# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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/. 
# 
# 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_1-co3
_database_code_depnum_ccdc_archive 'CCDC 823183'
_audit_update_record             
;
2014-12-09 deposited with the CCDC.
2014-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Co3-BPh4
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C100 H92 B2 Co3 N8 O8'
_chemical_formula_weight         1732.23

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5855(5)
_cell_length_b                   14.4488(6)
_cell_length_c                   15.1235(8)
_cell_angle_alpha                72.292(2)
_cell_angle_beta                 67.952(2)
_cell_angle_gamma                69.590(2)
_cell_volume                     2154.99(17)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20303
_cell_measurement_theta_min      3.395
_cell_measurement_theta_max      27.485

_exptl_crystal_description       Plate
_exptl_crystal_colour            Brown
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             903
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8575
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean 0.76
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29358
_diffrn_reflns_av_R_equivalents  0.1345
_diffrn_reflns_av_unetl/netl     0.1896
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         25.03
_reflns_number_total             7538
_reflns_number_gt                3147
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  CrystalMaker

_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. 
Refinement for the lattice solvent atoms (O1s, C1s, C1s') are restrainted as following:
ISOR 0.01 O1S > C1s'
DELU 0.01 O1s > C1s'
SIMU 0.01 O1s > C1s' 
The final RES filed was also attached here:
TITL a in P-1
CELL 0.71073  11.58550  14.44880  15.12350  72.2917  67.9520  69.5903
ZERR    1.00   0.00050   0.00059   0.00080   0.0021   0.0022   0.0021
LATT  1
SFAC C H B N O CO
UNIT 100 92 2 8 8 3
ACTA
SHEL 6 0.84
SIZE 0.25 0.14 0.04
L.S. 8
Temp 20
BOND
FMAP 2
PLAN 5
ISOR 0.01 O1S > C1s'
DELU 0.01 O1s > C1s'
SIMU 0.01 O1s > C1s'
WGHT    0.037900
FVAR       0.11704
CO1   6    0.000000    0.000000    0.500000    10.50000    0.04288    0.05747 =
         0.03861   -0.00913   -0.01009   -0.01993
CO2   6   -0.049451   -0.200159    0.522617    11.00000    0.05446    0.06022 =
         0.04682   -0.00854   -0.01519   -0.02272
O1    5    0.157350    0.049887    0.465396    11.00000    0.04008    0.06099 =
         0.04437   -0.01328   -0.00807   -0.01923
O2    5    0.085705   -0.157231    0.544951    11.00000    0.04878    0.05551 =
         0.04295   -0.00149   -0.01904   -0.01899
O3    5    0.075027   -0.341315    0.486918    11.00000    0.07475    0.06524 =
         0.08046   -0.02221   -0.01143   -0.00936
N1    4    0.068540   -0.031591    0.358027    11.00000    0.03718    0.05394 =
         0.03715   -0.01140   -0.00797   -0.01873
N2    4   -0.050930   -0.143195    0.378334    11.00000    0.04914    0.05885 =
         0.04746   -0.01319   -0.01498   -0.01769
N3    4   -0.104325   -0.259768    0.666266    11.00000    0.05161    0.06222 =
         0.04517   -0.00357   -0.01483   -0.02610
N4    4   -0.222270   -0.280074    0.589788    11.00000    0.05357    0.08468 =
         0.06066   -0.01619   -0.01966   -0.03155
B1    3   -0.377157   -0.311960    1.091602    11.00000    0.04144    0.03928 =
         0.05155   -0.00585   -0.01558   -0.01351
C1    1    0.270333    0.029262    0.394677    11.00000    0.04227    0.05071 =
         0.04832   -0.00382   -0.01476   -0.01709
C2    1    0.379010    0.041221    0.403089    11.00000    0.05064    0.07576 =
         0.06494   -0.01701   -0.01591   -0.02478
AFIX  43
H2A   2    0.373274    0.061036    0.457961    11.00000   -1.20000
AFIX   0
C3    1    0.496217    0.023989    0.330649    11.00000    0.04122    0.07473 =
         0.09932   -0.01174   -0.01645   -0.02823
AFIX  43
H3A   2    0.568672    0.031015    0.338089    11.00000   -1.20000
AFIX   0
C4    1    0.506759   -0.003428    0.247723    11.00000    0.04958    0.07953 =
         0.06637   -0.01831   -0.00284   -0.02198
AFIX  43
H4A   2    0.585009   -0.012693    0.198378    11.00000   -1.20000
AFIX   0
C5    1    0.401037   -0.016805    0.238911    11.00000    0.04591    0.07025 =
         0.05649   -0.01528   -0.00367   -0.01927
AFIX  43
H5A   2    0.408052   -0.035170    0.182888    11.00000   -1.20000
AFIX   0
C6    1    0.281819   -0.003528    0.312366    11.00000    0.04116    0.05666 =
         0.04129   -0.00916   -0.01203   -0.01394
C7    1    0.180479   -0.026674    0.297838    11.00000    0.05197    0.05925 =
         0.03888   -0.01101   -0.01443   -0.01367
AFIX  43
H7A   2    0.197869   -0.039863    0.236973    11.00000   -1.20000
AFIX   0
C8    1   -0.009927   -0.060654    0.323184    11.00000    0.04558    0.05586 =
         0.03997   -0.01688   -0.01114   -0.00784
C9    1   -0.042499   -0.007273    0.239264    11.00000    0.06328    0.06898 =
         0.04413   -0.01055   -0.01938   -0.01394
AFIX  43
H9A   2   -0.014388    0.049872    0.203320    11.00000   -1.20000
AFIX   0
C10   1   -0.117815   -0.040867    0.210087    11.00000    0.05979    0.09491 =
         0.05880   -0.02224   -0.02804   -0.01311
AFIX  43
H10A  2   -0.142210   -0.005548    0.154456    11.00000   -1.20000
AFIX   0
C11   1   -0.157078   -0.127015    0.263483    11.00000    0.06507    0.09944 =
         0.06440   -0.02419   -0.02329   -0.02954
AFIX  43
H11A  2   -0.204917   -0.152291    0.243556    11.00000   -1.20000
AFIX   0
C12   1   -0.122670   -0.173463    0.346737    11.00000    0.06420    0.07732 =
         0.06058   -0.02353   -0.01628   -0.03099
AFIX  43
H12A  2   -0.151176   -0.230109    0.384024    11.00000   -1.20000
AFIX   0
C13   1    0.127109   -0.191616    0.622158    11.00000    0.04461    0.04526 =
         0.06240   -0.00997   -0.01961   -0.01051
C14   1    0.242988   -0.175365    0.615685    11.00000    0.05629    0.05597 =
         0.07273   -0.00001   -0.02842   -0.01537
AFIX  43
H14A  2    0.287972   -0.141280    0.557171    11.00000   -1.20000
AFIX   0
C15   1    0.292316   -0.208411    0.693500    11.00000    0.06422    0.05950 =
         0.11521   -0.00377   -0.05305   -0.01843
AFIX  43
H15A  2    0.370216   -0.197276    0.685794    11.00000   -1.20000
AFIX   0
C16   1    0.228067   -0.257541    0.782245    11.00000    0.10557    0.06340 =
         0.08888    0.00454   -0.06090   -0.03360
AFIX  43
H16A  2    0.260847   -0.278614    0.834702    11.00000   -1.20000
AFIX   0
C17   1    0.115210   -0.274459    0.791161    11.00000    0.08336    0.07144 =
         0.06211   -0.00252   -0.03341   -0.02820
AFIX  43
H17A  2    0.071332   -0.307768    0.850742    11.00000   -1.20000
AFIX   0
C18   1    0.062863   -0.243314    0.713446    11.00000    0.05559    0.05968 =
         0.05451   -0.00341   -0.02469   -0.02070
C19   1   -0.052596   -0.271994    0.731478    11.00000    0.06607    0.07140 =
         0.04672   -0.01006   -0.00900   -0.02355
AFIX  43
H19A  2   -0.091928   -0.301333    0.794816    11.00000   -1.20000
AFIX   0
C20   1   -0.208238   -0.297141    0.677901    11.00000    0.04855    0.05765 =
         0.06145   -0.00770   -0.01816   -0.01619
C21   1   -0.282397   -0.344587    0.762472    11.00000    0.05620    0.09123 =
         0.06110    0.00354   -0.01656   -0.03205
AFIX  43
H21A  2   -0.269836   -0.353710    0.822111    11.00000   -1.20000
AFIX   0
C22   1   -0.375645   -0.377979    0.755589    11.00000    0.06836    0.11345 =
         0.07751    0.00485   -0.01998   -0.04406
AFIX  43
H22A  2   -0.428209   -0.409977    0.811035    11.00000   -1.20000
AFIX   0
C23   1   -0.390301   -0.363711    0.666630    11.00000    0.07202    0.10555 =
         0.10165   -0.01742   -0.02735   -0.04076
AFIX  43
H23A  2   -0.452282   -0.386429    0.660498    11.00000   -1.20000
AFIX   0
C24   1   -0.311788   -0.315071    0.585896    11.00000    0.07829    0.12055 =
         0.07799   -0.02583   -0.01902   -0.04193
AFIX  43
H24A  2   -0.322067   -0.306308    0.525514    11.00000   -1.20000
AFIX   0
C25   1   -0.299174   -0.403625    1.031149    11.00000    0.04273    0.03565 =
         0.04302    0.00226   -0.01908   -0.01447
C26   1   -0.362492   -0.470731    1.032310    11.00000    0.04550    0.04490 =
         0.06398   -0.01194   -0.01255   -0.01361
AFIX  43
H26A  2   -0.450129   -0.460413    1.065988    11.00000   -1.20000
AFIX   0
C27   1   -0.301039   -0.551966    0.985697    11.00000    0.07115    0.04546 =
         0.08106   -0.01008   -0.03572   -0.01499
AFIX  43
H27A  2   -0.347398   -0.594586    0.988720    11.00000   -1.20000
AFIX   0
C28   1   -0.171382   -0.569482    0.934950    11.00000    0.06496    0.04447 =
         0.08153   -0.02302   -0.02899   -0.00120
AFIX  43
H28A  2   -0.129773   -0.623799    0.903545    11.00000   -1.20000
AFIX   0
C29   1   -0.104061   -0.505883    0.931170    11.00000    0.05197    0.05599 =
         0.06624   -0.01955   -0.01916   -0.00841
AFIX  43
H29A  2   -0.016564   -0.516727    0.896908    11.00000   -1.20000
AFIX   0
C30   1   -0.167657   -0.425107    0.978955    11.00000    0.04240    0.04838 =
         0.05643   -0.00750   -0.02103   -0.01409
AFIX  43
H30A  2   -0.120245   -0.383315    0.976006    11.00000   -1.20000
AFIX   0
C31   1   -0.298764   -0.225123    1.055122    11.00000    0.03701    0.04024 =
         0.04351   -0.01059   -0.01289   -0.00946
C32   1   -0.342363   -0.125589    1.010231    11.00000    0.04728    0.04989 =
         0.05454   -0.00767   -0.02065   -0.01886
AFIX  43
H32A  2   -0.421026   -0.106023    0.997617    11.00000   -1.20000
AFIX   0
C33   1   -0.180789   -0.247059    1.072057    11.00000    0.05479    0.04329 =
         0.07095   -0.01221   -0.02584   -0.01241
AFIX  43
H33A  2   -0.148425   -0.311357    1.104747    11.00000   -1.20000
AFIX   0
C34   1   -0.109800   -0.177613    1.042477    11.00000    0.04158    0.07079 =
         0.09187   -0.02867   -0.01720   -0.02166
AFIX  43
H34A  2   -0.029713   -0.196967    1.052814    11.00000   -1.20000
AFIX   0
C35   1   -0.155744   -0.081233    0.998398    11.00000    0.06525    0.06205 =
         0.06038   -0.01217   -0.00891   -0.03793
AFIX  43
H35A  2   -0.108003   -0.034517    0.978774    11.00000   -1.20000
AFIX   0
C36   1   -0.274180   -0.054241    0.983426    11.00000    0.06891    0.04366 =
         0.05340   -0.00143   -0.01961   -0.02313
AFIX  43
H36A  2   -0.308523    0.011810    0.955347    11.00000   -1.20000
AFIX   0
C37   1   -0.431731   -0.290756    1.271772    11.00000    0.08550    0.07030 =
         0.06447   -0.01849   -0.02491   -0.01533
AFIX  43
H37A  2   -0.455248   -0.221841    1.247316    11.00000   -1.20000
AFIX   0
C38   1   -0.441499   -0.323672    1.369556    11.00000    0.11026    0.10476 =
         0.06436   -0.02645   -0.02816   -0.02575
AFIX  43
H38A  2   -0.472019   -0.277009    1.409463    11.00000   -1.20000
AFIX   0
C39   1   -0.406779   -0.423877    1.407879    11.00000    0.13140    0.12305 =
         0.05501    0.00594   -0.03859   -0.05597
AFIX  43
H39A  2   -0.411783   -0.446347    1.473398    11.00000   -1.20000
AFIX   0
C40   1   -0.364111   -0.491114    1.347364    11.00000    0.14486    0.08195 =
         0.06923    0.01609   -0.04351   -0.04900
AFIX  43
H40A  2   -0.341745   -0.559927    1.372566    11.00000   -1.20000
AFIX   0
C41   1   -0.354095   -0.457716    1.249762    11.00000    0.08771    0.06182 =
         0.05415    0.00240   -0.02679   -0.02785
AFIX  43
H41A  2   -0.323348   -0.504989    1.210467    11.00000   -1.20000
AFIX   0
C42   1   -0.387932   -0.356959    1.208315    11.00000    0.04927    0.05248 =
         0.05124   -0.00852   -0.01482   -0.01590
C43   1   -0.519985   -0.264203    1.075189    11.00000    0.04036    0.03539 =
         0.06637   -0.01746   -0.01409   -0.01131
C44   1   -0.637835   -0.259896    1.149024    11.00000    0.04487    0.06878 =
         0.08386   -0.02977   -0.00543   -0.01522
AFIX  43
H44A  2   -0.637709   -0.282636    1.213511    11.00000   -1.20000
AFIX   0
C45   1   -0.755492   -0.222546    1.128876    11.00000    0.03813    0.06467 =
         0.13327   -0.04378   -0.00205   -0.01304
AFIX  43
H45A  2   -0.831990   -0.221242    1.179890    11.00000   -1.20000
AFIX   0
C46   1   -0.759967   -0.188348    1.036659    11.00000    0.05465    0.04961 =
         0.17269   -0.02586   -0.05493   -0.01214
AFIX  43
H46A  2   -0.838983   -0.163360    1.023934    11.00000   -1.20000
AFIX   0
C47   1   -0.647645   -0.190636    0.961998    11.00000    0.07437    0.04872 =
         0.11114   -0.00937   -0.05413   -0.01987
AFIX  43
H47A  2   -0.649913   -0.166665    0.898051    11.00000   -1.20000
AFIX   0
C48   1   -0.530158   -0.228623    0.981288    11.00000    0.05416    0.04497 =
         0.07154   -0.01206   -0.03103   -0.01427
AFIX  43
H48A  2   -0.454764   -0.230414    0.929153    11.00000   -1.20000
AFIX   0
C49   1    0.209251   -0.342415    0.420928    11.00000    0.08863    0.13416 =
         0.09719   -0.01814    0.00038    0.01433
AFIX  33
H49A  2    0.255439   -0.409592    0.410401    11.00000   -1.50000
H49B  2    0.252964   -0.320493    0.450350    11.00000   -1.50000
H49C  2    0.205412   -0.297865    0.359723    11.00000   -1.50000
O1S   5    0.025311   -0.561215    0.684118    11.00000    0.30102    0.22091 =
         0.22630   -0.02677   -0.03755   -0.08284
PART   1
C1S   1    0.092171   -0.496135    0.641299    10.50000    0.10191    0.13174 =
         0.12041    0.03155   -0.06935   -0.02557
H1SA  2    0.112231   -0.478105    0.688879    10.50000   -1.50000
H1SB  2    0.170831   -0.524795    0.595327    10.50000   -1.50000
H1SC  2    0.043181   -0.437085    0.607818    10.50000   -1.50000
PART   2
C1S'  1    0.052371   -0.532934    0.588698    10.50000    0.17618    0.08442 =
         0.13975   -0.04864    0.00326   -0.03888
H1SD  2    0.015721   -0.567434    0.565299    10.50000   -1.50000
H1SE  2    0.016711   -0.461535    0.571898    10.50000   -1.50000
H1SF  2    0.144361   -0.549244    0.559409    10.50000   -1.50000
PART   0
 
HKLF               4
 
REM  a in P-1
REM R1 =  0.0484 for   3147 Fo > 4sig(Fo)  and  0.1626 for all   7538 data
REM    547 parameters refined using     38 restraints
 
END   
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0379P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7538
_refine_ls_number_parameters     547
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_restrained_S_all      0.870
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.0000 0.0000 0.5000 0.0452(3) Uani 1 2 d S . .
Co2 Co -0.04945(6) -0.20016(5) 0.52262(4) 0.0523(2) Uani 1 1 d . . .
O1 O 0.1573(2) 0.0499(2) 0.46540(18) 0.0476(8) Uani 1 1 d . . .
O2 O 0.0857(2) -0.1572(2) 0.54495(18) 0.0480(8) Uani 1 1 d . . .
O3 O 0.0750(3) -0.3413(2) 0.4869(2) 0.0779(10) Uani 1 1 d . . .
N1 N 0.0685(3) -0.0316(2) 0.3580(2) 0.0413(9) Uani 1 1 d . . .
N2 N -0.0509(3) -0.1432(3) 0.3783(2) 0.0501(10) Uani 1 1 d . . .
N3 N -0.1043(3) -0.2598(3) 0.6663(2) 0.0516(10) Uani 1 1 d . . .
N4 N -0.2223(4) -0.2801(3) 0.5898(3) 0.0614(11) Uani 1 1 d . . .
B1 B -0.3772(5) -0.3120(4) 1.0916(3) 0.0436(13) Uani 1 1 d . . .
C1 C 0.2703(4) 0.0293(3) 0.3947(3) 0.0469(11) Uani 1 1 d . . .
C2 C 0.3790(4) 0.0412(3) 0.4031(3) 0.0613(13) Uani 1 1 d . . .
H2A H 0.3733 0.0610 0.4580 0.074 Uiso 1 1 calc R . .
C3 C 0.4962(4) 0.0240(4) 0.3306(4) 0.0710(15) Uani 1 1 d . . .
H3A H 0.5687 0.0310 0.3381 0.085 Uiso 1 1 calc R . .
C4 C 0.5068(5) -0.0034(4) 0.2477(3) 0.0674(15) Uani 1 1 d . . .
H4A H 0.5850 -0.0127 0.1984 0.081 Uiso 1 1 calc R . .
C5 C 0.4010(4) -0.0168(3) 0.2389(3) 0.0595(13) Uani 1 1 d . . .
H5A H 0.4081 -0.0352 0.1829 0.071 Uiso 1 1 calc R . .
C6 C 0.2818(4) -0.0035(3) 0.3124(3) 0.0464(11) Uani 1 1 d . . .
C7 C 0.1805(4) -0.0267(3) 0.2978(3) 0.0498(12) Uani 1 1 d . . .
H7A H 0.1979 -0.0399 0.2370 0.060 Uiso 1 1 calc R . .
C8 C -0.0099(4) -0.0607(4) 0.3232(3) 0.0475(12) Uani 1 1 d . . .
C9 C -0.0425(4) -0.0073(4) 0.2393(3) 0.0590(13) Uani 1 1 d . . .
H9A H -0.0144 0.0499 0.2033 0.071 Uiso 1 1 calc R . .
C10 C -0.1178(4) -0.0409(4) 0.2101(3) 0.0685(15) Uani 1 1 d . . .
H10A H -0.1422 -0.0055 0.1545 0.082 Uiso 1 1 calc R . .
C11 C -0.1571(5) -0.1270(4) 0.2635(4) 0.0711(15) Uani 1 1 d . . .
H11A H -0.2049 -0.1523 0.2436 0.085 Uiso 1 1 calc R . .
C12 C -0.1227(4) -0.1735(4) 0.3467(3) 0.0623(14) Uani 1 1 d . . .
H12A H -0.1512 -0.2301 0.3840 0.075 Uiso 1 1 calc R . .
C13 C 0.1271(4) -0.1916(3) 0.6222(3) 0.0503(12) Uani 1 1 d . . .
C14 C 0.2430(5) -0.1754(3) 0.6157(3) 0.0619(13) Uani 1 1 d . . .
H14A H 0.2880 -0.1413 0.5572 0.074 Uiso 1 1 calc R . .
C15 C 0.2923(5) -0.2084(4) 0.6935(4) 0.0744(15) Uani 1 1 d . . .
H15A H 0.3702 -0.1973 0.6858 0.089 Uiso 1 1 calc R . .
C16 C 0.2281(6) -0.2575(4) 0.7822(4) 0.0778(16) Uani 1 1 d . . .
H16A H 0.2608 -0.2786 0.8347 0.093 Uiso 1 1 calc R . .
C17 C 0.1152(5) -0.2745(4) 0.7912(3) 0.0692(14) Uani 1 1 d . . .
H17A H 0.0713 -0.3078 0.8507 0.083 Uiso 1 1 calc R . .
C18 C 0.0629(4) -0.2433(3) 0.7134(3) 0.0545(12) Uani 1 1 d . . .
C19 C -0.0526(5) -0.2720(3) 0.7315(3) 0.0628(14) Uani 1 1 d . . .
H19A H -0.0919 -0.3013 0.7948 0.075 Uiso 1 1 calc R . .
C20 C -0.2082(4) -0.2971(3) 0.6779(3) 0.0558(13) Uani 1 1 d . . .
C21 C -0.2824(5) -0.3446(4) 0.7625(3) 0.0709(15) Uani 1 1 d . . .
H21A H -0.2698 -0.3537 0.8221 0.085 Uiso 1 1 calc R . .
C22 C -0.3756(5) -0.3780(4) 0.7556(4) 0.0872(18) Uani 1 1 d . . .
H22A H -0.4282 -0.4100 0.8110 0.105 Uiso 1 1 calc R . .
C23 C -0.3903(5) -0.3637(4) 0.6666(5) 0.0886(18) Uani 1 1 d . . .
H23A H -0.4523 -0.3864 0.6605 0.106 Uiso 1 1 calc R . .
C24 C -0.3118(5) -0.3151(4) 0.5859(4) 0.0878(18) Uani 1 1 d . . .
H24A H -0.3221 -0.3063 0.5255 0.105 Uiso 1 1 calc R . .
C25 C -0.2992(4) -0.4036(3) 1.0311(3) 0.0399(11) Uani 1 1 d . . .
C26 C -0.3625(4) -0.4707(3) 1.0323(3) 0.0520(12) Uani 1 1 d . . .
H26A H -0.4501 -0.4604 1.0660 0.062 Uiso 1 1 calc R . .
C27 C -0.3010(5) -0.5520(3) 0.9857(3) 0.0627(14) Uani 1 1 d . . .
H27A H -0.3474 -0.5946 0.9887 0.075 Uiso 1 1 calc R . .
C28 C -0.1714(5) -0.5695(3) 0.9349(3) 0.0628(14) Uani 1 1 d . . .
H28A H -0.1298 -0.6238 0.9035 0.075 Uiso 1 1 calc R . .
C29 C -0.1041(4) -0.5059(3) 0.9312(3) 0.0575(13) Uani 1 1 d . . .
H29A H -0.0166 -0.5167 0.8969 0.069 Uiso 1 1 calc R . .
C30 C -0.1677(4) -0.4251(3) 0.9790(3) 0.0473(11) Uani 1 1 d . . .
H30A H -0.1202 -0.3833 0.9760 0.057 Uiso 1 1 calc R . .
C31 C -0.2988(4) -0.2251(3) 1.0551(3) 0.0397(11) Uani 1 1 d . . .
C32 C -0.3424(4) -0.1256(4) 1.0102(3) 0.0479(12) Uani 1 1 d . . .
H32A H -0.4210 -0.1060 0.9976 0.058 Uiso 1 1 calc R . .
C33 C -0.1808(4) -0.2471(3) 1.0721(3) 0.0542(12) Uani 1 1 d . . .
H33A H -0.1484 -0.3114 1.1047 0.065 Uiso 1 1 calc R . .
C34 C -0.1098(4) -0.1776(4) 1.0425(3) 0.0640(14) Uani 1 1 d . . .
H34A H -0.0297 -0.1970 1.0528 0.077 Uiso 1 1 calc R . .
C35 C -0.1557(5) -0.0812(4) 0.9984(3) 0.0597(14) Uani 1 1 d . . .
H35A H -0.1080 -0.0345 0.9788 0.072 Uiso 1 1 calc R . .
C36 C -0.2742(5) -0.0542(3) 0.9834(3) 0.0547(13) Uani 1 1 d . . .
H36A H -0.3085 0.0118 0.9553 0.066 Uiso 1 1 calc R . .
C37 C -0.4317(5) -0.2908(4) 1.2718(4) 0.0730(15) Uani 1 1 d . . .
H37A H -0.4552 -0.2218 1.2473 0.088 Uiso 1 1 calc R . .
C38 C -0.4415(5) -0.3237(5) 1.3696(4) 0.0910(19) Uani 1 1 d . . .
H38A H -0.4720 -0.2770 1.4095 0.109 Uiso 1 1 calc R . .
C39 C -0.4068(6) -0.4239(6) 1.4079(4) 0.099(2) Uani 1 1 d . . .
H39A H -0.4118 -0.4463 1.4734 0.119 Uiso 1 1 calc R . .
C40 C -0.3641(6) -0.4911(5) 1.3474(4) 0.097(2) Uani 1 1 d . . .
H40A H -0.3417 -0.5599 1.3726 0.117 Uiso 1 1 calc R . .
C41 C -0.3541(4) -0.4577(4) 1.2498(3) 0.0674(14) Uani 1 1 d . . .
H41A H -0.3233 -0.5050 1.2105 0.081 Uiso 1 1 calc R . .
C42 C -0.3879(4) -0.3570(4) 1.2083(3) 0.0509(12) Uani 1 1 d . . .
C43 C -0.5200(4) -0.2642(3) 1.0752(3) 0.0459(11) Uani 1 1 d . . .
C44 C -0.6378(5) -0.2599(3) 1.1490(3) 0.0666(14) Uani 1 1 d . . .
H44A H -0.6377 -0.2826 1.2135 0.080 Uiso 1 1 calc R . .
C45 C -0.7555(5) -0.2225(4) 1.1289(5) 0.0804(18) Uani 1 1 d . . .
H45A H -0.8320 -0.2212 1.1799 0.096 Uiso 1 1 calc R . .
C46 C -0.7600(6) -0.1883(4) 1.0367(6) 0.0855(19) Uani 1 1 d . . .
H46A H -0.8390 -0.1634 1.0239 0.103 Uiso 1 1 calc R . .
C47 C -0.6476(6) -0.1906(3) 0.9620(4) 0.0706(15) Uani 1 1 d . . .
H47A H -0.6499 -0.1667 0.8981 0.085 Uiso 1 1 calc R . .
C48 C -0.5302(4) -0.2286(3) 0.9813(3) 0.0527(12) Uani 1 1 d . . .
H48A H -0.4548 -0.2304 0.9292 0.063 Uiso 1 1 calc R . .
C49 C 0.2093(4) -0.3424(3) 0.4209(3) 0.129(3) Uani 1 1 d . . .
H49A H 0.2554 -0.4096 0.4104 0.194 Uiso 1 1 calc R . .
H49B H 0.2530 -0.3205 0.4504 0.194 Uiso 1 1 calc R . .
H49C H 0.2054 -0.2979 0.3597 0.194 Uiso 1 1 calc R . .
O1S O 0.0253(4) -0.5612(3) 0.6841(3) 0.263(3) Uani 1 1 d RU . .
C1S C 0.0922(4) -0.4961(3) 0.6413(3) 0.122(4) Uani 0.50 1 d PRU A 1
H1SA H 0.1122 -0.4781 0.6889 0.183 Uiso 0.50 1 d PR B 1
H1SB H 0.1708 -0.5248 0.5953 0.183 Uiso 0.50 1 d PR C 1
H1SC H 0.0432 -0.4371 0.6078 0.183 Uiso 0.50 1 d PR D 1
C1S' C 0.0524(4) -0.5329(3) 0.5887(3) 0.142(5) Uani 0.50 1 d PRU A 2
H1SD H 0.0157 -0.5674 0.5653 0.212 Uiso 0.50 1 d PR E 2
H1SE H 0.0167 -0.4615 0.5719 0.212 Uiso 0.50 1 d PR F 2
H1SF H 0.1444 -0.5492 0.5594 0.212 Uiso 0.50 1 d PR G 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.022(3) . ?
Co1 O1 2.022(3) 2_556 ?
Co1 N1 2.124(3) . ?
Co1 N1 2.124(3) 2_556 ?
Co1 O2 2.145(3) 2_556 ?
Co1 O2 2.145(3) . ?
Co2 N3 2.018(3) . ?
Co2 O2 2.038(3) . ?
Co2 N2 2.089(3) . ?
Co2 O1 2.118(3) 2_556 ?
Co2 O3 2.137(3) . ?
Co2 N4 2.397(4) . ?
O1 C1 1.348(4) . ?
O1 Co2 2.118(3) 2_556 ?
O2 C13 1.320(5) . ?
O3 C49 1.497(4) . ?
N1 C7 1.286(4) . ?
N1 C8 1.429(5) . ?
N2 C12 1.338(5) . ?
N2 C8 1.355(5) . ?
N3 C19 1.276(5) . ?
N3 C20 1.417(5) . ?
N4 C24 1.328(6) . ?
N4 C20 1.341(5) . ?
B1 C43 1.638(6) . ?
B1 C25 1.640(6) . ?
B1 C31 1.643(6) . ?
B1 C42 1.657(6) . ?
C1 C2 1.384(5) . ?
C1 C6 1.408(5) . ?
C2 C3 1.385(5) . ?
C3 C4 1.378(6) . ?
C4 C5 1.363(6) . ?
C5 C6 1.404(5) . ?
C6 C7 1.432(5) . ?
C8 C9 1.382(5) . ?
C9 C10 1.381(6) . ?
C10 C11 1.384(6) . ?
C11 C12 1.368(6) . ?
C13 C14 1.405(5) . ?
C13 C18 1.417(5) . ?
C14 C15 1.383(6) . ?
C15 C16 1.378(6) . ?
C16 C17 1.363(6) . ?
C17 C18 1.405(6) . ?
C18 C19 1.442(6) . ?
C20 C21 1.377(5) . ?
C21 C22 1.374(6) . ?
C22 C23 1.364(6) . ?
C23 C24 1.379(6) . ?
C25 C26 1.398(5) . ?
C25 C30 1.399(5) . ?
C26 C27 1.388(5) . ?
C27 C28 1.377(5) . ?
C28 C29 1.375(6) . ?
C29 C30 1.393(5) . ?
C31 C32 1.393(5) . ?
C31 C33 1.395(5) . ?
C32 C36 1.387(5) . ?
C33 C34 1.382(5) . ?
C34 C35 1.361(6) . ?
C35 C36 1.376(6) . ?
C37 C38 1.382(6) . ?
C37 C42 1.396(5) . ?
C38 C39 1.361(7) . ?
C39 C40 1.376(7) . ?
C40 C41 1.379(6) . ?
C41 C42 1.377(6) . ?
C43 C48 1.391(5) . ?
C43 C44 1.398(5) . ?
C44 C45 1.393(7) . ?
C45 C46 1.345(7) . ?
C46 C47 1.363(7) . ?
C47 C48 1.385(6) . ?
O1S C1S 1.2902 . ?
O1S C1S' 1.3186 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 180.00(13) . 2_556 ?
O1 Co1 N1 88.29(11) . . ?
O1 Co1 N1 91.71(11) 2_556 . ?
O1 Co1 N1 91.71(11) . 2_556 ?
O1 Co1 N1 88.29(11) 2_556 2_556 ?
N1 Co1 N1 180.0 . 2_556 ?
O1 Co1 O2 82.09(10) . 2_556 ?
O1 Co1 O2 97.91(10) 2_556 2_556 ?
N1 Co1 O2 94.66(11) . 2_556 ?
N1 Co1 O2 85.34(11) 2_556 2_556 ?
O1 Co1 O2 97.91(10) . . ?
O1 Co1 O2 82.09(10) 2_556 . ?
N1 Co1 O2 85.34(11) . . ?
N1 Co1 O2 94.66(11) 2_556 . ?
O2 Co1 O2 180.00(15) 2_556 . ?
N3 Co2 O2 88.41(13) . . ?
N3 Co2 N2 161.30(15) . . ?
O2 Co2 N2 109.48(13) . . ?
N3 Co2 O1 96.22(12) . 2_556 ?
O2 Co2 O1 82.40(10) . 2_556 ?
N2 Co2 O1 81.31(12) . 2_556 ?
N3 Co2 O3 92.86(13) . . ?
O2 Co2 O3 95.76(12) . . ?
N2 Co2 O3 90.75(13) . . ?
O1 Co2 O3 170.67(11) 2_556 . ?
N3 Co2 N4 59.88(14) . . ?
O2 Co2 N4 148.29(12) . . ?
N2 Co2 N4 102.06(14) . . ?
O1 Co2 N4 99.51(11) 2_556 . ?
O3 Co2 N4 86.89(13) . . ?
C1 O1 Co1 128.5(3) . . ?
C1 O1 Co2 121.4(2) . 2_556 ?
Co1 O1 Co2 94.30(11) . 2_556 ?
C13 O2 Co2 126.1(3) . . ?
C13 O2 Co1 121.9(3) . . ?
Co2 O2 Co1 93.02(11) . . ?
C49 O3 Co2 117.3(2) . . ?
C7 N1 C8 115.2(3) . . ?
C7 N1 Co1 124.0(3) . . ?
C8 N1 Co1 120.8(2) . . ?
C12 N2 C8 117.0(4) . . ?
C12 N2 Co2 118.1(3) . . ?
C8 N2 Co2 122.9(3) . . ?
C19 N3 C20 126.2(4) . . ?
C19 N3 Co2 129.9(3) . . ?
C20 N3 Co2 103.5(3) . . ?
C24 N4 C20 116.1(4) . . ?
C24 N4 Co2 154.9(3) . . ?
C20 N4 Co2 88.9(3) . . ?
C43 B1 C25 107.5(4) . . ?
C43 B1 C31 110.8(4) . . ?
C25 B1 C31 111.5(3) . . ?
C43 B1 C42 111.6(3) . . ?
C25 B1 C42 109.4(4) . . ?
C31 B1 C42 106.1(3) . . ?
O1 C1 C2 118.8(4) . . ?
O1 C1 C6 122.5(4) . . ?
C2 C1 C6 118.8(4) . . ?
C1 C2 C3 120.7(4) . . ?
C4 C3 C2 120.8(5) . . ?
C5 C4 C3 119.2(4) . . ?
C4 C5 C6 121.6(4) . . ?
C5 C6 C1 118.8(4) . . ?
C5 C6 C7 116.4(4) . . ?
C1 C6 C7 124.8(4) . . ?
N1 C7 C6 128.4(4) . . ?
N2 C8 C9 122.5(4) . . ?
N2 C8 N1 115.5(4) . . ?
C9 C8 N1 122.0(4) . . ?
C10 C9 C8 118.4(5) . . ?
C9 C10 C11 120.1(5) . . ?
C12 C11 C10 117.3(5) . . ?
N2 C12 C11 124.6(5) . . ?
O2 C13 C14 118.6(4) . . ?
O2 C13 C18 125.2(4) . . ?
C14 C13 C18 116.1(4) . . ?
C15 C14 C13 122.1(5) . . ?
C16 C15 C14 121.2(5) . . ?
C17 C16 C15 118.3(5) . . ?
C16 C17 C18 122.3(5) . . ?
C17 C18 C13 120.0(4) . . ?
C17 C18 C19 116.2(4) . . ?
C13 C18 C19 123.7(4) . . ?
N3 C19 C18 124.3(4) . . ?
N4 C20 C21 124.4(5) . . ?
N4 C20 N3 107.7(4) . . ?
C21 C20 N3 127.9(5) . . ?
C22 C21 C20 117.6(5) . . ?
C23 C22 C21 119.3(5) . . ?
C22 C23 C24 119.0(5) . . ?
N4 C24 C23 123.5(5) . . ?
C26 C25 C30 114.4(4) . . ?
C26 C25 B1 120.4(4) . . ?
C30 C25 B1 125.2(4) . . ?
C27 C26 C25 123.2(4) . . ?
C28 C27 C26 120.0(5) . . ?
C29 C28 C27 119.4(4) . . ?
C28 C29 C30 119.6(4) . . ?
C29 C30 C25 123.4(4) . . ?
C32 C31 C33 114.3(4) . . ?
C32 C31 B1 125.4(4) . . ?
C33 C31 B1 120.3(4) . . ?
C36 C32 C31 123.2(4) . . ?
C34 C33 C31 123.0(4) . . ?
C35 C34 C33 120.8(5) . . ?
C34 C35 C36 118.7(4) . . ?
C35 C36 C32 120.0(5) . . ?
C38 C37 C42 122.5(5) . . ?
C39 C38 C37 120.5(5) . . ?
C38 C39 C40 118.4(5) . . ?
C39 C40 C41 120.8(6) . . ?
C42 C41 C40 122.5(5) . . ?
C41 C42 C37 115.3(4) . . ?
C41 C42 B1 124.8(4) . . ?
C37 C42 B1 119.9(4) . . ?
C48 C43 C44 114.8(4) . . ?
C48 C43 B1 119.8(4) . . ?
C44 C43 B1 125.3(4) . . ?
C45 C44 C43 121.9(5) . . ?
C46 C45 C44 120.9(5) . . ?
C45 C46 C47 119.4(6) . . ?
C46 C47 C48 120.1(5) . . ?
C47 C48 C43 122.9(4) . . ?
C1S O1S C1S' 62.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.051
