#------------------------------------------------------------------------------
#$Date: 2019-11-23 13:49:10 +0200 (Sat, 23 Nov 2019) $
#$Revision: 233503 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/89/4348946.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_4348946
loop_
_publ_author_name
'Fortea-Pérez, Francisco Ramón'
'Rothenpieler, Berit L.'
'Marino, Nadia'
'Armentano, Donatella'
'De Munno, Giovanni'
'Julve, Miguel'
'Stiriba, Salah-Eddine'
_publ_section_title
;
 Bis(N-substituted oxamate)palladate(ii) complexes as effective catalysts
 for sustainable Heck carbon--carbon coupling reactions in n-Bu4NBr as the
 solvent
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1029
_journal_paper_doi               10.1039/C5QI00093A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety
'3(C16 H8 Br2 N2 O6 Pd), 6(C16 H36 N), 3(H2 O)'
_chemical_formula_sum            'C144 H234 Br6 N12 O21 Pd3'
_chemical_formula_weight         3268.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.901(8)
_cell_angle_beta                 103.304(8)
_cell_angle_gamma                99.809(8)
_cell_formula_units_Z            1
_cell_length_a                   13.524(2)
_cell_length_b                   16.287(3)
_cell_length_c                   20.967(3)
_cell_measurement_reflns_used    9575
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.17
_cell_volume                     4301.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.457
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             1698
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         18125
_refine_ls_number_restraints     956
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1255P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9794
_reflns_number_total             18125
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5qi00093a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        4301.1(13)
_cod_database_code               4348946
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.843
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.5000 0.5000 0.05810(16) Uani 1 2 d S . P . .
C1A C 0.7044(4) 0.5172(3) 0.5800(2) 0.0696(12) Uani 1 1 d . . . . .
C2A C 0.7140(3) 0.5049(3) 0.5060(2) 0.0639(11) Uani 1 1 d . . . . .
O1A O 0.6111(2) 0.5163(2) 0.58657(14) 0.0725(8) Uani 1 1 d . . . . .
O2A O 0.7813(2) 0.5296(3) 0.62683(17) 0.0967(11) Uani 1 1 d . . . . .
O3A O 0.7992(2) 0.4979(2) 0.49427(17) 0.0806(9) Uani 1 1 d . . . . .
N1A N 0.6260(3) 0.5067(2) 0.46194(17) 0.0629(9) Uani 1 1 d . . . . .
C3A C 0.6246(3) 0.5076(3) 0.3942(2) 0.0646(11) Uani 1 1 d . . . . .
C4A C 0.6659(4) 0.4503(4) 0.3558(2) 0.0825(14) Uani 1 1 d . . . . .
H4A H 0.6956 0.4096 0.3740 0.099 Uiso 1 1 calc R U . . .
C5A C 0.6623(5) 0.4547(4) 0.2889(3) 0.0985(18) Uani 1 1 d . . . . .
H5A H 0.6902 0.4169 0.2630 0.118 Uiso 1 1 calc R U . . .
C6A C 0.6187(4) 0.5131(5) 0.2622(3) 0.0951(17) Uani 1 1 d . . . . .
C7A C 0.5776(4) 0.5715(4) 0.2994(3) 0.0953(17) Uani 1 1 d . . . . .
H7A H 0.5489 0.6125 0.2807 0.114 Uiso 1 1 calc R U . . .
C8A C 0.5806(4) 0.5670(4) 0.3656(3) 0.0825(14) Uani 1 1 d . . . . .
H8A H 0.5522 0.6050 0.3911 0.099 Uiso 1 1 calc R U . . .
Br1A Br 0.61542(7) 0.51689(7) 0.17089(4) 0.1576(4) Uani 1 1 d . . . . .
Pd2 Pd 0.0000 0.0000 0.0000 0.06466(17) Uani 1 2 d S . P . .
C1B C -0.2108(4) -0.0842(4) -0.0329(2) 0.0795(14) Uani 1 1 d . . . . .
C2B C -0.2094(3) 0.0108(3) -0.0021(2) 0.0714(13) Uani 1 1 d . . . . .
O1B O -0.1224(2) -0.1018(2) -0.03579(17) 0.0801(9) Uani 1 1 d . . . . .
O2B O -0.2948(3) -0.1369(3) -0.0533(2) 0.1131(14) Uani 1 1 d . . . . .
O3B O -0.2898(2) 0.0324(2) 0.00706(18) 0.0852(10) Uani 1 1 d . . . . .
N1B N -0.1158(3) 0.0636(3) 0.00729(19) 0.0700(10) Uani 1 1 d . . . . .
C3B C -0.1038(3) 0.1532(3) 0.0246(2) 0.0682(12) Uani 1 1 d . . . . .
C4B C -0.1447(4) 0.1967(4) 0.0720(3) 0.0895(15) Uani 1 1 d . . . . .
H4B H -0.1811 0.1659 0.0958 0.107 Uiso 1 1 calc R U . . .
C5B C -0.1328(5) 0.2857(4) 0.0851(3) 0.1043(18) Uani 1 1 d . . . . .
H5B H -0.1613 0.3137 0.1169 0.125 Uiso 1 1 calc R U . . .
C6B C -0.0792(5) 0.3308(4) 0.0510(3) 0.0993(17) Uani 1 1 d . . . . .
C7B C -0.0361(5) 0.2916(4) 0.0042(3) 0.0955(16) Uani 1 1 d . . . . .
H7B H 0.0001 0.3235 -0.0189 0.115 Uiso 1 1 calc R U . . .
C8B C -0.0474(4) 0.2033(4) -0.0081(3) 0.0889(16) Uani 1 1 d . . . . .
H8B H -0.0166 0.1765 -0.0390 0.107 Uiso 1 1 calc R U . . .
Br1B Br -0.06446(9) 0.45358(6) 0.06946(6) 0.1635(4) Uani 1 1 d . . . . .
Pd3 Pd 1.0000 1.0000 0.5000 0.0908(2) Uani 1 2 d S . P . .
C1C C 0.8021(7) 1.0344(4) 0.4553(4) 0.111(2) Uani 1 1 d . . . . .
C2C C 0.8093(6) 0.9663(4) 0.3961(3) 0.1040(19) Uani 1 1 d . . . . .
O1C O 0.8836(4) 1.0592(3) 0.5074(2) 0.1136(13) Uani 1 1 d . . . . .
O2C O 0.7242(5) 1.0629(4) 0.4516(3) 0.153(2) Uani 1 1 d . . . . .
O3C O 0.7357(4) 0.9417(3) 0.3443(3) 0.1380(17) Uani 1 1 d . . . . .
N1C N 0.8998(4) 0.9421(3) 0.4068(2) 0.0934(13) Uani 1 1 d . . . . .
C3C C 0.9180(6) 0.8796(4) 0.3557(3) 0.0960(18) Uani 1 1 d . . . . .
C4C C 0.8454(6) 0.8061(4) 0.3207(3) 0.109(2) Uani 1 1 d . . . . .
H4C H 0.7803 0.7960 0.3291 0.131 Uiso 1 1 calc R U . . .
C5C C 0.8687(9) 0.7460(4) 0.2723(3) 0.126(3) Uani 1 1 d . . . . .
H5C H 0.8179 0.6969 0.2483 0.151 Uiso 1 1 calc R U . . .
C6C C 0.9602(10) 0.7569(6) 0.2598(4) 0.135(3) Uani 1 1 d . . . . .
C7C C 1.0378(7) 0.8317(6) 0.2936(4) 0.132(3) Uani 1 1 d . . . . .
H7C H 1.1019 0.8409 0.2838 0.158 Uiso 1 1 calc R U . . .
C8C C 1.0152(7) 0.8917(4) 0.3424(3) 0.111(2) Uani 1 1 d . . . . .
H8C H 1.0661 0.9407 0.3665 0.133 Uiso 1 1 calc R U . . .
Br1C Br 0.98800(13) 0.67592(8) 0.19272(5) 0.2149(7) Uani 1 1 d . . . . .
N1 N 0.9557(3) 0.3187(3) 0.5289(2) 0.0739(9) Uani 1 1 d . U . . .
C1 C 1.0442(4) 0.2703(4) 0.5388(3) 0.0848(13) Uani 1 1 d . U . . .
H1A H 1.0761 0.2805 0.5869 0.102 Uiso 1 1 calc R U . . .
H1B H 1.0137 0.2093 0.5221 0.102 Uiso 1 1 calc R U . . .
C2 C 1.1301(5) 0.2935(4) 0.5047(4) 0.1117(19) Uani 1 1 d . U . . .
H2A H 1.0986 0.2872 0.4570 0.134 Uiso 1 1 calc R U . . .
H2B H 1.1654 0.3532 0.5240 0.134 Uiso 1 1 calc R U . . .
C3 C 1.2084(6) 0.2391(5) 0.5125(5) 0.136(2) Uani 1 1 d . U . . .
H3A H 1.1717 0.1795 0.5013 0.163 Uiso 1 1 calc R U . . .
H3B H 1.2483 0.2534 0.5594 0.163 Uiso 1 1 calc R U . . .
C4 C 1.2826(7) 0.2485(7) 0.4697(5) 0.171(4) Uani 1 1 d . U . . .
H4D H 1.2780 0.1936 0.4413 0.257 Uiso 1 1 calc R U . . .
H4E H 1.3524 0.2704 0.4983 0.257 Uiso 1 1 calc R U . . .
H4F H 1.2648 0.2875 0.4422 0.257 Uiso 1 1 calc R U . . .
C5 C 0.9135(4) 0.3175(3) 0.4540(2) 0.0833(13) Uani 1 1 d . U . . .
H5D H 0.8600 0.3504 0.4498 0.100 Uiso 1 1 calc R U . . .
H5E H 0.9697 0.3458 0.4387 0.100 Uiso 1 1 calc R U . . .
C6 C 0.8688(5) 0.2298(4) 0.4088(3) 0.1071(17) Uani 1 1 d . U . . .
H6A H 0.8065 0.2035 0.4193 0.128 Uiso 1 1 calc R U . . .
H6B H 0.9190 0.1940 0.4156 0.128 Uiso 1 1 calc R U . . .
C7 C 0.8418(7) 0.2373(5) 0.3344(3) 0.139(3) Uani 1 1 d . U . . .
H7D H 0.9036 0.2649 0.3240 0.167 Uiso 1 1 calc R U . . .
H7E H 0.7897 0.2713 0.3269 0.167 Uiso 1 1 calc R U . . .
C8 C 0.7988(9) 0.1445(6) 0.2888(5) 0.191(4) Uani 1 1 d . U . . .
H8D H 0.8508 0.1114 0.2969 0.286 Uiso 1 1 calc R U . . .
H8E H 0.7818 0.1468 0.2423 0.286 Uiso 1 1 calc R U . . .
H8F H 0.7373 0.1181 0.2993 0.286 Uiso 1 1 calc R U . . .
C9 C 0.8719(4) 0.2721(3) 0.5553(3) 0.0771(12) Uani 1 1 d . U . . .
H9A H 0.8514 0.2125 0.5306 0.093 Uiso 1 1 calc R U . . .
H9B H 0.9022 0.2734 0.6023 0.093 Uiso 1 1 calc R U . . .
C10 C 0.7746(4) 0.3077(4) 0.5505(3) 0.0952(15) Uani 1 1 d . U . . .
H10A H 0.7933 0.3667 0.5767 0.114 Uiso 1 1 calc R U . . .
H10B H 0.7436 0.3074 0.5039 0.114 Uiso 1 1 calc R U . . .
C11 C 0.6961(6) 0.2552(5) 0.5765(4) 0.130(2) Uani 1 1 d . U . . .
H11A H 0.6799 0.1961 0.5510 0.156 Uiso 1 1 calc R U . . .
H11B H 0.7277 0.2566 0.6232 0.156 Uiso 1 1 calc R U . . .
C12 C 0.5965(6) 0.2851(6) 0.5719(5) 0.158(3) Uani 1 1 d . U . . .
H12A H 0.6070 0.3340 0.6084 0.237 Uiso 1 1 calc R U . . .
H12B H 0.5432 0.2398 0.5746 0.237 Uiso 1 1 calc R U . . .
H12C H 0.5754 0.3007 0.5297 0.237 Uiso 1 1 calc R U . . .
C13 C 0.9930(4) 0.4124(3) 0.5653(2) 0.0764(11) Uani 1 1 d . U . . .
H13A H 0.9373 0.4412 0.5515 0.092 Uiso 1 1 calc R U . . .
H13B H 1.0512 0.4368 0.5498 0.092 Uiso 1 1 calc R U . . .
C14 C 1.0269(5) 0.4339(4) 0.6417(3) 0.0924(14) Uani 1 1 d . U . . .
H14A H 0.9719 0.4064 0.6584 0.111 Uiso 1 1 calc R U . . .
H14B H 1.0885 0.4122 0.6569 0.111 Uiso 1 1 calc R U . . .
C15 C 1.0504(4) 0.5293(4) 0.6692(3) 0.0972(15) Uani 1 1 d . U . . .
H15A H 1.1087 0.5550 0.6544 0.117 Uiso 1 1 calc R U . . .
H15B H 0.9906 0.5504 0.6492 0.117 Uiso 1 1 calc R U . . .
C16 C 1.0758(7) 0.5598(5) 0.7435(4) 0.146(3) Uani 1 1 d . U . . .
H16A H 1.0133 0.5487 0.7578 0.218 Uiso 1 1 calc R U . . .
H16B H 1.1056 0.6204 0.7564 0.218 Uiso 1 1 calc R U . . .
H16C H 1.1248 0.5302 0.7645 0.218 Uiso 1 1 calc R U . . .
N2 N 0.4868(3) 0.0850(4) 0.8716(2) 0.0974(11) Uani 1 1 d . U . . .
C17 C 0.5307(5) 0.1633(5) 0.9300(3) 0.1197(18) Uani 1 1 d . U . . .
H17A H 0.5981 0.1582 0.9555 0.144 Uiso 1 1 calc R U . . .
H17B H 0.4851 0.1628 0.9596 0.144 Uiso 1 1 calc R U . . .
C18 C 0.5443(8) 0.2503(6) 0.9116(4) 0.163(3) Uani 1 1 d . U . . .
H18A H 0.4769 0.2601 0.8906 0.196 Uiso 1 1 calc R U . . .
H18B H 0.5866 0.2516 0.8801 0.196 Uiso 1 1 calc R U . . .
C19 C 0.5988(9) 0.3210(7) 0.9780(5) 0.187(4) Uani 1 1 d . U . . .
H19A H 0.5539 0.3220 1.0080 0.225 Uiso 1 1 calc R U . . .
H19B H 0.6633 0.3081 1.0007 0.225 Uiso 1 1 calc R U . . .
C20 C 0.6208(13) 0.4044(8) 0.9622(7) 0.271(8) Uani 1 1 d . U . . .
H20A H 0.5673 0.4062 0.9238 0.407 Uiso 1 1 calc R U . . .
H20B H 0.6871 0.4135 0.9523 0.407 Uiso 1 1 calc R U . . .
H20C H 0.6224 0.4485 1.0002 0.407 Uiso 1 1 calc R U . . .
C21 C 0.3791(4) 0.0886(4) 0.8305(3) 0.0972(16) Uani 1 1 d . U . . .
H21A H 0.3552 0.0396 0.7920 0.117 Uiso 1 1 calc R U . . .
H21B H 0.3859 0.1399 0.8133 0.117 Uiso 1 1 calc R U . . .
C22 C 0.2951(4) 0.0889(5) 0.8695(3) 0.1033(17) Uani 1 1 d . U . . .
H22A H 0.2863 0.0372 0.8862 0.124 Uiso 1 1 calc R U . . .
H22B H 0.3178 0.1378 0.9081 0.124 Uiso 1 1 calc R U . . .
C23 C 0.1932(5) 0.0932(5) 0.8255(3) 0.118(2) Uani 1 1 d . U . . .
H23A H 0.2039 0.1437 0.8076 0.141 Uiso 1 1 calc R U . . .
H23B H 0.1711 0.0435 0.7876 0.141 Uiso 1 1 calc R U . . .
C24 C 0.1080(5) 0.0962(5) 0.8585(4) 0.129(2) Uani 1 1 d . U . . .
H24A H 0.0866 0.0417 0.8682 0.194 Uiso 1 1 calc R U . . .
H24B H 0.0500 0.1090 0.8290 0.194 Uiso 1 1 calc R U . . .
H24C H 0.1321 0.1400 0.8998 0.194 Uiso 1 1 calc R U . . .
C25 C 0.4820(4) 0.0079(5) 0.9030(3) 0.0993(14) Uani 1 1 d . U . . .
H25A H 0.5516 0.0097 0.9297 0.119 Uiso 1 1 calc R U . . .
H25B H 0.4382 0.0132 0.9336 0.119 Uiso 1 1 calc R U . . .
C26 C 0.4416(6) -0.0776(5) 0.8544(3) 0.1195(18) Uani 1 1 d . U . . .
H26A H 0.4871 -0.0859 0.8253 0.143 Uiso 1 1 calc R U . . .
H26B H 0.3726 -0.0803 0.8263 0.143 Uiso 1 1 calc R U . . .
C27 C 0.4364(5) -0.1492(5) 0.8939(3) 0.1157(17) Uani 1 1 d . U . . .
H27A H 0.5059 -0.1464 0.9211 0.139 Uiso 1 1 calc R U . . .
H27B H 0.3933 -0.1385 0.9244 0.139 Uiso 1 1 calc R U . . .
C28 C 0.3921(8) -0.2397(6) 0.8479(5) 0.164(3) Uani 1 1 d . U . . .
H28A H 0.3248 -0.2421 0.8192 0.246 Uiso 1 1 calc R U . . .
H28B H 0.3857 -0.2806 0.8751 0.246 Uiso 1 1 calc R U . . .
H28C H 0.4382 -0.2530 0.8208 0.246 Uiso 1 1 calc R U . . .
C29 C 0.5536(5) 0.0802(6) 0.8221(3) 0.133(2) Uani 1 1 d . U . . .
H29A H 0.5541 0.1298 0.8028 0.159 Uiso 1 1 calc R U . . .
H29B H 0.5218 0.0295 0.7856 0.159 Uiso 1 1 calc R U . . .
C30 C 0.6674(6) 0.0767(8) 0.8538(5) 0.185(4) Uani 1 1 d . U . . .
H30A H 0.6687 0.0302 0.8767 0.222 Uiso 1 1 calc R U . . .
H30B H 0.7034 0.1301 0.8866 0.222 Uiso 1 1 calc R U . . .
C31 C 0.7233(8) 0.0619(10) 0.7951(6) 0.228(5) Uani 1 1 d . U . . .
H31A H 0.6750 0.0188 0.7574 0.274 Uiso 1 1 calc R U . . .
H31B H 0.7343 0.1148 0.7803 0.274 Uiso 1 1 calc R U . . .
C32 C 0.8075(13) 0.0396(14) 0.8067(10) 0.333(9) Uani 1 1 d . U . . .
H32A H 0.8601 0.0855 0.8386 0.499 Uiso 1 1 calc R U . . .
H32B H 0.8275 0.0263 0.7655 0.499 Uiso 1 1 calc R U . . .
H32C H 0.8004 -0.0101 0.8250 0.499 Uiso 1 1 calc R U . . .
N3 N 0.2654(3) 0.3404(3) 0.19925(17) 0.0875(10) Uani 1 1 d D U . . .
C33 C 0.1775(6) 0.2570(5) 0.1819(4) 0.095(2) Uani 0.683(4) 1 d D U P A 1
H33A H 0.1246 0.2578 0.1421 0.114 Uiso 0.683(4) 1 calc R U P A 1
H33B H 0.2074 0.2081 0.1702 0.114 Uiso 0.683(4) 1 calc R U P A 1
C34 C 0.1251(10) 0.2430(7) 0.2351(6) 0.151(4) Uani 0.683(4) 1 d D U P A 1
H34A H 0.0809 0.2836 0.2399 0.181 Uiso 0.683(4) 1 calc R U P A 1
H34B H 0.1774 0.2537 0.2779 0.181 Uiso 0.683(4) 1 calc R U P A 1
C35 C 0.0586(11) 0.1515(8) 0.2188(6) 0.167(4) Uani 0.683(4) 1 d D U P A 1
H35A H -0.0122 0.1503 0.1948 0.200 Uiso 0.683(4) 1 calc R U P A 1
H35B H 0.0861 0.1133 0.1896 0.200 Uiso 0.683(4) 1 calc R U P A 1
C36 C 0.0580(11) 0.1206(9) 0.2810(7) 0.230(5) Uani 1 1 d D U . . .
C37 C 0.3217(6) 0.3356(6) 0.1445(3) 0.0882(19) Uani 0.683(4) 1 d D U P A 1
H37A H 0.3448 0.2821 0.1389 0.106 Uiso 0.683(4) 1 calc R U P A 1
H37B H 0.3834 0.3820 0.1592 0.106 Uiso 0.683(4) 1 calc R U P A 1
C38 C 0.2564(7) 0.3409(8) 0.0760(4) 0.102(2) Uani 0.683(4) 1 d D U P A 1
H38A H 0.1981 0.2916 0.0584 0.122 Uiso 0.683(4) 1 calc R U P A 1
H38B H 0.2288 0.3922 0.0813 0.122 Uiso 0.683(4) 1 calc R U P A 1
C39 C 0.3229(7) 0.3432(8) 0.0261(4) 0.112(3) Uani 0.683(4) 1 d D U P A 1
H39A H 0.3804 0.3931 0.0435 0.134 Uiso 0.683(4) 1 calc R U P A 1
H39B H 0.3519 0.2925 0.0219 0.134 Uiso 0.683(4) 1 calc R U P A 1
C40 C 0.2599(10) 0.3466(10) -0.0430(4) 0.142(4) Uani 0.683(4) 1 d D U P A 1
H40A H 0.2032 0.2971 -0.0605 0.213 Uiso 0.683(4) 1 calc R U P A 1
H40B H 0.3038 0.3474 -0.0729 0.213 Uiso 0.683(4) 1 calc R U P A 1
H40C H 0.2327 0.3976 -0.0391 0.213 Uiso 0.683(4) 1 calc R U P A 1
C41 C 0.3450(6) 0.3440(5) 0.2675(4) 0.0932(19) Uani 0.683(4) 1 d D U P A 1
H41A H 0.3988 0.3961 0.2785 0.112 Uiso 0.683(4) 1 calc R U P A 1
H41B H 0.3088 0.3486 0.3025 0.112 Uiso 0.683(4) 1 calc R U P A 1
C42 C 0.3976(11) 0.2693(8) 0.2700(5) 0.108(3) Uani 0.683(4) 1 d D U P A 1
H42A H 0.4465 0.2716 0.2427 0.130 Uiso 0.683(4) 1 calc R U P A 1
H42B H 0.3454 0.2161 0.2507 0.130 Uiso 0.683(4) 1 calc R U P A 1
C43 C 0.4557(7) 0.2694(7) 0.3418(5) 0.115(3) Uani 0.683(4) 1 d D U P A 1
H43A H 0.5043 0.3245 0.3618 0.138 Uiso 0.683(4) 1 calc R U P A 1
H43B H 0.4056 0.2641 0.3681 0.138 Uiso 0.683(4) 1 calc R U P A 1
C44 C 0.5134(14) 0.2016(10) 0.3473(7) 0.174(6) Uani 0.683(4) 1 d D U P A 1
H44A H 0.4669 0.1467 0.3259 0.261 Uiso 0.683(4) 1 calc R U P A 1
H44B H 0.5428 0.2039 0.3940 0.261 Uiso 0.683(4) 1 calc R U P A 1
H44C H 0.5683 0.2096 0.3255 0.261 Uiso 0.683(4) 1 calc R U P A 1
C45 C 0.2164(6) 0.4170(5) 0.2103(4) 0.0930(19) Uani 0.683(4) 1 d D U P A 1
H45A H 0.1885 0.4166 0.2489 0.112 Uiso 0.683(4) 1 calc R U P A 1
H45B H 0.1583 0.4101 0.1712 0.112 Uiso 0.683(4) 1 calc R U P A 1
C46 C 0.2881(9) 0.5042(6) 0.2219(7) 0.113(3) Uani 0.683(4) 1 d D U P A 1
H46A H 0.3370 0.5173 0.2663 0.136 Uiso 0.683(4) 1 calc R U P A 1
H46B H 0.3280 0.5011 0.1889 0.136 Uiso 0.683(4) 1 calc R U P A 1
C47 C 0.2326(12) 0.5765(6) 0.2174(9) 0.145(4) Uani 0.683(4) 1 d D U P A 1
H47A H 0.1806 0.5603 0.1741 0.173 Uiso 0.683(4) 1 calc R U P A 1
H47B H 0.1953 0.5799 0.2518 0.173 Uiso 0.683(4) 1 calc R U P A 1
C48 C 0.2917(10) 0.6616(5) 0.2242(6) 0.201(4) Uani 1 1 d D U . . .
C33A C 0.1675(12) 0.3083(10) 0.2182(11) 0.106(3) Uani 0.317(4) 1 d D U P A 2
H33C H 0.1113 0.3289 0.1928 0.127 Uiso 0.317(4) 1 calc R U P A 2
H33D H 0.1778 0.3339 0.2656 0.127 Uiso 0.317(4) 1 calc R U P A 2
C34A C 0.1326(19) 0.2110(10) 0.2065(12) 0.144(5) Uani 0.317(4) 1 d D U P A 2
H34C H 0.1061 0.1858 0.1584 0.173 Uiso 0.317(4) 1 calc R U P A 2
H34D H 0.1923 0.1881 0.2236 0.173 Uiso 0.317(4) 1 calc R U P A 2
C35A C 0.0487(15) 0.1858(15) 0.2409(15) 0.165(5) Uani 0.317(4) 1 d D U P A 2
H35C H 0.0437 0.2376 0.2705 0.198 Uiso 0.317(4) 1 calc R U P A 2
H35D H -0.0171 0.1657 0.2062 0.198 Uiso 0.317(4) 1 calc R U P A 2
C37A C 0.2268(12) 0.3257(13) 0.1205(6) 0.098(3) Uani 0.317(4) 1 d D U P A 2
H37C H 0.1995 0.2647 0.1013 0.118 Uiso 0.317(4) 1 calc R U P A 2
H37D H 0.1693 0.3537 0.1102 0.118 Uiso 0.317(4) 1 calc R U P A 2
C38A C 0.3061(15) 0.3568(19) 0.0853(6) 0.106(4) Uani 0.317(4) 1 d D U P A 2
H38C H 0.3641 0.3291 0.0946 0.127 Uiso 0.317(4) 1 calc R U P A 2
H38D H 0.3326 0.4182 0.1026 0.127 Uiso 0.317(4) 1 calc R U P A 2
C39A C 0.2581(16) 0.3371(19) 0.0095(6) 0.123(5) Uani 0.317(4) 1 d D U P A 2
H39C H 0.2222 0.2772 -0.0058 0.148 Uiso 0.317(4) 1 calc R U P A 2
H39D H 0.2062 0.3709 0.0007 0.148 Uiso 0.317(4) 1 calc R U P A 2
C40A C 0.331(2) 0.354(3) -0.0308(9) 0.152(9) Uani 0.317(4) 1 d D U P A 2
H40D H 0.3936 0.3361 -0.0129 0.228 Uiso 0.317(4) 1 calc R U P A 2
H40E H 0.3468 0.4138 -0.0294 0.228 Uiso 0.317(4) 1 calc R U P A 2
H40F H 0.2996 0.3217 -0.0767 0.228 Uiso 0.317(4) 1 calc R U P A 2
C41A C 0.3541(11) 0.2953(11) 0.2159(6) 0.085(3) Uani 0.317(4) 1 d D U P A 2
H41C H 0.3332 0.2373 0.1879 0.102 Uiso 0.317(4) 1 calc R U P A 2
H41D H 0.4140 0.3249 0.2046 0.102 Uiso 0.317(4) 1 calc R U P A 2
C42A C 0.386(2) 0.2915(19) 0.2894(7) 0.097(4) Uani 0.317(4) 1 d D U P A 2
H42C H 0.4093 0.3496 0.3174 0.116 Uiso 0.317(4) 1 calc R U P A 2
H42D H 0.3261 0.2635 0.3011 0.116 Uiso 0.317(4) 1 calc R U P A 2
C43A C 0.4725(14) 0.2442(14) 0.3049(8) 0.104(4) Uani 0.317(4) 1 d D U P A 2
H43C H 0.5323 0.2715 0.2923 0.125 Uiso 0.317(4) 1 calc R U P A 2
H43D H 0.4490 0.1857 0.2777 0.125 Uiso 0.317(4) 1 calc R U P A 2
C44A C 0.506(2) 0.242(2) 0.3785(9) 0.141(8) Uani 0.317(4) 1 d D U P A 2
H44D H 0.5353 0.2999 0.4054 0.212 Uiso 0.317(4) 1 calc R U P A 2
H44E H 0.5571 0.2084 0.3849 0.212 Uiso 0.317(4) 1 calc R U P A 2
H44F H 0.4464 0.2180 0.3920 0.212 Uiso 0.317(4) 1 calc R U P A 2
C45A C 0.3060(15) 0.4389(8) 0.2261(10) 0.101(4) Uani 0.317(4) 1 d D U P A 2
H45C H 0.3166 0.4518 0.2746 0.121 Uiso 0.317(4) 1 calc R U P A 2
H45D H 0.3740 0.4537 0.2181 0.121 Uiso 0.317(4) 1 calc R U P A 2
C46A C 0.241(2) 0.4984(9) 0.1982(16) 0.184(19) Uani 0.317(4) 1 d D . P A 2
H46C H 0.2540 0.5054 0.1557 0.221 Uiso 0.317(4) 1 calc R U P A 2
H46D H 0.1677 0.4723 0.1894 0.221 Uiso 0.317(4) 1 calc R U P A 2
C47A C 0.265(3) 0.5852(10) 0.2457(13) 0.23(3) Uani 0.317(4) 1 d D . P A 2
H47C H 0.2047 0.5890 0.2628 0.280 Uiso 0.317(4) 1 calc R U P A 2
H47D H 0.3220 0.5860 0.2838 0.280 Uiso 0.317(4) 1 calc R U P A 2
O1W O 0.5533(8) 0.7938(6) 0.2938(5) 0.128(3) Uiso 0.5 1 d . . P . .
O2W O 0.4299(12) -0.0265(10) 0.6722(8) 0.117(4) Uiso 0.3 1 d . . P . .
O2WA O 0.4777(17) 0.0372(15) 0.6530(11) 0.116(6) Uiso 0.2 1 d . . P . .
O3W O 0.5390(17) 0.0043(14) 0.5314(10) 0.145(7) Uiso 0.25 1 d . . P . .
O3WA O 0.624(2) -0.0221(18) 0.5631(14) 0.181(9) Uiso 0.25 1 d . . P . .
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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 '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
O1A Pd1 O1A 180.0 2_666 .
O1A Pd1 N1A 98.46(12) 2_666 .
O1A Pd1 N1A 81.54(12) . .
O1A Pd1 N1A 81.54(12) 2_666 2_666
O1A Pd1 N1A 98.46(12) . 2_666
N1A Pd1 N1A 180.0 . 2_666
O1A Pd1 Pd3 102.81(9) 2_666 .
O1A Pd1 Pd3 77.19(9) . .
N1A Pd1 Pd3 50.96(10) . .
N1A Pd1 Pd3 129.04(11) 2_666 .
O1A Pd1 Pd2 35.83(9) 2_666 .
O1A Pd1 Pd2 144.17(9) . .
N1A Pd1 Pd2 89.27(10) . .
N1A Pd1 Pd2 90.73(10) 2_666 .
Pd3 Pd1 Pd2 122.381(10) . .
O2A C1A O1A 124.1(4) . .
O2A C1A C2A 120.4(4) . .
O1A C1A C2A 115.4(4) . .
O3A C2A N1A 127.4(4) . .
O3A C2A C1A 119.8(4) . .
N1A C2A C1A 112.8(3) . .
C1A O1A Pd1 115.1(3) . .
C2A N1A C3A 120.3(3) . .
C2A N1A Pd1 113.9(3) . .
C3A N1A Pd1 125.7(3) . .
C8A C3A C4A 119.0(5) . .
C8A C3A N1A 118.9(4) . .
C4A C3A N1A 122.1(4) . .
C3A C4A C5A 119.3(5) . .
C3A C4A H4A 120.4 . .
C5A C4A H4A 120.4 . .
C6A C5A C4A 120.5(5) . .
C6A C5A H5A 119.8 . .
C4A C5A H5A 119.8 . .
C5A C6A C7A 121.7(5) . .
C5A C6A Br1A 119.1(5) . .
C7A C6A Br1A 119.2(5) . .
C6A C7A C8A 117.9(5) . .
C6A C7A H7A 121.0 . .
C8A C7A H7A 121.0 . .
C3A C8A C7A 121.6(5) . .
C3A C8A H8A 119.2 . .
C7A C8A H8A 119.2 . .
O1B Pd2 O1B 180.0(3) 2 .
O1B Pd2 N1B 98.28(14) 2 .
O1B Pd2 N1B 81.72(14) . .
O1B Pd2 N1B 81.72(14) 2 2
O1B Pd2 N1B 98.28(14) . 2
N1B Pd2 N1B 180.0(3) . 2
O1B Pd2 Pd1 37.82(10) 2 .
O1B Pd2 Pd1 142.18(10) . .
N1B Pd2 Pd1 85.98(10) . .
N1B Pd2 Pd1 94.02(10) 2 .
O1B Pd2 Pd3 13.32(9) 2 .
O1B Pd2 Pd3 166.68(9) . .
N1B Pd2 Pd3 89.95(11) . .
N1B Pd2 Pd3 90.05(11) 2 .
Pd1 Pd2 Pd3 25.722(4) . .
O2B C1B O1B 124.5(5) . .
O2B C1B C2B 118.8(4) . .
O1B C1B C2B 116.6(4) . .
O3B C2B N1B 126.6(5) . .
O3B C2B C1B 121.0(4) . .
N1B C2B C1B 112.2(4) . .
C1B O1B Pd2 114.5(3) . .
C2B N1B C3B 120.6(4) . .
C2B N1B Pd2 113.3(3) . .
C3B N1B Pd2 126.0(3) . .
C4B C3B C8B 116.5(5) . .
C4B C3B N1B 124.7(5) . .
C8B C3B N1B 118.7(4) . .
C3B C4B C5B 121.7(5) . .
C3B C4B H4B 119.2 . .
C5B C4B H4B 119.2 . .
C6B C5B C4B 119.2(6) . .
C6B C5B H5B 120.4 . .
C4B C5B H5B 120.4 . .
C5B C6B C7B 121.7(6) . .
C5B C6B Br1B 118.5(5) . .
C7B C6B Br1B 119.8(6) . .
C6B C7B C8B 118.8(6) . .
C6B C7B H7B 120.6 . .
C8B C7B H7B 120.6 . .
C7B C8B C3B 122.0(5) . .
C7B C8B H8B 119.0 . .
C3B C8B H8B 119.0 . .
O1C Pd3 O1C 180.0(3) 2_776 .
O1C Pd3 N1C 98.63(19) 2_776 .
O1C Pd3 N1C 81.4(2) . .
O1C Pd3 N1C 81.4(2) 2_776 2_776
O1C Pd3 N1C 98.63(19) . 2_776
N1C Pd3 N1C 180.0 . 2_776
O1C Pd3 Pd1 96.52(13) 2_776 .
O1C Pd3 Pd1 83.48(13) . .
N1C Pd3 Pd1 66.68(13) . .
N1C Pd3 Pd1 113.32(13) 2_776 .
O1C Pd3 Pd2 80.38(13) 2_776 1_665
O1C Pd3 Pd2 99.62(13) . 1_665
N1C Pd3 Pd2 44.37(14) . 1_665
N1C Pd3 Pd2 135.63(14) 2_776 1_665
Pd1 Pd3 Pd2 108.697(9) . 1_665
O1C Pd3 Pd2 91.35(12) 2_776 .
O1C Pd3 Pd2 88.65(12) . .
N1C Pd3 Pd2 36.32(13) . .
N1C Pd3 Pd2 143.68(12) 2_776 .
Pd1 Pd3 Pd2 31.897(7) . .
Pd2 Pd3 Pd2 76.800(10) 1_665 .
O2C C1C O1C 123.7(7) . .
O2C C1C C2C 120.1(7) . .
O1C C1C C2C 116.2(7) . .
O3C C2C N1C 127.1(6) . .
O3C C2C C1C 119.4(7) . .
N1C C2C C1C 113.5(6) . .
C1C O1C Pd3 115.0(4) . .
C2C N1C C3C 119.7(5) . .
C2C N1C Pd3 113.9(4) . .
C3C N1C Pd3 126.4(4) . .
C4C C3C C8C 118.1(7) . .
C4C C3C N1C 122.8(7) . .
C8C C3C N1C 119.1(6) . .
C3C C4C C5C 120.3(8) . .
C3C C4C H4C 119.9 . .
C5C C4C H4C 119.9 . .
C6C C5C C4C 121.9(8) . .
C6C C5C H5C 119.1 . .
C4C C5C H5C 119.1 . .
C5C C6C C7C 120.6(8) . .
C5C C6C Br1C 120.8(8) . .
C7C C6C Br1C 118.5(9) . .
C8C C7C C6C 117.8(9) . .
C8C C7C H7C 121.1 . .
C6C C7C H7C 121.1 . .
C3C C8C C7C 121.4(7) . .
C3C C8C H8C 119.3 . .
C7C C8C H8C 119.3 . .
C13 N1 C9 111.9(4) . .
C13 N1 C5 105.6(4) . .
C9 N1 C5 111.2(4) . .
C13 N1 C1 111.8(4) . .
C9 N1 C1 105.5(4) . .
C5 N1 C1 110.8(4) . .
C2 C1 N1 116.3(4) . .
C2 C1 H1A 108.2 . .
N1 C1 H1A 108.2 . .
C2 C1 H1B 108.2 . .
N1 C1 H1B 108.2 . .
H1A C1 H1B 107.4 . .
C3 C2 C1 112.8(5) . .
C3 C2 H2A 109.0 . .
C1 C2 H2A 109.0 . .
C3 C2 H2B 109.0 . .
C1 C2 H2B 109.0 . .
H2A C2 H2B 107.8 . .
C2 C3 C4 114.6(7) . .
C2 C3 H3A 108.6 . .
C4 C3 H3A 108.6 . .
C2 C3 H3B 108.6 . .
C4 C3 H3B 108.6 . .
H3A C3 H3B 107.6 . .
C3 C4 H4D 109.5 . .
C3 C4 H4E 109.5 . .
H4D C4 H4E 109.5 . .
C3 C4 H4F 109.5 . .
H4D C4 H4F 109.5 . .
H4E C4 H4F 109.5 . .
C6 C5 N1 114.4(4) . .
C6 C5 H5D 108.7 . .
N1 C5 H5D 108.7 . .
C6 C5 H5E 108.7 . .
N1 C5 H5E 108.7 . .
H5D C5 H5E 107.6 . .
C5 C6 C7 108.9(6) . .
C5 C6 H6A 109.9 . .
C7 C6 H6A 109.9 . .
C5 C6 H6B 109.9 . .
C7 C6 H6B 109.9 . .
H6A C6 H6B 108.3 . .
C6 C7 C8 107.3(7) . .
C6 C7 H7D 110.2 . .
C8 C7 H7D 110.2 . .
C6 C7 H7E 110.2 . .
C8 C7 H7E 110.2 . .
H7D C7 H7E 108.5 . .
C7 C8 H8D 109.5 . .
C7 C8 H8E 109.5 . .
H8D C8 H8E 109.5 . .
C7 C8 H8F 109.5 . .
H8D C8 H8F 109.5 . .
H8E C8 H8F 109.5 . .
C10 C9 N1 115.8(4) . .
C10 C9 H9A 108.3 . .
N1 C9 H9A 108.3 . .
C10 C9 H9B 108.3 . .
N1 C9 H9B 108.3 . .
H9A C9 H9B 107.4 . .
C11 C10 C9 111.1(5) . .
C11 C10 H10A 109.4 . .
C9 C10 H10A 109.4 . .
C11 C10 H10B 109.4 . .
C9 C10 H10B 109.4 . .
H10A C10 H10B 108.0 . .
C12 C11 C10 114.4(6) . .
C12 C11 H11A 108.7 . .
C10 C11 H11A 108.7 . .
C12 C11 H11B 108.7 . .
C10 C11 H11B 108.7 . .
H11A C11 H11B 107.6 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N1 C13 C14 117.5(4) . .
N1 C13 H13A 107.9 . .
C14 C13 H13A 107.9 . .
N1 C13 H13B 107.9 . .
C14 C13 H13B 107.9 . .
H13A C13 H13B 107.2 . .
C15 C14 C13 110.2(5) . .
C15 C14 H14A 109.6 . .
C13 C14 H14A 109.6 . .
C15 C14 H14B 109.6 . .
C13 C14 H14B 109.6 . .
H14A C14 H14B 108.1 . .
C16 C15 C14 116.4(6) . .
C16 C15 H15A 108.2 . .
C14 C15 H15A 108.2 . .
C16 C15 H15B 108.2 . .
C14 C15 H15B 108.2 . .
H15A C15 H15B 107.3 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C17 N2 C25 105.9(4) . .
C17 N2 C29 112.1(5) . .
C25 N2 C29 111.2(5) . .
C17 N2 C21 110.5(5) . .
C25 N2 C21 111.7(4) . .
C29 N2 C21 105.6(4) . .
N2 C17 C18 116.2(6) . .
N2 C17 H17A 108.2 . .
C18 C17 H17A 108.2 . .
N2 C17 H17B 108.2 . .
C18 C17 H17B 108.2 . .
H17A C17 H17B 107.4 . .
C17 C18 C19 107.9(7) . .
C17 C18 H18A 110.1 . .
C19 C18 H18A 110.1 . .
C17 C18 H18B 110.1 . .
C19 C18 H18B 110.1 . .
H18A C18 H18B 108.4 . .
C20 C19 C18 109.8(9) . .
C20 C19 H19A 109.7 . .
C18 C19 H19A 109.7 . .
C20 C19 H19B 109.7 . .
C18 C19 H19B 109.7 . .
H19A C19 H19B 108.2 . .
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 . .
N2 C21 C22 115.2(4) . .
N2 C21 H21A 108.5 . .
C22 C21 H21A 108.5 . .
N2 C21 H21B 108.5 . .
C22 C21 H21B 108.5 . .
H21A C21 H21B 107.5 . .
C23 C22 C21 111.2(5) . .
C23 C22 H22A 109.4 . .
C21 C22 H22A 109.4 . .
C23 C22 H22B 109.4 . .
C21 C22 H22B 109.4 . .
H22A C22 H22B 108.0 . .
C24 C23 C22 115.5(5) . .
C24 C23 H23A 108.4 . .
C22 C23 H23A 108.4 . .
C24 C23 H23B 108.4 . .
C22 C23 H23B 108.4 . .
H23A C23 H23B 107.5 . .
C23 C24 H24A 109.5 . .
C23 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C23 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 N2 115.5(5) . .
C26 C25 H25A 108.4 . .
N2 C25 H25A 108.4 . .
C26 C25 H25B 108.4 . .
N2 C25 H25B 108.4 . .
H25A C25 H25B 107.5 . .
C25 C26 C27 109.4(5) . .
C25 C26 H26A 109.8 . .
C27 C26 H26A 109.8 . .
C25 C26 H26B 109.8 . .
C27 C26 H26B 109.8 . .
H26A C26 H26B 108.2 . .
C28 C27 C26 113.2(6) . .
C28 C27 H27A 108.9 . .
C26 C27 H27A 108.9 . .
C28 C27 H27B 108.9 . .
C26 C27 H27B 108.9 . .
H27A C27 H27B 107.7 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
N2 C29 C30 114.1(5) . .
N2 C29 H29A 108.7 . .
C30 C29 H29A 108.7 . .
N2 C29 H29B 108.7 . .
C30 C29 H29B 108.7 . .
H29A C29 H29B 107.6 . .
C29 C30 C31 108.1(7) . .
C29 C30 H30A 110.1 . .
C31 C30 H30A 110.1 . .
C29 C30 H30B 110.1 . .
C31 C30 H30B 110.1 . .
H30A C30 H30B 108.4 . .
C32 C31 C30 118.8(12) . .
C32 C31 H31A 107.6 . .
C30 C31 H31A 107.6 . .
C32 C31 H31B 107.6 . .
C30 C31 H31B 107.6 . .
H31A C31 H31B 107.0 . .
C31 C32 H32A 109.5 . .
C31 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C31 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C45 N3 C37 115.3(5) . .
C33A N3 C41A 117.0(10) . .
C33A N3 C45A 112.0(10) . .
C41A N3 C45A 110.1(10) . .
C45 N3 C41 107.4(5) . .
C37 N3 C41 108.6(5) . .
C45 N3 C33 108.1(5) . .
C37 N3 C33 109.0(5) . .
C41 N3 C33 108.2(5) . .
C33A N3 C37A 103.2(10) . .
C41A N3 C37A 108.6(9) . .
C45A N3 C37A 105.0(11) . .
C34 C33 N3 117.0(7) . .
C34 C33 H33A 108.1 . .
N3 C33 H33A 108.1 . .
C34 C33 H33B 108.1 . .
N3 C33 H33B 108.1 . .
H33A C33 H33B 107.3 . .
C33 C34 C35 112.0(8) . .
C33 C34 H34A 109.2 . .
C35 C34 H34A 109.2 . .
C33 C34 H34B 109.2 . .
C35 C34 H34B 109.2 . .
H34A C34 H34B 107.9 . .
C36 C35 C34 111.6(10) . .
C36 C35 H35A 109.3 . .
C34 C35 H35A 109.3 . .
C36 C35 H35B 109.3 . .
C34 C35 H35B 109.3 . .
H35A C35 H35B 108.0 . .
N3 C37 C38 114.6(6) . .
N3 C37 H37A 108.6 . .
C38 C37 H37A 108.6 . .
N3 C37 H37B 108.6 . .
C38 C37 H37B 108.6 . .
H37A C37 H37B 107.6 . .
C39 C38 C37 110.4(7) . .
C39 C38 H38A 109.6 . .
C37 C38 H38A 109.6 . .
C39 C38 H38B 109.6 . .
C37 C38 H38B 109.6 . .
H38A C38 H38B 108.1 . .
C40 C39 C38 111.8(8) . .
C40 C39 H39A 109.3 . .
C38 C39 H39A 109.3 . .
C40 C39 H39B 109.3 . .
C38 C39 H39B 109.3 . .
H39A C39 H39B 107.9 . .
C39 C40 H40A 109.5 . .
C39 C40 H40B 109.5 . .
H40A C40 H40B 109.5 . .
C39 C40 H40C 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C42 C41 N3 116.8(6) . .
C42 C41 H41A 108.1 . .
N3 C41 H41A 108.1 . .
C42 C41 H41B 108.1 . .
N3 C41 H41B 108.1 . .
H41A C41 H41B 107.3 . .
C41 C42 C43 112.6(8) . .
C41 C42 H42A 109.1 . .
C43 C42 H42A 109.1 . .
C41 C42 H42B 109.1 . .
C43 C42 H42B 109.1 . .
H42A C42 H42B 107.8 . .
C44 C43 C42 115.2(9) . .
C44 C43 H43A 108.5 . .
C42 C43 H43A 108.5 . .
C44 C43 H43B 108.5 . .
C42 C43 H43B 108.5 . .
H43A C43 H43B 107.5 . .
C43 C44 H44A 109.5 . .
C43 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C43 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
N3 C45 C46 115.9(7) . .
N3 C45 H45A 108.3 . .
C46 C45 H45A 108.3 . .
N3 C45 H45B 108.3 . .
C46 C45 H45B 108.3 . .
H45A C45 H45B 107.4 . .
C47 C46 C45 114.3(9) . .
C47 C46 H46A 108.7 . .
C45 C46 H46A 108.7 . .
C47 C46 H46B 108.7 . .
C45 C46 H46B 108.7 . .
H46A C46 H46B 107.6 . .
C48 C47 C46 119.5(11) . .
C48 C47 H47A 107.4 . .
C46 C47 H47A 107.4 . .
C48 C47 H47B 107.4 . .
C46 C47 H47B 107.4 . .
H47A C47 H47B 107.0 . .
N3 C33A C34A 116.2(11) . .
N3 C33A H33C 108.2 . .
C34A C33A H33C 108.2 . .
N3 C33A H33D 108.2 . .
C34A C33A H33D 108.2 . .
H33C C33A H33D 107.4 . .
C35A C34A C33A 112.3(13) . .
C35A C34A H34C 109.1 . .
C33A C34A H34C 109.1 . .
C35A C34A H34D 109.1 . .
C33A C34A H34D 109.1 . .
H34C C34A H34D 107.9 . .
C36 C35A C34A 119.7(16) . .
C36 C35A H35C 107.4 . .
C34A C35A H35C 107.4 . .
C36 C35A H35D 107.4 . .
C34A C35A H35D 107.4 . .
H35C C35A H35D 106.9 . .
C38A C37A N3 116.8(10) . .
C38A C37A H37C 108.1 . .
N3 C37A H37C 108.1 . .
C38A C37A H37D 108.1 . .
N3 C37A H37D 108.1 . .
H37C C37A H37D 107.3 . .
C37A C38A C39A 111.0(12) . .
C37A C38A H38C 109.4 . .
C39A C38A H38C 109.4 . .
C37A C38A H38D 109.4 . .
C39A C38A H38D 109.4 . .
H38C C38A H38D 108.0 . .
C40A C39A C38A 115.8(13) . .
C40A C39A H39C 108.3 . .
C38A C39A H39C 108.3 . .
C40A C39A H39D 108.3 . .
C38A C39A H39D 108.3 . .
H39C C39A H39D 107.4 . .
C39A C40A H40D 109.5 . .
C39A C40A H40E 109.5 . .
H40D C40A H40E 109.5 . .
C39A C40A H40F 109.5 . .
H40D C40A H40F 109.5 . .
H40E C40A H40F 109.5 . .
C42A C41A N3 113.9(10) . .
C42A C41A H41C 108.8 . .
N3 C41A H41C 108.8 . .
C42A C41A H41D 108.8 . .
N3 C41A H41D 108.8 . .
H41C C41A H41D 107.7 . .
C43A C42A C41A 113.4(12) . .
C43A C42A H42C 108.9 . .
C41A C42A H42C 108.9 . .
C43A C42A H42D 108.9 . .
C41A C42A H42D 108.9 . .
H42C C42A H42D 107.7 . .
C42A C43A C44A 113.0(12) . .
C42A C43A H43C 109.0 . .
C44A C43A H43C 109.0 . .
C42A C43A H43D 109.0 . .
C44A C43A H43D 109.0 . .
H43C C43A H43D 107.8 . .
C43A C44A H44D 109.5 . .
C43A C44A H44E 109.5 . .
H44D C44A H44E 109.5 . .
C43A C44A H44F 109.5 . .
H44D C44A H44F 109.5 . .
H44E C44A H44F 109.5 . .
C46A C45A N3 119.3(12) . .
C46A C45A H45C 107.5 . .
N3 C45A H45C 107.5 . .
C46A C45A H45D 107.5 . .
N3 C45A H45D 107.5 . .
H45C C45A H45D 107.0 . .
C47A C46A C45A 112.7(14) . .
C47A C46A H46C 109.1 . .
C45A C46A H46C 109.1 . .
C47A C46A H46D 109.1 . .
C45A C46A H46D 109.1 . .
H46C C46A H46D 107.8 . .
C48 C47A C46A 121.3(17) . .
C48 C47A H47C 107.0 . .
C46A C47A H47C 107.0 . .
C48 C47A H47D 107.0 . .
C46A C47A H47D 107.0 . .
H47C C47A H47D 106.7 . .
O3WA O3W O3W 147(3) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 O1A 2.013(3) 2_666
Pd1 O1A 2.013(3) .
Pd1 N1A 2.036(3) .
Pd1 N1A 2.036(3) 2_666
Pd1 Pd3 9.6579(14) .
Pd1 Pd2 11.7585(19) .
C1A O2A 1.213(5) .
C1A O1A 1.298(5) .
C1A C2A 1.563(7) .
C2A O3A 1.252(5) .
C2A N1A 1.337(5) .
N1A C3A 1.418(5) .
C3A C8A 1.380(7) .
C3A C4A 1.390(6) .
C4A C5A 1.407(7) .
C4A H4A 0.9300 .
C5A C6A 1.344(9) .
C5A H5A 0.9300 .
C6A C7A 1.386(9) .
C6A Br1A 1.918(5) .
C7A C8A 1.396(8) .
C7A H7A 0.9300 .
C8A H8A 0.9300 .
Pd2 O1B 2.019(3) 2
Pd2 O1B 2.019(3) .
Pd2 N1B 2.038(3) .
Pd2 N1B 2.038(3) 2
Pd2 Pd3 18.793(3) .
C1B O2B 1.230(6) .
C1B O1B 1.287(5) .
C1B C2B 1.555(7) .
C2B O3B 1.243(5) .
C2B N1B 1.353(6) .
N1B C3B 1.407(6) .
C3B C4B 1.384(6) .
C3B C8B 1.399(7) .
C4B C5B 1.397(8) .
C4B H4B 0.9300 .
C5B C6B 1.354(9) .
C5B H5B 0.9300 .
C6B C7B 1.363(9) .
C6B Br1B 1.930(6) .
C7B C8B 1.388(8) .
C7B H7B 0.9300 .
C8B H8B 0.9300 .
Pd3 O1C 2.001(5) 2_776
Pd3 O1C 2.001(5) .
Pd3 N1C 2.048(4) .
Pd3 N1C 2.048(4) 2_776
Pd3 Pd2 10.4833(17) 1_665
C1C O2C 1.215(8) .
C1C O1C 1.303(8) .
C1C C2C 1.533(9) .
C2C O3C 1.238(7) .
C2C N1C 1.332(8) .
N1C C3C 1.428(7) .
C3C C4C 1.368(8) .
C3C C8C 1.394(9) .
C4C C5C 1.402(10) .
C4C H4C 0.9300 .
C5C C6C 1.312(12) .
C5C H5C 0.9300 .
C6C C7C 1.408(12) .
C6C Br1C 1.890(8) .
C7C C8C 1.402(10) .
C7C H7C 0.9300 .
C8C H8C 0.9300 .
N1 C13 1.513(6) .
N1 C9 1.524(6) .
N1 C5 1.537(6) .
N1 C1 1.538(6) .
C1 C2 1.530(8) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.493(9) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.498(11) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4D 0.9600 .
C4 H4E 0.9600 .
C4 H4F 0.9600 .
C5 C6 1.495(8) .
C5 H5D 0.9700 .
C5 H5E 0.9700 .
C6 C7 1.551(9) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.561(11) .
C7 H7D 0.9700 .
C7 H7E 0.9700 .
C8 H8D 0.9600 .
C8 H8E 0.9600 .
C8 H8F 0.9600 .
C9 C10 1.515(7) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.512(8) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 C12 1.497(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 C14 1.515(7) .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C15 1.503(8) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.482(9) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
N2 C17 1.515(8) .
N2 C25 1.524(8) .
N2 C29 1.524(7) .
N2 C21 1.529(7) .
C17 C18 1.530(11) .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
C18 C19 1.562(12) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.456(14) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 C22 1.546(8) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.492(8) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 C24 1.478(9) .
C23 H23A 0.9700 .
C23 H23B 0.9700 .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 C26 1.491(9) .
C25 H25A 0.9700 .
C25 H25B 0.9700 .
C26 C27 1.555(9) .
C26 H26A 0.9700 .
C26 H26B 0.9700 .
C27 C28 1.535(11) .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C29 C30 1.545(10) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C30 C31 1.589(12) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C31 C32 1.239(15) .
C31 H31A 0.9700 .
C31 H31B 0.9700 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
N3 C33A 1.507(11) .
N3 C45 1.514(8) .
N3 C37 1.514(7) .
N3 C41A 1.517(11) .
N3 C45A 1.551(12) .
N3 C41 1.564(7) .
N3 C33 1.567(7) .
N3 C37A 1.571(11) .
C33 C34 1.484(10) .
C33 H33A 0.9700 .
C33 H33B 0.9700 .
C34 C35 1.535(11) .
C34 H34A 0.9700 .
C34 H34B 0.9700 .
C35 C36 1.485(12) .
C35 H35A 0.9700 .
C35 H35B 0.9700 .
C36 C35A 1.479(15) .
C37 C38 1.530(9) .
C37 H37A 0.9700 .
C37 H37B 0.9700 .
C38 C39 1.528(10) .
C38 H38A 0.9700 .
C38 H38B 0.9700 .
C39 C40 1.519(10) .
C39 H39A 0.9700 .
C39 H39B 0.9700 .
C40 H40A 0.9600 .
C40 H40B 0.9600 .
C40 H40C 0.9600 .
C41 C42 1.515(10) .
C41 H41A 0.9700 .
C41 H41B 0.9700 .
C42 C43 1.529(10) .
C42 H42A 0.9700 .
C42 H42B 0.9700 .
C43 C44 1.464(11) .
C43 H43A 0.9700 .
C43 H43B 0.9700 .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .
C45 C46 1.519(10) .
C45 H45A 0.9700 .
C45 H45B 0.9700 .
C46 C47 1.507(12) .
C46 H46A 0.9700 .
C46 H46B 0.9700 .
C47 C48 1.441(11) .
C47 H47A 0.9700 .
C47 H47B 0.9700 .
C48 C47A 1.420(15) .
C33A C34A 1.529(14) .
C33A H33C 0.9700 .
C33A H33D 0.9700 .
C34A C35A 1.518(14) .
C34A H34C 0.9700 .
C34A H34D 0.9700 .
C35A H35C 0.9700 .
C35A H35D 0.9700 .
C37A C38A 1.507(13) .
C37A H37C 0.9700 .
C37A H37D 0.9700 .
C38A C39A 1.521(13) .
C38A H38C 0.9700 .
C38A H38D 0.9700 .
C39A C40A 1.458(14) .
C39A H39C 0.9700 .
C39A H39D 0.9700 .
C40A H40D 0.9600 .
C40A H40E 0.9600 .
C40A H40F 0.9600 .
C41A C42A 1.517(13) .
C41A H41C 0.9700 .
C41A H41D 0.9700 .
C42A C43A 1.512(13) .
C42A H42C 0.9700 .
C42A H42D 0.9700 .
C43A C44A 1.512(14) .
C43A H43C 0.9700 .
C43A H43D 0.9700 .
C44A H44D 0.9600 .
C44A H44E 0.9600 .
C44A H44F 0.9600 .
C45A C46A 1.524(15) .
C45A H45C 0.9700 .
C45A H45D 0.9700 .
C46A C47A 1.502(15) .
C46A H46C 0.9700 .
C46A H46D 0.9700 .
C47A H47C 0.9700 .
C47A H47D 0.9700 .
O2W O2WA 1.31(2) .
O3W O3WA 1.37(3) .
O3W O3W 1.45(4) 2_656
