# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1402358'
_audit_update_record             
;
2015-05-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_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

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.524(2)
_cell_length_b                   16.287(3)
_cell_length_c                   20.967(3)
_cell_angle_alpha                100.901(8)
_cell_angle_beta                 103.304(8)
_cell_angle_gamma                99.809(8)
_cell_volume                     4301.1(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9575
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      22.35

_exptl_crystal_description       prism
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             1698
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.762
_shelx_estimated_absorpt_T_min   0.719
_shelx_estimated_absorpt_T_max   0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88674
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.457
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18125
_reflns_number_gt                9794
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1255P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18125
_refine_ls_number_parameters     992
_refine_ls_number_restraints     956
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0599
_refine_ls_wR_factor_ref         0.2121
_refine_ls_wR_factor_gt          0.1750
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 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 ?

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
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 ?

_refine_diff_density_max         0.859
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.084

_shelxl_version_number           2013-4



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1402359'
_audit_update_record             
;
2015-05-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H14 N2 O8 Pd, 2(C16 H36 N)'
_chemical_formula_sum            'C50 H86 N4 O8 Pd'
_chemical_formula_weight         977.62

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.7928(5)
_cell_length_b                   16.3297(8)
_cell_length_c                   16.0978(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.392(2)
_cell_angle_gamma                90
_cell_volume                     2562.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9776
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.28

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_F_000             1048
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.416
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60847
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.780
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5228
_reflns_number_gt                4390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²+1.5167P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5228
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0956
_refine_ls_wR_factor_gt          0.0830
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.210
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 1.0000 0.0000 1.0000 0.01390(9) Uani 1 2 d S . P . .
O1 O 1.18526(16) 0.05234(10) 1.00168(10) 0.0195(4) Uani 1 1 d . . . . .
O2 O 1.31865(17) 0.12147(11) 0.92130(11) 0.0230(4) Uani 1 1 d . . . . .
O3 O 1.10337(17) 0.12997(11) 0.79844(11) 0.0241(4) Uani 1 1 d . . . . .
C1 C 1.2089(2) 0.08952(14) 0.93290(15) 0.0171(5) Uani 1 1 d . . . . .
C2 C 1.0864(2) 0.09476(14) 0.86491(15) 0.0171(5) Uani 1 1 d . . . . .
C3 C 0.8462(2) 0.06612(14) 0.83566(14) 0.0161(5) Uani 1 1 d . . . . .
C4 C 0.8416(2) 0.06475(15) 0.74800(15) 0.0190(5) Uani 1 1 d . . . . .
H4A H 0.9248 0.0643 0.7221 0.023 Uiso 1 1 calc R U . . .
C5 C 0.7172(2) 0.06411(15) 0.69879(15) 0.0204(5) Uani 1 1 d . . . . .
H5A H 0.7162 0.0626 0.6397 0.024 Uiso 1 1 calc R U . . .
C6 C 0.5940(2) 0.06562(15) 0.73538(15) 0.0192(5) Uani 1 1 d . . . . .
C7 C 0.5955(2) 0.06977(15) 0.82190(15) 0.0190(5) Uani 1 1 d . . . . .
H7A H 0.5120 0.0727 0.8474 0.023 Uiso 1 1 calc R U . . .
O1M O 0.47519(17) 0.06237(12) 0.68123(11) 0.0250(4) Uani 1 1 d . . . . .
C1M C 0.3534(3) 0.03638(17) 0.71700(17) 0.0248(5) Uani 1 1 d . . . . .
H1MA H 0.2759 0.0362 0.6738 0.037 Uiso 1 1 calc R U . . .
H1MB H 0.3341 0.0741 0.7618 0.037 Uiso 1 1 calc R U . . .
H1MC H 0.3671 -0.0190 0.7398 0.037 Uiso 1 1 calc R U . . .
N1 N 0.97077(19) 0.06164(12) 0.88925(12) 0.0157(4) Uani 1 1 d . . . . .
C8 C 0.7212(2) 0.06961(14) 0.87067(15) 0.0176(5) Uani 1 1 d . . . . .
H8A H 0.7217 0.0720 0.9297 0.021 Uiso 1 1 calc R U . . .
C9 C 0.7490(2) -0.27821(15) 0.85912(14) 0.0177(5) Uani 1 1 d . . . . .
H9A H 0.8142 -0.3083 0.8269 0.021 Uiso 1 1 calc R U . . .
H9B H 0.6683 -0.3139 0.8633 0.021 Uiso 1 1 calc R U . . .
C10 C 0.8178(3) -0.26309(16) 0.94729(15) 0.0226(5) Uani 1 1 d . . . . .
H10A H 0.7516 -0.2367 0.9817 0.027 Uiso 1 1 calc R U . . .
H10B H 0.8966 -0.2255 0.9445 0.027 Uiso 1 1 calc R U . . .
C11 C 0.8678(3) -0.34385(17) 0.98820(16) 0.0276(6) Uani 1 1 d . . . . .
H11A H 0.8920 -0.3343 1.0485 0.033 Uiso 1 1 calc R U . . .
H11B H 0.7917 -0.3840 0.9825 0.033 Uiso 1 1 calc R U . . .
C12 C 0.9909(3) -0.3804(2) 0.95116(19) 0.0379(7) Uani 1 1 d . . . . .
H12A H 1.0172 -0.4317 0.9800 0.057 Uiso 1 1 calc R U . . .
H12B H 1.0677 -0.3417 0.9579 0.057 Uiso 1 1 calc R U . . .
H12C H 0.9674 -0.3913 0.8917 0.057 Uiso 1 1 calc R U . . .
C13 C 0.8239(2) -0.14552(15) 0.79876(15) 0.0190(5) Uani 1 1 d . . . . .
H13A H 0.8622 -0.1253 0.8541 0.023 Uiso 1 1 calc R U . . .
H13B H 0.7904 -0.0975 0.7653 0.023 Uiso 1 1 calc R U . . .
C14 C 0.9384(2) -0.18658(16) 0.75577(16) 0.0224(5) Uani 1 1 d . . . . .
H14A H 0.9854 -0.2270 0.7943 0.027 Uiso 1 1 calc R U . . .
H14B H 0.8977 -0.2165 0.7059 0.027 Uiso 1 1 calc R U . . .
C15 C 1.0435(3) -0.12521(17) 0.72919(18) 0.0286(6) Uani 1 1 d . . . . .
H15A H 0.9973 -0.0851 0.6899 0.034 Uiso 1 1 calc R U . . .
H15B H 1.0844 -0.0950 0.7787 0.034 Uiso 1 1 calc R U . . .
C16 C 1.1565(3) -0.16878(19) 0.68730(19) 0.0340(7) Uani 1 1 d . . . . .
H16A H 1.2227 -0.1284 0.6706 0.051 Uiso 1 1 calc R U . . .
H16B H 1.1161 -0.1981 0.6379 0.051 Uiso 1 1 calc R U . . .
H16C H 1.2032 -0.2078 0.7265 0.051 Uiso 1 1 calc R U . . .
C17 C 0.6348(2) -0.23075(15) 0.72640(14) 0.0169(5) Uani 1 1 d . . . . .
H17A H 0.6998 -0.2669 0.7003 0.020 Uiso 1 1 calc R U . . .
H17B H 0.5532 -0.2639 0.7362 0.020 Uiso 1 1 calc R U . . .
C18 C 0.5905(3) -0.16222(16) 0.66527(15) 0.0233(5) Uani 1 1 d . . . . .
H18A H 0.5429 -0.1191 0.6947 0.028 Uiso 1 1 calc R U . . .
H18B H 0.6727 -0.1374 0.6441 0.028 Uiso 1 1 calc R U . . .
C19 C 0.4951(3) -0.19393(16) 0.59191(15) 0.0239(5) Uani 1 1 d . . . . .
H19A H 0.4132 -0.2191 0.6131 0.029 Uiso 1 1 calc R U . . .
H19B H 0.5430 -0.2368 0.5622 0.029 Uiso 1 1 calc R U . . .
C20 C 0.4497(3) -0.12537(18) 0.53086(17) 0.0313(6) Uani 1 1 d . . . . .
H20A H 0.3890 -0.1479 0.4846 0.047 Uiso 1 1 calc R U . . .
H20B H 0.5305 -0.1009 0.5091 0.047 Uiso 1 1 calc R U . . .
H20C H 0.4006 -0.0834 0.5598 0.047 Uiso 1 1 calc R U . . .
C21 C 0.6023(2) -0.15200(15) 0.85764(15) 0.0174(5) Uani 1 1 d . . . . .
H21A H 0.6501 -0.1345 0.9117 0.021 Uiso 1 1 calc R U . . .
H21B H 0.5771 -0.1019 0.8251 0.021 Uiso 1 1 calc R U . . .
C22 C 0.4713(2) -0.19624(16) 0.87469(15) 0.0213(5) Uani 1 1 d . . . . .
H22A H 0.4941 -0.2435 0.9119 0.026 Uiso 1 1 calc R U . . .
H22B H 0.4252 -0.2173 0.8216 0.026 Uiso 1 1 calc R U . . .
C23 C 0.3745(3) -0.13855(17) 0.91551(17) 0.0263(6) Uani 1 1 d . . . . .
H23A H 0.3510 -0.0918 0.8777 0.032 Uiso 1 1 calc R U . . .
H23B H 0.4217 -0.1167 0.9679 0.032 Uiso 1 1 calc R U . . .
C24 C 0.2425(3) -0.18175(18) 0.93484(17) 0.0281(6) Uani 1 1 d . . . . .
H24A H 0.1832 -0.1428 0.9608 0.042 Uiso 1 1 calc R U . . .
H24B H 0.2651 -0.2274 0.9732 0.042 Uiso 1 1 calc R U . . .
H24C H 0.1946 -0.2027 0.8830 0.042 Uiso 1 1 calc R U . . .
N2 N 0.70250(19) -0.20153(12) 0.81066(12) 0.0157(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 2.0034(16) 3_757 ?
Pd1 O1 2.0034(16) . ?
Pd1 N1 2.0439(19) . ?
Pd1 N1 2.0439(19) 3_757 ?
Pd1 Pd1 9.7928(5) 1_655 ?
Pd1 Pd1 11.4651(4) 2_746 ?
O1 C1 1.302(3) . ?
O2 C1 1.225(3) . ?
O3 C2 1.240(3) . ?
C1 C2 1.548(3) . ?
C2 N1 1.346(3) . ?
C3 C8 1.396(3) . ?
C3 C4 1.408(3) . ?
C3 N1 1.428(3) . ?
C4 C5 1.390(3) . ?
C5 C6 1.392(3) . ?
C6 O1M 1.387(3) . ?
C6 C7 1.393(3) . ?
C7 C8 1.397(3) . ?
O1M C1M 1.436(3) . ?
C9 N2 1.522(3) . ?
C9 C10 1.533(3) . ?
C10 C11 1.534(4) . ?
C11 C12 1.517(4) . ?
C13 N2 1.526(3) . ?
C13 C14 1.527(3) . ?
C14 C15 1.527(3) . ?
C15 C16 1.525(4) . ?
C17 C18 1.526(3) . ?
C17 N2 1.529(3) . ?
C18 C19 1.526(3) . ?
C19 C20 1.528(4) . ?
C21 C22 1.520(3) . ?
C21 N2 1.526(3) . ?
C22 C23 1.529(3) . ?
C23 C24 1.530(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 O1 180.0 3_757 . ?
O1 Pd1 N1 98.39(7) 3_757 . ?
O1 Pd1 N1 81.61(7) . . ?
O1 Pd1 N1 81.61(7) 3_757 3_757 ?
O1 Pd1 N1 98.39(7) . 3_757 ?
N1 Pd1 N1 180.0 . 3_757 ?
O1 Pd1 Pd1 154.73(5) 3_757 1_655 ?
O1 Pd1 Pd1 25.27(5) . 1_655 ?
N1 Pd1 Pd1 93.33(5) . 1_655 ?
N1 Pd1 Pd1 86.67(5) 3_757 1_655 ?
O1 Pd1 Pd1 75.31(5) 3_757 2_746 ?
O1 Pd1 Pd1 104.69(5) . 2_746 ?
N1 Pd1 Pd1 75.38(5) . 2_746 ?
N1 Pd1 Pd1 104.62(5) 3_757 2_746 ?
Pd1 Pd1 Pd1 86.218(2) 1_655 2_746 ?
C1 O1 Pd1 114.85(14) . . ?
O2 C1 O1 123.8(2) . . ?
O2 C1 C2 120.1(2) . . ?
O1 C1 C2 116.05(19) . . ?
O3 C2 N1 128.5(2) . . ?
O3 C2 C1 118.5(2) . . ?
N1 C2 C1 112.89(19) . . ?
C8 C3 C4 117.3(2) . . ?
C8 C3 N1 119.3(2) . . ?
C4 C3 N1 123.4(2) . . ?
C5 C4 C3 121.0(2) . . ?
C4 C5 C6 120.5(2) . . ?
O1M C6 C5 116.3(2) . . ?
O1M C6 C7 124.0(2) . . ?
C5 C6 C7 119.7(2) . . ?
C6 C7 C8 119.2(2) . . ?
C6 O1M C1M 115.97(19) . . ?
C2 N1 C3 119.84(19) . . ?
C2 N1 Pd1 113.53(16) . . ?
C3 N1 Pd1 126.43(15) . . ?
C3 C8 C7 122.2(2) . . ?
N2 C9 C10 115.2(2) . . ?
C9 C10 C11 110.7(2) . . ?
C12 C11 C10 113.7(2) . . ?
N2 C13 C14 114.05(19) . . ?
C15 C14 C13 112.5(2) . . ?
C16 C15 C14 110.7(2) . . ?
C18 C17 N2 114.61(19) . . ?
C19 C18 C17 111.5(2) . . ?
C18 C19 C20 111.7(2) . . ?
C22 C21 N2 115.50(19) . . ?
C21 C22 C23 110.7(2) . . ?
C22 C23 C24 111.9(2) . . ?
C9 N2 C21 110.95(17) . . ?
C9 N2 C13 110.99(17) . . ?
C21 N2 C13 106.80(17) . . ?
C9 N2 C17 106.37(17) . . ?
C21 N2 C17 111.08(17) . . ?
C13 N2 C17 110.71(17) . . ?

_refine_diff_density_max         0.461
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.144

_shelxl_version_number           2013-4



