# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_alpha_1
_database_code_depnum_ccdc_archive 'CCDC 1045817'
_audit_update_record             
;
2015-01-27 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
M-bis(hexafluoroacetylacetonato)(tris(o-tolyl)phosphino)palladium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H23 F12 O4 P Pd'
_chemical_formula_sum            'C31 H23 F12 O4 P Pd'
_chemical_formula_weight         824.86

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_int_tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.7139(18)
_cell_length_b                   11.2570(15)
_cell_length_c                   13.736(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.196(5)
_cell_angle_gamma                90.00
_cell_volume                     1573.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9743
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      25.00

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_type              RU-H3R
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            9743
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5424
_reflns_number_gt                5304
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    SIR92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'ORTEP-3 and PLUTON'
_computing_publication_material  SHELXL-97

_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)+(0.0300P)²+0.3323P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.032(12)
_refine_ls_number_reflns         5424
_refine_ls_number_parameters     445
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0186
_refine_ls_wR_factor_ref         0.0469
_refine_ls_wR_factor_gt          0.0464
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
C1 C 0.6888(2) 0.7509(2) 1.05145(17) 0.0167(5) Uani 1 1 d . . .
C2 C 0.71027(17) 0.8206(3) 0.96193(13) 0.0107(4) Uani 1 1 d . . .
C3 C 0.6724(2) 0.9396(2) 0.95069(17) 0.0119(4) Uani 1 1 d . . .
H3 H 0.6324 0.9721 0.9957 0.014 Uiso 1 1 calc R . .
C4 C 0.6925(2) 1.0113(2) 0.87471(16) 0.0115(5) Uani 1 1 d . . .
C5 C 0.6533(2) 1.1428(2) 0.87154(18) 0.0164(5) Uani 1 1 d . . .
C6 C 1.0059(3) 0.5091(2) 0.87034(18) 0.0202(5) Uani 1 1 d . . .
C7 C 0.8816(2) 0.5737(2) 0.80786(16) 0.0128(4) Uani 1 1 d . . .
C8 C 0.7630(2) 0.5199(2) 0.79399(18) 0.0171(5) Uani 1 1 d . . .
H8 H 0.7636 0.4425 0.8179 0.021 Uiso 1 1 calc R . .
C9 C 0.6374(2) 0.5739(2) 0.74519(18) 0.0172(5) Uani 1 1 d . . .
C10 C 0.5200(3) 0.5025(3) 0.7561(2) 0.0275(7) Uani 1 1 d . . .
C11 C 0.8311(2) 1.05348(19) 0.63719(16) 0.0110(4) Uani 1 1 d . . .
C12 C 0.9219(2) 1.1465(2) 0.66537(17) 0.0139(5) Uani 1 1 d . . .
H12 H 1.0108 1.1300 0.6952 0.017 Uiso 1 1 calc R . .
C13 C 0.8796(2) 1.2635(2) 0.64885(18) 0.0183(5) Uani 1 1 d . . .
H13 H 0.9400 1.3253 0.6678 0.022 Uiso 1 1 calc R . .
C14 C 0.7475(3) 1.2880(2) 0.60422(18) 0.0212(5) Uani 1 1 d . . .
H14 H 0.7193 1.3665 0.5934 0.025 Uiso 1 1 calc R . .
C15 C 0.6570(3) 1.1964(2) 0.57553(19) 0.0197(5) Uani 1 1 d . . .
H15 H 0.5686 1.2142 0.5446 0.024 Uiso 1 1 calc R . .
C16 C 0.6962(2) 1.0777(2) 0.59226(16) 0.0140(5) Uani 1 1 d . . .
C17 C 0.5927(2) 0.9814(2) 0.55984(19) 0.0206(5) Uani 1 1 d . . .
H17A H 0.5953 0.9464 0.4967 0.031 Uiso 1 1 calc R . .
H17B H 0.5075 1.0153 0.5503 0.031 Uiso 1 1 calc R . .
H17C H 0.6097 0.9213 0.6120 0.031 Uiso 1 1 calc R . .
C18 C 0.83270(17) 0.8231(3) 0.53860(14) 0.0111(4) Uani 1 1 d . . .
C19 C 0.7864(2) 0.7073(2) 0.53857(18) 0.0152(5) Uani 1 1 d . . .
H19 H 0.7825 0.6740 0.5995 0.018 Uiso 1 1 calc R . .
C20 C 0.7463(2) 0.6412(2) 0.44917(19) 0.0191(5) Uani 1 1 d . . .
H20 H 0.7168 0.5637 0.4502 0.023 Uiso 1 1 calc R . .
C21 C 0.7504(2) 0.6913(2) 0.35828(18) 0.0183(5) Uani 1 1 d . . .
H21 H 0.7233 0.6478 0.2978 0.022 Uiso 1 1 calc R . .
C22 C 0.7951(2) 0.8063(2) 0.35795(16) 0.0165(6) Uani 1 1 d . . .
H22 H 0.7953 0.8394 0.2960 0.020 Uiso 1 1 calc R . .
C23 C 0.8397(2) 0.8746(2) 0.44658(17) 0.0142(5) Uani 1 1 d . . .
C24 C 0.8918(2) 0.9969(2) 0.43799(17) 0.0180(5) Uani 1 1 d . . .
H24A H 0.9677 1.0118 0.4961 0.027 Uiso 1 1 calc R . .
H24B H 0.8253 1.0548 0.4360 0.027 Uiso 1 1 calc R . .
H24C H 0.9157 1.0022 0.3763 0.027 Uiso 1 1 calc R . .
C25 C 1.0662(2) 0.89210(19) 0.70428(17) 0.0119(4) Uani 1 1 d . . .
C26 C 1.1283(2) 0.8438(2) 0.63752(16) 0.0123(5) Uani 1 1 d . . .
H26 H 1.0779 0.8228 0.5714 0.015 Uiso 1 1 calc R . .
C27 C 1.26293(19) 0.8266(3) 0.66768(15) 0.0178(4) Uani 1 1 d . . .
H27 H 1.3026 0.7944 0.6223 0.021 Uiso 1 1 calc R . .
C28 C 1.3379(2) 0.8578(2) 0.76615(19) 0.0208(6) Uani 1 1 d . . .
H28 H 1.4285 0.8469 0.7871 0.025 Uiso 1 1 calc R . .
C29 C 1.2782(2) 0.9050(2) 0.83315(18) 0.0197(5) Uani 1 1 d . . .
H29 H 1.3299 0.9259 0.8989 0.024 Uiso 1 1 calc R . .
C30 C 1.1422(2) 0.9223(2) 0.80515(17) 0.0149(5) Uani 1 1 d . . .
C31 C 1.0838(2) 0.9660(2) 0.88495(17) 0.0188(5) Uani 1 1 d . . .
H31A H 1.1507 1.0041 0.9394 0.028 Uiso 1 1 calc R . .
H31B H 1.0484 0.9000 0.9120 0.028 Uiso 1 1 calc R . .
H31C H 1.0149 1.0218 0.8544 0.028 Uiso 1 1 calc R . .
O1 O 0.76381(15) 0.75964(14) 0.90999(12) 0.0144(3) Uani 1 1 d . . .
O2 O 0.73777(16) 0.98580(14) 0.80268(12) 0.0147(3) Uani 1 1 d . . .
O3 O 0.91137(16) 0.67590(14) 0.78000(12) 0.0140(3) Uani 1 1 d . . .
O4 O 0.61357(17) 0.66617(16) 0.69711(13) 0.0214(4) Uani 1 1 d . . .
F1 F 0.62583(15) 0.64941(12) 1.01807(11) 0.0231(3) Uani 1 1 d . . .
F2 F 0.80435(14) 0.72344(13) 1.12058(10) 0.0233(3) Uani 1 1 d . . .
F3 F 0.61971(14) 0.81103(15) 1.10072(10) 0.0239(3) Uani 1 1 d . . .
F4 F 0.63997(16) 1.18019(13) 0.95986(11) 0.0254(3) Uani 1 1 d . . .
F5 F 0.53976(17) 1.16006(15) 0.79856(13) 0.0303(4) Uani 1 1 d . . .
F6 F 0.74344(15) 1.21171(12) 0.85166(13) 0.0281(4) Uani 1 1 d . . .
F7 F 1.09486(15) 0.50369(15) 0.81965(12) 0.0286(4) Uani 1 1 d . . .
F8 F 1.06188(14) 0.56857(15) 0.95728(11) 0.0295(4) Uani 1 1 d . . .
F9 F 0.98596(17) 0.39826(14) 0.89587(13) 0.0331(4) Uani 1 1 d . . .
F10 F 0.5353(3) 0.4775(3) 0.85323(17) 0.0891(11) Uani 1 1 d . . .
F11 F 0.50848(16) 0.39891(14) 0.70947(15) 0.0387(4) Uani 1 1 d . . .
F12 F 0.40798(19) 0.55781(17) 0.7148(3) 0.0799(9) Uani 1 1 d . . .
P1 P 0.88689(5) 0.90079(5) 0.66130(4) 0.00929(11) Uani 1 1 d . . .
Pd1 Pd 0.812958(13) 0.826775(14) 0.785588(10) 0.00944(5) Uani 1 1 d . . .


_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
C1 F3 1.333(3) . ?
C1 F1 1.333(3) . ?
C1 F2 1.340(3) . ?
C1 C2 1.535(3) . ?
C2 O1 1.251(3) . ?
C2 C3 1.394(4) . ?
C3 C4 1.388(3) . ?
C4 O2 1.263(3) . ?
C4 C5 1.535(3) . ?
C5 F5 1.327(3) . ?
C5 F4 1.333(3) . ?
C5 F6 1.332(3) . ?
C6 F9 1.331(3) . ?
C6 F8 1.337(3) . ?
C6 F7 1.346(3) . ?
C6 C7 1.525(3) . ?
C7 O3 1.283(3) . ?
C7 C8 1.366(3) . ?
C8 C9 1.438(4) . ?
C9 O4 1.214(3) . ?
C9 C10 1.539(4) . ?
C10 F12 1.313(4) . ?
C10 F10 1.322(4) . ?
C10 F11 1.318(3) . ?
C11 C12 1.399(3) . ?
C11 C16 1.410(3) . ?
C11 P1 1.816(2) . ?
C12 C13 1.388(3) . ?
C13 C14 1.383(4) . ?
C14 C15 1.386(4) . ?
C15 C16 1.398(3) . ?
C16 C17 1.516(3) . ?
C18 C19 1.394(4) . ?
C18 C23 1.414(3) . ?
C18 P1 1.825(2) . ?
C19 C20 1.385(3) . ?
C20 C21 1.383(4) . ?
C21 C22 1.380(4) . ?
C22 C23 1.393(3) . ?
C23 C24 1.504(3) . ?
C25 C26 1.400(3) . ?
C25 C30 1.412(3) . ?
C25 P1 1.827(2) . ?
C26 C27 1.385(3) . ?
C27 C28 1.385(3) . ?
C28 C29 1.381(4) . ?
C29 C30 1.400(3) . ?
C30 C31 1.505(3) . ?
O1 Pd1 2.0810(15) . ?
O2 Pd1 2.0067(16) . ?
O3 Pd1 2.0131(16) . ?
P1 Pd1 2.2541(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
F3 C1 F1 107.96(19) . . ?
F3 C1 F2 107.10(18) . . ?
F1 C1 F2 107.57(19) . . ?
F3 C1 C2 113.2(2) . . ?
F1 C1 C2 110.40(19) . . ?
F2 C1 C2 110.42(18) . . ?
O1 C2 C3 129.3(2) . . ?
O1 C2 C1 112.8(2) . . ?
C3 C2 C1 117.93(19) . . ?
C4 C3 C2 122.3(2) . . ?
O2 C4 C3 130.1(2) . . ?
O2 C4 C5 111.42(19) . . ?
C3 C4 C5 118.47(19) . . ?
F5 C5 F4 107.92(19) . . ?
F5 C5 F6 108.19(19) . . ?
F4 C5 F6 107.1(2) . . ?
F5 C5 C4 109.91(19) . . ?
F4 C5 C4 112.61(19) . . ?
F6 C5 C4 110.98(19) . . ?
F9 C6 F8 107.35(19) . . ?
F9 C6 F7 107.0(2) . . ?
F8 C6 F7 107.0(2) . . ?
F9 C6 C7 114.3(2) . . ?
F8 C6 C7 109.45(19) . . ?
F7 C6 C7 111.44(19) . . ?
O3 C7 C8 131.6(2) . . ?
O3 C7 C6 109.9(2) . . ?
C8 C7 C6 118.5(2) . . ?
C7 C8 C9 124.8(2) . . ?
O4 C9 C8 128.5(2) . . ?
O4 C9 C10 117.4(2) . . ?
C8 C9 C10 114.1(2) . . ?
F12 C10 F10 110.2(3) . . ?
F12 C10 F11 106.0(2) . . ?
F10 C10 F11 105.4(3) . . ?
F12 C10 C9 112.0(2) . . ?
F10 C10 C9 111.3(2) . . ?
F11 C10 C9 111.7(2) . . ?
C12 C11 C16 120.3(2) . . ?
C12 C11 P1 119.84(17) . . ?
C16 C11 P1 119.80(17) . . ?
C13 C12 C11 120.1(2) . . ?
C14 C13 C12 119.9(2) . . ?
C13 C14 C15 120.4(2) . . ?
C14 C15 C16 121.1(2) . . ?
C15 C16 C11 118.2(2) . . ?
C15 C16 C17 118.7(2) . . ?
C11 C16 C17 123.1(2) . . ?
C19 C18 C23 120.1(2) . . ?
C19 C18 P1 117.31(16) . . ?
C23 C18 P1 122.6(2) . . ?
C20 C19 C18 121.0(2) . . ?
C21 C20 C19 119.5(2) . . ?
C22 C21 C20 119.6(2) . . ?
C21 C22 C23 122.7(2) . . ?
C22 C23 C18 117.1(2) . . ?
C22 C23 C24 118.2(2) . . ?
C18 C23 C24 124.8(2) . . ?
C26 C25 C30 119.3(2) . . ?
C26 C25 P1 118.40(16) . . ?
C30 C25 P1 122.03(17) . . ?
C27 C26 C25 121.5(2) . . ?
C28 C27 C26 119.3(2) . . ?
C29 C28 C27 120.0(2) . . ?
C28 C29 C30 122.0(2) . . ?
C29 C30 C25 117.9(2) . . ?
C29 C30 C31 118.7(2) . . ?
C25 C30 C31 123.3(2) . . ?
C2 O1 Pd1 123.22(16) . . ?
C4 O2 Pd1 124.10(14) . . ?
C7 O3 Pd1 124.23(14) . . ?
C11 P1 C18 107.08(11) . . ?
C11 P1 C25 111.24(10) . . ?
C18 P1 C25 105.77(9) . . ?
C11 P1 Pd1 108.34(7) . . ?
C18 P1 Pd1 115.88(8) . . ?
C25 P1 Pd1 108.54(7) . . ?
O2 Pd1 O3 172.41(7) . . ?
O2 Pd1 O1 90.81(6) . . ?
O3 Pd1 O1 89.70(6) . . ?
O2 Pd1 P1 90.44(5) . . ?
O3 Pd1 P1 88.33(5) . . ?
O1 Pd1 P1 174.31(5) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.044

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_beta_1
_database_code_depnum_ccdc_archive 'CCDC 1045818'
_audit_update_record             
;
2015-01-27 deposited with the CCDC.
2015-03-19 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
rac-bis(hexafluoroacetylacetonato)(tris(o-tolyl)phosphino)palladium(II)
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C31 H23 F12 O4 P Pd'
_chemical_formula_sum            'C31 H23 F12 O4 P Pd'
_chemical_formula_weight         824.86

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_int_tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.3510(14)
_cell_length_b                   14.4276(17)
_cell_length_c                   19.814(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.639(5)
_cell_angle_gamma                90.00
_cell_volume                     3229.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19581
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      25.0

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_type              RU-H3R
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       φ
_diffrn_detector_area_resol_mean 105
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19581
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_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         2.29
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5501
_reflns_number_gt                5131
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_structure_solution    SIR92
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'ORTEP-3 and PLUTON'
_computing_publication_material  SHELXL-97

_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)+(0.0298P)²+1.8574P] 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         5501
_refine_ls_number_parameters     445
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0539
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.002
_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
C10 C 0.27075(19) -0.27831(14) 0.46422(10) 0.0257(5) Uani 1 1 d . . .
C9 C 0.28637(16) -0.34672(12) 0.40591(9) 0.0154(4) Uani 1 1 d . . .
C8 C 0.39526(16) -0.39746(12) 0.41288(9) 0.0155(4) Uani 1 1 d . . .
H8 H 0.4496 -0.3817 0.4493 0.019 Uiso 1 1 calc R . .
C7 C 0.42723(15) -0.46638(12) 0.37154(9) 0.0130(4) Uani 1 1 d . . .
C6 C 0.54407(17) -0.51720(13) 0.39205(9) 0.0192(4) Uani 1 1 d . . .
C1 C -0.04924(18) -0.54619(15) 0.37669(10) 0.0242(4) Uani 1 1 d . . .
C2 C 0.01602(15) -0.50461(12) 0.31928(9) 0.0147(4) Uani 1 1 d . . .
C3 C -0.05268(16) -0.45325(13) 0.26945(9) 0.0167(4) Uani 1 1 d . . .
H3 H -0.1318 -0.4427 0.2753 0.020 Uiso 1 1 calc R . .
C4 C -0.00869(15) -0.41794(12) 0.21254(9) 0.0132(4) Uani 1 1 d . . .
C5 C -0.09393(16) -0.37329(15) 0.15713(10) 0.0212(4) Uani 1 1 d . . .
C11 C 0.44873(15) -0.31159(12) 0.23673(8) 0.0114(3) Uani 1 1 d . . .
C12 C 0.39513(15) -0.23465(12) 0.26493(9) 0.0140(4) Uani 1 1 d . . .
C13 C 0.46821(17) -0.17413(13) 0.30502(9) 0.0179(4) Uani 1 1 d . . .
H13 H 0.4347 -0.1227 0.3240 0.022 Uiso 1 1 calc R . .
C14 C 0.58925(17) -0.18852(13) 0.31731(9) 0.0205(4) Uani 1 1 d . . .
H14 H 0.6360 -0.1463 0.3433 0.025 Uiso 1 1 calc R . .
C15 C 0.64016(16) -0.26549(14) 0.29090(9) 0.0191(4) Uani 1 1 d . . .
H15 H 0.7211 -0.2759 0.2997 0.023 Uiso 1 1 calc R . .
C16 C 0.57001(15) -0.32739(12) 0.25110(8) 0.0137(4) Uani 1 1 d . . .
H16 H 0.6041 -0.3798 0.2339 0.016 Uiso 1 1 calc R . .
C17 C 0.26487(16) -0.21315(12) 0.25466(10) 0.0180(4) Uani 1 1 d . . .
H17A H 0.2224 -0.2670 0.2373 0.027 Uiso 1 1 calc R . .
H17B H 0.2515 -0.1631 0.2229 0.027 Uiso 1 1 calc R . .
H17C H 0.2375 -0.1957 0.2972 0.027 Uiso 1 1 calc R . .
C18 C 0.28650(15) -0.34538(12) 0.11188(8) 0.0122(3) Uani 1 1 d . . .
C19 C 0.21470(15) -0.39946(12) 0.06488(9) 0.0135(4) Uani 1 1 d . . .
C20 C 0.15623(16) -0.35415(14) 0.00893(9) 0.0178(4) Uani 1 1 d . . .
H20 H 0.1074 -0.3883 -0.0223 0.021 Uiso 1 1 calc R . .
C21 C 0.16880(16) -0.25973(14) -0.00144(9) 0.0204(4) Uani 1 1 d . . .
H21 H 0.1283 -0.2313 -0.0390 0.024 Uiso 1 1 calc R . .
C22 C 0.24171(17) -0.20796(13) 0.04416(10) 0.0199(4) Uani 1 1 d . . .
H22 H 0.2515 -0.1448 0.0370 0.024 Uiso 1 1 calc R . .
C23 C 0.29991(15) -0.25051(13) 0.10030(9) 0.0159(4) Uani 1 1 d . . .
H23 H 0.3488 -0.2155 0.1309 0.019 Uiso 1 1 calc R . .
C24 C 0.20149(16) -0.50297(13) 0.07083(9) 0.0173(4) Uani 1 1 d . . .
H24A H 0.1974 -0.5193 0.1175 0.026 Uiso 1 1 calc R . .
H24B H 0.2684 -0.5331 0.0543 0.026 Uiso 1 1 calc R . .
H24C H 0.1303 -0.5225 0.0445 0.026 Uiso 1 1 calc R . .
C25 C 0.46327(14) -0.48372(12) 0.15777(8) 0.0110(3) Uani 1 1 d . . .
C26 C 0.53877(15) -0.46349(12) 0.10714(9) 0.0133(4) Uani 1 1 d . . .
C27 C 0.60557(16) -0.53624(13) 0.08451(9) 0.0175(4) Uani 1 1 d . . .
H27 H 0.6565 -0.5243 0.0515 0.021 Uiso 1 1 calc R . .
C28 C 0.59885(16) -0.62559(13) 0.10933(9) 0.0188(4) Uani 1 1 d . . .
H28 H 0.6429 -0.6728 0.0921 0.023 Uiso 1 1 calc R . .
C29 C 0.52658(16) -0.64437(13) 0.15983(9) 0.0170(4) Uani 1 1 d . . .
H29 H 0.5226 -0.7040 0.1773 0.020 Uiso 1 1 calc R . .
C30 C 0.46011(15) -0.57356(12) 0.18407(9) 0.0143(4) Uani 1 1 d . . .
H30 H 0.4124 -0.5860 0.2185 0.017 Uiso 1 1 calc R . .
C31 C 0.55152(16) -0.36884(13) 0.07655(9) 0.0173(4) Uani 1 1 d . . .
H31A H 0.5504 -0.3226 0.1113 0.026 Uiso 1 1 calc R . .
H31B H 0.4872 -0.3582 0.0422 0.026 Uiso 1 1 calc R . .
H31C H 0.6251 -0.3655 0.0566 0.026 Uiso 1 1 calc R . .
O4 O 0.20435(11) -0.35074(9) 0.36126(6) 0.0186(3) Uani 1 1 d . . .
O3 O 0.37770(10) -0.50271(8) 0.31663(6) 0.0138(3) Uani 1 1 d . . .
O1 O 0.12351(10) -0.52367(8) 0.32222(6) 0.0137(3) Uani 1 1 d . . .
O2 O 0.09650(10) -0.41659(8) 0.19556(6) 0.0132(2) Uani 1 1 d . . .
F10 F 0.36944(13) -0.22965(10) 0.48237(8) 0.0504(4) Uani 1 1 d . . .
F11 F 0.24403(14) -0.32251(11) 0.51943(6) 0.0463(4) Uani 1 1 d . . .
F12 F 0.18711(13) -0.21679(9) 0.44656(7) 0.0442(4) Uani 1 1 d . . .
F7 F 0.52266(11) -0.60348(8) 0.41172(6) 0.0311(3) Uani 1 1 d . . .
F9 F 0.61028(10) -0.52291(10) 0.34013(6) 0.0345(3) Uani 1 1 d . . .
F8 F 0.61032(10) -0.47689(8) 0.44322(6) 0.0292(3) Uani 1 1 d . . .
F1 F 0.02322(12) -0.56433(13) 0.43092(7) 0.0558(5) Uani 1 1 d . . .
F3 F -0.13239(12) -0.49109(11) 0.39516(7) 0.0431(4) Uani 1 1 d . . .
F2 F -0.09993(18) -0.62529(12) 0.35666(8) 0.0710(6) Uani 1 1 d . . .
F4 F -0.20255(10) -0.36258(11) 0.17548(6) 0.0405(4) Uani 1 1 d . . .
F5 F -0.10337(12) -0.42643(11) 0.10179(6) 0.0406(3) Uani 1 1 d . . .
F6 F -0.05552(12) -0.29166(9) 0.13922(8) 0.0429(4) Uani 1 1 d . . .
P1 P 0.36138(4) -0.39866(3) 0.18754(2) 0.00915(9) Uani 1 1 d . . .
Pd1 Pd 0.235975(10) -0.459038(8) 0.257120(6) 0.00848(5) Uani 1 1 d . . .


_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
C10 F12 1.322(2) . ?
C10 F11 1.327(2) . ?
C10 F10 1.341(3) . ?
C10 C9 1.543(3) . ?
C9 O4 1.221(2) . ?
C9 C8 1.431(3) . ?
C8 C7 1.360(3) . ?
C7 O3 1.286(2) . ?
C7 C6 1.535(2) . ?
C6 F7 1.334(2) . ?
C6 F9 1.335(2) . ?
C6 F8 1.335(2) . ?
C1 F3 1.313(2) . ?
C1 F1 1.314(2) . ?
C1 F2 1.321(3) . ?
C1 C2 1.539(3) . ?
C2 O1 1.247(2) . ?
C2 C3 1.407(3) . ?
C3 C4 1.375(3) . ?
C4 O2 1.272(2) . ?
C4 C5 1.532(2) . ?
C5 F6 1.317(2) . ?
C5 F4 1.328(2) . ?
C5 F5 1.334(2) . ?
C11 C16 1.397(2) . ?
C11 C12 1.408(2) . ?
C11 P1 1.8224(17) . ?
C12 C13 1.397(3) . ?
C12 C17 1.505(2) . ?
C13 C14 1.387(3) . ?
C14 C15 1.379(3) . ?
C15 C16 1.389(3) . ?
C18 C23 1.399(3) . ?
C18 C19 1.411(2) . ?
C18 P1 1.8194(17) . ?
C19 C20 1.397(3) . ?
C19 C24 1.507(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.383(3) . ?
C22 C23 1.381(3) . ?
C25 C30 1.399(3) . ?
C25 C26 1.412(2) . ?
C25 P1 1.8236(17) . ?
C26 C27 1.394(3) . ?
C26 C31 1.507(3) . ?
C27 C28 1.384(3) . ?
C28 C29 1.382(3) . ?
C29 C30 1.384(3) . ?
O3 Pd1 2.0006(12) . ?
O1 Pd1 2.1181(12) . ?
O2 Pd1 1.9974(12) . ?
P1 Pd1 2.2520(5) . ?

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
F12 C10 F11 108.95(18) . . ?
F12 C10 F10 106.19(17) . . ?
F11 C10 F10 106.45(17) . . ?
F12 C10 C9 111.33(16) . . ?
F11 C10 C9 111.24(16) . . ?
F10 C10 C9 112.41(17) . . ?
O4 C9 C8 129.44(16) . . ?
O4 C9 C10 115.93(16) . . ?
C8 C9 C10 114.62(15) . . ?
C7 C8 C9 126.50(16) . . ?
O3 C7 C8 133.40(17) . . ?
O3 C7 C6 108.89(15) . . ?
C8 C7 C6 117.69(16) . . ?
F7 C6 F9 107.47(16) . . ?
F7 C6 F8 106.85(15) . . ?
F9 C6 F8 107.13(16) . . ?
F7 C6 C7 110.22(15) . . ?
F9 C6 C7 111.27(15) . . ?
F8 C6 C7 113.61(16) . . ?
F3 C1 F1 107.58(17) . . ?
F3 C1 F2 107.63(19) . . ?
F1 C1 F2 107.02(19) . . ?
F3 C1 C2 112.42(16) . . ?
F1 C1 C2 111.96(17) . . ?
F2 C1 C2 109.98(17) . . ?
O1 C2 C3 128.40(16) . . ?
O1 C2 C1 114.81(16) . . ?
C3 C2 C1 116.75(16) . . ?
C4 C3 C2 123.34(16) . . ?
O2 C4 C3 130.42(16) . . ?
O2 C4 C5 110.31(15) . . ?
C3 C4 C5 119.26(15) . . ?
F6 C5 F4 108.10(17) . . ?
F6 C5 F5 107.13(16) . . ?
F4 C5 F5 106.86(16) . . ?
F6 C5 C4 111.51(15) . . ?
F4 C5 C4 113.00(15) . . ?
F5 C5 C4 109.97(16) . . ?
C16 C11 C12 120.24(16) . . ?
C16 C11 P1 118.04(13) . . ?
C12 C11 P1 121.48(13) . . ?
C13 C12 C11 117.57(16) . . ?
C13 C12 C17 117.95(16) . . ?
C11 C12 C17 124.48(16) . . ?
C14 C13 C12 121.92(17) . . ?
C15 C14 C13 119.92(17) . . ?
C14 C15 C16 119.67(17) . . ?
C15 C16 C11 120.61(17) . . ?
C23 C18 C19 119.86(16) . . ?
C23 C18 P1 119.94(13) . . ?
C19 C18 P1 120.19(13) . . ?
C20 C19 C18 117.60(17) . . ?
C20 C19 C24 118.86(16) . . ?
C18 C19 C24 123.50(15) . . ?
C21 C20 C19 121.97(17) . . ?
C22 C21 C20 119.82(17) . . ?
C23 C22 C21 119.64(18) . . ?
C22 C23 C18 121.07(17) . . ?
C30 C25 C26 119.71(16) . . ?
C30 C25 P1 117.57(13) . . ?
C26 C25 P1 122.62(13) . . ?
C27 C26 C25 117.38(16) . . ?
C27 C26 C31 118.43(16) . . ?
C25 C26 C31 124.19(16) . . ?
C28 C27 C26 122.41(17) . . ?
C29 C28 C27 119.82(17) . . ?
C28 C29 C30 119.30(17) . . ?
C29 C30 C25 121.33(16) . . ?
C7 O3 Pd1 129.01(11) . . ?
C2 O1 Pd1 121.35(11) . . ?
C4 O2 Pd1 122.82(11) . . ?
C18 P1 C11 109.57(8) . . ?
C18 P1 C25 106.12(8) . . ?
C11 P1 C25 107.93(8) . . ?
C18 P1 Pd1 113.30(6) . . ?
C11 P1 Pd1 106.42(6) . . ?
C25 P1 Pd1 113.38(6) . . ?
O2 Pd1 O3 178.48(5) . . ?
O2 Pd1 O1 91.03(5) . . ?
O3 Pd1 O1 90.02(5) . . ?
O2 Pd1 P1 91.05(4) . . ?
O3 Pd1 P1 87.86(4) . . ?
O1 Pd1 P1 176.49(3) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.053
