#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318597.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_4318597
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            'C63 H107 B2 N13 O3 Pd2'
_chemical_formula_weight         1329.04
_chemical_name_common            'compound 5'
_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                92.24(4)
_cell_angle_beta                 104.75(3)
_cell_angle_gamma                106.99(2)
_cell_formula_units_Z            2
_cell_length_a                   14.324(7)
_cell_length_b                   20.487(8)
_cell_length_c                   13.161(8)
_cell_measurement_temperature    213(2)
_cell_volume                     3545(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.748
_diffrn_measured_fraction_theta_max 0.748
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0911
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11614
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.557
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1404
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.320
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         11614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_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          0.2148
_refine_ls_wR_factor_ref         0.2345
_reflns_number_gt                9471
_reflns_number_total             11614
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020355e_4.cif
_cod_data_source_block           shelxl
_cod_database_code               4318597
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 1.07370(4) 0.35509(3) 0.27694(4) 0.03416(17) Uani 1 1 d . . .
Pd2 Pd 0.96234(4) 0.17655(3) 0.14336(5) 0.03833(18) Uani 1 1 d . . .
O1 O 1.0750(4) 0.2629(3) 0.2244(4) 0.0434(12) Uani 1 1 d . . .
O2 O 1.0543(4) 0.2073(3) 0.2874(4) 0.0471(13) Uani 1 1 d . . .
O83 O 0.3712(11) 0.1380(9) 0.5495(15) 0.174(7) Uani 1 1 d . . .
N11 N 1.1000(4) 0.4545(3) 0.3209(5) 0.0380(14) Uani 1 1 d . . .
N12 N 1.2015(4) 0.4947(3) 0.3611(5) 0.0373(14) Uani 1 1 d . . .
N21 N 1.1523(4) 0.3539(3) 0.4263(5) 0.0364(14) Uani 1 1 d . . .
N22 N 1.2485(4) 0.4026(3) 0.4617(5) 0.0371(14) Uani 1 1 d . . .
N31 N 1.2894(5) 0.4624(4) 0.2045(6) 0.0496(17) Uani 1 1 d . . .
N32 N 1.2919(4) 0.4225(3) 0.2879(5) 0.0346(13) Uani 1 1 d . . .
N41 N 0.9992(4) 0.3633(3) 0.1273(5) 0.0362(14) Uani 1 1 d . . .
N51 N 0.8765(5) 0.0758(3) 0.1269(5) 0.0447(16) Uani 1 1 d . . .
N52 N 0.7821(5) 0.0519(3) 0.0589(5) 0.0452(16) Uani 1 1 d . . .
N61 N 0.8999(5) 0.1768(3) -0.0132(5) 0.0415(15) Uani 1 1 d . . .
N62 N 0.7990(5) 0.1422(4) -0.0645(5) 0.0467(16) Uani 1 1 d . . .
N71 N 0.6867(5) 0.2059(4) 0.0330(6) 0.0501(17) Uani 1 1 d . . .
N72 N 0.7099(5) 0.1509(3) 0.0777(5) 0.0439(16) Uani 1 1 d . . .
C11 C 1.0447(5) 0.4974(4) 0.3136(6) 0.0383(16) Uani 1 1 d . . .
C12 C 1.1084(6) 0.5640(4) 0.3480(6) 0.0391(16) Uani 1 1 d . . .
C13 C 1.2072(5) 0.5601(4) 0.3781(6) 0.0372(16) Uani 1 1 d . . .
C14 C 0.9295(6) 0.4714(4) 0.2764(7) 0.0467(19) Uani 1 1 d . . .
C15 C 0.8852(7) 0.4171(6) 0.3392(10) 0.078(3) Uani 1 1 d . . .
H4 H 0.8125 0.4016 0.3123 0.078 Uiso 1 1 calc R . .
H5 H 0.9043 0.4359 0.4122 0.078 Uiso 1 1 calc R . .
H6 H 0.9106 0.3790 0.3333 0.078 Uiso 1 1 calc R . .
C16 C 0.8860(7) 0.5309(5) 0.2763(9) 0.067(3) Uani 1 1 d . . .
H7 H 0.8887 0.5456 0.3475 0.067 Uiso 1 1 calc R . .
H8 H 0.8166 0.5162 0.2334 0.067 Uiso 1 1 calc R . .
H9 H 0.9251 0.5685 0.2480 0.067 Uiso 1 1 calc R . .
C17 C 1.3044(5) 0.6197(4) 0.4123(6) 0.0415(18) Uani 1 1 d . . .
C18 C 1.2963(9) 0.6744(6) 0.4861(11) 0.088(4) Uani 1 1 d . . .
H11 H 1.3628 0.7061 0.5189 0.088 Uiso 1 1 calc R . .
H12 H 1.2673 0.6534 0.5396 0.088 Uiso 1 1 calc R . .
H13 H 1.2537 0.6986 0.4469 0.088 Uiso 1 1 calc R . .
C19 C 1.3370(8) 0.6496(6) 0.3196(9) 0.078(3) Uani 1 1 d . . .
H14 H 1.4065 0.6785 0.3433 0.078 Uiso 1 1 calc R . .
H15 H 1.2946 0.6763 0.2885 0.078 Uiso 1 1 calc R . .
H16 H 1.3307 0.6130 0.2680 0.078 Uiso 1 1 calc R . .
C21 C 1.1364(6) 0.3178(4) 0.5052(6) 0.0418(18) Uani 1 1 d . . .
C22 C 1.2216(6) 0.3435(4) 0.5939(6) 0.0434(18) Uani 1 1 d . . .
C23 C 1.2910(6) 0.3957(4) 0.5634(6) 0.0391(16) Uani 1 1 d . . .
C24 C 1.0374(5) 0.2629(4) 0.4939(6) 0.0391(17) Uani 1 1 d . . .
C25 C 1.0549(8) 0.1981(5) 0.5344(8) 0.061(2) Uani 1 1 d . . .
H19 H 0.9909 0.1625 0.5211 0.061 Uiso 1 1 calc R . .
H20 H 1.0876 0.2072 0.6091 0.061 Uiso 1 1 calc R . .
H21 H 1.0975 0.1836 0.4987 0.061 Uiso 1 1 calc R . .
C26 C 0.9722(7) 0.2886(5) 0.5522(7) 0.055(2) Uani 1 1 d . . .
H22 H 1.0125 0.3088 0.6227 0.055 Uiso 1 1 calc R . .
H23 H 0.9154 0.2507 0.5557 0.055 Uiso 1 1 calc R . .
H24 H 0.9481 0.3224 0.5149 0.055 Uiso 1 1 calc R . .
C27 C 1.3942(6) 0.4412(4) 0.6264(6) 0.0434(18) Uani 1 1 d . . .
C28 C 1.4455(7) 0.4017(5) 0.7058(8) 0.066(3) Uani 1 1 d . . .
H26 H 1.4186 0.3993 0.7659 0.066 Uiso 1 1 calc R . .
H27 H 1.5174 0.4249 0.7285 0.066 Uiso 1 1 calc R . .
H28 H 1.4327 0.3560 0.6733 0.066 Uiso 1 1 calc R . .
C29 C 1.3901(7) 0.5068(5) 0.6805(7) 0.053(2) Uani 1 1 d . . .
H29 H 1.4577 0.5347 0.7187 0.053 Uiso 1 1 calc R . .
H30 H 1.3493 0.4954 0.7289 0.053 Uiso 1 1 calc R . .
H31 H 1.3607 0.5319 0.6282 0.053 Uiso 1 1 calc R . .
C31 C 1.3050(7) 0.4271(5) 0.1287(7) 0.055(2) Uani 1 1 d . . .
C32 C 1.3202(7) 0.3649(5) 0.1597(7) 0.052(2) Uani 1 1 d . . .
C33 C 1.3111(6) 0.3638(4) 0.2613(6) 0.0424(18) Uani 1 1 d . . .
C34 C 1.3015(11) 0.4532(8) 0.0213(9) 0.092(4) Uani 1 1 d . . .
C35 C 1.3008(12) 0.5224(7) 0.0205(10) 0.097(4) Uani 1 1 d . . .
H34 H 1.3684 0.5530 0.0518 0.097 Uiso 1 1 calc R . .
H35 H 1.2565 0.5300 0.0603 0.097 Uiso 1 1 calc R . .
H36 H 1.2770 0.5311 -0.0512 0.097 Uiso 1 1 calc R . .
C36 C 1.3720(14) 0.4297(10) -0.0298(12) 0.144(8) Uani 1 1 d . . .
H37 H 1.3607 0.3814 -0.0262 0.144 Uiso 1 1 calc R . .
H38 H 1.4413 0.4547 0.0071 0.144 Uiso 1 1 calc R . .
H39 H 1.3585 0.4382 -0.1025 0.144 Uiso 1 1 calc R . .
C37 C 1.3257(5) 0.3107(4) 0.3325(6) 0.0435(18) Uani 1 1 d . . .
C38 C 1.4325(7) 0.3328(5) 0.4064(7) 0.056(2) Uani 1 1 d . . .
H41 H 1.4416 0.2966 0.4481 0.056 Uiso 1 1 calc R . .
H42 H 1.4428 0.3734 0.4523 0.056 Uiso 1 1 calc R . .
H43 H 1.4808 0.3425 0.3657 0.056 Uiso 1 1 calc R . .
C39 C 1.3029(7) 0.2400(5) 0.2707(8) 0.063(3) Uani 1 1 d . . .
H44 H 1.2371 0.2277 0.2204 0.063 Uiso 1 1 calc R . .
H45 H 1.3040 0.2062 0.3191 0.063 Uiso 1 1 calc R . .
H46 H 1.3535 0.2420 0.2341 0.063 Uiso 1 1 calc R . .
C42 C 0.9049(6) 0.3218(4) 0.0785(6) 0.0415(17) Uani 1 1 d . . .
C43 C 0.8532(6) 0.3276(5) -0.0230(6) 0.0467(19) Uani 1 1 d . . .
C44 C 0.9027(6) 0.3773(5) -0.0757(7) 0.056(2) Uani 1 1 d . . .
C45 C 0.9989(7) 0.4198(5) -0.0261(7) 0.054(2) Uani 1 1 d . . .
C46 C 1.0466(5) 0.4119(4) 0.0753(7) 0.0424(18) Uani 1 1 d . . .
C51 C 0.9042(7) 0.0245(4) 0.1695(8) 0.057(2) Uani 1 1 d . . .
C52 C 0.8208(7) -0.0358(5) 0.1307(10) 0.072(3) Uani 1 1 d . . .
C53 C 0.7471(7) -0.0174(5) 0.0560(9) 0.062(3) Uani 1 1 d . . .
C54 C 1.0044(8) 0.0336(5) 0.2466(10) 0.076(3) Uani 1 1 d . . .
C55 C 0.9978(11) -0.0083(9) 0.3349(13) 0.142(8) Uani 1 1 d . . .
H55 H 0.9422 -0.0052 0.3609 0.142 Uiso 1 1 calc R . .
H56 H 1.0600 0.0084 0.3909 0.142 Uiso 1 1 calc R . .
H57 H 0.9868 -0.0554 0.3103 0.142 Uiso 1 1 calc R . .
C56 C 1.0756(10) 0.0205(9) 0.1873(13) 0.123(6) Uani 1 1 d . . .
H58 H 1.0606 -0.0281 0.1705 0.123 Uiso 1 1 calc R . .
H59 H 1.1445 0.0398 0.2305 0.123 Uiso 1 1 calc R . .
H60 H 1.0672 0.0415 0.1230 0.123 Uiso 1 1 calc R . .
C57 C 0.6450(7) -0.0615(5) -0.0136(10) 0.069(3) Uani 1 1 d . . .
C58 C 0.599(2) -0.1157(16) 0.062(3) 0.113(13) Uani 0.46 1 d P . .
C58A C 0.5633(12) -0.0694(14) 0.034(2) 0.091(9) Uani 0.54 1 d P . .
C59 C 0.647(2) -0.0865(19) -0.102(2) 0.093(10) Uani 0.46 1 d P . .
C59A C 0.6530(17) -0.1327(11) -0.059(2) 0.092(9) Uani 0.54 1 d P . .
C61 C 0.9442(7) 0.2009(5) -0.0873(6) 0.051(2) Uani 1 1 d . . .
C62 C 0.8745(7) 0.1843(5) -0.1867(7) 0.057(2) Uani 1 1 d . . .
C63 C 0.7841(7) 0.1449(5) -0.1697(7) 0.054(2) Uani 1 1 d . . .
C64 C 1.0566(7) 0.2395(5) -0.0585(7) 0.056(2) Uani 1 1 d . . .
C65 C 1.1198(8) 0.1925(6) -0.0329(10) 0.080(3) Uani 1 1 d . . .
H70 H 1.0991 0.1647 0.0193 0.080 Uiso 1 1 calc R . .
H71 H 1.1901 0.2193 -0.0058 0.080 Uiso 1 1 calc R . .
H72 H 1.1108 0.1634 -0.0959 0.080 Uiso 1 1 calc R . .
C66 C 1.0863(9) 0.2805(7) -0.1434(10) 0.093(4) Uani 1 1 d . . .
H73 H 1.1519 0.3141 -0.1145 0.093 Uiso 1 1 calc R . .
H74 H 1.0370 0.3034 -0.1706 0.093 Uiso 1 1 calc R . .
H75 H 1.0888 0.2504 -0.1997 0.093 Uiso 1 1 calc R . .
C67 C 0.6819(9) 0.1129(6) -0.2478(8) 0.069(3) Uani 1 1 d . . .
C68 C 0.6956(11) 0.1062(8) -0.3616(9) 0.102(5) Uani 1 1 d . . .
H77 H 0.7443 0.0825 -0.3618 0.102 Uiso 1 1 calc R . .
H78 H 0.7193 0.1512 -0.3821 0.102 Uiso 1 1 calc R . .
H79 H 0.6316 0.0808 -0.4107 0.102 Uiso 1 1 calc R . .
C69 C 0.6100(9) 0.1536(7) -0.2460(10) 0.089(4) Uani 1 1 d . . .
H80 H 0.6326 0.1962 -0.2740 0.089 Uiso 1 1 calc R . .
H81 H 0.6086 0.1630 -0.1745 0.089 Uiso 1 1 calc R . .
H82 H 0.5430 0.1276 -0.2884 0.089 Uiso 1 1 calc R . .
C71 C 0.6581(6) 0.2376(4) 0.1036(8) 0.050(2) Uani 1 1 d . . .
C72 C 0.6623(7) 0.2040(5) 0.1935(8) 0.058(2) Uani 1 1 d . . .
C73 C 0.6957(6) 0.1482(5) 0.1763(7) 0.053(2) Uani 1 1 d . . .
C74 C 0.6276(7) 0.3006(5) 0.0792(10) 0.068(3) Uani 1 1 d . . .
C75 C 0.5782(9) 0.3214(6) 0.1610(11) 0.087(4) Uani 1 1 d . . .
H85 H 0.6247 0.3294 0.2305 0.087 Uiso 1 1 calc R . .
H86 H 0.5172 0.2851 0.1589 0.087 Uiso 1 1 calc R . .
H87 H 0.5617 0.3627 0.1446 0.087 Uiso 1 1 calc R . .
C76 C 0.5591(10) 0.2930(6) -0.0316(10) 0.090(4) Uani 1 1 d . . .
H88 H 0.5348 0.3320 -0.0403 0.090 Uiso 1 1 calc R . .
H89 H 0.5024 0.2518 -0.0431 0.090 Uiso 1 1 calc R . .
H90 H 0.5964 0.2903 -0.0819 0.090 Uiso 1 1 calc R . .
C77 C 0.7074(7) 0.0947(5) 0.2479(7) 0.057(2) Uani 1 1 d . . .
C78 C 0.7831(13) 0.1257(9) 0.3517(11) 0.137(7) Uani 1 1 d . . .
H92 H 0.8301 0.0999 0.3692 0.137 Uiso 1 1 calc R . .
H93 H 0.7486 0.1246 0.4056 0.137 Uiso 1 1 calc R . .
H94 H 0.8195 0.1725 0.3472 0.137 Uiso 1 1 calc R . .
C79 C 0.6066(10) 0.0540(8) 0.2636(14) 0.119(6) Uani 1 1 d . . .
H95 H 0.5851 0.0824 0.3065 0.119 Uiso 1 1 calc R . .
H96 H 0.6139 0.0147 0.2981 0.119 Uiso 1 1 calc R . .
H97 H 0.5568 0.0390 0.1960 0.119 Uiso 1 1 calc R . .
C81 C 0.3332(19) 0.1930(13) 0.684(2) 0.192(12) Uani 1 1 d . . .
C82 C 0.3037(19) 0.1338(14) 0.612(2) 0.177(10) Uani 1 1 d . . .
C84 C 0.349(3) 0.0873(15) 0.472(2) 0.203(14) Uani 1 1 d . . .
C85 C 0.422(3) 0.098(2) 0.412(2) 0.28(2) Uani 1 1 d . . .
B1 B 1.2839(6) 0.4569(5) 0.3893(7) 0.0375(18) Uani 1 1 d . . .
B2 B 0.7303(7) 0.1014(5) 0.0008(8) 0.047(2) Uani 1 1 d . . .
H1 H 1.3482 0.4888 0.4257 0.045 Uiso 1 1 d . . .
H2 H 1.0893 0.6048 0.3500 0.048 Uiso 1 1 d . . .
H3 H 0.9100 0.4500 0.2047 0.058 Uiso 1 1 d . . .
H10 H 1.3559 0.6027 0.4514 0.051 Uiso 1 1 d . . .
H17 H 1.2302 0.3275 0.6625 0.053 Uiso 1 1 d . . .
H18 H 1.0014 0.2521 0.4200 0.048 Uiso 1 1 d . . .
H25 H 1.4354 0.4538 0.5794 0.053 Uiso 1 1 d . . .
H32 H 1.3349 0.3314 0.1200 0.064 Uiso 1 1 d . . .
H33 H 1.2328 0.4268 -0.0238 0.114 Uiso 1 1 d . . .
H40 H 1.2787 0.3063 0.3743 0.052 Uiso 1 1 d . . .
H47 H 0.8726 0.2869 0.1156 0.051 Uiso 1 1 d . . .
H48 H 0.7868 0.2973 -0.0558 0.056 Uiso 1 1 d . . .
H49 H 0.8678 0.3807 -0.1471 0.071 Uiso 1 1 d . . .
H50 H 1.0349 0.4554 -0.0618 0.065 Uiso 1 1 d . . .
H51 H 1.1149 0.4402 0.1107 0.051 Uiso 1 1 d . . .
H52 H 0.6664 0.0741 -0.0474 0.060 Uiso 1 1 d . . .
H53 H 0.8161 -0.0813 0.1507 0.089 Uiso 1 1 d . . .
H54 H 1.0310 0.0805 0.2792 0.093 Uiso 1 1 d . . .
H68 H 0.8888 0.1990 -0.2515 0.069 Uiso 1 1 d . . .
H69 H 1.0742 0.2706 0.0049 0.067 Uiso 1 1 d . . .
H76 H 0.6515 0.0670 -0.2313 0.083 Uiso 1 1 d . . .
H83 H 0.6450 0.2170 0.2567 0.069 Uiso 1 1 d . . .
H84 H 0.6884 0.3380 0.0849 0.081 Uiso 1 1 d . . .
H91 H 0.7324 0.0624 0.2142 0.069 Uiso 1 1 d . . .
H98 H 0.4029 0.2006 0.7332 0.206 Uiso 1 1 d . . .
H99 H 0.3372 0.2334 0.6514 0.206 Uiso 1 1 d . . .
H100 H 0.2924 0.1934 0.7347 0.206 Uiso 1 1 d . . .
H101 H 0.2332 0.1284 0.5773 0.209 Uiso 1 1 d . . .
H102 H 0.2992 0.0956 0.6590 0.209 Uiso 1 1 d . . .
H103 H 0.3468 0.0439 0.5019 0.214 Uiso 1 1 d . . .
H104 H 0.2837 0.0802 0.4238 0.214 Uiso 1 1 d . . .
H105 H 0.4870 0.1026 0.4590 0.246 Uiso 1 1 d . . .
H106 H 0.4039 0.0601 0.3592 0.246 Uiso 1 1 d . . .
H107 H 0.4237 0.1387 0.3806 0.246 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
Pd Pd -0.9988 1.0072 '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'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
N11 Pd1 O1 167.8(2) . . ?
N11 Pd1 N21 85.2(2) . . ?
O1 Pd1 N21 94.8(2) . . ?
N11 Pd1 N41 91.2(2) . . ?
O1 Pd1 N41 88.4(2) . . ?
N21 Pd1 N41 176.1(2) . . ?
O2 Pd2 N61 159.8(2) . . ?
O2 Pd2 N51 111.7(3) . . ?
N61 Pd2 N51 88.1(3) . . ?
O2 Pd2 O1 42.0(2) . . ?
N61 Pd2 O1 117.9(2) . . ?
N51 Pd2 O1 153.5(3) . . ?
O2 O1 Pd1 119.0(4) . . ?
O2 O1 Pd2 66.2(3) . . ?
Pd1 O1 Pd2 132.7(3) . . ?
O1 O2 Pd2 71.8(3) . . ?
C84 O83 C82 119(2) . . ?
C11 N11 N12 106.6(6) . . ?
C11 N11 Pd1 136.3(5) . . ?
N12 N11 Pd1 116.8(5) . . ?
C13 N12 N11 109.8(6) . . ?
C13 N12 B1 131.9(6) . . ?
N11 N12 B1 117.9(6) . . ?
C21 N21 N22 107.9(6) . . ?
C21 N21 Pd1 136.1(5) . . ?
N22 N21 Pd1 115.9(5) . . ?
C23 N22 N21 108.9(6) . . ?
C23 N22 B1 131.4(6) . . ?
N21 N22 B1 119.4(6) . . ?
C31 N31 N32 105.5(7) . . ?
C33 N32 N31 110.2(6) . . ?
C33 N32 B1 135.1(7) . . ?
N31 N32 B1 114.3(6) . . ?
C42 N41 C46 119.3(7) . . ?
C42 N41 Pd1 122.2(5) . . ?
C46 N41 Pd1 118.5(5) . . ?
C51 N51 N52 110.4(6) . . ?
C51 N51 Pd2 127.8(5) . . ?
N52 N51 Pd2 121.5(5) . . ?
C53 N52 N51 109.0(7) . . ?
C53 N52 B2 130.1(7) . . ?
N51 N52 B2 120.9(6) . . ?
C61 N61 N62 106.8(6) . . ?
C61 N61 Pd2 129.8(5) . . ?
N62 N61 Pd2 123.0(5) . . ?
C63 N62 N61 108.7(7) . . ?
C63 N62 B2 132.2(8) . . ?
N61 N62 B2 118.5(6) . . ?
C71 N71 N72 106.2(8) . . ?
C73 N72 N71 111.1(7) . . ?
C73 N72 B2 134.3(8) . . ?
N71 N72 B2 113.8(7) . . ?
N11 C11 C12 109.6(6) . . ?
N11 C11 C14 121.6(7) . . ?
C12 C11 C14 128.8(7) . . ?
C11 C12 C13 106.4(7) . . ?
N12 C13 C12 107.8(6) . . ?
N12 C13 C17 125.3(7) . . ?
C12 C13 C17 126.6(7) . . ?
C15 C14 C11 112.3(7) . . ?
C15 C14 C16 111.7(8) . . ?
C11 C14 C16 110.7(7) . . ?
C18 C17 C19 111.0(9) . . ?
C18 C17 C13 111.5(7) . . ?
C19 C17 C13 112.2(7) . . ?
N21 C21 C22 108.8(7) . . ?
N21 C21 C24 121.1(6) . . ?
C22 C21 C24 130.0(7) . . ?
C23 C22 C21 106.8(7) . . ?
N22 C23 C22 107.6(7) . . ?
N22 C23 C27 122.8(7) . . ?
C22 C23 C27 129.6(7) . . ?
C21 C24 C25 110.8(7) . . ?
C21 C24 C26 110.5(7) . . ?
C25 C24 C26 110.6(7) . . ?
C23 C27 C28 110.2(7) . . ?
C23 C27 C29 112.3(7) . . ?
C28 C27 C29 111.3(7) . . ?
N31 C31 C32 111.7(8) . . ?
N31 C31 C34 120.6(9) . . ?
C32 C31 C34 127.6(9) . . ?
C33 C32 C31 105.0(8) . . ?
N32 C33 C32 107.5(8) . . ?
N32 C33 C37 125.7(7) . . ?
C32 C33 C37 126.8(8) . . ?
C35 C34 C36 119.6(14) . . ?
C35 C34 C31 113.6(11) . . ?
C36 C34 C31 110.7(10) . . ?
C33 C37 C38 110.9(7) . . ?
C33 C37 C39 112.4(7) . . ?
C38 C37 C39 109.8(7) . . ?
N41 C42 C43 122.6(8) . . ?
C44 C43 C42 117.7(8) . . ?
C45 C44 C43 119.9(8) . . ?
C44 C45 C46 119.9(8) . . ?
N41 C46 C45 120.7(7) . . ?
N51 C51 C52 106.9(8) . . ?
N51 C51 C54 123.7(8) . . ?
C52 C51 C54 129.4(9) . . ?
C53 C52 C51 106.8(9) . . ?
N52 C53 C52 106.6(8) . . ?
N52 C53 C57 123.5(9) . . ?
C52 C53 C57 129.8(9) . . ?
C55 C54 C51 113.4(10) . . ?
C55 C54 C56 112.7(12) . . ?
C51 C54 C56 108.7(11) . . ?
C59 C57 C58A 131.5(17) . . ?
C59 C57 C53 114.6(17) . . ?
C58A C57 C53 113.9(12) . . ?
C59 C57 C59A 44.5(18) . . ?
C58A C57 C59A 114.0(16) . . ?
C53 C57 C59A 110.3(11) . . ?
C59 C57 C58 117(2) . . ?
C58A C57 C58 46.5(16) . . ?
C53 C57 C58 104.8(13) . . ?
C59A C57 C58 76.9(19) . . ?
C58A C58 C57 58.5(17) . . ?
C58 C58A C57 75(2) . . ?
C59A C59 C57 84(3) . . ?
C59 C59A C57 51.3(17) . . ?
N61 C61 C62 110.8(8) . . ?
N61 C61 C64 120.7(7) . . ?
C62 C61 C64 128.5(8) . . ?
C63 C62 C61 105.0(8) . . ?
N62 C63 C62 108.5(8) . . ?
N62 C63 C67 122.1(9) . . ?
C62 C63 C67 129.3(9) . . ?
C65 C64 C66 109.2(10) . . ?
C65 C64 C61 112.0(9) . . ?
C66 C64 C61 112.6(9) . . ?
C63 C67 C69 112.7(8) . . ?
C63 C67 C68 109.1(10) . . ?
C69 C67 C68 109.5(10) . . ?
N71 C71 C72 110.3(8) . . ?
N71 C71 C74 119.8(9) . . ?
C72 C71 C74 129.9(9) . . ?
C71 C72 C73 107.2(8) . . ?
N72 C73 C72 105.3(9) . . ?
N72 C73 C77 127.4(8) . . ?
C72 C73 C77 127.2(9) . . ?
C71 C74 C76 112.7(9) . . ?
C71 C74 C75 111.5(10) . . ?
C76 C74 C75 110.5(9) . . ?
C73 C77 C78 111.3(9) . . ?
C73 C77 C79 111.4(9) . . ?
C78 C77 C79 110.7(11) . . ?
C81 C82 O83 112(3) . . ?
O83 C84 C85 114(3) . . ?
N32 B1 N22 110.8(7) . . ?
N32 B1 N12 109.9(6) . . ?
N22 B1 N12 106.5(6) . . ?
N72 B2 N52 112.3(7) . . ?
N72 B2 N62 110.7(7) . . ?
N52 B2 N62 108.4(7) . . ?
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 N11 1.992(6) . ?
Pd1 O1 1.993(5) . ?
Pd1 N21 2.007(6) . ?
Pd1 N41 2.027(6) . ?
Pd2 O2 1.968(6) . ?
Pd2 N61 2.028(7) . ?
Pd2 N51 2.042(6) . ?
Pd2 O1 2.044(5) . ?
O1 O2 1.439(8) . ?
O83 C84 1.33(3) . ?
O83 C82 1.41(3) . ?
N11 C11 1.336(10) . ?
N11 N12 1.396(8) . ?
N12 C13 1.323(10) . ?
N12 B1 1.569(11) . ?
N21 C21 1.325(10) . ?
N21 N22 1.394(8) . ?
N22 C23 1.353(10) . ?
N22 B1 1.551(11) . ?
N31 C31 1.312(11) . ?
N31 N32 1.393(9) . ?
N32 C33 1.361(10) . ?
N32 B1 1.531(11) . ?
N41 C42 1.343(9) . ?
N41 C46 1.346(10) . ?
N51 C51 1.323(11) . ?
N51 N52 1.353(8) . ?
N52 C53 1.355(11) . ?
N52 B2 1.541(12) . ?
N61 C61 1.330(11) . ?
N61 N62 1.384(9) . ?
N62 C63 1.351(11) . ?
N62 B2 1.553(13) . ?
N71 C71 1.324(11) . ?
N71 N72 1.378(10) . ?
N72 C73 1.365(11) . ?
N72 B2 1.544(12) . ?
C11 C12 1.382(10) . ?
C11 C14 1.516(10) . ?
C12 C13 1.396(10) . ?
C13 C17 1.510(10) . ?
C14 C15 1.500(13) . ?
C14 C16 1.523(13) . ?
C17 C18 1.503(13) . ?
C17 C19 1.503(13) . ?
C21 C22 1.407(10) . ?
C21 C24 1.498(10) . ?
C22 C23 1.382(11) . ?
C23 C27 1.501(10) . ?
C24 C25 1.514(12) . ?
C24 C26 1.536(12) . ?
C27 C28 1.519(12) . ?
C27 C29 1.521(12) . ?
C31 C32 1.414(13) . ?
C31 C34 1.524(14) . ?
C32 C33 1.378(12) . ?
C33 C37 1.488(12) . ?
C34 C35 1.423(18) . ?
C34 C36 1.519(19) . ?
C37 C38 1.516(11) . ?
C37 C39 1.536(12) . ?
C42 C43 1.381(11) . ?
C43 C44 1.380(12) . ?
C44 C45 1.370(12) . ?
C45 C46 1.376(12) . ?
C51 C52 1.411(12) . ?
C51 C54 1.487(13) . ?
C52 C53 1.399(14) . ?
C53 C57 1.508(12) . ?
C54 C55 1.478(18) . ?
C54 C56 1.51(2) . ?
C57 C59 1.26(3) . ?
C57 C58A 1.44(2) . ?
C57 C59A 1.60(2) . ?
C57 C58 1.63(3) . ?
C58 C58A 1.22(4) . ?
C59 C59A 1.13(4) . ?
C61 C62 1.388(12) . ?
C61 C64 1.511(12) . ?
C62 C63 1.389(13) . ?
C63 C67 1.500(13) . ?
C64 C65 1.495(15) . ?
C64 C66 1.498(15) . ?
C67 C69 1.506(16) . ?
C67 C68 1.566(16) . ?
C71 C72 1.390(14) . ?
C71 C74 1.500(13) . ?
C72 C73 1.392(13) . ?
C73 C77 1.491(14) . ?
C74 C76 1.509(16) . ?
C74 C75 1.540(16) . ?
C77 C78 1.491(15) . ?
C77 C79 1.511(15) . ?
C81 C82 1.40(3) . ?
C84 C85 1.43(5) . ?
