7 . ?
O52 Pd3 O42 89.7(2) . . ?
C20 Pd3 O42 176.7(3) 7 . ?
O31 Pd3 Pd2 109.57(16) 7 . ?
O52 Pd3 Pd2 81.55(18) . . ?
C20 Pd3 Pd2 105.6(2) 7 . ?
O42 Pd3 Pd2 75.18(17) . . ?
Pd2 Cl1 Pd1 113.00(8) . . ?
C11 O11 Pd1 125.3(5) . . ?
C11 C10 Pd2 104.6(4) . . ?
C11 C10 H10A 110.8 . . ?
Pd2 C10 H10A 110.8 . . ?
C11 C10 H10B 110.8 . . ?
Pd2 C10 H10B 110.8 . . ?
H10A C10 H10B 108.9 . . ?
O11 C11 C10 121.5(6) . . ?
O11 C11 C12 118.2(7) . . ?
C10 C11 C12 120.1(6) . . ?
C14 C12 C11 116.0(9) . . ?
C14 C12 C13 108.0(9) . . ?
C11 C12 C13 105.1(7) . . ?
C14 C12 C15 110.6(9) . . ?
C11 C12 C15 109.5(7) . . ?
C13 C12 C15 107.1(8) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C21 O21 Pd1 131.5(5) . . ?
C21 C20 Pd3 103.3(4) . 7 ?
C21 C20 H20A 111.1 . . ?
Pd3 C20 H20A 111.1 7 . ?
C21 C20 H20B 111.1 . . ?
Pd3 C20 H20B 111.1 7 . ?
H20A C20 H20B 109.1 . . ?
O21 C21 C20 121.3(7) . . ?
O21 C21 C22 115.5(6) . . ?
C20 C21 C22 123.1(7) . . ?
C21 C22 C25 106.1(8) . . ?
C21 C22 C23 112.4(8) . . ?
C25 C22 C23 111.0(6) . . ?
C21 C22 C24 106.9(9) . . ?
C25 C22 C24 110.8(5) . . ?
C23 C22 C24 109.5(5) . . ?
C21 C22 C28 118.1(9) . . ?
C21 C22 C26 112.9(9) . . ?
C28 C22 C26 108.0(6) . . ?
C21 C22 C27 101.6(9) . . ?
C28 C22 C27 108.0(6) . . ?
C26 C22 C27 107.5(6) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
C22 C26 H26A 109.5 . . ?
C22 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C22 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C22 C27 H27A 109.5 . . ?
C22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C22 C28 H28A 109.5 . . ?
C22 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C22 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 O31 Pd3 135.4(6) . 7 ?
C31 C30 Pd1 106.6(5) . . ?
C31 C30 H30A 110.4 . . ?
Pd1 C30 H30A 110.4 . . ?
C31 C30 H30B 110.4 . . ?
Pd1 C30 H30B 110.4 . . ?
H30A C30 H30B 108.6 . . ?
O31 C31 C30 118.0(8) . . ?
O31 C31 C32 118.3(7) . . ?
C30 C31 C32 123.5(8) . . ?
C31 C32 C34 114.6(7) . . ?
C31 C32 C35 110.1(7) . . ?
C34 C32 C35 107.5(8) . . ?
C31 C32 C33 106.2(8) . . ?
C34 C32 C33 109.7(8) . . ?
C35 C32 C33 108.6(8) . . ?
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 Pd2 121.3(5) . . ?
C41 O42 Pd3 128.5(5) . . ?
O42 C41 O41 131.0(7) . . ?
O42 C41 C42 113.3(7) . . ?
O41 C41 C42 115.7(6) . . ?
F46 C42 F44 108.0(6) . . ?
F41 C42 F43 109.1(5) . . ?
F47 C42 F49 107.9(7) . . ?
F46 C42 F45 108.2(6) . . ?
F44 C42 F45 107.2(6) . . ?
F47 C42 F48 107.2(7) . . ?
F49 C42 F48 107.1(7) . . ?
F41 C42 F42 107.7(5) . . ?
F43 C42 F42 107.1(5) . . ?
F41 C42 C41 111.9(6) . . ?
F46 C42 C41 114.4(8) . . ?
F47 C42 C41 112.7(14) . . ?
F44 C42 C41 114.3(8) . . ?
F43 C42 C41 110.6(7) . . ?
F49 C42 C41 111.9(14) . . ?
F45 C42 C41 104.3(8) . . ?
F48 C42 C41 109.7(14) . . ?
F42 C42 C41 110.4(6) . . ?
C51 O51 Pd2 126.1(6) . . ?
C51 O52 Pd3 125.0(6) . . ?
O52 C51 O51 131.3(8) . . ?
O52 C51 C52 113.2(7) . . ?
O51 C51 C52 115.5(7) . . ?
F52 C52 F53 108.8(6) . . ?
F54 C52 F56 108.0(6) . . ?
F54 C52 F55 106.8(6) . . ?
F56 C52 F55 106.0(6) . . ?
F52 C52 F51 105.8(6) . . ?
F53 C52 F51 106.6(6) . . ?
F52 C52 C51 115.0(7) . . ?
F53 C52 C51 110.2(7) . . ?
F56 C52 C51 108.1(7) . . ?
F55 C52 C51 109.2(8) . . ?
F51 C52 C51 110.0(8) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 2.015
_refine_diff_density_min -1.147
_refine_diff_density_rms 0.182
data_6b
_database_code_depnum_ccdc_archive 'CCDC 893513'
#TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1351060002.6both_new.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C32 H44 Cl4 F12 O12 Pd6'
_chemical_formula_sum 'C32 H44 Cl4 F12 O12 Pd6'
_chemical_formula_weight 1628.87
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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 9.1569(14)
_cell_length_b 14.474(2)
_cell_length_c 19.072(3)
_cell_angle_alpha 90.00
_cell_angle_beta 95.500(2)
_cell_angle_gamma 90.00
_cell_volume 2516.0(7)
_cell_formula_units_Z 2
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 6906
_cell_measurement_theta_min 2.145
_cell_measurement_theta_max 29.717
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.20
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.150
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1568
_exptl_absorpt_coefficient_mu 2.407
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6446
_exptl_absorpt_correction_T_max 0.7141
_exptl_absorpt_process_details 'SADABS (Bruker, 2004)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART APEX II'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 17558
_diffrn_reflns_av_R_equivalents 0.0421
_diffrn_reflns_av_sigmaI/netI 0.0405
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 26.00
_reflns_number_total 4932
_reflns_number_gt 3722
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'APEX2 (Bruker, 2008)'
_computing_cell_refinement 'SAINT (Bruker, 2008)'
_computing_data_reduction 'SAINT (Bruker, 2008)'
_computing_structure_solution 'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material 'SHELXTL (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
All fluorine atoms were refined isotropically with restrained C-F
distances.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+7.8764P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4932
_refine_ls_number_parameters 298
_refine_ls_number_restraints 60
_refine_ls_R_factor_all 0.0740
_refine_ls_R_factor_gt 0.0497
_refine_ls_wR_factor_ref 0.1442
_refine_ls_wR_factor_gt 0.1314
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_restrained_S_all 1.084
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.0363(3) 0.0321(3) 0.0294(3) 0.0069(2) 0.0069(2) 0.0027(2)
Pd2 0.0387(3) 0.0297(3) 0.0271(3) 0.0028(2) 0.0070(2) 0.0034(2)
Pd3 0.0390(3) 0.0285(3) 0.0350(3) 0.0049(2) 0.0099(2) 0.0010(2)
Cl1 0.0498(11) 0.0343(9) 0.0302(9) 0.0010(7) 0.0068(8) 0.0067(8)
Cl2 0.0544(12) 0.0328(9) 0.0358(10) 0.0002(7) 0.0142(8) -0.0017(8)
O11 0.047(3) 0.031(3) 0.048(3) 0.004(2) 0.015(3) -0.002(2)
O12 0.052(4) 0.028(3) 0.061(4) 0.003(3) 0.020(3) 0.003(3)
C11 0.057(5) 0.033(4) 0.041(4) 0.003(3) 0.017(4) 0.009(4)
C12 0.054(5) 0.043(5) 0.059(6) 0.004(4) 0.014(4) 0.005(4)
O21 0.056(4) 0.050(3) 0.026(3) 0.003(2) 0.011(3) 0.003(3)
O22 0.044(3) 0.045(3) 0.037(3) 0.008(2) 0.003(2) -0.003(3)
C21 0.052(5) 0.033(4) 0.032(4) 0.005(3) 0.005(4) 0.006(3)
C22 0.067(6) 0.046(5) 0.040(5) 0.010(4) 0.004(4) -0.004(4)
O31 0.037(3) 0.048(3) 0.035(3) 0.008(2) 0.003(2) -0.003(2)
C30 0.041(4) 0.032(4) 0.036(4) 0.003(3) 0.011(3) 0.009(3)
C31 0.052(5) 0.033(4) 0.032(4) -0.001(3) 0.010(4) 0.004(3)
C32 0.051(5) 0.056(5) 0.027(4) 0.002(3) 0.006(4) -0.011(4)
C33 0.068(7) 0.085(8) 0.040(5) 0.008(5) -0.001(5) 0.030(6)
C34 0.075(7) 0.081(8) 0.048(6) -0.006(5) 0.000(5) -0.028(6)
C35 0.065(6) 0.066(6) 0.031(4) -0.006(4) 0.008(4) -0.011(5)
O41 0.042(3) 0.042(3) 0.038(3) 0.003(2) 0.011(2) 0.000(2)
C40 0.047(5) 0.035(4) 0.028(4) -0.006(3) 0.010(3) -0.007(3)
C41 0.047(5) 0.035(4) 0.029(4) 0.000(3) 0.012(3) 0.000(3)
C42 0.043(5) 0.041(4) 0.046(5) -0.003(4) 0.010(4) -0.006(4)
C43 0.063(6) 0.043(5) 0.103(9) -0.009(5) 0.013(6) -0.004(5)
C44 0.070(7) 0.065(6) 0.063(6) -0.016(5) 0.002(5) -0.024(5)
C45 0.050(5) 0.063(6) 0.063(6) 0.014(5) 0.012(5) -0.015(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 . ?
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
_geom_angle_publ_flag
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 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 2.333
_refine_diff_density_min -0.994
_refine_diff_density_rms 0.192