#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:31:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004885.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_7004885
loop_
_publ_author_name
'Reisinger, Corinna M.'
'Nowack, Rüdiger J'
'Volkmer, Dirk'
'Rieger, Bernhard'
_publ_section_title
;
 Novel palladium complexes employing mixed phosphine phosphonates and
 phosphine phosphinates as anionic chelating [P,O] ligands.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              272
_journal_page_last               278
_journal_paper_doi               10.1039/b612694d
_journal_year                    2007
_chemical_compound_source        Synthesis
_chemical_formula_moiety         C29H30O4P2Pd
_chemical_formula_sum            'C101 H106 O12 P6 Pd3'
_chemical_formula_weight         2016.88
_chemical_name_common            (Phosphinephosphonate)Pd(DCP-OMe)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.955(3)
_cell_length_b                   33.696(7)
_cell_length_c                   18.155(4)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.25
_cell_volume                     9303(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            72578
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         2.25
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4144
_exptl_crystal_recrystallization_method 'recrystallised from toluene'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.593
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         17313
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0909
_refine_ls_shift/su_max          1.986
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1719P)²+3.4379P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2618
_refine_ls_wR_factor_ref         0.2887
_reflns_number_gt                10260
_reflns_number_total             17313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b612694d.txt
_cod_data_source_block           rei568
_cod_original_cell_volume        9303(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7004885
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd -0.11863(5) 0.58056(2) -0.14756(4) 0.0616(2) Uani 1 1 d . . .
P1 P 0.00804(15) 0.58618(6) -0.23417(11) 0.0554(5) Uani 1 1 d . . .
P2 P 0.01736(15) 0.59550(6) -0.04641(11) 0.0527(5) Uani 1 1 d . . .
O1 O -0.0716(4) 0.5658(2) -0.2353(3) 0.0686(16) Uani 1 1 d . . .
O2 O 0.0017(5) 0.63141(18) -0.2251(3) 0.0718(17) Uani 1 1 d . . .
H2 H 0.0492 0.6421 -0.2180 0.108 Uiso 1 1 calc R . .
O3 O 0.0254(4) 0.57541(17) -0.3063(3) 0.0597(14) Uani 1 1 d . . .
O4 O -0.2189(7) 0.6650(3) -0.0621(8) 0.137(4) Uani 1 1 d . . .
C1 C 0.1014(5) 0.5694(2) -0.1427(4) 0.0496(17) Uani 1 1 d . . .
C2 C 0.1709(6) 0.5517(3) -0.1509(5) 0.062(2) Uani 1 1 d . . .
H2A H 0.1687 0.5503 -0.2040 0.074 Uiso 1 1 calc R . .
C3 C 0.2424(6) 0.5362(3) -0.0862(6) 0.072(2) Uani 1 1 d . . .
H3 H 0.2885 0.5241 -0.0943 0.087 Uiso 1 1 calc R . .
C4 C 0.2464(6) 0.5384(3) -0.0087(6) 0.070(2) Uani 1 1 d . . .
H4 H 0.2961 0.5281 0.0372 0.084 Uiso 1 1 calc R . .
C5 C 0.1769(6) 0.5560(2) 0.0028(5) 0.061(2) Uani 1 1 d . . .
H5 H 0.1793 0.5570 0.0561 0.073 Uiso 1 1 calc R . .
C6 C 0.1053(5) 0.5719(2) -0.0637(4) 0.0522(18) Uani 1 1 d . . .
C7 C 0.0488(6) 0.6473(2) -0.0253(5) 0.060(2) Uani 1 1 d . . .
C8 C 0.1274(10) 0.6614(3) -0.0161(11) 0.121(5) Uani 1 1 d . . .
H8 H 0.1665 0.6449 -0.0268 0.145 Uiso 1 1 calc R . .
C9 C 0.1498(11) 0.7007(4) 0.0094(11) 0.122(5) Uani 1 1 d . . .
H9 H 0.2055 0.7105 0.0171 0.147 Uiso 1 1 calc R . .
C10 C 0.0965(10) 0.7243(3) 0.0228(7) 0.095(4) Uani 1 1 d . . .
H10 H 0.1144 0.7505 0.0423 0.114 Uiso 1 1 calc R . .
C11 C 0.0180(10) 0.7116(3) 0.0093(8) 0.096(4) Uani 1 1 d . . .
H11 H -0.0219 0.7292 0.0160 0.115 Uiso 1 1 calc R . .
C12 C -0.0070(9) 0.6734(3) -0.0143(7) 0.087(3) Uani 1 1 d . . .
H12 H -0.0639 0.6647 -0.0233 0.104 Uiso 1 1 calc R . .
C13 C 0.0352(6) 0.5766(2) 0.0534(5) 0.063(2) Uani 1 1 d . . .
C14 C -0.0054(7) 0.5411(3) 0.0575(6) 0.067(2) Uani 1 1 d . . .
H14 H -0.0461 0.5287 0.0082 0.081 Uiso 1 1 calc R . .
C15 C 0.0128(8) 0.5238(3) 0.1317(7) 0.083(3) Uani 1 1 d . . .
H15 H -0.0169 0.5002 0.1330 0.099 Uiso 1 1 calc R . .
C16 C 0.0720(11) 0.5397(4) 0.2029(8) 0.102(4) Uani 1 1 d . . .
H16 H 0.0840 0.5272 0.2536 0.122 Uiso 1 1 calc R . .
C17 C 0.1156(10) 0.5747(4) 0.2018(6) 0.103(4) Uani 1 1 d . . .
H17 H 0.1574 0.5859 0.2520 0.123 Uiso 1 1 calc R . .
C18 C 0.0986(8) 0.5934(3) 0.1278(6) 0.081(3) Uani 1 1 d . . .
H18 H 0.1289 0.6170 0.1271 0.097 Uiso 1 1 calc R . .
C19 C -0.2348(7) 0.5383(4) -0.1981(8) 0.099(4) Uani 1 1 d . . .
H19 H -0.1922 0.5178 -0.1831 0.118 Uiso 1 1 calc R . .
C20 C -0.2544(9) 0.5644(5) -0.2634(7) 0.120(5) Uani 1 1 d . . .
H20 H -0.2229 0.5655 -0.2955 0.144 Uiso 1 1 calc R . .
C21 C -0.3311(10) 0.5904(7) -0.2768(9) 0.168(9) Uani 1 1 d . . .
H21A H -0.3822 0.5839 -0.3295 0.202 Uiso 1 1 calc R . .
H21B H -0.3159 0.6187 -0.2776 0.202 Uiso 1 1 calc R . .
C22 C -0.3521(8) 0.5817(4) -0.2027(7) 0.101(4) Uani 1 1 d . . .
H22 H -0.4151 0.5736 -0.2233 0.121 Uiso 1 1 calc R . .
C23 C -0.2913(8) 0.5473(4) -0.1542(7) 0.087(3) Uani 1 1 d . . .
H23 H -0.3255 0.5235 -0.1520 0.105 Uiso 1 1 calc R . .
C24 C -0.1764(6) 0.5969(3) -0.0748(5) 0.065(2) Uani 1 1 d . . .
H24 H -0.1315 0.6045 -0.0186 0.079 Uiso 1 1 calc R . .
C25 C -0.2387(7) 0.5647(3) -0.0707(6) 0.076(3) Uani 1 1 d . . .
H25 H -0.2096 0.5447 -0.0263 0.091 Uiso 1 1 calc R . .
C26 C -0.3096(8) 0.5900(4) -0.0606(8) 0.092(3) Uani 1 1 d . . .
H26A H -0.3606 0.5742 -0.0649 0.110 Uiso 1 1 calc R . .
H26B H -0.2856 0.6059 -0.0095 0.110 Uiso 1 1 calc R . .
C27 C -0.3297(8) 0.6150(4) -0.1373(7) 0.098(4) Uani 1 1 d . . .
H27 H -0.3770 0.6353 -0.1500 0.117 Uiso 1 1 calc R . .
C28 C -0.2388(8) 0.6322(3) -0.1180(8) 0.094(3) Uani 1 1 d . . .
H28 H -0.2347 0.6401 -0.1694 0.113 Uiso 1 1 calc R . .
C29 C -0.2535(15) 0.6994(5) -0.0934(17) 0.196(11) Uani 1 1 d . . .
H29A H -0.2228 0.7105 -0.1235 0.293 Uiso 1 1 calc R . .
H29B H -0.2477 0.7176 -0.0491 0.293 Uiso 1 1 calc R . .
H29C H -0.3159 0.6959 -0.1310 0.293 Uiso 1 1 calc R . .
Pd2 Pd 0.22687(6) 0.67094(2) -0.43369(6) 0.0804(3) Uani 1 1 d . . .
P3 P 0.09393(16) 0.66430(6) -0.35782(12) 0.0568(5) Uani 1 1 d . . .
P4 P 0.0995(2) 0.65206(6) -0.54025(15) 0.0727(7) Uani 1 1 d . . .
O5 O 0.1697(4) 0.68764(18) -0.3562(4) 0.0716(16) Uani 1 1 d . . .
O6 O 0.1128(4) 0.61960(16) -0.3557(3) 0.0620(14) Uani 1 1 d . . .
H6 H 0.0698 0.6068 -0.3567 0.093 Uiso 1 1 calc R . .
O7 O 0.0690(6) 0.67703(18) -0.2903(4) 0.082(2) Uani 1 1 d . . .
C30 C 0.0003(6) 0.6734(2) -0.4544(5) 0.057(2) Uani 1 1 d . . .
C31 C -0.0775(8) 0.6847(3) -0.4534(8) 0.084(3) Uani 1 1 d . . .
H31 H -0.0791 0.6875 -0.4020 0.101 Uiso 1 1 calc R . .
C32 C -0.1520(9) 0.6920(4) -0.5238(12) 0.112(5) Uani 1 1 d . . .
H32 H -0.2043 0.7002 -0.5211 0.134 Uiso 1 1 calc R . .
C33 C -0.1509(10) 0.6876(4) -0.5957(12) 0.131(7) Uani 1 1 d . . .
H33 H -0.2028 0.6925 -0.6448 0.157 Uiso 1 1 calc R . .
C34 C -0.0755(10) 0.6760(4) -0.6000(8) 0.113(5) Uani 1 1 d . . .
H34 H -0.0762 0.6729 -0.6523 0.136 Uiso 1 1 calc R . .
C35 C 0.0009(6) 0.6688(2) -0.5306(5) 0.067(2) Uani 1 1 d . . .
C36 C 0.0817(8) 0.5988(3) -0.5609(6) 0.075(3) Uani 1 1 d . . .
C37 C 0.0040(12) 0.5845(4) -0.6150(15) 0.156(8) Uani 1 1 d . . .
H37 H -0.0437 0.6025 -0.6404 0.187 Uiso 1 1 calc R . .
C38 C -0.0109(12) 0.5420(4) -0.6370(11) 0.135(6) Uani 1 1 d . . .
H38 H -0.0628 0.5320 -0.6808 0.162 Uiso 1 1 calc R . .
C39 C 0.0595(11) 0.5182(3) -0.5863(8) 0.103(4) Uani 1 1 d . . .
H39 H 0.0516 0.4903 -0.5854 0.123 Uiso 1 1 calc R . .
C40 C 0.1321(13) 0.5330(4) -0.5425(10) 0.180(11) Uani 1 1 d . . .
H40 H 0.1803 0.5155 -0.5149 0.216 Uiso 1 1 calc R . .
C41 C 0.1475(12) 0.5737(4) -0.5312(10) 0.168(10) Uani 1 1 d . . .
H41 H 0.2059 0.5833 -0.5018 0.201 Uiso 1 1 calc R . .
C42 C 0.0843(13) 0.6752(3) -0.6369(7) 0.127(6) Uani 1 1 d . . .
C43 C 0.1005(18) 0.7149(4) -0.6345(10) 0.188(11) Uani 1 1 d . . .
H43 H 0.1185 0.7286 -0.5838 0.226 Uiso 1 1 calc R . .
C44 C 0.092(2) 0.7361(5) -0.7030(11) 0.242(16) Uani 1 1 d . . .
H44 H 0.1001 0.7640 -0.7011 0.290 Uiso 1 1 calc R . .
C45 C 0.071(4) 0.7155(6) -0.7715(15) 0.44(4) Uani 1 1 d . . .
H45 H 0.0760 0.7280 -0.8160 0.527 Uiso 1 1 calc R . .
C46 C 0.042(3) 0.6768(5) -0.7806(13) 0.28(2) Uani 1 1 d . . .
H46 H 0.0126 0.6647 -0.8331 0.336 Uiso 1 1 calc R . .
C47 C 0.0573(16) 0.6563(4) -0.7080(9) 0.156(8) Uani 1 1 d . . .
H47 H 0.0484 0.6284 -0.7099 0.187 Uiso 1 1 calc R . .
C48 C 0.3399(9) 0.7157(4) -0.3658(8) 0.102(4) Uiso 1 1 d D . .
H48 H 0.2921 0.7337 -0.3806 0.123 Uiso 1 1 calc R . .
C49 C 0.3627(13) 0.6882(5) -0.3041(10) 0.148(6) Uiso 1 1 d D . .
H49 H 0.3227 0.6817 -0.2822 0.177 Uiso 1 1 calc R . .
C50 C 0.4474(15) 0.6689(7) -0.2722(14) 0.197(9) Uiso 1 1 d D . .
H50A H 0.4442 0.6400 -0.2639 0.237 Uiso 1 1 calc R . .
H50B H 0.4916 0.6815 -0.2215 0.237 Uiso 1 1 calc R . .
C51 C 0.4614(17) 0.6789(7) -0.3494(14) 0.186(9) Uiso 1 1 d D . .
H51 H 0.5223 0.6901 -0.3261 0.224 Uiso 1 1 calc R . .
C52 C 0.4007(15) 0.7140(7) -0.4078(13) 0.186(8) Uiso 1 1 d D . .
H52 H 0.4321 0.7392 -0.4067 0.223 Uiso 1 1 calc R . .
C53 C 0.2897(15) 0.6575(7) -0.5064(15) 0.182(8) Uiso 1 1 d D . .
H53 H 0.2536 0.6477 -0.5637 0.218 Uiso 1 1 calc R . .
C54 C 0.335(2) 0.6996(9) -0.494(2) 0.39(3) Uiso 1 1 d D . .
H54 H 0.2990 0.7207 -0.5328 0.463 Uiso 1 1 calc R . .
C55 C 0.405(2) 0.6814(10) -0.5111(17) 0.244(13) Uiso 1 1 d D . .
H55A H 0.4438 0.7015 -0.5179 0.292 Uiso 1 1 calc R . .
H55B H 0.3810 0.6635 -0.5593 0.292 Uiso 1 1 calc R . .
C56 C 0.450(2) 0.6587(9) -0.4294(17) 0.33(2) Uiso 1 1 d D . .
H56 H 0.5031 0.6433 -0.4236 0.393 Uiso 1 1 calc R . .
C57 C 0.3690(16) 0.6328(8) -0.4488(16) 0.190(9) Uiso 1 1 d D . .
H57 H 0.3650 0.6179 -0.4029 0.229 Uiso 1 1 calc R . .
O8 O 0.361(3) 0.6112(15) -0.520(2) 0.49(3) Uiso 1 1 d D . .
C58 C 0.377(4) 0.5770(17) -0.470(4) 0.48(4) Uiso 1 1 d D . .
H58A H 0.3990 0.5849 -0.4127 0.718 Uiso 1 1 calc R . .
H58B H 0.4207 0.5604 -0.4770 0.718 Uiso 1 1 calc R . .
H58C H 0.3221 0.5620 -0.4870 0.718 Uiso 1 1 calc R . .
Pd3 Pd 0.51872(5) 0.58954(2) -0.77873(4) 0.0782(3) Uani 1 1 d . . .
P5 P 0.49721(16) 0.51516(7) -0.89146(15) 0.0699(7) Uani 1 1 d . . .
P6 P 0.65332(16) 0.56201(7) -0.72923(13) 0.0682(6) Uani 1 1 d . . .
O9 O 0.4532(4) 0.5397(2) -0.8517(4) 0.082(2) Uani 1 1 d . . .
O10 O 0.4373(4) 0.4857(2) -0.9524(4) 0.0824(19) Uani 1 1 d . . .
O11 O 0.5405(4) 0.54295(18) -0.9299(4) 0.0757(18) Uani 1 1 d . . .
H11A H 0.5706 0.5295 -0.9473 0.114 Uiso 1 1 calc R . .
O12 O 0.6358(8) 0.6963(3) -0.7333(8) 0.169(6) Uani 1 1 d . . .
C59 C 0.5867(7) 0.4890(3) -0.8114(6) 0.071(2) Uani 1 1 d . . .
C60 C 0.5929(8) 0.4487(3) -0.8188(7) 0.086(3) Uani 1 1 d . . .
H60 H 0.5485 0.4356 -0.8649 0.103 Uiso 1 1 calc R . .
C61 C 0.6604(11) 0.4264(4) -0.7627(10) 0.109(4) Uani 1 1 d . . .
H61 H 0.6638 0.3987 -0.7700 0.131 Uiso 1 1 calc R . .
C62 C 0.7241(11) 0.4459(5) -0.6942(10) 0.123(5) Uani 1 1 d . . .
H62 H 0.7703 0.4311 -0.6531 0.147 Uiso 1 1 calc R . .
C63 C 0.7205(9) 0.4859(4) -0.6858(7) 0.099(4) Uani 1 1 d . . .
H63 H 0.7658 0.4987 -0.6401 0.119 Uiso 1 1 calc R . .
C64 C 0.6525(6) 0.5082(3) -0.7421(6) 0.073(2) Uani 1 1 d . . .
C65 C 0.7249(7) 0.5797(3) -0.7743(5) 0.076(3) Uani 1 1 d . . .
C66 C 0.7309(11) 0.6201(5) -0.7848(9) 0.121(5) Uani 1 1 d . . .
H66 H 0.6972 0.6384 -0.7707 0.145 Uiso 1 1 calc R . .
C67 C 0.7869(12) 0.6331(6) -0.8162(9) 0.128(6) Uani 1 1 d . . .
H67 H 0.7947 0.6608 -0.8200 0.154 Uiso 1 1 calc R . .
C68 C 0.8294(16) 0.6084(7) -0.8407(9) 0.149(8) Uani 1 1 d . . .
H68 H 0.8646 0.6188 -0.8648 0.179 Uiso 1 1 calc R . .
C69 C 0.8258(15) 0.5700(7) -0.8336(15) 0.173(9) Uani 1 1 d . . .
H69 H 0.8604 0.5526 -0.8486 0.207 Uiso 1 1 calc R . .
C70 C 0.7645(12) 0.5544(5) -0.8008(11) 0.134(5) Uani 1 1 d . . .
H70 H 0.7549 0.5267 -0.7995 0.160 Uiso 1 1 calc R . .
C71 C 0.7160(6) 0.5691(3) -0.6190(6) 0.077(3) Uani 1 1 d . . .
C72 C 0.6720(9) 0.5618(5) -0.5732(7) 0.114(5) Uani 1 1 d . . .
H72 H 0.6114 0.5549 -0.5984 0.137 Uiso 1 1 calc R . .
C73 C 0.7199(11) 0.5650(6) -0.4859(7) 0.145(7) Uani 1 1 d . . .
H73 H 0.6914 0.5597 -0.4522 0.174 Uiso 1 1 calc R . .
C74 C 0.8046(10) 0.5755(4) -0.4517(7) 0.116(5) Uani 1 1 d . . .
H74 H 0.8349 0.5781 -0.3937 0.139 Uiso 1 1 calc R . .
C75 C 0.8489(8) 0.5825(3) -0.4974(6) 0.083(3) Uani 1 1 d . . .
H75 H 0.9093 0.5898 -0.4720 0.100 Uiso 1 1 calc R . .
C76 C 0.8026(7) 0.5788(3) -0.5830(5) 0.074(3) Uani 1 1 d . . .
H76 H 0.8322 0.5832 -0.6162 0.089 Uiso 1 1 calc R . .
C77 C 0.3805(13) 0.6194(6) -0.8515(12) 0.160(10) Uani 1 1 d . . .
H77 H 0.3796 0.6017 -0.8925 0.192 Uiso 1 1 calc R . .
C78 C 0.3916(12) 0.6085(7) -0.7767(19) 0.184(11) Uani 1 1 d . . .
H78 H 0.3884 0.5821 -0.7599 0.221 Uiso 1 1 calc R . .
C79 C 0.4105(16) 0.6458(6) -0.7218(13) 0.163(8) Uani 1 1 d . . .
H79 H 0.3745 0.6468 -0.6907 0.195 Uiso 1 1 calc R . .
C80 C 0.4009(14) 0.6796(5) -0.7697(13) 0.164(9) Uani 1 1 d . . .
H80 H 0.3559 0.6981 -0.7675 0.196 Uiso 1 1 calc R . .
C81 C 0.3699(14) 0.6617(6) -0.8613(12) 0.167(8) Uani 1 1 d . . .
H81A H 0.3077 0.6685 -0.8968 0.200 Uiso 1 1 calc R . .
H81B H 0.4067 0.6724 -0.8864 0.200 Uiso 1 1 calc R . .
C82 C 0.5709(9) 0.6398(3) -0.7116(7) 0.112(5) Uani 1 1 d . . .
H82 H 0.6356 0.6361 -0.6780 0.134 Uiso 1 1 calc R . .
C83 C 0.5550(11) 0.6761(3) -0.7638(9) 0.118(5) Uani 1 1 d . . .
H83 H 0.5284 0.6706 -0.8241 0.142 Uiso 1 1 calc R . .
C84 C 0.4980(17) 0.7014(5) -0.7371(14) 0.174(9) Uani 1 1 d . . .
H84 H 0.4953 0.7301 -0.7521 0.209 Uiso 1 1 calc R . .
C85 C 0.5222(16) 0.6944(6) -0.6539(14) 0.197(11) Uani 1 1 d . . .
H85A H 0.4766 0.7033 -0.6376 0.236 Uiso 1 1 calc R . .
H85B H 0.5792 0.7069 -0.6179 0.236 Uiso 1 1 calc R . .
C86 C 0.5288(16) 0.6492(5) -0.6553(9) 0.157(8) Uani 1 1 d . . .
H86 H 0.5521 0.6350 -0.6014 0.188 Uiso 1 1 calc R . .
C87 C 0.6400(19) 0.7257(6) -0.7856(15) 0.252(17) Uani 1 1 d . . .
H87A H 0.6137 0.7157 -0.8421 0.378 Uiso 1 1 calc R . .
H87B H 0.7015 0.7328 -0.7691 0.378 Uiso 1 1 calc R . .
H87C H 0.6076 0.7492 -0.7824 0.378 Uiso 1 1 calc R . .
C88 C 0.2781(15) 0.6625(12) -1.116(2) 0.261(18) Uiso 1 1 d D . .
H88A H 0.2616 0.6453 -1.0815 0.391 Uiso 1 1 calc R . .
H88B H 0.2549 0.6514 -1.1715 0.391 Uiso 1 1 calc R . .
H88C H 0.2537 0.6891 -1.1181 0.391 Uiso 1 1 calc R . .
C89 C 0.3710(12) 0.6649(6) -1.0819(10) 0.28(2) Uani 1 1 d GD . .
C90 C 0.4113(17) 0.6991(5) -1.0919(9) 0.207(14) Uani 1 1 d G . .
H90 H 0.3765 0.7208 -1.1222 0.249 Uiso 1 1 calc R . .
C91 C 0.5024(17) 0.7014(4) -1.0573(12) 0.237(16) Uani 1 1 d G . .
H91 H 0.5299 0.7248 -1.0641 0.285 Uiso 1 1 calc R . .
C92 C 0.5534(12) 0.6696(6) -1.0129(11) 0.195(10) Uani 1 1 d G . .
H92 H 0.6157 0.6712 -0.9892 0.234 Uiso 1 1 calc R . .
C93 C 0.5132(15) 0.6354(4) -1.0029(9) 0.208(13) Uani 1 1 d G . .
H93 H 0.5480 0.6136 -0.9726 0.249 Uiso 1 1 calc R . .
C94 C 0.4220(15) 0.6330(4) -1.0375(11) 0.210(15) Uani 1 1 d G . .
H94 H 0.3945 0.6097 -1.0307 0.252 Uiso 1 1 calc R . .
C95 C -0.103(4) 0.7127(17) -0.1953(17) 0.60(6) Uiso 1 1 d D . .
H95A H -0.0713 0.7376 -0.1737 0.901 Uiso 1 1 calc R . .
H95B H -0.0611 0.6908 -0.1823 0.901 Uiso 1 1 calc R . .
H95C H -0.1429 0.7077 -0.1703 0.901 Uiso 1 1 calc R . .
C96 C -0.1553(13) 0.7159(8) -0.2863(11) 0.27(2) Uani 1 1 d GD . .
C97 C -0.2102(19) 0.6835(6) -0.3201(17) 0.242(16) Uani 1 1 d GD . .
H97 H -0.1964 0.6586 -0.2925 0.291 Uiso 1 1 calc R . .
C98 C -0.2852(15) 0.6874(9) -0.3942(19) 0.40(4) Uani 1 1 d G . .
H98 H -0.3226 0.6652 -0.4173 0.484 Uiso 1 1 calc R . .
C99 C -0.3053(14) 0.7237(11) -0.4345(14) 1.02(16) Uani 1 1 d G . .
H99 H -0.3565 0.7264 -0.4852 1.229 Uiso 1 1 calc R . .
C100 C -0.250(2) 0.7562(7) -0.4008(16) 0.43(4) Uani 1 1 d G . .
H100 H -0.2642 0.7810 -0.4283 0.512 Uiso 1 1 calc R . .
C101 C -0.1755(19) 0.7523(6) -0.3266(17) 0.49(5) Uani 1 1 d GD . .
H101 H -0.1380 0.7745 -0.3035 0.592 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C24 Pd1 O1 173.4(3) . . ?
C24 Pd1 C19 81.5(4) . . ?
O1 Pd1 C19 95.5(4) . . ?
C24 Pd1 P2 91.3(3) . . ?
O1 Pd1 P2 94.27(17) . . ?
C19 Pd1 P2 148.5(4) . . ?
C24 Pd1 C20 94.6(5) . . ?
O1 Pd1 C20 79.8(4) . . ?
C19 Pd1 C20 34.6(5) . . ?
P2 Pd1 C20 174.0(4) . . ?
O3 P1 O1 113.3(3) . . ?
O3 P1 O2 112.4(3) . . ?
O1 P1 O2 110.3(4) . . ?
O3 P1 C1 107.2(4) . . ?
O1 P1 C1 106.6(3) . . ?
O2 P1 C1 106.6(3) . . ?
C13 P2 C7 102.8(4) . . ?
C13 P2 C6 103.2(4) . . ?
C7 P2 C6 105.6(4) . . ?
C13 P2 Pd1 112.9(3) . . ?
C7 P2 Pd1 118.7(3) . . ?
C6 P2 Pd1 112.1(2) . . ?
P1 O1 Pd1 120.8(3) . . ?
C29 O4 C28 117.0(16) . . ?
C2 C1 C6 118.3(7) . . ?
C2 C1 P1 118.5(6) . . ?
C6 C1 P1 123.1(6) . . ?
C3 C2 C1 123.1(8) . . ?
C2 C3 C4 118.8(10) . . ?
C3 C4 C5 120.2(8) . . ?
C6 C5 C4 120.0(8) . . ?
C5 C6 C1 119.5(8) . . ?
C5 C6 P2 118.9(6) . . ?
C1 C6 P2 121.6(6) . . ?
C8 C7 C12 117.7(9) . . ?
C8 C7 P2 122.9(8) . . ?
C12 C7 P2 119.3(8) . . ?
C7 C8 C9 118.7(13) . . ?
C10 C9 C8 121.9(14) . . ?
C9 C10 C11 119.6(11) . . ?
C10 C11 C12 121.1(12) . . ?
C11 C12 C7 120.7(12) . . ?
C14 C13 C18 118.3(8) . . ?
C14 C13 P2 118.9(6) . . ?
C18 C13 P2 122.2(7) . . ?
C15 C14 C13 120.8(9) . . ?
C16 C15 C14 121.5(11) . . ?
C15 C16 C17 119.7(10) . . ?
C18 C17 C16 120.7(12) . . ?
C17 C18 C13 119.0(11) . . ?
C20 C19 C23 110.7(12) . . ?
C20 C19 Pd1 77.7(8) . . ?
C23 C19 Pd1 107.4(7) . . ?
C19 C20 C21 111.8(13) . . ?
C19 C20 Pd1 67.7(6) . . ?
C21 C20 Pd1 116.0(11) . . ?
C20 C21 C22 105.1(12) . . ?
C23 C22 C27 103.3(9) . . ?
C23 C22 C21 106.5(12) . . ?
C27 C22 C21 116.6(13) . . ?
C25 C23 C19 112.2(9) . . ?
C25 C23 C22 103.4(10) . . ?
C19 C23 C22 105.4(10) . . ?
C25 C24 C28 103.6(9) . . ?
C25 C24 Pd1 112.2(6) . . ?
C28 C24 Pd1 107.1(7) . . ?
C23 C25 C24 110.0(8) . . ?
C23 C25 C26 101.0(9) . . ?
C24 C25 C26 101.7(8) . . ?
C27 C26 C25 93.9(9) . . ?
C28 C27 C26 101.7(10) . . ?
C28 C27 C22 109.2(11) . . ?
C26 C27 C22 100.2(10) . . ?
O4 C28 C27 110.4(11) . . ?
O4 C28 C24 109.6(10) . . ?
C27 C28 C24 102.6(9) . . ?
C53 Pd2 O5 176.1(7) . . ?
C53 Pd2 P4 87.7(7) . . ?
O5 Pd2 P4 95.66(18) . . ?
C53 Pd2 C48 86.8(8) . . ?
O5 Pd2 C48 89.3(4) . . ?
P4 Pd2 C48 152.8(3) . . ?
C53 Pd2 C49 97.4(8) . . ?
O5 Pd2 C49 79.4(5) . . ?
P4 Pd2 C49 173.4(4) . . ?
C48 Pd2 C49 32.5(4) . . ?
O5 P3 O7 112.2(4) . . ?
O5 P3 O6 110.3(4) . . ?
O7 P3 O6 112.6(3) . . ?
O5 P3 C30 108.0(4) . . ?
O7 P3 C30 107.3(4) . . ?
O6 P3 C30 106.0(3) . . ?
C42 P4 C36 106.2(5) . . ?
C42 P4 C35 102.2(6) . . ?
C36 P4 C35 104.2(5) . . ?
C42 P4 Pd2 112.1(6) . . ?
C36 P4 Pd2 117.3(4) . . ?
C35 P4 Pd2 113.3(3) . . ?
P3 O5 Pd2 119.4(3) . . ?
C31 C30 C35 118.0(9) . . ?
C31 C30 P3 118.1(8) . . ?
C35 C30 P3 123.9(7) . . ?
C32 C31 C30 122.1(13) . . ?
C33 C32 C31 119.5(14) . . ?
C32 C33 C34 120.6(13) . . ?
C33 C34 C35 121.5(15) . . ?
C34 C35 C30 118.2(12) . . ?
C34 C35 P4 119.6(10) . . ?
C30 C35 P4 122.2(7) . . ?
C41 C36 C37 117.0(11) . . ?
C41 C36 P4 121.0(11) . . ?
C37 C36 P4 121.4(10) . . ?
C36 C37 C38 122.8(15) . . ?
C39 C38 C37 112.6(15) . . ?
C40 C39 C38 120.8(12) . . ?
C39 C40 C41 123.9(14) . . ?
C36 C41 C40 120.3(16) . . ?
C47 C42 C43 118.7(11) . . ?
C47 C42 P4 124.8(9) . . ?
C43 C42 P4 116.4(9) . . ?
C42 C43 C44 122.5(14) . . ?
C45 C44 C43 116.8(15) . . ?
C44 C45 C46 122.7(16) . . ?
C45 C46 C47 116(2) . . ?
C42 C47 C46 121.2(14) . . ?
C49 C48 C52 111.8(15) . . ?
C49 C48 Pd2 82.1(10) . . ?
C52 C48 Pd2 106.8(12) . . ?
C48 C49 C50 120.2(18) . . ?
C48 C49 Pd2 65.3(9) . . ?
C50 C49 Pd2 127.3(15) . . ?
C49 C50 C51 93.6(18) . . ?
C56 C51 C50 139(2) . . ?
C56 C51 C52 85.8(19) . . ?
C50 C51 C52 116.2(19) . . ?
C48 C52 C54 100(2) . . ?
C48 C52 C51 94.3(15) . . ?
C54 C52 C51 114(2) . . ?
C57 C53 C54 100(2) . . ?
C57 C53 Pd2 103.1(17) . . ?
C54 C53 Pd2 93.6(19) . . ?
C55 C54 C52 93(2) . . ?
C55 C54 C53 89(2) . . ?
C52 C54 C53 121(3) . . ?
C54 C55 C56 96.0(17) . . ?
C57 C56 C51 101(2) . . ?
C57 C56 C55 93(2) . . ?
C51 C56 C55 119(2) . . ?
O8 C57 C53 87(3) . . ?
O8 C57 C56 103(3) . . ?
C53 C57 C56 106(2) . . ?
C58 O8 C57 86(4) . . ?
C82 Pd3 O9 174.8(4) . . ?
C82 Pd3 P6 90.5(4) . . ?
O9 Pd3 P6 94.68(19) . . ?
C82 Pd3 C78 85.4(7) . . ?
O9 Pd3 C78 89.7(6) . . ?
P6 Pd3 C78 156.1(9) . . ?
C82 Pd3 C77 92.4(6) . . ?
O9 Pd3 C77 82.6(5) . . ?
P6 Pd3 C77 170.1(6) . . ?
C78 Pd3 C77 33.7(8) . . ?
O9 P5 O10 113.8(4) . . ?
O9 P5 O11 108.9(4) . . ?
O10 P5 O11 111.9(4) . . ?
O9 P5 C59 107.6(4) . . ?
O10 P5 C59 109.0(4) . . ?
O11 P5 C59 105.3(4) . . ?
C71 P6 C64 103.8(5) . . ?
C71 P6 C65 105.5(5) . . ?
C64 P6 C65 103.5(5) . . ?
C71 P6 Pd3 112.4(4) . . ?
C64 P6 Pd3 114.2(3) . . ?
C65 P6 Pd3 116.2(4) . . ?
P5 O9 Pd3 120.2(4) . . ?
C87 O12 C83 114.2(14) . . ?
C60 C59 C64 118.3(10) . . ?
C60 C59 P5 118.6(8) . . ?
C64 C59 P5 123.1(7) . . ?
C61 C60 C59 122.8(12) . . ?
C60 C61 C62 117.9(12) . . ?
C63 C62 C61 120.6(12) . . ?
C62 C63 C64 121.5(12) . . ?
C63 C64 C59 118.8(10) . . ?
C63 C64 P6 119.3(8) . . ?
C59 C64 P6 121.7(7) . . ?
C70 C65 C66 120.7(14) . . ?
C70 C65 P6 120.3(11) . . ?
C66 C65 P6 118.9(11) . . ?
C67 C66 C65 118.3(16) . . ?
C68 C67 C66 121.8(18) . . ?
C67 C68 C69 122.9(18) . . ?
C68 C69 C70 117.2(19) . . ?
C65 C70 C69 118.6(16) . . ?
C76 C71 C72 121.1(9) . . ?
C76 C71 P6 122.9(9) . . ?
C72 C71 P6 115.9(8) . . ?
C71 C72 C73 117.8(12) . . ?
C74 C73 C72 120.2(15) . . ?
C73 C74 C75 122.0(11) . . ?
C74 C75 C76 118.0(11) . . ?
C71 C76 C75 120.7(11) . . ?
C78 C77 C81 110.5(19) . . ?
C78 C77 Pd3 69.7(10) . . ?
C81 C77 Pd3 122.2(15) . . ?
C77 C78 C79 109(2) . . ?
C77 C78 Pd3 76.6(14) . . ?
C79 C78 Pd3 108.2(13) . . ?
C80 C79 C78 109(2) . . ?
C80 C79 C86 98.7(18) . . ?
C78 C79 C86 109.4(13) . . ?
C79 C80 C81 103.2(15) . . ?
C79 C80 C84 108.4(17) . . ?
C81 C80 C84 111(2) . . ?
C77 C81 C80 106.1(16) . . ?
C83 C82 C86 104.4(12) . . ?
C83 C82 Pd3 113.0(8) . . ?
C86 C82 Pd3 111.5(11) . . ?
O12 C83 C82 106.0(11) . . ?
O12 C83 C84 104.4(14) . . ?
C82 C83 C84 102.7(15) . . ?
C85 C84 C83 108.9(17) . . ?
C85 C84 C80 95(2) . . ?
C83 C84 C80 108.0(14) . . ?
C84 C85 C86 98.0(14) . . ?
C82 C86 C85 106.2(17) . . ?
C82 C86 C79 104.3(11) . . ?
C85 C86 C79 90.4(15) . . ?
C90 C89 C94 120.0 . . ?
C90 C89 C88 120(2) . . ?
C94 C89 C88 120(2) . . ?
C91 C90 C89 120.0 . . ?
C92 C91 C90 120.0 . . ?
C93 C92 C91 120.0 . . ?
C92 C93 C94 120.0 . . ?
C93 C94 C89 120.0 . . ?
C97 C96 C101 120.0 . . ?
C97 C96 C95 113(2) . . ?
C101 C96 C95 122(2) . . ?
C96 C97 C98 120.0 . . ?
C99 C98 C97 120.0 . . ?
C98 C99 C100 120.0 . . ?
C101 C100 C99 120.0 . . ?
C100 C101 C96 120.0 . . ?
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 C24 2.039(9) . ?
Pd1 O1 2.131(6) . ?
Pd1 C19 2.269(10) . ?
Pd1 P2 2.280(2) . ?
Pd1 C20 2.395(13) . ?
P1 O3 1.508(6) . ?
P1 O1 1.508(7) . ?
P1 O2 1.542(6) . ?
P1 C1 1.804(7) . ?
P2 C13 1.815(8) . ?
P2 C7 1.817(8) . ?
P2 C6 1.834(9) . ?
O4 C29 1.310(19) . ?
O4 C28 1.438(16) . ?
C1 C2 1.386(12) . ?
C1 C6 1.410(10) . ?
C2 C3 1.365(12) . ?
C3 C4 1.380(14) . ?
C4 C5 1.415(13) . ?
C5 C6 1.385(11) . ?
C7 C8 1.353(16) . ?
C7 C12 1.368(14) . ?
C8 C9 1.399(17) . ?
C9 C10 1.305(19) . ?
C10 C11 1.313(18) . ?
C11 C12 1.364(15) . ?
C13 C14 1.400(12) . ?
C13 C18 1.420(13) . ?
C14 C15 1.372(13) . ?
C15 C16 1.347(17) . ?
C16 C17 1.397(19) . ?
C17 C18 1.394(14) . ?
C19 C20 1.392(19) . ?
C19 C23 1.523(17) . ?
C20 C21 1.50(2) . ?
C21 C22 1.56(2) . ?
C22 C23 1.543(17) . ?
C22 C27 1.555(19) . ?
C23 C25 1.498(14) . ?
C24 C25 1.538(13) . ?
C24 C28 1.553(14) . ?
C25 C26 1.548(16) . ?
C26 C27 1.531(16) . ?
C27 C28 1.535(17) . ?
Pd2 C53 2.08(2) . ?
Pd2 O5 2.108(7) . ?
Pd2 P4 2.263(3) . ?
Pd2 C48 2.319(13) . ?
Pd2 C49 2.527(18) . ?
P3 O5 1.495(7) . ?
P3 O7 1.524(6) . ?
P3 O6 1.537(6) . ?
P3 C30 1.797(8) . ?
P4 C42 1.831(10) . ?
P4 C36 1.831(9) . ?
P4 C35 1.844(11) . ?
C30 C31 1.381(14) . ?
C30 C35 1.395(13) . ?
C31 C32 1.365(19) . ?
C32 C33 1.32(2) . ?
C33 C34 1.37(2) . ?
C34 C35 1.372(14) . ?
C36 C41 1.311(18) . ?
C36 C37 1.34(2) . ?
C37 C38 1.480(19) . ?
C38 C39 1.39(2) . ?
C39 C40 1.24(2) . ?
C40 C41 1.396(18) . ?
C42 C47 1.326(17) . ?
C42 C43 1.364(16) . ?
C43 C44 1.383(17) . ?
C44 C45 1.33(2) . ?
C45 C46 1.38(3) . ?
C46 C47 1.41(2) . ?
C48 C49 1.372(15) . ?
C48 C52 1.531(16) . ?
C49 C50 1.443(17) . ?
C50 C51 1.558(17) . ?
C51 C56 1.537(19) . ?
C51 C52 1.617(17) . ?
C52 C54 1.542(19) . ?
C53 C57 1.533(17) . ?
C53 C54 1.579(19) . ?
C54 C55 1.488(19) . ?
C55 C56 1.539(18) . ?
C56 C57 1.534(19) . ?
C57 O8 1.432(19) . ?
O8 C58 1.41(2) . ?
Pd3 C82 2.044(11) . ?
Pd3 O9 2.123(6) . ?
Pd3 P6 2.250(3) . ?
Pd3 C78 2.264(18) . ?
Pd3 C77 2.349(15) . ?
P5 O9 1.496(7) . ?
P5 O10 1.500(6) . ?
P5 O11 1.535(7) . ?
P5 C59 1.800(10) . ?
P6 C71 1.820(9) . ?
P6 C64 1.826(10) . ?
P6 C65 1.837(12) . ?
O12 C87 1.39(2) . ?
O12 C83 1.406(19) . ?
C59 C60 1.376(14) . ?
C59 C64 1.416(13) . ?
C60 C61 1.370(18) . ?
C61 C62 1.40(2) . ?
C62 C63 1.361(19) . ?
C63 C64 1.377(14) . ?
C65 C70 1.30(2) . ?
C65 C66 1.387(17) . ?
C66 C67 1.38(2) . ?
C67 C68 1.30(3) . ?
C68 C69 1.31(3) . ?
C69 C70 1.50(2) . ?
C71 C76 1.357(14) . ?
C71 C72 1.363(16) . ?
C72 C73 1.429(16) . ?
C73 C74 1.34(2) . ?
C74 C75 1.36(2) . ?
C75 C76 1.404(13) . ?
C77 C78 1.34(3) . ?
C77 C81 1.44(2) . ?
C78 C79 1.54(3) . ?
C79 C80 1.40(3) . ?
C79 C86 1.83(3) . ?
C80 C81 1.62(3) . ?
C80 C84 1.65(3) . ?
C82 C83 1.497(18) . ?
C82 C86 1.52(2) . ?
C83 C84 1.52(2) . ?
C84 C85 1.40(3) . ?
C85 C86 1.53(3) . ?
C88 C89 1.417(18) . ?
C89 C90 1.3900 . ?
C89 C94 1.3900 . ?
C90 C91 1.3900 . ?
C91 C92 1.3900 . ?
C92 C93 1.3900 . ?
C93 C94 1.3900 . ?
C95 C96 1.493(17) . ?
C96 C97 1.3900 . ?
C96 C101 1.3900 . ?
C97 C98 1.3900 . ?
C98 C99 1.3900 . ?
C99 C100 1.3900 . ?
C100 C101 1.3900 . ?
