#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:00:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180118 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/16/7101624.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7101624
loop_
_publ_author_name
'Agostinho, Magno'
'Braunstein, Pierre'
_publ_section_title
;
 Structurally characterized intermediates in the stepwise insertion of
 CO-ethylene or CO-methyl acrylate into the metal-carbon bond of Pd(II)
 complexes stabilized by (phosphinomethyl)oxazoline ligands.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              58
_journal_page_last               60
_journal_paper_doi               10.1039/b613865a
_journal_year                    2007
_chemical_formula_sum            'C23 H27 F3 N O5 P Pd S'
_chemical_formula_weight         623.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.4860(15)
_cell_angle_beta                 96.7650(15)
_cell_angle_gamma                112.951(3)
_cell_formula_units_Z            4
_cell_length_a                   11.4740(5)
_cell_length_b                   13.9030(7)
_cell_length_c                   18.0810(10)
_cell_measurement_reflns_used    20669
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2624.9(2)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24511
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.433
_refine_diff_density_min         -1.753
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         15294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0965P)²+2.1850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1840
_refine_ls_wR_factor_ref         0.2146
_reflns_number_gt                8608
_reflns_number_total             15294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613865a.txt
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101624
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
Pd2 Pd 0.01558(5) 0.61133(3) 0.29734(3) 0.05463(16) Uani 1 1 d
Pd1 Pd 0.86966(4) 0.04645(3) 0.195015(18) 0.03663(13) Uani 1 1 d
S1 S 0.46119(17) 0.75812(17) 0.10878(9) 0.0670(5) Uani 1 1 d
S2 S 0.2119(4) 0.2553(2) 0.43826(15) 0.1267(12) Uani 1 1 d
P2 P 0.21091(18) 0.68747(12) 0.35869(8) 0.0510(4) Uani 1 1 d
P1 P 1.04072(14) 0.01217(11) 0.19849(7) 0.0377(3) Uani 1 1 d
F1 F 0.4393(11) 0.5808(8) 0.0494(6) 0.237(6) Uani 1 1 d
F2 F 0.3615(6) 0.6608(6) -0.0224(3) 0.163(3) Uani 1 1 d
F3 F 0.2648(7) 0.5877(5) 0.0622(4) 0.159(3) Uani 1 1 d
F4 F 0.3751(7) 0.4159(6) 0.3993(4) 0.156(3) Uani 1 1 d
F5 F 0.3571(11) 0.3843(17) 0.5161(5) 0.412(13) Uani 1 1 d
F6 F 0.2118(10) 0.4342(5) 0.4434(6) 0.219(4) Uani 1 1 d
O3 O 0.2516(6) 0.4640(4) 0.2334(3) 0.0781(16) Uani 1 1 d
O4 O -0.1787(5) 0.5456(3) 0.2424(3) 0.0690(13) Uani 1 1 d
O1 O 0.9725(4) -0.0314(3) 0.40698(18) 0.0493(10) Uani 1 1 d
O2 O 0.6980(4) 0.0723(3) 0.18157(18) 0.0432(9) Uani 1 1 d
O5 O 0.5808(6) 0.8093(7) 0.0829(3) 0.131(3) Uani 1 1 d
O6 O 0.4662(9) 0.7268(5) 0.1799(3) 0.128(3) Uani 1 1 d
O7 O 0.3851(7) 0.8198(5) 0.0970(4) 0.128(3) Uani 1 1 d
O8 O 0.1098(8) 0.2349(5) 0.4873(4) 0.148(3) Uani 1 1 d
O9 O 0.1157(9) 0.2454(8) 0.3570(4) 0.174(4) Uani 1 1 d
O10 O 0.2804(8) 0.1994(6) 0.4294(4) 0.137(3) Uani 1 1 d
N2 N 0.0874(6) 0.5076(4) 0.2486(3) 0.0593(14) Uani 1 1 d
N1 N 0.8743(4) 0.0077(3) 0.3062(2) 0.0379(9) Uani 1 1 d
C23 C 0.0256(9) 0.4095(5) 0.1970(4) 0.073(2) Uani 1 1 d
C24 C 0.1365(11) 0.3768(6) 0.1921(5) 0.097(3) Uani 1 1 d
H24A H 0.1215 0.3106 0.2154 0.117 Uiso 1 1 calc
H24B H 0.1473 0.3663 0.1393 0.117 Uiso 1 1 calc
C25 C 0.2044(8) 0.5288(5) 0.2630(3) 0.0612(19) Uani 1 1 d
C26 C 0.3025(7) 0.6248(5) 0.3118(3) 0.0626(18) Uani 1 1 d
H26A H 0.3592 0.6741 0.2808 0.075 Uiso 1 1 calc
H26B H 0.3558 0.6038 0.3494 0.075 Uiso 1 1 calc
C27 C 0.2949(6) 0.8268(4) 0.3542(3) 0.0458(13) Uani 1 1 d
C32 C 0.3306(6) 0.8646(5) 0.2873(3) 0.0468(13) Uani 1 1 d
H32 H 0.3139 0.8177 0.2439 0.056 Uiso 1 1 calc
C31 C 0.3919(6) 0.9733(6) 0.2846(4) 0.0614(17) Uani 1 1 d
H31 H 0.4182 0.9992 0.2389 0.074 Uiso 1 1 calc
C30 C 0.4149(6) 1.0432(5) 0.3458(4) 0.0607(17) Uani 1 1 d
H30 H 0.4564 1.1165 0.3428 0.073 Uiso 1 1 calc
C29 C 0.3773(7) 1.0055(5) 0.4109(4) 0.0607(17) Uani 1 1 d
H29 H 0.3922 1.0533 0.4536 0.073 Uiso 1 1 calc
C28 C 0.3169(7) 0.8978(5) 0.4161(3) 0.0562(16) Uani 1 1 d
H28 H 0.2909 0.8729 0.4620 0.067 Uiso 1 1 calc
C33 C 0.2342(8) 0.6683(5) 0.4574(3) 0.0587(17) Uani 1 1 d
C34 C 0.1289(8) 0.6300(5) 0.4949(4) 0.072(2) Uani 1 1 d
H34 H 0.0450 0.6142 0.4699 0.087 Uiso 1 1 calc
C35 C 0.1498(12) 0.6153(6) 0.5711(5) 0.099(3) Uani 1 1 d
H35 H 0.0793 0.5897 0.5980 0.119 Uiso 1 1 calc
C36 C 0.2704(13) 0.6375(7) 0.6067(5) 0.097(3) Uani 1 1 d
H36 H 0.2825 0.6270 0.6581 0.116 Uiso 1 1 calc
C37 C 0.3745(10) 0.6745(7) 0.5694(4) 0.088(3) Uani 1 1 d
H37 H 0.4576 0.6884 0.5947 0.106 Uiso 1 1 calc
C38 C 0.3572(9) 0.6916(6) 0.4943(4) 0.076(2) Uani 1 1 d
H38 H 0.4288 0.7190 0.4684 0.091 Uiso 1 1 calc
C39 C -0.0494(8) 0.7122(7) 0.3424(6) 0.105(3) Uani 1 1 d
H39A H -0.0300 0.7176 0.3976 0.126 Uiso 1 1 calc
H39B H -0.0042 0.7827 0.3261 0.126 Uiso 1 1 calc
C40 C -0.1798(9) 0.6811(8) 0.3218(6) 0.108(3) Uani 1 1 d
H40A H -0.1955 0.7420 0.3041 0.130 Uiso 1 1 calc
H40B H -0.2217 0.6621 0.3670 0.130 Uiso 1 1 calc
C41 C -0.2426(8) 0.5916(5) 0.2629(4) 0.072(2) Uani 1 1 d
C42 C -0.3807(10) 0.5612(7) 0.2321(7) 0.117(4) Uani 1 1 d
H42A H -0.4083 0.5014 0.1939 0.176 Uiso 1 1 calc
H42B H -0.3913 0.6206 0.2095 0.176 Uiso 1 1 calc
H42C H -0.4327 0.5417 0.2726 0.176 Uiso 1 1 calc
C43 C -0.0271(9) 0.4340(6) 0.1215(4) 0.084(2) Uani 1 1 d
H43A H 0.0431 0.4852 0.0999 0.126 Uiso 1 1 calc
H43B H -0.0906 0.4631 0.1290 0.126 Uiso 1 1 calc
H43C H -0.0675 0.3694 0.0875 0.126 Uiso 1 1 calc
C44 C -0.0807(10) 0.3306(5) 0.2319(5) 0.100(3) Uani 1 1 d
H44A H -0.0453 0.3163 0.2802 0.150 Uiso 1 1 calc
H44B H -0.1211 0.2653 0.1986 0.150 Uiso 1 1 calc
H44C H -0.1447 0.3590 0.2396 0.150 Uiso 1 1 calc
C1 C 0.7875(5) 0.0009(5) 0.3632(3) 0.0482(14) Uani 1 1 d
C2 C 0.8651(6) -0.0151(6) 0.4337(3) 0.0586(17) Uani 1 1 d
H2A H 0.8965 0.0475 0.4706 0.070 Uiso 1 1 calc
H2B H 0.8121 -0.0769 0.4575 0.070 Uiso 1 1 calc
C3 C 0.9695(5) -0.0094(4) 0.3360(3) 0.0382(11) Uani 1 1 d
C4 C 1.0779(5) -0.0057(4) 0.2975(3) 0.0426(12) Uani 1 1 d
H4A H 1.0908 -0.0718 0.3015 0.051 Uiso 1 1 calc
H4B H 1.1574 0.0533 0.3210 0.051 Uiso 1 1 calc
C11 C 1.1839(5) 0.1096(4) 0.1723(3) 0.0424(12) Uani 1 1 d
C12 C 1.2746(7) 0.1879(5) 0.2251(3) 0.0561(16) Uani 1 1 d
H12 H 1.2656 0.1853 0.2766 0.067 Uiso 1 1 calc
C13 C 1.3762(8) 0.2683(5) 0.2033(4) 0.073(2) Uani 1 1 d
H13 H 1.4364 0.3206 0.2399 0.087 Uiso 1 1 calc
C14 C 1.3914(8) 0.2738(5) 0.1288(4) 0.071(2) Uani 1 1 d
H14 H 1.4609 0.3302 0.1140 0.085 Uiso 1 1 calc
C15 C 1.3037(7) 0.1956(5) 0.0753(3) 0.0607(17) Uani 1 1 d
H15 H 1.3146 0.1975 0.0240 0.073 Uiso 1 1 calc
C16 C 1.2001(6) 0.1150(5) 0.0974(3) 0.0543(15) Uani 1 1 d
H16 H 1.1397 0.0630 0.0608 0.065 Uiso 1 1 calc
C5 C 1.0090(5) -0.1120(4) 0.1451(3) 0.0432(12) Uani 1 1 d
C6 C 1.1073(6) -0.1426(5) 0.1303(3) 0.0528(14) Uani 1 1 d
H6 H 1.1943 -0.0965 0.1451 0.063 Uiso 1 1 calc
C7 C 1.0757(8) -0.2416(6) 0.0936(4) 0.0671(19) Uani 1 1 d
H7 H 1.1417 -0.2635 0.0841 0.081 Uiso 1 1 calc
C8 C 0.9486(8) -0.3085(5) 0.0710(4) 0.071(2) Uani 1 1 d
H8 H 0.9281 -0.3751 0.0448 0.085 Uiso 1 1 calc
C9 C 0.8534(7) -0.2788(5) 0.0861(4) 0.0692(19) Uani 1 1 d
H9 H 0.7666 -0.3256 0.0716 0.083 Uiso 1 1 calc
C10 C 0.8825(6) -0.1799(5) 0.1228(4) 0.0601(16) Uani 1 1 d
H10 H 0.8156 -0.1592 0.1325 0.072 Uiso 1 1 calc
C17 C 0.8741(6) 0.0841(5) 0.0879(3) 0.0444(13) Uani 1 1 d
H17A H 0.9309 0.1587 0.0865 0.053 Uiso 1 1 calc
H17B H 0.9056 0.0398 0.0586 0.053 Uiso 1 1 calc
C18 C 0.7363(6) 0.0639(6) 0.0564(3) 0.0561(16) Uani 1 1 d
H18A H 0.7371 0.1141 0.0191 0.067 Uiso 1 1 calc
H18B H 0.6946 -0.0077 0.0302 0.067 Uiso 1 1 calc
C19 C 0.6592(5) 0.0742(4) 0.1144(3) 0.0437(12) Uani 1 1 d
C20 C 0.5367(7) 0.0842(6) 0.0947(3) 0.0634(18) Uani 1 1 d
H20A H 0.4666 0.0145 0.0889 0.095 Uiso 1 1 calc
H20B H 0.5369 0.1164 0.0475 0.095 Uiso 1 1 calc
H20C H 0.5249 0.1283 0.1345 0.095 Uiso 1 1 calc
C22 C 0.6629(6) -0.0943(5) 0.3380(4) 0.0587(16) Uani 1 1 d
H22A H 0.6247 -0.0861 0.2885 0.088 Uiso 1 1 calc
H22B H 0.6034 -0.1000 0.3740 0.088 Uiso 1 1 calc
H22C H 0.6803 -0.1578 0.3354 0.088 Uiso 1 1 calc
C21 C 0.7673(7) 0.1003(6) 0.3719(3) 0.0619(18) Uani 1 1 d
H21A H 0.8503 0.1596 0.3852 0.093 Uiso 1 1 calc
H21B H 0.7148 0.0965 0.4116 0.093 Uiso 1 1 calc
H21C H 0.7237 0.1100 0.3247 0.093 Uiso 1 1 calc
C45 C 0.3820(9) 0.6417(9) 0.0478(5) 0.096(3) Uani 1 1 d
C46 C 0.2873(15) 0.3859(8) 0.4477(6) 0.1267(12) Uani 1 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C39 Pd2 N2 178.7(3) y
C39 Pd2 O4 80.1(3) y
N2 Pd2 O4 100.6(2) y
C39 Pd2 P2 95.5(3) y
N2 Pd2 P2 83.88(18) y
O4 Pd2 P2 175.56(13) y
C17 Pd1 N1 177.1(2) y
C17 Pd1 O2 82.80(18) y
N1 Pd1 O2 100.03(14) y
C17 Pd1 P1 93.30(16) y
N1 Pd1 P1 83.91(12) y
O2 Pd1 P1 174.72(10) y
O6 S1 O5 116.3(5) ?
O6 S1 O7 113.1(5) ?
O5 S1 O7 109.7(5) ?
O6 S1 C45 105.9(4) ?
O5 S1 C45 104.6(4) ?
O7 S1 C45 106.3(5) ?
O10 S2 O8 126.9(5) ?
O10 S2 C46 118.0(7) ?
O8 S2 C46 103.5(5) ?
O10 S2 O9 109.6(5) ?
O8 S2 O9 95.8(5) ?
C46 S2 O9 96.9(6) ?
C27 P2 C33 105.1(3) ?
C27 P2 C26 105.6(3) ?
C33 P2 C26 106.1(3) ?
C27 P2 Pd2 117.52(19) ?
C33 P2 Pd2 117.4(3) ?
C26 P2 Pd2 104.0(2) ?
C11 P1 C5 107.5(2) ?
C11 P1 C4 107.2(2) ?
C5 P1 C4 106.5(2) ?
C11 P1 Pd1 118.77(17) ?
C5 P1 Pd1 112.25(19) ?
C4 P1 Pd1 103.76(18) ?
C25 O3 C24 103.8(6) ?
C41 O4 Pd2 113.1(5) ?
C3 O1 C2 106.0(4) ?
C19 O2 Pd1 111.9(3) ?
C25 N2 C23 109.0(6) ?
C25 N2 Pd2 118.2(4) ?
C23 N2 Pd2 132.8(5) ?
C3 N1 C1 109.0(4) ?
C3 N1 Pd1 118.5(3) ?
C1 N1 Pd1 132.4(3) ?
N2 C23 C44 109.0(5) ?
N2 C23 C24 101.7(7) ?
C44 C23 C24 112.5(6) ?
N2 C23 C43 109.5(5) ?
C44 C23 C43 110.7(8) ?
C24 C23 C43 113.0(6) ?
O3 C24 C23 105.9(5) ?
O3 C24 H24A 110.6 ?
C23 C24 H24A 110.6 ?
O3 C24 H24B 110.6 ?
C23 C24 H24B 110.6 ?
H24A C24 H24B 108.7 ?
N2 C25 O3 119.2(7) ?
N2 C25 C26 125.5(5) ?
O3 C25 C26 115.3(7) ?
C25 C26 P2 106.6(5) ?
C25 C26 H26A 110.4 ?
P2 C26 H26A 110.4 ?
C25 C26 H26B 110.4 ?
P2 C26 H26B 110.4 ?
H26A C26 H26B 108.6 ?
C32 C27 C28 119.0(5) ?
C32 C27 P2 120.0(4) ?
C28 C27 P2 120.9(4) ?
C27 C32 C31 119.0(5) ?
C27 C32 H32 120.5 ?
C31 C32 H32 120.5 ?
C30 C31 C32 121.9(6) ?
C30 C31 H31 119.1 ?
C32 C31 H31 119.1 ?
C29 C30 C31 118.7(6) ?
C29 C30 H30 120.6 ?
C31 C30 H30 120.6 ?
C30 C29 C28 121.1(6) ?
C30 C29 H29 119.5 ?
C28 C29 H29 119.5 ?
C27 C28 C29 120.3(5) ?
C27 C28 H28 119.9 ?
C29 C28 H28 119.9 ?
C34 C33 C38 120.8(6) ?
C34 C33 P2 119.4(6) ?
C38 C33 P2 119.8(5) ?
C33 C34 C35 118.1(9) ?
C33 C34 H34 121.0 ?
C35 C34 H34 121.0 ?
C36 C35 C34 120.8(8) ?
C36 C35 H35 119.6 ?
C34 C35 H35 119.6 ?
C35 C36 C37 121.1(8) ?
C35 C36 H36 119.4 ?
C37 C36 H36 119.4 ?
C36 C37 C38 119.5(9) ?
C36 C37 H37 120.2 ?
C38 C37 H37 120.2 ?
C37 C38 C33 119.7(8) ?
C37 C38 H38 120.2 ?
C33 C38 H38 120.2 ?
C40 C39 Pd2 112.1(6) ?
C40 C39 H39A 109.2 ?
Pd2 C39 H39A 109.2 ?
C40 C39 H39B 109.2 ?
Pd2 C39 H39B 109.2 ?
H39A C39 H39B 107.9 ?
C39 C40 C41 116.2(7) ?
C39 C40 H40A 108.2 ?
C41 C40 H40A 108.2 ?
C39 C40 H40B 108.2 ?
C41 C40 H40B 108.2 ?
H40A C40 H40B 107.4 ?
O4 C41 C40 117.9(7) ?
O4 C41 C42 123.1(7) ?
C40 C41 C42 119.0(8) ?
C41 C42 H42A 109.5 ?
C41 C42 H42B 109.5 ?
H42A C42 H42B 109.5 ?
C41 C42 H42C 109.5 ?
H42A C42 H42C 109.5 ?
H42B C42 H42C 109.5 ?
C23 C43 H43A 109.5 ?
C23 C43 H43B 109.5 ?
H43A C43 H43B 109.5 ?
C23 C43 H43C 109.5 ?
H43A C43 H43C 109.5 ?
H43B C43 H43C 109.5 ?
C23 C44 H44A 109.5 ?
C23 C44 H44B 109.5 ?
H44A C44 H44B 109.5 ?
C23 C44 H44C 109.5 ?
H44A C44 H44C 109.5 ?
H44B C44 H44C 109.5 ?
C21 C1 N1 110.3(5) ?
C21 C1 C22 112.4(5) ?
N1 C1 C22 107.6(4) ?
C21 C1 C2 112.2(5) ?
N1 C1 C2 101.3(4) ?
C22 C1 C2 112.4(5) ?
O1 C2 C1 105.1(4) ?
O1 C2 H2A 110.7 ?
C1 C2 H2A 110.7 ?
O1 C2 H2B 110.7 ?
C1 C2 H2B 110.7 ?
H2A C2 H2B 108.8 ?
N1 C3 O1 117.7(5) ?
N1 C3 C4 124.6(4) ?
O1 C3 C4 117.7(4) ?
C3 C4 P1 108.3(3) ?
C3 C4 H4A 110.0 ?
P1 C4 H4A 110.0 ?
C3 C4 H4B 110.0 ?
P1 C4 H4B 110.0 ?
H4A C4 H4B 108.4 ?
C16 C11 C12 118.1(5) ?
C16 C11 P1 120.1(5) ?
C12 C11 P1 121.4(4) ?
C13 C12 C11 121.0(5) ?
C13 C12 H12 119.5 ?
C11 C12 H12 119.5 ?
C12 C13 C14 120.7(6) ?
C12 C13 H13 119.7 ?
C14 C13 H13 119.7 ?
C13 C14 C15 119.4(6) ?
C13 C14 H14 120.3 ?
C15 C14 H14 120.3 ?
C16 C15 C14 119.8(5) ?
C16 C15 H15 120.1 ?
C14 C15 H15 120.1 ?
C11 C16 C15 121.0(6) ?
C11 C16 H16 119.5 ?
C15 C16 H16 119.5 ?
C10 C5 C6 119.8(5) ?
C10 C5 P1 117.9(4) ?
C6 C5 P1 122.2(4) ?
C7 C6 C5 119.1(6) ?
C7 C6 H6 120.4 ?
C5 C6 H6 120.4 ?
C8 C7 C6 120.5(6) ?
C8 C7 H7 119.7 ?
C6 C7 H7 119.7 ?
C9 C8 C7 120.2(6) ?
C9 C8 H8 119.9 ?
C7 C8 H8 119.9 ?
C8 C9 C10 120.4(7) ?
C8 C9 H9 119.8 ?
C10 C9 H9 119.8 ?
C5 C10 C9 120.0(6) ?
C5 C10 H10 120.0 ?
C9 C10 H10 120.0 ?
C18 C17 Pd1 105.6(4) ?
C18 C17 H17A 110.6 ?
Pd1 C17 H17A 110.6 ?
C18 C17 H17B 110.6 ?
Pd1 C17 H17B 110.6 ?
H17A C17 H17B 108.7 ?
C19 C18 C17 113.5(4) ?
C19 C18 H18A 108.9 ?
C17 C18 H18A 108.9 ?
C19 C18 H18B 108.9 ?
C17 C18 H18B 108.9 ?
H18A C18 H18B 107.7 ?
O2 C19 C20 119.0(5) ?
O2 C19 C18 119.3(5) ?
C20 C19 C18 121.7(5) ?
C19 C20 H20A 109.5 ?
C19 C20 H20B 109.5 ?
H20A C20 H20B 109.5 ?
C19 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
C1 C22 H22A 109.5 ?
C1 C22 H22B 109.5 ?
H22A C22 H22B 109.5 ?
C1 C22 H22C 109.5 ?
H22A C22 H22C 109.5 ?
H22B C22 H22C 109.5 ?
C1 C21 H21A 109.5 ?
C1 C21 H21B 109.5 ?
H21A C21 H21B 109.5 ?
C1 C21 H21C 109.5 ?
H21A C21 H21C 109.5 ?
H21B C21 H21C 109.5 ?
F1 C45 F2 107.9(9) ?
F1 C45 F3 107.4(11) ?
F2 C45 F3 102.6(8) ?
F1 C45 S1 114.1(8) ?
F2 C45 S1 112.3(8) ?
F3 C45 S1 111.9(6) ?
F6 C46 F4 113.5(9) ?
F6 C46 F5 121.0(11) ?
F4 C46 F5 105.0(12) ?
F6 C46 S2 113.9(11) ?
F4 C46 S2 109.4(7) ?
F5 C46 S2 91.6(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd2 C39 2.012(7) y
Pd2 N2 2.127(5) y
Pd2 O4 2.145(5) y
Pd2 P2 2.1992(19) y
Pd1 C17 2.030(5) y
Pd1 N1 2.104(4) y
Pd1 O2 2.125(4) y
Pd1 P1 2.1878(14) y
S1 O6 1.378(5) ?
S1 O5 1.424(6) ?
S1 O7 1.448(6) ?
S1 C45 1.767(10) ?
S2 O10 1.321(6) ?
S2 O8 1.499(7) ?
S2 C46 1.670(10) ?
S2 O9 1.697(8) ?
P2 C27 1.807(6) ?
P2 C33 1.820(6) ?
P2 C26 1.855(6) y
P1 C11 1.806(6) ?
P1 C5 1.824(5) ?
P1 C4 1.841(5) y
F1 C45 1.258(11) ?
F2 C45 1.322(10) ?
F3 C45 1.324(10) ?
F4 C46 1.366(12) ?
F5 C46 1.398(15) ?
F6 C46 1.284(13) ?
O3 C25 1.340(7) ?
O3 C24 1.488(11) ?
O4 C41 1.223(9) y
O1 C3 1.332(5) ?
O1 C2 1.467(7) ?
O2 C19 1.248(6) y
N2 C25 1.249(9) y
N2 C23 1.488(8) ?
N1 C3 1.270(6) y
N1 C1 1.497(6) ?
C23 C44 1.513(11) ?
C23 C24 1.519(12) ?
C23 C43 1.533(10) ?
C24 H24A 0.9900 ?
C24 H24B 0.9900 ?
C25 C26 1.523(10) y
C26 H26A 0.9900 ?
C26 H26B 0.9900 ?
C27 C32 1.383(7) ?
C27 C28 1.389(8) ?
C32 C31 1.402(9) ?
C32 H32 0.9500 ?
C31 C30 1.371(10) ?
C31 H31 0.9500 ?
C30 C29 1.357(9) ?
C30 H30 0.9500 ?
C29 C28 1.397(9) ?
C29 H29 0.9500 ?
C28 H28 0.9500 ?
C33 C34 1.389(9) ?
C33 C38 1.394(11) ?
C34 C35 1.407(11) ?
C34 H34 0.9500 ?
C35 C36 1.366(14) ?
C35 H35 0.9500 ?
C36 C37 1.372(13) ?
C36 H36 0.9500 ?
C37 C38 1.393(9) ?
C37 H37 0.9500 ?
C38 H38 0.9500 ?
C39 C40 1.383(12) y
C39 H39A 0.9900 ?
C39 H39B 0.9900 ?
C40 C41 1.485(11) y
C40 H40A 0.9900 ?
C40 H40B 0.9900 ?
C41 C42 1.499(12) ?
C42 H42A 0.9800 ?
C42 H42B 0.9800 ?
C42 H42C 0.9800 ?
C43 H43A 0.9800 ?
C43 H43B 0.9800 ?
C43 H43C 0.9800 ?
C44 H44A 0.9800 ?
C44 H44B 0.9800 ?
C44 H44C 0.9800 ?
C1 C21 1.493(9) ?
C1 C22 1.524(9) ?
C1 C2 1.542(7) ?
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 C4 1.480(7) y
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C11 C16 1.389(7) ?
C11 C12 1.405(8) ?
C12 C13 1.376(9) ?
C12 H12 0.9500 ?
C13 C14 1.381(9) ?
C13 H13 0.9500 ?
C14 C15 1.399(10) ?
C14 H14 0.9500 ?
C15 C16 1.393(9) ?
C15 H15 0.9500 ?
C16 H16 0.9500 ?
C5 C10 1.386(8) ?
C5 C6 1.400(8) ?
C6 C7 1.392(9) ?
C6 H6 0.9500 ?
C7 C8 1.389(10) ?
C7 H7 0.9500 ?
C8 C9 1.360(10) ?
C8 H8 0.9500 ?
C9 C10 1.398(9) ?
C9 H9 0.9500 ?
C10 H10 0.9500 ?
C17 C18 1.527(8) y
C17 H17A 0.9900 ?
C17 H17B 0.9900 ?
C18 C19 1.485(8) y
C18 H18A 0.9900 ?
C18 H18B 0.9900 ?
C19 C20 1.470(8) ?
C20 H20A 0.9800 ?
C20 H20B 0.9800 ?
C20 H20C 0.9800 ?
C22 H22A 0.9800 ?
C22 H22B 0.9800 ?
C22 H22C 0.9800 ?
C21 H21A 0.9800 ?
C21 H21B 0.9800 ?
C21 H21C 0.9800 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C39 Pd2 P2 C27 -52.2(4)
N2 Pd2 P2 C27 126.6(2)
O4 Pd2 P2 C27 -56.8(17)
C39 Pd2 P2 C33 74.8(4)
N2 Pd2 P2 C33 -106.4(2)
O4 Pd2 P2 C33 70.1(17)
C39 Pd2 P2 C26 -168.4(4)
N2 Pd2 P2 C26 10.4(3)
O4 Pd2 P2 C26 -173.0(17)
C17 Pd1 P1 C11 52.5(3)
N1 Pd1 P1 C11 -126.9(2)
O2 Pd1 P1 C11 94.7(12)
C17 Pd1 P1 C5 -74.1(2)
N1 Pd1 P1 C5 106.5(2)
O2 Pd1 P1 C5 -31.9(12)
C17 Pd1 P1 C4 171.3(2)
N1 Pd1 P1 C4 -8.1(2)
O2 Pd1 P1 C4 -146.5(12)
C39 Pd2 O4 C41 -2.7(6)
N2 Pd2 O4 C41 178.5(5)
P2 Pd2 O4 C41 2(2)
C17 Pd1 O2 C19 15.2(4)
N1 Pd1 O2 C19 -165.2(4)
P1 Pd1 O2 C19 -27.3(14)
C39 Pd2 N2 C25 55(15)
O4 Pd2 N2 C25 173.3(5)
P2 Pd2 N2 C25 -6.9(5)
C39 Pd2 N2 C23 -124(15)
O4 Pd2 N2 C23 -5.7(5)
P2 Pd2 N2 C23 174.0(5)
C17 Pd1 N1 C3 -6(4)
O2 Pd1 N1 C3 -177.1(4)
P1 Pd1 N1 C3 6.4(4)
C17 Pd1 N1 C1 170(4)
O2 Pd1 N1 C1 -1.2(5)
P1 Pd1 N1 C1 -177.7(5)
C25 N2 C23 C44 123.8(7)
Pd2 N2 C23 C44 -57.0(8)
C25 N2 C23 C24 4.8(7)
Pd2 N2 C23 C24 -176.0(4)
C25 N2 C23 C43 -114.9(7)
Pd2 N2 C23 C43 64.2(8)
C25 O3 C24 C23 5.8(7)
N2 C23 C24 O3 -6.3(7)
C44 C23 C24 O3 -122.7(7)
C43 C23 C24 O3 111.0(7)
C23 N2 C25 O3 -1.3(8)
Pd2 N2 C25 O3 179.4(4)
C23 N2 C25 C26 178.0(5)
Pd2 N2 C25 C26 -1.3(8)
C24 O3 C25 N2 -3.0(8)
C24 O3 C25 C26 177.6(5)
N2 C25 C26 P2 10.5(8)
O3 C25 C26 P2 -170.2(4)
C27 P2 C26 C25 -137.7(4)
C33 P2 C26 C25 111.1(4)
Pd2 P2 C26 C25 -13.3(4)
C33 P2 C27 C32 160.0(5)
C26 P2 C27 C32 48.1(6)
Pd2 P2 C27 C32 -67.3(5)
C33 P2 C27 C28 -24.3(6)
C26 P2 C27 C28 -136.2(5)
Pd2 P2 C27 C28 108.4(5)
C28 C27 C32 C31 2.1(9)
P2 C27 C32 C31 177.9(5)
C27 C32 C31 C30 -1.4(9)
C32 C31 C30 C29 0.1(10)
C31 C30 C29 C28 0.4(10)
C32 C27 C28 C29 -1.6(10)
P2 C27 C28 C29 -177.3(5)
C30 C29 C28 C27 0.3(10)
C27 P2 C33 C34 117.2(5)
C26 P2 C33 C34 -131.3(5)
Pd2 P2 C33 C34 -15.6(5)
C27 P2 C33 C38 -63.1(6)
C26 P2 C33 C38 48.4(6)
Pd2 P2 C33 C38 164.1(5)
C38 C33 C34 C35 -0.2(9)
P2 C33 C34 C35 179.6(5)
C33 C34 C35 C36 -0.4(11)
C34 C35 C36 C37 -0.1(13)
C35 C36 C37 C38 1.1(13)
C36 C37 C38 C33 -1.7(11)
C34 C33 C38 C37 1.2(10)
P2 C33 C38 C37 -178.5(5)
N2 Pd2 C39 C40 125(14)
O4 Pd2 C39 C40 6.3(8)
P2 Pd2 C39 C40 -173.3(9)
Pd2 C39 C40 C41 -9.0(13)
Pd2 O4 C41 C40 -1.4(9)
Pd2 O4 C41 C42 179.3(7)
C39 C40 C41 O4 7.1(14)
C39 C40 C41 C42 -173.5(10)
C3 N1 C1 C21 123.5(5)
Pd1 N1 C1 C21 -52.7(6)
C3 N1 C1 C22 -113.5(5)
Pd1 N1 C1 C22 70.3(6)
C3 N1 C1 C2 4.5(6)
Pd1 N1 C1 C2 -171.6(4)
C3 O1 C2 C1 9.5(6)
C21 C1 C2 O1 -126.0(6)
N1 C1 C2 O1 -8.3(6)
C22 C1 C2 O1 106.3(6)
C1 N1 C3 O1 1.6(7)
Pd1 N1 C3 O1 178.4(3)
C1 N1 C3 C4 -177.8(5)
Pd1 N1 C3 C4 -1.0(7)
C2 O1 C3 N1 -7.4(7)
C2 O1 C3 C4 172.1(5)
N1 C3 C4 P1 -6.4(7)
O1 C3 C4 P1 174.1(4)
C11 P1 C4 C3 136.3(4)
C5 P1 C4 C3 -108.9(4)
Pd1 P1 C4 C3 9.8(4)
C5 P1 C11 C16 44.5(5)
C4 P1 C11 C16 158.7(4)
Pd1 P1 C11 C16 -84.3(5)
C5 P1 C11 C12 -142.2(5)
C4 P1 C11 C12 -28.0(5)
Pd1 P1 C11 C12 89.0(5)
C16 C11 C12 C13 0.5(9)
P1 C11 C12 C13 -172.9(5)
C11 C12 C13 C14 -0.1(11)
C12 C13 C14 C15 -1.1(12)
C13 C14 C15 C16 1.9(11)
C12 C11 C16 C15 0.3(9)
P1 C11 C16 C15 173.8(5)
C14 C15 C16 C11 -1.4(10)
C11 P1 C5 C10 -145.9(5)
C4 P1 C5 C10 99.4(5)
Pd1 P1 C5 C10 -13.5(5)
C11 P1 C5 C6 38.0(5)
C4 P1 C5 C6 -76.6(5)
Pd1 P1 C5 C6 170.5(4)
C10 C5 C6 C7 -0.3(9)
P1 C5 C6 C7 175.6(4)
C5 C6 C7 C8 1.0(9)
C6 C7 C8 C9 -1.6(11)
C7 C8 C9 C10 1.6(11)
C6 C5 C10 C9 0.3(9)
P1 C5 C10 C9 -175.8(5)
C8 C9 C10 C5 -1.0(11)
N1 Pd1 C17 C18 167(4)
O2 Pd1 C17 C18 -21.8(4)
P1 Pd1 C17 C18 154.6(4)
Pd1 C17 C18 C19 27.2(6)
Pd1 O2 C19 C20 175.9(4)
Pd1 O2 C19 C18 -2.8(7)
C17 C18 C19 O2 -17.0(8)
C17 C18 C19 C20 164.4(6)
O6 S1 C45 F1 -61.9(10)
O5 S1 C45 F1 61.5(10)
O7 S1 C45 F1 177.6(9)
O6 S1 C45 F2 175.0(7)
O5 S1 C45 F2 -61.6(8)
O7 S1 C45 F2 54.4(8)
O6 S1 C45 F3 60.2(9)
O5 S1 C45 F3 -176.4(8)
O7 S1 C45 F3 -60.4(9)
O10 S2 C46 F6 168.9(8)
O8 S2 C46 F6 -45.4(10)
O9 S2 C46 F6 52.3(9)
O10 S2 C46 F4 40.6(11)
O8 S2 C46 F4 -173.7(9)
O9 S2 C46 F4 -76.0(10)
O10 S2 C46 F5 -65.9(9)
O8 S2 C46 F5 79.8(9)
O9 S2 C46 F5 177.5(8)
