# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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. 
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data_Os4Cd4
_database_code_depnum_ccdc_archive 'CCDC 1413546'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C336 H266 Cd4 Cl16 N72 O65 Os4'
_chemical_formula_weight         8129.79

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   28.987(8)
_cell_length_b                   28.987(8)
_cell_length_c                   54.10(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     39367(28)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    22538
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_F_000             12222
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.261
_shelx_estimated_absorpt_T_min   0.787
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           'Mo K\a'
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            215867
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_theta_min         2.485
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             19846
_reflns_number_gt                16327
_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       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2012)
;

_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          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 The structure consists of a coordination cage complex cation with the formula 
 Os4Cd4(C28H22N6)12, 16 ClO4 counter anions and one water molecule. One sixth
 of this is found in the asymmetric unit. Fifteen of the required sixteen anions
 could be located from the data (three anions with occupancies 1.0, 1.0 and 0.5
 in the asymmetric unit). Accordingly, the calculated formula does not match
 the reported formula in which all anions are accounted for.
 
 All anions were positionally disordered, and were left isotropic. All anions
 also needed weak DFIX restraints to fix the geometry.
 
 Weak global restraints were applied to all C,N,O and Cl atoms to achieve a 
 more chemically reasonable model. The water molecule occupying the central 
 cavity (occupancy 0.16667) was also left as isotropic, and the hydrogen atoms
 were not modelled. The aromatic rings of the ligands were fixed with AFIX
 restraints.

 After the cage and anions were located, a large solvent accessible void
 remained, in which disorded solvent molecules resided. This region of 
 diffuse electron density was removed with the SQUEEZE command on PLATON.
 details are given below.

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000      4962       856 ' '
   2  0.667  0.333  0.333      4960       856 ' '
   3  1.000  0.000  0.500       312        45 ' '
   4  0.333 -0.333  0.667      4960       856 ' '
   5  0.667  0.333  0.833       307        46 ' '
   6  0.333  0.667  0.167       307        46 ' '
_platon_squeeze_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19846
_refine_ls_number_parameters     618
_refine_ls_number_restraints     728
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.1527
_refine_ls_wR_factor_ref         0.4451
_refine_ls_wR_factor_gt          0.4270
_refine_ls_goodness_of_fit_ref   1.715
_refine_ls_restrained_S_all      1.709
_refine_ls_shift/su_max          0.002
_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
Os1 Os 0.61005(2) 1.02066(2) 0.10686(2) 0.0873(2) Uani 0.5 1 d . . P A 1
Cd1 Cd 0.61005(2) 1.02066(2) 0.10686(2) 0.0873(2) Uani 0.5 1 d . . P A 2
Os2 Os 0.3333 0.6667 -0.00802(2) 0.0888(3) Uani 0.5 3 d S T P B 1
Cd2 Cd 0.3333 0.6667 -0.00802(2) 0.0888(3) Uani 0.5 3 d S T P B 2
N11A N 0.5842(2) 1.0683(2) 0.12955(11) 0.114(2) Uani 1 1 d G U . . .
C12A C 0.5386(2) 1.0686(2) 0.12187(10) 0.105(2) Uani 1 1 d G U . A .
C13A C 0.5194(2) 1.0961(3) 0.13551(13) 0.118(3) Uani 1 1 d G U . A .
H13A H 0.4882 1.0963 0.1303 0.141 Uiso 1 1 calc R U . . .
C14A C 0.5458(3) 1.1233(3) 0.15682(12) 0.127(3) Uani 1 1 d G U . A .
H14A H 0.5327 1.1421 0.1661 0.152 Uiso 1 1 calc R U . . .
C15A C 0.5914(3) 1.1230(3) 0.16449(10) 0.134(3) Uani 1 1 d G U . A .
H15A H 0.6094 1.1415 0.1791 0.161 Uiso 1 1 calc R U . . .
C16A C 0.6106(2) 1.0955(3) 0.15086(12) 0.121(3) Uani 1 1 d G U . A .
H16A H 0.6418 1.0953 0.1561 0.145 Uiso 1 1 calc R U . . .
N21A N 0.5127(3) 0.9925(3) 0.06591(10) 0.122(2) Uani 1 1 d G U . . .
N22A N 0.5402(2) 1.0140(3) 0.08847(11) 0.114(2) Uani 1 1 d G U . . .
C23A C 0.5174(3) 1.0419(3) 0.10002(10) 0.113(2) Uani 1 1 d G U . . .
C24A C 0.4758(3) 1.0376(3) 0.08459(14) 0.115(2) Uani 1 1 d G U . . .
H24A H 0.4537 1.0525 0.0878 0.138 Uiso 1 1 calc R U . . .
C25A C 0.4729(3) 1.0071(3) 0.06351(12) 0.133(3) Uani 1 1 d G U . . .
H25A H 0.4486 0.9980 0.0501 0.160 Uiso 1 1 calc R U . . .
C26A C 0.5202(4) 0.9556(5) 0.05161(19) 0.129(3) Uani 1 1 d . U . . .
H26A H 0.5585 0.9665 0.0523 0.155 Uiso 1 1 calc R U . . .
H26B H 0.5117 0.9588 0.0342 0.155 Uiso 1 1 calc R U . . .
N31A N 0.3365(3) 0.6035(3) -0.03003(12) 0.126(3) Uani 1 1 d G U . . .
C32A C 0.3744(3) 0.5899(3) -0.02315(12) 0.121(3) Uani 1 1 d G U . B .
C33A C 0.3777(3) 0.5498(4) -0.03572(16) 0.150(4) Uani 1 1 d G U . B .
H33A H 0.4035 0.5405 -0.0310 0.179 Uiso 1 1 calc R U . . .
C34A C 0.3431(4) 0.5233(3) -0.05517(17) 0.173(4) Uani 1 1 d G U . B .
H34A H 0.3453 0.4959 -0.0638 0.208 Uiso 1 1 calc R U . . .
C35A C 0.3052(4) 0.5369(4) -0.06205(14) 0.171(4) Uani 1 1 d G U . B .
H35A H 0.2816 0.5188 -0.0753 0.205 Uiso 1 1 calc R U . . .
C36A C 0.3019(3) 0.5770(3) -0.04948(13) 0.150(4) Uani 1 1 d G U . B .
H36A H 0.2760 0.5863 -0.0542 0.180 Uiso 1 1 calc R U . . .
N41A N 0.4279(2) 0.6717(2) 0.03025(11) 0.123(2) Uani 1 1 d G U . . .
N42A N 0.3920(2) 0.6508(2) 0.01003(11) 0.111(2) Uani 1 1 d G U . . .
C43A C 0.4036(2) 0.6154(3) -0.00320(11) 0.110(2) Uani 1 1 d G U . . .
C44A C 0.4467(3) 0.6145(3) 0.00884(14) 0.123(3) Uani 1 1 d G U . . .
H44A H 0.4626 0.5943 0.0039 0.148 Uiso 1 1 calc R U . . .
C45A C 0.4617(2) 0.6493(3) 0.02951(13) 0.122(3) Uani 1 1 d G U . . .
H45A H 0.4895 0.6563 0.0409 0.147 Uiso 1 1 calc R U . . .
C46A C 0.4289(4) 0.7102(5) 0.0470(2) 0.128(3) Uani 1 1 d . U . . .
H46A H 0.4401 0.7043 0.0634 0.153 Uiso 1 1 calc R U . . .
H46B H 0.3922 0.7040 0.0487 0.153 Uiso 1 1 calc R U . . .
C51A C 0.4890(2) 0.89854(18) 0.05868(10) 0.123(3) Uani 1 1 d G U . . .
C52A C 0.4557(2) 0.8855(2) 0.07913(10) 0.121(3) Uani 1 1 d G U . . .
H52A H 0.4538 0.9127 0.0881 0.146 Uiso 1 1 calc R U . . .
C53A C 0.4253(2) 0.8326(3) 0.08650(9) 0.124(3) Uani 1 1 d G U . . .
H53A H 0.4026 0.8237 0.1005 0.148 Uiso 1 1 calc R U . . .
C54A C 0.42815(19) 0.7928(2) 0.07341(9) 0.130(3) Uani 1 1 d G U . . .
H54A H 0.4074 0.7567 0.0784 0.156 Uiso 1 1 calc R U . . .
C55A C 0.46142(14) 0.80592(17) 0.05296(7) 0.125(3) Uani 1 1 d G U . . .
C56A C 0.49185(14) 0.85877(17) 0.04560(7) 0.124(3) Uani 1 1 d G U . . .
C61A C 0.52512(19) 0.8718(2) 0.02515(9) 0.130(3) Uani 1 1 d G U . . .
H61A H 0.5459 0.9080 0.0201 0.156 Uiso 1 1 calc R U . . .
C62A C 0.5280(2) 0.8321(3) 0.01206(9) 0.136(3) Uani 1 1 d G U . . .
H62A H 0.5507 0.8410 -0.0019 0.163 Uiso 1 1 calc R U . . .
C63A C 0.4975(2) 0.7792(2) 0.01943(11) 0.134(3) Uani 1 1 d G U . . .
H63A H 0.4995 0.7520 0.0105 0.161 Uiso 1 1 calc R U . . .
C64A C 0.4643(2) 0.76615(18) 0.03988(10) 0.121(3) Uani 1 1 d G U . . .
N11B N 0.6617(3) 1.0906(2) 0.08302(12) 0.134(3) Uani 1 1 d G U . . .
C12B C 0.7147(3) 1.1205(3) 0.09023(12) 0.130(3) Uani 1 1 d G U . A .
C13B C 0.7508(3) 1.1625(3) 0.07559(17) 0.159(4) Uani 1 1 d G U . A .
H13B H 0.7871 1.1829 0.0805 0.191 Uiso 1 1 calc R U . . .
C14B C 0.7340(4) 1.1746(3) 0.05375(16) 0.176(5) Uani 1 1 d G U . A .
H14B H 0.7587 1.2034 0.0437 0.211 Uiso 1 1 calc R U . . .
C15B C 0.6810(4) 1.1448(3) 0.04654(13) 0.177(5) Uani 1 1 d G U . A .
H15B H 0.6694 1.1531 0.0316 0.212 Uiso 1 1 calc R U . . .
C16B C 0.6448(3) 1.1028(3) 0.06118(15) 0.157(4) Uani 1 1 d G U . A .
H16B H 0.6086 1.0824 0.0563 0.189 Uiso 1 1 calc R U . . .
N21B N 0.7132(3) 1.0497(2) 0.14478(11) 0.127(2) Uani 1 1 d G U . . .
N22B N 0.6901(2) 1.0578(2) 0.12326(12) 0.112(2) Uani 1 1 d G U . . .
C23B C 0.7302(3) 1.1033(3) 0.11078(12) 0.126(3) Uani 1 1 d G U . . .
C24B C 0.7781(2) 1.1233(3) 0.12457(16) 0.140(4) Uani 1 1 d G U . . .
H24B H 0.8114 1.1536 0.1205 0.168 Uiso 1 1 calc R U . . .
C25B C 0.7676(3) 1.0901(3) 0.14558(14) 0.134(3) Uani 1 1 d G U . . .
H25B H 0.7925 1.0943 0.1580 0.160 Uiso 1 1 calc R U . . .
C26B C 0.6848(5) 1.0050(4) 0.16059(18) 0.118(3) Uani 1 1 d . U . . .
H26C H 0.6478 0.9978 0.1621 0.142 Uiso 1 1 calc R U . . .
H26D H 0.7012 1.0146 0.1772 0.142 Uiso 1 1 calc R U . . .
N31B N 0.6240(2) 0.9628(2) 0.08502(11) 0.110(2) Uani 1 1 d G U . . .
C32B C 0.5978(2) 0.9104(3) 0.09331(10) 0.100(2) Uani 1 1 d G U . A .
C33B C 0.6029(3) 0.8717(2) 0.08042(14) 0.123(3) Uani 1 1 d G U . A .
H33B H 0.5850 0.8359 0.0861 0.147 Uiso 1 1 calc R U . . .
C34B C 0.6342(3) 0.8854(3) 0.05924(14) 0.145(3) Uani 1 1 d G U . A .
H34B H 0.6377 0.8589 0.0504 0.174 Uiso 1 1 calc R U . . .
C35B C 0.6604(3) 0.9378(4) 0.05095(12) 0.150(3) Uani 1 1 d G U . A .
H35B H 0.6818 0.9472 0.0365 0.180 Uiso 1 1 calc R U . . .
C36B C 0.6553(3) 0.9765(3) 0.06384(12) 0.132(3) Uani 1 1 d G U . A .
H36B H 0.6732 1.0123 0.0582 0.159 Uiso 1 1 calc R U . . .
N41B N 0.5393(2) 0.9230(3) 0.14973(10) 0.114(2) Uani 1 1 d G U . . .
N42B N 0.5693(2) 0.94375(18) 0.12771(10) 0.1010(18) Uani 1 1 d G U . . .
C43B C 0.5704(3) 0.9013(2) 0.11514(10) 0.101(2) Uani 1 1 d G U . . .
C44B C 0.5411(3) 0.85431(19) 0.12940(14) 0.116(3) Uani 1 1 d G U . . .
H44B H 0.5354 0.8199 0.1253 0.139 Uiso 1 1 calc R U . . .
C45B C 0.5218(3) 0.8677(2) 0.15078(12) 0.121(3) Uani 1 1 d G U . . .
H45B H 0.5010 0.8438 0.1635 0.146 Uiso 1 1 calc R U . . .
C46B C 0.5266(4) 0.9543(5) 0.16603(17) 0.119(3) Uani 1 1 d . U . . .
H46C H 0.5568 0.9914 0.1660 0.142 Uiso 1 1 calc R U . . .
H46D H 0.5232 0.9403 0.1830 0.142 Uiso 1 1 calc R U . . .
C51B C 0.6828(2) 0.95225(16) 0.15230(9) 0.103(2) Uani 1 1 d G U . . .
C52B C 0.7089(2) 0.9504(2) 0.13108(8) 0.113(2) Uani 1 1 d G U . . .
H52B H 0.7287 0.9816 0.1214 0.136 Uiso 1 1 calc R U . . .
C53B C 0.7061(2) 0.9030(2) 0.12403(7) 0.116(2) Uani 1 1 d G U . . .
H53B H 0.7239 0.9017 0.1095 0.139 Uiso 1 1 calc R U . . .
C54B C 0.6772(2) 0.8573(2) 0.13821(7) 0.108(2) Uani 1 1 d G U . . .
H54B H 0.6753 0.8249 0.1334 0.130 Uiso 1 1 calc R U . . .
C55B C 0.65112(15) 0.85915(15) 0.15943(6) 0.0979(19) Uani 1 1 d G U . . .
C56B C 0.65394(15) 0.90661(14) 0.16647(6) 0.102(2) Uani 1 1 d G U . . .
C61B C 0.6279(2) 0.90843(18) 0.18769(8) 0.111(2) Uani 1 1 d G U . . .
H61B H 0.6298 0.9409 0.1925 0.133 Uiso 1 1 calc R U . . .
C62B C 0.5990(2) 0.8628(2) 0.20187(7) 0.111(2) Uani 1 1 d G U . . .
H62B H 0.5811 0.8640 0.2164 0.133 Uiso 1 1 calc R U . . .
C63B C 0.5961(2) 0.81533(18) 0.19483(8) 0.110(2) Uani 1 1 d G U . . .
H63B H 0.5764 0.7841 0.2045 0.132 Uiso 1 1 calc R U . . .
C64B C 0.6222(2) 0.81351(15) 0.17361(8) 0.099(2) Uani 1 1 d G U . . .
Cl1 Cl 0.5691(2) 0.5944(2) 0.00052(9) 0.1225(16) Uiso 0.635(7) 1 d D U P C 1
O11 O 0.5791(5) 0.5545(4) 0.0091(2) 0.155(4) Uiso 0.635(7) 1 d D U P C 1
O12 O 0.6104(4) 0.6290(4) -0.0154(2) 0.140(4) Uiso 0.635(7) 1 d D U P C 1
O13 O 0.5662(5) 0.6242(5) 0.02086(18) 0.150(4) Uiso 0.635(7) 1 d D U P C 1
O14 O 0.5204(3) 0.5713(4) -0.0124(2) 0.141(4) Uiso 0.635(7) 1 d D U P C 1
Cl1' Cl 0.5958(2) 0.6289(3) 0.00774(11) 0.098(2) Uiso 0.365(7) 1 d D U P C 2
O11' O 0.5867(8) 0.6665(7) 0.0189(4) 0.164(7) Uiso 0.365(7) 1 d D U P C 2
O12' O 0.6312(7) 0.6506(8) -0.0124(3) 0.154(7) Uiso 0.365(7) 1 d D U P C 2
O13' O 0.6160(8) 0.6061(8) 0.0245(3) 0.163(6) Uiso 0.365(7) 1 d D U P C 2
O14' O 0.5467(6) 0.5863(6) -0.0019(4) 0.154(5) Uiso 0.365(7) 1 d D U P C 2
Cl2 Cl 0.8978(3) 0.2778(2) 0.10703(11) 0.1280(19) Uiso 0.552(9) 1 d D U P D 1
O21 O 0.9529(4) 0.3119(5) 0.1084(3) 0.172(6) Uiso 0.552(9) 1 d D U P D 1
O22 O 0.8752(7) 0.2687(8) 0.1310(2) 0.219(6) Uiso 0.552(9) 1 d D U P D 1
O23 O 0.8860(7) 0.2285(4) 0.0967(3) 0.190(7) Uiso 0.552(9) 1 d D U P D 1
O24 O 0.8743(7) 0.3009(7) 0.0924(3) 0.204(6) Uiso 0.552(9) 1 d D U P D 1
Cl2' Cl 0.8752(3) 0.2833(2) 0.11192(11) 0.1035(19) Uiso 0.448(9) 1 d D U P D 2
O21' O 0.8402(7) 0.3035(8) 0.1127(4) 0.207(8) Uiso 0.448(9) 1 d D U P D 2
O22' O 0.8638(9) 0.2463(8) 0.1309(3) 0.223(9) Uiso 0.448(9) 1 d D U P D 2
O23' O 0.8700(9) 0.2582(9) 0.0887(3) 0.210(7) Uiso 0.448(9) 1 d D U P D 2
O24' O 0.9282(5) 0.3259(6) 0.1143(4) 0.186(6) Uiso 0.448(9) 1 d D U P D 2
Cl3 Cl 0.5357(4) 0.7200(5) 0.0985(2) 0.149(4) Uiso 0.279(6) 1 d D U P E 1
O31 O 0.5391(9) 0.7614(9) 0.0833(4) 0.163(7) Uiso 0.279(6) 1 d D U P E 1
O32 O 0.5848(5) 0.7353(10) 0.1094(4) 0.146(7) Uiso 0.279(6) 1 d D U P E 1
O33 O 0.4958(4) 0.7073(4) 0.11623(19) 0.052(3) Uiso 0.279(6) 1 d D U P E 1
O34 O 0.5205(10) 0.6746(8) 0.0833(4) 0.215(11) Uiso 0.279(6) 1 d D U P E 1
Cl3' Cl 0.5728(5) 0.7261(5) 0.0883(2) 0.120(4) Uiso 0.221(6) 1 d D U P E 2
O31' O 0.5662(12) 0.7522(11) 0.1090(4) 0.132(6) Uiso 0.221(6) 1 d D U P E 2
O32' O 0.5260(9) 0.6762(8) 0.0852(7) 0.217(12) Uiso 0.221(6) 1 d D U P E 2
O33' O 0.6161(10) 0.7181(13) 0.0927(6) 0.167(10) Uiso 0.221(6) 1 d D U P E 2
O34' O 0.5820(14) 0.7569(12) 0.0670(4) 0.166(10) Uiso 0.221(6) 1 d D U P E 2
O1S O 0.3333 0.6667 0.0976(7) 0.164(11) Uiso 0.5 3 d S . 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
Os1 N22A 2.176(5) . ?
Os1 N22B 2.197(5) . ?
Os1 N11B 2.231(6) . ?
Os1 N42B 2.237(4) . ?
Os1 N11A 2.239(5) . ?
Os1 N31B 2.248(5) . ?
Os2 N42A 2.201(11) 2_665 ?
Os2 N42A 2.201(12) 3_565 ?
Os2 N42A 2.201(5) . ?
Os2 N31A 2.225(5) . ?
Os2 N31A 2.225(5) 3_565 ?
Os2 N31A 2.225(5) 2_665 ?
N11A C12A 1.3900 . ?
N11A C16A 1.3900 . ?
C12A C23A 1.379(7) . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C13A H13A 0.9500 . ?
C14A C15A 1.3900 . ?
C14A H14A 0.9500 . ?
C15A C16A 1.3900 . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
N21A N22A 1.4200 . ?
N21A C25A 1.4200 . ?
N21A C26A 1.421(12) . ?
N22A C23A 1.4200 . ?
C23A C24A 1.4200 . ?
C24A C25A 1.4200 . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
C26A C51A 1.485(12) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
N31A C32A 1.3900 . ?
N31A C36A 1.3900 . ?
C32A C43A 1.343(8) . ?
C32A C33A 1.3900 . ?
C33A C34A 1.3900 . ?
C33A H33A 0.9500 . ?
C34A C35A 1.3900 . ?
C34A H34A 0.9500 . ?
C35A C36A 1.3900 . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
N41A N42A 1.4200 . ?
N41A C45A 1.4200 . ?
N41A C46A 1.427(11) . ?
N42A C43A 1.4200 . ?
C43A C44A 1.4200 . ?
C44A C45A 1.4200 . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9500 . ?
C46A C64A 1.472(12) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C51A C52A 1.3900 . ?
C51A C56A 1.3900 . ?
C52A C53A 1.3900 . ?
C52A H52A 0.9500 . ?
C53A C54A 1.3900 . ?
C53A H53A 0.9500 . ?
C54A C55A 1.3900 . ?
C54A H54A 0.9500 . ?
C55A C56A 1.3900 . ?
C55A C64A 1.3900 . ?
C56A C61A 1.3900 . ?
C61A C62A 1.3900 . ?
C61A H61A 0.9500 . ?
C62A C63A 1.3900 . ?
C62A H62A 0.9500 . ?
C63A C64A 1.3900 . ?
C63A H63A 0.9500 . ?
N11B C12B 1.3900 . ?
N11B C16B 1.3900 . ?
C12B C23B 1.382(7) . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C13B H13B 0.9500 . ?
C14B C15B 1.3900 . ?
C14B H14B 0.9500 . ?
C15B C16B 1.3900 . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
N21B N22B 1.4200 . ?
N21B C25B 1.4200 . ?
N21B C26B 1.421(11) . ?
N22B C23B 1.4200 . ?
C23B C24B 1.4200 . ?
C24B C25B 1.4200 . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
C26B C51B 1.566(12) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
N31B C32B 1.3900 . ?
N31B C36B 1.3900 . ?
C32B C43B 1.374(7) . ?
C32B C33B 1.3900 . ?
C33B C34B 1.3900 . ?
C33B H33B 0.9500 . ?
C34B C35B 1.3900 . ?
C34B H34B 0.9500 . ?
C35B C36B 1.3900 . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
N41B C45B 1.4200 . ?
N41B N42B 1.4200 . ?
N41B C46B 1.440(11) . ?
N42B C43B 1.4200 . ?
C43B C44B 1.4200 . ?
C44B C45B 1.4200 . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
C46B C64B 1.540(17) 15 ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C51B C52B 1.3900 . ?
C51B C56B 1.3900 . ?
C52B C53B 1.3900 . ?
C52B H52B 0.9500 . ?
C53B C54B 1.3900 . ?
C53B H53B 0.9500 . ?
C54B C55B 1.3900 . ?
C54B H54B 0.9500 . ?
C55B C56B 1.3900 . ?
C55B C64B 1.3900 . ?
C56B C61B 1.3900 . ?
C61B C62B 1.3900 . ?
C61B H61B 0.9500 . ?
C62B C63B 1.3900 . ?
C62B H62B 0.9500 . ?
C63B C64B 1.3900 . ?
C63B H63B 0.9500 . ?
C64B C46B 1.540(11) 14_455 ?
Cl1 O12 1.405(7) . ?
Cl1 O11 1.407(7) . ?
Cl1 O14 1.411(7) . ?
Cl1 O13 1.426(7) . ?
Cl1' O11' 1.382(8) . ?
Cl1' O13' 1.410(8) . ?
Cl1' O12' 1.412(8) . ?
Cl1' O14' 1.437(8) . ?
Cl2 O21 1.398(8) . ?
Cl2 O23 1.410(8) . ?
Cl2 O24 1.412(8) . ?
Cl2 O22 1.420(8) . ?
Cl2' O22' 1.400(8) . ?
Cl2' O21' 1.401(8) . ?
Cl2' O24' 1.416(8) . ?
Cl2' O23' 1.423(8) . ?
Cl3 O32 1.393(8) . ?
Cl3 O33 1.404(8) . ?
Cl3 O31 1.417(8) . ?
Cl3 O34 1.421(9) . ?
Cl3' O34' 1.402(9) . ?
Cl3' O33' 1.406(9) . ?
Cl3' O31' 1.413(9) . ?
Cl3' O32' 1.414(9) . ?

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
N22A Os1 N22B 159.3(2) . . ?
N22A Os1 N11B 89.3(3) . . ?
N22B Os1 N11B 74.0(2) . . ?
N22A Os1 N42B 97.9(3) . . ?
N22B Os1 N42B 100.8(2) . . ?
N11B Os1 N42B 167.7(3) . . ?
N22A Os1 N11A 73.8(2) . . ?
N22B Os1 N11A 94.2(3) . . ?
N11B Os1 N11A 92.0(3) . . ?
N42B Os1 N11A 99.5(2) . . ?
N22A Os1 N31B 101.6(2) . . ?
N22B Os1 N31B 92.2(2) . . ?
N11B Os1 N31B 94.9(3) . . ?
N42B Os1 N31B 74.0(2) . . ?
N11A Os1 N31B 171.7(2) . . ?
N42A Os2 N42A 101.8(5) 2_665 3_565 ?
N42A Os2 N42A 101.8(5) 2_665 . ?
N42A Os2 N42A 101.8(4) 3_565 . ?
N42A Os2 N31A 166.3(5) 2_665 . ?
N42A Os2 N31A 91.7(5) 3_565 . ?
N42A Os2 N31A 73.2(2) . . ?
N42A Os2 N31A 91.7(5) 2_665 3_565 ?
N42A Os2 N31A 73.2(5) 3_565 3_565 ?
N42A Os2 N31A 166.3(2) . 3_565 ?
N31A Os2 N31A 94.0(3) . 3_565 ?
N42A Os2 N31A 73.2(5) 2_665 2_665 ?
N42A Os2 N31A 166.3(5) 3_565 2_665 ?
N42A Os2 N31A 91.7(2) . 2_665 ?
N31A Os2 N31A 94.0(3) . 2_665 ?
N31A Os2 N31A 94.0(3) 3_565 2_665 ?
C12A N11A C16A 120.0 . . ?
C12A N11A Os1 116.9(3) . . ?
C16A N11A Os1 123.0(3) . . ?
C23A C12A N11A 114.3(5) . . ?
C23A C12A C13A 125.7(5) . . ?
N11A C12A C13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C15A C16A N11A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
N11A C16A H16A 120.0 . . ?
N22A N21A C25A 108.0 . . ?
N22A N21A C26A 122.4(7) . . ?
C25A N21A C26A 128.8(6) . . ?
N21A N22A C23A 108.0 . . ?
N21A N22A Os1 136.4(4) . . ?
C23A N22A Os1 115.3(4) . . ?
C12A C23A C24A 132.4(5) . . ?
C12A C23A N22A 119.5(5) . . ?
C24A C23A N22A 108.0 . . ?
C23A C24A C25A 108.0 . . ?
C23A C24A H24A 126.0 . . ?
C25A C24A H24A 126.0 . . ?
N21A C25A C24A 108.0 . . ?
N21A C25A H25A 126.0 . . ?
C24A C25A H25A 126.0 . . ?
N21A C26A C51A 117.4(8) . . ?
N21A C26A H26A 107.9 . . ?
C51A C26A H26A 107.9 . . ?
N21A C26A H26B 107.9 . . ?
C51A C26A H26B 107.9 . . ?
H26A C26A H26B 107.2 . . ?
C32A N31A C36A 120.0 . . ?
C32A N31A Os2 117.0(4) . . ?
C36A N31A Os2 123.0(4) . . ?
C43A C32A C33A 124.5(6) . . ?
C43A C32A N31A 115.3(6) . . ?
C33A C32A N31A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C36A C35A C34A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C35A C36A N31A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
N31A C36A H36A 120.0 . . ?
N42A N41A C45A 108.0 . . ?
N42A N41A C46A 123.2(7) . . ?
C45A N41A C46A 128.8(7) . . ?
C43A N42A N41A 108.0 . . ?
C43A N42A Os2 114.4(3) . . ?
N41A N42A Os2 136.9(3) . . ?
C32A C43A C44A 132.5(6) . . ?
C32A C43A N42A 119.5(6) . . ?
C44A C43A N42A 108.0 . . ?
C43A C44A C45A 108.0 . . ?
C43A C44A H44A 126.0 . . ?
C45A C44A H44A 126.0 . . ?
C44A C45A N41A 108.0 . . ?
C44A C45A H45A 126.0 . . ?
N41A C45A H45A 126.0 . . ?
N41A C46A C64A 115.3(7) . . ?
N41A C46A H46A 108.5 . . ?
C64A C46A H46A 108.5 . . ?
N41A C46A H46B 108.5 . . ?
C64A C46A H46B 108.5 . . ?
H46A C46A H46B 107.5 . . ?
C52A C51A C56A 120.0 . . ?
C52A C51A C26A 117.5(5) . . ?
C56A C51A C26A 122.5(5) . . ?
C51A C52A C53A 120.0 . . ?
C51A C52A H52A 120.0 . . ?
C53A C52A H52A 120.0 . . ?
C52A C53A C54A 120.0 . . ?
C52A C53A H53A 120.0 . . ?
C54A C53A H53A 120.0 . . ?
C53A C54A C55A 120.0 . . ?
C53A C54A H54A 120.0 . . ?
C55A C54A H54A 120.0 . . ?
C56A C55A C54A 120.0 . . ?
C56A C55A C64A 120.0 . . ?
C54A C55A C64A 120.0 . . ?
C55A C56A C61A 120.0 . . ?
C55A C56A C51A 120.0 . . ?
C61A C56A C51A 120.0 . . ?
C56A C61A C62A 120.0 . . ?
C56A C61A H61A 120.0 . . ?
C62A C61A H61A 120.0 . . ?
C63A C62A C61A 120.0 . . ?
C63A C62A H62A 120.0 . . ?
C61A C62A H62A 120.0 . . ?
C62A C63A C64A 120.0 . . ?
C62A C63A H63A 120.0 . . ?
C64A C63A H63A 120.0 . . ?
C63A C64A C55A 120.0 . . ?
C63A C64A C46A 120.9(5) . . ?
C55A C64A C46A 118.9(5) . . ?
C12B N11B C16B 120.0 . . ?
C12B N11B Os1 115.7(4) . . ?
C16B N11B Os1 124.1(4) . . ?
C23B C12B C13B 122.3(6) . . ?
C23B C12B N11B 117.3(6) . . ?
C13B C12B N11B 120.0 . . ?
C12B C13B C14B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C14B C13B H13B 120.0 . . ?
C15B C14B C13B 120.0 . . ?
C15B C14B H14B 120.0 . . ?
C13B C14B H14B 120.0 . . ?
C16B C15B C14B 120.0 . . ?
C16B C15B H15B 120.0 . . ?
C14B C15B H15B 120.0 . . ?
C15B C16B N11B 120.0 . . ?
C15B C16B H16B 120.0 . . ?
N11B C16B H16B 120.0 . . ?
N22B N21B C25B 108.0 . . ?
N22B N21B C26B 122.6(6) . . ?
C25B N21B C26B 129.2(6) . . ?
N21B N22B C23B 108.0 . . ?
N21B N22B Os1 136.0(3) . . ?
C23B N22B Os1 115.9(3) . . ?
C12B C23B C24B 134.8(6) . . ?
C12B C23B N22B 117.0(6) . . ?
C24B C23B N22B 108.0 . . ?
C23B C24B C25B 108.0 . . ?
C23B C24B H24B 126.0 . . ?
C25B C24B H24B 126.0 . . ?
C24B C25B N21B 108.0 . . ?
C24B C25B H25B 126.0 . . ?
N21B C25B H25B 126.0 . . ?
N21B C26B C51B 116.1(8) . . ?
N21B C26B H26C 108.3 . . ?
C51B C26B H26C 108.3 . . ?
N21B C26B H26D 108.3 . . ?
C51B C26B H26D 108.3 . . ?
H26C C26B H26D 107.4 . . ?
C32B N31B C36B 120.0 . . ?
C32B N31B Os1 116.2(3) . . ?
C36B N31B Os1 123.7(3) . . ?
C43B C32B C33B 124.1(5) . . ?
C43B C32B N31B 115.8(5) . . ?
C33B C32B N31B 120.0 . . ?
C32B C33B C34B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C36B C35B C34B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C35B C36B N31B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
N31B C36B H36B 120.0 . . ?
C45B N41B N42B 108.0 . . ?
C45B N41B C46B 129.0(6) . . ?
N42B N41B C46B 122.8(6) . . ?
C43B N42B N41B 108.0 . . ?
C43B N42B Os1 113.1(3) . . ?
N41B N42B Os1 138.8(3) . . ?
C32B C43B C44B 131.5(5) . . ?
C32B C43B N42B 120.5(5) . . ?
C44B C43B N42B 108.0 . . ?
C43B C44B C45B 108.0 . . ?
C43B C44B H44B 126.0 . . ?
C45B C44B H44B 126.0 . . ?
N41B C45B C44B 108.0 . . ?
N41B C45B H45B 126.0 . . ?
C44B C45B H45B 126.0 . . ?
N41B C46B C64B 115.6(8) . 15 ?
N41B C46B H46C 108.4 . . ?
C64B C46B H46C 108.4 15 . ?
N41B C46B H46D 108.4 . . ?
C64B C46B H46D 108.4 15 . ?
H46C C46B H46D 107.4 . . ?
C52B C51B C56B 120.0 . . ?
C52B C51B C26B 121.2(5) . . ?
C56B C51B C26B 118.8(5) . . ?
C51B C52B C53B 120.0 . . ?
C51B C52B H52B 120.0 . . ?
C53B C52B H52B 120.0 . . ?
C54B C53B C52B 120.0 . . ?
C54B C53B H53B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C53B C54B C55B 120.0 . . ?
C53B C54B H54B 120.0 . . ?
C55B C54B H54B 120.0 . . ?
C56B C55B C54B 120.0 . . ?
C56B C55B C64B 120.0 . . ?
C54B C55B C64B 120.0 . . ?
C55B C56B C61B 120.0 . . ?
C55B C56B C51B 120.0 . . ?
C61B C56B C51B 120.0 . . ?
C56B C61B C62B 120.0 . . ?
C56B C61B H61B 120.0 . . ?
C62B C61B H61B 120.0 . . ?
C63B C62B C61B 120.0 . . ?
C63B C62B H62B 120.0 . . ?
C61B C62B H62B 120.0 . . ?
C62B C63B C64B 120.0 . . ?
C62B C63B H63B 120.0 . . ?
C64B C63B H63B 120.0 . . ?
C55B C64B C63B 120.0 . . ?
C55B C64B C46B 121.5(4) . 14_455 ?
C63B C64B C46B 118.4(4) . 14_455 ?
O12 Cl1 O11 109.8(6) . . ?
O12 Cl1 O14 109.2(6) . . ?
O11 Cl1 O14 110.0(6) . . ?
O12 Cl1 O13 109.1(6) . . ?
O11 Cl1 O13 109.9(6) . . ?
O14 Cl1 O13 108.8(6) . . ?
O11' Cl1' O13' 112.1(8) . . ?
O11' Cl1' O12' 111.7(8) . . ?
O13' Cl1' O12' 109.0(8) . . ?
O11' Cl1' O14' 109.8(8) . . ?
O13' Cl1' O14' 107.3(7) . . ?
O12' Cl1' O14' 106.7(8) . . ?
O21 Cl2 O23 110.4(7) . . ?
O21 Cl2 O24 110.2(7) . . ?
O23 Cl2 O24 109.2(7) . . ?
O21 Cl2 O22 110.0(7) . . ?
O23 Cl2 O22 108.7(7) . . ?
O24 Cl2 O22 108.3(7) . . ?
O22' Cl2' O21' 110.9(8) . . ?
O22' Cl2' O24' 109.7(8) . . ?
O21' Cl2' O24' 109.3(8) . . ?
O22' Cl2' O23' 109.3(8) . . ?
O21' Cl2' O23' 109.1(8) . . ?
O24' Cl2' O23' 108.6(8) . . ?
O32 Cl3 O33 111.8(8) . . ?
O32 Cl3 O31 110.3(8) . . ?
O33 Cl3 O31 108.5(8) . . ?
O32 Cl3 O34 109.5(8) . . ?
O33 Cl3 O34 108.6(8) . . ?
O31 Cl3 O34 108.0(8) . . ?
O34' Cl3' O33' 110.0(8) . . ?
O34' Cl3' O31' 110.1(8) . . ?
O33' Cl3' O31' 109.2(8) . . ?
O34' Cl3' O32' 109.3(8) . . ?
O33' Cl3' O32' 109.2(8) . . ?
O31' Cl3' O32' 109.0(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
C16A N11A C12A C23A 177.8(6) . . . . ?
Os1 N11A C12A C23A -4.1(6) . . . . ?
C16A N11A C12A C13A 0.0 . . . . ?
Os1 N11A C12A C13A 178.1(4) . . . . ?
C23A C12A C13A C14A -177.5(7) . . . . ?
N11A C12A C13A C14A 0.0 . . . . ?
C12A C13A C14A C15A 0.0 . . . . ?
C13A C14A C15A C16A 0.0 . . . . ?
C14A C15A C16A N11A 0.0 . . . . ?
C12A N11A C16A C15A 0.0 . . . . ?
Os1 N11A C16A C15A -178.0(4) . . . . ?
C25A N21A N22A C23A 0.0 . . . . ?
C26A N21A N22A C23A -170.3(8) . . . . ?
C25A N21A N22A Os1 -172.9(7) . . . . ?
C26A N21A N22A Os1 16.8(10) . . . . ?
N11A C12A C23A C24A -171.9(6) . . . . ?
C13A C12A C23A C24A 5.7(10) . . . . ?
N11A C12A C23A N22A 4.4(7) . . . . ?
C13A C12A C23A N22A -178.0(4) . . . . ?
N21A N22A C23A C12A -177.2(7) . . . . ?
Os1 N22A C23A C12A -2.5(7) . . . . ?
N21A N22A C23A C24A 0.0 . . . . ?
Os1 N22A C23A C24A 174.6(5) . . . . ?
C12A C23A C24A C25A 176.7(9) . . . . ?
N22A C23A C24A C25A 0.0 . . . . ?
N22A N21A C25A C24A 0.0 . . . . ?
C26A N21A C25A C24A 169.4(9) . . . . ?
C23A C24A C25A N21A 0.0 . . . . ?
N22A N21A C26A C51A 83.6(10) . . . . ?
C25A N21A C26A C51A -84.5(11) . . . . ?
C36A N31A C32A C43A -176.0(7) . . . . ?
Os2 N31A C32A C43A 2.4(7) . . . . ?
C36A N31A C32A C33A 0.0 . . . . ?
Os2 N31A C32A C33A 178.4(5) . . . . ?
C43A C32A C33A C34A 175.6(8) . . . . ?
N31A C32A C33A C34A 0.0 . . . . ?
C32A C33A C34A C35A 0.0 . . . . ?
C33A C34A C35A C36A 0.0 . . . . ?
C34A C35A C36A N31A 0.0 . . . . ?
C32A N31A C36A C35A 0.0 . . . . ?
Os2 N31A C36A C35A -178.3(5) . . . . ?
C45A N41A N42A C43A 0.0 . . . . ?
C46A N41A N42A C43A 177.6(8) . . . . ?
C45A N41A N42A Os2 -169.8(6) . . . . ?
C46A N41A N42A Os2 7.7(9) . . . . ?
C33A C32A C43A C44A 7.1(10) . . . . ?
N31A C32A C43A C44A -177.0(5) . . . . ?
C33A C32A C43A N42A -171.8(5) . . . . ?
N31A C32A C43A N42A 4.0(8) . . . . ?
N41A N42A C43A C32A 179.2(7) . . . . ?
Os2 N42A C43A C32A -8.4(7) . . . . ?
N41A N42A C43A C44A 0.0 . . . . ?
Os2 N42A C43A C44A 172.4(4) . . . . ?
C32A C43A C44A C45A -179.1(9) . . . . ?
N42A C43A C44A C45A 0.0 . . . . ?
C43A C44A C45A N41A 0.0 . . . . ?
N42A N41A C45A C44A 0.0 . . . . ?
C46A N41A C45A C44A -177.4(8) . . . . ?
N42A N41A C46A C64A -89.5(9) . . . . ?
C45A N41A C46A C64A 87.6(11) . . . . ?
N21A C26A C51A C52A -1.5(11) . . . . ?
N21A C26A C51A C56A 178.0(6) . . . . ?
C56A C51A C52A C53A 0.0 . . . . ?
C26A C51A C52A C53A 179.6(7) . . . . ?
C51A C52A C53A C54A 0.0 . . . . ?
C52A C53A C54A C55A 0.0 . . . . ?
C53A C54A C55A C56A 0.0 . . . . ?
C53A C54A C55A C64A 180.0 . . . . ?
C54A C55A C56A C61A 180.0 . . . . ?
C64A C55A C56A C61A 0.0 . . . . ?
C54A C55A C56A C51A 0.0 . . . . ?
C64A C55A C56A C51A 180.0 . . . . ?
C52A C51A C56A C55A 0.0 . . . . ?
C26A C51A C56A C55A -179.5(7) . . . . ?
C52A C51A C56A C61A 180.0 . . . . ?
C26A C51A C56A C61A 0.5(7) . . . . ?
C55A C56A C61A C62A 0.0 . . . . ?
C51A C56A C61A C62A 180.0 . . . . ?
C56A C61A C62A C63A 0.0 . . . . ?
C61A C62A C63A C64A 0.0 . . . . ?
C62A C63A C64A C55A 0.0 . . . . ?
C62A C63A C64A C46A 175.7(7) . . . . ?
C56A C55A C64A C63A 0.0 . . . . ?
C54A C55A C64A C63A 180.0 . . . . ?
C56A C55A C64A C46A -175.8(7) . . . . ?
C54A C55A C64A C46A 4.2(7) . . . . ?
N41A C46A C64A C63A -5.8(12) . . . . ?
N41A C46A C64A C55A 170.0(6) . . . . ?
C16B N11B C12B C23B -173.8(8) . . . . ?
Os1 N11B C12B C23B 1.5(8) . . . . ?
C16B N11B C12B C13B 0.0 . . . . ?
Os1 N11B C12B C13B 175.3(5) . . . . ?
C23B C12B C13B C14B 173.5(9) . . . . ?
N11B C12B C13B C14B 0.0 . . . . ?
C12B C13B C14B C15B 0.0 . . . . ?
C13B C14B C15B C16B 0.0 . . . . ?
C14B C15B C16B N11B 0.0 . . . . ?
C12B N11B C16B C15B 0.0 . . . . ?
Os1 N11B C16B C15B -174.9(6) . . . . ?
C25B N21B N22B C23B 0.0 . . . . ?
C26B N21B N22B C23B -175.3(9) . . . . ?
C25B N21B N22B Os1 -176.3(7) . . . . ?
C26B N21B N22B Os1 8.5(11) . . . . ?
C13B C12B C23B C24B 10.5(12) . . . . ?
N11B C12B C23B C24B -175.8(7) . . . . ?
C13B C12B C23B N22B -175.9(5) . . . . ?
N11B C12B C23B N22B -2.3(10) . . . . ?
N21B N22B C23B C12B -175.2(9) . . . . ?
Os1 N22B C23B C12B 2.0(8) . . . . ?
N21B N22B C23B C24B 0.0 . . . . ?
Os1 N22B C23B C24B 177.1(5) . . . . ?
C12B C23B C24B C25B 173.9(11) . . . . ?
N22B C23B C24B C25B 0.0 . . . . ?
C23B C24B C25B N21B 0.0 . . . . ?
N22B N21B C25B C24B 0.0 . . . . ?
C26B N21B C25B C24B 174.9(10) . . . . ?
N22B N21B C26B C51B 82.4(10) . . . . ?
C25B N21B C26B C51B -91.8(10) . . . . ?
C36B N31B C32B C43B 176.4(6) . . . . ?
Os1 N31B C32B C43B -5.7(5) . . . . ?
C36B N31B C32B C33B 0.0 . . . . ?
Os1 N31B C32B C33B 178.0(4) . . . . ?
C43B C32B C33B C34B -176.0(6) . . . . ?
N31B C32B C33B C34B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B N31B 0.0 . . . . ?
C32B N31B C36B C35B 0.0 . . . . ?
Os1 N31B C36B C35B -177.8(4) . . . . ?
C45B N41B N42B C43B 0.0 . . . . ?
C46B N41B N42B C43B -175.1(8) . . . . ?
C45B N41B N42B Os1 175.7(6) . . . . ?
C46B N41B N42B Os1 0.6(9) . . . . ?
C33B C32B C43B C44B -1.4(8) . . . . ?
N31B C32B C43B C44B -177.6(5) . . . . ?
C33B C32B C43B N42B 177.0(4) . . . . ?
N31B C32B C43B N42B 0.8(7) . . . . ?
N41B N42B C43B C32B -178.8(7) . . . . ?
Os1 N42B C43B C32B 4.3(6) . . . . ?
N41B N42B C43B C44B 0.0 . . . . ?
Os1 N42B C43B C44B -176.9(4) . . . . ?
C32B C43B C44B C45B 178.6(8) . . . . ?
N42B C43B C44B C45B 0.0 . . . . ?
N42B N41B C45B C44B 0.0 . . . . ?
C46B N41B C45B C44B 174.7(8) . . . . ?
C43B C44B C45B N41B 0.0 . . . . ?
C45B N41B C46B C64B -86.7(11) . . . 15 ?
N42B N41B C46B C64B 87.2(10) . . . 15 ?
N21B C26B C51B C52B 2.0(10) . . . . ?
N21B C26B C51B C56B -177.5(6) . . . . ?
C56B C51B C52B C53B 0.0 . . . . ?
C26B C51B C52B C53B -179.4(6) . . . . ?
C51B C52B C53B C54B 0.0 . . . . ?
C52B C53B C54B C55B 0.0 . . . . ?
C53B C54B C55B C56B 0.0 . . . . ?
C53B C54B C55B C64B 180.0 . . . . ?
C54B C55B C56B C61B 180.0 . . . . ?
C64B C55B C56B C61B 0.0 . . . . ?
C54B C55B C56B C51B 0.0 . . . . ?
C64B C55B C56B C51B 180.0 . . . . ?
C52B C51B C56B C55B 0.0 . . . . ?
C26B C51B C56B C55B 179.5(6) . . . . ?
C52B C51B C56B C61B 180.0 . . . . ?
C26B C51B C56B C61B -0.5(6) . . . . ?
C55B C56B C61B C62B 0.0 . . . . ?
C51B C56B C61B C62B 180.0 . . . . ?
C56B C61B C62B C63B 0.0 . . . . ?
C61B C62B C63B C64B 0.0 . . . . ?
C56B C55B C64B C63B 0.0 . . . . ?
C54B C55B C64B C63B 180.0 . . . . ?
C56B C55B C64B C46B -176.2(6) . . . 14_455 ?
C54B C55B C64B C46B 3.8(6) . . . 14_455 ?
C62B C63B C64B C55B 0.0 . . . . ?
C62B C63B C64B C46B 176.3(6) . . . 14_455 ?

_refine_diff_density_max         5.987
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.189

_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_r-3_sq
_database_code_depnum_ccdc_archive 'CCDC 1413547'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C336 H266 Cl16 Co4 N72 O65 Os4'
_chemical_formula_weight         7915.91

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'
Co Co 0.3494 0.9721 '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'
Os Os -1.2165 7.6030 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   28.9579(16)
_cell_length_b                   28.9579(16)
_cell_length_c                   52.757(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     38313(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56774
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_F_000             11970
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.259
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.601
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_radiation_monochromator  Mirrors
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_device       
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_reflns_number            84474
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_av_R_equivalents  0.1349
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_limit_l_max       62
_diffrn_reflns_theta_min         2.436
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14953
_reflns_number_gt                5893
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_cell_refinement       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_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          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14953
_refine_ls_number_parameters     555
_refine_ls_number_restraints     576
_refine_ls_R_factor_all          0.2219
_refine_ls_R_factor_gt           0.1271
_refine_ls_wR_factor_ref         0.4483
_refine_ls_wR_factor_gt          0.3825
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_restrained_S_all      1.252
_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
Os1 Os 0.27874(4) 0.35679(3) 0.94072(2) 0.1094(4) Uani 0.5 1 d . . P A 1
Co1 Co 0.27874(4) 0.35679(3) 0.94072(2) 0.1094(4) Uani 0.5 1 d . . P A 2
Os2 Os 0.0000 0.0000 0.82323(3) 0.1048(6) Uani 0.5 3 d S T P B 1
Co2 Co 0.0000 0.0000 0.82323(3) 0.1048(6) Uani 0.5 3 d S T P B 2
N11A N 0.2562(4) 0.4017(3) 0.96385(19) 0.133(4) Uani 1 1 d G U . . .
C12A C 0.2102(4) 0.4016(4) 0.95616(19) 0.138(5) Uani 1 1 d G U . A .
C13A C 0.1914(4) 0.4297(5) 0.9700(2) 0.154(5) Uani 1 1 d G U . A .
H13A H 0.1600 0.4296 0.9647 0.184 Uiso 1 1 calc R U . . .
C14A C 0.2185(5) 0.4578(4) 0.9915(2) 0.158(6) Uani 1 1 d G U . A .
H14A H 0.2056 0.4769 1.0010 0.190 Uiso 1 1 calc R U . . .
C15A C 0.2645(5) 0.4579(4) 0.99923(18) 0.152(5) Uani 1 1 d G U . A .
H15A H 0.2830 0.4771 1.0140 0.182 Uiso 1 1 calc R U . . .
C16A C 0.2833(4) 0.4299(4) 0.9854(2) 0.138(5) Uani 1 1 d G U . A .
H16A H 0.3147 0.4299 0.9906 0.166 Uiso 1 1 calc R U . . .
N21A N 0.1802(5) 0.3257(4) 0.89954(19) 0.161(5) Uani 1 1 d G U . . .
N22A N 0.2095(3) 0.3482(4) 0.9222(2) 0.125(3) Uani 1 1 d G U . . .
C23A C 0.1880(5) 0.3771(4) 0.93423(19) 0.129(4) Uani 1 1 d G U . . .
C24A C 0.1454(5) 0.3726(5) 0.9191(3) 0.165(6) Uani 1 1 d G U . . .
H24A H 0.1240 0.3881 0.9226 0.198 Uiso 1 1 calc R U . . .
C25A C 0.1406(5) 0.3408(6) 0.8976(2) 0.184(7) Uani 1 1 d G U . . .
H25A H 0.1153 0.3314 0.8843 0.221 Uiso 1 1 calc R U . . .
C26A C 0.1898(8) 0.2895(7) 0.8826(4) 0.164(5) Uani 1 1 d . U . . .
H26A H 0.1799 0.2923 0.8649 0.197 Uiso 1 1 calc R U . . .
H26B H 0.2281 0.3003 0.8828 0.197 Uiso 1 1 calc R U . . .
N31A N -0.0008(4) -0.0624(3) 0.80125(17) 0.124(3) Uani 1 1 d G U . . .
C32A C 0.0373(4) -0.0762(4) 0.80778(17) 0.123(4) Uani 1 1 d G U . B .
C33A C 0.0408(4) -0.1155(5) 0.7942(2) 0.155(6) Uani 1 1 d G U . B .
H33A H 0.0668 -0.1249 0.7987 0.187 Uiso 1 1 calc R U . . .
C34A C 0.0062(5) -0.1410(4) 0.7741(2) 0.182(7) Uani 1 1 d G U . B .
H34A H 0.0086 -0.1679 0.7649 0.218 Uiso 1 1 calc R U . . .
C35A C -0.0318(5) -0.1272(5) 0.76759(18) 0.173(7) Uani 1 1 d G U . B .
H35A H -0.0555 -0.1447 0.7539 0.207 Uiso 1 1 calc R U . . .
C36A C -0.0353(4) -0.0879(5) 0.7812(2) 0.141(5) Uani 1 1 d G U . B .
H36A H -0.0613 -0.0785 0.7767 0.170 Uiso 1 1 calc R U . . .
N41A N 0.0915(4) 0.0049(3) 0.86281(15) 0.120(3) Uani 1 1 d G U . . .
N42A N 0.0568(3) -0.0154(4) 0.84161(17) 0.117(3) Uani 1 1 d G U . . .
C43A C 0.0690(4) -0.0505(4) 0.82824(15) 0.123(4) Uani 1 1 d G U . . .
C44A C 0.1112(4) -0.0520(4) 0.84118(19) 0.119(4) Uani 1 1 d G U . . .
H44A H 0.1273 -0.0723 0.8364 0.143 Uiso 1 1 calc R U . . .
C45A C 0.1252(3) -0.0177(4) 0.86255(16) 0.114(4) Uani 1 1 d G U . . .
H45A H 0.1522 -0.0111 0.8746 0.137 Uiso 1 1 calc R U . . .
C46A C 0.0940(6) 0.0428(6) 0.8802(3) 0.122(4) Uani 1 1 d . U . . .
H46A H 0.1071 0.0373 0.8966 0.146 Uiso 1 1 calc R U . . .
H46B H 0.0575 0.0366 0.8829 0.146 Uiso 1 1 calc R U . . .
C51A C 0.1569(3) 0.2331(2) 0.89171(15) 0.126(4) Uani 1 1 d G U . . .
C52A C 0.1228(3) 0.2201(3) 0.91235(15) 0.134(4) Uani 1 1 d G U . . .
H52A H 0.1213 0.2475 0.9216 0.160 Uiso 1 1 calc R U . . .
C53A C 0.0910(3) 0.1672(4) 0.91951(13) 0.125(4) Uani 1 1 d G U . . .
H53A H 0.0677 0.1583 0.9336 0.150 Uiso 1 1 calc R U . . .
C54A C 0.0932(3) 0.1271(3) 0.90602(13) 0.122(4) Uani 1 1 d G U . . .
H54A H 0.0715 0.0909 0.9109 0.147 Uiso 1 1 calc R U . . .
C55A C 0.1274(2) 0.1400(2) 0.88538(11) 0.119(4) Uani 1 1 d G U . . .
C56A C 0.1592(2) 0.1930(2) 0.87823(11) 0.119(4) Uani 1 1 d G U . . .
C61A C 0.1933(3) 0.2060(3) 0.85759(14) 0.123(4) Uani 1 1 d G U . . .
H61A H 0.2151 0.2422 0.8527 0.147 Uiso 1 1 calc R U . . .
C62A C 0.1956(3) 0.1659(4) 0.84410(14) 0.155(6) Uani 1 1 d G U . . .
H62A H 0.2189 0.1747 0.8300 0.186 Uiso 1 1 calc R U . . .
C63A C 0.1638(3) 0.1129(3) 0.85126(15) 0.132(5) Uani 1 1 d G U . . .
H63A H 0.1653 0.0855 0.8420 0.159 Uiso 1 1 calc R U . . .
C64A C 0.1296(3) 0.1000(2) 0.87190(15) 0.113(4) Uani 1 1 d G U . . .
N11B N 0.3274(4) 0.4247(3) 0.91742(18) 0.127(4) Uani 1 1 d G U . . .
C12B C 0.3809(4) 0.4529(4) 0.92424(17) 0.137(5) Uani 1 1 d G U . A .
C13B C 0.4171(3) 0.4953(4) 0.9094(2) 0.158(6) Uani 1 1 d G U . A .
H13B H 0.4536 0.5146 0.9141 0.190 Uiso 1 1 calc R U . . .
C14B C 0.3997(5) 0.5095(4) 0.8878(2) 0.172(7) Uani 1 1 d G U . A .
H14B H 0.4245 0.5385 0.8776 0.206 Uiso 1 1 calc R U . . .
C15B C 0.3462(5) 0.4813(5) 0.88093(19) 0.172(7) Uani 1 1 d G U . A .
H15B H 0.3344 0.4910 0.8661 0.207 Uiso 1 1 calc R U . . .
C16B C 0.3101(4) 0.4388(4) 0.8958(2) 0.149(5) Uani 1 1 d G U . A .
H16B H 0.2735 0.4195 0.8911 0.179 Uiso 1 1 calc R U . . .
N21B N 0.3796(4) 0.3812(3) 0.97803(16) 0.126(4) Uani 1 1 d G U . . .
N22B N 0.3555(3) 0.3899(3) 0.95650(18) 0.126(4) Uani 1 1 d G U . . .
C23B C 0.3949(4) 0.4363(4) 0.94390(17) 0.118(4) Uani 1 1 d G U . . .
C24B C 0.4433(3) 0.4563(4) 0.9577(2) 0.145(5) Uani 1 1 d G U . . .
H24B H 0.4763 0.4870 0.9535 0.174 Uiso 1 1 calc R U . . .
C25B C 0.4339(4) 0.4222(4) 0.9787(2) 0.148(5) Uani 1 1 d G U . . .
H25B H 0.4594 0.4262 0.9912 0.177 Uiso 1 1 calc R U . . .
C26B C 0.3504(6) 0.3377(6) 0.9943(3) 0.120(4) Uani 1 1 d . U . . .
H26C H 0.3131 0.3304 0.9952 0.144 Uiso 1 1 calc R U . . .
H26D H 0.3657 0.3474 1.0116 0.144 Uiso 1 1 calc R U . . .
N31B N 0.2958(4) 0.3053(3) 0.91846(17) 0.116(3) Uani 1 1 d G U . . .
C32B C 0.2685(3) 0.2522(4) 0.92594(16) 0.113(4) Uani 1 1 d G U . A .
C33B C 0.2743(4) 0.2143(3) 0.9123(2) 0.130(4) Uani 1 1 d G U . A .
H33B H 0.2556 0.1780 0.9174 0.156 Uiso 1 1 calc R U . . .
C34B C 0.3073(5) 0.2296(4) 0.8911(2) 0.150(5) Uani 1 1 d G U . A .
H34B H 0.3112 0.2038 0.8818 0.180 Uiso 1 1 calc R U . . .
C35B C 0.3346(4) 0.2828(5) 0.88363(18) 0.161(6) Uani 1 1 d G U . A .
H35B H 0.3571 0.2932 0.8692 0.193 Uiso 1 1 calc R U . . .
C36B C 0.3288(4) 0.3206(3) 0.8973(2) 0.144(5) Uani 1 1 d G U . A .
H36B H 0.3474 0.3569 0.8922 0.172 Uiso 1 1 calc R U . . .
N41B N 0.2072(3) 0.2616(3) 0.98299(15) 0.116(3) Uani 1 1 d G U . . .
N42B N 0.2382(3) 0.2835(3) 0.96075(17) 0.109(3) Uani 1 1 d G U . . .
C43B C 0.2410(4) 0.2420(4) 0.94781(16) 0.108(3) Uani 1 1 d G U . . .
C44B C 0.2116(4) 0.1944(3) 0.9621(2) 0.127(4) Uani 1 1 d G U . . .
H44B H 0.2068 0.1604 0.9578 0.153 Uiso 1 1 calc R U . . .
C45B C 0.1908(3) 0.2065(3) 0.98379(17) 0.120(4) Uani 1 1 d G U . . .
H45B H 0.1695 0.1820 0.9966 0.145 Uiso 1 1 calc R U . . .
C46B C 0.1941(6) 0.2912(6) 0.9979(3) 0.124(4) Uani 1 1 d . U . . .
H46C H 0.2239 0.3285 0.9970 0.148 Uiso 1 1 calc R U . . .
H46D H 0.1925 0.2789 1.0155 0.148 Uiso 1 1 calc R U . . .
C51B C 0.3500(3) 0.2864(2) 0.98591(14) 0.110(3) Uani 1 1 d G U . . .
C52B C 0.3773(3) 0.2859(3) 0.96432(14) 0.123(4) Uani 1 1 d G U . . .
H52B H 0.3967 0.3175 0.9546 0.147 Uiso 1 1 calc R U . . .
C53B C 0.3761(3) 0.2393(4) 0.95696(12) 0.130(5) Uani 1 1 d G U . . .
H53B H 0.3948 0.2390 0.9422 0.156 Uiso 1 1 calc R U . . .
C54B C 0.3477(3) 0.1931(3) 0.97121(13) 0.118(4) Uani 1 1 d G U . . .
H54B H 0.3469 0.1612 0.9662 0.141 Uiso 1 1 calc R U . . .
C55B C 0.3204(2) 0.1935(2) 0.99280(10) 0.117(4) Uani 1 1 d G U . . .
C56B C 0.3216(2) 0.2401(2) 1.00016(10) 0.116(4) Uani 1 1 d G U . . .
C61B C 0.2943(3) 0.2406(3) 1.02175(13) 0.126(4) Uani 1 1 d G U . . .
H61B H 0.2951 0.2724 1.0268 0.151 Uiso 1 1 calc R U . . .
C62B C 0.2659(3) 0.1943(3) 1.03600(12) 0.134(5) Uani 1 1 d G U . . .
H62B H 0.2472 0.1946 1.0508 0.161 Uiso 1 1 calc R U . . .
C63B C 0.2647(3) 0.1477(3) 1.02865(14) 0.119(4) Uani 1 1 d G U . . .
H63B H 0.2453 0.1161 1.0384 0.143 Uiso 1 1 calc R U . . .
C64B C 0.2920(3) 0.1473(2) 1.00705(14) 0.108(4) Uani 1 1 d G U . . .
Cl11 Cl 0.5478(3) 0.6161(3) 0.94236(13) 0.220(3) Uiso 1 1 d D . . . .
O11 O 0.5379(8) 0.5775(7) 0.9609(3) 0.339(12) Uiso 1 1 d D . . . .
O12 O 0.6002(5) 0.6603(7) 0.9456(5) 0.392(15) Uiso 1 1 d D . . . .
O13 O 0.5435(10) 0.5950(9) 0.9181(3) 0.415(17) Uiso 1 1 d D . . . .
O14 O 0.5108(8) 0.6341(9) 0.9453(4) 0.363(13) Uiso 1 1 d D . . . .
O1S O 0.0000 0.0000 0.9308(7) 0.143(12) Uiso 0.5 3 d S . P . .
Cl21 Cl 0.0539(3) 0.3009(3) 0.84043(16) 0.243(3) Uiso 1 1 d D . . . .
O21 O 0.0305(6) 0.2616(5) 0.8591(2) 0.233(7) Uiso 1 1 d D . . . .
O22 O 0.0932(6) 0.2939(7) 0.8274(3) 0.268(8) Uiso 1 1 d D . . . .
O23 O 0.0165(6) 0.2983(8) 0.8230(3) 0.351(13) Uiso 1 1 d D . . . .
O24 O 0.0801(8) 0.3520(5) 0.8520(4) 0.376(14) Uiso 1 1 d D . . . .
Cl31 Cl 0.1475(4) 0.2067(4) 0.07111(19) 0.171(4) Uiso 0.5 1 d D . P . .
O31 O 0.1293(8) 0.1746(7) 0.0492(3) 0.178(9) Uiso 0.5 1 d D . P . .
O32 O 0.1789(6) 0.1914(7) 0.0856(3) 0.130(6) Uiso 0.5 1 d D . P . .
O33 O 0.1768(9) 0.2603(5) 0.0651(4) 0.223(12) Uiso 0.5 1 d D . P . .
O34 O 0.1021(8) 0.1965(12) 0.0857(4) 0.39(3) Uiso 0.5 1 d 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
Os1 N22B 2.103(7) . ?
Os1 N11A 2.112(8) . ?
Os1 N42B 2.122(7) . ?
Os1 N22A 2.131(8) . ?
Os1 N31B 2.140(7) . ?
Os1 N11B 2.142(8) . ?
Os2 N31A 2.139(8) . ?
Os2 N31A 2.139(8) 3 ?
Os2 N31A 2.139(8) 2 ?
Os2 N42A 2.139(7) . ?
Os2 N42A 2.139(16) 2 ?
Os2 N42A 2.139(15) 3 ?
N11A C12A 1.3900 . ?
N11A C16A 1.3900 . ?
C12A C23A 1.341(12) . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C13A H13A 0.9500 . ?
C14A C15A 1.3900 . ?
C14A H14A 0.9500 . ?
C15A C16A 1.3900 . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
N21A N22A 1.4200 . ?
N21A C25A 1.4200 . ?
N21A C26A 1.509(19) . ?
N22A C23A 1.4200 . ?
C23A C24A 1.4200 . ?
C24A C25A 1.4200 . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
C26A C51A 1.502(18) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
N31A C32A 1.3900 . ?
N31A C36A 1.3900 . ?
C32A C43A 1.371(10) . ?
C32A C33A 1.3900 . ?
C33A C34A 1.3900 . ?
C33A H33A 0.9500 . ?
C34A C35A 1.3900 . ?
C34A H34A 0.9500 . ?
C35A C36A 1.3900 . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
N41A C46A 1.403(15) . ?
N41A C45A 1.4200 . ?
N41A N42A 1.4200 . ?
N42A C43A 1.4200 . ?
C43A C44A 1.4200 . ?
C44A C45A 1.4200 . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9500 . ?
C46A C64A 1.514(15) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C51A C52A 1.3900 . ?
C51A C56A 1.3900 . ?
C52A C53A 1.3900 . ?
C52A H52A 0.9500 . ?
C53A C54A 1.3900 . ?
C53A H53A 0.9500 . ?
C54A C55A 1.3900 . ?
C54A H54A 0.9500 . ?
C55A C56A 1.3900 . ?
C55A C64A 1.3900 . ?
C56A C61A 1.3900 . ?
C61A C62A 1.3900 . ?
C61A H61A 0.9500 . ?
C62A C63A 1.3900 . ?
C62A H62A 0.9500 . ?
C63A C64A 1.3900 . ?
C63A H63A 0.9500 . ?
N11B C12B 1.3900 . ?
N11B C16B 1.3900 . ?
C12B C23B 1.291(10) . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C13B H13B 0.9500 . ?
C14B C15B 1.3900 . ?
C14B H14B 0.9500 . ?
C15B C16B 1.3900 . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
N21B C26B 1.405(15) . ?
N21B N22B 1.4200 . ?
N21B C25B 1.4200 . ?
N22B C23B 1.4200 . ?
C23B C24B 1.4200 . ?
C24B C25B 1.4200 . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
C26B C51B 1.546(15) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
N31B C32B 1.3900 . ?
N31B C36B 1.3900 . ?
C32B C43B 1.349(10) . ?
C32B C33B 1.3900 . ?
C33B C34B 1.3900 . ?
C33B H33B 0.9500 . ?
C34B C35B 1.3900 . ?
C34B H34B 0.9500 . ?
C35B C36B 1.3900 . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
N41B C46B 1.347(15) . ?
N41B C45B 1.4200 . ?
N41B N42B 1.4200 . ?
N42B C43B 1.4200 . ?
C43B C44B 1.4200 . ?
C44B C45B 1.4200 . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
C46B C64B 1.46(2) 12_557 ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C51B C52B 1.3900 . ?
C51B C56B 1.3900 . ?
C52B C53B 1.3900 . ?
C52B H52B 0.9500 . ?
C53B C54B 1.3900 . ?
C53B H53B 0.9500 . ?
C54B C55B 1.3900 . ?
C54B H54B 0.9500 . ?
C55B C56B 1.3900 . ?
C55B C64B 1.3900 . ?
C56B C61B 1.3900 . ?
C61B C62B 1.3900 . ?
C61B H61B 0.9500 . ?
C62B C63B 1.3900 . ?
C62B H62B 0.9500 . ?
C63B C64B 1.3900 . ?
C63B H63B 0.9500 . ?
C64B C46B 1.465(15) 11_557 ?
Cl11 O13 1.398(8) . ?
Cl11 O11 1.402(8) . ?
Cl11 O14 1.416(8) . ?
Cl11 O12 1.422(9) . ?
Cl21 O23 1.394(8) . ?
Cl21 O21 1.395(8) . ?
Cl21 O24 1.419(8) . ?
Cl21 O22 1.428(8) . ?
Cl31 O33 1.382(8) . ?
Cl31 O31 1.411(8) . ?
Cl31 O32 1.417(8) . ?
Cl31 O34 1.421(8) . ?

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
N22B Os1 N11A 94.2(4) . . ?
N22B Os1 N42B 100.9(3) . . ?
N11A Os1 N42B 98.1(4) . . ?
N22B Os1 N22A 162.5(4) . . ?
N11A Os1 N22A 77.0(4) . . ?
N42B Os1 N22A 95.4(3) . . ?
N22B Os1 N31B 88.6(4) . . ?
N11A Os1 N31B 175.2(4) . . ?
N42B Os1 N31B 77.4(4) . . ?
N22A Os1 N31B 101.4(4) . . ?
N22B Os1 N11B 75.4(4) . . ?
N11A Os1 N11B 91.7(4) . . ?
N42B Os1 N11B 169.8(4) . . ?
N22A Os1 N11B 89.6(4) . . ?
N31B Os1 N11B 92.8(4) . . ?
N31A Os2 N31A 93.4(4) . 3 ?
N31A Os2 N31A 93.4(4) . 2 ?
N31A Os2 N31A 93.4(4) 3 2 ?
N31A Os2 N42A 75.8(4) . . ?
N31A Os2 N42A 168.8(4) 3 . ?
N31A Os2 N42A 90.2(3) 2 . ?
N31A Os2 N42A 168.8(7) . 2 ?
N31A Os2 N42A 90.1(7) 3 2 ?
N31A Os2 N42A 75.8(7) 2 2 ?
N42A Os2 N42A 101.1(7) . 2 ?
N31A Os2 N42A 90.1(7) . 3 ?
N31A Os2 N42A 75.8(8) 3 3 ?
N31A Os2 N42A 168.8(8) 2 3 ?
N42A Os2 N42A 101.1(7) . 3 ?
N42A Os2 N42A 101.1(8) 2 3 ?
C12A N11A C16A 120.0 . . ?
C12A N11A Os1 114.9(6) . . ?
C16A N11A Os1 125.1(6) . . ?
C23A C12A N11A 117.3(10) . . ?
C23A C12A C13A 122.5(10) . . ?
N11A C12A C13A 120.0 . . ?
C14A C13A C12A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C13A C14A C15A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C16A C15A C14A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C15A C16A N11A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
N11A C16A H16A 120.0 . . ?
N22A N21A C25A 108.0 . . ?
N22A N21A C26A 122.7(11) . . ?
C25A N21A C26A 129.1(11) . . ?
N21A N22A C23A 108.0 . . ?
N21A N22A Os1 138.8(7) . . ?
C23A N22A Os1 112.9(7) . . ?
C12A C23A C24A 134.4(10) . . ?
C12A C23A N22A 117.6(10) . . ?
C24A C23A N22A 108.0 . . ?
C23A C24A C25A 108.0 . . ?
C23A C24A H24A 126.0 . . ?
C25A C24A H24A 126.0 . . ?
C24A C25A N21A 108.0 . . ?
C24A C25A H25A 126.0 . . ?
N21A C25A H25A 126.0 . . ?
C51A C26A N21A 109.2(13) . . ?
C51A C26A H26A 109.8 . . ?
N21A C26A H26A 109.8 . . ?
C51A C26A H26B 109.8 . . ?
N21A C26A H26B 109.8 . . ?
H26A C26A H26B 108.3 . . ?
C32A N31A C36A 120.0 . . ?
C32A N31A Os2 115.7(6) . . ?
C36A N31A Os2 124.3(6) . . ?
C43A C32A C33A 123.2(9) . . ?
C43A C32A N31A 116.8(9) . . ?
C33A C32A N31A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C34A C35A C36A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C35A C36A N31A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
N31A C36A H36A 120.0 . . ?
C46A N41A C45A 126.0(10) . . ?
C46A N41A N42A 125.9(10) . . ?
C45A N41A N42A 108.0 . . ?
C43A N42A N41A 108.0 . . ?
C43A N42A Os2 114.6(6) . . ?
N41A N42A Os2 136.9(6) . . ?
C32A C43A N42A 116.2(9) . . ?
C32A C43A C44A 135.7(9) . . ?
N42A C43A C44A 108.0 . . ?
C45A C44A C43A 108.0 . . ?
C45A C44A H44A 126.0 . . ?
C43A C44A H44A 126.0 . . ?
C44A C45A N41A 108.0 . . ?
C44A C45A H45A 126.0 . . ?
N41A C45A H45A 126.0 . . ?
N41A C46A C64A 114.1(10) . . ?
N41A C46A H46A 108.7 . . ?
C64A C46A H46A 108.7 . . ?
N41A C46A H46B 108.7 . . ?
C64A C46A H46B 108.7 . . ?
H46A C46A H46B 107.6 . . ?
C52A C51A C56A 120.0 . . ?
C52A C51A C26A 121.6(9) . . ?
C56A C51A C26A 118.3(9) . . ?
C51A C52A C53A 120.0 . . ?
C51A C52A H52A 120.0 . . ?
C53A C52A H52A 120.0 . . ?
C52A C53A C54A 120.0 . . ?
C52A C53A H53A 120.0 . . ?
C54A C53A H53A 120.0 . . ?
C55A C54A C53A 120.0 . . ?
C55A C54A H54A 120.0 . . ?
C53A C54A H54A 120.0 . . ?
C54A C55A C56A 120.0 . . ?
C54A C55A C64A 120.0 . . ?
C56A C55A C64A 120.0 . . ?
C61A C56A C55A 120.0 . . ?
C61A C56A C51A 120.0 . . ?
C55A C56A C51A 120.0 . . ?
C62A C61A C56A 120.0 . . ?
C62A C61A H61A 120.0 . . ?
C56A C61A H61A 120.0 . . ?
C61A C62A C63A 120.0 . . ?
C61A C62A H62A 120.0 . . ?
C63A C62A H62A 120.0 . . ?
C64A C63A C62A 120.0 . . ?
C64A C63A H63A 120.0 . . ?
C62A C63A H63A 120.0 . . ?
C63A C64A C55A 120.0 . . ?
C63A C64A C46A 121.6(7) . . ?
C55A C64A C46A 118.4(7) . . ?
C12B N11B C16B 120.0 . . ?
C12B N11B Os1 114.8(6) . . ?
C16B N11B Os1 125.0(6) . . ?
C23B C12B N11B 117.0(9) . . ?
C23B C12B C13B 122.9(9) . . ?
N11B C12B C13B 120.0 . . ?
C14B C13B C12B 120.0 . . ?
C14B C13B H13B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C15B C14B C13B 120.0 . . ?
C15B C14B H14B 120.0 . . ?
C13B C14B H14B 120.0 . . ?
C14B C15B C16B 120.0 . . ?
C14B C15B H15B 120.0 . . ?
C16B C15B H15B 120.0 . . ?
C15B C16B N11B 120.0 . . ?
C15B C16B H16B 120.0 . . ?
N11B C16B H16B 120.0 . . ?
C26B N21B N22B 121.3(9) . . ?
C26B N21B C25B 130.7(9) . . ?
N22B N21B C25B 108.0 . . ?
N21B N22B C23B 108.0 . . ?
N21B N22B Os1 137.5(5) . . ?
C23B N22B Os1 114.3(5) . . ?
C12B C23B N22B 118.4(9) . . ?
C12B C23B C24B 133.5(9) . . ?
N22B C23B C24B 108.0 . . ?
C25B C24B C23B 108.0 . . ?
C25B C24B H24B 126.0 . . ?
C23B C24B H24B 126.0 . . ?
N21B C25B C24B 108.0 . . ?
N21B C25B H25B 126.0 . . ?
C24B C25B H25B 126.0 . . ?
N21B C26B C51B 113.5(11) . . ?
N21B C26B H26C 108.9 . . ?
C51B C26B H26C 108.9 . . ?
N21B C26B H26D 108.9 . . ?
C51B C26B H26D 108.9 . . ?
H26C C26B H26D 107.7 . . ?
C32B N31B C36B 120.0 . . ?
C32B N31B Os1 114.5(6) . . ?
C36B N31B Os1 125.4(6) . . ?
C43B C32B N31B 115.5(8) . . ?
C43B C32B C33B 124.2(8) . . ?
N31B C32B C33B 120.0 . . ?
C34B C33B C32B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C33B C34B C35B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C36B C35B C34B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C35B C36B N31B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
N31B C36B H36B 120.0 . . ?
C46B N41B C45B 130.9(10) . . ?
C46B N41B N42B 120.8(10) . . ?
C45B N41B N42B 108.0 . . ?
C43B N42B N41B 108.0 . . ?
C43B N42B Os1 111.7(5) . . ?
N41B N42B Os1 140.3(5) . . ?
C32B C43B N42B 120.3(8) . . ?
C32B C43B C44B 131.7(8) . . ?
N42B C43B C44B 108.0 . . ?
C45B C44B C43B 108.0 . . ?
C45B C44B H44B 126.0 . . ?
C43B C44B H44B 126.0 . . ?
C44B C45B N41B 108.0 . . ?
C44B C45B H45B 126.0 . . ?
N41B C45B H45B 126.0 . . ?
N41B C46B C64B 119.6(13) . 12_557 ?
N41B C46B H46C 107.4 . . ?
C64B C46B H46C 107.4 12_557 . ?
N41B C46B H46D 107.4 . . ?
C64B C46B H46D 107.4 12_557 . ?
H46C C46B H46D 107.0 . . ?
C52B C51B C56B 120.0 . . ?
C52B C51B C26B 120.8(7) . . ?
C56B C51B C26B 119.2(7) . . ?
C53B C52B C51B 120.0 . . ?
C53B C52B H52B 120.0 . . ?
C51B C52B H52B 120.0 . . ?
C52B C53B C54B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C54B C53B H53B 120.0 . . ?
C53B C54B C55B 120.0 . . ?
C53B C54B H54B 120.0 . . ?
C55B C54B H54B 120.0 . . ?
C56B C55B C54B 120.0 . . ?
C56B C55B C64B 120.0 . . ?
C54B C55B C64B 120.0 . . ?
C61B C56B C55B 120.0 . . ?
C61B C56B C51B 120.0 . . ?
C55B C56B C51B 120.0 . . ?
C62B C61B C56B 120.0 . . ?
C62B C61B H61B 120.0 . . ?
C56B C61B H61B 120.0 . . ?
C61B C62B C63B 120.0 . . ?
C61B C62B H62B 120.0 . . ?
C63B C62B H62B 120.0 . . ?
C64B C63B C62B 120.0 . . ?
C64B C63B H63B 120.0 . . ?
C62B C63B H63B 120.0 . . ?
C63B C64B C55B 120.0 . . ?
C63B C64B C46B 115.2(7) . 11_557 ?
C55B C64B C46B 124.6(7) . 11_557 ?
O13 Cl11 O11 110.6(8) . . ?
O13 Cl11 O14 110.0(8) . . ?
O11 Cl11 O14 109.0(8) . . ?
O13 Cl11 O12 109.0(8) . . ?
O11 Cl11 O12 109.6(8) . . ?
O14 Cl11 O12 108.6(8) . . ?
O23 Cl21 O21 111.9(8) . . ?
O23 Cl21 O24 109.6(8) . . ?
O21 Cl21 O24 109.6(8) . . ?
O23 Cl21 O22 109.1(8) . . ?
O21 Cl21 O22 108.7(7) . . ?
O24 Cl21 O22 107.8(8) . . ?
O33 Cl31 O31 111.7(8) . . ?
O33 Cl31 O32 110.2(8) . . ?
O31 Cl31 O32 108.8(8) . . ?
O33 Cl31 O34 110.0(8) . . ?
O31 Cl31 O34 107.8(8) . . ?
O32 Cl31 O34 108.3(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
C16A N11A C12A C23A 175.2(11) . . . . ?
Os1 N11A C12A C23A -5.1(9) . . . . ?
C16A N11A C12A C13A 0.0 . . . . ?
Os1 N11A C12A C13A 179.7(6) . . . . ?
C23A C12A C13A C14A -174.9(11) . . . . ?
N11A C12A C13A C14A 0.0 . . . . ?
C12A C13A C14A C15A 0.0 . . . . ?
C13A C14A C15A C16A 0.0 . . . . ?
C14A C15A C16A N11A 0.0 . . . . ?
C12A N11A C16A C15A 0.0 . . . . ?
Os1 N11A C16A C15A -179.7(7) . . . . ?
C25A N21A N22A C23A 0.0 . . . . ?
C26A N21A N22A C23A -176.3(13) . . . . ?
C25A N21A N22A Os1 -172.4(10) . . . . ?
C26A N21A N22A Os1 11.3(16) . . . . ?
N11A C12A C23A C24A -173.0(8) . . . . ?
C13A C12A C23A C24A 2.1(15) . . . . ?
N11A C12A C23A N22A 7.1(12) . . . . ?
C13A C12A C23A N22A -177.9(6) . . . . ?
N21A N22A C23A C12A 180.0(12) . . . . ?
Os1 N22A C23A C12A -5.4(11) . . . . ?
N21A N22A C23A C24A 0.0 . . . . ?
Os1 N22A C23A C24A 174.6(7) . . . . ?
C12A C23A C24A C25A -180.0(14) . . . . ?
N22A C23A C24A C25A 0.0 . . . . ?
C23A C24A C25A N21A 0.0 . . . . ?
N22A N21A C25A C24A 0.0 . . . . ?
C26A N21A C25A C24A 176.0(14) . . . . ?
N22A N21A C26A C51A 87.0(15) . . . . ?
C25A N21A C26A C51A -88.5(15) . . . . ?
C36A N31A C32A C43A -178.2(10) . . . . ?
Os2 N31A C32A C43A 3.3(9) . . . . ?
C36A N31A C32A C33A 0.0 . . . . ?
Os2 N31A C32A C33A -178.5(6) . . . . ?
C43A C32A C33A C34A 178.0(10) . . . . ?
N31A C32A C33A C34A 0.0 . . . . ?
C32A C33A C34A C35A 0.0 . . . . ?
C33A C34A C35A C36A 0.0 . . . . ?
C34A C35A C36A N31A 0.0 . . . . ?
C32A N31A C36A C35A 0.0 . . . . ?
Os2 N31A C36A C35A 178.4(7) . . . . ?
C46A N41A N42A C43A 176.9(11) . . . . ?
C45A N41A N42A C43A 0.0 . . . . ?
C46A N41A N42A Os2 5.7(13) . . . . ?
C45A N41A N42A Os2 -171.2(8) . . . . ?
C33A C32A C43A N42A -173.7(6) . . . . ?
N31A C32A C43A N42A 4.4(11) . . . . ?
C33A C32A C43A C44A 1.7(14) . . . . ?
N31A C32A C43A C44A 179.8(7) . . . . ?
N41A N42A C43A C32A 176.7(10) . . . . ?
Os2 N42A C43A C32A -9.9(9) . . . . ?
N41A N42A C43A C44A 0.0 . . . . ?
Os2 N42A C43A C44A 173.4(6) . . . . ?
C32A C43A C44A C45A -175.7(13) . . . . ?
N42A C43A C44A C45A 0.0 . . . . ?
C43A C44A C45A N41A 0.0 . . . . ?
C46A N41A C45A C44A -176.9(11) . . . . ?
N42A N41A C45A C44A 0.0 . . . . ?
C45A N41A C46A C64A 91.0(13) . . . . ?
N42A N41A C46A C64A -85.4(13) . . . . ?
N21A C26A C51A C52A 1.8(17) . . . . ?
N21A C26A C51A C56A 178.6(9) . . . . ?
C56A C51A C52A C53A 0.0 . . . . ?
C26A C51A C52A C53A 176.8(11) . . . . ?
C51A C52A C53A C54A 0.0 . . . . ?
C52A C53A C54A C55A 0.0 . . . . ?
C53A C54A C55A C56A 0.0 . . . . ?
C53A C54A C55A C64A 180.0 . . . . ?
C54A C55A C56A C61A 180.0 . . . . ?
C64A C55A C56A C61A 0.0 . . . . ?
C54A C55A C56A C51A 0.0 . . . . ?
C64A C55A C56A C51A 180.0 . . . . ?
C52A C51A C56A C61A 180.0 . . . . ?
C26A C51A C56A C61A 3.1(10) . . . . ?
C52A C51A C56A C55A 0.0 . . . . ?
C26A C51A C56A C55A -176.9(10) . . . . ?
C55A C56A C61A C62A 0.0 . . . . ?
C51A C56A C61A C62A 180.0 . . . . ?
C56A C61A C62A C63A 0.0 . . . . ?
C61A C62A C63A C64A 0.0 . . . . ?
C62A C63A C64A C55A 0.0 . . . . ?
C62A C63A C64A C46A 179.5(9) . . . . ?
C54A C55A C64A C63A 180.0 . . . . ?
C56A C55A C64A C63A 0.0 . . . . ?
C54A C55A C64A C46A 0.5(9) . . . . ?
C56A C55A C64A C46A -179.5(9) . . . . ?
N41A C46A C64A C63A -10.9(15) . . . . ?
N41A C46A C64A C55A 168.6(8) . . . . ?
C16B N11B C12B C23B -177.0(11) . . . . ?
Os1 N11B C12B C23B -1.8(10) . . . . ?
C16B N11B C12B C13B 0.0 . . . . ?
Os1 N11B C12B C13B 175.2(7) . . . . ?
C23B C12B C13B C14B 176.8(12) . . . . ?
N11B C12B C13B C14B 0.0 . . . . ?
C12B C13B C14B C15B 0.0 . . . . ?
C13B C14B C15B C16B 0.0 . . . . ?
C14B C15B C16B N11B 0.0 . . . . ?
C12B N11B C16B C15B 0.0 . . . . ?
Os1 N11B C16B C15B -174.7(7) . . . . ?
C26B N21B N22B C23B -179.7(12) . . . . ?
C25B N21B N22B C23B 0.0 . . . . ?
C26B N21B N22B Os1 6.1(14) . . . . ?
C25B N21B N22B Os1 -174.2(10) . . . . ?
N11B C12B C23B N22B 2.1(13) . . . . ?
C13B C12B C23B N22B -174.8(7) . . . . ?
N11B C12B C23B C24B -174.1(8) . . . . ?
C13B C12B C23B C24B 9.0(16) . . . . ?
N21B N22B C23B C12B -177.1(12) . . . . ?
Os1 N22B C23B C12B -1.4(11) . . . . ?
N21B N22B C23B C24B 0.0 . . . . ?
Os1 N22B C23B C24B 175.7(8) . . . . ?
C12B C23B C24B C25B 176.5(14) . . . . ?
N22B C23B C24B C25B 0.0 . . . . ?
C26B N21B C25B C24B 179.7(13) . . . . ?
N22B N21B C25B C24B 0.0 . . . . ?
C23B C24B C25B N21B 0.0 . . . . ?
N22B N21B C26B C51B 87.6(13) . . . . ?
C25B N21B C26B C51B -92.1(13) . . . . ?
C36B N31B C32B C43B 174.8(9) . . . . ?
Os1 N31B C32B C43B -8.1(8) . . . . ?
C36B N31B C32B C33B 0.0 . . . . ?
Os1 N31B C32B C33B 177.0(6) . . . . ?
C43B C32B C33B C34B -174.4(10) . . . . ?
N31B C32B C33B C34B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B N31B 0.0 . . . . ?
C32B N31B C36B C35B 0.0 . . . . ?
Os1 N31B C36B C35B -176.7(6) . . . . ?
C46B N41B N42B C43B -174.3(11) . . . . ?
C45B N41B N42B C43B 0.0 . . . . ?
C46B N41B N42B Os1 3.2(13) . . . . ?
C45B N41B N42B Os1 177.5(8) . . . . ?
N31B C32B C43B N42B 4.1(11) . . . . ?
C33B C32B C43B N42B 178.7(6) . . . . ?
N31B C32B C43B C44B -175.5(7) . . . . ?
C33B C32B C43B C44B -0.9(12) . . . . ?
N41B N42B C43B C32B -179.7(10) . . . . ?
Os1 N42B C43B C32B 2.0(9) . . . . ?
N41B N42B C43B C44B 0.0 . . . . ?
Os1 N42B C43B C44B -178.3(6) . . . . ?
C32B C43B C44B C45B 179.7(11) . . . . ?
N42B C43B C44B C45B 0.0 . . . . ?
C43B C44B C45B N41B 0.0 . . . . ?
C46B N41B C45B C44B 173.6(13) . . . . ?
N42B N41B C45B C44B 0.0 . . . . ?
C45B N41B C46B C64B -83.0(18) . . . 12_557 ?
N42B N41B C46B C64B 89.8(16) . . . 12_557 ?
N21B C26B C51B C52B 0.8(14) . . . . ?
N21B C26B C51B C56B -178.8(8) . . . . ?
C56B C51B C52B C53B 0.0 . . . . ?
C26B C51B C52B C53B -179.5(9) . . . . ?
C51B C52B C53B C54B 0.0 . . . . ?
C52B C53B C54B C55B 0.0 . . . . ?
C53B C54B C55B C56B 0.0 . . . . ?
C53B C54B C55B C64B 180.0 . . . . ?
C54B C55B C56B C61B 180.0 . . . . ?
C64B C55B C56B C61B 0.0 . . . . ?
C54B C55B C56B C51B 0.0 . . . . ?
C64B C55B C56B C51B 180.0 . . . . ?
C52B C51B C56B C61B 180.0 . . . . ?
C26B C51B C56B C61B -0.5(9) . . . . ?
C52B C51B C56B C55B 0.0 . . . . ?
C26B C51B C56B C55B 179.5(9) . . . . ?
C55B C56B C61B C62B 0.0 . . . . ?
C51B C56B C61B C62B 180.0 . . . . ?
C56B C61B C62B C63B 0.0 . . . . ?
C61B C62B C63B C64B 0.0 . . . . ?
C62B C63B C64B C55B 0.0 . . . . ?
C62B C63B C64B C46B 175.8(9) . . . 11_557 ?
C56B C55B C64B C63B 0.0 . . . . ?
C54B C55B C64B C63B 180.0 . . . . ?
C56B C55B C64B C46B -175.4(10) . . . 11_557 ?
C54B C55B C64B C46B 4.6(10) . . . 11_557 ?

_refine_diff_density_max         1.350
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.107

_shelxl_version_number           2013-4



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: MeNO2, di(isopropeyl)ether'
_chemical_properties_physical    Efflorescent
####################################################################### 
# 
# 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_Ru4Co4
_database_code_depnum_ccdc_archive 'CCDC 1413548'
_audit_update_record             
;
2015-07-17 deposited with the CCDC.
2015-09-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C339 H273 B16 Co4 F64 N75 O6 Ru4'
_chemical_formula_weight         7522.27

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Ru Ru -1.2594 0.8363 '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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   34.091(2)
_cell_length_b                   34.091(2)
_cell_length_c                   35.5084(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     35740(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5509
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      20.52

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.048
_exptl_crystal_F_000             11460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.334
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6087
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_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            41881
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_av_R_equivalents  0.0919
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         0.897
_diffrn_reflns_theta_max         20.830
_diffrn_reflns_theta_full        22.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.798
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.798
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.798
_reflns_number_total             8305
_reflns_number_gt                4633
_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.

 The structure consists of a coordination cage complex cation with the formula 
 Ru4Co4(C28H22N6)12, 16 BF4 counter anions and three nitromethane molecules.
 One sixth of this is found in the asymmetric unit. Twelve of the required
 sixteen anions could be located from the data (two anions with full occupancy
 in the asymmetric unit). Accordingly, the calculated formula does not match
 the reported formula in which all anions are accounted for.
 
 The nitromethane molecule was restrained with weak DFIX commands to fix the
 geometry. The aromatic rings of the ligands were fixed with AFIX restraints.
 
 Weak global restraints were applied to all ligand and solvent atoms to
 achieve a more chemically reasonable model. 

 After the cage and anions were located, a very large solvent accessible void
 remained, in which disorded anions and solvent molecules resided. This region
 of diffuse electron density was removed with the SQUEEZE command on PLATON,
 details are given below.

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.006 -0.009 -0.001     12719      5091 ' '
   2  0.000  0.000  0.500       473       166 ' '
   3  0.667  0.333  0.833       473       166 ' '
   4  0.333  0.667  0.167       473       166 ' '
_platon_squeeze_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)+(0.1598P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8305
_refine_ls_number_parameters     620
_refine_ls_number_restraints     672
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0773
_refine_ls_wR_factor_ref         0.2460
_refine_ls_wR_factor_gt          0.2194
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_restrained_S_all      0.958
_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_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
Ru1 Ru 0.62337(3) 0.92733(3) 0.07669(2) 0.0755(4) Uani 0.5 1 d . . P A 1
Co1 Co 0.62337(3) 0.92733(3) 0.07669(2) 0.0755(4) Uani 0.5 1 d . . P A 2
Co2 Co 0.3333 0.6667 -0.09897(3) 0.0680(5) Uani 0.5 3 d S T P B 1
Ru2 Ru 0.3333 0.6667 -0.09897(3) 0.0680(5) Uani 0.5 3 d S T P B 2
N11A N 0.61981(18) 0.97473(15) 0.11256(12) 0.0828(17) Uani 1 1 d G U . . .
C12A C 0.58870(17) 0.98771(17) 0.10194(11) 0.0819(18) Uani 1 1 d G U . A .
C13A C 0.58336(18) 1.01860(18) 0.12373(15) 0.089(2) Uani 1 1 d G U . A .
H13A H 0.5621 1.0275 0.1165 0.107 Uiso 1 1 calc R U . . .
C14A C 0.6091(2) 1.03649(16) 0.15614(14) 0.098(2) Uani 1 1 d G U . A .
H14A H 0.6055 1.0576 0.1710 0.117 Uiso 1 1 calc R U . . .
C15A C 0.64022(19) 1.02351(18) 0.16676(12) 0.097(2) Uani 1 1 d G U . A .
H15A H 0.6578 1.0357 0.1889 0.117 Uiso 1 1 calc R U . . .
C16A C 0.64556(17) 0.99262(18) 0.14498(14) 0.091(2) Uani 1 1 d G U . A .
H16A H 0.6668 0.9837 0.1522 0.109 Uiso 1 1 calc R U . . .
N21A N 0.54947(17) 0.92626(15) 0.01629(11) 0.0786(16) Uani 1 1 d G U . . .
N22A N 0.57439(15) 0.93802(16) 0.05049(12) 0.0776(16) Uani 1 1 d G U . . .
C23A C 0.56730(19) 0.97078(17) 0.06920(11) 0.0821(18) Uani 1 1 d G U . . .
C24A C 0.5380(2) 0.97927(17) 0.04656(15) 0.0844(19) Uani 1 1 d G U . . .
H24A H 0.5276 0.9998 0.0523 0.101 Uiso 1 1 calc R U . . .
C25A C 0.52699(16) 0.95175(18) 0.01386(13) 0.0838(19) Uani 1 1 d G U . . .
H25A H 0.5079 0.9506 -0.0061 0.101 Uiso 1 1 calc R U . . .
C26A C 0.5442(3) 0.8911(2) -0.00722(19) 0.0737(19) Uani 1 1 d . U . . .
H26A H 0.5725 0.8897 -0.0068 0.088 Uiso 1 1 calc R U . . .
H26B H 0.5396 0.8981 -0.0333 0.088 Uiso 1 1 calc R U . . .
N31A N 0.31545(19) 0.60791(16) -0.13133(13) 0.0942(18) Uani 1 1 d G U . . .
C32A C 0.33629(18) 0.58332(19) -0.12122(12) 0.0880(18) Uani 1 1 d G U . B .
C33A C 0.3276(2) 0.54496(19) -0.14157(16) 0.104(2) Uani 1 1 d G U . B .
H33A H 0.3418 0.5282 -0.1347 0.125 Uiso 1 1 calc R U . . .
C34A C 0.2980(2) 0.53119(18) -0.17203(16) 0.122(3) Uani 1 1 d G U . B .
H34A H 0.2921 0.5050 -0.1859 0.147 Uiso 1 1 calc R U . . .
C35A C 0.2772(2) 0.5558(2) -0.18214(14) 0.126(3) Uani 1 1 d G U . B .
H35A H 0.2570 0.5464 -0.2030 0.151 Uiso 1 1 calc R U . . .
C36A C 0.2859(2) 0.5941(2) -0.16179(15) 0.112(2) Uani 1 1 d G U . B .
H36A H 0.2717 0.6109 -0.1687 0.135 Uiso 1 1 calc R U . . .
N41A N 0.39642(15) 0.64634(13) -0.04098(10) 0.0622(13) Uani 1 1 d G U . . .
N42A N 0.36685(15) 0.63672(15) -0.07213(11) 0.0646(14) Uani 1 1 d G U . . .
C43A C 0.36306(16) 0.59829(16) -0.09108(11) 0.0729(16) Uani 1 1 d G U . . .
C44A C 0.39028(18) 0.58417(15) -0.07164(14) 0.0739(17) Uani 1 1 d G U . . .
H44A H 0.3940 0.5592 -0.0782 0.089 Uiso 1 1 calc R U . . .
C45A C 0.41090(15) 0.61386(17) -0.04068(12) 0.0701(17) Uani 1 1 d G U . . .
H45A H 0.4309 0.6123 -0.0229 0.084 Uiso 1 1 calc R U . . .
C46A C 0.4074(2) 0.6815(2) -0.01563(17) 0.0565(16) Uani 1 1 d . U . . .
H46A H 0.4124 0.6721 0.0095 0.068 Uiso 1 1 calc R U . . .
H46B H 0.3812 0.6865 -0.0135 0.068 Uiso 1 1 calc R U . . .
C51A C 0.50486(12) 0.84475(9) 0.00346(9) 0.0656(17) Uani 1 1 d G U . . .
C52A C 0.47797(14) 0.84210(11) 0.03387(9) 0.0655(18) Uani 1 1 d G U . . .
H52A H 0.4846 0.8687 0.0476 0.079 Uiso 1 1 calc R U . . .
C53A C 0.44131(13) 0.80058(13) 0.04424(8) 0.0618(17) Uani 1 1 d G U . . .
H53A H 0.4229 0.7988 0.0650 0.074 Uiso 1 1 calc R U . . .
C54A C 0.43154(10) 0.76171(11) 0.02420(8) 0.0569(16) Uani 1 1 d G U . . .
H54A H 0.4065 0.7333 0.0313 0.068 Uiso 1 1 calc R U . . .
C55A C 0.45843(9) 0.76436(9) -0.00621(7) 0.0547(15) Uani 1 1 d G U . . .
C56A C 0.49509(9) 0.80588(9) -0.01659(7) 0.0605(16) Uani 1 1 d G U . . .
C61A C 0.52198(11) 0.80852(12) -0.04700(9) 0.0690(18) Uani 1 1 d G U . . .
H61A H 0.5470 0.8369 -0.0541 0.083 Uiso 1 1 calc R U . . .
C62A C 0.51221(13) 0.76965(14) -0.06704(8) 0.0692(18) Uani 1 1 d G U . . .
H62A H 0.5306 0.7715 -0.0878 0.083 Uiso 1 1 calc R U . . .
C63A C 0.47555(14) 0.72813(12) -0.05667(9) 0.0633(17) Uani 1 1 d G U . . .
H63A H 0.4689 0.7016 -0.0704 0.076 Uiso 1 1 calc R U . . .
C64A C 0.44866(12) 0.72549(9) -0.02626(9) 0.0576(15) Uani 1 1 d G U . . .
N11B N 0.62155(18) 0.87713(16) 0.04099(12) 0.0852(17) Uani 1 1 d G U . . .
C12B C 0.58907(16) 0.83277(18) 0.04959(12) 0.0798(18) Uani 1 1 d G U . A .
C13B C 0.58487(17) 0.79735(14) 0.02730(15) 0.088(2) Uani 1 1 d G U . A .
H13B H 0.5627 0.7670 0.0332 0.106 Uiso 1 1 calc R U . . .
C14B C 0.6132(2) 0.80629(18) -0.00359(14) 0.094(2) Uani 1 1 d G U . A .
H14B H 0.6103 0.7821 -0.0188 0.113 Uiso 1 1 calc R U . . .
C15B C 0.64564(18) 0.8507(2) -0.01219(12) 0.102(2) Uani 1 1 d G U . A .
H15B H 0.6650 0.8568 -0.0333 0.123 Uiso 1 1 calc R U . . .
C16B C 0.64983(16) 0.88607(16) 0.01010(14) 0.095(2) Uani 1 1 d G U . A .
H16B H 0.6720 0.9164 0.0042 0.115 Uiso 1 1 calc R U . . .
N21B N 0.54690(16) 0.85209(15) 0.13536(11) 0.0696(14) Uani 1 1 d G U . . .
N22B N 0.57449(14) 0.86639(13) 0.10260(12) 0.0697(15) Uani 1 1 d G U . . .
C23B C 0.56494(17) 0.82724(17) 0.08146(11) 0.0719(17) Uani 1 1 d G U . . .
C24B C 0.53145(18) 0.78875(13) 0.10115(14) 0.0777(19) Uani 1 1 d G U . . .
H24B H 0.5187 0.7581 0.0934 0.093 Uiso 1 1 calc R U . . .
C25B C 0.52030(15) 0.80410(15) 0.13446(12) 0.0743(18) Uani 1 1 d G U . . .
H25B H 0.4988 0.7855 0.1529 0.089 Uiso 1 1 calc R U . . .
C26B C 0.5462(3) 0.8814(3) 0.16284(19) 0.0690(16) Uani 1 1 d . U . . .
H26C H 0.5765 0.9089 0.1640 0.083 Uiso 1 1 calc R U . . .
H26D H 0.5401 0.8662 0.1877 0.083 Uiso 1 1 calc R U . . .
N31B N 0.67572(17) 0.98203(17) 0.04676(14) 0.102(2) Uani 1 1 d G U . . .
C32B C 0.7195(2) 0.9941(2) 0.05770(14) 0.106(2) Uani 1 1 d G U . A .
C33B C 0.75639(16) 1.0302(2) 0.04031(18) 0.123(3) Uani 1 1 d G U . A .
H33B H 0.7863 1.0385 0.0478 0.147 Uiso 1 1 calc R U . . .
C34B C 0.74955(18) 1.0543(2) 0.01199(17) 0.133(3) Uani 1 1 d G U . A .
H34B H 0.7748 1.0790 0.0001 0.159 Uiso 1 1 calc R U . . .
C35B C 0.7058(2) 1.0423(2) 0.00105(16) 0.136(3) Uani 1 1 d G U . A .
H35B H 0.7011 1.0587 -0.0183 0.163 Uiso 1 1 calc R U . . .
C36B C 0.66888(17) 1.0061(2) 0.01843(16) 0.116(3) Uani 1 1 d G U . A .
H36B H 0.6390 0.9979 0.0110 0.140 Uiso 1 1 calc R U . . .
N41B N 0.69301(17) 0.91481(16) 0.13218(13) 0.0857(17) Uani 1 1 d G U . . .
N42B N 0.68176(15) 0.93486(19) 0.10211(14) 0.0896(18) Uani 1 1 d G U . . .
C43B C 0.7228(2) 0.96938(19) 0.08611(14) 0.101(2) Uani 1 1 d G U . . .
C44B C 0.75934(14) 0.9707(2) 0.10629(17) 0.105(2) Uani 1 1 d G U . . .
H44B H 0.7906 0.9906 0.1016 0.126 Uiso 1 1 calc R U . . .
C45B C 0.74096(17) 0.9369(2) 0.13476(15) 0.098(2) Uani 1 1 d G U . . .
H45B H 0.7578 0.9303 0.1524 0.117 Uiso 1 1 calc R U . . .
C46B C 0.6607(3) 0.8820(3) 0.1554(2) 0.081(2) Uani 1 1 d . U . . .
H46C H 0.6343 0.8866 0.1565 0.098 Uiso 1 1 calc R U . . .
H46D H 0.6734 0.8866 0.1812 0.098 Uiso 1 1 calc R U . . .
C51B C 0.51076(13) 0.89576(12) 0.15578(10) 0.0650(15) Uani 1 1 d G U . . .
C52B C 0.48365(15) 0.87873(12) 0.12395(9) 0.0686(17) Uani 1 1 d G U . . .
H52B H 0.4850 0.8563 0.1090 0.082 Uiso 1 1 calc R U . . .
C53B C 0.45460(13) 0.89455(13) 0.11393(8) 0.0686(17) Uani 1 1 d G U . . .
H53B H 0.4361 0.8829 0.0922 0.082 Uiso 1 1 calc R U . . .
C54B C 0.45266(12) 0.92740(13) 0.13574(9) 0.0676(17) Uani 1 1 d G U . . .
H54B H 0.4328 0.9382 0.1289 0.081 Uiso 1 1 calc R U . . .
C55B C 0.47978(9) 0.94443(10) 0.16757(7) 0.0646(15) Uani 1 1 d G U . . .
C56B C 0.50883(9) 0.92861(10) 0.17759(7) 0.0649(15) Uani 1 1 d G U . . .
C61B C 0.53594(12) 0.94564(14) 0.20942(9) 0.0718(18) Uani 1 1 d G U . . .
H61B H 0.5558 0.9348 0.2163 0.086 Uiso 1 1 calc R U . . .
C62B C 0.53401(14) 0.97849(14) 0.23123(9) 0.0792(18) Uani 1 1 d G U . . .
H62B H 0.5525 0.9901 0.2530 0.095 Uiso 1 1 calc R U . . .
C63B C 0.50496(15) 0.99431(13) 0.22121(10) 0.0772(18) Uani 1 1 d G U . . .
H63B H 0.5036 1.0168 0.2361 0.093 Uiso 1 1 calc R U . . .
C64B C 0.47785(14) 0.97728(12) 0.18938(10) 0.0699(18) Uani 1 1 d G U . . .
B1 B 0.5634(5) 0.4888(4) 0.0928(3) 0.082(3) Uani 1 1 d . . . . .
F1 F 0.54854(19) 0.46203(19) 0.06168(15) 0.1175(18) Uani 1 1 d . . . . .
F2 F 0.6090(2) 0.5112(2) 0.09549(15) 0.1198(19) Uani 1 1 d . . . . .
F3 F 0.5463(2) 0.4638(2) 0.12459(16) 0.136(2) Uani 1 1 d . . . . .
F4 F 0.5466(2) 0.5172(2) 0.09062(16) 0.149(2) Uani 1 1 d . . . . .
B11 B 0.1636(5) 0.5002(6) 0.0518(4) 0.105(4) Uani 1 1 d . . . . .
F11 F 0.1485(2) 0.5245(2) 0.03339(15) 0.133(2) Uani 1 1 d . . . . .
F12 F 0.2094(2) 0.5182(2) 0.04512(18) 0.153(2) Uani 1 1 d . . . . .
F13 F 0.1563(2) 0.4974(3) 0.08703(17) 0.160(3) Uani 1 1 d . . . . .
F14 F 0.1408(3) 0.4543(3) 0.0372(2) 0.158(2) Uani 1 1 d . . . . .
N1S N 0.6158(4) 0.0154(4) 0.9244(3) 0.067(3) Uani 0.5 1 d D U P . .
O2S O 0.6134(3) -0.0186(3) 0.9392(2) 0.070(3) Uani 0.5 1 d D U P . .
O3S O 0.6249(3) 0.0260(3) 0.8915(2) 0.065(3) Uani 0.5 1 d D U P . .
C4S C 0.6022(5) 0.0429(4) 0.9464(3) 0.068(4) Uani 0.5 1 d D U P . .
H4S1 H 0.5841 0.0514 0.9306 0.102 Uiso 0.5 1 calc R U P . .
H4S2 H 0.6292 0.0702 0.9553 0.102 Uiso 0.5 1 calc R U P . .
H4S3 H 0.5841 0.0253 0.9680 0.102 Uiso 0.5 1 calc R U 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
Ru1 N42B 2.081(4) . ?
Ru1 N22A 2.097(4) . ?
Ru1 N11B 2.106(4) . ?
Ru1 N11A 2.108(4) . ?
Ru1 N31B 2.113(4) . ?
Ru1 N22B 2.116(4) . ?
Co2 N42A 2.103(3) . ?
Co2 N42A 2.103(7) 2_665 ?
Co2 N42A 2.103(8) 3_565 ?
Co2 N31A 2.117(4) 3_565 ?
Co2 N31A 2.117(4) 2_665 ?
Co2 N31A 2.117(4) . ?
N11A C12A 1.3900 . ?
N11A C16A 1.3900 . ?
C12A C23A 1.340(5) . ?
C12A C13A 1.3900 . ?
C13A C14A 1.3900 . ?
C13A H13A 0.9500 . ?
C14A C15A 1.3900 . ?
C14A H14A 0.9500 . ?
C15A C16A 1.3900 . ?
C15A H15A 0.9500 . ?
C16A H16A 0.9500 . ?
N21A C26A 1.397(8) . ?
N21A C25A 1.4200 . ?
N21A N22A 1.4200 . ?
N22A C23A 1.4200 . ?
C23A C24A 1.4200 . ?
C24A C25A 1.4200 . ?
C24A H24A 0.9500 . ?
C25A H25A 0.9500 . ?
C26A C51A 1.523(8) . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
N31A C32A 1.3900 . ?
N31A C36A 1.3900 . ?
C32A C43A 1.332(5) . ?
C32A C33A 1.3900 . ?
C33A C34A 1.3900 . ?
C33A H33A 0.9500 . ?
C34A C35A 1.3900 . ?
C34A H34A 0.9500 . ?
C35A C36A 1.3900 . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
N41A C46A 1.392(7) . ?
N41A C45A 1.4200 . ?
N41A N42A 1.4200 . ?
N42A C43A 1.4200 . ?
C43A C44A 1.4200 . ?
C44A C45A 1.4200 . ?
C44A H44A 0.9500 . ?
C45A H45A 0.9500 . ?
C46A C64A 1.505(7) . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C51A C52A 1.3900 . ?
C51A C56A 1.3900 . ?
C52A C53A 1.3900 . ?
C52A H52A 0.9500 . ?
C53A C54A 1.3900 . ?
C53A H53A 0.9500 . ?
C54A C55A 1.3900 . ?
C54A H54A 0.9500 . ?
C55A C56A 1.3900 . ?
C55A C64A 1.3900 . ?
C56A C61A 1.3900 . ?
C61A C62A 1.3900 . ?
C61A H61A 0.9500 . ?
C62A C63A 1.3900 . ?
C62A H62A 0.9500 . ?
C63A C64A 1.3900 . ?
C63A H63A 0.9500 . ?
N11B C12B 1.3900 . ?
N11B C16B 1.3900 . ?
C12B C23B 1.356(5) . ?
C12B C13B 1.3900 . ?
C13B C14B 1.3900 . ?
C13B H13B 0.9500 . ?
C14B C15B 1.3900 . ?
C14B H14B 0.9500 . ?
C15B C16B 1.3900 . ?
C15B H15B 0.9500 . ?
C16B H16B 0.9500 . ?
N21B C26B 1.406(8) . ?
N21B N22B 1.4200 . ?
N21B C25B 1.4200 . ?
N22B C23B 1.4200 . ?
C23B C24B 1.4200 . ?
C24B C25B 1.4200 . ?
C24B H24B 0.9500 . ?
C25B H25B 0.9500 . ?
C26B C51B 1.533(8) . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?
N31B C32B 1.3900 . ?
N31B C36B 1.3900 . ?
C32B C43B 1.354(6) . ?
C32B C33B 1.3900 . ?
C33B C34B 1.3900 . ?
C33B H33B 0.9500 . ?
C34B C35B 1.3900 . ?
C34B H34B 0.9500 . ?
C35B C36B 1.3900 . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
N41B C46B 1.383(8) . ?
N41B N42B 1.4200 . ?
N41B C45B 1.4200 . ?
N42B C43B 1.4200 . ?
C43B C44B 1.4200 . ?
C44B C45B 1.4200 . ?
C44B H44B 0.9500 . ?
C45B H45B 0.9500 . ?
C46B C64B 1.533(10) 14_455 ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C51B C52B 1.3900 . ?
C51B C56B 1.3900 . ?
C52B C53B 1.3900 . ?
C52B H52B 0.9500 . ?
C53B C54B 1.3900 . ?
C53B H53B 0.9500 . ?
C54B C55B 1.3900 . ?
C54B H54B 0.9500 . ?
C55B C56B 1.3900 . ?
C55B C64B 1.3900 . ?
C56B C61B 1.3900 . ?
C61B C62B 1.3900 . ?
C61B H61B 0.9500 . ?
C62B C63B 1.3900 . ?
C62B H62B 0.9500 . ?
C63B C64B 1.3900 . ?
C63B H63B 0.9500 . ?
C64B C46B 1.533(9) 15 ?
B1 F2 1.349(12) . ?
B1 F4 1.351(11) . ?
B1 F3 1.357(11) . ?
B1 F1 1.360(12) . ?
B11 F13 1.269(13) . ?
B11 F11 1.344(14) . ?
B11 F12 1.384(14) . ?
B11 F14 1.452(15) . ?
N1S O3S 1.216(8) . ?
N1S O2S 1.236(8) . ?
N1S C4S 1.462(9) . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?

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
N42B Ru1 N22A 165.2(2) . . ?
N42B Ru1 N11B 89.9(2) . . ?
N22A Ru1 N11B 99.89(19) . . ?
N42B Ru1 N11A 93.5(2) . . ?
N22A Ru1 N11A 77.2(2) . . ?
N11B Ru1 N11A 175.7(2) . . ?
N42B Ru1 N31B 77.0(2) . . ?
N22A Ru1 N31B 91.0(2) . . ?
N11B Ru1 N31B 94.8(2) . . ?
N11A Ru1 N31B 88.5(2) . . ?
N42B Ru1 N22B 99.7(2) . . ?
N22A Ru1 N22B 93.38(18) . . ?
N11B Ru1 N22B 77.01(19) . . ?
N11A Ru1 N22B 99.84(18) . . ?
N31B Ru1 N22B 171.2(2) . . ?
N42A Co2 N42A 101.1(3) . 2_665 ?
N42A Co2 N42A 101.1(3) . 3_565 ?
N42A Co2 N42A 101.1(4) 2_665 3_565 ?
N42A Co2 N31A 168.9(2) . 3_565 ?
N42A Co2 N31A 90.0(4) 2_665 3_565 ?
N42A Co2 N31A 75.9(4) 3_565 3_565 ?
N42A Co2 N31A 90.03(19) . 2_665 ?
N42A Co2 N31A 75.9(3) 2_665 2_665 ?
N42A Co2 N31A 168.9(4) 3_565 2_665 ?
N31A Co2 N31A 93.3(2) 3_565 2_665 ?
N42A Co2 N31A 75.89(19) . . ?
N42A Co2 N31A 168.9(3) 2_665 . ?
N42A Co2 N31A 90.0(4) 3_565 . ?
N31A Co2 N31A 93.3(2) 3_565 . ?
N31A Co2 N31A 93.3(2) 2_665 . ?
C12A N11A C16A 120.0 . . ?
C12A N11A Ru1 115.2(3) . . ?
C16A N11A Ru1 124.8(3) . . ?
C23A C12A N11A 115.8(5) . . ?
C23A C12A C13A 124.0(5) . . ?
N11A C12A C13A 120.0 . . ?
C12A C13A C14A 120.0 . . ?
C12A C13A H13A 120.0 . . ?
C14A C13A H13A 120.0 . . ?
C15A C14A C13A 120.0 . . ?
C15A C14A H14A 120.0 . . ?
C13A C14A H14A 120.0 . . ?
C14A C15A C16A 120.0 . . ?
C14A C15A H15A 120.0 . . ?
C16A C15A H15A 120.0 . . ?
C15A C16A N11A 120.0 . . ?
C15A C16A H16A 120.0 . . ?
N11A C16A H16A 120.0 . . ?
C26A N21A C25A 127.7(5) . . ?
C26A N21A N22A 123.8(5) . . ?
C25A N21A N22A 108.0 . . ?
C23A N22A N21A 108.0 . . ?
C23A N22A Ru1 113.1(3) . . ?
N21A N22A Ru1 138.3(3) . . ?
C12A C23A N22A 118.3(5) . . ?
C12A C23A C24A 133.7(5) . . ?
N22A C23A C24A 108.0 . . ?
C23A C24A C25A 108.0 . . ?
C23A C24A H24A 126.0 . . ?
C25A C24A H24A 126.0 . . ?
N21A C25A C24A 108.0 . . ?
N21A C25A H25A 126.0 . . ?
C24A C25A H25A 126.0 . . ?
N21A C26A C51A 114.3(5) . . ?
N21A C26A H26A 108.7 . . ?
C51A C26A H26A 108.7 . . ?
N21A C26A H26B 108.7 . . ?
C51A C26A H26B 108.7 . . ?
H26A C26A H26B 107.6 . . ?
C32A N31A C36A 120.0 . . ?
C32A N31A Co2 116.0(3) . . ?
C36A N31A Co2 124.0(3) . . ?
C43A C32A N31A 115.8(4) . . ?
C43A C32A C33A 124.2(4) . . ?
N31A C32A C33A 120.0 . . ?
C34A C33A C32A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C36A C35A C34A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C35A C36A N31A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
N31A C36A H36A 120.0 . . ?
C46A N41A C45A 128.2(4) . . ?
C46A N41A N42A 123.8(4) . . ?
C45A N41A N42A 108.0 . . ?
C43A N42A N41A 108.0 . . ?
C43A N42A Co2 114.3(3) . . ?
N41A N42A Co2 137.4(3) . . ?
C32A C43A N42A 117.6(4) . . ?
C32A C43A C44A 134.4(4) . . ?
N42A C43A C44A 108.0 . . ?
C43A C44A C45A 108.0 . . ?
C43A C44A H44A 126.0 . . ?
C45A C44A H44A 126.0 . . ?
N41A C45A C44A 108.0 . . ?
N41A C45A H45A 126.0 . . ?
C44A C45A H45A 126.0 . . ?
N41A C46A C64A 114.2(5) . . ?
N41A C46A H46A 108.7 . . ?
C64A C46A H46A 108.7 . . ?
N41A C46A H46B 108.7 . . ?
C64A C46A H46B 108.7 . . ?
H46A C46A H46B 107.6 . . ?
C52A C51A C56A 120.0 . . ?
C52A C51A C26A 118.1(3) . . ?
C56A C51A C26A 121.9(3) . . ?
C53A C52A C51A 120.0 . . ?
C53A C52A H52A 120.0 . . ?
C51A C52A H52A 120.0 . . ?
C52A C53A C54A 120.0 . . ?
C52A C53A H53A 120.0 . . ?
C54A C53A H53A 120.0 . . ?
C55A C54A C53A 120.0 . . ?
C55A C54A H54A 120.0 . . ?
C53A C54A H54A 120.0 . . ?
C54A C55A C56A 120.0 . . ?
C54A C55A C64A 120.0 . . ?
C56A C55A C64A 120.0 . . ?
C55A C56A C61A 120.0 . . ?
C55A C56A C51A 120.0 . . ?
C61A C56A C51A 120.0 . . ?
C62A C61A C56A 120.0 . . ?
C62A C61A H61A 120.0 . . ?
C56A C61A H61A 120.0 . . ?
C63A C62A C61A 120.0 . . ?
C63A C62A H62A 120.0 . . ?
C61A C62A H62A 120.0 . . ?
C64A C63A C62A 120.0 . . ?
C64A C63A H63A 120.0 . . ?
C62A C63A H63A 120.0 . . ?
C63A C64A C55A 120.0 . . ?
C63A C64A C46A 121.2(3) . . ?
C55A C64A C46A 118.8(3) . . ?
C12B N11B C16B 120.0 . . ?
C12B N11B Ru1 115.8(3) . . ?
C16B N11B Ru1 124.2(3) . . ?
C23B C12B C13B 124.3(4) . . ?
C23B C12B N11B 115.6(4) . . ?
C13B C12B N11B 120.0 . . ?
C14B C13B C12B 120.0 . . ?
C14B C13B H13B 120.0 . . ?
C12B C13B H13B 120.0 . . ?
C13B C14B C15B 120.0 . . ?
C13B C14B H14B 120.0 . . ?
C15B C14B H14B 120.0 . . ?
C14B C15B C16B 120.0 . . ?
C14B C15B H15B 120.0 . . ?
C16B C15B H15B 120.0 . . ?
C15B C16B N11B 120.0 . . ?
C15B C16B H16B 120.0 . . ?
N11B C16B H16B 120.0 . . ?
C26B N21B N22B 124.7(4) . . ?
C26B N21B C25B 127.3(4) . . ?
N22B N21B C25B 108.0 . . ?
N21B N22B C23B 108.0 . . ?
N21B N22B Ru1 139.0(3) . . ?
C23B N22B Ru1 113.0(3) . . ?
C12B C23B C24B 133.7(4) . . ?
C12B C23B N22B 118.2(4) . . ?
C24B C23B N22B 108.0 . . ?
C23B C24B C25B 108.0 . . ?
C23B C24B H24B 126.0 . . ?
C25B C24B H24B 126.0 . . ?
N21B C25B C24B 108.0 . . ?
N21B C25B H25B 126.0 . . ?
C24B C25B H25B 126.0 . . ?
N21B C26B C51B 114.2(5) . . ?
N21B C26B H26C 108.7 . . ?
C51B C26B H26C 108.7 . . ?
N21B C26B H26D 108.7 . . ?
C51B C26B H26D 108.7 . . ?
H26C C26B H26D 107.6 . . ?
C32B N31B C36B 120.0 . . ?
C32B N31B Ru1 115.4(3) . . ?
C36B N31B Ru1 124.6(3) . . ?
C43B C32B C33B 124.2(5) . . ?
C43B C32B N31B 115.8(5) . . ?
C33B C32B N31B 120.0 . . ?
C32B C33B C34B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C34B C35B C36B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C35B C36B N31B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
N31B C36B H36B 120.0 . . ?
C46B N41B N42B 122.7(5) . . ?
C46B N41B C45B 129.1(5) . . ?
N42B N41B C45B 108.0 . . ?
C43B N42B N41B 108.0 . . ?
C43B N42B Ru1 114.4(3) . . ?
N41B N42B Ru1 137.6(3) . . ?
C32B C43B N42B 117.4(5) . . ?
C32B C43B C44B 134.5(5) . . ?
N42B C43B C44B 108.0 . . ?
C45B C44B C43B 108.0 . . ?
C45B C44B H44B 126.0 . . ?
C43B C44B H44B 126.0 . . ?
C44B C45B N41B 108.0 . . ?
C44B C45B H45B 126.0 . . ?
N41B C45B H45B 126.0 . . ?
N41B C46B C64B 115.9(7) . 14_455 ?
N41B C46B H46C 108.3 . . ?
C64B C46B H46C 108.3 14_455 . ?
N41B C46B H46D 108.3 . . ?
C64B C46B H46D 108.3 14_455 . ?
H46C C46B H46D 107.4 . . ?
C52B C51B C56B 120.0 . . ?
C52B C51B C26B 117.7(3) . . ?
C56B C51B C26B 121.9(3) . . ?
C53B C52B C51B 120.0 . . ?
C53B C52B H52B 120.0 . . ?
C51B C52B H52B 120.0 . . ?
C52B C53B C54B 120.0 . . ?
C52B C53B H53B 120.0 . . ?
C54B C53B H53B 120.0 . . ?
C55B C54B C53B 120.0 . . ?
C55B C54B H54B 120.0 . . ?
C53B C54B H54B 120.0 . . ?
C54B C55B C56B 120.0 . . ?
C54B C55B C64B 120.0 . . ?
C56B C55B C64B 120.0 . . ?
C61B C56B C55B 120.0 . . ?
C61B C56B C51B 120.0 . . ?
C55B C56B C51B 120.0 . . ?
C56B C61B C62B 120.0 . . ?
C56B C61B H61B 120.0 . . ?
C62B C61B H61B 120.0 . . ?
C63B C62B C61B 120.0 . . ?
C63B C62B H62B 120.0 . . ?
C61B C62B H62B 120.0 . . ?
C64B C63B C62B 120.0 . . ?
C64B C63B H63B 120.0 . . ?
C62B C63B H63B 120.0 . . ?
C63B C64B C55B 120.0 . . ?
C63B C64B C46B 120.9(3) . 15 ?
C55B C64B C46B 119.1(3) . 15 ?
F2 B1 F4 112.3(10) . . ?
F2 B1 F3 107.9(10) . . ?
F4 B1 F3 107.2(8) . . ?
F2 B1 F1 112.0(8) . . ?
F4 B1 F1 106.6(10) . . ?
F3 B1 F1 110.8(10) . . ?
F13 B11 F11 114.0(11) . . ?
F13 B11 F12 109.7(12) . . ?
F11 B11 F12 109.8(11) . . ?
F13 B11 F14 106.9(12) . . ?
F11 B11 F14 109.2(12) . . ?
F12 B11 F14 107.1(10) . . ?
O3S N1S O2S 125.1(10) . . ?
O3S N1S C4S 115.9(9) . . ?
O2S N1S C4S 118.7(9) . . ?
N1S C4S H4S1 109.5 . . ?
N1S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
N1S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?

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
C16A N11A C12A C23A 176.3(5) . . . . ?
Ru1 N11A C12A C23A -4.2(4) . . . . ?
C16A N11A C12A C13A 0.0 . . . . ?
Ru1 N11A C12A C13A 179.6(3) . . . . ?
C23A C12A C13A C14A -176.0(5) . . . . ?
N11A C12A C13A C14A 0.0 . . . . ?
C12A C13A C14A C15A 0.0 . . . . ?
C13A C14A C15A C16A 0.0 . . . . ?
C14A C15A C16A N11A 0.0 . . . . ?
C12A N11A C16A C15A 0.0 . . . . ?
Ru1 N11A C16A C15A -179.5(3) . . . . ?
C26A N21A N22A C23A -172.1(6) . . . . ?
C25A N21A N22A C23A 0.0 . . . . ?
C26A N21A N22A Ru1 17.8(7) . . . . ?
C25A N21A N22A Ru1 -170.0(5) . . . . ?
N11A C12A C23A N22A 6.4(5) . . . . ?
C13A C12A C23A N22A -177.4(3) . . . . ?
N11A C12A C23A C24A -171.4(4) . . . . ?
C13A C12A C23A C24A 4.7(7) . . . . ?
N21A N22A C23A C12A -178.4(5) . . . . ?
Ru1 N22A C23A C12A -5.6(5) . . . . ?
N21A N22A C23A C24A 0.0 . . . . ?
Ru1 N22A C23A C24A 172.8(3) . . . . ?
C12A C23A C24A C25A 178.0(6) . . . . ?
N22A C23A C24A C25A 0.0 . . . . ?
C26A N21A C25A C24A 171.7(6) . . . . ?
N22A N21A C25A C24A 0.0 . . . . ?
C23A C24A C25A N21A 0.0 . . . . ?
C25A N21A C26A C51A -84.8(7) . . . . ?
N22A N21A C26A C51A 85.7(7) . . . . ?
C36A N31A C32A C43A -178.2(5) . . . . ?
Co2 N31A C32A C43A 3.6(5) . . . . ?
C36A N31A C32A C33A 0.0 . . . . ?
Co2 N31A C32A C33A -178.2(4) . . . . ?
C43A C32A C33A C34A 178.1(6) . . . . ?
N31A C32A C33A C34A 0.0 . . . . ?
C32A C33A C34A C35A 0.0 . . . . ?
C33A C34A C35A C36A 0.0 . . . . ?
C34A C35A C36A N31A 0.0 . . . . ?
C32A N31A C36A C35A 0.0 . . . . ?
Co2 N31A C36A C35A 178.0(4) . . . . ?
C46A N41A N42A C43A -178.9(5) . . . . ?
C45A N41A N42A C43A 0.0 . . . . ?
C46A N41A N42A Co2 7.7(6) . . . . ?
C45A N41A N42A Co2 -173.4(4) . . . . ?
N31A C32A C43A N42A 1.2(6) . . . . ?
C33A C32A C43A N42A -176.9(3) . . . . ?
N31A C32A C43A C44A -179.5(4) . . . . ?
C33A C32A C43A C44A 2.3(7) . . . . ?
N41A N42A C43A C32A 179.4(5) . . . . ?
Co2 N42A C43A C32A -5.5(5) . . . . ?
N41A N42A C43A C44A 0.0 . . . . ?
Co2 N42A C43A C44A 175.1(3) . . . . ?
C32A C43A C44A C45A -179.3(6) . . . . ?
N42A C43A C44A C45A 0.0 . . . . ?
C46A N41A C45A C44A 178.8(6) . . . . ?
N42A N41A C45A C44A 0.0 . . . . ?
C43A C44A C45A N41A 0.0 . . . . ?
C45A N41A C46A C64A 90.7(6) . . . . ?
N42A N41A C46A C64A -90.6(6) . . . . ?
N21A C26A C51A C52A 1.9(7) . . . . ?
N21A C26A C51A C56A -179.1(4) . . . . ?
C56A C51A C52A C53A 0.0 . . . . ?
C26A C51A C52A C53A 179.0(4) . . . . ?
C51A C52A C53A C54A 0.0 . . . . ?
C52A C53A C54A C55A 0.0 . . . . ?
C53A C54A C55A C56A 0.0 . . . . ?
C53A C54A C55A C64A 180.0 . . . . ?
C54A C55A C56A C61A 180.0 . . . . ?
C64A C55A C56A C61A 0.0 . . . . ?
C54A C55A C56A C51A 0.0 . . . . ?
C64A C55A C56A C51A 180.0 . . . . ?
C52A C51A C56A C55A 0.0 . . . . ?
C26A C51A C56A C55A -179.0(5) . . . . ?
C52A C51A C56A C61A 180.0 . . . . ?
C26A C51A C56A C61A 1.0(5) . . . . ?
C55A C56A C61A C62A 0.0 . . . . ?
C51A C56A C61A C62A 180.0 . . . . ?
C56A C61A C62A C63A 0.0 . . . . ?
C61A C62A C63A C64A 0.0 . . . . ?
C62A C63A C64A C55A 0.0 . . . . ?
C62A C63A C64A C46A 176.8(4) . . . . ?
C54A C55A C64A C63A 180.0 . . . . ?
C56A C55A C64A C63A 0.0 . . . . ?
C54A C55A C64A C46A 3.1(4) . . . . ?
C56A C55A C64A C46A -176.9(4) . . . . ?
N41A C46A C64A C63A -6.8(7) . . . . ?
N41A C46A C64A C55A 170.0(4) . . . . ?
C16B N11B C12B C23B 176.3(5) . . . . ?
Ru1 N11B C12B C23B -4.6(4) . . . . ?
C16B N11B C12B C13B 0.0 . . . . ?
Ru1 N11B C12B C13B 179.1(3) . . . . ?
C23B C12B C13B C14B -175.9(5) . . . . ?
N11B C12B C13B C14B 0.0 . . . . ?
C12B C13B C14B C15B 0.0 . . . . ?
C13B C14B C15B C16B 0.0 . . . . ?
C14B C15B C16B N11B 0.0 . . . . ?
C12B N11B C16B C15B 0.0 . . . . ?
Ru1 N11B C16B C15B -179.0(3) . . . . ?
C26B N21B N22B C23B -178.6(6) . . . . ?
C25B N21B N22B C23B 0.0 . . . . ?
C26B N21B N22B Ru1 0.1(7) . . . . ?
C25B N21B N22B Ru1 178.8(5) . . . . ?
C13B C12B C23B C24B 0.4(7) . . . . ?
N11B C12B C23B C24B -175.7(4) . . . . ?
C13B C12B C23B N22B 176.6(3) . . . . ?
N11B C12B C23B N22B 0.5(5) . . . . ?
N21B N22B C23B C12B -177.1(5) . . . . ?
Ru1 N22B C23B C12B 3.7(5) . . . . ?
N21B N22B C23B C24B 0.0 . . . . ?
Ru1 N22B C23B C24B -179.1(3) . . . . ?
C12B C23B C24B C25B 176.5(6) . . . . ?
N22B C23B C24B C25B 0.0 . . . . ?
C26B N21B C25B C24B 178.6(6) . . . . ?
N22B N21B C25B C24B 0.0 . . . . ?
C23B C24B C25B N21B 0.0 . . . . ?
N22B N21B C26B C51B 91.1(6) . . . . ?
C25B N21B C26B C51B -87.2(6) . . . . ?
C36B N31B C32B C43B 178.5(6) . . . . ?
Ru1 N31B C32B C43B -0.3(6) . . . . ?
C36B N31B C32B C33B 0.0 . . . . ?
Ru1 N31B C32B C33B -178.7(4) . . . . ?
C43B C32B C33B C34B -178.3(7) . . . . ?
N31B C32B C33B C34B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B N31B 0.0 . . . . ?
C32B N31B C36B C35B 0.0 . . . . ?
Ru1 N31B C36B C35B 178.6(4) . . . . ?
C46B N41B N42B C43B 175.5(7) . . . . ?
C45B N41B N42B C43B 0.0 . . . . ?
C46B N41B N42B Ru1 -4.2(8) . . . . ?
C45B N41B N42B Ru1 -179.6(6) . . . . ?
C33B C32B C43B N42B 177.1(4) . . . . ?
N31B C32B C43B N42B -1.3(7) . . . . ?
C33B C32B C43B C44B 0.5(9) . . . . ?
N31B C32B C43B C44B -177.9(5) . . . . ?
N41B N42B C43B C32B -177.5(6) . . . . ?
Ru1 N42B C43B C32B 2.3(6) . . . . ?
N41B N42B C43B C44B 0.0 . . . . ?
Ru1 N42B C43B C44B 179.7(4) . . . . ?
C32B C43B C44B C45B 176.8(8) . . . . ?
N42B C43B C44B C45B 0.0 . . . . ?
C43B C44B C45B N41B 0.0 . . . . ?
C46B N41B C45B C44B -175.1(7) . . . . ?
N42B N41B C45B C44B 0.0 . . . . ?
N42B N41B C46B C64B 93.6(10) . . . 14_455 ?
C45B N41B C46B C64B -91.9(10) . . . 14_455 ?
N21B C26B C51B C52B 0.3(7) . . . . ?
N21B C26B C51B C56B -172.4(4) . . . . ?
C56B C51B C52B C53B 0.0 . . . . ?
C26B C51B C52B C53B -172.8(4) . . . . ?
C51B C52B C53B C54B 0.0 . . . . ?
C52B C53B C54B C55B 0.0 . . . . ?
C53B C54B C55B C56B 0.0 . . . . ?
C53B C54B C55B C64B 180.0 . . . . ?
C54B C55B C56B C61B 180.0 . . . . ?
C64B C55B C56B C61B 0.0 . . . . ?
C54B C55B C56B C51B 0.0 . . . . ?
C64B C55B C56B C51B 180.0 . . . . ?
C52B C51B C56B C61B 180.0 . . . . ?
C26B C51B C56B C61B -7.5(4) . . . . ?
C52B C51B C56B C55B 0.0 . . . . ?
C26B C51B C56B C55B 172.5(4) . . . . ?
C55B C56B C61B C62B 0.0 . . . . ?
C51B C56B C61B C62B 180.0 . . . . ?
C56B C61B C62B C63B 0.0 . . . . ?
C61B C62B C63B C64B 0.0 . . . . ?
C62B C63B C64B C55B 0.0 . . . . ?
C62B C63B C64B C46B 179.7(5) . . . 15 ?
C54B C55B C64B C63B 180.0 . . . . ?
C56B C55B C64B C63B 0.0 . . . . ?
C54B C55B C64B C46B 0.3(5) . . . 15 ?
C56B C55B C64B C46B -179.7(5) . . . 15 ?

_refine_diff_density_max         0.532
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.073

_shelxl_version_number           2013-4

#===END

