#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318599.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_4318599
loop_
_publ_author_name
'Taichi Miyaji'
'Masato Kujime'
'Shiro Hikichi'
'Yoshihiko Moro-oka'
'Munetaka Akita'
_publ_section_title
;
 Synthesis and Characterization of a Series of (Hydroperoxo)-,
 (Alkylperoxo)-, and (μ-Peroxo)palladium Complexes Containing the
 Hydrotris(3,5-diisopropylpyrazolyl)borato Ligand (TpiPr2):
 (TpiPr2)(py)Pd-OO-X [X = H, t-Bu, Pd(TpiPr2)(py)] and
 (TpiPr2)(py)Pd-(μ-κ1:κ2-OO)-PdTpiPr2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5286
_journal_page_last               5295
_journal_paper_doi               10.1021/ic020355e
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C68 H119 B2 N14 O4 Pd2'
_chemical_formula_weight         1431.19
_chemical_name_common            'compound 8'
_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                104.1680(10)
_cell_angle_beta                 103.024(5)
_cell_angle_gamma                92.205(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0619(11)
_cell_length_b                   22.884(2)
_cell_length_c                   12.3043(8)
_cell_measurement_temperature    213(2)
_cell_volume                     3986.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.824
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0797
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15065
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.501
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1518
_refine_diff_density_max         0.617
_refine_diff_density_min         -1.974
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.248
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     818
_refine_ls_number_reflns         15065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.248
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.0814
_refine_ls_shift/su_max          1.178
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2082
_reflns_number_gt                9721
_reflns_number_total             15065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020355e_6.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        3986.6(5)
_cod_database_code               4318599
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.10608(3) 0.282444(19) 0.46962(4) 0.04019(14) Uani 1 1 d . . .
Pd2 Pd 0.29123(3) 0.20248(2) 0.22358(4) 0.04095(14) Uani 1 1 d . . .
O1 O 0.2093(4) 0.2560(2) 0.4009(4) 0.0623(13) Uani 1 1 d . . .
O2 O 0.1842(3) 0.21715(18) 0.2884(3) 0.0468(10) Uani 1 1 d . . .
O3 O 0.0776(4) 0.0287(3) 0.1214(6) 0.0881(18) Uani 1 1 d . . .
O91 O 0.339(3) 0.6638(19) 1.068(3) 0.279(17) Uiso 0.50 1 d P . .
O91A O 0.242(3) 0.735(2) 1.130(5) 0.31(2) Uiso 0.50 1 d P . .
N1 N 0.3562(3) 0.2565(2) 0.3748(4) 0.0353(10) Uani 1 1 d . . .
N11 N 0.0015(4) 0.3131(2) 0.5364(4) 0.0457(12) Uani 1 1 d . . .
N12 N 0.0194(4) 0.3620(2) 0.6306(5) 0.0481(12) Uani 1 1 d . . .
N21 N 0.1358(3) 0.3686(2) 0.4677(4) 0.0421(11) Uani 1 1 d . . .
N22 N 0.1413(3) 0.4142(2) 0.5666(4) 0.0419(11) Uani 1 1 d . . .
N31 N 0.1756(4) 0.3045(2) 0.7169(5) 0.0504(13) Uani 1 1 d . . .
N32 N 0.1857(4) 0.3665(2) 0.7392(4) 0.0463(12) Uani 1 1 d . . .
N41 N 0.0752(3) 0.1958(2) 0.4805(5) 0.0460(12) Uani 1 1 d . . .
N51 N 0.4054(3) 0.1932(2) 0.1657(4) 0.0421(11) Uani 1 1 d . . .
N52 N 0.4204(3) 0.1383(2) 0.1006(4) 0.0409(11) Uani 1 1 d . . .
N61 N 0.2203(3) 0.1465(2) 0.0740(5) 0.0453(12) Uani 1 1 d . . .
N62 N 0.2566(3) 0.0952(2) 0.0230(4) 0.0421(11) Uani 1 1 d . . .
N71 N 0.2755(3) 0.0258(2) 0.1873(4) 0.0444(12) Uani 1 1 d . . .
N72 N 0.3492(3) 0.0654(2) 0.1953(5) 0.0453(12) Uani 1 1 d . . .
C1 C 0.2984(4) 0.2748(3) 0.4375(6) 0.0464(15) Uani 1 1 d . . .
C2 C 0.3347(5) 0.3192(3) 0.5522(6) 0.0530(16) Uani 1 1 d . . .
H1 H 0.3921 0.3080 0.5897 0.053 Uiso 1 1 calc R . .
H2 H 0.2918 0.3192 0.5992 0.053 Uiso 1 1 calc R . .
H3 H 0.3437 0.3589 0.5413 0.053 Uiso 1 1 calc R . .
C11 C -0.0879(4) 0.2933(3) 0.5156(7) 0.0533(16) Uani 1 1 d . . .
C12 C -0.1259(5) 0.3294(3) 0.5980(7) 0.063(2) Uani 1 1 d . . .
C13 C -0.0582(4) 0.3715(3) 0.6687(6) 0.0506(16) Uani 1 1 d . . .
C14 C -0.1323(5) 0.2408(3) 0.4131(7) 0.0610(18) Uani 1 1 d . . .
C15 C -0.2136(8) 0.2079(6) 0.4341(11) 0.134(5) Uani 1 1 d . . .
H6 H -0.2565 0.2362 0.4535 0.134 Uiso 1 1 calc R . .
H7 H -0.1930 0.1897 0.4966 0.134 Uiso 1 1 calc R . .
H8 H -0.2426 0.1771 0.3654 0.134 Uiso 1 1 calc R . .
C16 C -0.1591(8) 0.2614(4) 0.3031(8) 0.106(4) Uani 1 1 d . . .
H9 H -0.1057 0.2796 0.2890 0.106 Uiso 1 1 calc R . .
H10 H -0.2030 0.2905 0.3111 0.106 Uiso 1 1 calc R . .
H11 H -0.1855 0.2271 0.2394 0.106 Uiso 1 1 calc R . .
C17 C -0.0600(6) 0.4207(3) 0.7752(7) 0.0638(19) Uani 1 1 d . . .
C18 C -0.0056(7) 0.4052(4) 0.8856(7) 0.084(3) Uani 1 1 d . . .
H13 H -0.0328 0.3679 0.8919 0.084 Uiso 1 1 calc R . .
H14 H -0.0071 0.4371 0.9521 0.084 Uiso 1 1 calc R . .
H15 H 0.0567 0.4010 0.8811 0.084 Uiso 1 1 calc R . .
C19 C -0.1577(6) 0.4315(4) 0.7825(8) 0.078(2) Uani 1 1 d . . .
H16 H -0.1569 0.4631 0.8505 0.078 Uiso 1 1 calc R . .
H17 H -0.1890 0.3950 0.7861 0.078 Uiso 1 1 calc R . .
H18 H -0.1890 0.4434 0.7153 0.078 Uiso 1 1 calc R . .
C21 C 0.1559(4) 0.3942(3) 0.3871(5) 0.0446(14) Uani 1 1 d . . .
C22 C 0.1743(5) 0.4561(3) 0.4345(6) 0.0547(16) Uani 1 1 d . . .
C23 C 0.1642(4) 0.4678(3) 0.5465(6) 0.0463(14) Uani 1 1 d . . .
C24 C 0.1499(5) 0.3590(3) 0.2647(6) 0.0569(17) Uani 1 1 d . . .
C25 C 0.2371(6) 0.3703(4) 0.2285(8) 0.086(3) Uani 1 1 d . . .
H22 H 0.2885 0.3628 0.2839 0.086 Uiso 1 1 calc R . .
H23 H 0.2441 0.4115 0.2247 0.086 Uiso 1 1 calc R . .
H24 H 0.2342 0.3436 0.1540 0.086 Uiso 1 1 calc R . .
C26 C 0.0699(7) 0.3735(5) 0.1812(7) 0.096(3) Uani 1 1 d . . .
H25 H 0.0765 0.4158 0.1841 0.096 Uiso 1 1 calc R . .
H26 H 0.0142 0.3641 0.2016 0.096 Uiso 1 1 calc R . .
H27 H 0.0679 0.3499 0.1044 0.096 Uiso 1 1 calc R . .
C27 C 0.1733(5) 0.5284(3) 0.6316(6) 0.0554(17) Uani 1 1 d . . .
C28 C 0.2530(6) 0.5691(3) 0.6260(8) 0.078(2) Uani 1 1 d . . .
H29 H 0.3077 0.5488 0.6358 0.078 Uiso 1 1 calc R . .
H30 H 0.2611 0.6060 0.6863 0.078 Uiso 1 1 calc R . .
H31 H 0.2405 0.5784 0.5523 0.078 Uiso 1 1 calc R . .
C29 C 0.0865(5) 0.5591(3) 0.6106(8) 0.078(3) Uani 1 1 d . . .
H32 H 0.0939 0.5975 0.6666 0.078 Uiso 1 1 calc R . .
H33 H 0.0365 0.5341 0.6176 0.078 Uiso 1 1 calc R . .
H34 H 0.0739 0.5652 0.5344 0.078 Uiso 1 1 calc R . .
C31 C 0.2471(5) 0.2887(3) 0.7871(6) 0.0513(15) Uani 1 1 d . . .
C32 C 0.3039(5) 0.3410(3) 0.8571(6) 0.0626(19) Uani 1 1 d . . .
C33 C 0.2623(5) 0.3894(3) 0.8251(6) 0.0594(18) Uani 1 1 d . . .
C34 C 0.2603(5) 0.2234(3) 0.7828(7) 0.0605(18) Uani 1 1 d . . .
C35 C 0.3006(6) 0.1936(4) 0.6827(8) 0.081(2) Uani 1 1 d . . .
H37 H 0.3048 0.1516 0.6801 0.081 Uiso 1 1 calc R . .
H38 H 0.3606 0.2132 0.6933 0.081 Uiso 1 1 calc R . .
H39 H 0.2619 0.1973 0.6116 0.081 Uiso 1 1 calc R . .
C36 C 0.3162(6) 0.2167(4) 0.8970(7) 0.078(2) Uani 1 1 d . . .
H40 H 0.3206 0.1745 0.8929 0.078 Uiso 1 1 calc R . .
H41 H 0.2870 0.2342 0.9574 0.078 Uiso 1 1 calc R . .
H42 H 0.3765 0.2370 0.9132 0.078 Uiso 1 1 calc R . .
C37 C 0.2926(6) 0.4567(4) 0.8726(7) 0.074(2) Uani 1 1 d . . .
C38 C 0.3636(11) 0.4767(7) 0.8199(19) 0.104(6) Uani 0.65 1 d P . .
C38A C 0.4040(17) 0.4651(14) 0.890(3) 0.101(11) Uani 0.35 1 d P . .
C39 C 0.3253(16) 0.4726(7) 1.0115(14) 0.113(7) Uani 0.65 1 d P . .
C39A C 0.254(2) 0.4807(14) 0.964(3) 0.128(16) Uani 0.35 1 d P . .
C42 C 0.0766(5) 0.1467(3) 0.3957(6) 0.0538(16) Uani 1 1 d . . .
C43 C 0.0486(7) 0.0900(3) 0.4021(7) 0.079(3) Uani 1 1 d . . .
C44 C 0.0217(9) 0.0832(4) 0.4969(8) 0.104(4) Uani 1 1 d . . .
C45 C 0.0217(7) 0.1327(4) 0.5851(8) 0.090(3) Uani 1 1 d . . .
C46 C 0.0491(5) 0.1886(3) 0.5755(6) 0.0565(17) Uani 1 1 d . . .
C51 C 0.4757(4) 0.2342(3) 0.1737(6) 0.0455(14) Uani 1 1 d . . .
C52 C 0.5356(4) 0.2044(3) 0.1134(6) 0.0523(16) Uani 1 1 d . . .
C53 C 0.5006(4) 0.1442(3) 0.0674(6) 0.0441(14) Uani 1 1 d . . .
C54 C 0.4829(5) 0.2985(3) 0.2386(6) 0.0533(16) Uani 1 1 d . . .
C55 C 0.5573(6) 0.3102(4) 0.3513(7) 0.081(3) Uani 1 1 d . . .
H58 H 0.5448 0.2825 0.3944 0.081 Uiso 1 1 calc R . .
H59 H 0.5578 0.3510 0.3962 0.081 Uiso 1 1 calc R . .
H60 H 0.6159 0.3046 0.3339 0.081 Uiso 1 1 calc R . .
C56 C 0.5016(7) 0.3414(3) 0.1680(8) 0.082(3) Uani 1 1 d . . .
H61 H 0.5573 0.3331 0.1443 0.082 Uiso 1 1 calc R . .
H62 H 0.5074 0.3824 0.2140 0.082 Uiso 1 1 calc R . .
H63 H 0.4518 0.3357 0.1009 0.082 Uiso 1 1 calc R . .
C57 C 0.5351(5) 0.0951(3) -0.0090(7) 0.0579(18) Uani 1 1 d . . .
C58 C 0.6399(5) 0.1044(3) 0.0130(8) 0.077(2) Uani 1 1 d . . .
H65 H 0.6671 0.1092 0.0935 0.077 Uiso 1 1 calc R . .
H66 H 0.6569 0.1400 -0.0086 0.077 Uiso 1 1 calc R . .
H67 H 0.6612 0.0698 -0.0320 0.077 Uiso 1 1 calc R . .
C59 C 0.4909(7) 0.0895(4) -0.1351(8) 0.091(3) Uani 1 1 d . . .
H68 H 0.5094 0.1252 -0.1556 0.091 Uiso 1 1 calc R . .
H69 H 0.4255 0.0852 -0.1473 0.091 Uiso 1 1 calc R . .
H70 H 0.5099 0.0546 -0.1823 0.091 Uiso 1 1 calc R . .
C61 C 0.1367(4) 0.1476(3) 0.0049(6) 0.0502(15) Uani 1 1 d . . .
C62 C 0.1202(4) 0.0962(3) -0.0889(6) 0.0514(16) Uani 1 1 d . . .
C63 C 0.1960(4) 0.0647(3) -0.0754(5) 0.0466(14) Uani 1 1 d . . .
C64 C 0.0777(5) 0.1975(3) 0.0311(6) 0.0573(17) Uani 1 1 d . . .
C65 C -0.0056(6) 0.1750(4) 0.0671(8) 0.081(2) Uani 1 1 d . . .
C66 C 0.0468(6) 0.2243(4) -0.0726(8) 0.081(3) Uani 1 1 d . . .
C67 C 0.2111(4) 0.0054(3) -0.1515(6) 0.0525(16) Uani 1 1 d . . .
C68 C 0.1518(5) -0.0458(3) -0.1372(7) 0.067(2) Uani 1 1 d . . .
H80 H 0.0889 -0.0375 -0.1532 0.067 Uiso 1 1 calc R . .
H81 H 0.1704 -0.0494 -0.0593 0.067 Uiso 1 1 calc R . .
H82 H 0.1586 -0.0830 -0.1898 0.067 Uiso 1 1 calc R . .
C69 C 0.1922(7) 0.0090(4) -0.2767(7) 0.084(3) Uani 1 1 d . . .
H83 H 0.2315 0.0415 -0.2823 0.084 Uiso 1 1 calc R . .
H84 H 0.1294 0.0161 -0.3021 0.084 Uiso 1 1 calc R . .
H85 H 0.2037 -0.0285 -0.3245 0.084 Uiso 1 1 calc R . .
C71 C 0.2910(5) 0.0089(3) 0.2866(6) 0.0564(17) Uani 1 1 d . . .
C72 C 0.3749(6) 0.0366(4) 0.3584(7) 0.068(2) Uani 1 1 d . . .
C73 C 0.4115(5) 0.0721(3) 0.2985(6) 0.0555(16) Uani 1 1 d . . .
C74 C 0.2236(5) -0.0363(4) 0.3040(7) 0.070(2) Uani 1 1 d . . .
C75 C 0.2285(8) -0.0312(6) 0.4289(9) 0.125(5) Uani 1 1 d . . .
H88 H 0.2832 -0.0470 0.4623 0.125 Uiso 1 1 calc R . .
H89 H 0.1760 -0.0538 0.4357 0.125 Uiso 1 1 calc R . .
H90 H 0.2296 0.0106 0.4689 0.125 Uiso 1 1 calc R . .
C76 C 0.2344(10) -0.0995(5) 0.2443(13) 0.159(6) Uani 1 1 d . . .
H91 H 0.1887 -0.1266 0.2547 0.159 Uiso 1 1 calc R . .
H92 H 0.2942 -0.1096 0.2763 0.159 Uiso 1 1 calc R . .
H93 H 0.2271 -0.1030 0.1634 0.159 Uiso 1 1 calc R . .
C77 C 0.5022(5) 0.1101(4) 0.3378(7) 0.0640(19) Uani 1 1 d . . .
C78 C 0.5224(8) 0.1424(5) 0.4654(8) 0.110(4) Uani 1 1 d . . .
H95 H 0.5240 0.1131 0.5096 0.110 Uiso 1 1 calc R . .
H96 H 0.4754 0.1684 0.4794 0.110 Uiso 1 1 calc R . .
H97 H 0.5806 0.1662 0.4880 0.110 Uiso 1 1 calc R . .
C79 C 0.5780(6) 0.0719(5) 0.3101(10) 0.100(3) Uani 1 1 d . . .
H98 H 0.5822 0.0407 0.3505 0.100 Uiso 1 1 calc R . .
H99 H 0.6351 0.0970 0.3339 0.100 Uiso 1 1 calc R . .
H100 H 0.5648 0.0536 0.2285 0.100 Uiso 1 1 calc R . .
C81 C 0.479(2) 0.4768(12) 0.510(3) 0.266(12) Uiso 1 1 d . . .
C82 C 0.5685(19) 0.4805(13) 0.613(2) 0.253(11) Uiso 1 1 d . . .
C83 C 0.569(2) 0.4429(15) 0.672(3) 0.293(14) Uiso 1 1 d . . .
C91 C 0.219(2) 0.6689(15) 0.968(3) 0.299(14) Uiso 1 1 d . . .
C92 C 0.299(4) 0.715(2) 1.069(4) 0.39(2) Uiso 1 1 d . . .
C93 C 0.410(4) 0.702(3) 1.130(5) 0.219(19) Uiso 0.50 1 d P . .
C93A C 0.317(4) 0.742(2) 1.256(4) 0.206(17) Uiso 0.50 1 d P . .
C94 C 0.395(4) 0.732(2) 1.232(5) 0.43(3) Uiso 1 1 d . . .
B1 B 0.1135(5) 0.3998(3) 0.6733(7) 0.0483(17) Uani 1 1 d . . .
B2 B 0.3520(5) 0.0820(3) 0.0802(6) 0.0420(15) Uani 1 1 d . . .
H01 H 0.1392 0.0480 0.1440 0.054 Uiso 1 1 d . . .
H02 H 0.0145 0.0463 0.2208 0.054 Uiso 1 1 d . . .
H4 H -0.1872 0.3259 0.6061 0.076 Uiso 1 1 d . . .
H5 H -0.0880 0.2125 0.4020 0.080 Uiso 1 1 d . . .
H12 H -0.0304 0.4582 0.7696 0.081 Uiso 1 1 d . . .
H19 H 0.1078 0.4375 0.7279 0.058 Uiso 1 1 d . . .
H20 H 0.1888 0.4860 0.3971 0.065 Uiso 1 1 d . . .
H21 H 0.1420 0.3162 0.2600 0.070 Uiso 1 1 d . . .
H28 H 0.1842 0.5219 0.7084 0.070 Uiso 1 1 d . . .
H35 H 0.3612 0.3418 0.9131 0.073 Uiso 1 1 d . . .
H36 H 0.2010 0.2027 0.7683 0.076 Uiso 1 1 d . . .
H50 H 0.0958 0.1516 0.3289 0.067 Uiso 1 1 d . . .
H51 H 0.0469 0.0553 0.3393 0.090 Uiso 1 1 d . . .
H52 H 0.0082 0.0428 0.5022 0.127 Uiso 1 1 d . . .
H53 H 0.0024 0.1288 0.6550 0.112 Uiso 1 1 d . . .
H54 H 0.0494 0.2242 0.6365 0.070 Uiso 1 1 d . . .
H55 H 0.3698 0.0481 0.0294 0.051 Uiso 1 1 d . . .
H56 H 0.5931 0.2224 0.1079 0.063 Uiso 1 1 d . . .
H57 H 0.4250 0.3063 0.2599 0.065 Uiso 1 1 d . . .
H64 H 0.5185 0.0576 0.0069 0.068 Uiso 1 1 d . . .
H71 H 0.0670 0.0856 -0.1537 0.063 Uiso 1 1 d . . .
H72 H 0.1130 0.2290 0.0967 0.075 Uiso 1 1 d . . .
H73 H -0.0428 0.2063 0.0883 0.100 Uiso 1 1 d . . .
H74 H -0.0418 0.1428 0.0071 0.100 Uiso 1 1 d . . .
H75 H 0.0139 0.1586 0.1348 0.100 Uiso 1 1 d . . .
H76 H 0.1000 0.2401 -0.0947 0.100 Uiso 1 1 d . . .
H77 H 0.0140 0.1934 -0.1407 0.100 Uiso 1 1 d . . .
H78 H 0.0094 0.2563 -0.0598 0.100 Uiso 1 1 d . . .
H79 H 0.2735 -0.0023 -0.1273 0.064 Uiso 1 1 d . . .
H86 H 0.4007 0.0326 0.4375 0.082 Uiso 1 1 d . . .
H87 H 0.1633 -0.0278 0.2689 0.088 Uiso 1 1 d . . .
H94 H 0.4990 0.1414 0.2929 0.076 Uiso 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'
B B 0.0013 0.0007 '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
O1 Pd1 N11 177.04(19) . . ?
O1 Pd1 N21 91.2(2) . . ?
N11 Pd1 N21 85.97(19) . . ?
O1 Pd1 N41 90.8(2) . . ?
N11 Pd1 N41 92.1(2) . . ?
N21 Pd1 N41 177.0(2) . . ?
O2 Pd2 N1 82.69(17) . . ?
O2 Pd2 N51 175.73(18) . . ?
N1 Pd2 N51 93.35(18) . . ?
O2 Pd2 N61 94.65(18) . . ?
N1 Pd2 N61 177.04(19) . . ?
N51 Pd2 N61 89.3(2) . . ?
C1 O1 O2 113.9(5) . . ?
C1 O1 Pd1 130.3(4) . . ?
O2 O1 Pd1 115.3(4) . . ?
O1 O2 Pd2 111.1(3) . . ?
C93 O91 C92 82(4) . . ?
C93 O91 C91 136(4) . . ?
C92 O91 C91 56(3) . . ?
C92 O91A C93A 94(4) . . ?
C1 N1 Pd2 110.4(4) . . ?
C11 N11 N12 106.9(5) . . ?
C11 N11 Pd1 134.3(4) . . ?
N12 N11 Pd1 118.6(4) . . ?
C13 N12 N11 109.1(5) . . ?
C13 N12 B1 129.5(5) . . ?
N11 N12 B1 121.3(5) . . ?
C21 N21 N22 107.9(5) . . ?
C21 N21 Pd1 133.3(4) . . ?
N22 N21 Pd1 118.8(4) . . ?
C23 N22 N21 108.6(5) . . ?
C23 N22 B1 130.8(5) . . ?
N21 N22 B1 120.3(5) . . ?
C31 N31 N32 107.0(5) . . ?
C33 N32 N31 109.8(5) . . ?
C33 N32 B1 129.8(5) . . ?
N31 N32 B1 120.4(5) . . ?
C42 N41 C46 118.9(5) . . ?
C42 N41 Pd1 122.5(4) . . ?
C46 N41 Pd1 118.6(4) . . ?
C51 N51 N52 108.0(5) . . ?
C51 N51 Pd2 131.3(4) . . ?
N52 N51 Pd2 120.6(4) . . ?
N51 N52 C53 109.5(5) . . ?
N51 N52 B2 119.4(5) . . ?
C53 N52 B2 131.0(5) . . ?
C61 N61 N62 107.2(5) . . ?
C61 N61 Pd2 132.4(4) . . ?
N62 N61 Pd2 120.4(4) . . ?
C63 N62 N61 109.3(5) . . ?
C63 N62 B2 131.1(5) . . ?
N61 N62 B2 119.6(5) . . ?
C71 N71 N72 106.9(5) . . ?
C73 N72 N71 109.9(5) . . ?
C73 N72 B2 134.2(5) . . ?
N71 N72 B2 114.5(5) . . ?
N1 C1 O1 121.9(6) . . ?
N1 C1 C2 117.8(5) . . ?
O1 C1 C2 120.3(6) . . ?
N11 C11 C12 108.9(6) . . ?
N11 C11 C14 121.2(6) . . ?
C12 C11 C14 130.0(6) . . ?
C13 C12 C11 107.0(6) . . ?
C12 C13 N12 108.1(6) . . ?
C12 C13 C17 129.8(6) . . ?
N12 C13 C17 122.1(6) . . ?
C15 C14 C11 111.9(7) . . ?
C15 C14 C16 111.1(8) . . ?
C11 C14 C16 111.3(6) . . ?
C13 C17 C19 111.2(7) . . ?
C13 C17 C18 110.8(6) . . ?
C19 C17 C18 111.0(7) . . ?
N21 C21 C22 108.5(6) . . ?
N21 C21 C24 123.1(5) . . ?
C22 C21 C24 128.2(6) . . ?
C23 C22 C21 107.1(6) . . ?
N22 C23 C22 107.9(5) . . ?
N22 C23 C27 124.8(6) . . ?
C22 C23 C27 127.2(6) . . ?
C26 C24 C21 111.8(6) . . ?
C26 C24 C25 109.6(7) . . ?
C21 C24 C25 111.4(6) . . ?
C23 C27 C29 111.2(6) . . ?
C23 C27 C28 111.2(6) . . ?
C29 C27 C28 109.4(6) . . ?
N31 C31 C32 110.0(6) . . ?
N31 C31 C34 121.6(6) . . ?
C32 C31 C34 128.4(6) . . ?
C33 C32 C31 105.4(6) . . ?
N32 C33 C32 107.8(6) . . ?
N32 C33 C37 123.4(6) . . ?
C32 C33 C37 128.8(7) . . ?
C31 C34 C36 111.4(6) . . ?
C31 C34 C35 111.8(6) . . ?
C36 C34 C35 111.9(7) . . ?
C39A C37 C38 137.4(15) . . ?
C39A C37 C33 109.8(15) . . ?
C38 C37 C33 112.1(9) . . ?
C39A C37 C39 44.4(17) . . ?
C38 C37 C39 112.4(12) . . ?
C33 C37 C39 109.3(8) . . ?
C39A C37 C38A 120.4(19) . . ?
C38 C37 C38A 38.3(14) . . ?
C33 C37 C38A 107.1(12) . . ?
C39 C37 C38A 79.9(16) . . ?
C38A C38 C37 79(2) . . ?
C38 C38A C37 62.4(16) . . ?
C39A C39 C37 57.4(18) . . ?
C39 C39A C37 78(2) . . ?
N41 C42 C43 120.8(7) . . ?
C44 C43 C42 120.0(7) . . ?
C45 C44 C43 119.9(7) . . ?
C44 C45 C46 118.7(8) . . ?
N41 C46 C45 121.7(7) . . ?
N51 C51 C52 107.9(5) . . ?
N51 C51 C54 123.2(6) . . ?
C52 C51 C54 128.9(6) . . ?
C53 C52 C51 108.2(5) . . ?
N52 C53 C52 106.4(5) . . ?
N52 C53 C57 124.1(5) . . ?
C52 C53 C57 129.3(5) . . ?
C51 C54 C56 112.2(6) . . ?
C51 C54 C55 110.0(6) . . ?
C56 C54 C55 110.6(6) . . ?
C53 C57 C59 111.4(6) . . ?
C53 C57 C58 111.1(6) . . ?
C59 C57 C58 110.2(7) . . ?
N61 C61 C62 108.2(5) . . ?
N61 C61 C64 122.5(6) . . ?
C62 C61 C64 129.2(6) . . ?
C63 C62 C61 107.2(5) . . ?
N62 C63 C62 108.0(5) . . ?
N62 C63 C67 124.0(5) . . ?
C62 C63 C67 127.9(6) . . ?
C61 C64 C65 110.6(6) . . ?
C61 C64 C66 111.2(6) . . ?
C65 C64 C66 110.4(7) . . ?
C63 C67 C68 110.0(6) . . ?
C63 C67 C69 109.8(6) . . ?
C68 C67 C69 112.0(6) . . ?
N71 C71 C72 110.0(6) . . ?
N71 C71 C74 120.2(6) . . ?
C72 C71 C74 129.8(7) . . ?
C71 C72 C73 106.3(6) . . ?
N72 C73 C72 106.9(6) . . ?
N72 C73 C77 125.9(6) . . ?
C72 C73 C77 127.2(6) . . ?
C76 C74 C75 110.0(9) . . ?
C76 C74 C71 111.9(8) . . ?
C75 C74 C71 112.8(8) . . ?
C73 C77 C79 110.5(7) . . ?
C73 C77 C78 111.3(7) . . ?
C79 C77 C78 111.4(8) . . ?
C81 C81 C82 86(3) 2_666 . ?
C81 C81 C82 53(2) 2_666 2_666 ?
C82 C81 C82 139.3(17) . 2_666 ?
C83 C82 C81 118(3) . . ?
C83 C82 C81 158(3) . 2_666 ?
C81 C82 C81 40.7(17) . 2_666 ?
C92 C91 O91 42(2) . . ?
O91A C92 C91 93(5) . . ?
O91A C92 O91 126(5) . . ?
C91 C92 O91 82(4) . . ?
O91A C92 C93 123(5) . . ?
C91 C92 C93 129(5) . . ?
O91 C92 C93 49(3) . . ?
O91 C93 C94 110(5) . . ?
O91 C93 C92 50(3) . . ?
C94 C93 C92 86(4) . . ?
C94 C93A O91A 106(4) . . ?
C93 C94 C93A 127(6) . . ?
N12 B1 N32 110.9(5) . . ?
N12 B1 N22 108.4(5) . . ?
N32 B1 N22 112.5(5) . . ?
N62 B2 N52 108.7(5) . . ?
N62 B2 N72 109.3(5) . . ?
N52 B2 N72 112.0(5) . . ?
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 O1 1.978(5) . ?
Pd1 N11 2.009(5) . ?
Pd1 N21 2.013(5) . ?
Pd1 N41 2.061(5) . ?
Pd2 O2 1.959(4) . ?
Pd2 N1 1.977(5) . ?
Pd2 N51 2.004(5) . ?
Pd2 N61 2.006(5) . ?
O1 C1 1.333(7) . ?
O1 O2 1.409(6) . ?
O91 C93 1.32(6) . ?
O91 C92 1.34(6) . ?
O91 C91 1.97(5) . ?
O91A C92 1.28(6) . ?
O91A C93A 1.66(5) . ?
N1 C1 1.305(8) . ?
N11 C11 1.351(8) . ?
N11 N12 1.368(7) . ?
N12 C13 1.360(8) . ?
N12 B1 1.543(9) . ?
N21 C21 1.350(7) . ?
N21 N22 1.379(6) . ?
N22 C23 1.355(7) . ?
N22 B1 1.568(9) . ?
N31 C31 1.340(8) . ?
N31 N32 1.374(7) . ?
N32 C33 1.362(9) . ?
N32 B1 1.546(9) . ?
N41 C42 1.338(8) . ?
N41 C46 1.359(8) . ?
N51 C51 1.358(7) . ?
N51 N52 1.372(6) . ?
N52 C53 1.371(7) . ?
N52 B2 1.551(8) . ?
N61 C61 1.356(8) . ?
N61 N62 1.383(6) . ?
N62 C63 1.351(7) . ?
N62 B2 1.528(8) . ?
N71 C71 1.346(8) . ?
N71 N72 1.375(6) . ?
N72 C73 1.369(8) . ?
N72 B2 1.563(9) . ?
C1 C2 1.493(9) . ?
C11 C12 1.388(10) . ?
C11 C14 1.515(10) . ?
C12 C13 1.356(10) . ?
C13 C17 1.510(10) . ?
C14 C15 1.515(11) . ?
C14 C16 1.517(12) . ?
C17 C19 1.520(10) . ?
C17 C18 1.548(11) . ?
C21 C22 1.385(8) . ?
C21 C24 1.505(9) . ?
C22 C23 1.383(9) . ?
C23 C27 1.500(8) . ?
C24 C26 1.503(11) . ?
C24 C25 1.511(11) . ?
C27 C29 1.508(10) . ?
C27 C28 1.516(10) . ?
C31 C32 1.410(9) . ?
C31 C34 1.505(9) . ?
C32 C33 1.390(10) . ?
C33 C37 1.520(10) . ?
C34 C36 1.514(10) . ?
C34 C35 1.519(11) . ?
C37 C39A 1.39(3) . ?
C37 C38 1.480(19) . ?
C37 C39 1.612(18) . ?
C37 C38A 1.64(3) . ?
C38 C38A 1.03(3) . ?
C39 C39A 1.15(4) . ?
C42 C43 1.376(9) . ?
C43 C44 1.359(12) . ?
C44 C45 1.364(13) . ?
C45 C46 1.371(10) . ?
C51 C52 1.389(9) . ?
C51 C54 1.479(8) . ?
C52 C53 1.388(8) . ?
C53 C57 1.471(8) . ?
C54 C56 1.517(10) . ?
C54 C55 1.531(10) . ?
C57 C59 1.516(11) . ?
C57 C58 1.538(10) . ?
C61 C62 1.401(9) . ?
C61 C64 1.492(9) . ?
C62 C63 1.373(8) . ?
C63 C67 1.506(8) . ?
C64 C65 1.531(11) . ?
C64 C66 1.536(10) . ?
C67 C68 1.513(10) . ?
C67 C69 1.525(10) . ?
C71 C72 1.393(10) . ?
C71 C74 1.506(10) . ?
C72 C73 1.396(10) . ?
C73 C77 1.505(9) . ?
C74 C76 1.486(14) . ?
C74 C75 1.497(12) . ?
C77 C79 1.513(11) . ?
C77 C78 1.518(12) . ?
C81 C81 1.31(5) 2_666 ?
C81 C82 1.61(4) . ?
C81 C82 2.01(4) 2_666 ?
C82 C83 1.25(3) . ?
C82 C81 2.01(4) 2_666 ?
C91 C92 1.64(5) . ?
C92 C93 1.74(7) . ?
C93 C94 1.35(6) . ?
C93A C94 1.29(6) . ?
