data_04src0896r

_exptl_special_details
;
 There is one molecule of chloroform in the asymmetric unit. This is disordered
 (and modelled) over 4 main sites. A side effect of this is that there are some
 closer intermolecular contacts than expected, which are unlikely to truly exist
 in the actual crystal. 
;
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 Dr. R. B. Bedford
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C52 H47 O3 P4 Pd, F6 Sb, C H Cl3'
_chemical_formula_sum
 'C53 H48 Cl3 F6 O3 P4 Pd Sb'
_chemical_formula_weight          1305.29
 
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'
 'P'  'P'   0.1023   0.0942
 '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'
 'Sb'  'Sb'  -0.5866   1.5461
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/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                    12.677(4)
_cell_length_b                    26.381(11)
_cell_length_c                    16.334(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  95.89(3)
_cell_angle_gamma                 90.00
_cell_volume                      5434(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     8435
_cell_measurement_theta_min       2.910
_cell_measurement_theta_max       27.485
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.17
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.596
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2608
_exptl_absorpt_coefficient_mu     1.156
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8277
_exptl_absorpt_correction_T_max   0.9339
_exptl_absorpt_process_details       'SADABS V2.10 (Sheldrick, G.M., 2003)'

_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             46944
_diffrn_reflns_av_R_equivalents   0.0919
_diffrn_reflns_av_sigmaI/netI     0.1176
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -34
_diffrn_reflns_limit_k_max        34
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          2.94
_diffrn_reflns_theta_max          27.48
_reflns_number_total              12362
_reflns_number_gt                 7741
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997a)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997b)' 
_computing_molecular_graphics     'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0894P)²+41.1500P] where P=(Fo²+2Fc²)/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          12362
_refine_ls_number_parameters      753
_refine_ls_number_restraints      225
_refine_ls_R_factor_all           0.1514
_refine_ls_R_factor_gt            0.0951
_refine_ls_wR_factor_ref          0.2409
_refine_ls_wR_factor_gt           0.2105
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.041
_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 0.69957(4) 0.34949(2) 0.07567(4) 0.02688(17) Uani 1 1 d . . .
C1 C 0.6834(6) 0.4327(3) 0.1962(6) 0.035(2) Uani 1 1 d . . .
C2 C 0.7016(6) 0.4239(3) 0.1173(5) 0.0303(18) Uani 1 1 d . . .
C3 C 0.7310(6) 0.4660(3) 0.0717(6) 0.0334(19) Uani 1 1 d . . .
H3 H 0.7405 0.4619 0.0151 0.040 Uiso 1 1 calc R . .
C4 C 0.7463(7) 0.5131(3) 0.1082(6) 0.041(2) Uani 1 1 d . . .
H4 H 0.7678 0.5410 0.0772 0.049 Uiso 1 1 calc R . .
C5 C 0.7304(7) 0.5193(4) 0.1894(6) 0.043(2) Uani 1 1 d . . .
H5 H 0.7422 0.5515 0.2149 0.052 Uiso 1 1 calc R . .
C6 C 0.6973(7) 0.4790(3) 0.2344(6) 0.042(2) Uani 1 1 d . . .
H6 H 0.6845 0.4832 0.2903 0.050 Uiso 1 1 calc R . .
C7 C 0.4635(7) 0.3171(4) 0.2726(6) 0.040(2) Uani 1 1 d . . .
C8 C 0.4704(8) 0.3498(4) 0.3368(7) 0.051(3) Uani 1 1 d . . .
H8 H 0.5184 0.3775 0.3388 0.061 Uiso 1 1 calc R . .
C9 C 0.4053(9) 0.3421(5) 0.4008(7) 0.065(3) Uani 1 1 d . . .
H9 H 0.4086 0.3648 0.4461 0.078 Uiso 1 1 calc R . .
C10 C 0.3375(8) 0.3018(5) 0.3967(7) 0.061(3) Uani 1 1 d . . .
H10 H 0.2947 0.2959 0.4402 0.073 Uiso 1 1 calc R . .
C11 C 0.3310(8) 0.2702(4) 0.3310(8) 0.059(3) Uani 1 1 d . . .
H11 H 0.2816 0.2430 0.3281 0.071 Uiso 1 1 calc R . .
C12 C 0.3943(7) 0.2768(4) 0.2688(7) 0.047(3) Uani 1 1 d . . .
H12 H 0.3905 0.2539 0.2237 0.056 Uiso 1 1 calc R . .
C13 C 0.7991(7) 0.3059(3) 0.2993(5) 0.036(2) Uani 1 1 d . . .
C14 C 0.8657(7) 0.2699(4) 0.2743(6) 0.043(2) Uani 1 1 d . . .
H14 H 0.8392 0.2437 0.2379 0.051 Uiso 1 1 calc R . .
C15 C 0.9727(7) 0.2718(5) 0.3027(7) 0.058(3) Uani 1 1 d . . .
H15 H 1.0208 0.2476 0.2845 0.070 Uiso 1 1 calc R . .
C16 C 1.0085(8) 0.3093(5) 0.3576(7) 0.059(3) Uani 1 1 d . . .
H16 H 1.0810 0.3099 0.3791 0.071 Uiso 1 1 calc R . .
C17 C 0.9415(9) 0.3456(4) 0.3815(7) 0.060(3) Uani 1 1 d . . .
H17 H 0.9682 0.3719 0.4177 0.072 Uiso 1 1 calc R . .
C18 C 0.8345(8) 0.3444(3) 0.3532(5) 0.038(2) Uani 1 1 d . . .
H18 H 0.7869 0.3692 0.3703 0.046 Uiso 1 1 calc R . .
O1 O 0.6518(5) 0.3930(2) 0.2446(4) 0.0356(14) Uani 1 1 d . . .
O2 O 0.5205(4) 0.3231(2) 0.2042(4) 0.0364(14) Uani 1 1 d . . .
O3 O 0.6908(4) 0.3022(2) 0.2728(4) 0.0325(13) Uani 1 1 d . . .
P1 P 0.64061(16) 0.33864(8) 0.20094(15) 0.0303(5) Uani 1 1 d . . .
C21 C 0.9196(6) 0.2814(3) 0.0506(6) 0.0316(19) Uani 1 1 d . . .
H21A H 0.9873 0.2782 0.0256 0.038 Uiso 1 1 calc R . .
H21B H 0.9293 0.2656 0.1058 0.038 Uiso 1 1 calc R . .
C22 C 0.8326(6) 0.2534(3) -0.0027(6) 0.036(2) Uani 1 1 d . . .
H22A H 0.8457 0.2165 0.0019 0.043 Uiso 1 1 calc R . .
H22B H 0.8355 0.2632 -0.0610 0.043 Uiso 1 1 calc R . .
C23 C 0.6162(6) 0.2636(3) -0.0711(5) 0.0331(19) Uani 1 1 d . . .
H23A H 0.6395 0.2352 -0.1045 0.040 Uiso 1 1 calc R . .
H23B H 0.5417 0.2575 -0.0607 0.040 Uiso 1 1 calc R . .
C24 C 0.6241(6) 0.3131(3) -0.1171(5) 0.035(2) Uani 1 1 d . . .
H24A H 0.5732 0.3131 -0.1674 0.042 Uiso 1 1 calc R . .
H24B H 0.6965 0.3171 -0.1339 0.042 Uiso 1 1 calc R . .
C25 C 0.9854(6) 0.3713(3) 0.1417(5) 0.0309(18) Uani 1 1 d . . .
C26 C 0.9642(7) 0.4124(3) 0.1888(6) 0.037(2) Uani 1 1 d . . .
H26 H 0.8965 0.4281 0.1811 0.044 Uiso 1 1 calc R . .
C27 C 1.0398(7) 0.4309(3) 0.2470(6) 0.039(2) Uani 1 1 d . . .
H27 H 1.0246 0.4597 0.2788 0.047 Uiso 1 1 calc R . .
C28 C 1.1379(7) 0.4081(4) 0.2596(6) 0.044(2) Uani 1 1 d . . .
H28 H 1.1905 0.4214 0.2994 0.053 Uiso 1 1 calc R . .
C29 C 1.1590(6) 0.3671(4) 0.2157(6) 0.040(2) Uani 1 1 d . . .
H29 H 1.2257 0.3507 0.2265 0.049 Uiso 1 1 calc R . .
C30 C 1.0862(6) 0.3483(4) 0.1556(6) 0.041(2) Uani 1 1 d . . .
H30 H 1.1034 0.3199 0.1236 0.050 Uiso 1 1 calc R . .
C31 C 0.9317(5) 0.3779(3) -0.0318(5) 0.0286(18) Uani 1 1 d . . .
C32 C 0.9462(6) 0.3507(3) -0.1022(6) 0.0339(19) Uani 1 1 d . . .
H32 H 0.9367 0.3150 -0.1027 0.041 Uiso 1 1 calc R . .
C33 C 0.9745(7) 0.3751(4) -0.1720(6) 0.040(2) Uani 1 1 d . . .
H33 H 0.9850 0.3560 -0.2198 0.048 Uiso 1 1 calc R . .
C34 C 0.9873(7) 0.4259(4) -0.1724(6) 0.043(2) Uani 1 1 d . . .
H34 H 1.0056 0.4427 -0.2204 0.052 Uiso 1 1 calc R . .
C35 C 0.9734(7) 0.4530(3) -0.1021(6) 0.043(2) Uani 1 1 d . . .
H35 H 0.9833 0.4887 -0.1026 0.051 Uiso 1 1 calc R . .
C36 C 0.9459(6) 0.4304(3) -0.0312(6) 0.039(2) Uani 1 1 d . . .
H36 H 0.9368 0.4499 0.0165 0.047 Uiso 1 1 calc R . .
C37 C 0.6628(6) 0.2135(3) 0.0856(5) 0.0317(19) Uani 1 1 d . . .
C38 C 0.5576(7) 0.2084(4) 0.1016(6) 0.043(2) Uani 1 1 d . . .
H38 H 0.5069 0.2335 0.0832 0.051 Uiso 1 1 calc R . .
C39 C 0.5270(8) 0.1664(4) 0.1446(7) 0.051(3) Uani 1 1 d . . .
H39 H 0.4552 0.1632 0.1556 0.061 Uiso 1 1 calc R . .
C40 C 0.5990(8) 0.1291(4) 0.1716(6) 0.046(2) Uani 1 1 d . . .
H40 H 0.5767 0.1000 0.1994 0.055 Uiso 1 1 calc R . .
C41 C 0.7043(8) 0.1351(4) 0.1576(7) 0.052(3) Uani 1 1 d . . .
H41 H 0.7548 0.1101 0.1772 0.063 Uiso 1 1 calc R . .
C42 C 0.7364(7) 0.1761(3) 0.1160(6) 0.041(2) Uani 1 1 d . . .
H42 H 0.8091 0.1796 0.1074 0.049 Uiso 1 1 calc R . .
C43 C 0.4507(6) 0.3588(3) -0.0493(6) 0.036(2) Uani 1 1 d . . .
C44 C 0.3838(6) 0.3626(3) -0.1214(6) 0.040(2) Uani 1 1 d . . .
H44 H 0.4116 0.3709 -0.1715 0.048 Uiso 1 1 calc R . .
C45 C 0.2764(7) 0.3543(3) -0.1204(6) 0.040(2) Uani 1 1 d . . .
H45 H 0.2307 0.3564 -0.1701 0.048 Uiso 1 1 calc R . .
C46 C 0.2365(7) 0.3432(5) -0.0498(7) 0.060(3) Uani 1 1 d . . .
H46 H 0.1622 0.3389 -0.0493 0.072 Uiso 1 1 calc R . .
C47 C 0.3025(9) 0.3380(7) 0.0225(9) 0.110(7) Uani 1 1 d . . .
H47 H 0.2755 0.3284 0.0724 0.131 Uiso 1 1 calc R . .
C48 C 0.4087(7) 0.3473(5) 0.0196(7) 0.073(4) Uani 1 1 d . . .
H48 H 0.4544 0.3454 0.0694 0.088 Uiso 1 1 calc R . .
C49 C 0.6101(6) 0.4239(3) -0.1048(5) 0.035(2) Uani 1 1 d . . .
C50 C 0.5421(7) 0.4644(3) -0.0924(6) 0.042(2) Uani 1 1 d . . .
H50 H 0.4835 0.4601 -0.0612 0.050 Uiso 1 1 calc R . .
C51 C 0.5624(7) 0.5108(4) -0.1266(7) 0.050(3) Uani 1 1 d . . .
H51 H 0.5158 0.5382 -0.1190 0.060 Uiso 1 1 calc R . .
C52 C 0.6453(7) 0.5189(4) -0.1704(7) 0.054(3) Uani 1 1 d . . .
H52 H 0.6568 0.5515 -0.1927 0.065 Uiso 1 1 calc R . .
C53 C 0.7139(7) 0.4790(4) -0.1826(6) 0.046(2) Uani 1 1 d . . .
H53 H 0.7720 0.4842 -0.2140 0.056 Uiso 1 1 calc R . .
C54 C 0.6973(7) 0.4318(3) -0.1488(6) 0.038(2) Uani 1 1 d . . .
H54 H 0.7453 0.4048 -0.1556 0.045 Uiso 1 1 calc R . .
P21 P 0.88723(15) 0.34818(8) 0.06076(14) 0.0288(5) Uani 1 1 d . . .
P22 P 0.70062(15) 0.26722(8) 0.02679(14) 0.0298(5) Uani 1 1 d . . .
P23 P 0.59418(16) 0.36543(8) -0.04969(14) 0.0303(5) Uani 1 1 d . . .
F1 F 0.1496(6) 0.2202(3) 0.0469(5) 0.091(2) Uani 1 1 d . . .
F2 F 0.2849(7) 0.1608(6) 0.1319(10) 0.202(7) Uani 1 1 d . . .
F3 F 0.1320(9) 0.2025(4) 0.2028(5) 0.129(4) Uani 1 1 d . . .
F4 F 0.1292(7) 0.1050(3) 0.1754(5) 0.098(3) Uani 1 1 d . . .
F5 F -0.0026(5) 0.1654(3) 0.0907(6) 0.102(3) Uani 1 1 d . . .
F6 F 0.1497(7) 0.1211(3) 0.0201(5) 0.100(3) Uani 1 1 d . . .
Sb1 Sb 0.14195(5) 0.16182(3) 0.11158(5) 0.0520(2) Uani 1 1 d . . .
C61 C 0.1682(9) 0.4956(5) 0.4725(6) 0.099(4) Uani 0.367(3) 1 d PDU A 1
H61 H 0.1377 0.4606 0.4726 0.119 Uiso 0.367(3) 1 calc PR A 1
Cl61 Cl 0.0810(8) 0.5345(4) 0.4131(7) 0.076(3) Uani 0.367(3) 1 d PDU A 1
Cl62 Cl 0.1829(11) 0.5184(5) 0.5726(6) 0.109(4) Uani 0.367(3) 1 d PDU A 1
Cl63 Cl 0.2878(9) 0.4933(5) 0.4302(7) 0.098(3) Uani 0.367(3) 1 d PDU A 1
C66 C 0.1470(14) 0.5003(8) 0.4906(10) 0.098(5) Uani 0.185(5) 1 d PDU B 2
H66 H 0.1236 0.4661 0.4693 0.117 Uiso 0.185(5) 1 calc PR B 2
Cl66 Cl 0.1068(14) 0.5455(6) 0.4174(13) 0.077(6) Uani 0.185(5) 1 d PDU B 2
Cl67 Cl 0.0892(18) 0.5125(8) 0.5803(12) 0.097(6) Uani 0.185(5) 1 d PDU B 2
Cl68 Cl 0.2840(14) 0.5008(10) 0.5099(13) 0.120(4) Uani 0.185(5) 1 d PDU B 2
C71 C 0.3470(14) 0.4918(4) 0.4960(6) 0.094(4) Uani 0.381(6) 1 d PDU C 3
H71 H 0.2716 0.4814 0.4987 0.113 Uiso 0.381(6) 1 calc PR C 3
Cl71 Cl 0.3610(10) 0.5539(3) 0.5302(5) 0.100(4) Uani 0.381(6) 1 d PDU C 3
Cl72 Cl 0.3752(12) 0.4864(3) 0.3950(5) 0.096(4) Uani 0.381(6) 1 d PDU C 3
Cl73 Cl 0.4269(13) 0.4522(4) 0.5595(6) 0.114(4) Uani 0.381(6) 1 d PDU C 3
C76 C 0.252(4) 0.4857(13) 0.481(3) 0.099(4) Uani 0.068(6) 1 d PDU D 4
H76 H 0.1826 0.4677 0.4729 0.118 Uiso 0.068(6) 1 calc PR D 4
Cl76 Cl 0.236(4) 0.5431(14) 0.530(3) 0.110(6) Uani 0.068(6) 1 d PDU D 4
Cl77 Cl 0.298(6) 0.497(2) 0.386(2) 0.091(7) Uani 0.068(6) 1 d PDU D 4
Cl78 Cl 0.343(6) 0.4485(18) 0.541(3) 0.093(6) Uani 0.068(6) 1 d PDU D 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 C2 2.077(8) . ?
Pd1 P1 2.267(3) . ?
Pd1 P22 2.313(2) . ?
Pd1 P23 2.365(2) . ?
Pd1 P21 2.416(2) . ?
C1 C2 1.353(12) . ?
C1 C6 1.375(12) . ?
C1 O1 1.395(10) . ?
C2 C3 1.407(12) . ?
C3 C4 1.384(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(13) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.353(14) . ?
C7 C12 1.376(13) . ?
C7 O2 1.401(11) . ?
C8 C9 1.411(14) . ?
C8 H8 0.9500 . ?
C9 C10 1.364(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.354(16) . ?
C10 H10 0.9500 . ?
C11 C12 1.369(14) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.363(13) . ?
C13 C18 1.387(12) . ?
C13 O3 1.400(9) . ?
C14 C15 1.389(12) . ?
C14 H14 0.9500 . ?
C15 C16 1.381(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.363(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(14) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
O1 P1 1.602(6) . ?
O2 P1 1.584(6) . ?
O3 P1 1.597(6) . ?
C21 C22 1.524(11) . ?
C21 P21 1.821(8) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 P22 1.825(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.515(12) . ?
C23 P22 1.833(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 P23 1.830(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.372(12) . ?
C25 C30 1.413(11) . ?
C25 P21 1.825(8) . ?
C26 C27 1.369(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.378(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.340(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(12) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.383(12) . ?
C31 C36 1.396(12) . ?
C31 P21 1.842(8) . ?
C32 C33 1.389(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.348(13) . ?
C33 H33 0.9500 . ?
C34 C35 1.379(13) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(13) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.393(11) . ?
C37 C42 1.412(12) . ?
C37 P22 1.805(9) . ?
C38 C39 1.387(13) . ?
C38 H38 0.9500 . ?
C39 C40 1.382(14) . ?
C39 H39 0.9500 . ?
C40 C41 1.386(13) . ?
C40 H40 0.9500 . ?
C41 C42 1.363(14) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.328(14) . ?
C43 C44 1.383(13) . ?
C43 P23 1.828(8) . ?
C44 C45 1.380(11) . ?
C44 H44 0.9500 . ?
C45 C46 1.339(14) . ?
C45 H45 0.9500 . ?
C46 C47 1.383(17) . ?
C46 H46 0.9500 . ?
C47 C48 1.373(14) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.394(12) . ?
C49 C50 1.401(12) . ?
C49 P23 1.808(9) . ?
C50 C51 1.379(13) . ?
C50 H50 0.9500 . ?
C51 C52 1.348(13) . ?
C51 H51 0.9500 . ?
C52 C53 1.392(13) . ?
C52 H52 0.9500 . ?
C53 C54 1.388(12) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
F1 Sb1 1.876(8) . ?
F2 Sb1 1.809(8) . ?
F3 Sb1 1.852(8) . ?
F4 Sb1 1.842(8) . ?
F5 Sb1 1.832(6) . ?
F6 Sb1 1.850(8) . ?
C61 Cl63 1.731(8) . ?
C61 Cl61 1.731(8) . ?
C61 Cl62 1.734(8) . ?
C61 H61 1.0000 . ?
C66 Cl66 1.730(12) . ?
C66 Cl68 1.733(9) . ?
C66 Cl67 1.733(9) . ?
C66 H66 1.0000 . ?
C71 Cl73 1.727(9) . ?
C71 Cl72 1.730(8) . ?
C71 Cl71 1.733(9) . ?
C71 H71 1.0000 . ?
C76 Cl78 1.734(9) . ?
C76 Cl76 1.734(12) . ?
C76 Cl77 1.735(9) . ?
C76 H76 1.0000 . ?
 
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
C2 Pd1 P1 79.5(3) . . ?
C2 Pd1 P22 178.4(2) . . ?
P1 Pd1 P22 101.95(8) . . ?
C2 Pd1 P23 95.9(2) . . ?
P1 Pd1 P23 126.48(8) . . ?
P22 Pd1 P23 83.73(8) . . ?
C2 Pd1 P21 93.8(2) . . ?
P1 Pd1 P21 120.55(8) . . ?
P22 Pd1 P21 84.90(7) . . ?
P23 Pd1 P21 112.94(8) . . ?
C2 C1 C6 123.9(9) . . ?
C2 C1 O1 119.9(8) . . ?
C6 C1 O1 116.1(8) . . ?
C1 C2 C3 116.7(8) . . ?
C1 C2 Pd1 118.4(6) . . ?
C3 C2 Pd1 124.5(6) . . ?
C4 C3 C2 120.9(9) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.8(9) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.3(9) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 118.3(9) . . ?
C1 C6 H6 120.9 . . ?
C5 C6 H6 120.9 . . ?
C8 C7 C12 121.2(10) . . ?
C8 C7 O2 123.3(9) . . ?
C12 C7 O2 115.4(9) . . ?
C7 C8 C9 119.1(11) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C10 C9 C8 119.3(11) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 120.3(10) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 121.2(11) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 H11 119.4 . . ?
C11 C12 C7 118.9(11) . . ?
C11 C12 H12 120.5 . . ?
C7 C12 H12 120.5 . . ?
C14 C13 C18 122.1(8) . . ?
C14 C13 O3 118.4(8) . . ?
C18 C13 O3 119.4(8) . . ?
C13 C14 C15 119.2(10) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 119.2(11) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C17 C16 C15 121.1(9) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.3(11) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 118.0(10) . . ?
C13 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C1 O1 P1 115.9(5) . . ?
C7 O2 P1 129.2(6) . . ?
C13 O3 P1 119.3(5) . . ?
O2 P1 O3 97.6(3) . . ?
O2 P1 O1 105.0(3) . . ?
O3 P1 O1 101.6(3) . . ?
O2 P1 Pd1 118.0(3) . . ?
O3 P1 Pd1 126.5(2) . . ?
O1 P1 Pd1 105.5(2) . . ?
C22 C21 P21 111.3(6) . . ?
C22 C21 H21A 109.4 . . ?
P21 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
P21 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
C21 C22 P22 112.5(6) . . ?
C21 C22 H22A 109.1 . . ?
P22 C22 H22A 109.1 . . ?
C21 C22 H22B 109.1 . . ?
P22 C22 H22B 109.1 . . ?
H22A C22 H22B 107.8 . . ?
C24 C23 P22 109.0(6) . . ?
C24 C23 H23A 109.9 . . ?
P22 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
P22 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
C23 C24 P23 108.8(6) . . ?
C23 C24 H24A 109.9 . . ?
P23 C24 H24A 109.9 . . ?
C23 C24 H24B 109.9 . . ?
P23 C24 H24B 109.9 . . ?
H24A C24 H24B 108.3 . . ?
C26 C25 C30 118.4(8) . . ?
C26 C25 P21 120.8(6) . . ?
C30 C25 P21 120.7(7) . . ?
C27 C26 C25 120.6(8) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C26 C27 C28 120.3(9) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 120.0(9) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 121.3(9) . . ?
C28 C29 H29 119.4 . . ?
C30 C29 H29 119.4 . . ?
C29 C30 C25 119.4(9) . . ?
C29 C30 H30 120.3 . . ?
C25 C30 H30 120.3 . . ?
C32 C31 C36 119.5(8) . . ?
C32 C31 P21 122.6(6) . . ?
C36 C31 P21 117.8(7) . . ?
C31 C32 C33 120.7(8) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C34 C33 C32 120.3(9) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.0(9) . . ?
C33 C34 H34 120.5 . . ?
C35 C34 H34 120.5 . . ?
C34 C35 C36 122.7(9) . . ?
C34 C35 H35 118.6 . . ?
C36 C35 H35 118.6 . . ?
C35 C36 C31 117.8(9) . . ?
C35 C36 H36 121.1 . . ?
C31 C36 H36 121.1 . . ?
C38 C37 C42 118.5(8) . . ?
C38 C37 P22 119.2(7) . . ?
C42 C37 P22 122.3(7) . . ?
C39 C38 C37 119.7(9) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C40 C39 C38 121.3(9) . . ?
C40 C39 H39 119.3 . . ?
C38 C39 H39 119.3 . . ?
C39 C40 C41 118.9(9) . . ?
C39 C40 H40 120.6 . . ?
C41 C40 H40 120.6 . . ?
C42 C41 C40 120.9(10) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C37 120.6(9) . . ?
C41 C42 H42 119.7 . . ?
C37 C42 H42 119.7 . . ?
C48 C43 C44 118.3(8) . . ?
C48 C43 P23 120.7(7) . . ?
C44 C43 P23 120.9(7) . . ?
C45 C44 C43 119.9(9) . . ?
C45 C44 H44 120.1 . . ?
C43 C44 H44 120.1 . . ?
C46 C45 C44 120.3(9) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C45 C46 C47 120.6(9) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C48 C47 C46 117.5(12) . . ?
C48 C47 H47 121.2 . . ?
C46 C47 H47 121.2 . . ?
C43 C48 C47 123.4(11) . . ?
C43 C48 H48 118.3 . . ?
C47 C48 H48 118.3 . . ?
C54 C49 C50 119.6(8) . . ?
C54 C49 P23 121.2(7) . . ?
C50 C49 P23 118.5(7) . . ?
C51 C50 C49 118.3(9) . . ?
C51 C50 H50 120.8 . . ?
C49 C50 H50 120.8 . . ?
C52 C51 C50 122.9(9) . . ?
C52 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
C51 C52 C53 119.2(9) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 H52 120.4 . . ?
C54 C53 C52 120.0(8) . . ?
C54 C53 H53 120.0 . . ?
C52 C53 H53 120.0 . . ?
C53 C54 C49 119.9(9) . . ?
C53 C54 H54 120.0 . . ?
C49 C54 H54 120.1 . . ?
C21 P21 C25 104.3(4) . . ?
C21 P21 C31 104.2(4) . . ?
C25 P21 C31 102.0(4) . . ?
C21 P21 Pd1 104.9(3) . . ?
C25 P21 Pd1 121.8(3) . . ?
C31 P21 Pd1 117.6(2) . . ?
C37 P22 C22 106.5(4) . . ?
C37 P22 C23 105.1(4) . . ?
C22 P22 C23 103.2(4) . . ?
C37 P22 Pd1 122.8(3) . . ?
C22 P22 Pd1 108.4(3) . . ?
C23 P22 Pd1 109.0(3) . . ?
C49 P23 C43 104.2(4) . . ?
C49 P23 C24 107.7(4) . . ?
C43 P23 C24 101.4(4) . . ?
C49 P23 Pd1 120.0(3) . . ?
C43 P23 Pd1 117.0(3) . . ?
C24 P23 Pd1 104.7(3) . . ?
F2 Sb1 F5 177.8(5) . . ?
F2 Sb1 F4 91.7(6) . . ?
F5 Sb1 F4 90.2(4) . . ?
F2 Sb1 F6 90.2(6) . . ?
F5 Sb1 F6 90.9(4) . . ?
F4 Sb1 F6 90.0(4) . . ?
F2 Sb1 F3 90.6(6) . . ?
F5 Sb1 F3 88.3(5) . . ?
F4 Sb1 F3 90.0(4) . . ?
F6 Sb1 F3 179.1(4) . . ?
F2 Sb1 F1 90.4(6) . . ?
F5 Sb1 F1 87.8(3) . . ?
F4 Sb1 F1 177.9(3) . . ?
F6 Sb1 F1 90.6(4) . . ?
F3 Sb1 F1 89.4(4) . . ?
Cl63 C61 Cl61 109.3(6) . . ?
Cl63 C61 Cl62 111.9(6) . . ?
Cl61 C61 Cl62 108.9(6) . . ?
Cl63 C61 H61 108.9 . . ?
Cl61 C61 H61 108.9 . . ?
Cl62 C61 H61 108.9 . . ?
Cl66 C66 Cl68 109.8(8) . . ?
Cl66 C66 Cl67 109.6(8) . . ?
Cl68 C66 Cl67 110.4(7) . . ?
Cl66 C66 H66 109.0 . . ?
Cl68 C66 H66 109.0 . . ?
Cl67 C66 H66 109.0 . . ?
Cl73 C71 Cl72 110.9(6) . . ?
Cl73 C71 Cl71 110.2(7) . . ?
Cl72 C71 Cl71 111.2(7) . . ?
Cl73 C71 H71 108.2 . . ?
Cl72 C71 H71 108.2 . . ?
Cl71 C71 H71 108.2 . . ?
Cl78 C76 Cl76 109.6(8) . . ?
Cl78 C76 Cl77 109.9(7) . . ?
Cl76 C76 Cl77 109.7(8) . . ?
Cl78 C76 H76 109.2 . . ?
Cl76 C76 H76 109.2 . . ?
Cl77 C76 H76 109.2 . . ?
 
_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    1.181
_refine_diff_density_min   -1.523
_refine_diff_density_rms    0.163
