# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2009

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'Emma Gallo'
_publ_contact_author_email       EMMA.GALLO@UNIMI.IT

_publ_section_title              
;
The Key-Intermediate in the Aminations of Saturated
C-H Bonds: Synthesis, X-ray Characterization and Catalytic Activity of
Ru(TPP)(NAr)2 (Ar = 3,5-(CF3)2C6H3)
;
loop_
_publ_author_name
'Emma Gallo'
'Nicola Casati'
'Alessandro Caselli'
'Sergio Cenini'
'Simone Fantauzzi'
'Piero Macchi'
;
F.Ragaini
;

# Attachment 'complexes 1 and 2-revised-2.cif'

data_complex1
_database_code_depnum_ccdc_archive 'CCDC 720709'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H34 F12 N6 Ru'
_chemical_formula_sum            'C60 H34 F12 N6 Ru'
_chemical_formula_weight         1168.00

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'
F F 0.0171 0.0103 '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'

_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                   11.961(2)
_cell_length_b                   13.080(2)
_cell_length_c                   17.084(3)
_cell_angle_alpha                107.893(2)
_cell_angle_beta                 104.084(2)
_cell_angle_gamma                93.677(2)
_cell_volume                     2439.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(1)
_cell_measurement_reflns_used    2313
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      21.9

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART-ApexII'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19912
_diffrn_reflns_av_R_equivalents  0.0744
_diffrn_reflns_av_sigmaI/netI    0.0979
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.30
_diffrn_reflns_theta_max         23.27
_reflns_number_total             7010
_reflns_number_gt                4412
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+0.8982P] 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         7010
_refine_ls_number_parameters     652
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1156
_refine_ls_wR_factor_gt          0.0948
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.3159(4) 0.5350(4) 0.7925(3) 0.0207(13) Uani 1 1 d . . .
C12 C 0.4367(4) 0.5466(4) 0.8167(3) 0.0224(13) Uani 1 1 d . . .
C13 C 0.5067(5) 0.4809(4) 0.8558(3) 0.0261(14) Uani 1 1 d . . .
H13 H 0.4788 0.4221 0.8691 0.031 Uiso 1 1 calc R . .
C14 C 0.6194(5) 0.5188(4) 0.8700(3) 0.0266(14) Uani 1 1 d . . .
H14 H 0.6830 0.4921 0.8962 0.032 Uiso 1 1 calc R . .
C15 C 0.6248(5) 0.6073(4) 0.8377(3) 0.0214(13) Uani 1 1 d . . .
C21 C 0.7260(4) 0.6663(4) 0.8374(3) 0.0214(13) Uani 1 1 d . . .
C22 C 0.7301(5) 0.7513(4) 0.8030(3) 0.0234(13) Uani 1 1 d . . .
C23 C 0.8348(5) 0.8077(4) 0.7986(3) 0.0277(14) Uani 1 1 d . . .
H23 H 0.9104 0.7942 0.8172 0.033 Uiso 1 1 calc R . .
C24 C 0.8033(5) 0.8831(5) 0.7627(4) 0.0335(15) Uani 1 1 d . . .
H24 H 0.8530 0.9309 0.7514 0.040 Uiso 1 1 calc R . .
C25 C 0.6790(4) 0.8768(4) 0.7449(3) 0.0202(13) Uani 1 1 d . . .
C31 C 0.6132(5) 0.9426(4) 0.7074(3) 0.0249(14) Uani 1 1 d . . .
C32 C 0.4914(5) 0.9301(4) 0.6834(3) 0.0232(13) Uani 1 1 d . . .
C33 C 0.4218(5) 1.0010(4) 0.6487(3) 0.0277(14) Uani 1 1 d . . .
H33 H 0.4500 1.0623 0.6388 0.033 Uiso 1 1 calc R . .
C34 C 0.3096(5) 0.9623(4) 0.6338(3) 0.0294(14) Uani 1 1 d . . .
H34 H 0.2461 0.9909 0.6096 0.035 Uiso 1 1 calc R . .
C35 C 0.3036(4) 0.8695(4) 0.6611(3) 0.0225(13) Uani 1 1 d . . .
C41 C 0.2028(4) 0.8085(4) 0.6599(3) 0.0203(13) Uani 1 1 d . . .
C42 C 0.1980(4) 0.7235(4) 0.6921(3) 0.0211(13) Uani 1 1 d . . .
C43 C 0.0938(5) 0.6671(4) 0.6959(3) 0.0280(14) Uani 1 1 d . . .
H43 H 0.0182 0.6799 0.6764 0.034 Uiso 1 1 calc R . .
C44 C 0.1249(4) 0.5924(4) 0.7328(3) 0.0272(14) Uani 1 1 d . . .
H44 H 0.0741 0.5443 0.7431 0.033 Uiso 1 1 calc R . .
C45 C 0.2487(4) 0.5988(4) 0.7538(3) 0.0220(13) Uani 1 1 d . . .
C2 C 0.5460(3) 0.9387(2) 0.90210(19) 0.0234(13) Uani 1 1 d G . .
C52 C 0.5147(2) 1.0358(3) 0.89298(19) 0.0260(13) Uani 1 1 d G . .
H52 H 0.4478 1.0351 0.8513 0.031 Uiso 1 1 calc R . .
C53 C 0.5833(3) 1.1339(2) 0.9461(2) 0.0305(14) Uani 1 1 d G . .
C54 C 0.6834(3) 1.1349(2) 1.0084(2) 0.0319(15) Uani 1 1 d G . .
H54 H 0.7293 1.2006 1.0439 0.038 Uiso 1 1 calc R . .
C55 C 0.7147(2) 1.0379(3) 1.01749(19) 0.0287(14) Uani 1 1 d G . .
C56 C 0.6460(3) 0.9397(2) 0.9644(2) 0.0272(14) Uani 1 1 d G . .
H56 H 0.6670 0.8748 0.9705 0.033 Uiso 1 1 calc R . .
C1 C 0.5469(4) 0.6317(4) 0.5934(3) 0.0248(13) Uani 1 1 d . . .
C62 C 0.6369(5) 0.5683(4) 0.6010(3) 0.0258(13) Uani 1 1 d . . .
H62 H 0.6531 0.5407 0.6459 0.031 Uiso 1 1 calc R . .
C63 C 0.7017(4) 0.5464(4) 0.5422(3) 0.0258(14) Uani 1 1 d . . .
C64 C 0.6786(5) 0.5863(4) 0.4744(4) 0.0314(14) Uani 1 1 d . . .
H64 H 0.7202 0.5694 0.4338 0.038 Uiso 1 1 calc R . .
C65 C 0.5917(5) 0.6522(4) 0.4681(3) 0.0296(14) Uani 1 1 d . . .
C66 C 0.5277(4) 0.6749(4) 0.5255(3) 0.0264(14) Uani 1 1 d . . .
H66 H 0.4706 0.7193 0.5200 0.032 Uiso 1 1 calc R . .
C111 C 0.2506(3) 0.4426(2) 0.8071(2) 0.0244(13) Uani 1 1 d G . .
C112 C 0.2724(3) 0.4323(3) 0.88788(19) 0.0266(14) Uani 1 1 d G . .
H112 H 0.3253 0.4844 0.9345 0.032 Uiso 1 1 calc R . .
C113 C 0.2150(3) 0.3442(3) 0.8990(2) 0.0352(15) Uani 1 1 d G . .
H113 H 0.2296 0.3374 0.9530 0.042 Uiso 1 1 calc R . .
C114 C 0.1358(3) 0.2664(2) 0.8294(3) 0.0423(17) Uani 1 1 d G . .
H114 H 0.0974 0.2074 0.8368 0.051 Uiso 1 1 calc R . .
C115 C 0.1140(3) 0.2766(2) 0.7487(2) 0.0351(15) Uani 1 1 d G . .
H115 H 0.0610 0.2246 0.7021 0.042 Uiso 1 1 calc R . .
C116 C 0.1714(3) 0.3648(3) 0.73752(18) 0.0303(14) Uani 1 1 d G . .
H116 H 0.1568 0.3716 0.6835 0.036 Uiso 1 1 calc R . .
C121 C 0.8414(2) 0.6395(3) 0.8776(2) 0.0218(13) Uani 1 1 d G . .
C122 C 0.8733(3) 0.5382(2) 0.84456(19) 0.0293(14) Uani 1 1 d G . .
H122 H 0.8224 0.4854 0.7972 0.035 Uiso 1 1 calc R . .
C123 C 0.9814(3) 0.5157(2) 0.8823(2) 0.0330(15) Uani 1 1 d G . .
H123 H 1.0028 0.4479 0.8602 0.040 Uiso 1 1 calc R . .
C124 C 1.0575(2) 0.5946(3) 0.9530(2) 0.0354(15) Uani 1 1 d G . .
H124 H 1.1298 0.5796 0.9783 0.042 Uiso 1 1 calc R . .
C125 C 1.0256(3) 0.6960(3) 0.98604(19) 0.0337(15) Uani 1 1 d G . .
H125 H 1.0765 0.7487 1.0334 0.040 Uiso 1 1 calc R . .
C126 C 0.9175(3) 0.7184(2) 0.9483(2) 0.0278(14) Uani 1 1 d G . .
H126 H 0.8962 0.7862 0.9704 0.033 Uiso 1 1 calc R . .
C131 C 0.6768(3) 1.0379(2) 0.6963(2) 0.0230(13) Uani 1 1 d G . .
C132 C 0.6650(3) 1.0461(3) 0.61552(19) 0.0275(14) Uani 1 1 d G . .
H132 H 0.6194 0.9909 0.5672 0.033 Uiso 1 1 calc R . .
C133 C 0.7213(3) 1.1368(3) 0.6071(2) 0.0356(15) Uani 1 1 d G . .
H133 H 0.7134 1.1423 0.5530 0.043 Uiso 1 1 calc R . .
C134 C 0.7894(3) 1.2193(3) 0.6793(3) 0.0389(16) Uani 1 1 d G . .
H134 H 0.8270 1.2800 0.6737 0.047 Uiso 1 1 calc R . .
C135 C 0.8012(3) 1.2112(3) 0.7601(2) 0.0413(16) Uani 1 1 d G . .
H135 H 0.8467 1.2664 0.8084 0.050 Uiso 1 1 calc R . .
C136 C 0.7449(3) 1.1205(3) 0.76855(18) 0.0341(15) Uani 1 1 d G . .
H136 H 0.7528 1.1150 0.8226 0.041 Uiso 1 1 calc R . .
C141 C 0.0890(2) 0.8410(3) 0.6212(2) 0.0243(13) Uani 1 1 d G . .
C142 C 0.0573(3) 0.9396(3) 0.66200(18) 0.0301(14) Uani 1 1 d G . .
H142 H 0.1046 0.9847 0.7149 0.036 Uiso 1 1 calc R . .
C143 C -0.0450(3) 0.9709(2) 0.6237(2) 0.0327(15) Uani 1 1 d G . .
H143 H -0.0662 1.0369 0.6510 0.039 Uiso 1 1 calc R . .
C144 C -0.1157(2) 0.9035(3) 0.5447(2) 0.0390(16) Uani 1 1 d G . .
H144 H -0.1842 0.9244 0.5191 0.047 Uiso 1 1 calc R . .
C145 C -0.0840(3) 0.8048(3) 0.50396(19) 0.0451(17) Uani 1 1 d G . .
H145 H -0.1313 0.7598 0.4511 0.054 Uiso 1 1 calc R . .
C146 C 0.0183(3) 0.7736(2) 0.5422(2) 0.0376(16) Uani 1 1 d G . .
H146 H 0.0395 0.7076 0.5150 0.045 Uiso 1 1 calc R . .
C510 C 0.8232(6) 1.0380(6) 1.0818(4) 0.0497(18) Uani 1 1 d . . .
C511 C 0.5490(6) 1.2363(5) 0.9360(5) 0.0459(18) Uani 1 1 d . . .
C610 C 0.5644(6) 0.6972(5) 0.3968(4) 0.0380(16) Uani 1 1 d . . .
C611 C 0.7935(5) 0.4753(5) 0.5499(4) 0.0359(15) Uani 1 1 d . . .
N11 N 0.5113(4) 0.6233(3) 0.8059(3) 0.0200(10) Uani 1 1 d . . .
N21 N 0.6360(4) 0.7938(3) 0.7682(3) 0.0194(11) Uani 1 1 d . . .
N31 N 0.4164(4) 0.8509(3) 0.6902(3) 0.0227(11) Uani 1 1 d . . .
N41 N 0.2917(4) 0.6805(3) 0.7276(3) 0.0218(11) Uani 1 1 d . . .
N2 N 0.4763(3) 0.8409(3) 0.8488(3) 0.0216(10) Uani 1 1 d . . .
N1 N 0.4781(3) 0.6477(3) 0.6475(3) 0.0226(11) Uani 1 1 d . . .
F51 F 0.9083(4) 1.0116(4) 1.0467(3) 0.111(2) Uani 1 1 d . . .
F52 F 0.8114(5) 0.9642(4) 1.1167(3) 0.141(3) Uani 1 1 d . . .
F53 F 0.8646(3) 1.1303(3) 1.1423(2) 0.0629(11) Uani 1 1 d . . .
F54 F 0.4890(4) 1.2830(3) 0.9884(3) 0.0966(17) Uani 1 1 d . . .
F55 F 0.6401(4) 1.3098(3) 0.9509(4) 0.1079(19) Uani 1 1 d . . .
F56 F 0.4834(4) 1.2242(3) 0.8585(3) 0.0847(15) Uani 1 1 d . . .
F61 F 0.5551(4) 0.8016(3) 0.4245(2) 0.0779(14) Uani 1 1 d . . .
F62 F 0.4620(3) 0.6503(3) 0.3407(2) 0.0699(12) Uani 1 1 d . . .
F63 F 0.6409(3) 0.6864(3) 0.3516(2) 0.0620(11) Uani 1 1 d . . .
F64 F 0.8503(3) 0.4913(3) 0.6315(2) 0.0532(10) Uani 1 1 d . . .
F65 F 0.8746(3) 0.4916(3) 0.5123(2) 0.0575(11) Uani 1 1 d . . .
F66 F 0.7516(3) 0.3699(3) 0.5153(2) 0.0562(10) Uani 1 1 d . . .
Ru1 Ru 0.46352(4) 0.73611(4) 0.74806(3) 0.02172(15) Uani 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
C11 0.021(3) 0.022(3) 0.020(3) 0.004(3) 0.009(3) 0.006(3)
C12 0.024(3) 0.016(3) 0.025(3) 0.005(3) 0.007(3) -0.002(3)
C13 0.031(4) 0.021(3) 0.036(4) 0.018(3) 0.015(3) 0.003(3)
C14 0.028(4) 0.029(4) 0.028(3) 0.016(3) 0.008(3) 0.008(3)
C15 0.028(3) 0.020(3) 0.026(3) 0.015(3) 0.012(3) 0.010(3)
C21 0.019(3) 0.028(3) 0.020(3) 0.010(3) 0.007(3) 0.008(3)
C22 0.026(3) 0.022(3) 0.025(3) 0.009(3) 0.009(3) 0.006(3)
C23 0.015(3) 0.038(4) 0.035(4) 0.020(3) 0.003(3) 0.008(3)
C24 0.033(4) 0.038(4) 0.040(4) 0.022(3) 0.015(3) 0.008(3)
C25 0.016(3) 0.023(3) 0.024(3) 0.008(3) 0.009(3) 0.003(3)
C31 0.024(3) 0.024(3) 0.026(3) 0.008(3) 0.009(3) -0.001(3)
C32 0.026(3) 0.024(3) 0.024(3) 0.012(3) 0.007(3) 0.007(3)
C33 0.025(3) 0.030(4) 0.035(4) 0.023(3) 0.007(3) 0.004(3)
C34 0.021(3) 0.035(4) 0.041(4) 0.026(3) 0.006(3) 0.009(3)
C35 0.019(3) 0.030(4) 0.020(3) 0.009(3) 0.007(3) 0.005(3)
C41 0.017(3) 0.026(3) 0.019(3) 0.008(3) 0.006(2) 0.006(3)
C42 0.022(3) 0.025(3) 0.018(3) 0.007(3) 0.007(3) 0.010(3)
C43 0.022(3) 0.032(4) 0.032(4) 0.013(3) 0.009(3) 0.001(3)
C44 0.022(3) 0.028(4) 0.033(4) 0.013(3) 0.007(3) 0.003(3)
C45 0.021(3) 0.020(3) 0.023(3) 0.006(3) 0.004(3) 0.005(3)
C2 0.027(3) 0.023(3) 0.022(3) 0.006(3) 0.012(3) 0.010(3)
C52 0.023(3) 0.028(3) 0.029(3) 0.011(3) 0.006(3) 0.010(3)
C53 0.033(4) 0.025(4) 0.033(4) 0.006(3) 0.011(3) 0.009(3)
C54 0.032(4) 0.025(4) 0.033(4) 0.001(3) 0.012(3) -0.005(3)
C55 0.029(3) 0.030(4) 0.025(3) 0.007(3) 0.006(3) 0.005(3)
C56 0.027(3) 0.030(4) 0.030(3) 0.014(3) 0.012(3) 0.012(3)
C1 0.023(3) 0.024(3) 0.024(3) 0.006(3) 0.003(3) 0.002(3)
C62 0.033(3) 0.022(3) 0.021(3) 0.006(3) 0.007(3) 0.004(3)
C63 0.016(3) 0.023(3) 0.035(4) 0.008(3) 0.002(3) 0.002(3)
C64 0.036(4) 0.029(4) 0.032(4) 0.008(3) 0.014(3) 0.007(3)
C65 0.036(4) 0.034(4) 0.026(3) 0.013(3) 0.017(3) 0.010(3)
C66 0.025(3) 0.028(3) 0.028(3) 0.009(3) 0.009(3) 0.012(3)
C111 0.022(3) 0.020(3) 0.034(4) 0.014(3) 0.007(3) 0.006(3)
C112 0.019(3) 0.032(4) 0.033(4) 0.015(3) 0.008(3) 0.006(3)
C113 0.027(3) 0.042(4) 0.050(4) 0.030(4) 0.014(3) 0.010(3)
C114 0.039(4) 0.033(4) 0.070(5) 0.029(4) 0.026(4) 0.008(3)
C115 0.026(3) 0.028(4) 0.047(4) 0.008(3) 0.009(3) -0.002(3)
C116 0.028(3) 0.027(4) 0.035(4) 0.008(3) 0.011(3) 0.002(3)
C121 0.015(3) 0.033(4) 0.022(3) 0.015(3) 0.003(3) 0.004(3)
C122 0.025(3) 0.030(4) 0.038(4) 0.015(3) 0.013(3) 0.006(3)
C123 0.033(4) 0.034(4) 0.041(4) 0.018(3) 0.017(3) 0.014(3)
C124 0.021(3) 0.053(4) 0.043(4) 0.030(4) 0.009(3) 0.013(3)
C125 0.030(4) 0.042(4) 0.030(4) 0.020(3) 0.003(3) -0.004(3)
C126 0.022(3) 0.031(4) 0.035(4) 0.017(3) 0.007(3) 0.009(3)
C131 0.024(3) 0.018(3) 0.029(3) 0.013(3) 0.005(3) 0.005(3)
C132 0.025(3) 0.028(3) 0.037(4) 0.018(3) 0.012(3) 0.007(3)
C133 0.033(4) 0.048(4) 0.043(4) 0.030(4) 0.020(3) 0.017(3)
C134 0.034(4) 0.030(4) 0.061(5) 0.026(4) 0.014(3) 0.002(3)
C135 0.040(4) 0.032(4) 0.048(4) 0.014(3) 0.009(3) -0.006(3)
C136 0.037(4) 0.033(4) 0.035(4) 0.017(3) 0.009(3) 0.002(3)
C141 0.021(3) 0.030(4) 0.030(4) 0.016(3) 0.014(3) 0.009(3)
C142 0.031(4) 0.030(4) 0.028(3) 0.009(3) 0.007(3) 0.006(3)
C143 0.029(4) 0.031(4) 0.046(4) 0.021(3) 0.012(3) 0.012(3)
C144 0.023(3) 0.052(4) 0.046(4) 0.022(4) 0.007(3) 0.014(3)
C145 0.032(4) 0.055(5) 0.032(4) 0.001(3) -0.004(3) 0.012(3)
C146 0.031(4) 0.044(4) 0.030(4) 0.005(3) 0.002(3) 0.015(3)
C510 0.044(5) 0.048(5) 0.048(5) 0.010(4) 0.002(4) 0.009(4)
C511 0.057(5) 0.023(4) 0.054(5) 0.012(3) 0.007(4) 0.011(4)
C610 0.045(4) 0.038(4) 0.037(4) 0.016(3) 0.018(4) 0.010(3)
C611 0.033(4) 0.038(4) 0.034(4) 0.010(3) 0.007(3) 0.005(3)
N11 0.021(3) 0.019(3) 0.022(3) 0.006(2) 0.008(2) 0.007(2)
N21 0.026(3) 0.014(3) 0.025(3) 0.011(2) 0.014(2) 0.004(2)
N31 0.021(3) 0.026(3) 0.021(3) 0.008(2) 0.005(2) 0.006(2)
N41 0.020(3) 0.025(3) 0.021(3) 0.010(2) 0.002(2) 0.005(2)
N2 0.023(3) 0.019(3) 0.023(3) 0.008(2) 0.008(2) 0.002(2)
N1 0.025(3) 0.020(3) 0.022(3) 0.006(2) 0.006(2) 0.001(2)
F51 0.058(3) 0.151(5) 0.073(3) -0.021(3) -0.013(3) 0.055(3)
F52 0.130(5) 0.115(4) 0.137(5) 0.098(4) -0.089(4) -0.057(4)
F53 0.051(2) 0.056(3) 0.046(2) -0.011(2) -0.0116(19) 0.006(2)
F54 0.154(5) 0.071(3) 0.095(4) 0.038(3) 0.061(3) 0.077(3)
F55 0.074(3) 0.050(3) 0.195(6) 0.070(3) -0.005(3) -0.008(3)
F56 0.138(4) 0.035(2) 0.063(3) 0.021(2) -0.013(3) 0.020(2)
F61 0.158(4) 0.047(3) 0.054(3) 0.034(2) 0.048(3) 0.039(3)
F62 0.054(3) 0.107(4) 0.056(3) 0.050(3) 0.001(2) 0.002(2)
F63 0.056(3) 0.103(3) 0.056(3) 0.052(2) 0.032(2) 0.029(2)
F64 0.039(2) 0.073(3) 0.046(2) 0.020(2) 0.0046(19) 0.027(2)
F65 0.045(2) 0.072(3) 0.083(3) 0.043(2) 0.041(2) 0.026(2)
F66 0.038(2) 0.034(2) 0.085(3) 0.012(2) 0.007(2) 0.0121(18)
Ru1 0.0203(3) 0.0232(3) 0.0230(3) 0.0098(2) 0.0053(2) 0.00570(19)

_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
C11 C12 1.387(7) . ?
C11 C45 1.395(7) . ?
C11 C111 1.515(6) . ?
C12 N11 1.384(6) . ?
C12 C13 1.435(7) . ?
C13 C14 1.343(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.431(7) . ?
C14 H14 0.9300 . ?
C15 N11 1.389(6) . ?
C15 C21 1.395(7) . ?
C21 C22 1.411(7) . ?
C21 C121 1.499(5) . ?
C22 N21 1.375(6) . ?
C22 C23 1.443(7) . ?
C23 C24 1.339(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.435(7) . ?
C24 H24 0.9300 . ?
C25 N21 1.376(6) . ?
C25 C31 1.397(7) . ?
C31 C32 1.398(7) . ?
C31 C131 1.505(6) . ?
C32 N31 1.378(6) . ?
C32 C33 1.448(7) . ?
C33 C34 1.337(7) . ?
C33 H33 0.9300 . ?
C34 C35 1.432(7) . ?
C34 H34 0.9300 . ?
C35 N31 1.385(6) . ?
C35 C41 1.395(7) . ?
C41 C42 1.386(7) . ?
C41 C141 1.510(5) . ?
C42 N41 1.380(6) . ?
C42 C43 1.433(7) . ?
C43 C44 1.342(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.426(7) . ?
C44 H44 0.9300 . ?
C45 N41 1.393(6) . ?
C2 C52 1.3900 . ?
C2 C56 1.3900 . ?
C2 N2 1.392(4) . ?
C52 C53 1.3900 . ?
C52 H52 0.9300 . ?
C53 C54 1.3900 . ?
C53 C511 1.474(6) . ?
C54 C55 1.3900 . ?
C54 H54 0.9300 . ?
C55 C56 1.3900 . ?
C55 C510 1.482(7) . ?
C56 H56 0.9300 . ?
C1 N1 1.361(6) . ?
C1 C62 1.405(7) . ?
C1 C66 1.417(7) . ?
C62 C63 1.386(7) . ?
C62 H62 0.9300 . ?
C63 C64 1.387(7) . ?
C63 C611 1.491(7) . ?
C64 C65 1.397(7) . ?
C64 H64 0.9300 . ?
C65 C66 1.360(7) . ?
C65 C610 1.487(8) . ?
C66 H66 0.9300 . ?
C111 C112 1.3900 . ?
C111 C116 1.3900 . ?
C112 C113 1.3900 . ?
C112 H112 0.9300 . ?
C113 C114 1.3900 . ?
C113 H113 0.9300 . ?
C114 C115 1.3900 . ?
C114 H114 0.9300 . ?
C115 C116 1.3900 . ?
C115 H115 0.9300 . ?
C116 H116 0.9300 . ?
C121 C122 1.3900 . ?
C121 C126 1.3900 . ?
C122 C123 1.3900 . ?
C122 H122 0.9300 . ?
C123 C124 1.3900 . ?
C123 H123 0.9300 . ?
C124 C125 1.3900 . ?
C124 H124 0.9300 . ?
C125 C126 1.3900 . ?
C125 H125 0.9300 . ?
C126 H126 0.9300 . ?
C131 C132 1.3900 . ?
C131 C136 1.3900 . ?
C132 C133 1.3900 . ?
C132 H132 0.9300 . ?
C133 C134 1.3900 . ?
C133 H133 0.9300 . ?
C134 C135 1.3900 . ?
C134 H134 0.9300 . ?
C135 C136 1.3900 . ?
C135 H135 0.9300 . ?
C136 H136 0.9300 . ?
C141 C142 1.3900 . ?
C141 C146 1.3900 . ?
C142 C143 1.3900 . ?
C142 H142 0.9300 . ?
C143 C144 1.3900 . ?
C143 H143 0.9300 . ?
C144 C145 1.3900 . ?
C144 H144 0.9300 . ?
C145 C146 1.3900 . ?
C145 H145 0.9300 . ?
C146 H146 0.9300 . ?
C510 F53 1.295(7) . ?
C510 F52 1.298(7) . ?
C510 F51 1.315(7) . ?
C511 F54 1.313(7) . ?
C511 F56 1.321(7) . ?
C511 F55 1.325(7) . ?
C610 F63 1.322(6) . ?
C610 F61 1.323(6) . ?
C610 F62 1.330(7) . ?
C611 F65 1.326(6) . ?
C611 F66 1.330(6) . ?
C611 F64 1.338(6) . ?
N11 Ru1 2.052(4) . ?
N21 Ru1 2.059(4) . ?
N31 Ru1 2.073(4) . ?
N41 Ru1 2.044(4) . ?
N2 Ru1 1.806(4) . ?
N1 Ru1 1.808(4) . ?

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
C12 C11 C45 126.1(5) . . ?
C12 C11 C111 117.1(4) . . ?
C45 C11 C111 116.8(4) . . ?
N11 C12 C11 125.7(5) . . ?
N11 C12 C13 107.7(5) . . ?
C11 C12 C13 126.6(5) . . ?
C14 C13 C12 108.3(5) . . ?
C14 C13 H13 125.8 . . ?
C12 C13 H13 125.8 . . ?
C13 C14 C15 108.2(5) . . ?
C13 C14 H14 125.9 . . ?
C15 C14 H14 125.9 . . ?
N11 C15 C21 126.1(5) . . ?
N11 C15 C14 107.8(4) . . ?
C21 C15 C14 126.1(5) . . ?
C15 C21 C22 125.6(5) . . ?
C15 C21 C121 118.3(4) . . ?
C22 C21 C121 116.1(4) . . ?
N21 C22 C21 126.0(5) . . ?
N21 C22 C23 108.7(5) . . ?
C21 C22 C23 125.2(5) . . ?
C24 C23 C22 107.5(5) . . ?
C24 C23 H23 126.2 . . ?
C22 C23 H23 126.2 . . ?
C23 C24 C25 107.7(5) . . ?
C23 C24 H24 126.1 . . ?
C25 C24 H24 126.1 . . ?
N21 C25 C31 126.1(5) . . ?
N21 C25 C24 109.0(4) . . ?
C31 C25 C24 124.9(5) . . ?
C25 C31 C32 124.7(5) . . ?
C25 C31 C131 118.3(4) . . ?
C32 C31 C131 116.9(4) . . ?
N31 C32 C31 126.6(5) . . ?
N31 C32 C33 107.8(5) . . ?
C31 C32 C33 125.6(5) . . ?
C34 C33 C32 107.7(5) . . ?
C34 C33 H33 126.1 . . ?
C32 C33 H33 126.1 . . ?
C33 C34 C35 108.5(5) . . ?
C33 C34 H34 125.7 . . ?
C35 C34 H34 125.7 . . ?
N31 C35 C41 125.4(5) . . ?
N31 C35 C34 107.9(4) . . ?
C41 C35 C34 126.7(5) . . ?
C42 C41 C35 126.3(5) . . ?
C42 C41 C141 117.8(4) . . ?
C35 C41 C141 115.8(4) . . ?
N41 C42 C41 126.4(5) . . ?
N41 C42 C43 108.2(5) . . ?
C41 C42 C43 125.4(5) . . ?
C44 C43 C42 107.8(5) . . ?
C44 C43 H43 126.1 . . ?
C42 C43 H43 126.1 . . ?
C43 C44 C45 108.7(5) . . ?
C43 C44 H44 125.6 . . ?
C45 C44 H44 125.6 . . ?
N41 C45 C11 125.4(5) . . ?
N41 C45 C44 107.6(4) . . ?
C11 C45 C44 127.0(5) . . ?
C52 C2 C56 120.0 . . ?
C52 C2 N2 119.5(3) . . ?
C56 C2 N2 120.5(3) . . ?
C2 C52 C53 120.0 . . ?
C2 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 C511 120.5(4) . . ?
C52 C53 C511 119.5(4) . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C56 C55 C54 120.0 . . ?
C56 C55 C510 119.6(4) . . ?
C54 C55 C510 120.3(4) . . ?
C55 C56 C2 120.0 . . ?
C55 C56 H56 120.0 . . ?
C2 C56 H56 120.0 . . ?
N1 C1 C62 121.0(5) . . ?
N1 C1 C66 121.2(5) . . ?
C62 C1 C66 117.7(5) . . ?
C63 C62 C1 120.8(5) . . ?
C63 C62 H62 119.6 . . ?
C1 C62 H62 119.6 . . ?
C62 C63 C64 120.6(5) . . ?
C62 C63 C611 119.6(5) . . ?
C64 C63 C611 119.8(5) . . ?
C63 C64 C65 118.8(5) . . ?
C63 C64 H64 120.6 . . ?
C65 C64 H64 120.6 . . ?
C66 C65 C64 121.3(5) . . ?
C66 C65 C610 118.0(5) . . ?
C64 C65 C610 120.7(5) . . ?
C65 C66 C1 120.7(5) . . ?
C65 C66 H66 119.6 . . ?
C1 C66 H66 119.6 . . ?
C112 C111 C116 120.0 . . ?
C112 C111 C11 121.1(3) . . ?
C116 C111 C11 118.9(3) . . ?
C113 C112 C111 120.0 . . ?
C113 C112 H112 120.0 . . ?
C111 C112 H112 120.0 . . ?
C112 C113 C114 120.0 . . ?
C112 C113 H113 120.0 . . ?
C114 C113 H113 120.0 . . ?
C113 C114 C115 120.0 . . ?
C113 C114 H114 120.0 . . ?
C115 C114 H114 120.0 . . ?
C116 C115 C114 120.0 . . ?
C116 C115 H115 120.0 . . ?
C114 C115 H115 120.0 . . ?
C115 C116 C111 120.0 . . ?
C115 C116 H116 120.0 . . ?
C111 C116 H116 120.0 . . ?
C122 C121 C126 120.0 . . ?
C122 C121 C21 121.0(3) . . ?
C126 C121 C21 119.0(3) . . ?
C123 C122 C121 120.0 . . ?
C123 C122 H122 120.0 . . ?
C121 C122 H122 120.0 . . ?
C122 C123 C124 120.0 . . ?
C122 C123 H123 120.0 . . ?
C124 C123 H123 120.0 . . ?
C125 C124 C123 120.0 . . ?
C125 C124 H124 120.0 . . ?
C123 C124 H124 120.0 . . ?
C124 C125 C126 120.0 . . ?
C124 C125 H125 120.0 . . ?
C126 C125 H125 120.0 . . ?
C125 C126 C121 120.0 . . ?
C125 C126 H126 120.0 . . ?
C121 C126 H126 120.0 . . ?
C132 C131 C136 120.0 . . ?
C132 C131 C31 121.0(3) . . ?
C136 C131 C31 118.9(3) . . ?
C131 C132 C133 120.0 . . ?
C131 C132 H132 120.0 . . ?
C133 C132 H132 120.0 . . ?
C134 C133 C132 120.0 . . ?
C134 C133 H133 120.0 . . ?
C132 C133 H133 120.0 . . ?
C135 C134 C133 120.0 . . ?
C135 C134 H134 120.0 . . ?
C133 C134 H134 120.0 . . ?
C134 C135 C136 120.0 . . ?
C134 C135 H135 120.0 . . ?
C136 C135 H135 120.0 . . ?
C135 C136 C131 120.0 . . ?
C135 C136 H136 120.0 . . ?
C131 C136 H136 120.0 . . ?
C142 C141 C146 120.0 . . ?
C142 C141 C41 120.6(3) . . ?
C146 C141 C41 119.4(3) . . ?
C143 C142 C141 120.0 . . ?
C143 C142 H142 120.0 . . ?
C141 C142 H142 120.0 . . ?
C144 C143 C142 120.0 . . ?
C144 C143 H143 120.0 . . ?
C142 C143 H143 120.0 . . ?
C143 C144 C145 120.0 . . ?
C143 C144 H144 120.0 . . ?
C145 C144 H144 120.0 . . ?
C146 C145 C144 120.0 . . ?
C146 C145 H145 120.0 . . ?
C144 C145 H145 120.0 . . ?
C145 C146 C141 120.0 . . ?
C145 C146 H146 120.0 . . ?
C141 C146 H146 120.0 . . ?
F53 C510 F52 108.3(6) . . ?
F53 C510 F51 105.4(6) . . ?
F52 C510 F51 103.2(6) . . ?
F53 C510 C55 115.1(5) . . ?
F52 C510 C55 112.1(6) . . ?
F51 C510 C55 111.8(6) . . ?
F54 C511 F56 105.5(6) . . ?
F54 C511 F55 105.7(6) . . ?
F56 C511 F55 106.0(6) . . ?
F54 C511 C53 113.1(5) . . ?
F56 C511 C53 113.4(5) . . ?
F55 C511 C53 112.5(5) . . ?
F63 C610 F61 107.4(5) . . ?
F63 C610 F62 105.6(5) . . ?
F61 C610 F62 104.6(5) . . ?
F63 C610 C65 114.7(5) . . ?
F61 C610 C65 111.8(5) . . ?
F62 C610 C65 112.2(5) . . ?
F65 C611 F66 105.8(5) . . ?
F65 C611 F64 105.9(5) . . ?
F66 C611 F64 106.0(5) . . ?
F65 C611 C63 113.1(5) . . ?
F66 C611 C63 113.3(5) . . ?
F64 C611 C63 112.2(5) . . ?
C12 N11 C15 107.9(4) . . ?
C12 N11 Ru1 126.3(3) . . ?
C15 N11 Ru1 125.7(3) . . ?
C22 N21 C25 107.0(4) . . ?
C22 N21 Ru1 125.8(3) . . ?
C25 N21 Ru1 127.1(3) . . ?
C32 N31 C35 107.9(4) . . ?
C32 N31 Ru1 126.2(4) . . ?
C35 N31 Ru1 125.5(4) . . ?
C42 N41 C45 107.7(4) . . ?
C42 N41 Ru1 125.9(4) . . ?
C45 N41 Ru1 126.2(3) . . ?
C2 N2 Ru1 139.8(3) . . ?
C1 N1 Ru1 143.7(4) . . ?
N2 Ru1 N1 167.97(18) . . ?
N2 Ru1 N41 94.98(17) . . ?
N1 Ru1 N41 96.42(17) . . ?
N2 Ru1 N11 92.82(17) . . ?
N1 Ru1 N11 91.00(17) . . ?
N41 Ru1 N11 90.10(16) . . ?
N2 Ru1 N21 84.84(17) . . ?
N1 Ru1 N21 83.71(17) . . ?
N41 Ru1 N21 179.29(18) . . ?
N11 Ru1 N21 90.60(16) . . ?
N2 Ru1 N31 86.91(17) . . ?
N1 Ru1 N31 89.20(17) . . ?
N41 Ru1 N31 90.28(17) . . ?
N11 Ru1 N31 179.55(19) . . ?
N21 Ru1 N31 89.03(16) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        23.27
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.084

#END

data_complex2
_database_code_depnum_ccdc_archive 'CCDC 720710'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H52 F12 N6 Ru1'
_chemical_formula_sum            'C72 H52 F12 N6 Ru1'
_chemical_formula_weight         1330.26

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'
F F 0.0171 0.0103 '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'

_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                   10.550(5)
_cell_length_b                   11.624(5)
_cell_length_c                   13.338(5)
_cell_angle_alpha                77.057(5)
_cell_angle_beta                 76.063(5)
_cell_angle_gamma                75.063(5)
_cell_volume                     1510.9(11)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3113
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      20.1

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             678
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART-ApexII'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14498
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.60
_diffrn_reflns_theta_max         24.91
_reflns_number_total             5232
_reflns_number_gt                4405
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+0.9307P] 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         5232
_refine_ls_number_parameters     422
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1454
_refine_ls_wR_factor_gt          0.1369
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.051
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.1782(4) -0.1946(3) -0.1256(3) 0.0402(9) Uani 1 1 d . . .
C13 C 0.2859(4) -0.2963(4) -0.1175(3) 0.0473(10) Uani 1 1 d . . .
H13 H 0.3275 -0.3439 -0.1687 0.057 Uiso 1 1 calc R . .
C14 C 0.3172(4) -0.3116(4) -0.0229(3) 0.0497(11) Uani 1 1 d . . .
H14 H 0.3848 -0.3712 0.0029 0.060 Uiso 1 1 calc R . .
C15 C -0.2274(4) 0.2191(4) -0.0314(3) 0.0403(9) Uani 1 1 d . . .
C16 C -0.2241(4) 0.2069(4) -0.1333(3) 0.0417(9) Uani 1 1 d . . .
C22 C -0.1403(4) 0.1149(4) -0.1859(3) 0.0429(10) Uani 1 1 d . . .
C23 C -0.1373(5) 0.1017(4) -0.2905(3) 0.0519(11) Uani 1 1 d . . .
H23 H -0.1910 0.1526 -0.3356 0.062 Uiso 1 1 calc R . .
C24 C -0.0450(5) 0.0044(4) -0.3120(3) 0.0525(11) Uani 1 1 d . . .
H24 H -0.0230 -0.0256 -0.3745 0.063 Uiso 1 1 calc R . .
C25 C 0.0152(4) -0.0463(4) -0.2216(3) 0.0425(9) Uani 1 1 d . . .
C26 C 0.1171(4) -0.1485(4) -0.2126(3) 0.0420(9) Uani 1 1 d . . .
C3 C 0.2033(4) 0.1076(4) -0.1632(3) 0.0469(10) Uani 1 1 d . . .
C32 C 0.3271(5) 0.0315(4) -0.1842(4) 0.0543(11) Uani 1 1 d . . .
H32 H 0.3620 -0.0227 -0.1297 0.065 Uiso 1 1 calc R . .
C33 C 0.4001(5) 0.0356(5) -0.2867(4) 0.0599(12) Uani 1 1 d . . .
C34 C 0.3484(5) 0.1137(5) -0.3675(4) 0.0658(14) Uani 1 1 d . . .
H34 H 0.3980 0.1167 -0.4355 0.079 Uiso 1 1 calc R . .
C35 C 0.2236(5) 0.1875(5) -0.3487(4) 0.0625(13) Uani 1 1 d . . .
C36 C 0.1525(5) 0.1848(4) -0.2468(4) 0.0558(12) Uani 1 1 d . . .
H36 H 0.0687 0.2358 -0.2340 0.067 Uiso 1 1 calc R . .
C37 C 0.1685(8) 0.2689(6) -0.4370(5) 0.0891(19) Uani 1 1 d . . .
C38 C 0.5319(6) -0.0448(7) -0.3078(5) 0.0816(17) Uani 1 1 d . . .
C4 C 0.1517(5) 0.1903(4) -0.0043(4) 0.0541(11) Uani 1 1 d . . .
C42 C 0.2927(6) 0.1571(6) 0.0170(5) 0.0785(16) Uani 0.50 1 d PD . .
H42 H 0.3330 0.0754 0.0290 0.094 Uiso 0.50 1 calc PR . .
C43 C 0.3657(12) 0.2387(10) 0.0199(12) 0.087(3) Uani 0.50 1 d PD . .
H43 H 0.4521 0.2122 0.0330 0.104 Uiso 0.50 1 calc PR . .
C44 C 0.3034(9) 0.3698(7) 0.0019(6) 0.115(3) Uani 0.50 1 d PD . .
H44A H 0.3157 0.4064 0.0565 0.138 Uiso 1 1 calc R . .
H44B H 0.3487 0.4077 -0.0647 0.138 Uiso 1 1 calc R . .
C45 C 0.1621(12) 0.3929(13) 0.0013(12) 0.099(4) Uani 0.50 1 d PD . .
H45A H 0.1336 0.4775 -0.0280 0.119 Uiso 0.50 1 calc PR . .
H45B H 0.1146 0.3807 0.0734 0.119 Uiso 0.50 1 calc PR . .
C46 C 0.1201(7) 0.3209(6) -0.0559(5) 0.0871(18) Uani 0.50 1 d PD . .
H46A H 0.1670 0.3303 -0.1284 0.105 Uiso 0.50 1 calc PR . .
H46B H 0.0249 0.3477 -0.0549 0.105 Uiso 0.50 1 calc PR . .
C421 C 0.2927(6) 0.1571(6) 0.0170(5) 0.0785(16) Uani 0.50 1 d PD . .
H42A H 0.3070 0.0803 0.0642 0.094 Uiso 0.50 1 calc PR . .
H42B H 0.3578 0.1509 -0.0478 0.094 Uiso 0.50 1 calc PR . .
C431 C 0.3057(15) 0.2554(10) 0.0657(11) 0.099(4) Uani 0.50 1 d PD . .
H43A H 0.2338 0.2641 0.1263 0.119 Uiso 0.50 1 calc PR . .
H43B H 0.3891 0.2300 0.0911 0.119 Uiso 0.50 1 calc PR . .
C441 C 0.3034(9) 0.3698(7) 0.0019(6) 0.115(3) Uani 0.50 1 d PD . .
C451 C 0.1816(12) 0.4100(11) -0.0505(12) 0.087(3) Uani 0.50 1 d PD . .
H451 H 0.1505 0.4907 -0.0776 0.104 Uiso 0.50 1 calc PR . .
C461 C 0.1201(7) 0.3209(6) -0.0559(5) 0.0871(18) Uani 0.50 1 d PD . .
H461 H 0.0529 0.3436 -0.0950 0.105 Uiso 0.50 1 calc PR . .
C161 C -0.3184(5) 0.2998(4) -0.1930(3) 0.0527(11) Uani 1 1 d . . .
C162 C -0.3017(6) 0.4162(5) -0.2223(4) 0.0729(15) Uani 1 1 d . . .
H162 H -0.2313 0.4372 -0.2050 0.088 Uiso 1 1 calc R . .
C163 C -0.3889(9) 0.5036(6) -0.2778(5) 0.100(2) Uani 1 1 d . . .
H163 H -0.3769 0.5826 -0.2981 0.120 Uiso 1 1 calc R . .
C164 C -0.4920(9) 0.4717(8) -0.3017(5) 0.111(3) Uani 1 1 d . . .
H164 H -0.5515 0.5302 -0.3378 0.134 Uiso 1 1 calc R . .
C165 C -0.5101(6) 0.3559(8) -0.2741(5) 0.098(2) Uani 1 1 d . . .
H165 H -0.5803 0.3353 -0.2920 0.118 Uiso 1 1 calc R . .
C166 C -0.4236(5) 0.2702(6) -0.2196(4) 0.0711(15) Uani 1 1 d . . .
H166 H -0.4358 0.1912 -0.2002 0.085 Uiso 1 1 calc R . .
C261 C 0.1607(5) -0.2188(4) -0.3013(3) 0.0491(11) Uani 1 1 d . . .
C262 C 0.1064(7) -0.3128(6) -0.2972(5) 0.094(2) Uani 1 1 d . . .
H262 H 0.0431 -0.3345 -0.2387 0.113 Uiso 1 1 calc R . .
C263 C 0.1435(8) -0.3786(7) -0.3795(6) 0.115(3) Uani 1 1 d . . .
H263 H 0.1035 -0.4421 -0.3767 0.139 Uiso 1 1 calc R . .
C264 C 0.2376(7) -0.3492(6) -0.4625(5) 0.088(2) Uani 1 1 d . . .
H264 H 0.2636 -0.3928 -0.5174 0.105 Uiso 1 1 calc R . .
C265 C 0.2935(6) -0.2575(6) -0.4662(4) 0.0820(18) Uani 1 1 d . . .
H265 H 0.3593 -0.2380 -0.5235 0.098 Uiso 1 1 calc R . .
C266 C 0.2552(6) -0.1913(5) -0.3863(4) 0.0700(14) Uani 1 1 d . . .
H266 H 0.2946 -0.1270 -0.3907 0.084 Uiso 1 1 calc R . .
N1 N 0.1280(3) 0.1051(3) -0.0596(2) 0.0428(8) Uani 1 1 d . . .
N11 N -0.1451(3) 0.1482(3) 0.0338(2) 0.0377(7) Uani 1 1 d . . .
N21 N -0.0461(3) 0.0231(3) -0.1448(2) 0.0393(8) Uani 1 1 d . . .
F31 F 0.2466(6) 0.3415(5) -0.4907(4) 0.178(3) Uani 1 1 d . . .
F32 F 0.1488(6) 0.2117(4) -0.5036(4) 0.154(2) Uani 1 1 d . . .
F33 F 0.0535(5) 0.3404(4) -0.4094(3) 0.1303(16) Uani 1 1 d . . .
F34 F 0.6087(4) -0.0458(5) -0.2450(4) 0.151(2) Uani 1 1 d . . .
F35 F 0.5296(4) -0.1546(4) -0.3019(6) 0.202(3) Uani 1 1 d . . .
F36 F 0.6048(5) -0.0124(6) -0.3981(4) 0.175(2) Uani 1 1 d . . .
Ru1 Ru 0.0000 0.0000 0.0000 0.03511(17) Uani 1 2 d S . .
H41A H 0.094(4) 0.183(4) 0.066(4) 0.053 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
C12 0.046(2) 0.038(2) 0.034(2) -0.0128(17) -0.0028(17) -0.0047(18)
C13 0.054(3) 0.044(2) 0.041(2) -0.0185(19) -0.0075(19) 0.003(2)
C14 0.050(3) 0.045(2) 0.049(3) -0.014(2) -0.009(2) 0.004(2)
C15 0.043(2) 0.039(2) 0.038(2) -0.0089(18) -0.0078(18) -0.0041(18)
C16 0.045(2) 0.043(2) 0.035(2) -0.0088(18) -0.0093(18) -0.0034(18)
C22 0.045(2) 0.045(2) 0.036(2) -0.0090(18) -0.0103(18) -0.0033(19)
C23 0.062(3) 0.056(3) 0.036(2) -0.011(2) -0.017(2) 0.002(2)
C24 0.064(3) 0.060(3) 0.031(2) -0.019(2) -0.011(2) 0.002(2)
C25 0.052(2) 0.045(2) 0.030(2) -0.0121(18) -0.0055(18) -0.0072(19)
C26 0.049(2) 0.042(2) 0.033(2) -0.0141(18) -0.0024(18) -0.0050(19)
C3 0.051(3) 0.049(3) 0.041(2) -0.012(2) -0.0033(19) -0.014(2)
C32 0.057(3) 0.055(3) 0.049(3) -0.011(2) -0.007(2) -0.009(2)
C33 0.058(3) 0.069(3) 0.053(3) -0.027(3) 0.002(2) -0.012(2)
C34 0.078(4) 0.075(4) 0.043(3) -0.015(3) 0.007(3) -0.027(3)
C35 0.080(4) 0.066(3) 0.040(3) -0.008(2) -0.004(2) -0.021(3)
C36 0.061(3) 0.053(3) 0.049(3) -0.004(2) -0.009(2) -0.011(2)
C37 0.110(5) 0.090(5) 0.047(3) -0.003(3) -0.005(3) -0.005(4)
C38 0.069(4) 0.106(5) 0.063(4) -0.031(3) 0.002(3) -0.008(3)
C4 0.059(3) 0.057(3) 0.047(3) -0.013(2) -0.003(2) -0.017(2)
C42 0.090(4) 0.079(4) 0.077(4) -0.018(3) -0.027(3) -0.024(3)
C43 0.067(6) 0.083(7) 0.102(8) 0.014(6) -0.008(6) -0.036(5)
C44 0.167(8) 0.100(6) 0.109(6) -0.031(4) -0.018(5) -0.078(6)
C45 0.077(6) 0.087(7) 0.121(10) 0.000(6) 0.011(6) -0.041(5)
C46 0.103(5) 0.077(4) 0.086(4) -0.025(3) -0.021(4) -0.015(4)
C421 0.090(4) 0.079(4) 0.077(4) -0.018(3) -0.027(3) -0.024(3)
C431 0.077(6) 0.087(7) 0.121(10) 0.000(6) 0.011(6) -0.041(5)
C441 0.167(8) 0.100(6) 0.109(6) -0.031(4) -0.018(5) -0.078(6)
C451 0.067(6) 0.083(7) 0.102(8) 0.014(6) -0.008(6) -0.036(5)
C461 0.103(5) 0.077(4) 0.086(4) -0.025(3) -0.021(4) -0.015(4)
C161 0.058(3) 0.054(3) 0.036(2) -0.014(2) -0.011(2) 0.012(2)
C162 0.092(4) 0.058(3) 0.057(3) -0.008(3) -0.018(3) 0.005(3)
C163 0.141(6) 0.068(4) 0.057(4) -0.005(3) -0.016(4) 0.026(4)
C164 0.121(6) 0.121(6) 0.055(4) -0.022(4) -0.034(4) 0.060(5)
C165 0.069(4) 0.147(7) 0.067(4) -0.041(4) -0.031(3) 0.033(4)
C166 0.055(3) 0.094(4) 0.058(3) -0.024(3) -0.018(2) 0.010(3)
C261 0.062(3) 0.048(3) 0.036(2) -0.0146(19) -0.014(2) 0.001(2)
C262 0.116(5) 0.096(5) 0.079(4) -0.051(4) 0.016(4) -0.040(4)
C263 0.147(7) 0.111(6) 0.114(6) -0.077(5) -0.003(5) -0.043(5)
C264 0.112(5) 0.091(5) 0.058(4) -0.046(3) -0.028(4) 0.021(4)
C265 0.096(4) 0.096(5) 0.042(3) -0.022(3) -0.004(3) -0.001(4)
C266 0.086(4) 0.078(4) 0.044(3) -0.024(3) 0.002(3) -0.016(3)
N1 0.047(2) 0.048(2) 0.0328(18) -0.0129(15) -0.0026(15) -0.0080(16)
N11 0.0425(18) 0.0387(18) 0.0310(17) -0.0107(14) -0.0081(14) -0.0025(15)
N21 0.0471(19) 0.0394(18) 0.0307(17) -0.0086(14) -0.0083(15) -0.0054(15)
F31 0.195(5) 0.174(5) 0.129(4) 0.079(4) -0.021(4) -0.076(4)
F32 0.232(6) 0.137(4) 0.094(3) -0.034(3) -0.090(4) 0.023(4)
F33 0.154(4) 0.120(3) 0.077(3) 0.006(2) -0.033(3) 0.028(3)
F34 0.087(3) 0.200(5) 0.164(5) -0.083(4) -0.041(3) 0.030(3)
F35 0.085(3) 0.092(3) 0.420(11) -0.111(5) 0.007(4) 0.000(2)
F36 0.106(3) 0.215(6) 0.118(4) -0.004(4) 0.047(3) 0.031(3)
Ru1 0.0414(3) 0.0360(3) 0.0267(3) -0.00923(18) -0.00657(18) -0.00281(19)

_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
C12 N11 1.380(5) 2 ?
C12 C26 1.398(6) . ?
C12 C13 1.417(5) . ?
C13 C14 1.343(6) . ?
C14 C15 1.439(6) 2 ?
C15 N11 1.365(5) . ?
C15 C16 1.390(5) . ?
C15 C14 1.439(6) 2 ?
C16 C22 1.402(6) . ?
C16 C161 1.494(6) . ?
C22 N21 1.371(5) . ?
C22 C23 1.430(6) . ?
C23 C24 1.324(6) . ?
C24 C25 1.437(6) . ?
C25 N21 1.379(5) . ?
C25 C26 1.386(6) . ?
C26 C261 1.501(6) . ?
C3 C32 1.380(6) . ?
C3 C36 1.388(6) . ?
C3 N1 1.417(5) . ?
C32 C33 1.396(6) . ?
C33 C34 1.368(7) . ?
C33 C38 1.465(7) . ?
C34 C35 1.374(7) . ?
C35 C36 1.382(6) . ?
C35 C37 1.472(8) . ?
C37 F32 1.304(8) . ?
C37 F33 1.304(7) . ?
C37 F31 1.307(8) . ?
C38 F35 1.267(8) . ?
C38 F34 1.295(7) . ?
C38 F36 1.298(7) . ?
C4 N1 1.459(6) . ?
C4 C46 1.508(8) . ?
C4 C42 1.517(7) . ?
C42 C43 1.379(12) . ?
C43 C44 1.485(13) . ?
C44 C45 1.447(13) . ?
C45 C46 1.455(13) . ?
C161 C162 1.367(7) . ?
C161 C166 1.385(7) . ?
C162 C163 1.391(8) . ?
C163 C164 1.361(11) . ?
C164 C165 1.364(11) . ?
C165 C166 1.371(8) . ?
C261 C262 1.344(7) . ?
C261 C266 1.357(7) . ?
C262 C263 1.400(8) . ?
C263 C264 1.344(10) . ?
C264 C265 1.332(9) . ?
C265 C266 1.374(7) . ?
N1 Ru1 1.962(3) . ?
N11 C12 1.380(5) 2 ?
N11 Ru1 2.042(3) . ?
N21 Ru1 2.046(3) . ?
Ru1 N1 1.962(3) 2 ?
Ru1 N11 2.042(3) 2 ?
Ru1 N21 2.046(3) 2 ?

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
N11 C12 C26 125.9(4) 2 . ?
N11 C12 C13 108.6(3) 2 . ?
C26 C12 C13 125.6(4) . . ?
C14 C13 C12 107.9(4) . . ?
C13 C14 C15 107.8(4) . 2 ?
N11 C15 C16 126.5(4) . . ?
N11 C15 C14 108.0(3) . 2 ?
C16 C15 C14 125.5(4) . 2 ?
C15 C16 C22 126.0(4) . . ?
C15 C16 C161 117.4(4) . . ?
C22 C16 C161 116.6(4) . . ?
N21 C22 C16 125.0(4) . . ?
N21 C22 C23 108.8(4) . . ?
C16 C22 C23 126.1(4) . . ?
C24 C23 C22 108.2(4) . . ?
C23 C24 C25 107.7(4) . . ?
N21 C25 C26 125.7(4) . . ?
N21 C25 C24 108.6(3) . . ?
C26 C25 C24 125.7(4) . . ?
C25 C26 C12 125.2(4) . . ?
C25 C26 C261 117.4(4) . . ?
C12 C26 C261 117.3(4) . . ?
C32 C3 C36 118.3(4) . . ?
C32 C3 N1 121.1(4) . . ?
C36 C3 N1 120.6(4) . . ?
C3 C32 C33 120.3(4) . . ?
C34 C33 C32 120.2(5) . . ?
C34 C33 C38 120.0(5) . . ?
C32 C33 C38 119.8(5) . . ?
C33 C34 C35 120.4(5) . . ?
C34 C35 C36 119.3(5) . . ?
C34 C35 C37 119.5(5) . . ?
C36 C35 C37 121.2(5) . . ?
C35 C36 C3 121.5(5) . . ?
F32 C37 F33 105.0(6) . . ?
F32 C37 F31 106.5(6) . . ?
F33 C37 F31 104.6(6) . . ?
F32 C37 C35 113.3(6) . . ?
F33 C37 C35 114.3(5) . . ?
F31 C37 C35 112.3(6) . . ?
F35 C38 F34 105.4(7) . . ?
F35 C38 F36 106.9(6) . . ?
F34 C38 F36 101.0(6) . . ?
F35 C38 C33 114.7(6) . . ?
F34 C38 C33 113.4(5) . . ?
F36 C38 C33 114.2(6) . . ?
N1 C4 C46 114.8(4) . . ?
N1 C4 C42 112.2(4) . . ?
C46 C4 C42 109.8(5) . . ?
C43 C42 C4 125.1(7) . . ?
C42 C43 C44 118.7(9) . . ?
C45 C44 C43 112.7(8) . . ?
C44 C45 C46 117.2(10) . . ?
C45 C46 C4 108.5(8) . . ?
C162 C161 C166 118.9(5) . . ?
C162 C161 C16 120.1(5) . . ?
C166 C161 C16 121.1(5) . . ?
C161 C162 C163 120.6(6) . . ?
C164 C163 C162 119.0(7) . . ?
C163 C164 C165 121.4(6) . . ?
C164 C165 C166 119.2(7) . . ?
C165 C166 C161 120.8(6) . . ?
C262 C261 C266 118.1(5) . . ?
C262 C261 C26 119.9(4) . . ?
C266 C261 C26 122.1(4) . . ?
C261 C262 C263 121.1(6) . . ?
C264 C263 C262 119.3(7) . . ?
C265 C264 C263 119.9(5) . . ?
C264 C265 C266 120.8(6) . . ?
C261 C266 C265 120.8(6) . . ?
C3 N1 C4 113.7(3) . . ?
C3 N1 Ru1 122.2(3) . . ?
C4 N1 Ru1 124.0(3) . . ?
C15 N11 C12 107.7(3) . 2 ?
C15 N11 Ru1 125.5(3) . . ?
C12 N11 Ru1 126.7(3) 2 . ?
C22 N21 C25 106.7(3) . . ?
C22 N21 Ru1 126.2(3) . . ?
C25 N21 Ru1 127.0(3) . . ?
N1 Ru1 N1 180.00(18) . 2 ?
N1 Ru1 N11 89.24(14) . . ?
N1 Ru1 N11 90.76(14) 2 . ?
N1 Ru1 N11 90.76(14) . 2 ?
N1 Ru1 N11 89.24(14) 2 2 ?
N11 Ru1 N11 180.0(3) . 2 ?
N1 Ru1 N21 90.52(13) . 2 ?
N1 Ru1 N21 89.48(13) 2 2 ?
N11 Ru1 N21 89.39(12) . 2 ?
N11 Ru1 N21 90.61(12) 2 2 ?
N1 Ru1 N21 89.48(13) . . ?
N1 Ru1 N21 90.52(13) 2 . ?
N11 Ru1 N21 90.61(12) . . ?
N11 Ru1 N21 89.39(12) 2 . ?
N21 Ru1 N21 180.00(4) 2 . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.91
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.073
#END