Supplementary Material (ESI) for Chemical Communications
This journal is (C) The Royal Society of Chemistry 2002

data_global

_database_code_CSD_184116

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Seeber, Georg.'
'Kariuki, Benson M.'
'Cronin, Leroy.'

_publ_contact_author_name     'Dr L Cronin'  
_publ_contact_author_address 
;
Department of Chemistry
University of Glasgow
Glasgow
G12 8QQ
UK
;

_publ_contact_author_email       'L.Cronin@chem.gla.ac.uk'

_publ_section_title
;
Self-assembly of a twelve-component hexanuclear metallosupramolecular ring 
constructed with a novel tri-amino ligand
; 

data_gs101lc
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C36 H113.12 Cl12 N18 O11.56 Pd6'
_chemical_formula_weight          2047.32
 
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'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 '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'
 
_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'p - 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    11.924(2)
_cell_length_b                    12.710(3)
_cell_length_c                    13.929(3)
_cell_angle_alpha                 79.12(3)
_cell_angle_beta                  68.93(3)
_cell_angle_gamma                 88.33(3)
_cell_volume                      1932.7(7)
_cell_formula_units_Z             1
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'pale yellow'
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.759
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1028
_exptl_absorpt_coefficient_mu     1.837
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Rigaku R-axis Diffractometer'
_diffrn_measurement_method        'Image plate detector'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             15688
_diffrn_reflns_av_R_equivalents   0.0439
_diffrn_reflns_av_sigmaI/netI     0.0479
_diffrn_reflns_limit_h_min        -16
_diffrn_reflns_limit_h_max        16
_diffrn_reflns_limit_k_min        -17
_diffrn_reflns_limit_k_max        17
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.60
_diffrn_reflns_theta_max          29.09
_reflns_number_total              8782
_reflns_number_gt                 8002
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        'texray'
_computing_cell_refinement        'texray'
_computing_data_reduction         'texray'
_computing_structure_solution     'wingx'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'wingx'
_computing_publication_material   'wingx'
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.  The structure contained 
 disordered solvent waters (O6A and O6B, O7A and O7B).  The structure also
 contains under occupied chloride positions (Cl4 and Cl5) and disordered 
 chloride counter ions (Cl6A and Cl6B, Cl7a and Cl7b).  It was possible to
 determine between the under occupied chloride positions and water molecules
 through the peak heights, and checking the refinement by substituting the
 chloride by oxygen and refining in borderline cases - in each test the R 
 values increased and the refinement would not converge. The sum of the 
 occupancies for ALL the chloride anions sums to 3 in the assymmetic unit
 and then six in the unit cell, the number expected to charge balance the 6+ 
 charge on the cluster cation.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+7.7900P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0058(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          8782
_refine_ls_number_parameters      431
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0685
_refine_ls_R_factor_gt            0.0614
_refine_ls_wR_factor_ref          0.1395
_refine_ls_wR_factor_gt           0.1344
_refine_ls_goodness_of_fit_ref    1.175
_refine_ls_restrained_S_all       1.175
_refine_ls_shift/su_max           0.004
_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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
O1 O 0.244(2) 0.1727(16) 0.552(2) 0.284(15) Uani 0.75 1 d P . .
O2 O 0.330(3) 0.101(3) 0.400(4) 0.106(13) Uani 0.20 1 d P . .
O3 O 0.3894(8) 0.4432(7) 0.0712(7) 0.117(3) Uani 1 1 d . . .
O4 O 0.7879(7) 0.5724(7) 0.4650(6) 0.099(2) Uani 1 1 d . . .
O5 O 0.0128(9) 0.6733(7) 0.3205(7) 0.123(3) Uani 1 1 d . . .
O6B O 0.3302(4) 0.1735(5) 0.1430(4) 0.0364(11) Uani 0.79 1 d P . .
O6A O 0.289(2) 0.247(2) 0.109(2) 0.071(9) Uani 0.21 1 d P . .
O7A O 0.5000 0.0000 0.0000 0.066(10) Uani 0.20 2 d SP . .
O7B O 0.4254(6) 0.0448(5) 0.0723(6) 0.0540(17) Uani 0.73 1 d P . .
Cl1 Cl 0.05213(19) 0.48189(14) 0.85113(14) 0.0575(4) Uani 1 1 d . . .
Cl2 Cl 0.47306(19) 0.67112(13) 0.59076(12) 0.0541(4) Uani 1 1 d . . .
Cl3 Cl 0.3933(2) 0.98041(15) 0.62800(13) 0.0618(5) Uani 1 1 d . . .
Cl4 Cl 0.2476(2) 0.5273(2) 0.2891(2) 0.0750(6) Uani 0.95 1 d P . .
Cl5 Cl 0.2750(7) 0.9242(5) 0.2718(6) 0.120(2) Uani 0.52 1 d P . .
Cl6A Cl 0.8694(15) 0.9011(11) 0.9483(10) 0.145(5) Uani 0.33 1 d P . .
Cl6B Cl 0.9644(4) 0.9525(3) 0.9272(3) 0.0609(9) Uani 0.50 1 d P . .
Cl7A Cl 0.9863(6) 0.0680(5) 0.7537(6) 0.0621(15) Uani 0.40 1 d P . .
Cl7B Cl 0.970(3) 0.1011(15) 0.7246(16) 0.187(10) Uani 0.30 1 d P . .
C1 C 0.0190(7) 0.6747(7) 0.5649(7) 0.063(2) Uani 1 1 d . . .
H1 H -0.0094 0.6354 0.5233 0.076 Uiso 1 1 calc R . .
C6 C -0.0586(7) 0.7717(8) 0.5835(8) 0.071(2) Uani 1 1 d . . .
H2A H -0.0626 0.8087 0.5173 0.085 Uiso 1 1 calc R . .
H2B H -0.1396 0.7472 0.6299 0.085 Uiso 1 1 calc R . .
C5 C -0.0116(7) 0.8495(7) 0.6308(7) 0.065(2) Uani 1 1 d . . .
H3 H -0.0563 0.9151 0.6269 0.078 Uiso 1 1 calc R . .
C4 C 0.1222(7) 0.8802(6) 0.5698(7) 0.0605(19) Uani 1 1 d . . .
H4A H 0.1504 0.9228 0.6081 0.073 Uiso 1 1 calc R . .
H4B H 0.1306 0.9248 0.5026 0.073 Uiso 1 1 calc R . .
C3 C 0.2027(6) 0.7838(5) 0.5505(6) 0.0470(15) Uani 1 1 d . . .
H5 H 0.2047 0.7453 0.6178 0.056 Uiso 1 1 calc R . .
C2 C 0.1518(7) 0.7076(6) 0.5022(6) 0.0559(18) Uani 1 1 d . . .
H6A H 0.1984 0.6436 0.4978 0.067 Uiso 1 1 calc R . .
H6B H 0.1603 0.7420 0.4314 0.067 Uiso 1 1 calc R . .
C11 C 0.2499(8) 0.8021(5) 1.0279(5) 0.0532(18) Uani 1 1 d . . .
H7 H 0.2380 0.8021 1.1013 0.064 Uiso 1 1 calc R . .
C12 C 0.3510(7) 0.7262(5) 0.9878(5) 0.0525(17) Uani 1 1 d . . .
H8A H 0.4262 0.7569 0.9843 0.063 Uiso 1 1 calc R . .
H8B H 0.3344 0.6584 1.0371 0.063 Uiso 1 1 calc R . .
C7 C 0.3645(7) 0.7056(5) 0.8795(5) 0.0463(15) Uani 1 1 d . . .
H9 H 0.4202 0.6474 0.8647 0.056 Uiso 1 1 calc R . .
C8 C 0.2457(7) 0.6693(5) 0.8764(5) 0.0495(16) Uani 1 1 d . . .
H10A H 0.2233 0.5978 0.9184 0.059 Uiso 1 1 calc R . .
H10B H 0.2567 0.6651 0.8048 0.059 Uiso 1 1 calc R . .
C9 C 0.1421(6) 0.7437(5) 0.9167(5) 0.0434(14) Uani 1 1 d . . .
H11 H 0.1597 0.8125 0.8675 0.052 Uiso 1 1 calc R . .
C10 C 0.1315(7) 0.7641(6) 1.0248(5) 0.0517(17) Uani 1 1 d . . .
H12A H 0.0723 0.8177 1.0445 0.062 Uiso 1 1 calc R . .
H12B H 0.1028 0.6984 1.0761 0.062 Uiso 1 1 calc R . .
C13 C 0.6594(7) 0.6126(5) 0.2677(5) 0.0470(15) Uani 1 1 d . . .
H13 H 0.7109 0.5510 0.2583 0.056 Uiso 1 1 calc R . .
C14 C 0.5837(7) 0.6143(6) 0.1986(5) 0.0538(17) Uani 1 1 d . . .
H14A H 0.6360 0.6070 0.1287 0.065 Uiso 1 1 calc R . .
H14B H 0.5264 0.5535 0.2270 0.065 Uiso 1 1 calc R . .
C15 C 0.5162(7) 0.7170(6) 0.1919(5) 0.0509(16) Uani 1 1 d . . .
H15 H 0.4812 0.7177 0.1379 0.061 Uiso 1 1 calc R . .
C16 C 0.5969(7) 0.8170(5) 0.1600(5) 0.0490(16) Uani 1 1 d . . .
H16A H 0.5478 0.8794 0.1645 0.059 Uiso 1 1 calc R . .
H16B H 0.6502 0.8227 0.0875 0.059 Uiso 1 1 calc R . .
C17 C 0.6719(6) 0.8166(5) 0.2284(5) 0.0397(13) Uani 1 1 d . . .
H17 H 0.6172 0.8209 0.2994 0.048 Uiso 1 1 calc R . .
C18 C 0.7411(6) 0.7126(5) 0.2347(6) 0.0488(15) Uani 1 1 d . . .
H18A H 0.8027 0.7116 0.1667 0.059 Uiso 1 1 calc R . .
H18B H 0.7808 0.7121 0.2845 0.059 Uiso 1 1 calc R . .
Pd1 Pd 0.01488(4) 0.65492(4) 0.79074(4) 0.04418(15) Uani 1 1 d . . .
Pd2 Pd 0.44904(4) 0.70292(4) 0.43014(3) 0.03702(13) Uani 1 1 d . . .
Pd3 Pd 0.33065(4) 0.94381(4) 0.80856(3) 0.03791(13) Uani 1 1 d . . .
N1 N 0.0033(6) 0.6017(5) 0.6656(5) 0.0565(15) Uani 1 1 d . . .
H1A H 0.0580 0.5511 0.6511 0.068 Uiso 1 1 calc R . .
H1B H -0.0695 0.5683 0.6874 0.068 Uiso 1 1 calc R . .
N2 N -0.0352(6) 0.8057(5) 0.7439(5) 0.0584(16) Uani 1 1 d . . .
H2A H -0.1149 0.8079 0.7784 0.070 Uiso 1 1 calc R . .
H2B H 0.0008 0.8516 0.7668 0.070 Uiso 1 1 calc R . .
N3 N 0.3274(5) 0.8189(4) 0.4794(4) 0.0431(12) Uani 1 1 d . . .
H3A H 0.3581 0.8589 0.5116 0.052 Uiso 1 1 calc R . .
H3B H 0.3230 0.8623 0.4218 0.052 Uiso 1 1 calc R . .
N5 N 0.2836(6) 0.9140(4) 0.9687(4) 0.0465(13) Uani 1 1 d . . .
H4A H 0.3457 0.9371 0.9826 0.056 Uiso 1 1 calc R . .
H4B H 0.2213 0.9549 0.9949 0.056 Uiso 1 1 calc R . .
N4 N 0.4194(5) 0.8025(4) 0.7977(4) 0.0452(12) Uani 1 1 d . . .
H5A H 0.4286 0.7866 0.7350 0.054 Uiso 1 1 calc R . .
H5B H 0.4934 0.8146 0.7975 0.054 Uiso 1 1 calc R . .
N6 N 0.0256(5) 0.6981(5) 0.9228(4) 0.0472(13) Uani 1 1 d . . .
H6A H -0.0306 0.7464 0.9427 0.057 Uiso 1 1 calc R . .
H6B H 0.0053 0.6396 0.9743 0.057 Uiso 1 1 calc R . .
N7 N 0.5795(5) 0.5957(4) 0.3808(4) 0.0421(11) Uani 1 1 d . . .
H7A H 0.6271 0.5936 0.4187 0.051 Uiso 1 1 calc R . .
H7B H 0.5428 0.5304 0.3976 0.051 Uiso 1 1 calc R . .
N8 N 0.4144(5) 0.7185(5) 0.2934(4) 0.0475(13) Uani 1 1 d . . .
H8A H 0.3611 0.6655 0.3025 0.057 Uiso 1 1 calc R . .
H8B H 0.3776 0.7807 0.2858 0.057 Uiso 1 1 calc R . .
N9 N 0.7563(5) 0.9130(4) 0.1882(4) 0.0441(12) Uani 1 1 d . . .
H9A H 0.8047 0.9117 0.1218 0.053 Uiso 1 1 calc R . .
H9B H 0.8029 0.9097 0.2271 0.053 Uiso 1 1 calc R . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
O1 0.34(3) 0.167(17) 0.48(4) -0.01(2) -0.35(3) 0.002(18)
O2 0.046(17) 0.08(2) 0.17(4) -0.03(3) -0.01(2) -0.020(18)
O3 0.128(7) 0.097(6) 0.108(6) -0.022(5) -0.022(5) 0.020(5)
O4 0.089(5) 0.122(6) 0.089(5) 0.008(4) -0.050(4) -0.016(5)
O5 0.147(8) 0.113(7) 0.135(7) -0.017(6) -0.083(7) -0.005(6)
O6B 0.015(2) 0.044(3) 0.049(3) -0.005(2) -0.011(2) -0.007(2)
O6A 0.047(13) 0.056(15) 0.071(16) -0.041(13) 0.040(12) -0.024(13)
O7A 0.07(3) 0.07(3) 0.05(2) -0.01(2) -0.019(19) 0.01(2)
O7B 0.060(4) 0.047(4) 0.067(4) 0.012(3) -0.047(4) -0.016(3)
Cl1 0.0688(12) 0.0360(8) 0.0546(9) -0.0080(7) -0.0062(8) -0.0073(8)
Cl2 0.0827(13) 0.0427(8) 0.0405(7) -0.0118(6) -0.0246(8) 0.0051(8)
Cl3 0.0923(15) 0.0498(9) 0.0359(7) -0.0084(7) -0.0135(8) -0.0069(10)
Cl4 0.0646(13) 0.0777(15) 0.0847(15) -0.0249(13) -0.0227(12) -0.0252(12)
Cl5 0.133(6) 0.087(4) 0.153(6) -0.003(4) -0.079(5) 0.019(4)
Cl6A 0.194(14) 0.121(9) 0.112(8) -0.041(7) -0.041(9) 0.055(10)
Cl6B 0.062(2) 0.0462(19) 0.074(2) -0.0246(18) -0.018(2) 0.0123(18)
Cl7A 0.057(3) 0.049(3) 0.087(4) -0.020(3) -0.031(3) 0.000(2)
Cl7B 0.31(3) 0.110(14) 0.120(13) -0.027(10) -0.052(14) 0.010(15)
C1 0.057(4) 0.075(5) 0.067(5) -0.023(4) -0.028(4) -0.013(4)
C6 0.043(4) 0.090(7) 0.086(6) -0.014(5) -0.032(4) 0.002(4)
C5 0.052(4) 0.057(5) 0.086(6) -0.017(4) -0.026(4) 0.018(4)
C4 0.057(5) 0.042(4) 0.083(5) -0.018(4) -0.024(4) 0.006(4)
C3 0.046(4) 0.043(3) 0.054(4) -0.018(3) -0.016(3) 0.004(3)
C2 0.058(4) 0.054(4) 0.060(4) -0.020(3) -0.021(4) -0.008(4)
C11 0.086(5) 0.037(3) 0.034(3) -0.001(2) -0.019(3) -0.017(4)
C12 0.072(5) 0.039(3) 0.053(4) -0.003(3) -0.032(4) -0.004(3)
C7 0.061(4) 0.028(3) 0.054(4) -0.009(3) -0.026(3) 0.002(3)
C8 0.061(4) 0.039(3) 0.050(3) -0.015(3) -0.018(3) 0.000(3)
C9 0.048(4) 0.037(3) 0.038(3) -0.011(2) -0.005(3) -0.006(3)
C10 0.061(4) 0.048(4) 0.038(3) -0.016(3) -0.003(3) -0.011(3)
C13 0.058(4) 0.031(3) 0.045(3) -0.011(3) -0.009(3) -0.001(3)
C14 0.073(5) 0.045(4) 0.043(3) -0.019(3) -0.015(3) -0.007(4)
C15 0.068(5) 0.051(4) 0.041(3) -0.011(3) -0.027(3) -0.012(4)
C16 0.071(5) 0.037(3) 0.039(3) 0.004(3) -0.025(3) -0.015(3)
C17 0.047(3) 0.029(3) 0.040(3) -0.003(2) -0.013(3) -0.009(3)
C18 0.049(4) 0.037(3) 0.053(4) -0.007(3) -0.010(3) 0.001(3)
Pd1 0.0381(3) 0.0385(3) 0.0537(3) -0.0143(2) -0.0106(2) -0.0057(2)
Pd2 0.0437(3) 0.0304(2) 0.0365(2) -0.00797(17) -0.01279(19) -0.00358(19)
Pd3 0.0455(3) 0.0312(2) 0.0341(2) -0.00677(17) -0.01010(19) -0.00643(19)
N1 0.052(3) 0.053(3) 0.070(4) -0.017(3) -0.025(3) -0.014(3)
N2 0.055(4) 0.049(3) 0.078(4) -0.024(3) -0.028(3) 0.014(3)
N3 0.045(3) 0.033(2) 0.052(3) -0.013(2) -0.015(2) 0.000(2)
N5 0.065(4) 0.038(3) 0.035(2) -0.010(2) -0.014(2) -0.006(3)
N4 0.051(3) 0.039(3) 0.045(3) -0.012(2) -0.014(2) 0.002(2)
N6 0.047(3) 0.042(3) 0.044(3) -0.014(2) -0.003(2) -0.008(3)
N7 0.050(3) 0.031(2) 0.039(2) -0.005(2) -0.009(2) -0.002(2)
N8 0.058(3) 0.043(3) 0.052(3) -0.011(2) -0.032(3) -0.004(3)
N9 0.052(3) 0.030(2) 0.044(3) -0.005(2) -0.010(2) -0.006(2)
 
_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
O6B O6A 1.15(3) . ?
O7A O7B 1.294(8) 2_655 ?
O7A O7B 1.294(8) . ?
Cl1 Pd1 2.292(2) . ?
Cl2 Pd2 2.3159(17) . ?
Cl3 Pd3 2.3082(18) . ?
Cl6A Cl6B 1.235(17) . ?
Cl7A Cl7B 0.61(2) . ?
C1 N1 1.481(11) . ?
C1 C6 1.525(12) . ?
C1 C2 1.533(11) . ?
C6 C5 1.507(12) . ?
C5 N2 1.493(11) . ?
C5 C4 1.534(11) . ?
C4 C3 1.538(9) . ?
C3 N3 1.485(9) . ?
C3 C2 1.528(9) . ?
C11 N5 1.489(8) . ?
C11 C10 1.523(10) . ?
C11 C12 1.532(11) . ?
C12 C7 1.530(9) . ?
C7 N4 1.491(9) . ?
C7 C8 1.521(10) . ?
C8 C9 1.539(9) . ?
C9 N6 1.488(8) . ?
C9 C10 1.535(8) . ?
C13 N7 1.497(8) . ?
C13 C18 1.519(9) . ?
C13 C14 1.535(10) . ?
C14 C15 1.519(10) . ?
C15 N8 1.499(9) . ?
C15 C16 1.513(9) . ?
C16 C17 1.523(8) . ?
C17 N9 1.495(8) . ?
C17 C18 1.542(9) . ?
Pd1 N1 2.034(6) . ?
Pd1 N2 2.048(6) . ?
Pd1 N6 2.064(5) . ?
Pd2 N7 2.052(5) . ?
Pd2 N8 2.063(5) . ?
Pd2 N3 2.071(5) . ?
Pd3 N5 2.056(5) . ?
Pd3 N4 2.060(5) . ?
Pd3 N9 2.068(5) 2_676 ?
N9 Pd3 2.068(5) 2_676 ?
 
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
O7B O7A O7B 180.0(12) 2_655 . ?
N1 C1 C6 110.5(7) . . ?
N1 C1 C2 111.5(7) . . ?
C6 C1 C2 112.0(7) . . ?
C5 C6 C1 113.1(6) . . ?
N2 C5 C6 110.5(8) . . ?
N2 C5 C4 111.5(7) . . ?
C6 C5 C4 112.0(7) . . ?
C5 C4 C3 114.1(6) . . ?
N3 C3 C2 108.9(5) . . ?
N3 C3 C4 111.2(6) . . ?
C2 C3 C4 110.2(6) . . ?
C3 C2 C1 113.0(6) . . ?
N5 C11 C10 110.8(6) . . ?
N5 C11 C12 111.2(6) . . ?
C10 C11 C12 111.7(5) . . ?
C7 C12 C11 112.4(6) . . ?
N4 C7 C8 111.9(5) . . ?
N4 C7 C12 110.2(5) . . ?
C8 C7 C12 111.8(6) . . ?
C7 C8 C9 113.8(5) . . ?
N6 C9 C10 109.8(5) . . ?
N6 C9 C8 111.3(5) . . ?
C10 C9 C8 110.7(6) . . ?
C11 C10 C9 113.3(5) . . ?
N7 C13 C18 112.3(5) . . ?
N7 C13 C14 110.2(6) . . ?
C18 C13 C14 111.7(6) . . ?
C15 C14 C13 112.2(5) . . ?
N8 C15 C16 110.5(5) . . ?
N8 C15 C14 110.6(6) . . ?
C16 C15 C14 112.9(6) . . ?
C15 C16 C17 112.5(5) . . ?
N9 C17 C16 110.0(5) . . ?
N9 C17 C18 110.9(5) . . ?
C16 C17 C18 111.6(5) . . ?
C13 C18 C17 112.4(6) . . ?
N1 Pd1 N2 92.9(3) . . ?
N1 Pd1 N6 176.1(2) . . ?
N2 Pd1 N6 90.7(2) . . ?
N1 Pd1 Cl1 86.86(19) . . ?
N2 Pd1 Cl1 174.6(2) . . ?
N6 Pd1 Cl1 89.36(17) . . ?
N7 Pd2 N8 91.1(2) . . ?
N7 Pd2 N3 175.7(2) . . ?
N8 Pd2 N3 90.7(2) . . ?
N7 Pd2 Cl2 88.95(15) . . ?
N8 Pd2 Cl2 174.12(17) . . ?
N3 Pd2 Cl2 89.69(16) . . ?
N5 Pd3 N4 91.4(2) . . ?
N5 Pd3 N9 91.4(2) . 2_676 ?
N4 Pd3 N9 177.3(2) . 2_676 ?
N5 Pd3 Cl3 177.00(18) . . ?
N4 Pd3 Cl3 88.15(16) . . ?
N9 Pd3 Cl3 89.13(16) 2_676 . ?
C1 N1 Pd1 122.4(5) . . ?
C5 N2 Pd1 120.8(5) . . ?
C3 N3 Pd2 118.5(4) . . ?
C11 N5 Pd3 119.0(4) . . ?
C7 N4 Pd3 118.4(4) . . ?
C9 N6 Pd1 118.6(4) . . ?
C13 N7 Pd2 119.3(4) . . ?
C15 N8 Pd2 119.6(4) . . ?
C17 N9 Pd3 113.3(4) . 2_676 ?
 
_diffrn_measured_fraction_theta_max    0.847
_diffrn_reflns_theta_full              29.09
_diffrn_measured_fraction_theta_full   0.847
_refine_diff_density_max    0.730
_refine_diff_density_min   -0.940
_refine_diff_density_rms    0.118