# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Takumi Konno'
_publ_contact_author_email       KONNO@CHEM.SCI.OSAKA-U.AC.JP

_publ_section_title              
;
Excellent chiralselectivity in sulfur-bridged
CoIIIMCoIII (M = NiII and PdII) trinuclear complexes containing
1,2-cyclohexanediamine
;
loop_
_publ_author_name
'Takumi Konno'
'Asako Igashira-Kamiyama'
'Tatsuya Kawamoto'
'Toshihiro Tamai'

# Attachment 'Konno_cif.cif'

data_[1a](ClO4)4
_database_code_depnum_ccdc_archive 'CCDC 689764'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H54.67 Cl4 Co2 N8 Ni O17.33 S4'
_chemical_formula_weight         1131.28

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'
S S 0.1246 0.1234 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P63

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

_cell_length_a                   14.815(2)
_cell_length_b                   14.815(2)
_cell_length_c                   34.618(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6579.8(18)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    874
_cell_measurement_theta_min      0.59
_cell_measurement_theta_max      23.36

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3500
_exptl_absorpt_coefficient_mu    1.679
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.296318
_exptl_absorpt_correction_T_max  0.545702
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
The reflections were collected in a range of 2theta <
46 degree, because there were no strong reflections
in a range of 2theta > 46 degree.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30948
_diffrn_reflns_av_R_equivalents  0.1017
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         0.59
_diffrn_reflns_theta_max         23.36
_reflns_number_total             5740
_reflns_number_gt                3708
_reflns_threshold_expression     >2sigma(I)
_chemical_absolute_configuration rm

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    SIR97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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 crystal was twinned to contain two microdomains, and the
twin law was 0 1 0, 1 0 0, 0 0 -1. One major component was
contained with the batch scale factor (BASF) of 0.23.
;

_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^)+(0.0772P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_number_reflns         5740
_refine_ls_number_parameters     291
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0684
_refine_ls_wR_factor_ref         0.1663
_refine_ls_wR_factor_gt          0.1586
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.996
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66325(19) 0.99382(15) 0.73113(10) 0.0230(4) Uani 1 1 d . . .
Co1 Co 0.63767(18) 0.98930(16) 0.63783(6) 0.0227(6) Uani 1 1 d . . .
Co2 Co 0.68436(18) 0.99993(19) 0.82402(6) 0.0283(7) Uani 1 1 d . . .
S1 S 0.6669(3) 1.0996(3) 0.68575(13) 0.0293(10) Uani 1 1 d . . .
S2 S 0.6436(3) 0.8859(3) 0.68397(13) 0.0305(10) Uani 1 1 d . . .
S3 S 0.6545(3) 1.0876(3) 0.77817(13) 0.0317(10) Uani 1 1 d . . .
S4 S 0.6852(3) 0.9001(3) 0.77516(13) 0.0348(11) Uani 1 1 d . . .
N1 N 0.4857(8) 0.9306(9) 0.6466(3) 0.022(3) Uiso 1 1 d . . .
H1 H 0.4581 0.9462 0.6255 0.027 Uiso 1 1 calc R . .
H2 H 0.4545 0.8592 0.6480 0.027 Uiso 1 1 calc R . .
N2 N 0.7873(9) 1.0441(9) 0.6317(4) 0.030(3) Uiso 1 1 d . . .
H3 H 0.7977 1.0164 0.6095 0.036 Uiso 1 1 calc R . .
H4 H 0.8189 1.1151 0.6283 0.036 Uiso 1 1 calc R . .
N3 N 0.5344(10) 0.9033(10) 0.8299(4) 0.040(4) Uiso 1 1 d . . .
H5 H 0.5237 0.8628 0.8515 0.048 Uiso 1 1 calc R . .
H6 H 0.5015 0.9412 0.8340 0.048 Uiso 1 1 calc R . .
N4 N 0.8364(9) 1.0980(10) 0.8155(4) 0.033(3) Uiso 1 1 d . . .
H7 H 0.8633 1.1364 0.8377 0.039 Uiso 1 1 calc R . .
H8 H 0.8683 1.0589 0.8121 0.039 Uiso 1 1 calc R . .
N5 N 0.6382(9) 1.0828(9) 0.5959(3) 0.020(3) Uiso 1 1 d . . .
H9 H 0.5771 1.0846 0.5969 0.024 Uiso 1 1 calc R . .
H10 H 0.6924 1.1493 0.6000 0.024 Uiso 1 1 calc R . .
N6 N 0.6032(9) 0.8883(9) 0.5956(3) 0.022(3) Uiso 1 1 d . . .
H11 H 0.6598 0.8802 0.5907 0.026 Uiso 1 1 calc R . .
H12 H 0.5488 0.8247 0.6031 0.026 Uiso 1 1 calc R . .
N7 N 0.6814(10) 1.0884(10) 0.8670(4) 0.032(4) Uiso 1 1 d . . .
H13 H 0.7422 1.1516 0.8676 0.039 Uiso 1 1 calc R . .
H14 H 0.6263 1.1000 0.8641 0.039 Uiso 1 1 calc R . .
N8 N 0.7172(11) 0.9264(11) 0.8659(4) 0.051(4) Uiso 1 1 d . . .
H15 H 0.6620 0.8599 0.8691 0.061 Uiso 1 1 calc R . .
H16 H 0.7749 0.9219 0.8592 0.061 Uiso 1 1 calc R . .
C1 C 0.5384(12) 1.0813(12) 0.6880(5) 0.039(4) Uiso 1 1 d . . .
H17 H 0.5262 1.1021 0.7138 0.047 Uiso 1 1 calc R . .
H18 H 0.5305 1.1254 0.6683 0.047 Uiso 1 1 calc R . .
C2 C 0.4600(13) 0.9675(12) 0.6806(5) 0.039(5) Uiso 1 1 d . . .
H19 H 0.4586 0.9254 0.7031 0.047 Uiso 1 1 calc R . .
H20 H 0.3896 0.9589 0.6777 0.047 Uiso 1 1 calc R . .
C3 C 0.7743(12) 0.9119(13) 0.6742(5) 0.040(5) Uiso 1 1 d . . .
H21 H 0.8025 0.8947 0.6973 0.048 Uiso 1 1 calc R . .
H22 H 0.7733 0.8679 0.6525 0.048 Uiso 1 1 calc R . .
C4 C 0.8414(13) 1.0235(12) 0.6643(5) 0.039(5) Uiso 1 1 d . . .
H23 H 0.9115 1.0378 0.6562 0.046 Uiso 1 1 calc R . .
H24 H 0.8492 1.0680 0.6869 0.046 Uiso 1 1 calc R . .
C5 C 0.5575(12) 0.7929(13) 0.7819(5) 0.040(5) Uiso 1 1 d . . .
H25 H 0.5308 0.7548 0.7572 0.048 Uiso 1 1 calc R . .
H26 H 0.5587 0.7443 0.8012 0.048 Uiso 1 1 calc R . .
C6 C 0.4861(13) 0.8338(13) 0.7959(5) 0.038(5) Uiso 1 1 d . . .
H27 H 0.4756 0.8729 0.7749 0.046 Uiso 1 1 calc R . .
H28 H 0.4172 0.7745 0.8032 0.046 Uiso 1 1 calc R . .
C7 C 0.7818(13) 1.2070(13) 0.7789(6) 0.049(5) Uiso 1 1 d . . .
H29 H 0.7913 1.2483 0.7553 0.058 Uiso 1 1 calc R . .
H30 H 0.7870 1.2500 0.8016 0.058 Uiso 1 1 calc R . .
C8 C 0.8673(14) 1.1748(14) 0.7811(5) 0.051(5) Uiso 1 1 d . . .
H31 H 0.8693 1.1407 0.7568 0.061 Uiso 1 1 calc R . .
H32 H 0.9368 1.2367 0.7856 0.061 Uiso 1 1 calc R . .
C9 C 0.5747(12) 0.9216(12) 0.5604(5) 0.030(4) Uiso 1 1 d . . .
H33 H 0.5009 0.9054 0.5631 0.035 Uiso 1 1 calc R . .
C10 C 0.5843(11) 0.8765(11) 0.5225(4) 0.023(4) Uiso 1 1 d . . .
H34 H 0.5327 0.8011 0.5221 0.028 Uiso 1 1 calc R . .
H35 H 0.6545 0.8843 0.5210 0.028 Uiso 1 1 calc R . .
C11 C 0.5675(13) 0.9271(13) 0.4871(5) 0.042(5) Uiso 1 1 d . . .
H36 H 0.4929 0.9066 0.4855 0.051 Uiso 1 1 calc R . .
H37 H 0.5847 0.9003 0.4637 0.051 Uiso 1 1 calc R . .
C12 C 0.6357(14) 1.0505(13) 0.4874(5) 0.041(5) Uiso 1 1 d . . .
H38 H 0.7091 1.0714 0.4818 0.050 Uiso 1 1 calc R . .
H39 H 0.6110 1.0788 0.4666 0.050 Uiso 1 1 calc R . .
C13 C 0.6308(12) 1.0961(11) 0.5245(4) 0.024(4) Uiso 1 1 d . . .
H40 H 0.6833 1.1713 0.5243 0.029 Uiso 1 1 calc R . .
H41 H 0.5612 1.0897 0.5270 0.029 Uiso 1 1 calc R . .
C14 C 0.6488(12) 1.0481(12) 0.5580(5) 0.028(4) Uiso 1 1 d . . .
H42 H 0.7222 1.0626 0.5560 0.034 Uiso 1 1 calc R . .
C15 C 0.6689(15) 1.0262(14) 0.9045(6) 0.048(5) Uiso 1 1 d . . .
H43 H 0.5961 0.9657 0.9050 0.058 Uiso 1 1 calc R . .
C16 C 0.6839(13) 1.0894(12) 0.9399(5) 0.037(4) Uiso 1 1 d . . .
H44 H 0.7525 1.1542 0.9391 0.044 Uiso 1 1 calc R . .
H45 H 0.6289 1.1087 0.9416 0.044 Uiso 1 1 calc R . .
C17 C 0.6784(16) 1.0264(14) 0.9739(5) 0.056(5) Uiso 1 1 d . . .
H46 H 0.6985 1.0716 0.9970 0.067 Uiso 1 1 calc R . .
H47 H 0.6049 0.9708 0.9774 0.067 Uiso 1 1 calc R . .
C18 C 0.7415(16) 0.9790(16) 0.9724(6) 0.062(6) Uiso 1 1 d . . .
H48 H 0.7265 0.9339 0.9954 0.075 Uiso 1 1 calc R . .
H49 H 0.8157 1.0342 0.9736 0.075 Uiso 1 1 calc R . .
C19 C 0.7236(16) 0.9126(15) 0.9354(5) 0.064(6) Uiso 1 1 d . . .
H50 H 0.7752 0.8889 0.9337 0.076 Uiso 1 1 calc R . .
H51 H 0.6526 0.8510 0.9352 0.076 Uiso 1 1 calc R . .
C20 C 0.7376(13) 0.9859(13) 0.9027(5) 0.037(5) Uiso 1 1 d . . .
H52 H 0.8111 1.0451 0.9027 0.044 Uiso 1 1 calc R . .
Cl1 Cl 0.9690(3) 1.2971(3) 0.58972(13) 0.0315(11) Uiso 1 1 d . . .
O1 O 0.8797(9) 1.2302(9) 0.5681(3) 0.047(3) Uiso 1 1 d . . .
O2 O 0.9993(10) 1.4027(10) 0.5823(3) 0.050(3) Uiso 1 1 d . . .
O3 O 0.9515(8) 1.2779(8) 0.6298(3) 0.035(3) Uiso 1 1 d . . .
O4 O 1.0569(11) 1.2826(11) 0.5777(4) 0.075(4) Uiso 1 1 d . . .
Cl2 Cl 1.0000 1.0000 0.7573(2) 0.0317(18) Uiso 1 3 d SDU . .
O5 O 1.0000 1.0000 0.7189(11) 0.127(19) Uiso 0.50 3 d SPDU A 1
O6 O 1.052(3) 1.106(2) 0.7751(10) 0.112(10) Uiso 0.50 1 d PDU A 1
O7 O 1.0000 1.0000 0.7948(11) 0.113(16) Uiso 0.50 3 d SPDU A 2
O8 O 1.1073(18) 1.0478(18) 0.7418(7) 0.047(7) Uiso 0.50 1 d P A 2
Cl3 Cl 1.0000 1.0000 0.8838(2) 0.0409(19) Uiso 1 3 d SU . .
O9 O 1.0000 1.0000 0.9251(10) 0.146(13) Uiso 1 3 d SU . .
O10 O 0.9073(9) 0.9056(9) 0.8718(3) 0.050(3) Uiso 1 1 d . . .
Cl4 Cl 0.6667 1.3333 0.6259(2) 0.0385(19) Uiso 1 3 d S . .
O11 O 0.6667 1.3333 0.6696(6) 0.068(7) Uiso 1 3 d S . .
O12 O 0.7534(8) 1.3227(8) 0.6093(3) 0.038(3) Uiso 1 1 d . . .
Cl5 Cl 0.3333 0.6667 0.5759(2) 0.0227(16) Uiso 1 3 d S . .
O13 O 0.3333 0.6667 0.5357(9) 0.109(11) Uiso 1 3 d S . .
O14 O 0.3359(9) 0.7566(9) 0.5914(3) 0.049(3) Uiso 1 1 d . . .
Cl6 Cl 0.3333 0.6667 0.6991(2) 0.037(2) Uiso 1 3 d SDU . .
O15 O 0.3333 0.6667 0.741(2) 0.13(2) Uiso 0.50 3 d SPU B 1
O16 O 0.2871(19) 0.7211(19) 0.6794(7) 0.054(7) Uiso 0.50 1 d P B 1
O17 O 0.3333 0.6667 0.6600(11) 0.14(2) Uiso 0.50 3 d SPDU B 2
O18 O 0.390(2) 0.625(2) 0.7203(7) 0.071(9) Uiso 0.50 1 d P B 2
Cl7 Cl 0.3333 0.6667 0.8923(5) 0.138(6) Uiso 1 3 d SD . 1
O19 O 0.3333 0.6667 0.9322(10) 0.061(14) Uiso 0.50 3 d SPD C 1
O20 O 0.262(2) 0.5484(19) 0.8842(8) 0.084(10) Uiso 0.50 1 d PD D 1
Cl8 Cl 0.6387(8) 0.6169(9) 0.8682(3) 0.019(3) Uiso 0.50 1 d PD E 1
Cl9 Cl 0.6436(10) 0.5908(10) 0.8650(4) 0.050(5) Uiso 0.50 1 d PD E 2
O21 O 0.628(3) 0.706(3) 0.8784(11) 0.132(14) Uiso 0.50 1 d P E 1
O22 O 0.654(2) 0.499(2) 0.8595(9) 0.090(9) Uiso 0.50 1 d P E 2
O23 O 0.6105(15) 0.6033(15) 0.8282(6) 0.118(6) Uiso 1 1 d . . .
O24 O 0.7410(13) 0.6571(13) 0.8801(5) 0.093(5) Uiso 1 1 d . . .
O25 O 0.5621(11) 0.5625(11) 0.8948(4) 0.072(4) Uiso 1 1 d . . .
O26 O 0.8962(13) 0.8689(13) 1.0665(5) 0.103(6) Uiso 1 1 d . . .
O27 O 1.0000 1.0000 1.0039(7) 0.087(8) Uiso 1 3 d S . .

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
Ni1 0.0273(11) 0.0250(12) 0.0189(8) -0.0007(11) -0.0053(8) 0.0148(11)
Co1 0.0266(13) 0.0220(13) 0.0180(15) 0.0011(11) -0.0022(12) 0.0110(10)
Co2 0.0369(15) 0.0496(16) 0.0151(15) 0.0035(11) 0.0010(12) 0.0341(14)
S1 0.039(3) 0.024(2) 0.026(3) -0.001(2) -0.005(2) 0.016(2)
S2 0.036(3) 0.023(2) 0.028(3) 0.003(2) -0.008(2) 0.011(2)
S3 0.042(3) 0.040(3) 0.021(3) -0.002(2) -0.003(2) 0.027(2)
S4 0.047(3) 0.050(3) 0.025(3) 0.000(2) -0.001(2) 0.037(3)

_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
Ni1 S3 2.186(5) . ?
Ni1 S4 2.193(5) . ?
Ni1 S2 2.200(6) . ?
Ni1 S1 2.201(5) . ?
Ni1 Co2 3.228(4) . ?
Ni1 Co1 3.249(4) . ?
Co1 N2 1.954(12) . ?
Co1 N6 1.968(11) . ?
Co1 N1 1.989(11) . ?
Co1 N5 2.003(11) . ?
Co1 S1 2.214(5) . ?
Co1 S2 2.245(5) . ?
Co2 N3 1.961(13) . ?
Co2 N7 1.998(12) . ?
Co2 N4 1.999(13) . ?
Co2 N8 2.015(14) . ?
Co2 S3 2.230(5) . ?
Co2 S4 2.251(5) . ?
S1 C1 1.785(17) . ?
S2 C3 1.808(17) . ?
S3 C7 1.831(18) . ?
S4 C5 1.775(16) . ?
N1 C2 1.430(18) . ?
N2 C4 1.502(19) . ?
N3 C6 1.49(2) . ?
N4 C8 1.55(2) . ?
N5 C14 1.447(19) . ?
N6 C9 1.454(18) . ?
N7 C15 1.55(2) . ?
N8 C20 1.49(2) . ?
C1 C2 1.52(2) . ?
C3 C4 1.48(2) . ?
C5 C6 1.54(2) . ?
C7 C8 1.56(2) . ?
C9 C10 1.51(2) . ?
C9 C14 1.63(2) . ?
C10 C11 1.52(2) . ?
C11 C12 1.59(2) . ?
C12 C13 1.47(2) . ?
C13 C14 1.45(2) . ?
C15 C20 1.42(2) . ?
C15 C16 1.49(2) . ?
C16 C17 1.48(2) . ?
C17 C18 1.42(3) . ?
C18 C19 1.55(2) . ?
C19 C20 1.51(2) . ?
Cl1 O1 1.408(12) . ?
Cl1 O3 1.415(11) . ?
Cl1 O2 1.419(13) . ?
Cl1 O4 1.482(15) . ?
Cl2 O7 1.30(3) . ?
Cl2 O5 1.33(4) . ?
Cl2 O8 1.48(2) 4_675 ?
Cl2 O8 1.48(2) . ?
Cl2 O8 1.48(2) 3_765 ?
Cl2 O6 1.49(3) 4_675 ?
Cl2 O6 1.49(3) . ?
Cl2 O6 1.49(3) 3_765 ?
Cl3 O9 1.43(3) . ?
Cl3 O10 1.447(12) . ?
Cl3 O10 1.447(12) 4_675 ?
Cl3 O10 1.447(12) 3_765 ?
Cl4 O12 1.486(11) . ?
Cl4 O12 1.486(11) 4_575 ?
Cl4 O12 1.486(11) 3_775 ?
Cl4 O11 1.51(2) . ?
Cl5 O13 1.39(3) . ?
Cl5 O14 1.419(12) . ?
Cl5 O14 1.419(12) 3_665 ?
Cl5 O14 1.419(12) 4_565 ?
Cl6 O17 1.35(4) . ?
Cl6 O18 1.46(3) 3_665 ?
Cl6 O18 1.46(3) 4_565 ?
Cl6 O18 1.46(3) . ?
Cl6 O16 1.46(2) . ?
Cl6 O16 1.46(2) 3_665 ?
Cl6 O16 1.46(2) 4_565 ?
Cl6 O15 1.47(7) . ?
Cl7 O19 1.38(3) . ?
Cl7 O20 1.55(2) 4_565 ?
Cl7 O20 1.55(2) . ?
Cl7 O20 1.55(2) 3_665 ?
Cl8 O25 1.369(16) . ?
Cl8 O24 1.385(19) . ?
Cl8 O23 1.43(2) . ?
Cl8 O21 1.44(4) . ?
Cl9 O24 1.38(2) . ?
Cl9 O23 1.41(2) . ?
Cl9 O22 1.47(3) . ?
Cl9 O25 1.482(18) . ?

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
S3 Ni1 S4 87.6(2) . . ?
S3 Ni1 S2 170.5(2) . . ?
S4 Ni1 S2 93.64(16) . . ?
S3 Ni1 S1 93.87(16) . . ?
S4 Ni1 S1 171.3(2) . . ?
S2 Ni1 S1 86.3(2) . . ?
Co2 Ni1 Co1 178.60(11) . . ?
N2 Co1 N6 92.6(5) . . ?
N2 Co1 N1 177.2(5) . . ?
N6 Co1 N1 88.5(5) . . ?
N2 Co1 N5 91.3(5) . . ?
N6 Co1 N5 84.1(5) . . ?
N1 Co1 N5 91.4(5) . . ?
N2 Co1 S1 90.7(4) . . ?
N6 Co1 S1 176.8(4) . . ?
N1 Co1 S1 88.3(4) . . ?
N5 Co1 S1 95.8(4) . . ?
N2 Co1 S2 86.4(4) . . ?
N6 Co1 S2 95.4(4) . . ?
N1 Co1 S2 90.9(4) . . ?
N5 Co1 S2 177.6(4) . . ?
S1 Co1 S2 84.87(18) . . ?
N3 Co2 N7 90.7(6) . . ?
N3 Co2 N4 177.5(6) . . ?
N7 Co2 N4 91.2(5) . . ?
N3 Co2 N8 91.3(6) . . ?
N7 Co2 N8 84.8(6) . . ?
N4 Co2 N8 90.6(6) . . ?
N3 Co2 S3 91.0(4) . . ?
N7 Co2 S3 94.2(4) . . ?
N4 Co2 S3 87.2(4) . . ?
N8 Co2 S3 177.5(5) . . ?
N3 Co2 S4 88.6(4) . . ?
N7 Co2 S4 179.0(4) . . ?
N4 Co2 S4 89.5(4) . . ?
N8 Co2 S4 95.9(4) . . ?
S3 Co2 S4 85.14(18) . . ?
C1 S1 Ni1 102.5(6) . . ?
C1 S1 Co1 96.9(6) . . ?
Ni1 S1 Co1 94.75(17) . . ?
C3 S2 Ni1 104.2(6) . . ?
C3 S2 Co1 97.2(6) . . ?
Ni1 S2 Co1 93.93(18) . . ?
C7 S3 Ni1 105.4(6) . . ?
C7 S3 Co2 98.3(6) . . ?
Ni1 S3 Co2 93.93(17) . . ?
C5 S4 Ni1 103.2(6) . . ?
C5 S4 Co2 97.8(6) . . ?
Ni1 S4 Co2 93.17(18) . . ?
C2 N1 Co1 114.7(9) . . ?
C4 N2 Co1 116.4(10) . . ?
C6 N3 Co2 113.5(10) . . ?
C8 N4 Co2 117.3(10) . . ?
C14 N5 Co1 112.1(9) . . ?
C9 N6 Co1 111.9(9) . . ?
C15 N7 Co2 105.7(10) . . ?
C20 N8 Co2 109.1(10) . . ?
C2 C1 S1 109.1(11) . . ?
N1 C2 C1 111.2(13) . . ?
C4 C3 S2 109.3(12) . . ?
C3 C4 N2 105.8(13) . . ?
C6 C5 S4 108.9(12) . . ?
N3 C6 C5 109.5(13) . . ?
C8 C7 S3 107.8(12) . . ?
N4 C8 C7 106.0(14) . . ?
N6 C9 C10 118.0(13) . . ?
N6 C9 C14 106.9(12) . . ?
C10 C9 C14 107.7(13) . . ?
C9 C10 C11 114.1(13) . . ?
C10 C11 C12 113.3(14) . . ?
C13 C12 C11 112.7(14) . . ?
C14 C13 C12 114.2(13) . . ?
N5 C14 C13 118.1(13) . . ?
N5 C14 C9 103.3(12) . . ?
C13 C14 C9 114.8(13) . . ?
C20 C15 C16 112.9(16) . . ?
C20 C15 N7 108.4(15) . . ?
C16 C15 N7 112.4(14) . . ?
C17 C16 C15 108.3(14) . . ?
C18 C17 C16 116.2(17) . . ?
C17 C18 C19 113.3(17) . . ?
C20 C19 C18 104.2(16) . . ?
C15 C20 N8 108.2(15) . . ?
C15 C20 C19 113.6(16) . . ?
N8 C20 C19 107.5(14) . . ?
O1 Cl1 O3 111.6(7) . . ?
O1 Cl1 O2 110.3(7) . . ?
O3 Cl1 O2 108.9(7) . . ?
O1 Cl1 O4 109.5(8) . . ?
O3 Cl1 O4 109.5(8) . . ?
O2 Cl1 O4 107.0(8) . . ?
O7 Cl2 O8 111.3(9) . 4_675 ?
O7 Cl2 O8 111.3(9) . . ?
O8 Cl2 O8 107.6(10) 4_675 . ?
O7 Cl2 O8 111.3(9) . 3_765 ?
O8 Cl2 O8 107.6(10) 4_675 3_765 ?
O8 Cl2 O8 107.6(10) . 3_765 ?
O5 Cl2 O6 114.4(14) . 4_675 ?
O5 Cl2 O6 114.4(14) . . ?
O6 Cl2 O6 104.1(16) 4_675 . ?
O5 Cl2 O6 114.4(14) . 3_765 ?
O6 Cl2 O6 104.1(16) 4_675 3_765 ?
O6 Cl2 O6 104.1(16) . 3_765 ?
O9 Cl3 O10 106.7(6) . . ?
O9 Cl3 O10 106.7(6) . 4_675 ?
O10 Cl3 O10 112.1(5) . 4_675 ?
O9 Cl3 O10 106.7(6) . 3_765 ?
O10 Cl3 O10 112.1(5) . 3_765 ?
O10 Cl3 O10 112.1(5) 4_675 3_765 ?
O12 Cl4 O12 106.1(5) . 4_575 ?
O12 Cl4 O12 106.1(5) . 3_775 ?
O12 Cl4 O12 106.1(5) 4_575 3_775 ?
O12 Cl4 O11 112.7(5) . . ?
O12 Cl4 O11 112.7(5) 4_575 . ?
O12 Cl4 O11 112.7(5) 3_775 . ?
O13 Cl5 O14 112.2(5) . . ?
O13 Cl5 O14 112.2(5) . 3_665 ?
O14 Cl5 O14 106.6(6) . 3_665 ?
O13 Cl5 O14 112.2(5) . 4_565 ?
O14 Cl5 O14 106.6(6) . 4_565 ?
O14 Cl5 O14 106.6(6) 3_665 4_565 ?
O17 Cl6 O18 120.1(10) . 3_665 ?
O17 Cl6 O18 120.1(10) . 4_565 ?
O18 Cl6 O18 97.0(13) 3_665 4_565 ?
O17 Cl6 O18 120.1(10) . . ?
O18 Cl6 O18 97.0(13) 3_665 . ?
O18 Cl6 O18 97.0(13) 4_565 . ?
O16 Cl6 O16 99.9(12) . 3_665 ?
O16 Cl6 O16 99.9(12) . 4_565 ?
O16 Cl6 O16 99.9(12) 3_665 4_565 ?
O16 Cl6 O15 117.9(10) . . ?
O16 Cl6 O15 117.9(10) 3_665 . ?
O16 Cl6 O15 117.9(10) 4_565 . ?
O19 Cl7 O20 100.4(13) . 4_565 ?
O19 Cl7 O20 100.4(13) . . ?
O20 Cl7 O20 116.8(8) 4_565 . ?
O19 Cl7 O20 100.4(13) . 3_665 ?
O20 Cl7 O20 116.8(8) 4_565 3_665 ?
O20 Cl7 O20 116.8(8) . 3_665 ?
O25 Cl8 O24 117.3(11) . . ?
O25 Cl8 O23 118.1(12) . . ?
O24 Cl8 O23 122.0(12) . . ?
O25 Cl8 O21 86.2(18) . . ?
O24 Cl8 O21 97.4(19) . . ?
O23 Cl8 O21 102.0(18) . . ?
O24 Cl9 O23 123.9(14) . . ?
O24 Cl9 O22 98.7(16) . . ?
O23 Cl9 O22 102.3(16) . . ?
O24 Cl9 O25 110.4(12) . . ?
O23 Cl9 O25 112.3(13) . . ?
O22 Cl9 O25 106.3(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
S3 Ni1 S1 C1 -69.1(6) . . . . ?
S2 Ni1 S1 C1 101.4(6) . . . . ?
S3 Ni1 S1 Co1 -167.24(16) . . . . ?
S2 Ni1 S1 Co1 3.21(17) . . . . ?
N2 Co1 S1 C1 167.3(7) . . . . ?
N1 Co1 S1 C1 -15.3(6) . . . . ?
N5 Co1 S1 C1 75.9(6) . . . . ?
S2 Co1 S1 C1 -106.4(6) . . . . ?
N2 Co1 S1 Ni1 -89.5(4) . . . . ?
N1 Co1 S1 Ni1 87.9(4) . . . . ?
N5 Co1 S1 Ni1 179.1(4) . . . . ?
S2 Co1 S1 Ni1 -3.15(17) . . . . ?
S4 Ni1 S2 C3 -76.0(6) . . . . ?
S1 Ni1 S2 C3 95.3(6) . . . . ?
S4 Ni1 S2 Co1 -174.48(17) . . . . ?
S1 Ni1 S2 Co1 -3.16(17) . . . . ?
N2 Co1 S2 C3 -10.7(7) . . . . ?
N6 Co1 S2 C3 81.5(7) . . . . ?
N1 Co1 S2 C3 170.1(7) . . . . ?
S1 Co1 S2 C3 -101.7(6) . . . . ?
N2 Co1 S2 Ni1 94.1(4) . . . . ?
N6 Co1 S2 Ni1 -173.6(4) . . . . ?
N1 Co1 S2 Ni1 -85.0(4) . . . . ?
S1 Co1 S2 Ni1 3.15(17) . . . . ?
S4 Ni1 S3 C7 102.3(6) . . . . ?
S1 Ni1 S3 C7 -69.1(6) . . . . ?
S4 Ni1 S3 Co2 2.61(18) . . . . ?
S1 Ni1 S3 Co2 -168.84(17) . . . . ?
N3 Co2 S3 C7 162.8(7) . . . . ?
N7 Co2 S3 C7 72.0(7) . . . . ?
N4 Co2 S3 C7 -19.0(7) . . . . ?
S4 Co2 S3 C7 -108.7(6) . . . . ?
N3 Co2 S3 Ni1 -91.0(4) . . . . ?
N7 Co2 S3 Ni1 178.2(4) . . . . ?
N4 Co2 S3 Ni1 87.2(4) . . . . ?
S4 Co2 S3 Ni1 -2.55(18) . . . . ?
S3 Ni1 S4 C5 96.2(6) . . . . ?
S2 Ni1 S4 C5 -74.4(6) . . . . ?
S3 Ni1 S4 Co2 -2.59(18) . . . . ?
S2 Ni1 S4 Co2 -173.13(17) . . . . ?
N3 Co2 S4 C5 -10.2(7) . . . . ?
N4 Co2 S4 C5 171.5(7) . . . . ?
N8 Co2 S4 C5 81.0(7) . . . . ?
S3 Co2 S4 C5 -101.3(6) . . . . ?
N3 Co2 S4 Ni1 93.6(4) . . . . ?
N4 Co2 S4 Ni1 -84.7(4) . . . . ?
N8 Co2 S4 Ni1 -175.2(4) . . . . ?
S3 Co2 S4 Ni1 2.54(18) . . . . ?
N6 Co1 N1 C2 171.1(11) . . . . ?
N5 Co1 N1 C2 -104.9(11) . . . . ?
S1 Co1 N1 C2 -9.1(10) . . . . ?
S2 Co1 N1 C2 75.7(10) . . . . ?
N6 Co1 N2 C4 -112.7(10) . . . . ?
N5 Co1 N2 C4 163.2(11) . . . . ?
S1 Co1 N2 C4 67.3(10) . . . . ?
S2 Co1 N2 C4 -17.5(10) . . . . ?
N7 Co2 N3 C6 162.9(11) . . . . ?
N8 Co2 N3 C6 -112.4(11) . . . . ?
S3 Co2 N3 C6 68.7(11) . . . . ?
S4 Co2 N3 C6 -16.4(11) . . . . ?
N7 Co2 N4 C8 -101.4(12) . . . . ?
N8 Co2 N4 C8 173.8(12) . . . . ?
S3 Co2 N4 C8 -7.3(11) . . . . ?
S4 Co2 N4 C8 77.9(11) . . . . ?
N2 Co1 N5 C14 73.6(10) . . . . ?
N6 Co1 N5 C14 -18.8(10) . . . . ?
N1 Co1 N5 C14 -107.2(10) . . . . ?
S1 Co1 N5 C14 164.4(9) . . . . ?
N2 Co1 N6 C9 -103.3(10) . . . . ?
N1 Co1 N6 C9 79.3(10) . . . . ?
N5 Co1 N6 C9 -12.3(10) . . . . ?
S2 Co1 N6 C9 170.0(9) . . . . ?
N3 Co2 N7 C15 73.1(11) . . . . ?
N4 Co2 N7 C15 -108.6(11) . . . . ?
N8 Co2 N7 C15 -18.1(11) . . . . ?
S3 Co2 N7 C15 164.1(10) . . . . ?
N3 Co2 N8 C20 -99.5(11) . . . . ?
N7 Co2 N8 C20 -8.9(11) . . . . ?
N4 Co2 N8 C20 82.2(11) . . . . ?
S4 Co2 N8 C20 171.8(10) . . . . ?
Ni1 S1 C1 C2 -59.0(12) . . . . ?
Co1 S1 C1 C2 37.5(12) . . . . ?
Co1 N1 C2 C1 36.4(17) . . . . ?
S1 C1 C2 N1 -50.2(17) . . . . ?
Ni1 S2 C3 C4 -57.5(13) . . . . ?
Co1 S2 C3 C4 38.4(12) . . . . ?
S2 C3 C4 N2 -54.2(15) . . . . ?
Co1 N2 C4 C3 46.0(15) . . . . ?
Ni1 S4 C5 C6 -60.5(12) . . . . ?
Co2 S4 C5 C6 34.6(12) . . . . ?
Co2 N3 C6 C5 43.1(16) . . . . ?
S4 C5 C6 N3 -51.8(16) . . . . ?
Ni1 S3 C7 C8 -52.9(14) . . . . ?
Co2 S3 C7 C8 43.5(13) . . . . ?
Co2 N4 C8 C7 36.3(17) . . . . ?
S3 C7 C8 N4 -51.7(17) . . . . ?
Co1 N6 C9 C10 158.1(11) . . . . ?
Co1 N6 C9 C14 36.7(14) . . . . ?
N6 C9 C10 C11 -171.8(13) . . . . ?
C14 C9 C10 C11 -50.8(17) . . . . ?
C9 C10 C11 C12 50.8(18) . . . . ?
C10 C11 C12 C13 -47.4(19) . . . . ?
C11 C12 C13 C14 49.2(19) . . . . ?
Co1 N5 C14 C13 168.6(11) . . . . ?
Co1 N5 C14 C9 40.6(13) . . . . ?
C12 C13 C14 N5 -175.7(14) . . . . ?
C12 C13 C14 C9 -53.3(19) . . . . ?
N6 C9 C14 N5 -49.5(15) . . . . ?
C10 C9 C14 N5 -177.2(11) . . . . ?
N6 C9 C14 C13 -179.5(12) . . . . ?
C10 C9 C14 C13 52.7(17) . . . . ?
Co2 N7 C15 C20 44.5(16) . . . . ?
Co2 N7 C15 C16 170.0(12) . . . . ?
C20 C15 C16 C17 -53(2) . . . . ?
N7 C15 C16 C17 -175.8(15) . . . . ?
C15 C16 C17 C18 50(2) . . . . ?
C16 C17 C18 C19 -53(2) . . . . ?
C17 C18 C19 C20 53(2) . . . . ?
C16 C15 C20 N8 -178.9(15) . . . . ?
N7 C15 C20 N8 -53.7(18) . . . . ?
C16 C15 C20 C19 62(2) . . . . ?
N7 C15 C20 C19 -173.0(14) . . . . ?
Co2 N8 C20 C15 37.0(17) . . . . ?
Co2 N8 C20 C19 160.1(12) . . . . ?
C18 C19 C20 C15 -58(2) . . . . ?
C18 C19 C20 N8 -177.7(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.36
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.163

#===END

data_[2a](ClO4)4
_database_code_depnum_ccdc_archive 'CCDC 689765'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H54.67 Cl4 Co2 N8 O17.33 Pd S4'
_chemical_formula_weight         1179.02

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'
Co Co 0.3494 0.9721 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P63

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

_cell_length_a                   14.936(4)
_cell_length_b                   14.936(4)
_cell_length_c                   35.317(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6824(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      12.5
_cell_measurement_theta_max      15.0

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3608
_exptl_absorpt_coefficient_mu    1.601
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_T_max  0.9242
_exptl_absorpt_process_details   '(North et al., 1968)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         3
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        3.72
_diffrn_reflns_number            6236
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_sigmaI/netI    0.1248
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5470
_reflns_number_gt                2670
_reflns_threshold_expression     >2sigma(I)
_chemical_absolute_configuration rm

_computing_data_collection       WinAFC
_computing_cell_refinement       WinAFC
_computing_data_reduction        CrystalStructure
_computing_structure_solution    'DIRDIF99 (PATTY)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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.
;

_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^)+(0.1066P)^2^+0.0000P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_number_reflns         5470
_refine_ls_number_parameters     505
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1693
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1891
_refine_ls_wR_factor_gt          0.1491
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.001
_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
Pd1 Pd 0.33015(10) -0.00893(8) 0.35751(6) 0.0425(3) Uani 1 1 d . . .
Co1 Co 0.31349(16) -0.00233(15) 0.26316(6) 0.0427(6) Uani 1 1 d . . .
Co2 Co 0.35258(16) -0.01149(14) 0.45165(5) 0.0390(5) Uani 1 1 d . . .
S1 S 0.4323(3) 0.0908(3) 0.30771(12) 0.0520(10) Uani 1 1 d . . .
S2 S 0.2125(3) -0.1064(3) 0.30998(11) 0.0493(9) Uani 1 1 d . . .
S3 S 0.4367(3) 0.0995(3) 0.40472(11) 0.0496(9) Uani 1 1 d . . .
S4 S 0.2385(3) -0.1168(3) 0.40745(11) 0.0499(9) Uani 1 1 d . . .
N1 N 0.2564(10) 0.0910(10) 0.2710(4) 0.052(3) Uani 1 1 d . . .
H1 H 0.2671 0.1281 0.2497 0.063 Uiso 1 1 calc R . .
H2 H 0.1876 0.0517 0.2742 0.063 Uiso 1 1 calc R . .
N2 N 0.3703(10) -0.0953(10) 0.2579(4) 0.061(3) Uani 1 1 d . . .
H3 H 0.3447 -0.1331 0.2367 0.073 Uiso 1 1 calc R . .
H4 H 0.4393 -0.0570 0.2552 0.073 Uiso 1 1 calc R . .
N3 N 0.4455(9) -0.0693(9) 0.4427(3) 0.049(3) Uani 1 1 d . . .
H5 H 0.4862 -0.0559 0.4632 0.059 Uiso 1 1 calc R . .
H6 H 0.4063 -0.1385 0.4407 0.059 Uiso 1 1 calc R . .
N4 N 0.2618(9) 0.0491(10) 0.4579(4) 0.055(3) Uani 1 1 d . . .
H7 H 0.2282 0.0274 0.4801 0.067 Uiso 1 1 calc R . .
H8 H 0.3017 0.1183 0.4591 0.067 Uiso 1 1 calc R . .
N5 N 0.4018(9) 0.0826(11) 0.2202(4) 0.054(3) Uani 1 1 d . . .
H9 H 0.4029 0.1433 0.2194 0.064 Uiso 1 1 calc R . .
H10 H 0.4671 0.0957 0.2235 0.064 Uiso 1 1 calc R . .
N6 N 0.2073(10) -0.0811(11) 0.2222(3) 0.063(4) Uani 1 1 d . . .
H11 H 0.2006 -0.1439 0.2189 0.075 Uiso 1 1 calc R . .
H12 H 0.1454 -0.0896 0.2289 0.075 Uiso 1 1 calc R . .
N7 N 0.4432(9) 0.0830(8) 0.4915(3) 0.040(3) Uani 1 1 d . . .
H13 H 0.5053 0.0870 0.4903 0.049 Uiso 1 1 calc R . .
H14 H 0.4529 0.1467 0.4873 0.049 Uiso 1 1 calc R . .
N8 N 0.2857(9) -0.1087(8) 0.4938(3) 0.045(3) Uani 1 1 d . . .
H15 H 0.2229 -0.1161 0.4981 0.054 Uiso 1 1 calc R . .
H16 H 0.2767 -0.1710 0.4874 0.054 Uiso 1 1 calc R . .
C1 C 0.4150(16) 0.2032(12) 0.3060(5) 0.073(5) Uani 1 1 d . . .
H17 H 0.4435 0.2448 0.3286 0.087 Uiso 1 1 calc R . .
H18 H 0.4504 0.2456 0.2842 0.087 Uiso 1 1 calc R . .
C2 C 0.2987(14) 0.1642(14) 0.3034(4) 0.064(5) Uani 1 1 d . . .
H19 H 0.2646 0.1296 0.3267 0.076 Uiso 1 1 calc R . .
H20 H 0.2870 0.2218 0.2995 0.076 Uiso 1 1 calc R . .
C3 C 0.2373(14) -0.2099(14) 0.3023(6) 0.072(5) Uani 1 1 d . . .
H21 H 0.2240 -0.2499 0.3254 0.087 Uiso 1 1 calc R . .
H22 H 0.1920 -0.2553 0.2827 0.087 Uiso 1 1 calc R . .
C4 C 0.3464(14) -0.1669(13) 0.2909(5) 0.064(5) Uani 1 1 d . . .
H23 H 0.3586 -0.2227 0.2839 0.077 Uiso 1 1 calc R . .
H24 H 0.3914 -0.1297 0.3120 0.077 Uiso 1 1 calc R . .
C5 C 0.5501(12) 0.0820(13) 0.4033(5) 0.068(5) Uani 1 1 d . . .
H25 H 0.5857 0.1062 0.3793 0.082 Uiso 1 1 calc R . .
H26 H 0.5978 0.1213 0.4235 0.082 Uiso 1 1 calc R . .
C6 C 0.5139(15) -0.0290(17) 0.4081(5) 0.077(5) Uani 1 1 d . . .
H27 H 0.5727 -0.0393 0.4109 0.092 Uiso 1 1 calc R . .
H28 H 0.4753 -0.0667 0.3858 0.092 Uiso 1 1 calc R . .
C7 C 0.1375(11) -0.0855(12) 0.4173(5) 0.059(4) Uani 1 1 d . . .
H29 H 0.0943 -0.0993 0.3950 0.071 Uiso 1 1 calc R . .
H30 H 0.0943 -0.1281 0.4379 0.071 Uiso 1 1 calc R . .
C8 C 0.1848(15) 0.0230(16) 0.4274(5) 0.075(5) Uani 1 1 d . . .
H31 H 0.1318 0.0378 0.4359 0.090 Uiso 1 1 calc R . .
H32 H 0.2183 0.0654 0.4054 0.090 Uiso 1 1 calc R . .
C9 C 0.3598(11) 0.0255(14) 0.1841(4) 0.052(4) Uani 1 1 d . . .
H33 H 0.3744 -0.0315 0.1830 0.063 Uiso 1 1 calc R . .
C10 C 0.4021(14) 0.0902(17) 0.1482(5) 0.079(6) Uani 1 1 d . . .
H34 H 0.4763 0.1190 0.1467 0.095 Uiso 1 1 calc R . .
H35 H 0.3876 0.1467 0.1483 0.095 Uiso 1 1 calc R . .
C11 C 0.3490(19) 0.019(2) 0.1145(6) 0.097(8) Uani 1 1 d . . .
H36 H 0.3750 0.0575 0.0912 0.116 Uiso 1 1 calc R . .
H37 H 0.3652 -0.0365 0.1145 0.116 Uiso 1 1 calc R . .
C12 C 0.2359(17) -0.026(2) 0.1163(5) 0.100(8) Uani 1 1 d . . .
H38 H 0.2046 -0.0698 0.0944 0.119 Uiso 1 1 calc R . .
H39 H 0.2199 0.0296 0.1153 0.119 Uiso 1 1 calc R . .
C13 C 0.1902(15) -0.0879(17) 0.1518(5) 0.084(6) Uani 1 1 d . . .
H40 H 0.1997 -0.1476 0.1519 0.101 Uiso 1 1 calc R . .
H41 H 0.1166 -0.1123 0.1528 0.101 Uiso 1 1 calc R . .
C14 C 0.2439(12) -0.0196(15) 0.1861(5) 0.067(5) Uani 1 1 d . . .
H42 H 0.2284 0.0368 0.1870 0.080 Uiso 1 1 calc R . .
C15 C 0.3991(12) 0.0481(11) 0.5292(4) 0.041(3) Uani 1 1 d . . .
H43 H 0.3422 0.0627 0.5316 0.049 Uiso 1 1 calc R . .
C16 C 0.4662(17) 0.0962(15) 0.5619(5) 0.080(6) Uani 1 1 d . . .
H44 H 0.4915 0.1700 0.5616 0.096 Uiso 1 1 calc R . .
H45 H 0.5253 0.0860 0.5603 0.096 Uiso 1 1 calc R . .
C17 C 0.408(2) 0.0500(18) 0.5989(6) 0.096(8) Uani 1 1 d . . .
H46 H 0.3533 0.0660 0.6017 0.115 Uiso 1 1 calc R . .
H47 H 0.4555 0.0807 0.6201 0.115 Uiso 1 1 calc R . .
C18 C 0.3614(15) -0.0700(16) 0.5997(5) 0.071(5) Uani 1 1 d . . .
H48 H 0.4167 -0.0864 0.5993 0.085 Uiso 1 1 calc R . .
H49 H 0.3219 -0.0982 0.6228 0.085 Uiso 1 1 calc R . .
C19 C 0.2903(14) -0.1191(14) 0.5648(4) 0.070(5) Uani 1 1 d . . .
H50 H 0.2645 -0.1930 0.5645 0.084 Uiso 1 1 calc R . .
H51 H 0.2315 -0.1084 0.5665 0.084 Uiso 1 1 calc R . .
C20 C 0.3489(11) -0.0714(11) 0.5288(4) 0.045(3) Uani 1 1 d . . .
H52 H 0.4046 -0.0879 0.5268 0.054 Uiso 1 1 calc R . .
Cl1 Cl 0.2963(3) -0.0264(3) -0.00041(14) 0.0556(11) Uani 1 1 d . . .
O1 O 0.2744(10) -0.0509(12) -0.0402(4) 0.090(4) Uani 1 1 d . . .
O2 O 0.2282(11) -0.1139(10) 0.0203(4) 0.105(5) Uani 1 1 d . . .
O3 O 0.2780(16) 0.0531(11) 0.0098(6) 0.135(7) Uani 1 1 d . . .
O4 O 0.4006(9) 0.0060(12) 0.0074(5) 0.111(6) Uani 1 1 d . . .
Cl2 Cl -0.0333(4) -0.3920(4) 0.21915(13) 0.0739(14) Uani 1 1 d D . .
O5 O -0.1067(16) -0.3647(19) 0.2118(6) 0.079(7) Uiso 0.50 1 d PD A 1
O6 O -0.035(2) -0.4613(19) 0.1917(6) 0.111(12) Uiso 0.50 1 d PD A 1
O7 O -0.046(3) -0.438(2) 0.2547(5) 0.137(13) Uiso 0.50 1 d PD A 1
O8 O 0.0668(14) -0.3012(18) 0.2177(10) 0.20(2) Uiso 0.50 1 d PD A 1
O9 O 0.0163(19) -0.4229(19) 0.1941(6) 0.079(8) Uiso 0.50 1 d PD A 2
O10 O -0.038(3) -0.3067(17) 0.2074(7) 0.126(13) Uiso 0.50 1 d PD A 2
O11 O 0.016(2) -0.372(2) 0.2552(5) 0.110(10) Uiso 0.50 1 d PD A 2
O12 O -0.1371(13) -0.4764(18) 0.2247(9) 0.149(15) Uiso 0.50 1 d PD A 2
Cl3 Cl 0.3333 -0.3333 0.5121(2) 0.0534(18) Uani 1 3 d S . .
O13 O 0.3333 -0.3333 0.5540(9) 0.172(16) Uani 1 3 d S . .
O14 O 0.3314(9) -0.4239(9) 0.4989(4) 0.085(4) Uani 1 1 d . . .
Cl4 Cl 0.3333 -0.3333 0.3859(2) 0.0583(17) Uani 1 3 d SDU . .
O15 O 0.3333 -0.3333 0.3458(6) 0.091(8) Uiso 0.50 3 d SPDU B 1
O16 O 0.292(2) -0.431(2) 0.4054(9) 0.099(7) Uiso 0.50 1 d PU B 1
O17 O 0.3333 -0.3333 0.4255(6) 0.097(9) Uiso 0.50 3 d SPDU B 2
O18 O 0.382(2) -0.385(2) 0.3681(7) 0.079(6) Uiso 0.50 1 d PU B 2
Cl5 Cl 0.0000 0.0000 0.2046(2) 0.0579(17) Uani 1 3 d S . .
O19 O 0.0000 0.0000 0.1664(8) 0.159(14) Uani 1 3 d S . .
O20 O 0.0899(10) 0.0900(9) 0.2181(5) 0.094(5) Uani 1 1 d . . .
Cl6 Cl 0.0000 0.0000 0.3331(2) 0.0530(16) Uani 1 3 d S . .
O21 O 0.0000 0.0000 0.298(2) 0.17(2) Uiso 0.60 3 d SP C 1
O22 O 0.103(2) 0.054(2) 0.3482(7) 0.109(8) Uiso 0.60 1 d P C 1
O23 O 0.0000 0.0000 0.372(3) 0.16(3) Uiso 0.40 3 d SP C 2
O24 O 0.050(3) -0.051(3) 0.3145(10) 0.088(9) Uiso 0.40 1 d P C 2
Cl7 Cl 0.3333 -0.3333 0.1942(4) 0.137(5) Uani 1 3 d SD . .
O25 O 0.3333 -0.3333 0.1553(7) 0.16(2) Uiso 0.60 3 d SPD D 1
O26 O 0.281(3) -0.446(3) 0.2056(11) 0.159(13) Uiso 0.60 1 d P D 1
O27 O 0.3333 -0.3333 0.2335(7) 0.22(5) Uiso 0.40 3 d SPD D 2
O28 O 0.239(7) -0.423(8) 0.171(3) 0.29(4) Uiso 0.40 1 d P D 2
Cl8 Cl 0.6667 0.3333 0.4664(4) 0.102(4) Uani 1 3 d S . 1
O29 O 0.6667 0.3333 0.4236(8) 0.159(14) Uani 1 3 d S E 1
O30 O 0.5699(9) 0.3209(11) 0.4789(5) 0.098(5) Uani 1 1 d . F 1
O31 O -0.015(2) -0.128(2) 0.0216(7) 0.219(12) Uani 1 1 d . . .
O32 O 0.0000 0.0000 0.0863(14) 0.214(19) Uani 1 3 d S . .

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
Pd1 0.0444(6) 0.0428(6) 0.0357(4) 0.0022(6) -0.0057(5) 0.0183(5)
Co1 0.0347(10) 0.0549(13) 0.0381(13) 0.0016(10) -0.0010(10) 0.0221(10)
Co2 0.0450(11) 0.0366(11) 0.0346(12) 0.0021(9) -0.0034(10) 0.0199(10)
S1 0.048(2) 0.057(2) 0.044(2) 0.0023(19) -0.0051(18) 0.0206(18)
S2 0.0405(19) 0.054(2) 0.0440(19) 0.0022(18) -0.0028(17) 0.0168(17)
S3 0.057(2) 0.0402(19) 0.0390(19) -0.0006(17) -0.0070(19) 0.0150(17)
S4 0.058(2) 0.0380(19) 0.0429(19) 0.0031(16) -0.0087(19) 0.0159(18)
N1 0.055(7) 0.057(7) 0.049(7) 0.001(6) 0.006(6) 0.031(6)
N2 0.054(8) 0.073(9) 0.067(9) 0.000(7) 0.008(7) 0.040(7)
N3 0.062(8) 0.051(7) 0.039(6) -0.005(5) -0.001(6) 0.031(6)
N4 0.045(7) 0.060(8) 0.067(9) 0.010(7) -0.007(6) 0.030(6)
N5 0.041(7) 0.066(9) 0.062(9) 0.001(7) 0.005(6) 0.033(7)
N6 0.050(8) 0.083(10) 0.047(8) 0.001(7) -0.002(6) 0.028(8)
N7 0.046(7) 0.037(6) 0.031(6) -0.003(5) 0.006(5) 0.016(5)
N8 0.052(7) 0.035(6) 0.041(7) 0.005(5) -0.001(6) 0.016(5)
C1 0.119(16) 0.045(9) 0.050(10) -0.006(8) -0.007(10) 0.037(10)
C2 0.090(13) 0.097(14) 0.021(7) 0.011(8) 0.017(7) 0.060(11)
C3 0.071(12) 0.065(11) 0.080(14) 0.020(9) -0.004(10) 0.033(10)
C4 0.075(12) 0.059(10) 0.052(10) 0.001(8) -0.012(9) 0.028(9)
C5 0.049(9) 0.077(12) 0.049(9) -0.004(9) -0.010(8) 0.008(9)
C6 0.087(13) 0.128(17) 0.033(9) -0.005(11) 0.001(9) 0.068(13)
C7 0.051(9) 0.056(10) 0.069(11) 0.007(8) -0.019(8) 0.026(8)
C8 0.088(13) 0.109(16) 0.065(11) -0.018(11) -0.002(10) 0.077(13)
C9 0.040(8) 0.085(12) 0.032(8) -0.005(8) 0.009(6) 0.032(8)
C10 0.066(11) 0.126(17) 0.051(10) 0.010(11) 0.018(9) 0.052(12)
C11 0.106(18) 0.16(2) 0.046(11) -0.001(12) -0.004(11) 0.079(17)
C12 0.086(15) 0.18(2) 0.046(11) -0.039(13) -0.016(10) 0.078(16)
C13 0.084(13) 0.136(18) 0.045(10) -0.022(11) -0.014(9) 0.065(13)
C14 0.050(10) 0.088(13) 0.037(9) -0.013(9) -0.001(8) 0.015(9)
C15 0.049(9) 0.053(9) 0.035(7) -0.001(7) -0.002(7) 0.037(7)
C16 0.120(16) 0.089(13) 0.034(9) -0.026(9) -0.020(10) 0.054(12)
C17 0.12(2) 0.112(18) 0.088(17) -0.053(14) -0.052(15) 0.083(17)
C18 0.082(13) 0.095(15) 0.040(10) 0.010(9) 0.001(9) 0.048(12)
C19 0.081(12) 0.070(11) 0.050(10) 0.016(9) 0.026(9) 0.031(10)
C20 0.053(9) 0.055(9) 0.023(7) 0.004(6) 0.007(6) 0.023(7)
Cl1 0.0397(19) 0.052(2) 0.064(3) 0.004(2) 0.0001(19) 0.0141(17)
O1 0.074(9) 0.121(11) 0.060(8) 0.014(8) 0.011(7) 0.037(8)
O2 0.089(10) 0.061(8) 0.116(12) 0.026(8) 0.031(9) 0.001(7)
O3 0.200(18) 0.074(10) 0.155(16) 0.018(10) 0.034(14) 0.086(12)
O4 0.027(6) 0.146(13) 0.139(14) 0.022(11) 0.005(7) 0.027(7)
Cl2 0.106(4) 0.095(4) 0.053(3) -0.010(3) -0.001(3) 0.075(3)
Cl3 0.042(2) 0.042(2) 0.075(5) 0.000 0.000 0.0212(11)
O13 0.23(3) 0.23(3) 0.057(18) 0.000 0.000 0.114(13)
O14 0.059(7) 0.044(6) 0.148(13) -0.010(8) 0.011(8) 0.022(6)
Cl4 0.058(2) 0.058(2) 0.059(4) 0.000 0.000 0.0290(12)
Cl5 0.056(2) 0.056(2) 0.063(5) 0.000 0.000 0.0278(12)
O19 0.21(2) 0.21(2) 0.051(17) 0.000 0.000 0.107(11)
O20 0.074(9) 0.050(7) 0.137(12) 0.006(8) -0.047(9) 0.015(7)
Cl6 0.047(2) 0.047(2) 0.065(4) 0.000 0.000 0.0234(12)
Cl7 0.156(8) 0.156(8) 0.100(9) 0.000 0.000 0.078(4)
Cl8 0.042(2) 0.042(2) 0.222(14) 0.000 0.000 0.0208(12)
O29 0.21(2) 0.21(2) 0.052(17) 0.000 0.000 0.106(12)
O30 0.038(6) 0.100(10) 0.163(15) 0.019(10) 0.020(8) 0.041(7)
O31 0.30(3) 0.25(3) 0.17(2) -0.08(2) -0.02(2) 0.18(3)
O32 0.23(3) 0.23(3) 0.18(4) 0.000 0.000 0.116(14)

_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 S3 2.315(4) . ?
Pd1 S1 2.317(5) . ?
Pd1 S4 2.318(4) . ?
Pd1 S2 2.338(4) . ?
Pd1 Co2 3.344(3) . ?
Pd1 Co1 3.347(3) . ?
Co1 N2 1.964(12) . ?
Co1 N1 1.983(12) . ?
Co1 N5 1.995(13) . ?
Co1 N6 2.031(12) . ?
Co1 S2 2.254(5) . ?
Co1 S1 2.256(5) . ?
Co2 N8 1.968(10) . ?
Co2 N7 1.974(11) . ?
Co2 N4 1.983(12) . ?
Co2 N3 1.992(11) . ?
Co2 S3 2.234(4) . ?
Co2 S4 2.266(4) . ?
S1 C1 1.823(17) . ?
S2 C3 1.781(17) . ?
S3 C5 1.839(18) . ?
S4 C7 1.821(16) . ?
N1 C2 1.488(19) . ?
N2 C4 1.50(2) . ?
N3 C6 1.513(19) . ?
N4 C8 1.48(2) . ?
N5 C9 1.49(2) . ?
N6 C14 1.50(2) . ?
N7 C15 1.463(18) . ?
N8 C20 1.485(17) . ?
C1 C2 1.53(3) . ?
C3 C4 1.48(2) . ?
C5 C6 1.47(2) . ?
C7 C8 1.45(2) . ?
C9 C14 1.51(2) . ?
C9 C10 1.53(2) . ?
C10 C11 1.53(3) . ?
C11 C12 1.47(3) . ?
C12 C13 1.51(3) . ?
C13 C14 1.53(2) . ?
C15 C16 1.46(2) . ?
C15 C20 1.55(2) . ?
C16 C17 1.53(3) . ?
C17 C18 1.56(3) . ?
C18 C19 1.55(2) . ?
C19 C20 1.51(2) . ?
Cl1 O3 1.393(15) . ?
Cl1 O2 1.395(13) . ?
Cl1 O4 1.409(12) . ?
Cl1 O1 1.448(14) . ?
Cl2 O5 1.373(13) . ?
Cl2 O9 1.374(13) . ?
Cl2 O10 1.376(14) . ?
Cl2 O7 1.398(14) . ?
Cl2 O6 1.411(14) . ?
Cl2 O11 1.423(13) . ?
Cl2 O8 1.432(14) . ?
Cl2 O12 1.440(14) . ?
Cl3 O14 1.418(11) 5_655 ?
Cl3 O14 1.418(12) 3_545 ?
Cl3 O14 1.418(11) . ?
Cl3 O13 1.48(3) . ?
Cl4 O17 1.40(2) . ?
Cl4 O15 1.417(19) . ?
Cl4 O18 1.44(3) 5_655 ?
Cl4 O18 1.44(3) 3_545 ?
Cl4 O18 1.44(3) . ?
Cl4 O16 1.45(3) 5_655 ?
Cl4 O16 1.45(3) 3_545 ?
Cl4 O16 1.45(3) . ?
Cl5 O19 1.35(3) . ?
Cl5 O20 1.426(12) . ?
Cl5 O20 1.426(12) 5 ?
Cl5 O20 1.426(12) 3 ?
Cl6 O21 1.23(7) . ?
Cl6 O23 1.39(10) . ?
Cl6 O22 1.44(3) 5 ?
Cl6 O22 1.44(3) 3 ?
Cl6 O22 1.44(3) . ?
Cl6 O24 1.46(4) 5 ?
Cl6 O24 1.46(4) . ?
Cl6 O24 1.46(4) 3 ?
Cl7 O25 1.37(2) . ?
Cl7 O27 1.39(2) . ?
Cl7 O26 1.51(4) 5_655 ?
Cl7 O26 1.51(4) 3_545 ?
Cl7 O26 1.51(4) . ?
Cl7 O28 1.60(10) 5_655 ?
Cl7 O28 1.60(10) . ?
Cl7 O28 1.60(10) 3_545 ?
Cl8 O30 1.432(12) 3_655 ?
Cl8 O30 1.432(12) 5_665 ?
Cl8 O30 1.432(12) . ?
Cl8 O29 1.51(3) . ?

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
S3 Pd1 S1 95.49(13) . . ?
S3 Pd1 S4 84.20(15) . . ?
S1 Pd1 S4 174.05(16) . . ?
S3 Pd1 S2 173.01(15) . . ?
S1 Pd1 S2 84.46(16) . . ?
S4 Pd1 S2 96.58(13) . . ?
Co2 Pd1 Co1 178.68(7) . . ?
N2 Co1 N1 177.4(6) . . ?
N2 Co1 N5 89.7(5) . . ?
N1 Co1 N5 92.3(5) . . ?
N2 Co1 N6 90.7(6) . . ?
N1 Co1 N6 91.2(6) . . ?
N5 Co1 N6 84.4(5) . . ?
N2 Co1 S2 87.6(4) . . ?
N1 Co1 S2 90.4(4) . . ?
N5 Co1 S2 176.7(4) . . ?
N6 Co1 S2 93.7(4) . . ?
N2 Co1 S1 91.0(4) . . ?
N1 Co1 S1 87.2(4) . . ?
N5 Co1 S1 94.1(4) . . ?
N6 Co1 S1 177.8(4) . . ?
S2 Co1 S1 87.84(17) . . ?
N8 Co2 N7 84.4(4) . . ?
N8 Co2 N4 92.4(5) . . ?
N7 Co2 N4 88.6(5) . . ?
N8 Co2 N3 90.4(5) . . ?
N7 Co2 N3 92.6(5) . . ?
N4 Co2 N3 177.1(5) . . ?
N8 Co2 S3 176.9(4) . . ?
N7 Co2 S3 93.9(3) . . ?
N4 Co2 S3 90.2(4) . . ?
N3 Co2 S3 87.1(4) . . ?
N8 Co2 S4 94.6(3) . . ?
N7 Co2 S4 175.3(4) . . ?
N4 Co2 S4 86.8(4) . . ?
N3 Co2 S4 92.0(4) . . ?
S3 Co2 S4 87.30(15) . . ?
C1 S1 Co1 96.6(6) . . ?
C1 S1 Pd1 105.4(7) . . ?
Co1 S1 Pd1 94.07(15) . . ?
C3 S2 Co1 97.5(6) . . ?
C3 S2 Pd1 103.4(6) . . ?
Co1 S2 Pd1 93.56(15) . . ?
C5 S3 Co2 97.5(6) . . ?
C5 S3 Pd1 104.0(6) . . ?
Co2 S3 Pd1 94.60(14) . . ?
C7 S4 Co2 97.1(5) . . ?
C7 S4 Pd1 104.1(5) . . ?
Co2 S4 Pd1 93.66(15) . . ?
C2 N1 Co1 116.8(10) . . ?
C4 N2 Co1 113.5(10) . . ?
C6 N3 Co2 115.6(10) . . ?
C8 N4 Co2 114.7(10) . . ?
C9 N5 Co1 109.4(10) . . ?
C14 N6 Co1 108.0(9) . . ?
C15 N7 Co2 111.6(9) . . ?
C20 N8 Co2 111.1(8) . . ?
C2 C1 S1 107.9(12) . . ?
N1 C2 C1 108.0(12) . . ?
C4 C3 S2 109.1(13) . . ?
C3 C4 N2 109.9(14) . . ?
C6 C5 S3 108.1(11) . . ?
C5 C6 N3 109.6(14) . . ?
C8 C7 S4 109.3(11) . . ?
C7 C8 N4 110.8(14) . . ?
N5 C9 C14 106.0(11) . . ?
N5 C9 C10 115.3(15) . . ?
C14 C9 C10 110.0(14) . . ?
C9 C10 C11 107.3(18) . . ?
C12 C11 C10 111.1(17) . . ?
C11 C12 C13 112.2(18) . . ?
C12 C13 C14 108.9(17) . . ?
N6 C14 C9 107.3(14) . . ?
N6 C14 C13 110.8(15) . . ?
C9 C14 C13 111.2(15) . . ?
C16 C15 N7 117.9(14) . . ?
C16 C15 C20 113.0(13) . . ?
N7 C15 C20 105.8(10) . . ?
C15 C16 C17 111.1(17) . . ?
C16 C17 C18 111.1(16) . . ?
C19 C18 C17 109.6(14) . . ?
C20 C19 C18 110.4(14) . . ?
N8 C20 C19 114.5(12) . . ?
N8 C20 C15 106.9(11) . . ?
C19 C20 C15 111.6(12) . . ?
O3 Cl1 O2 107.5(11) . . ?
O3 Cl1 O4 108.1(12) . . ?
O2 Cl1 O4 112.4(10) . . ?
O3 Cl1 O1 110.5(11) . . ?
O2 Cl1 O1 107.8(9) . . ?
O4 Cl1 O1 110.4(9) . . ?
O9 Cl2 O10 113.8(11) . . ?
O5 Cl2 O7 112.8(11) . . ?
O5 Cl2 O6 111.6(10) . . ?
O7 Cl2 O6 108.0(10) . . ?
O9 Cl2 O11 109.8(10) . . ?
O10 Cl2 O11 109.6(10) . . ?
O5 Cl2 O8 108.8(10) . . ?
O7 Cl2 O8 108.3(11) . . ?
O6 Cl2 O8 107.2(10) . . ?
O9 Cl2 O12 108.7(10) . . ?
O10 Cl2 O12 108.7(10) . . ?
O11 Cl2 O12 106.1(10) . . ?
O14 Cl3 O14 109.7(7) 5_655 3_545 ?
O14 Cl3 O14 109.7(7) 5_655 . ?
O14 Cl3 O14 109.7(7) 3_545 . ?
O14 Cl3 O13 109.2(7) 5_655 . ?
O14 Cl3 O13 109.2(7) 3_545 . ?
O14 Cl3 O13 109.2(7) . . ?
O17 Cl4 O18 115.9(10) . 5_655 ?
O17 Cl4 O18 115.9(10) . 3_545 ?
O18 Cl4 O18 102.4(12) 5_655 3_545 ?
O17 Cl4 O18 115.9(10) . . ?
O18 Cl4 O18 102.4(12) 5_655 . ?
O18 Cl4 O18 102.4(12) 3_545 . ?
O15 Cl4 O16 118.4(12) . 5_655 ?
O15 Cl4 O16 118.4(12) . 3_545 ?
O16 Cl4 O16 99.3(16) 5_655 3_545 ?
O15 Cl4 O16 118.4(12) . . ?
O16 Cl4 O16 99.3(16) 5_655 . ?
O16 Cl4 O16 99.3(16) 3_545 . ?
O19 Cl5 O20 109.5(7) . . ?
O19 Cl5 O20 109.5(7) . 5 ?
O20 Cl5 O20 109.4(7) . 5 ?
O19 Cl5 O20 109.5(7) . 3 ?
O20 Cl5 O20 109.4(7) . 3 ?
O20 Cl5 O20 109.4(7) 5 3 ?
O21 Cl6 O22 111.8(11) . 5 ?
O21 Cl6 O22 111.8(11) . 3 ?
O22 Cl6 O22 107.1(12) 5 3 ?
O21 Cl6 O22 111.8(11) . . ?
O22 Cl6 O22 107.1(12) 5 . ?
O22 Cl6 O22 107.1(12) 3 . ?
O23 Cl6 O24 116.7(14) . 5 ?
O23 Cl6 O24 116.7(14) . . ?
O24 Cl6 O24 101.4(17) 5 . ?
O23 Cl6 O24 116.7(14) . 3 ?
O24 Cl6 O24 101.4(17) 5 3 ?
O24 Cl6 O24 101.4(17) . 3 ?
O25 Cl7 O26 105.4(16) . 5_655 ?
O25 Cl7 O26 105.4(16) . 3_545 ?
O26 Cl7 O26 113.2(13) 5_655 3_545 ?
O25 Cl7 O26 105.4(16) . . ?
O26 Cl7 O26 113.2(13) 5_655 . ?
O26 Cl7 O26 113.2(13) 3_545 . ?
O27 Cl7 O28 121(4) . 5_655 ?
O27 Cl7 O28 121(4) . . ?
O28 Cl7 O28 96(5) 5_655 . ?
O27 Cl7 O28 121(4) . 3_545 ?
O28 Cl7 O28 96(5) 5_655 3_545 ?
O28 Cl7 O28 96(5) . 3_545 ?
O30 Cl8 O30 110.9(8) 3_655 5_665 ?
O30 Cl8 O30 110.9(8) 3_655 . ?
O30 Cl8 O30 110.9(8) 5_665 . ?
O30 Cl8 O29 108.0(8) 3_655 . ?
O30 Cl8 O29 108.0(8) 5_665 . ?
O30 Cl8 O29 108.0(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Co1 S1 C1 164.3(8) . . . . ?
N1 Co1 S1 C1 -17.6(7) . . . . ?
N5 Co1 S1 C1 74.5(7) . . . . ?
S2 Co1 S1 C1 -108.2(7) . . . . ?
N2 Co1 S1 Pd1 -89.7(4) . . . . ?
N1 Co1 S1 Pd1 88.5(4) . . . . ?
N5 Co1 S1 Pd1 -179.5(4) . . . . ?
S2 Co1 S1 Pd1 -2.10(16) . . . . ?
S3 Pd1 S1 C1 -72.9(6) . . . . ?
S2 Pd1 S1 C1 100.1(6) . . . . ?
S3 Pd1 S1 Co1 -170.95(16) . . . . ?
S2 Pd1 S1 Co1 2.03(15) . . . . ?
N2 Co1 S2 C3 -10.9(8) . . . . ?
N1 Co1 S2 C3 170.9(7) . . . . ?
N6 Co1 S2 C3 79.6(8) . . . . ?
S1 Co1 S2 C3 -101.9(7) . . . . ?
N2 Co1 S2 Pd1 93.2(4) . . . . ?
N1 Co1 S2 Pd1 -85.1(4) . . . . ?
N6 Co1 S2 Pd1 -176.3(4) . . . . ?
S1 Co1 S2 Pd1 2.08(16) . . . . ?
S1 Pd1 S2 C3 96.5(6) . . . . ?
S4 Pd1 S2 C3 -77.6(6) . . . . ?
S1 Pd1 S2 Co1 -2.03(15) . . . . ?
S4 Pd1 S2 Co1 -176.14(15) . . . . ?
N7 Co2 S3 C5 76.0(6) . . . . ?
N4 Co2 S3 C5 164.6(7) . . . . ?
N3 Co2 S3 C5 -16.4(6) . . . . ?
S4 Co2 S3 C5 -108.6(6) . . . . ?
N7 Co2 S3 Pd1 -179.2(4) . . . . ?
N4 Co2 S3 Pd1 -90.7(4) . . . . ?
N3 Co2 S3 Pd1 88.4(4) . . . . ?
S4 Co2 S3 Pd1 -3.83(16) . . . . ?
S1 Pd1 S3 C5 -71.3(6) . . . . ?
S4 Pd1 S3 C5 102.7(6) . . . . ?
S1 Pd1 S3 Co2 -170.27(16) . . . . ?
S4 Pd1 S3 Co2 3.75(16) . . . . ?
N8 Co2 S4 C7 81.6(6) . . . . ?
N4 Co2 S4 C7 -10.5(6) . . . . ?
N3 Co2 S4 C7 172.1(6) . . . . ?
S3 Co2 S4 C7 -100.9(5) . . . . ?
N8 Co2 S4 Pd1 -173.7(4) . . . . ?
N4 Co2 S4 Pd1 94.2(4) . . . . ?
N3 Co2 S4 Pd1 -83.2(4) . . . . ?
S3 Co2 S4 Pd1 3.82(16) . . . . ?
S3 Pd1 S4 C7 94.5(5) . . . . ?
S2 Pd1 S4 C7 -78.5(5) . . . . ?
S3 Pd1 S4 Co2 -3.70(15) . . . . ?
S2 Pd1 S4 Co2 -176.71(15) . . . . ?
N5 Co1 N1 C2 -102.8(11) . . . . ?
N6 Co1 N1 C2 172.7(11) . . . . ?
S2 Co1 N1 C2 79.1(10) . . . . ?
S1 Co1 N1 C2 -8.7(10) . . . . ?
N5 Co1 N2 C4 166.7(11) . . . . ?
N6 Co1 N2 C4 -108.9(11) . . . . ?
S2 Co1 N2 C4 -15.3(10) . . . . ?
S1 Co1 N2 C4 72.5(10) . . . . ?
N8 Co2 N3 C6 173.6(11) . . . . ?
N7 Co2 N3 C6 -102.0(11) . . . . ?
S3 Co2 N3 C6 -8.2(11) . . . . ?
S4 Co2 N3 C6 78.9(11) . . . . ?
N8 Co2 N4 C8 -109.1(12) . . . . ?
N7 Co2 N4 C8 166.6(12) . . . . ?
S3 Co2 N4 C8 72.7(12) . . . . ?
S4 Co2 N4 C8 -14.6(11) . . . . ?
N2 Co1 N5 C9 73.0(10) . . . . ?
N1 Co1 N5 C9 -108.7(10) . . . . ?
N6 Co1 N5 C9 -17.7(10) . . . . ?
S1 Co1 N5 C9 163.9(9) . . . . ?
N2 Co1 N6 C14 -101.8(12) . . . . ?
N1 Co1 N6 C14 80.0(12) . . . . ?
N5 Co1 N6 C14 -12.1(11) . . . . ?
S2 Co1 N6 C14 170.6(11) . . . . ?
N8 Co2 N7 C15 -16.2(9) . . . . ?
N4 Co2 N7 C15 76.4(9) . . . . ?
N3 Co2 N7 C15 -106.3(9) . . . . ?
S3 Co2 N7 C15 166.5(8) . . . . ?
N7 Co2 N8 C20 -12.4(9) . . . . ?
N4 Co2 N8 C20 -100.7(10) . . . . ?
N3 Co2 N8 C20 80.2(10) . . . . ?
S4 Co2 N8 C20 172.3(9) . . . . ?
Co1 S1 C1 C2 41.9(11) . . . . ?
Pd1 S1 C1 C2 -54.2(11) . . . . ?
Co1 N1 C2 C1 38.2(15) . . . . ?
S1 C1 C2 N1 -53.1(15) . . . . ?
Co1 S2 C3 C4 36.3(13) . . . . ?
Pd1 S2 C3 C4 -59.1(13) . . . . ?
S2 C3 C4 N2 -53.0(17) . . . . ?
Co1 N2 C4 C3 43.5(17) . . . . ?
Co2 S3 C5 C6 40.8(12) . . . . ?
Pd1 S3 C5 C6 -55.9(12) . . . . ?
S3 C5 C6 N3 -51.7(16) . . . . ?
Co2 N3 C6 C5 37.8(17) . . . . ?
Co2 S4 C7 C8 35.4(13) . . . . ?
Pd1 S4 C7 C8 -60.1(13) . . . . ?
S4 C7 C8 N4 -51.8(17) . . . . ?
Co2 N4 C8 C7 42.8(17) . . . . ?
Co1 N5 C9 C14 43.5(16) . . . . ?
Co1 N5 C9 C10 165.4(11) . . . . ?
N5 C9 C10 C11 -179.3(14) . . . . ?
C14 C9 C10 C11 -59.6(19) . . . . ?
C9 C10 C11 C12 60(2) . . . . ?
C10 C11 C12 C13 -60(3) . . . . ?
C11 C12 C13 C14 56(2) . . . . ?
Co1 N6 C14 C9 39.1(16) . . . . ?
Co1 N6 C14 C13 160.7(12) . . . . ?
N5 C9 C14 N6 -54.1(18) . . . . ?
C10 C9 C14 N6 -179.3(15) . . . . ?
N5 C9 C14 C13 -175.4(15) . . . . ?
C10 C9 C14 C13 59(2) . . . . ?
C12 C13 C14 N6 -175.0(16) . . . . ?
C12 C13 C14 C9 -56(2) . . . . ?
Co2 N7 C15 C16 166.7(12) . . . . ?
Co2 N7 C15 C20 39.1(12) . . . . ?
N7 C15 C16 C17 -179.3(14) . . . . ?
C20 C15 C16 C17 -55(2) . . . . ?
C15 C16 C17 C18 56(2) . . . . ?
C16 C17 C18 C19 -56(2) . . . . ?
C17 C18 C19 C20 56(2) . . . . ?
Co2 N8 C20 C19 160.3(11) . . . . ?
Co2 N8 C20 C15 36.2(12) . . . . ?
C18 C19 C20 N8 -176.4(14) . . . . ?
C18 C19 C20 C15 -54.9(18) . . . . ?
C16 C15 C20 N8 -178.5(13) . . . . ?
N7 C15 C20 N8 -48.1(13) . . . . ?
C16 C15 C20 C19 55.6(18) . . . . ?
N7 C15 C20 C19 -173.9(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.131