# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef '- Rubim_Cl.cif'

#===================================================================
_audit_creation_date             2010/07/15
_audit_creation_method           
'from SHELXL97 and KenX, based on form.cif supplied from IUCr'

_audit_update_record             
;
2012-03-01 Manually Edited
;
#===================================================================
# 1. SUBMISSION DETAILS

_publ_contact_author_name        'Shigeyuki Masaoka'
_publ_contact_author_address     
;

Institute for Molecular Science
National Institutes of Natural Sciences
5-1 Higashiyama, Myodaiji, Okazaki 444-8787, JAPAN
;
_publ_contact_author_phone       '+81 (0)564 59 5587'
_publ_contact_author_fax         '+81 (0)564 59 5589'
_publ_contact_author_email       masaoka@ims.ac.jp
_publ_requested_category         FA
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
NONE

;

#=====================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic    ?
_journal_date_to_coeditor        ?
_journal_date_from_coeditor      ?
_journal_date_accepted           ?
_journal_date_printers_first     ?
_journal_date_printers_final     ?
_journal_date_proofs_out         ?
_journal_date_proofs_in          ?
_journal_coeditor_name           ?
_journal_coeditor_code           ?
_journal_coeditor_notes          
;
;
_journal_techeditor_code         ?
_journal_techeditor_notes        
;
;
_journal_coden_ASTM              ACSCEE
_journal_year                    ?
_journal_volume                  ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?
_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?

#=====================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
NONE
;

loop_
_publ_author_name
_publ_author_address
'Masaya Okamura'
;
Institute for Molecular Science
National Institutes of Natural Sciences
5-1 Higashiyama, Myodaiji, Okazaki 444-8787, JAPAN
;
'Masaki Yoshida'
;
Institute for Molecular Science
National Institutes of Natural Sciences
5-1 Higashiyama, Myodaiji, Okazaki 444-8787, JAPAN

;
'Reiko Kuga' ''
'Ken Sakai' ''
'Mio Kondo' ''
S.Masaoka ''

#======================================================================
# 4. TEXT

_publ_section_abstract           
;
???????????????????????????
???????????????????????????
???????????????????????????
???????????????????????????
;

_publ_section_comment            
;
NONE
;

_publ_section_exptl_prep         
;
NONE
;

_publ_section_exptl_refinement   
;
NONE
;

_publ_section_references         
;
Bruker (2006). APEX2. Bruker AXS Inc., Madison, Wisconsin, USA.
Bruker (2004). SAINT. Bruker AXS Inc., Madison, Wisconsin, USA.

Johnson, C.K., (1976) ORTEP - A Fortran Thermal Ellipsoid Plot
Program, Technical Report ORNL-5138, Oak Ridge National Lab., U.S.A.

Sakai, K. (2004). KENX. GUI for SHELXL97. Kyushu University, Japan.

Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.

Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of G\"ottingen,
Germany.
;

_publ_section_figure_captions    
;
NONE
;

_publ_section_acknowledgements   
;
NONE
;

#=====================================================================

data_Rubim_Cl
_database_code_depnum_ccdc_archive 'CCDC 875208'
#TrackingRef '- Rubim_Cl.cif'

#=====================================================================

# 5. Chemical Data
_chemical_name_systematic        
;
Rubim_Cl
;

_chemical_name_common            Rubim_Cl
_chemical_formula_iupac          'C21 H17 Cl F6 N7 P Ru'
_chemical_formula_moiety         'C21 H17 Cl N7 Ru, F6 P'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C21 H17 Cl F6 N7 P Ru'
_chemical_formula_weight         648.91
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
P P 0.1023 0.0942 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==========================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'P 41'
_symmetry_space_group_name_Hall  'P 4w'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, -y, z+1/2'

_cell_length_a                   8.6074(19)
_cell_length_b                   8.6074(19)
_cell_length_c                   32.612(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2416.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9949
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.97
_cell_measurement_wavelength     0.71075

_cell_special_details            
;
? # Insert any comments here.
;

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1288
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, G. M., 1996)'
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_T_max  0.956

#==========================================================================
# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
The first 50 frames were rescanned at the end of data collection to
evaluate any possible decay phenomenon. Since it was judged to be
negligible, no decay correction was applied to the data.
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'Bruker SMART APEX CCD-detector diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.333
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19765
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         2.37
_diffrn_reflns_theta_max         26.02
_reflns_number_total             4769
_reflns_number_gt                4490
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics    'KENX (Sakai, 2002)'
_computing_publication_material  
;
SHELXL97, TEXSAN (Molecular Structure Corporation, 2001),
KENX, and ORTEP (Johnson, 1976)
;

#=========================================================================

# 8. Refinement Data

_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^)+(0.0000P)^2^+2.4661P] 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         4769
_refine_ls_number_parameters     334
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_abs_structure_details 'Flack (1983), 6881 Friedel pairs'
_refine_ls_abs_structure_Flack   0.05(3)
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.066

#=========================================================================
# 9. Atomic Coordinates and Displacement Parameters

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
Ru1 Ru 0.03973(3) -0.01688(4) 0.876208(10) 0.02142(8) Uani 1 1 d . . .
Cl1 Cl -0.12777(13) 0.07646(13) 0.82211(3) 0.0279(2) Uani 1 1 d . . .
P1 P 0.52619(15) 0.34516(18) 0.72650(4) 0.0446(3) Uani 1 1 d . . .
F1 F 0.5758(4) 0.1673(4) 0.72444(10) 0.0609(9) Uani 1 1 d . . .
F2 F 0.3817(4) 0.3004(5) 0.75503(10) 0.0777(12) Uani 1 1 d . . .
F3 F 0.4791(5) 0.5212(4) 0.72856(11) 0.0809(12) Uani 1 1 d . . .
F4 F 0.6716(3) 0.3900(3) 0.69779(8) 0.0441(7) Uani 1 1 d . . .
F5 F 0.6342(4) 0.3665(4) 0.76618(9) 0.0611(9) Uani 1 1 d . . .
F6 F 0.4231(4) 0.3192(5) 0.68614(10) 0.0749(11) Uani 1 1 d . . .
N4 N 0.1496(4) -0.0952(4) 0.92871(9) 0.0239(7) Uani 1 1 d . . .
N7 N 0.1432(4) -0.1392(4) 0.99493(10) 0.0289(8) Uani 1 1 d . . .
H15 H 0.1092 -0.1461 1.0203 0.035 Uiso 1 1 calc R . .
N6 N -0.2121(4) -0.0150(5) 0.98425(10) 0.0353(9) Uani 1 1 d . . .
H14 H -0.2097 -0.0351 1.0107 0.042 Uiso 1 1 calc R . .
N5 N -0.1371(5) 0.0102(4) 0.92018(10) 0.0289(8) Uani 1 1 d . . .
N2 N 0.2147(4) -0.0511(5) 0.84002(10) 0.0285(8) Uani 1 1 d . . .
N1 N 0.1519(4) 0.1923(4) 0.88302(10) 0.0321(8) Uani 1 1 d . . .
N3 N -0.0093(4) -0.2385(4) 0.85708(10) 0.0327(8) Uani 1 1 d . . .
C19 C 0.0608(5) -0.0890(5) 0.96245(11) 0.0263(9) Uani 1 1 d . . .
C20 C 0.2891(5) -0.1777(5) 0.98164(13) 0.0320(10) Uani 1 1 d . . .
H16 H 0.3722 -0.2165 0.9979 0.038 Uiso 1 1 calc R . .
C21 C 0.2914(5) -0.1493(5) 0.94044(12) 0.0294(9) Uani 1 1 d . . .
H17 H 0.3780 -0.1648 0.9228 0.035 Uiso 1 1 calc R . .
C18 C -0.0935(5) -0.0333(5) 0.95755(12) 0.0280(9) Uani 1 1 d . . .
C17 C -0.3371(5) 0.0406(6) 0.96271(12) 0.0370(11) Uani 1 1 d . . .
H13 H -0.4374 0.0633 0.9733 0.044 Uiso 1 1 calc R . .
C16 C -0.2888(5) 0.0568(5) 0.92314(13) 0.0327(10) Uani 1 1 d . . .
H12 H -0.3506 0.0943 0.9011 0.039 Uiso 1 1 calc R . .
C10 C 0.2258(6) -0.1886(6) 0.82043(13) 0.0409(12) Uani 1 1 d . . .
C9 C 0.3547(8) -0.2151(8) 0.79476(16) 0.0652(19) Uani 1 1 d . . .
H7 H 0.3663 -0.3099 0.7802 0.078 Uiso 1 1 calc R . .
C8 C 0.4643(8) -0.0968(11) 0.79167(19) 0.079(2) Uani 1 1 d . . .
H6 H 0.5525 -0.1128 0.7747 0.095 Uiso 1 1 calc R . .
C7 C 0.4509(6) 0.0403(8) 0.81186(17) 0.0599(17) Uani 1 1 d . . .
H5 H 0.5278 0.1188 0.8090 0.072 Uiso 1 1 calc R . .
C6 C 0.3231(5) 0.0629(6) 0.83657(13) 0.0380(12) Uani 1 1 d . . .
C5 C 0.2869(6) 0.2016(6) 0.86107(14) 0.0410(12) Uani 1 1 d . . .
C1 C 0.1124(7) 0.3131(6) 0.90798(14) 0.0445(13) Uani 1 1 d . . .
H1 H 0.0185 0.3061 0.9232 0.053 Uiso 1 1 calc R . .
C2 C 0.2006(9) 0.4428(7) 0.91221(18) 0.0627(18) Uani 1 1 d . . .
H2 H 0.1696 0.5251 0.9298 0.075 Uiso 1 1 calc R . .
C3 C 0.3357(9) 0.4511(7) 0.8902(2) 0.071(2) Uani 1 1 d . . .
H3 H 0.4001 0.5401 0.8930 0.085 Uiso 1 1 calc R . .
C4 C 0.3808(7) 0.3334(7) 0.86404(18) 0.0610(18) Uani 1 1 d . . .
H4 H 0.4736 0.3418 0.8484 0.073 Uiso 1 1 calc R . .
C11 C 0.0966(6) -0.2947(5) 0.82960(13) 0.0407(12) Uani 1 1 d . . .
C15 C -0.1297(6) -0.3291(6) 0.86736(15) 0.0469(13) Uani 1 1 d . . .
H11 H -0.2044 -0.2911 0.8863 0.056 Uiso 1 1 calc R . .
C14 C -0.1485(9) -0.4769(7) 0.85115(19) 0.075(2) Uani 1 1 d . . .
H10 H -0.2336 -0.5402 0.8592 0.090 Uiso 1 1 calc R . .
C13 C -0.0419(12) -0.5295(7) 0.8234(2) 0.086(3) Uani 1 1 d . . .
H9 H -0.0544 -0.6295 0.8115 0.103 Uiso 1 1 calc R . .
C12 C 0.0816(9) -0.4404(6) 0.81257(16) 0.0640(19) Uani 1 1 d . . .
H8 H 0.1565 -0.4779 0.7936 0.077 Uiso 1 1 calc R . .

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
Ru1 0.02837(19) 0.0251(2) 0.01080(11) -0.00132(12) 0.00218(17) -0.00588(17)
Cl1 0.0387(6) 0.0327(6) 0.0125(4) 0.0003(4) -0.0005(4) -0.0059(5)
P1 0.0353(7) 0.0679(9) 0.0307(7) 0.0176(6) 0.0047(5) 0.0089(6)
F1 0.063(2) 0.057(2) 0.063(2) 0.0180(16) 0.0137(17) -0.0049(16)
F2 0.040(2) 0.140(3) 0.052(2) 0.040(2) 0.0172(14) 0.017(2)
F3 0.104(3) 0.087(3) 0.051(2) 0.0238(19) 0.024(2) 0.055(2)
F4 0.0417(16) 0.0494(17) 0.0413(16) 0.0070(13) 0.0099(12) -0.0033(13)
F5 0.063(2) 0.086(2) 0.0345(16) 0.0105(15) -0.0091(15) 0.0011(19)
F6 0.0418(18) 0.138(3) 0.0448(18) 0.024(2) -0.0041(14) -0.0034(19)
N4 0.0295(19) 0.0279(19) 0.0144(16) -0.0015(14) 0.0036(13) -0.0052(15)
N7 0.0326(19) 0.041(2) 0.0130(16) 0.0030(14) 0.0015(14) -0.0009(17)
N6 0.040(2) 0.053(2) 0.0135(16) 0.0033(16) 0.0053(15) 0.0137(18)
N5 0.038(2) 0.036(2) 0.0122(15) 0.0017(14) 0.0043(14) 0.0053(17)
N2 0.028(2) 0.046(2) 0.0119(16) 0.0058(15) 0.0029(14) 0.0031(17)
N1 0.045(2) 0.031(2) 0.0206(19) 0.0063(14) -0.0098(15) -0.0097(16)
N3 0.043(2) 0.034(2) 0.0203(17) 0.0003(15) -0.0111(16) -0.0039(17)
C19 0.034(2) 0.030(2) 0.0148(18) 0.0001(15) 0.0007(16) -0.0008(18)
C20 0.030(2) 0.042(3) 0.024(2) -0.0018(18) -0.0035(18) -0.0012(19)
C21 0.027(2) 0.039(2) 0.023(2) -0.0046(18) 0.0027(17) -0.0015(19)
C18 0.032(2) 0.035(2) 0.017(2) 0.0006(17) 0.0039(16) 0.0037(19)
C17 0.037(3) 0.056(3) 0.018(2) 0.0019(19) 0.0050(18) 0.015(2)
C16 0.036(3) 0.041(3) 0.021(2) 0.0044(18) -0.0004(17) 0.009(2)
C10 0.047(3) 0.057(3) 0.018(2) -0.002(2) -0.001(2) 0.024(3)
C9 0.078(5) 0.089(5) 0.028(3) -0.006(3) 0.005(3) 0.047(4)
C8 0.047(4) 0.143(7) 0.047(4) 0.027(4) 0.021(3) 0.040(5)
C7 0.030(3) 0.103(5) 0.046(3) 0.031(3) 0.009(2) 0.010(3)
C6 0.028(2) 0.066(3) 0.020(2) 0.020(2) -0.0006(17) -0.004(2)
C5 0.038(3) 0.049(3) 0.036(2) 0.017(2) -0.016(2) -0.015(2)
C1 0.073(4) 0.036(3) 0.025(2) -0.003(2) -0.018(2) -0.006(3)
C2 0.105(5) 0.045(3) 0.037(3) 0.002(2) -0.033(3) -0.017(3)
C3 0.105(6) 0.044(3) 0.064(4) 0.011(3) -0.051(4) -0.036(4)
C4 0.049(3) 0.075(4) 0.059(4) 0.034(3) -0.025(3) -0.026(3)
C11 0.066(3) 0.033(3) 0.023(2) -0.0047(19) -0.015(2) 0.012(2)
C15 0.060(3) 0.040(3) 0.041(3) 0.009(2) -0.022(2) -0.024(2)
C14 0.129(6) 0.050(4) 0.046(4) 0.020(3) -0.047(4) -0.050(4)
C13 0.189(9) 0.026(3) 0.043(4) -0.002(3) -0.051(5) -0.014(4)
C12 0.124(6) 0.038(3) 0.030(3) -0.011(2) -0.032(3) 0.022(4)

#=========================================================================
# 10. Molecular Geometry

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru1 N2 1.936(3) . ?
Ru1 N3 2.051(4) . ?
Ru1 N1 2.055(4) . ?
Ru1 N4 2.069(3) . ?
Ru1 N5 2.104(4) . ?
Ru1 Cl1 2.4158(11) . ?
P1 F3 1.570(4) . ?
P1 F1 1.591(4) . ?
P1 F2 1.600(3) . ?
P1 F6 1.603(3) . ?
P1 F5 1.604(3) . ?
P1 F4 1.610(3) . ?
N4 C19 1.341(5) . ?
N4 C21 1.362(5) . ?
N7 C19 1.346(5) . ?
N7 C20 1.369(6) . ?
N7 H15 0.8800 . ?
N6 C18 1.351(5) . ?
N6 C17 1.371(6) . ?
N6 H14 0.8800 . ?
N5 C18 1.329(5) . ?
N5 C16 1.370(6) . ?
N2 C10 1.348(6) . ?
N2 C6 1.358(6) . ?
N1 C1 1.364(6) . ?
N1 C5 1.367(6) . ?
N3 C15 1.339(6) . ?
N3 C11 1.367(6) . ?
C19 C18 1.421(6) . ?
C20 C21 1.366(6) . ?
C20 H16 0.9500 . ?
C21 H17 0.9500 . ?
C17 C16 1.363(6) . ?
C17 H13 0.9500 . ?
C16 H12 0.9500 . ?
C10 C9 1.408(7) . ?
C10 C11 1.470(7) . ?
C9 C8 1.392(10) . ?
C9 H7 0.9500 . ?
C8 C7 1.356(10) . ?
C8 H6 0.9500 . ?
C7 C6 1.378(7) . ?
C7 H5 0.9500 . ?
C6 C5 1.470(7) . ?
C5 C4 1.396(7) . ?
C1 C2 1.357(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.369(10) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(9) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C11 C12 1.378(7) . ?
C15 C14 1.387(8) . ?
C15 H11 0.9500 . ?
C14 C13 1.367(11) . ?
C14 H10 0.9500 . ?
C13 C12 1.358(10) . ?
C13 H9 0.9500 . ?
C12 H8 0.9500 . ?

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
N2 Ru1 N3 80.41(16) . . ?
N2 Ru1 N1 80.42(16) . . ?
N3 Ru1 N1 160.83(15) . . ?
N2 Ru1 N4 95.69(14) . . ?
N3 Ru1 N4 92.47(14) . . ?
N1 Ru1 N4 88.92(14) . . ?
N2 Ru1 N5 174.30(14) . . ?
N3 Ru1 N5 99.29(15) . . ?
N1 Ru1 N5 99.73(15) . . ?
N4 Ru1 N5 78.62(14) . . ?
N2 Ru1 Cl1 94.00(10) . . ?
N3 Ru1 Cl1 87.95(10) . . ?
N1 Ru1 Cl1 93.89(10) . . ?
N4 Ru1 Cl1 170.23(10) . . ?
N5 Ru1 Cl1 91.68(10) . . ?
F3 P1 F1 179.4(2) . . ?
F3 P1 F2 90.4(2) . . ?
F1 P1 F2 90.08(19) . . ?
F3 P1 F6 91.5(2) . . ?
F1 P1 F6 88.8(2) . . ?
F2 P1 F6 90.8(2) . . ?
F3 P1 F5 90.3(2) . . ?
F1 P1 F5 89.35(19) . . ?
F2 P1 F5 90.51(19) . . ?
F6 P1 F5 177.8(2) . . ?
F3 P1 F4 89.66(18) . . ?
F1 P1 F4 89.84(16) . . ?
F2 P1 F4 179.9(2) . . ?
F6 P1 F4 89.21(17) . . ?
F5 P1 F4 89.49(17) . . ?
C19 N4 C21 107.1(3) . . ?
C19 N4 Ru1 113.9(3) . . ?
C21 N4 Ru1 138.9(3) . . ?
C19 N7 C20 108.2(3) . . ?
C19 N7 H15 125.9 . . ?
C20 N7 H15 125.9 . . ?
C18 N6 C17 107.7(3) . . ?
C18 N6 H14 126.2 . . ?
C17 N6 H14 126.2 . . ?
C18 N5 C16 106.7(3) . . ?
C18 N5 Ru1 112.9(3) . . ?
C16 N5 Ru1 140.4(3) . . ?
C10 N2 C6 123.1(4) . . ?
C10 N2 Ru1 118.5(3) . . ?
C6 N2 Ru1 118.3(3) . . ?
C1 N1 C5 118.7(4) . . ?
C1 N1 Ru1 128.0(3) . . ?
C5 N1 Ru1 113.2(3) . . ?
C15 N3 C11 118.3(4) . . ?
C15 N3 Ru1 128.7(3) . . ?
C11 N3 Ru1 113.0(3) . . ?
N4 C19 N7 109.4(4) . . ?
N4 C19 C18 117.0(4) . . ?
N7 C19 C18 133.6(4) . . ?
C21 C20 N7 106.3(4) . . ?
C21 C20 H16 126.8 . . ?
N7 C20 H16 126.8 . . ?
N4 C21 C20 108.9(4) . . ?
N4 C21 H17 125.5 . . ?
C20 C21 H17 125.5 . . ?
N5 C18 N6 110.2(4) . . ?
N5 C18 C19 117.5(4) . . ?
N6 C18 C19 132.3(4) . . ?
C16 C17 N6 106.4(4) . . ?
C16 C17 H13 126.8 . . ?
N6 C17 H13 126.8 . . ?
C17 C16 N5 109.1(4) . . ?
C17 C16 H12 125.4 . . ?
N5 C16 H12 125.4 . . ?
N2 C10 C9 118.7(5) . . ?
N2 C10 C11 113.3(4) . . ?
C9 C10 C11 128.0(5) . . ?
C8 C9 C10 117.3(6) . . ?
C8 C9 H7 121.4 . . ?
C10 C9 H7 121.4 . . ?
C7 C8 C9 122.9(6) . . ?
C7 C8 H6 118.5 . . ?
C9 C8 H6 118.5 . . ?
C8 C7 C6 118.3(6) . . ?
C8 C7 H5 120.8 . . ?
C6 C7 H5 120.8 . . ?
N2 C6 C7 119.7(5) . . ?
N2 C6 C5 113.3(4) . . ?
C7 C6 C5 127.0(5) . . ?
N1 C5 C4 120.2(5) . . ?
N1 C5 C6 114.7(4) . . ?
C4 C5 C6 125.1(5) . . ?
C2 C1 N1 123.3(6) . . ?
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
C1 C2 C3 117.7(6) . . ?
C1 C2 H2 121.2 . . ?
C3 C2 H2 121.2 . . ?
C2 C3 C4 121.7(5) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 118.5(6) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N3 C11 C12 121.6(6) . . ?
N3 C11 C10 114.7(4) . . ?
C12 C11 C10 123.7(5) . . ?
N3 C15 C14 121.9(6) . . ?
N3 C15 H11 119.0 . . ?
C14 C15 H11 119.0 . . ?
C13 C14 C15 118.6(6) . . ?
C13 C14 H10 120.7 . . ?
C15 C14 H10 120.7 . . ?
C12 C13 C14 120.7(6) . . ?
C12 C13 H9 119.6 . . ?
C14 C13 H9 119.6 . . ?
C13 C12 C11 118.9(6) . . ?
C13 C12 H8 120.6 . . ?
C11 C12 H8 120.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 N4 C19 N7 -0.5(5) . . . . ?
Ru1 N4 C19 N7 -178.8(3) . . . . ?
C21 N4 C19 C18 179.2(4) . . . . ?
Ru1 N4 C19 C18 0.9(5) . . . . ?
C20 N7 C19 N4 0.4(5) . . . . ?
C20 N7 C19 C18 -179.3(5) . . . . ?
C19 N7 C20 C21 0.0(5) . . . . ?
C19 N4 C21 C20 0.5(5) . . . . ?
Ru1 N4 C21 C20 178.1(3) . . . . ?
N7 C20 C21 N4 -0.3(5) . . . . ?
C16 N5 C18 N6 -0.4(5) . . . . ?
Ru1 N5 C18 N6 -179.3(3) . . . . ?
C16 N5 C18 C19 179.2(4) . . . . ?
Ru1 N5 C18 C19 0.4(5) . . . . ?
C17 N6 C18 N5 0.9(5) . . . . ?
C17 N6 C18 C19 -178.7(5) . . . . ?
N4 C19 C18 N5 -0.9(6) . . . . ?
N7 C19 C18 N5 178.8(4) . . . . ?
N4 C19 C18 N6 178.7(5) . . . . ?
N7 C19 C18 N6 -1.7(9) . . . . ?
C18 N6 C17 C16 -0.9(5) . . . . ?
N6 C17 C16 N5 0.7(6) . . . . ?
C18 N5 C16 C17 -0.2(5) . . . . ?
Ru1 N5 C16 C17 178.2(4) . . . . ?
C6 N2 C10 C9 -0.8(6) . . . . ?
Ru1 N2 C10 C9 -178.7(3) . . . . ?
C6 N2 C10 C11 178.7(4) . . . . ?
Ru1 N2 C10 C11 0.8(5) . . . . ?
N2 C10 C9 C8 0.7(7) . . . . ?
C11 C10 C9 C8 -178.6(5) . . . . ?
C10 C9 C8 C7 -0.5(9) . . . . ?
C9 C8 C7 C6 0.1(9) . . . . ?
C10 N2 C6 C7 0.4(6) . . . . ?
Ru1 N2 C6 C7 178.4(3) . . . . ?
C10 N2 C6 C5 -179.4(4) . . . . ?
Ru1 N2 C6 C5 -1.5(5) . . . . ?
C8 C7 C6 N2 -0.1(7) . . . . ?
C8 C7 C6 C5 179.7(5) . . . . ?
C1 N1 C5 C4 -0.7(6) . . . . ?
Ru1 N1 C5 C4 -176.8(3) . . . . ?
C1 N1 C5 C6 177.3(4) . . . . ?
Ru1 N1 C5 C6 1.2(4) . . . . ?
N2 C6 C5 N1 0.1(5) . . . . ?
C7 C6 C5 N1 -179.7(4) . . . . ?
N2 C6 C5 C4 178.0(4) . . . . ?
C7 C6 C5 C4 -1.9(7) . . . . ?
C5 N1 C1 C2 0.0(7) . . . . ?
Ru1 N1 C1 C2 175.5(4) . . . . ?
N1 C1 C2 C3 -0.1(8) . . . . ?
C1 C2 C3 C4 0.9(8) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
N1 C5 C4 C3 1.4(7) . . . . ?
C6 C5 C4 C3 -176.3(4) . . . . ?
C15 N3 C11 C12 0.1(6) . . . . ?
Ru1 N3 C11 C12 -178.6(4) . . . . ?
C15 N3 C11 C10 -179.3(4) . . . . ?
Ru1 N3 C11 C10 2.0(5) . . . . ?
N2 C10 C11 N3 -1.9(6) . . . . ?
C9 C10 C11 N3 177.6(4) . . . . ?
N2 C10 C11 C12 178.8(4) . . . . ?
C9 C10 C11 C12 -1.8(8) . . . . ?
C11 N3 C15 C14 0.4(7) . . . . ?
Ru1 N3 C15 C14 178.9(4) . . . . ?
N3 C15 C14 C13 -1.1(8) . . . . ?
C15 C14 C13 C12 1.5(9) . . . . ?
C14 C13 C12 C11 -1.0(8) . . . . ?
N3 C11 C12 C13 0.2(7) . . . . ?
C10 C11 C12 C13 179.6(5) . . . . ?

_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.

Mean-plane data from final SHELXL refinement run:-

Least-squares planes (x,y,z in crystal coordinates) and deviations from them
(* indicates atom used to define plane)

;

#==============================================================================

#------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_Rubim_OH2
_database_code_depnum_ccdc_archive 'CCDC 875212'
#TrackingRef '- Rubim_OH2.cif'

_audit_creation_date             2012-03-05T14:21:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
data_Rubim_OH2_2
;
_chemical_formula_moiety         'C21 H19 N7 O Ru, 2(B F4)'
_chemical_formula_sum            'C21 H19 B2 F8 N7 O1 Ru1'
_chemical_formula_weight         660.12
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, z'

_cell_length_a                   10.0573(38)
_cell_length_b                   15.8424(60)
_cell_length_c                   16.3412(66)
_cell_angle_alpha                90.000
_cell_angle_beta                 105.9706(51)
_cell_angle_gamma                90.000
_cell_volume                     2503.1(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    6402
_cell_measurement_theta_min      3.0458
_cell_measurement_theta_max      27.4855
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       chip
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9042
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  Graphite
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_number            18702
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_reflns_number_total             5569
_reflns_number_gt                4799
_reflns_threshold_expression     >2\s(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        
'CrystalClear (Rigaku Inc., 2008), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.0598P)^2^+8.4040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5569
_refine_ls_number_parameters     369
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0609
_refine_ls_wR_factor_ref         0.154
_refine_ls_wR_factor_gt          0.1484
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.827
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.115

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
P P 0.1023 0.0942 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Ru1 Ru 0.69182(4) 0.04168(2) 0.78024(2) 0.02747(14) Uani 1 1 d . . .
F4 F 0.7622(4) 0.0049(3) 0.0228(2) 0.0663(11) Uani 1 1 d . . .
F7 F 0.3377(3) 0.3140(2) 0.4603(2) 0.0480(8) Uani 1 1 d . . .
F6 F 0.3059(4) 0.1729(2) 0.4599(2) 0.0692(12) Uani 1 1 d . . .
F8 F 0.2624(4) 0.2452(2) 0.3355(2) 0.0525(8) Uani 1 1 d . . .
F2 F 0.9404(4) 0.0846(2) 0.0984(2) 0.0602(9) Uani 1 1 d . . .
F5 F 0.4822(4) 0.2281(2) 0.4158(3) 0.0670(11) Uani 1 1 d . . .
N6 N 0.4914(5) -0.1891(3) 0.7641(3) 0.0429(10) Uani 1 1 d . . .
H15 H 0.4217 -0.2196 0.7343 0.051 Uiso 1 1 calc R . .
N7 N 0.3659(4) -0.0645(3) 0.6022(3) 0.0371(9) Uani 1 1 d . . .
H14 H 0.3104 -0.1083 0.5877 0.045 Uiso 1 1 calc R . .
N4 N 0.5286(4) 0.0188(2) 0.6766(2) 0.0286(8) Uani 1 1 d . . .
N5 N 0.6334(4) -0.0818(2) 0.8050(2) 0.0325(8) Uani 1 1 d . . .
F3 F 0.7350(5) 0.0836(4) 0.1307(4) 0.1048(18) Uani 1 1 d . . .
F1 F 0.8735(5) -0.0298(3) 0.1554(3) 0.0810(14) Uani 1 1 d . . .
N2 N 0.7302(4) 0.1542(2) 0.7458(2) 0.0283(8) Uani 1 1 d . . .
C5 C 0.8644(5) 0.0816(3) 0.6709(3) 0.0306(9) Uani 1 1 d . . .
C6 C 0.8074(5) 0.1624(3) 0.6898(3) 0.0293(9) Uani 1 1 d . . .
N3 N 0.5797(4) 0.1132(2) 0.8445(2) 0.0303(8) Uani 1 1 d . . .
C18 C 0.5229(5) -0.1101(3) 0.7463(3) 0.0348(10) Uani 1 1 d . . .
C16 C 0.6739(6) -0.1473(3) 0.8621(3) 0.0428(12) Uani 1 1 d . . .
H17 H 0.7506 -0.1464 0.9113 0.051 Uiso 1 1 calc R . .
C8 C 0.7740(5) 0.3118(3) 0.6902(3) 0.0395(11) Uani 1 1 d . . .
H6 H 0.787 0.3663 0.6695 0.047 Uiso 1 1 calc R . .
C20 C 0.3648(5) 0.0060(3) 0.5544(3) 0.0344(10) Uani 1 1 d . . .
H13 H 0.3052 0.0171 0.4994 0.041 Uiso 1 1 calc R . .
C11 C 0.5977(5) 0.1985(3) 0.8365(3) 0.0313(9) Uani 1 1 d . . .
C13 C 0.4691(6) 0.2286(3) 0.9357(3) 0.0419(12) Uani 1 1 d . . .
H9 H 0.4323 0.2678 0.9676 0.05 Uiso 1 1 calc R . .
O1 O 0.8613(4) 0.0518(3) 0.8920(2) 0.0378(8) Uani 1 1 d . . .
C15 C 0.5045(5) 0.0874(3) 0.8960(3) 0.0348(10) Uani 1 1 d . . .
H11 H 0.4893 0.0286 0.9008 0.042 Uiso 1 1 calc R . .
C14 C 0.4481(6) 0.1435(4) 0.9424(3) 0.0410(12) Uani 1 1 d . . .
H10 H 0.3955 0.1233 0.9785 0.049 Uiso 1 1 calc R . .
C9 C 0.7001(5) 0.3025(3) 0.7504(3) 0.0348(10) Uani 1 1 d . . .
H7 H 0.6659 0.3506 0.773 0.042 Uiso 1 1 calc R . .
N1 N 0.8247(4) 0.0129(3) 0.7088(2) 0.0312(8) Uani 1 1 d . . .
C4 C 0.9556(5) 0.0747(3) 0.6213(3) 0.0339(10) Uani 1 1 d . . .
H4 H 0.9817 0.1229 0.5948 0.041 Uiso 1 1 calc R . .
C12 C 0.5444(5) 0.2564(3) 0.8819(3) 0.0353(10) Uani 1 1 d . . .
H8 H 0.5594 0.3151 0.8763 0.042 Uiso 1 1 calc R . .
C19 C 0.4664(5) -0.0556(3) 0.6753(3) 0.0330(10) Uani 1 1 d . . .
C21 C 0.4660(5) 0.0575(3) 0.6010(3) 0.0304(9) Uani 1 1 d . . .
H12 H 0.4892 0.1115 0.5839 0.036 Uiso 1 1 calc R . .
C7 C 0.8283(5) 0.2420(3) 0.6606(3) 0.0362(10) Uani 1 1 d . . .
H5 H 0.8798 0.2485 0.6202 0.043 Uiso 1 1 calc R . .
C3 C 1.0083(5) -0.0054(4) 0.6113(3) 0.0410(12) Uani 1 1 d . . .
H3 H 1.0721 -0.0117 0.5783 0.049 Uiso 1 1 calc R . .
B2 B 0.8240(6) 0.0388(4) 0.1033(4) 0.0375(12) Uani 1 1 d . . .
C2 C 0.9682(6) -0.0747(4) 0.6488(4) 0.0446(12) Uani 1 1 d . . .
H2 H 1.0028 -0.1293 0.6419 0.054 Uiso 1 1 calc R . .
C17 C 0.5864(7) -0.2132(3) 0.8364(3) 0.0477(13) Uani 1 1 d . . .
H16 H 0.591 -0.2663 0.864 0.057 Uiso 1 1 calc R . .
C10 C 0.6776(5) 0.2225(3) 0.7765(3) 0.0301(9) Uani 1 1 d . . .
C1 C 0.8751(5) -0.0629(3) 0.6974(3) 0.0387(11) Uani 1 1 d . . .
H1 H 0.8464 -0.1106 0.7234 0.046 Uiso 1 1 calc R . .
B1 B 0.3501(6) 0.2366(3) 0.4206(4) 0.0370(12) Uani 1 1 d . . .
H18 H 0.844(9) 0.043(5) 0.944(6) 0.09(3) Uiso 1 1 d . . .
H19 H 0.921(11) 0.026(6) 0.896(6) 0.10(4) 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
Ru1 0.0308(2) 0.0244(2) 0.0290(2) 0.00047(13) 0.01138(15) -0.00055(13)
F4 0.076(3) 0.079(3) 0.0408(18) 0.0025(18) 0.0114(18) -0.031(2)
F7 0.056(2) 0.0409(17) 0.0428(16) -0.0081(13) 0.0074(14) 0.0125(14)
F6 0.084(3) 0.051(2) 0.059(2) 0.0248(17) -0.004(2) -0.0182(19)
F8 0.069(2) 0.0435(18) 0.0380(16) -0.0006(14) 0.0035(15) 0.0025(16)
F2 0.065(2) 0.050(2) 0.070(2) -0.0070(18) 0.0261(19) -0.0205(17)
F5 0.049(2) 0.057(2) 0.096(3) -0.012(2) 0.022(2) 0.0131(17)
N6 0.062(3) 0.029(2) 0.040(2) -0.0022(17) 0.018(2) -0.010(2)
N7 0.034(2) 0.034(2) 0.044(2) -0.0096(18) 0.0131(18) -0.0051(17)
N4 0.029(2) 0.0270(18) 0.0321(19) -0.0028(15) 0.0127(16) -0.0001(15)
N5 0.043(2) 0.0229(18) 0.036(2) 0.0003(15) 0.0168(18) 0.0004(16)
F3 0.083(3) 0.097(4) 0.150(5) -0.038(4) 0.059(3) 0.009(3)
F1 0.090(3) 0.056(2) 0.074(3) 0.029(2) -0.017(2) -0.013(2)
N2 0.0273(19) 0.0289(19) 0.0294(18) 0.0005(15) 0.0091(15) -0.0006(15)
C5 0.031(2) 0.036(2) 0.024(2) -0.0031(17) 0.0067(17) 0.0023(18)
C6 0.029(2) 0.031(2) 0.028(2) 0.0025(17) 0.0081(18) -0.0056(17)
N3 0.032(2) 0.0319(19) 0.0288(18) 0.0006(15) 0.0116(15) 0.0020(16)
C18 0.044(3) 0.026(2) 0.038(2) -0.0035(18) 0.017(2) -0.0050(19)
C16 0.056(3) 0.031(3) 0.042(3) 0.005(2) 0.015(2) 0.004(2)
C8 0.037(3) 0.032(2) 0.050(3) 0.010(2) 0.014(2) -0.003(2)
C20 0.033(2) 0.037(3) 0.033(2) -0.0029(19) 0.0089(19) 0.0030(19)
C11 0.030(2) 0.031(2) 0.032(2) -0.0002(18) 0.0083(18) 0.0015(18)
C13 0.046(3) 0.044(3) 0.040(3) -0.002(2) 0.018(2) 0.011(2)
O1 0.035(2) 0.047(2) 0.0307(18) 0.0011(15) 0.0085(15) 0.0011(17)
C15 0.032(2) 0.036(2) 0.039(2) 0.008(2) 0.015(2) 0.0022(19)
C14 0.041(3) 0.049(3) 0.038(3) 0.005(2) 0.020(2) 0.003(2)
C9 0.031(2) 0.026(2) 0.046(3) 0.0007(19) 0.008(2) -0.0033(18)
N1 0.029(2) 0.033(2) 0.0305(19) -0.0046(16) 0.0061(15) 0.0018(16)
C4 0.031(2) 0.040(3) 0.033(2) 0.0041(19) 0.0118(19) -0.003(2)
C12 0.036(3) 0.033(2) 0.037(2) -0.0036(19) 0.010(2) -0.0001(19)
C19 0.034(3) 0.028(2) 0.040(2) -0.0035(19) 0.014(2) -0.0009(18)
C21 0.030(2) 0.032(2) 0.029(2) -0.0002(17) 0.0078(18) 0.0057(18)
C7 0.034(3) 0.039(3) 0.039(3) 0.007(2) 0.016(2) -0.001(2)
C3 0.034(3) 0.053(3) 0.037(3) -0.004(2) 0.012(2) 0.004(2)
B2 0.036(3) 0.040(3) 0.038(3) 0.001(2) 0.012(2) -0.003(2)
C2 0.045(3) 0.043(3) 0.048(3) -0.008(2) 0.016(2) 0.006(2)
C17 0.075(4) 0.029(2) 0.042(3) 0.007(2) 0.021(3) -0.005(3)
C10 0.030(2) 0.029(2) 0.031(2) 0.0010(17) 0.0078(18) 0.0013(18)
C1 0.041(3) 0.036(3) 0.040(3) -0.004(2) 0.012(2) 0.003(2)
B1 0.043(3) 0.025(2) 0.045(3) -0.004(2) 0.016(3) 0.002(2)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
Ru1 N2 1.939(4) . ?
Ru1 N4 2.041(4) . ?
Ru1 N1 2.053(4) . ?
Ru1 N3 2.076(4) . ?
Ru1 N5 2.113(4) . ?
Ru1 O1 2.134(4) . ?
F4 B2 1.398(7) . ?
F7 B1 1.409(6) . ?
F6 B1 1.336(7) . ?
F8 B1 1.434(7) . ?
F2 B2 1.398(7) . ?
F5 B1 1.358(7) . ?
N6 C18 1.341(6) . ?
N6 C17 1.354(7) . ?
N6 H15 0.88 . ?
N7 C19 1.344(7) . ?
N7 C20 1.361(7) . ?
N7 H14 0.88 . ?
N4 C19 1.332(6) . ?
N4 C21 1.366(6) . ?
N5 C18 1.331(6) . ?
N5 C16 1.380(6) . ?
F3 B2 1.314(8) . ?
F1 B2 1.386(7) . ?
N2 C10 1.360(6) . ?
N2 C6 1.360(6) . ?
C5 N1 1.365(6) . ?
C5 C4 1.386(6) . ?
C5 C6 1.469(6) . ?
C6 C7 1.384(6) . ?
N3 C15 1.341(6) . ?
N3 C11 1.374(6) . ?
C18 C19 1.432(7) . ?
C16 C17 1.354(8) . ?
C16 H17 0.95 . ?
C8 C7 1.378(7) . ?
C8 C9 1.395(7) . ?
C8 H6 0.95 . ?
C20 C21 1.362(7) . ?
C20 H13 0.95 . ?
C11 C12 1.378(7) . ?
C11 C10 1.479(6) . ?
C13 C14 1.374(8) . ?
C13 C12 1.380(7) . ?
C13 H9 0.95 . ?
O1 H18 0.92(10) . ?
O1 H19 0.72(10) . ?
C15 C14 1.387(7) . ?
C15 H11 0.95 . ?
C14 H10 0.95 . ?
C9 C10 1.376(6) . ?
C9 H7 0.95 . ?
N1 C1 1.336(6) . ?
C4 C3 1.402(7) . ?
C4 H4 0.95 . ?
C12 H8 0.95 . ?
C21 H12 0.95 . ?
C7 H5 0.95 . ?
C3 C2 1.371(8) . ?
C3 H3 0.95 . ?
C2 C1 1.397(7) . ?
C2 H2 0.95 . ?
C17 H16 0.95 . ?
C1 H1 0.95 . ?

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
N2 Ru1 N4 95.81(15) . . ?
N2 Ru1 N1 79.98(16) . . ?
N4 Ru1 N1 89.38(15) . . ?
N2 Ru1 N3 79.88(15) . . ?
N4 Ru1 N3 95.27(15) . . ?
N1 Ru1 N3 159.69(16) . . ?
N2 Ru1 N5 173.81(16) . . ?
N4 Ru1 N5 78.02(16) . . ?
N1 Ru1 N5 99.36(16) . . ?
N3 Ru1 N5 100.95(15) . . ?
N2 Ru1 O1 90.18(16) . . ?
N4 Ru1 O1 173.93(15) . . ?
N1 Ru1 O1 90.69(16) . . ?
N3 Ru1 O1 86.74(16) . . ?
N5 Ru1 O1 95.98(16) . . ?
C18 N6 C17 107.4(5) . . ?
C18 N6 H15 126.3 . . ?
C17 N6 H15 126.3 . . ?
C19 N7 C20 108.0(4) . . ?
C19 N7 H14 126 . . ?
C20 N7 H14 126 . . ?
C19 N4 C21 106.6(4) . . ?
C19 N4 Ru1 115.9(3) . . ?
C21 N4 Ru1 137.3(3) . . ?
C18 N5 C16 105.4(4) . . ?
C18 N5 Ru1 113.3(3) . . ?
C16 N5 Ru1 141.3(4) . . ?
C10 N2 C6 121.6(4) . . ?
C10 N2 Ru1 119.7(3) . . ?
C6 N2 Ru1 118.7(3) . . ?
N1 C5 C4 121.7(4) . . ?
N1 C5 C6 114.9(4) . . ?
C4 C5 C6 123.4(4) . . ?
N2 C6 C7 119.2(4) . . ?
N2 C6 C5 112.7(4) . . ?
C7 C6 C5 128.1(4) . . ?
C15 N3 C11 118.2(4) . . ?
C15 N3 Ru1 129.0(3) . . ?
C11 N3 Ru1 112.6(3) . . ?
N5 C18 N6 111.0(4) . . ?
N5 C18 C19 116.5(4) . . ?
N6 C18 C19 132.3(5) . . ?
C17 C16 N5 109.0(5) . . ?
C17 C16 H17 125.5 . . ?
N5 C16 H17 125.5 . . ?
C7 C8 C9 120.2(5) . . ?
C7 C8 H6 119.9 . . ?
C9 C8 H6 119.9 . . ?
N7 C20 C21 106.5(4) . . ?
N7 C20 H13 126.7 . . ?
C21 C20 H13 126.7 . . ?
N3 C11 C12 121.5(4) . . ?
N3 C11 C10 115.2(4) . . ?
C12 C11 C10 123.3(4) . . ?
C14 C13 C12 119.2(5) . . ?
C14 C13 H9 120.4 . . ?
C12 C13 H9 120.4 . . ?
Ru1 O1 H18 118(6) . . ?
Ru1 O1 H19 119(8) . . ?
H18 O1 H19 101(9) . . ?
N3 C15 C14 122.2(5) . . ?
N3 C15 H11 118.9 . . ?
C14 C15 H11 118.9 . . ?
C13 C14 C15 119.4(5) . . ?
C13 C14 H10 120.3 . . ?
C15 C14 H10 120.3 . . ?
C10 C9 C8 118.7(5) . . ?
C10 C9 H7 120.7 . . ?
C8 C9 H7 120.7 . . ?
C1 N1 C5 118.9(4) . . ?
C1 N1 Ru1 127.6(4) . . ?
C5 N1 Ru1 113.5(3) . . ?
C5 C4 C3 118.2(5) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
C11 C12 C13 119.5(5) . . ?
C11 C12 H8 120.3 . . ?
C13 C12 H8 120.3 . . ?
N4 C19 N7 110.0(4) . . ?
N4 C19 C18 116.2(4) . . ?
N7 C19 C18 133.7(5) . . ?
C20 C21 N4 108.9(4) . . ?
C20 C21 H12 125.6 . . ?
N4 C21 H12 125.6 . . ?
C8 C7 C6 119.8(4) . . ?
C8 C7 H5 120.1 . . ?
C6 C7 H5 120.1 . . ?
C2 C3 C4 120.4(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
F3 B2 F1 112.2(6) . . ?
F3 B2 F2 113.5(5) . . ?
F1 B2 F2 106.2(5) . . ?
F3 B2 F4 111.0(5) . . ?
F1 B2 F4 105.6(5) . . ?
F2 B2 F4 108.0(5) . . ?
C3 C2 C1 118.2(5) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
N6 C17 C16 107.2(5) . . ?
N6 C17 H16 126.4 . . ?
C16 C17 H16 126.4 . . ?
N2 C10 C9 120.4(4) . . ?
N2 C10 C11 112.2(4) . . ?
C9 C10 C11 127.4(4) . . ?
N1 C1 C2 122.7(5) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
F6 B1 F5 114.4(5) . . ?
F6 B1 F7 110.6(5) . . ?
F5 B1 F7 108.9(5) . . ?
F6 B1 F8 109.9(5) . . ?
F5 B1 F8 107.7(5) . . ?
F7 B1 F8 104.8(4) . . ?