# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
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#  fide research purposes only. It may contain copyright material 
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data_bis3
_database_code_depnum_ccdc_archive 'CCDC 804874'
#TrackingRef 'bis3.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C68 H63 Cl2 Co2 N21 O4 2+, 2(C2 H3 N), 2(B F4 -)'
_chemical_formula_sum            'C72 H69 B2 Cl2 Co2 F8 N23 O4'
_chemical_formula_weight         1682.88
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'
B B 0.0013 0.0007 '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'
_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                   11.2933(4)
_cell_length_b                   11.5315(4)
_cell_length_c                   16.4162(6)
_cell_angle_alpha                108.969(3)
_cell_angle_beta                 91.903(3)
_cell_angle_gamma                110.416(3)
_cell_volume                     1868.66(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    25772
_cell_measurement_theta_min      1.33
_cell_measurement_theta_max      26.76
_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7228
_exptl_absorpt_correction_T_max  0.9291
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 2002)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      133(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  'Stoe IPDS II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25772
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         26.76
_reflns_number_total             7927
_reflns_number_gt                6196
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2002)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+1.1032P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7927
_refine_ls_number_parameters     523
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.0988
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.73234(3) 0.56158(3) 0.32390(2) 0.02285(10) Uani 1 1 d . . .
Cl1 Cl 0.71417(7) 0.74877(8) 0.64461(5) 0.04233(19) Uani 1 1 d . . .
N1 N 0.78780(18) 0.5822(2) 0.18210(13) 0.0208(4) Uani 1 1 d . . .
N30 N 0.91499(18) 0.7158(2) 0.34782(13) 0.0217(4) Uani 1 1 d . A .
N31 N 0.98037(18) 0.8120(2) 0.42197(13) 0.0237(4) Uani 1 1 d . . .
N32 N 1.09110(18) 0.8803(2) 0.40225(13) 0.0218(4) Uani 1 1 d . A .
N20 N 0.7252(2) 0.3792(2) 0.23761(14) 0.0252(4) Uani 1 1 d . A .
N21 N 0.7056(2) 0.2720(2) 0.25669(15) 0.0300(5) Uani 1 1 d . . .
N22 N 0.67393(19) 0.1719(2) 0.18026(15) 0.0277(5) Uani 1 1 d . A .
N10 N 0.60717(18) 0.6312(2) 0.27545(13) 0.0227(4) Uani 1 1 d . A .
N11 N 0.49594(19) 0.6290(2) 0.29953(14) 0.0241(4) Uani 1 1 d . . .
N12 N 0.44340(18) 0.6682(2) 0.24493(14) 0.0229(4) Uani 1 1 d . A .
O1 O 0.72074(17) 0.6293(2) 0.45286(12) 0.0371(5) Uani 1 1 d . A .
O2 O 0.54704(17) 0.41971(18) 0.33718(13) 0.0312(4) Uani 1 1 d . A .
C30 C 0.9280(2) 0.6237(3) 0.19237(16) 0.0221(5) Uani 1 1 d . A .
H1A H 0.9605 0.6625 0.1494 0.027 Uiso 1 1 calc R . .
H1B H 0.9512 0.5476 0.1837 0.027 Uiso 1 1 calc R . .
C31 C 0.9841(2) 0.7227(2) 0.28185(16) 0.0202(5) Uani 1 1 d . . .
C32 C 1.0978(2) 0.8289(2) 0.31700(16) 0.0222(5) Uani 1 1 d . A .
H3 H 1.1650 0.8589 0.2883 0.027 Uiso 1 1 calc R . .
C33 C 1.1911(2) 0.9872(3) 0.47205(17) 0.0263(5) Uani 1 1 d . . .
H4A H 1.1515 1.0305 0.5174 0.032 Uiso 1 1 calc R A .
H4B H 1.2421 1.0525 0.4489 0.032 Uiso 1 1 calc R . .
C34 C 1.2780(2) 0.9382(2) 0.51157(15) 0.0226(5) Uani 1 1 d . A .
C39 C 1.3851(2) 1.0318(3) 0.57212(17) 0.0276(5) Uani 1 1 d . . .
H6 H 1.4028 1.1217 0.5861 0.033 Uiso 1 1 calc R A .
C38 C 1.4655(3) 0.9916(3) 0.61166(18) 0.0329(6) Uani 1 1 d . A .
H7 H 1.5370 1.0549 0.6522 0.040 Uiso 1 1 calc R . .
C37 C 1.4413(3) 0.8592(3) 0.59179(19) 0.0352(6) Uani 1 1 d . . .
H8 H 1.4948 0.8330 0.6196 0.042 Uiso 1 1 calc R A .
C36 C 1.3365(3) 0.7656(3) 0.5301(2) 0.0367(6) Uani 1 1 d . A .
H9 H 1.3207 0.6759 0.5150 0.044 Uiso 1 1 calc R . .
C35 C 1.2549(2) 0.8049(3) 0.49056(18) 0.0296(6) Uani 1 1 d . . .
H10 H 1.1841 0.7413 0.4496 0.035 Uiso 1 1 calc R A .
C10 C 0.7458(2) 0.6841(3) 0.17006(17) 0.0232(5) Uani 1 1 d . A .
H11A H 0.7313 0.6706 0.1085 0.028 Uiso 1 1 calc R . .
H11B H 0.8109 0.7718 0.2004 0.028 Uiso 1 1 calc R . .
C11 C 0.6242(2) 0.6715(2) 0.20651(16) 0.0221(5) Uani 1 1 d . . .
C12 C 0.5185(2) 0.6951(2) 0.18517(17) 0.0237(5) Uani 1 1 d . A .
H13 H 0.5020 0.7229 0.1403 0.028 Uiso 1 1 calc R . .
C13 C 0.3155(2) 0.6730(3) 0.25317(17) 0.0257(5) Uani 1 1 d . . .
H14A H 0.3080 0.7401 0.2323 0.031 Uiso 1 1 calc R A .
H14B H 0.3066 0.6987 0.3144 0.031 Uiso 1 1 calc R . .
C14 C 0.2087(2) 0.5421(3) 0.20268(17) 0.0238(5) Uani 1 1 d . A .
C19 C 0.1401(2) 0.4601(3) 0.24470(18) 0.0295(6) Uani 1 1 d . . .
H16 H 0.1615 0.4849 0.3048 0.035 Uiso 1 1 calc R A .
C18 C 0.0400(3) 0.3415(3) 0.1980(2) 0.0352(6) Uani 1 1 d . A .
H17 H -0.0062 0.2877 0.2269 0.042 Uiso 1 1 calc R . .
C17 C 0.0087(3) 0.3032(3) 0.1090(2) 0.0344(6) Uani 1 1 d . . .
H18 H -0.0580 0.2232 0.0776 0.041 Uiso 1 1 calc R A .
C16 C 0.0769(3) 0.3842(3) 0.06643(19) 0.0371(7) Uani 1 1 d . A .
H19 H 0.0563 0.3583 0.0062 0.045 Uiso 1 1 calc R . .
C15 C 0.1758(3) 0.5036(3) 0.11314(18) 0.0330(6) Uani 1 1 d . . .
H20 H 0.2204 0.5584 0.0843 0.040 Uiso 1 1 calc R A .
C20 C 0.7220(2) 0.4524(2) 0.11260(16) 0.0244(5) Uani 1 1 d . A .
H21A H 0.7716 0.4423 0.0655 0.029 Uiso 1 1 calc R . .
H21B H 0.6386 0.4451 0.0893 0.029 Uiso 1 1 calc R . .
C21 C 0.7070(2) 0.3471(2) 0.14992(16) 0.0220(5) Uani 1 1 d . . .
C22 C 0.6738(2) 0.2129(3) 0.11241(17) 0.0265(5) Uani 1 1 d . A .
H23 H 0.6552 0.1615 0.0532 0.032 Uiso 1 1 calc R . .
C23 C 0.6539(3) 0.0379(3) 0.1780(2) 0.0330(6) Uani 1 1 d . . .
H24A H 0.6037 -0.0269 0.1224 0.040 Uiso 1 1 calc R A .
H24B H 0.6067 0.0206 0.2239 0.040 Uiso 1 1 calc R . .
C24 C 0.7813(2) 0.0247(2) 0.19051(18) 0.0268(5) Uani 1 1 d . A .
C25 C 0.8392(3) -0.0153(3) 0.11880(19) 0.0303(6) Uani 1 1 d . . .
H26 H 0.7975 -0.0383 0.0627 0.036 Uiso 1 1 calc R A .
C26 C 0.9591(3) -0.0212(3) 0.1306(2) 0.0339(6) Uani 1 1 d . A .
H27 H 0.9975 -0.0484 0.0826 0.041 Uiso 1 1 calc R . .
C27 C 1.0214(3) 0.0137(3) 0.2141(2) 0.0340(6) Uani 1 1 d . . .
H28 H 1.1021 0.0108 0.2222 0.041 Uiso 1 1 calc R A .
C28 C 0.9636(3) 0.0528(3) 0.2858(2) 0.0353(6) Uani 1 1 d . A .
H29 H 1.0054 0.0758 0.3418 0.042 Uiso 1 1 calc R . .
C29 C 0.8435(3) 0.0576(3) 0.27364(19) 0.0315(6) Uani 1 1 d . . .
H30 H 0.8046 0.0830 0.3217 0.038 Uiso 1 1 calc R A .
C3 C 0.5983(2) 0.6132(3) 0.56493(17) 0.0278(5) Uani 1 1 d . . .
C1 C 0.6205(2) 0.5737(3) 0.48018(17) 0.0268(5) Uani 1 1 d . . .
C2 C 0.5183(2) 0.4526(3) 0.41133(17) 0.0241(5) Uani 1 1 d . . .
B1 B 0.7158(3) 0.1185(3) 0.8801(2) 0.0315(7) Uani 1 1 d . . .
F1 F 0.67488(18) 0.0490(2) 0.79187(11) 0.0479(5) Uani 1 1 d . . .
F2 F 0.84245(19) 0.2021(3) 0.89020(17) 0.0793(8) Uani 1 1 d . . .
F3 F 0.64647(16) 0.19644(19) 0.91276(12) 0.0428(4) Uani 1 1 d . . .
F4 F 0.7088(3) 0.0367(2) 0.92474(15) 0.0913(10) Uani 1 1 d . . .
N200 N 0.5927(3) 0.6961(4) 0.9896(2) 0.0728(11) Uani 1 1 d . . .
C201 C 0.6224(3) 0.7102(3) 0.9272(2) 0.0418(7) Uani 1 1 d . . .
C200 C 0.6595(3) 0.7305(3) 0.8483(2) 0.0430(7) Uani 1 1 d . . .
H42A H 0.6765 0.8208 0.8546 0.064 Uiso 1 1 calc R . .
H42B H 0.5914 0.6722 0.8001 0.064 Uiso 1 1 calc R . .
H42C H 0.7352 0.7120 0.8376 0.064 Uiso 1 1 calc R . .
N100 N 0.8758(5) 0.4972(5) 0.4021(4) 0.0424(12) Uani 0.50 1 d P A -1
C101 C 0.9486(6) 0.4708(8) 0.4361(6) 0.0510(18) Uani 0.50 1 d P A -1
C100 C 1.0382(8) 0.4304(12) 0.4714(9) 0.092(4) Uani 0.50 1 d P A -1
H44A H 1.0024 0.3360 0.4564 0.137 Uiso 0.50 1 calc PR A -1
H44B H 1.0567 0.4732 0.5338 0.137 Uiso 0.50 1 calc PR A -1
H44C H 1.1159 0.4549 0.4476 0.137 Uiso 0.50 1 calc PR A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.01709(16) 0.02302(18) 0.02349(17) 0.00561(14) 0.00756(12) 0.00405(13)
Cl1 0.0307(3) 0.0473(4) 0.0299(3) 0.0167(3) -0.0004(3) -0.0095(3)
N1 0.0168(9) 0.0232(11) 0.0234(10) 0.0104(9) 0.0039(8) 0.0068(8)
N30 0.0181(9) 0.0264(11) 0.0218(10) 0.0104(9) 0.0049(8) 0.0079(8)
N31 0.0179(9) 0.0274(11) 0.0244(10) 0.0100(9) 0.0045(8) 0.0061(8)
N32 0.0174(9) 0.0220(11) 0.0262(10) 0.0098(9) 0.0031(8) 0.0068(8)
N20 0.0285(11) 0.0267(11) 0.0269(11) 0.0144(9) 0.0105(9) 0.0130(9)
N21 0.0346(12) 0.0282(12) 0.0346(12) 0.0164(10) 0.0136(10) 0.0151(10)
N22 0.0205(10) 0.0244(11) 0.0401(13) 0.0138(10) 0.0094(9) 0.0083(9)
N10 0.0176(9) 0.0262(11) 0.0233(10) 0.0091(9) 0.0066(8) 0.0068(8)
N11 0.0178(9) 0.0276(11) 0.0254(10) 0.0085(9) 0.0043(8) 0.0076(8)
N12 0.0179(9) 0.0210(11) 0.0275(11) 0.0071(9) 0.0047(8) 0.0063(8)
O1 0.0194(9) 0.0555(13) 0.0275(10) 0.0237(9) 0.0019(7) -0.0040(8)
O2 0.0295(9) 0.0246(10) 0.0360(10) 0.0095(8) 0.0140(8) 0.0065(8)
C30 0.0182(11) 0.0269(13) 0.0234(12) 0.0113(10) 0.0067(9) 0.0087(10)
C31 0.0168(10) 0.0263(13) 0.0240(12) 0.0138(10) 0.0068(9) 0.0109(9)
C32 0.0203(11) 0.0282(13) 0.0253(12) 0.0151(10) 0.0075(9) 0.0122(10)
C33 0.0215(11) 0.0228(13) 0.0305(13) 0.0080(11) 0.0009(10) 0.0056(10)
C34 0.0210(11) 0.0234(12) 0.0197(11) 0.0071(10) 0.0049(9) 0.0047(9)
C39 0.0262(12) 0.0238(13) 0.0261(13) 0.0055(11) 0.0011(10) 0.0053(10)
C38 0.0249(13) 0.0368(16) 0.0272(13) 0.0075(12) -0.0043(10) 0.0048(11)
C37 0.0300(14) 0.0424(17) 0.0353(15) 0.0184(13) -0.0006(11) 0.0125(12)
C36 0.0378(15) 0.0291(15) 0.0441(17) 0.0150(13) 0.0002(12) 0.0128(12)
C35 0.0268(13) 0.0246(13) 0.0320(14) 0.0095(11) -0.0008(10) 0.0047(10)
C10 0.0201(11) 0.0249(13) 0.0284(13) 0.0146(11) 0.0055(9) 0.0082(10)
C11 0.0195(11) 0.0173(12) 0.0265(12) 0.0078(10) 0.0044(9) 0.0036(9)
C12 0.0201(11) 0.0219(12) 0.0296(13) 0.0118(10) 0.0063(9) 0.0061(9)
C13 0.0193(11) 0.0253(13) 0.0321(13) 0.0086(11) 0.0082(10) 0.0094(10)
C14 0.0160(11) 0.0258(13) 0.0299(13) 0.0094(11) 0.0064(9) 0.0085(9)
C19 0.0283(13) 0.0325(15) 0.0311(14) 0.0159(12) 0.0070(11) 0.0111(11)
C18 0.0271(13) 0.0324(15) 0.0479(17) 0.0216(13) 0.0093(12) 0.0065(11)
C17 0.0240(13) 0.0249(14) 0.0488(17) 0.0111(13) 0.0040(12) 0.0051(11)
C16 0.0352(15) 0.0367(16) 0.0284(14) 0.0069(12) 0.0018(11) 0.0057(12)
C15 0.0294(13) 0.0314(15) 0.0324(14) 0.0132(12) 0.0074(11) 0.0032(11)
C20 0.0238(12) 0.0257(13) 0.0220(12) 0.0091(10) 0.0011(9) 0.0074(10)
C21 0.0159(11) 0.0252(13) 0.0239(12) 0.0084(10) 0.0038(9) 0.0071(9)
C22 0.0186(11) 0.0272(13) 0.0296(13) 0.0083(11) 0.0021(10) 0.0061(10)
C23 0.0258(13) 0.0227(14) 0.0513(17) 0.0152(13) 0.0094(12) 0.0082(11)
C24 0.0240(12) 0.0155(12) 0.0394(15) 0.0122(11) 0.0067(11) 0.0037(10)
C25 0.0313(13) 0.0218(13) 0.0351(14) 0.0104(11) 0.0046(11) 0.0070(11)
C26 0.0326(14) 0.0245(14) 0.0464(17) 0.0128(13) 0.0161(12) 0.0121(11)
C27 0.0233(12) 0.0280(14) 0.0556(18) 0.0220(13) 0.0079(12) 0.0089(11)
C28 0.0369(15) 0.0284(15) 0.0414(16) 0.0193(13) 0.0023(12) 0.0073(12)
C29 0.0341(14) 0.0236(14) 0.0380(15) 0.0148(12) 0.0111(12) 0.0085(11)
C3 0.0191(11) 0.0328(14) 0.0285(13) 0.0164(11) 0.0001(10) 0.0020(10)
C1 0.0167(11) 0.0381(15) 0.0302(13) 0.0223(12) 0.0025(9) 0.0066(10)
C2 0.0220(11) 0.0278(13) 0.0296(13) 0.0174(11) 0.0063(10) 0.0110(10)
B1 0.0328(15) 0.0330(17) 0.0302(15) 0.0131(13) 0.0018(12) 0.0128(13)
F1 0.0483(10) 0.0537(12) 0.0314(9) 0.0103(8) 0.0006(8) 0.0128(9)
F2 0.0282(10) 0.0861(18) 0.0837(17) -0.0062(14) 0.0002(10) 0.0101(11)
F3 0.0401(9) 0.0546(12) 0.0448(10) 0.0220(9) 0.0107(8) 0.0265(9)
F4 0.207(3) 0.0590(15) 0.0463(12) 0.0319(12) 0.0431(16) 0.0804(19)
N200 0.0358(15) 0.124(3) 0.0444(18) 0.040(2) 0.0028(13) 0.0056(18)
C201 0.0258(14) 0.0485(19) 0.0340(16) 0.0083(14) -0.0023(12) 0.0008(13)
C200 0.0524(19) 0.0346(17) 0.0418(17) 0.0115(14) 0.0154(14) 0.0177(14)
N100 0.042(3) 0.037(3) 0.045(3) 0.016(2) 0.001(2) 0.011(2)
C101 0.029(3) 0.056(4) 0.088(6) 0.052(4) 0.013(3) 0.015(3)
C100 0.043(4) 0.126(9) 0.149(11) 0.108(9) 0.014(5) 0.029(5)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 2.031(2) . ?
Co1 N20 2.091(2) . ?
Co1 N10 2.100(2) . ?
Co1 N30 2.122(2) . ?
Co1 O2 2.2309(18) . ?
Co1 N100 2.479(5) . ?
Cl1 C3 1.731(3) . ?
N1 C20 1.467(3) . ?
N1 C30 1.471(3) . ?
N1 C10 1.475(3) . ?
N30 N31 1.323(3) . ?
N30 C31 1.363(3) . ?
N31 N32 1.339(3) . ?
N32 C32 1.347(3) . ?
N32 C33 1.460(3) . ?
N20 N21 1.320(3) . ?
N20 C21 1.354(3) . ?
N21 N22 1.332(3) . ?
N22 C22 1.344(3) . ?
N22 C23 1.469(3) . ?
N10 N11 1.323(3) . ?
N10 C11 1.352(3) . ?
N11 N12 1.332(3) . ?
N12 C12 1.359(3) . ?
N12 C13 1.474(3) . ?
O1 C1 1.268(3) . ?
O2 C2 1.242(3) . ?
C30 C31 1.485(3) . ?
C31 C32 1.369(3) . ?
C33 C34 1.513(3) . ?
C34 C35 1.385(4) . ?
C34 C39 1.388(3) . ?
C39 C38 1.383(4) . ?
C38 C37 1.374(4) . ?
C37 C36 1.382(4) . ?
C36 C35 1.384(4) . ?
C10 C11 1.495(3) . ?
C11 C12 1.372(3) . ?
C13 C14 1.507(3) . ?
C14 C19 1.385(4) . ?
C14 C15 1.386(4) . ?
C19 C18 1.385(4) . ?
C18 C17 1.376(4) . ?
C17 C16 1.383(4) . ?
C16 C15 1.384(4) . ?
C20 C21 1.492(3) . ?
C21 C22 1.370(4) . ?
C23 C24 1.513(4) . ?
C24 C29 1.383(4) . ?
C24 C25 1.391(4) . ?
C25 C26 1.390(4) . ?
C26 C27 1.384(4) . ?
C27 C28 1.386(4) . ?
C28 C29 1.387(4) . ?
C3 C1 1.377(4) . ?
C3 C2 1.411(3) 2_666 ?
C1 C2 1.524(4) . ?
C2 C3 1.411(3) 2_666 ?
B1 F4 1.355(4) . ?
B1 F1 1.377(4) . ?
B1 F3 1.383(4) . ?
B1 F2 1.386(4) . ?
N200 C201 1.132(4) . ?
C201 C200 1.440(4) . ?
N100 C101 1.156(8) . ?
C101 C100 1.429(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
O1 Co1 N20 133.05(9) . . ?
O1 Co1 N10 99.51(8) . . ?
N20 Co1 N10 112.85(8) . . ?
O1 Co1 N30 89.96(8) . . ?
N20 Co1 N30 112.71(8) . . ?
N10 Co1 N30 103.91(8) . . ?
O1 Co1 O2 75.01(7) . . ?
N20 Co1 O2 77.40(7) . . ?
N10 Co1 O2 81.09(8) . . ?
N30 Co1 O2 164.83(7) . . ?
O1 Co1 N100 72.33(14) . . ?
N20 Co1 N100 74.41(14) . . ?
N10 Co1 N100 171.78(14) . . ?
N30 Co1 N100 75.70(14) . . ?
O2 Co1 N100 97.27(14) . . ?
C20 N1 C30 112.06(19) . . ?
C20 N1 C10 111.88(19) . . ?
C30 N1 C10 111.99(19) . . ?
N31 N30 C31 110.17(19) . . ?
N31 N30 Co1 129.36(15) . . ?
C31 N30 Co1 120.44(16) . . ?
N30 N31 N32 105.69(18) . . ?
N31 N32 C32 111.9(2) . . ?
N31 N32 C33 119.6(2) . . ?
C32 N32 C33 128.2(2) . . ?
N21 N20 C21 110.1(2) . . ?
N21 N20 Co1 125.76(17) . . ?
C21 N20 Co1 122.13(17) . . ?
N20 N21 N22 105.8(2) . . ?
N21 N22 C22 112.1(2) . . ?
N21 N22 C23 119.8(2) . . ?
C22 N22 C23 127.9(2) . . ?
N11 N10 C11 110.1(2) . . ?
N11 N10 Co1 126.54(16) . . ?
C11 N10 Co1 122.94(15) . . ?
N10 N11 N12 105.68(19) . . ?
N11 N12 C12 112.31(19) . . ?
N11 N12 C13 119.1(2) . . ?
C12 N12 C13 128.5(2) . . ?
C1 O1 Co1 119.93(18) . . ?
C2 O2 Co1 113.91(16) . . ?
N1 C30 C31 108.40(19) . . ?
N30 C31 C32 107.3(2) . . ?
N30 C31 C30 119.1(2) . . ?
C32 C31 C30 133.6(2) . . ?
N32 C32 C31 105.0(2) . . ?
N32 C33 C34 112.5(2) . . ?
C35 C34 C39 119.0(2) . . ?
C35 C34 C33 123.0(2) . . ?
C39 C34 C33 118.0(2) . . ?
C38 C39 C34 120.1(3) . . ?
C37 C38 C39 120.9(2) . . ?
C38 C37 C36 119.3(3) . . ?
C37 C36 C35 120.2(3) . . ?
C36 C35 C34 120.5(2) . . ?
N1 C10 C11 107.55(19) . . ?
N10 C11 C12 108.1(2) . . ?
N10 C11 C10 118.9(2) . . ?
C12 C11 C10 133.0(2) . . ?
N12 C12 C11 103.7(2) . . ?
N12 C13 C14 112.7(2) . . ?
C19 C14 C15 119.0(2) . . ?
C19 C14 C13 121.0(2) . . ?
C15 C14 C13 120.0(2) . . ?
C14 C19 C18 120.6(3) . . ?
C17 C18 C19 120.1(3) . . ?
C18 C17 C16 119.7(3) . . ?
C17 C16 C15 120.2(3) . . ?
C16 C15 C14 120.4(3) . . ?
N1 C20 C21 108.60(19) . . ?
N20 C21 C22 107.5(2) . . ?
N20 C21 C20 119.8(2) . . ?
C22 C21 C20 132.7(2) . . ?
N22 C22 C21 104.6(2) . . ?
N22 C23 C24 110.3(2) . . ?
C29 C24 C25 119.5(2) . . ?
C29 C24 C23 120.2(2) . . ?
C25 C24 C23 120.2(3) . . ?
C26 C25 C24 120.2(3) . . ?
C27 C26 C25 119.8(3) . . ?
C26 C27 C28 120.1(3) . . ?
C27 C28 C29 119.9(3) . . ?
C24 C29 C28 120.4(3) . . ?
C1 C3 C2 121.6(2) . 2_666 ?
C1 C3 Cl1 119.75(19) . . ?
C2 C3 Cl1 118.6(2) 2_666 . ?
O1 C1 C3 125.7(3) . . ?
O1 C1 C2 115.4(2) . . ?
C3 C1 C2 118.9(2) . . ?
O2 C2 C3 125.3(2) . 2_666 ?
O2 C2 C1 115.3(2) . . ?
C3 C2 C1 119.4(2) 2_666 . ?
F4 B1 F1 111.7(3) . . ?
F4 B1 F3 110.5(3) . . ?
F1 B1 F3 110.8(2) . . ?
F4 B1 F2 109.1(3) . . ?
F1 B1 F2 106.7(3) . . ?
F3 B1 F2 107.8(3) . . ?
N200 C201 C200 178.8(4) . . ?
C101 N100 Co1 175.8(5) . . ?
N100 C101 C100 175.4(11) . . ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.76
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.058


data_sar38
_database_code_depnum_ccdc_archive 'CCDC 911111'
#TrackingRef 'sar38.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H62 B4 Co2 F16 N20 O2'
_chemical_formula_weight         1560.40
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'
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'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
_cell_length_a                   21.184(2)
_cell_length_b                   14.3717(17)
_cell_length_c                   22.001(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6698.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8309
_cell_measurement_theta_min      1.5
_cell_measurement_theta_max      26
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3184
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.696
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa Apex II duo'
_diffrn_measurement_method       'omega phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            110712
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         28.31
_reflns_number_total             8309
_reflns_number_gt                6352
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       'Bruker Apex II Suite, 2008'
_computing_cell_refinement       'Bruker Apex II Suite, 2008'
_computing_data_reduction        'Bruker Apex II Suite, 2008'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_publication_material  'Diamond 3, 2008'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+19.7688P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8309
_refine_ls_number_parameters     473
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1846
_refine_ls_wR_factor_gt          0.1630
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.11355(13) 0.1606(2) 0.07080(15) 0.0237(6) Uani 1 1 d . . .
H10B H 0.1301 0.1571 0.0288 0.028 Uiso 1 1 calc R . .
H10A H 0.1382 0.2076 0.0936 0.028 Uiso 1 1 calc R . .
C11 C 0.11727(14) 0.0685(2) 0.10095(14) 0.0225(6) Uani 1 1 d . . .
C12 C 0.15670(15) 0.0215(2) 0.13935(15) 0.0258(6) Uani 1 1 d . . .
H12A H 0.1962 0.0417 0.1550 0.031 Uiso 1 1 calc R . .
C13 C 0.14408(18) -0.1339(3) 0.19278(17) 0.0343(8) Uani 1 1 d . . .
H13B H 0.1906 -0.1409 0.1932 0.041 Uiso 1 1 calc R . .
H13A H 0.1257 -0.1935 0.1787 0.041 Uiso 1 1 calc R . .
C14 C 0.12132(17) -0.1140(2) 0.25666(17) 0.0331(8) Uani 1 1 d . . .
C15 C 0.06433(19) -0.0705(3) 0.26809(18) 0.0398(9) Uani 1 1 d . . .
H15A H 0.0378 -0.0535 0.2351 0.048 Uiso 1 1 calc R . .
C16 C 0.0454(2) -0.0513(3) 0.3270(2) 0.0463(10) Uani 1 1 d . . .
H16A H 0.0066 -0.0201 0.3343 0.056 Uiso 1 1 calc R . .
C17 C 0.0833(2) -0.0778(4) 0.3753(2) 0.0533(12) Uani 1 1 d . . .
H17A H 0.0710 -0.0638 0.4158 0.064 Uiso 1 1 calc R . .
C18 C 0.1393(2) -0.1248(4) 0.3643(2) 0.0513(12) Uani 1 1 d . . .
H18A H 0.1646 -0.1450 0.3975 0.062 Uiso 1 1 calc R . .
C19 C 0.15872(19) -0.1424(3) 0.30530(19) 0.0425(9) Uani 1 1 d . . .
H19A H 0.1974 -0.1739 0.2980 0.051 Uiso 1 1 calc R . .
C20 C 0.02940(15) 0.2565(2) 0.02311(17) 0.0307(7) Uani 1 1 d . . .
H20B H 0.0347 0.3200 0.0397 0.037 Uiso 1 1 calc R . .
H20A H 0.0578 0.2491 -0.0123 0.037 Uiso 1 1 calc R . .
C21 C -0.03739(16) 0.2403(2) 0.00504(16) 0.0298(7) Uani 1 1 d . . .
C22 C -0.08568(18) 0.2913(3) -0.01921(17) 0.0380(9) Uani 1 1 d . . .
H22A H -0.0856 0.3555 -0.0294 0.046 Uiso 1 1 calc R . .
C23 C -0.19760(18) 0.2484(4) -0.04846(18) 0.0509(12) Uani 1 1 d . . .
H23B H -0.2175 0.1886 -0.0599 0.061 Uiso 1 1 calc R . .
H23A H -0.1950 0.2874 -0.0855 0.061 Uiso 1 1 calc R . .
C24 C -0.23815(14) 0.2964(2) -0.00237(14) 0.0242(6) Uani 1 1 d . . .
C25 C -0.24527(18) 0.3923(3) -0.0032(2) 0.0474(11) Uani 1 1 d . . .
H25A H -0.2246 0.4302 -0.0324 0.057 Uiso 1 1 calc R . .
C26 C -0.2870(2) 0.4325(3) 0.0442(3) 0.0604(16) Uani 1 1 d . . .
H26A H -0.2940 0.4976 0.0468 0.073 Uiso 1 1 calc R . .
C27 C -0.3148(2) 0.3726(4) 0.0836(2) 0.0519(12) Uani 1 1 d . . .
H27A H -0.3417 0.3980 0.1140 0.062 Uiso 1 1 calc R . .
C28 C -0.3071(2) 0.2816(4) 0.0826(2) 0.0568(13) Uani 1 1 d . . .
H28A H -0.3285 0.2431 0.1111 0.068 Uiso 1 1 calc R . .
C29 C -0.26873(17) 0.2441(3) 0.04085(19) 0.0418(9) Uani 1 1 d . . .
H29A H -0.2624 0.1786 0.0411 0.050 Uiso 1 1 calc R . .
C30 C 0.02386(16) 0.2181(2) 0.13355(16) 0.0305(7) Uani 1 1 d . . .
H30B H 0.0610 0.2210 0.1607 0.037 Uiso 1 1 calc R . .
H30A H 0.0055 0.2812 0.1307 0.037 Uiso 1 1 calc R . .
C31 C -0.02357(14) 0.1528(2) 0.15907(15) 0.0258(6) Uani 1 1 d . . .
C32 C -0.05508(15) 0.1441(3) 0.21319(16) 0.0305(7) Uani 1 1 d . . .
H32A H -0.0521 0.1832 0.2479 0.037 Uiso 1 1 calc R . .
C33 C -0.13701(17) 0.0269(3) 0.24927(16) 0.0327(7) Uani 1 1 d . . .
H33B H -0.1193 0.0295 0.2909 0.039 Uiso 1 1 calc R . .
H33A H -0.1440 -0.0393 0.2388 0.039 Uiso 1 1 calc R . .
C34 C -0.19939(16) 0.0779(2) 0.24796(15) 0.0275(7) Uani 1 1 d . . .
C35 C -0.21030(16) 0.1497(2) 0.28931(16) 0.0302(7) Uani 1 1 d . . .
H35A H -0.1790 0.1645 0.3187 0.036 Uiso 1 1 calc R . .
C36 C -0.26659(16) 0.1997(3) 0.28801(18) 0.0344(8) Uani 1 1 d . . .
H36A H -0.2737 0.2487 0.3162 0.041 Uiso 1 1 calc R . .
C37 C -0.31225(17) 0.1773(3) 0.24519(18) 0.0377(8) Uani 1 1 d . . .
H37A H -0.3506 0.2116 0.2436 0.045 Uiso 1 1 calc R . .
C38 C -0.30191(18) 0.1049(3) 0.20467(18) 0.0410(9) Uani 1 1 d . . .
H38A H -0.3337 0.0887 0.1761 0.049 Uiso 1 1 calc R . .
C39 C -0.24563(18) 0.0563(3) 0.20556(17) 0.0365(8) Uani 1 1 d . . .
H39A H -0.2386 0.0078 0.1770 0.044 Uiso 1 1 calc R . .
B1 B 0.0257(2) 0.2656(4) -0.1511(2) 0.0497(13) Uani 1 1 d . . .
B2 B 0.1585(2) 0.4247(3) 0.1049(2) 0.0417(11) Uani 1 1 d . . .
N1 N 0.04419(12) 0.18514(18) 0.07065(12) 0.0228(5) Uani 1 1 d . . .
N10 N 0.06666(11) 0.01187(18) 0.09119(11) 0.0204(5) Uani 1 1 d . . .
N11 N 0.07139(12) -0.06622(18) 0.12144(12) 0.0236(5) Uani 1 1 d . . .
N12 N 0.12682(13) -0.06019(19) 0.15019(13) 0.0255(6) Uani 1 1 d . . .
N20 N -0.05944(12) 0.1518(2) 0.01157(12) 0.0250(6) Uani 1 1 d . . .
N21 N -0.11851(12) 0.1447(2) -0.00608(13) 0.0304(6) Uani 1 1 d . . .
N22 N -0.13322(14) 0.2305(2) -0.02547(14) 0.0370(8) Uani 1 1 d . . .
N30 N -0.04299(11) 0.08207(19) 0.12366(12) 0.0226(5) Uani 1 1 d . . .
N31 N -0.08453(12) 0.0289(2) 0.15131(12) 0.0243(5) Uani 1 1 d . . .
N32 N -0.09128(13) 0.0676(2) 0.20615(12) 0.0274(6) Uani 1 1 d . . .
O1 O 0.04283(9) 0.04526(16) -0.02571(10) 0.0203(4) Uani 1 1 d . . .
F1 F 0.0579(2) 0.3402(3) -0.1302(3) 0.146(3) Uani 1 1 d . . .
F2 F 0.04401(15) 0.2453(4) -0.20910(17) 0.121(2) Uani 1 1 d . . .
F3 F -0.03916(11) 0.28461(17) -0.15108(10) 0.0434(6) Uani 1 1 d . . .
F4 F 0.03960(11) 0.19128(17) -0.11317(11) 0.0443(6) Uani 1 1 d . . .
F5 F 0.13780(14) 0.51578(19) 0.10364(12) 0.0543(7) Uani 1 1 d . . .
F6 F 0.21708(14) 0.4223(2) 0.1296(2) 0.0876(12) Uani 1 1 d . . .
F7 F 0.11882(17) 0.3710(2) 0.1386(2) 0.0940(14) Uani 1 1 d . . .
F8 F 0.1600(2) 0.3873(3) 0.04751(17) 0.1010(14) Uani 1 1 d . . .
Co1 Co -0.001525(17) 0.06724(3) 0.048436(18) 0.01895(12) Uani 1 1 d . . .
H1 H 0.037(2) 0.084(3) -0.053(2) 0.044(13) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C10 0.0132(12) 0.0298(16) 0.0281(16) -0.0019(13) -0.0023(11) -0.0025(11)
C11 0.0155(13) 0.0296(16) 0.0223(14) -0.0056(12) -0.0026(11) 0.0001(11)
C12 0.0198(14) 0.0304(16) 0.0273(16) -0.0055(13) -0.0046(12) 0.0000(12)
C13 0.0351(18) 0.0301(17) 0.038(2) 0.0036(15) -0.0108(15) 0.0069(14)
C14 0.0339(18) 0.0312(17) 0.0342(19) 0.0076(15) -0.0131(15) -0.0074(14)
C15 0.0368(19) 0.050(2) 0.0329(19) 0.0112(17) -0.0070(15) 0.0024(17)
C16 0.044(2) 0.057(3) 0.038(2) 0.0152(19) 0.0017(18) -0.0041(19)
C17 0.056(3) 0.071(3) 0.032(2) 0.017(2) -0.0020(19) -0.020(2)
C18 0.049(2) 0.068(3) 0.037(2) 0.023(2) -0.0153(19) -0.014(2)
C19 0.0350(19) 0.048(2) 0.044(2) 0.0159(18) -0.0152(17) -0.0069(17)
C20 0.0247(15) 0.0273(16) 0.0400(19) 0.0003(14) -0.0088(14) -0.0010(13)
C21 0.0259(15) 0.0333(17) 0.0303(17) -0.0045(14) -0.0057(13) 0.0072(13)
C22 0.0357(19) 0.046(2) 0.0324(19) -0.0102(16) -0.0107(15) 0.0174(16)
C23 0.0291(18) 0.094(3) 0.0301(19) -0.022(2) -0.0143(15) 0.030(2)
C24 0.0183(13) 0.0335(17) 0.0207(14) -0.0032(12) -0.0052(11) 0.0049(12)
C25 0.0284(18) 0.036(2) 0.078(3) 0.012(2) -0.018(2) -0.0035(15)
C26 0.050(3) 0.037(2) 0.094(4) -0.028(2) -0.039(3) 0.0115(19)
C27 0.0312(19) 0.086(4) 0.039(2) -0.019(2) -0.0048(17) 0.007(2)
C28 0.037(2) 0.098(4) 0.035(2) 0.007(2) 0.0019(17) 0.005(2)
C29 0.0298(18) 0.055(2) 0.041(2) 0.0122(18) -0.0090(15) -0.0039(17)
C30 0.0247(15) 0.0342(18) 0.0327(18) -0.0147(14) -0.0011(13) -0.0020(13)
C31 0.0178(13) 0.0335(17) 0.0261(16) -0.0113(13) -0.0032(12) 0.0027(12)
C32 0.0257(15) 0.0408(19) 0.0249(16) -0.0107(14) -0.0019(13) 0.0037(14)
C33 0.0326(17) 0.0430(19) 0.0224(16) 0.0022(15) 0.0055(13) 0.0063(15)
C34 0.0263(15) 0.0347(17) 0.0214(15) 0.0038(13) 0.0048(12) -0.0024(13)
C35 0.0256(15) 0.0361(18) 0.0290(17) 0.0010(14) 0.0050(13) -0.0067(13)
C36 0.0293(17) 0.0320(17) 0.042(2) -0.0002(15) 0.0105(15) -0.0024(14)
C37 0.0237(16) 0.046(2) 0.044(2) 0.0106(17) 0.0058(15) 0.0005(15)
C38 0.0317(18) 0.057(2) 0.034(2) 0.0026(18) -0.0061(15) -0.0043(17)
C39 0.0357(18) 0.047(2) 0.0270(17) -0.0045(15) 0.0015(15) -0.0026(16)
B1 0.034(2) 0.065(3) 0.050(3) 0.032(2) -0.011(2) -0.015(2)
B2 0.035(2) 0.039(2) 0.051(3) -0.017(2) 0.015(2) -0.0085(18)
N1 0.0167(11) 0.0261(13) 0.0255(13) -0.0051(10) -0.0040(10) 0.0007(10)
N10 0.0161(11) 0.0264(13) 0.0187(12) -0.0032(10) -0.0008(9) -0.0002(9)
N11 0.0213(12) 0.0279(13) 0.0217(13) -0.0042(10) -0.0030(10) 0.0005(10)
N12 0.0227(12) 0.0281(13) 0.0258(14) -0.0009(11) -0.0057(10) 0.0026(10)
N20 0.0149(11) 0.0393(15) 0.0209(13) -0.0080(11) -0.0032(9) 0.0035(10)
N21 0.0157(12) 0.0514(18) 0.0242(14) -0.0157(13) -0.0044(10) 0.0058(12)
N22 0.0256(14) 0.057(2) 0.0278(15) -0.0177(14) -0.0104(12) 0.0172(14)
N30 0.0151(11) 0.0315(14) 0.0211(13) -0.0079(10) -0.0012(9) -0.0011(10)
N31 0.0197(12) 0.0345(14) 0.0187(12) -0.0060(11) 0.0010(10) 0.0016(10)
N32 0.0229(13) 0.0400(16) 0.0193(13) -0.0067(11) 0.0013(10) 0.0038(11)
O1 0.0163(9) 0.0275(11) 0.0171(10) -0.0033(9) -0.0005(8) -0.0016(8)
F1 0.107(3) 0.063(2) 0.268(6) 0.070(3) -0.118(4) -0.045(2)
F2 0.0474(17) 0.252(6) 0.064(2) 0.067(3) 0.0163(15) 0.043(3)
F3 0.0391(12) 0.0556(14) 0.0356(12) 0.0137(11) -0.0026(10) -0.0004(10)
F4 0.0368(12) 0.0475(13) 0.0486(14) 0.0174(11) -0.0080(10) -0.0077(10)
F5 0.0679(17) 0.0504(15) 0.0447(14) -0.0047(12) 0.0101(13) 0.0160(13)
F6 0.0419(16) 0.0627(19) 0.158(4) 0.001(2) -0.028(2) -0.0010(14)
F7 0.079(2) 0.0524(17) 0.151(4) -0.024(2) 0.065(2) -0.0318(16)
F8 0.127(3) 0.101(3) 0.075(2) -0.052(2) 0.011(2) 0.009(3)
Co1 0.01262(19) 0.0262(2) 0.0181(2) -0.00485(15) -0.00119(14) -0.00108(14)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
C10 C11 1.482(5) . ?
C10 N1 1.511(4) . ?
C11 N10 1.363(4) . ?
C11 C12 1.367(4) . ?
C12 N12 1.356(4) . ?
C13 N12 1.461(4) . ?
C13 C14 1.513(5) . ?
C14 C15 1.383(6) . ?
C14 C19 1.393(5) . ?
C15 C16 1.385(6) . ?
C16 C17 1.385(6) . ?
C17 C18 1.387(7) . ?
C18 C19 1.385(7) . ?
C20 C21 1.488(4) . ?
C20 N1 1.498(4) . ?
C21 N20 1.363(5) . ?
C21 C22 1.367(5) . ?
C22 N22 1.340(5) . ?
C23 N22 1.477(4) . ?
C23 C24 1.497(5) . ?
C24 C29 1.375(5) . ?
C24 C25 1.387(5) . ?
C25 C26 1.483(7) . ?
C26 C27 1.356(8) . ?
C27 C28 1.319(8) . ?
C28 C29 1.340(6) . ?
C30 C31 1.485(5) . ?
C30 N1 1.525(4) . ?
C31 N30 1.345(4) . ?
C31 C32 1.371(5) . ?
C32 N32 1.349(5) . ?
C33 N32 1.477(4) . ?
C33 C34 1.512(5) . ?
C34 C39 1.388(5) . ?
C34 C35 1.394(5) . ?
C35 C36 1.393(5) . ?
C36 C37 1.388(6) . ?
C37 C38 1.388(6) . ?
C38 C39 1.382(6) . ?
B1 F1 1.352(7) . ?
B1 F2 1.365(7) . ?
B1 F4 1.386(5) . ?
B1 F3 1.402(6) . ?
B2 F6 1.356(6) . ?
B2 F7 1.361(5) . ?
B2 F8 1.373(6) . ?
B2 F5 1.380(5) . ?
N1 Co1 2.012(3) . ?
N10 N11 1.309(4) . ?
N10 Co1 1.899(3) . ?
N11 N12 1.336(4) . ?
N20 N21 1.314(3) . ?
N20 Co1 1.908(3) . ?
N21 N22 1.342(5) . ?
N30 N31 1.315(4) . ?
N30 Co1 1.886(3) . ?
N31 N32 1.337(4) . ?
O1 Co1 1.905(2) 5 ?
O1 Co1 1.909(2) . ?
Co1 O1 1.905(2) 5 ?
Co1 Co1 2.8779(8) 5 ?
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
C11 C10 N1 105.1(2) . . ?
N10 C11 C12 106.4(3) . . ?
N10 C11 C10 114.9(3) . . ?
C12 C11 C10 138.6(3) . . ?
N12 C12 C11 104.6(3) . . ?
N12 C13 C14 112.2(3) . . ?
C15 C14 C19 119.3(4) . . ?
C15 C14 C13 122.2(3) . . ?
C19 C14 C13 118.5(4) . . ?
C14 C15 C16 120.9(4) . . ?
C15 C16 C17 119.7(4) . . ?
C18 C17 C16 119.7(4) . . ?
C19 C18 C17 120.5(4) . . ?
C18 C19 C14 119.8(4) . . ?
C21 C20 N1 106.2(3) . . ?
N20 C21 C22 106.6(3) . . ?
N20 C21 C20 116.3(3) . . ?
C22 C21 C20 137.1(4) . . ?
N22 C22 C21 104.7(4) . . ?
N22 C23 C24 112.2(3) . . ?
C29 C24 C25 120.1(4) . . ?
C29 C24 C23 119.1(4) . . ?
C25 C24 C23 120.8(4) . . ?
C24 C25 C26 116.3(4) . . ?
C27 C26 C25 117.5(4) . . ?
C28 C27 C26 124.3(4) . . ?
C27 C28 C29 119.1(5) . . ?
C28 C29 C24 122.7(5) . . ?
C31 C30 N1 109.8(3) . . ?
N30 C31 C32 106.5(3) . . ?
N30 C31 C30 117.7(3) . . ?
C32 C31 C30 135.7(3) . . ?
N32 C32 C31 104.6(3) . . ?
N32 C33 C34 111.7(3) . . ?
C39 C34 C35 119.2(3) . . ?
C39 C34 C33 121.4(3) . . ?
C35 C34 C33 119.4(3) . . ?
C36 C35 C34 120.7(3) . . ?
C37 C36 C35 119.4(4) . . ?
C38 C37 C36 120.0(3) . . ?
C39 C38 C37 120.4(4) . . ?
C38 C39 C34 120.3(4) . . ?
F1 B1 F2 110.1(5) . . ?
F1 B1 F4 107.5(4) . . ?
F2 B1 F4 109.8(5) . . ?
F1 B1 F3 109.9(5) . . ?
F2 B1 F3 108.6(4) . . ?
F4 B1 F3 111.0(3) . . ?
F6 B2 F7 109.4(5) . . ?
F6 B2 F8 109.7(4) . . ?
F7 B2 F8 107.1(4) . . ?
F6 B2 F5 108.8(4) . . ?
F7 B2 F5 110.6(4) . . ?
F8 B2 F5 111.2(5) . . ?
C20 N1 C10 111.4(2) . . ?
C20 N1 C30 111.2(3) . . ?
C10 N1 C30 110.2(2) . . ?
C20 N1 Co1 107.83(19) . . ?
C10 N1 Co1 105.78(18) . . ?
C30 N1 Co1 110.2(2) . . ?
N11 N10 C11 111.8(2) . . ?
N11 N10 Co1 132.0(2) . . ?
C11 N10 Co1 115.2(2) . . ?
N10 N11 N12 104.6(2) . . ?
N11 N12 C12 112.5(3) . . ?
N11 N12 C13 118.4(3) . . ?
C12 N12 C13 128.6(3) . . ?
N21 N20 C21 111.5(3) . . ?
N21 N20 Co1 133.5(3) . . ?
C21 N20 Co1 114.8(2) . . ?
N20 N21 N22 104.1(3) . . ?
C22 N22 N21 113.1(3) . . ?
C22 N22 C23 128.0(4) . . ?
N21 N22 C23 118.9(4) . . ?
N31 N30 C31 112.1(3) . . ?
N31 N30 Co1 130.7(2) . . ?
C31 N30 Co1 116.8(2) . . ?
N30 N31 N32 104.3(3) . . ?
N31 N32 C32 112.5(3) . . ?
N31 N32 C33 119.0(3) . . ?
C32 N32 C33 128.5(3) . . ?
Co1 O1 Co1 97.97(10) 5 . ?
N30 Co1 N10 88.11(11) . . ?
N30 Co1 O1 96.45(10) . 5 ?
N10 Co1 O1 97.11(10) . 5 ?
N30 Co1 N20 90.09(11) . . ?
N10 Co1 N20 165.21(12) . . ?
O1 Co1 N20 97.68(11) 5 . ?
N30 Co1 O1 176.38(11) . . ?
N10 Co1 O1 88.83(10) . . ?
O1 Co1 O1 82.03(10) 5 . ?
N20 Co1 O1 93.36(11) . . ?
N30 Co1 N1 85.18(11) . . ?
N10 Co1 N1 82.32(11) . . ?
O1 Co1 N1 178.27(10) 5 . ?
N20 Co1 N1 82.90(11) . . ?
O1 Co1 N1 96.32(10) . . ?
N30 Co1 Co1 137.42(8) . 5 ?
N10 Co1 Co1 93.92(8) . 5 ?
O1 Co1 Co1 41.06(6) 5 5 ?
N20 Co1 Co1 97.32(8) . 5 ?
O1 Co1 Co1 40.97(6) . 5 ?
N1 Co1 Co1 137.28(8) . 5 ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.31
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.400
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.104