# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_antonio3
_database_code_depnum_ccdc_archive 'CCDC 1915847'
loop_
_audit_author_name
_audit_author_address
'Eduardo Castellano'
;Instituto de fisica de sao carlos
Brazil
;
_audit_update_record             
;
2019-05-15 deposited with the CCDC.	2019-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6


_chemical_name_common            ?
_chemical_name_systematic        Antonio
_chemical_formula_moiety         '2(C6 H18 N7 O5 Ru S), 2(F6 P)'
_chemical_formula_sum            'C12 H36 F12 N14 O10 P2 Ru2 S2'
_chemical_formula_weight         1092.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C6 H18 P F6 N7 O2'



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'
F F 0.0171 0.0103 '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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7298(6)
_cell_length_b                   9.1139(6)
_cell_length_c                   13.8569(10)
_cell_angle_alpha                78.234(6)
_cell_angle_beta                 82.835(6)
_cell_angle_gamma                69.877(7)
_cell_volume                     895.77(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2858
_cell_measurement_theta_max      31.1580
_cell_measurement_theta_min      2.6210

_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?

_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?





_diffrn_ambient_temperature      296(2)

_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5465
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.616
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     88.00 115.00   1.00   30.00    --   27.63  54.00 -60.00   27
  2  ω    -69.00  39.00   1.00   30.00    --   27.63  54.00-180.00  108
  3  ω    -69.00  37.00   1.00   30.00    --   27.63  54.00  60.00  106
  4  ω    -69.00  46.00   1.00   30.00    --   27.63  54.00 -60.00  115
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0818646000
_diffrn_orient_matrix_UB_12      0.0053348000
_diffrn_orient_matrix_UB_13      -0.0277017000
_diffrn_orient_matrix_UB_21      -0.0485026000
_diffrn_orient_matrix_UB_22      0.0786714000
_diffrn_orient_matrix_UB_23      -0.0221939000
_diffrn_orient_matrix_UB_31      0.0230255000
_diffrn_orient_matrix_UB_32      0.0293918000
_diffrn_orient_matrix_UB_33      0.0385171000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2966
_reflns_number_total             3516
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;









_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'



_refine_diff_density_max         0.825
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3516
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0443P)²+1.4855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0959
_refine_special_details          ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.33345(5) 0.83969(4) 0.84185(2) 0.03223(12) Uani 1 1 d . . . . .
S S 0.18141(17) 0.71705(14) 1.06672(7) 0.0433(3) Uani 1 1 d . . . . .
O2 O 0.3255(6) 0.9711(4) 0.3112(2) 0.0655(11) Uani 1 1 d . . . . .
O1 O 0.4002(6) 0.8804(5) 1.0253(2) 0.0762(13) Uani 1 1 d . . . . .
O12 O 0.0041(5) 0.7761(6) 1.0274(3) 0.0964(17) Uani 1 1 d . . . . .
O13 O 0.2767(6) 0.5602(4) 1.0593(3) 0.0899(16) Uani 1 1 d . . . . .
O11 O 0.1789(10) 0.7611(8) 1.1577(3) 0.137(3) Uani 1 1 d . . . . .
N1 N 0.3167(6) 0.8237(5) 0.9797(2) 0.0450(9) Uani 1 1 d . . . . .
N5 N 0.0456(5) 0.8996(6) 0.8296(3) 0.0567(11) Uani 1 1 d . . . . .
H5A H -0.0036 0.8558 0.8845 0.085 Uiso 1 1 calc R U . . .
H5B H 0.0264 0.8637 0.7782 0.085 Uiso 1 1 calc R U . . .
H5C H -0.0066 1.0046 0.8209 0.085 Uiso 1 1 calc R U . . .
N4 N 0.3500(7) 0.6008(5) 0.8487(3) 0.0547(11) Uani 1 1 d . . . . .
H4A H 0.4628 0.5369 0.8643 0.082 Uiso 1 1 calc R U . . .
H4B H 0.3269 0.5879 0.7902 0.082 Uiso 1 1 calc R U . . .
H4C H 0.2674 0.5774 0.8944 0.082 Uiso 1 1 calc R U . . .
N3 N 0.6220(5) 0.7805(4) 0.8454(3) 0.0427(8) Uani 1 1 d . . . . .
H3A H 0.6470 0.8181 0.8945 0.064 Uiso 1 1 calc R U . . .
H3B H 0.6665 0.8230 0.7883 0.064 Uiso 1 1 calc R U . . .
H3C H 0.6740 0.6755 0.8548 0.064 Uiso 1 1 calc R U . . .
N2 N 0.3224(5) 1.0775(4) 0.8310(2) 0.0403(8) Uani 1 1 d . . . . .
H2A H 0.2139 1.1426 0.8094 0.060 Uiso 1 1 calc R U . . .
H2B H 0.4127 1.0954 0.7889 0.060 Uiso 1 1 calc R U . . .
H2C H 0.3358 1.0947 0.8902 0.060 Uiso 1 1 calc R U . . .
N6 N 0.3543(4) 0.8647(4) 0.6823(2) 0.0306(7) Uani 1 1 d . . . . .
N7 N 0.2625(6) 0.7454(5) 0.3636(3) 0.0515(10) Uani 1 1 d . . . . .
H7A H 0.2443 0.7380 0.3051 0.062 Uiso 1 1 calc R U . . .
H7B H 0.2514 0.6741 0.4130 0.062 Uiso 1 1 calc R U . . .
C4 C 0.2408(6) 0.9894(5) 0.6262(3) 0.0368(9) Uani 1 1 d . . . . .
H4 H 0.1668 1.0748 0.6557 0.044 Uiso 1 1 calc R U . . .
C5 C 0.4669(5) 0.7485(5) 0.6367(3) 0.0372(9) Uani 1 1 d . . . . .
H5 H 0.5552 0.6657 0.6729 0.045 Uiso 1 1 calc R U . . .
C6 C 0.4588(6) 0.7453(5) 0.5387(3) 0.0396(9) Uani 1 1 d . . . . .
H6 H 0.5369 0.6599 0.5105 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3335(5) 0.8699(5) 0.4827(3) 0.0326(8) Uani 1 1 d . . . . .
C3 C 0.2283(6) 0.9974(5) 0.5268(3) 0.0370(9) Uani 1 1 d . . . . .
H3 H 0.1499 1.0875 0.4900 0.044 Uiso 1 1 calc R U . . .
C1 C 0.3076(6) 0.8664(5) 0.3778(3) 0.0364(9) Uani 1 1 d . . . . .
P P 1.08146(16) 0.51978(13) 0.65988(8) 0.0382(3) Uani 1 1 d . . . . .
F1 F 1.2957(5) 0.4644(5) 0.6766(3) 0.0955(13) Uani 1 1 d . . . . .
F2 F 1.1267(7) 0.5608(6) 0.5479(2) 0.1038(15) Uani 1 1 d . . . . .
F3 F 1.0997(6) 0.3485(4) 0.6477(3) 0.1016(14) Uani 1 1 d . . . . .
F4 F 0.8733(5) 0.5717(6) 0.6450(4) 0.1240(18) Uani 1 1 d . . . . .
F5 F 1.0501(8) 0.4790(7) 0.7745(3) 0.132(2) Uani 1 1 d . . . . .
F6 F 1.0691(6) 0.6917(4) 0.6736(3) 0.0926(12) Uani 1 1 d . . . . .


_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
Ru N1 1.877(3) . ?
Ru N3 2.111(3) . ?
Ru N2 2.115(3) . ?
Ru N4 2.119(4) . ?
Ru N5 2.120(4) . ?
Ru N6 2.167(3) . ?
S O13 1.383(4) . ?
S O11 1.395(4) . ?
S O12 1.423(4) . ?
S N1 1.844(4) . ?
O2 C1 1.217(5) . ?
O1 N1 1.244(5) . ?
N6 C5 1.335(5) . ?
N6 C4 1.338(5) . ?
N7 C1 1.322(6) . ?
C4 C3 1.378(5) . ?
C5 C6 1.373(6) . ?
C6 C2 1.379(6) . ?
C2 C3 1.379(6) . ?
C2 C1 1.500(5) . ?
P F4 1.541(4) . ?
P F2 1.546(3) . ?
P F3 1.561(3) . ?
P F5 1.563(4) . ?
P F6 1.585(3) . ?
P F1 1.589(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
N1 Ru N3 88.36(16) . . ?
N1 Ru N2 87.89(14) . . ?
N3 Ru N2 86.05(14) . . ?
N1 Ru N4 93.59(15) . . ?
N3 Ru N4 93.01(16) . . ?
N2 Ru N4 178.23(15) . . ?
N1 Ru N5 94.86(16) . . ?
N3 Ru N5 176.78(14) . . ?
N2 Ru N5 94.13(17) . . ?
N4 Ru N5 86.73(18) . . ?
N1 Ru N6 178.32(14) . . ?
N3 Ru N6 91.19(13) . . ?
N2 Ru N6 90.47(12) . . ?
N4 Ru N6 88.05(13) . . ?
N5 Ru N6 85.60(13) . . ?
O13 S O11 116.7(4) . . ?
O13 S O12 113.9(3) . . ?
O11 S O12 112.5(4) . . ?
O13 S N1 102.6(2) . . ?
O11 S N1 105.7(2) . . ?
O12 S N1 103.7(2) . . ?
O1 N1 S 110.4(3) . . ?
O1 N1 Ru 124.4(3) . . ?
S N1 Ru 125.20(19) . . ?
C5 N6 C4 116.9(3) . . ?
C5 N6 Ru 121.3(2) . . ?
C4 N6 Ru 121.4(3) . . ?
N6 C4 C3 123.2(4) . . ?
N6 C5 C6 123.2(4) . . ?
C5 C6 C2 119.3(4) . . ?
C6 C2 C3 117.9(3) . . ?
C6 C2 C1 121.5(4) . . ?
C3 C2 C1 120.5(4) . . ?
C4 C3 C2 119.0(4) . . ?
O2 C1 N7 123.2(4) . . ?
O2 C1 C2 120.9(4) . . ?
N7 C1 C2 115.9(3) . . ?
F4 P F2 91.9(3) . . ?
F4 P F3 89.1(3) . . ?
F2 P F3 89.9(2) . . ?
F4 P F5 92.2(3) . . ?
F2 P F5 175.7(3) . . ?
F3 P F5 91.6(3) . . ?
F4 P F6 92.6(2) . . ?
F2 P F6 90.5(2) . . ?
F3 P F6 178.2(2) . . ?
F5 P F6 87.9(3) . . ?
F4 P F1 179.2(3) . . ?
F2 P F1 88.8(3) . . ?
F3 P F1 90.5(2) . . ?
F5 P F1 87.1(3) . . ?
F6 P F1 87.8(2) . . ?



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1922883'
loop_
_audit_author_name
_audit_author_address
'Eduardo Castellano'
;Instituto de fisica de sao carlos
Brazil
;
_audit_update_record             
;
2019-06-13 deposited with the CCDC.	2019-06-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H18 N7 O2 Ru,3(B F4)'
_chemical_formula_sum            'C6 H18 B3 F12 N7 O2 Ru'
_chemical_formula_weight         581.77

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'
F F 0.0171 0.0103 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   24.6469(14)
_cell_length_b                   8.6875(5)
_cell_length_c                   9.7514(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2088.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6189
_cell_measurement_theta_min      3.1070
_cell_measurement_theta_max      32.7040

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?

_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    0.874

_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.99119
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.952
_oxdiff_exptl_absorpt_empirical_full_max 1.033
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;



_diffrn_ambient_temperature      293(2)

_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_detector                 'CCD plate'
_diffrn_measurement_method       'ω scans'


_diffrn_reflns_number            19332
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.664
_diffrn_reflns_theta_max         34.533
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4454
_reflns_number_gt                3350
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0528P)²+1.2336P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4454
_refine_ls_number_parameters     166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru Ru 0.15973(2) 0.7500 -0.01209(2) 0.02216(8) Uani 1 2 d S T P . .
O1 O 0.20068(13) 0.7500 -0.2874(3) 0.0613(10) Uani 1 2 d S T P . .
O2 O 0.08068(12) 0.7500 0.6796(3) 0.0503(8) Uani 1 2 d S T P . .
N1 N 0.18678(12) 0.7500 -0.1781(3) 0.0328(6) Uani 1 2 d S T P . .
N2 N 0.10250(8) 0.9166(2) -0.0692(2) 0.0297(4) Uani 1 1 d . . . . .
H2A H 0.0817 0.9395 0.0026 0.036 Uiso 1 1 d R U . . .
H2B H 0.1196 1.0011 -0.0976 0.036 Uiso 1 1 d R U . . .
H2C H 0.0819 0.8801 -0.1368 0.036 Uiso 1 1 d R U . . .
N4 N 0.21435(8) 0.5823(2) 0.0616(2) 0.0305(4) Uani 1 1 d . . . . .
H4A H 0.2075 0.5635 0.1496 0.037 Uiso 1 1 d R U . . .
H4B H 0.2104 0.4959 0.0134 0.037 Uiso 1 1 d R U . . .
H4C H 0.2482 0.6166 0.0527 0.037 Uiso 1 1 d R U . . .
N6 N 0.12375(11) 0.7500 0.1830(3) 0.0237(5) Uani 1 2 d S T P . .
N7 N -0.00222(14) 0.7500 0.5860(4) 0.0612(12) Uani 1 2 d S T P . .
H7A H -0.0184 0.7500 0.6642 0.073 Uiso 1 2 d R U P . .
H7B H -0.0209 0.7500 0.5115 0.073 Uiso 1 2 d R U P . .
C1 C 0.11132(11) 0.6177(3) 0.2468(2) 0.0328(5) Uani 1 1 d . . . . .
H1 H 0.1190 0.5250 0.2031 0.039 Uiso 1 1 calc R U . . .
C2 C 0.08769(12) 0.6142(3) 0.3745(3) 0.0388(6) Uani 1 1 d . . . . .
H2 H 0.0803 0.5206 0.4169 0.047 Uiso 1 1 calc R U . . .
C3 C 0.07503(14) 0.7500 0.4387(3) 0.0302(7) Uani 1 2 d S T P . .
C6 C 0.05075(16) 0.7500 0.5804(3) 0.0365(8) Uani 1 2 d S T P . .
F11 F 0.12193(12) 0.2500 0.3186(4) 0.0754(10) Uani 1 2 d S T P . .
F12 F 0.20116(8) 0.1210(2) 0.3263(3) 0.0708(6) Uani 1 1 d . . . . .
F13 F 0.1737(2) 0.2500 0.5057(3) 0.1027(17) Uani 1 2 d S T P . .
B1 B 0.17310(19) 0.2500 0.3651(5) 0.0409(9) Uani 1 2 d S T P . .
F21 F 0.31485(9) 0.6193(2) 0.3009(2) 0.0619(5) Uani 1 1 d . . . . .
F22 F 0.29735(15) 0.7500 0.4928(2) 0.0588(8) Uani 1 2 d S T P . .
F23 F 0.23756(12) 0.7500 0.3177(3) 0.0671(8) Uani 1 2 d S T P . .
B2 B 0.2912(2) 0.7500 0.3528(5) 0.0383(9) Uani 1 2 d S T P . .
F31 F 0.08088(12) 0.2500 -0.0332(4) 0.0672(9) Uani 1 2 d S T P . .
F32 F 0.02688(8) 0.1203(2) 0.11277(19) 0.0521(4) Uani 1 1 d . . . . .
F33 F -0.00865(12) 0.2500 -0.0646(3) 0.0624(8) Uani 1 2 d S T P . .
B3 B 0.03139(18) 0.2500 0.0313(4) 0.0338(8) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ru N1 1.750(3) . ?
Ru N2 2.0964(19) 8_575 ?
Ru N2 2.0964(19) . ?
Ru N6 2.099(3) . ?
Ru N4 2.1097(19) . ?
Ru N4 2.1097(19) 8_575 ?
O1 N1 1.119(4) . ?
O2 C6 1.216(4) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8901 . ?
N2 H2C 0.8900 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 H4C 0.8901 . ?
N6 C1 1.343(3) . ?
N6 C1 1.343(3) 8_575 ?
N7 C6 1.307(5) . ?
N7 H7A 0.8600 . ?
N7 H7B 0.8600 . ?
C1 C2 1.374(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.372(3) . ?
C2 H2 0.9300 . ?
C3 C2 1.372(3) 8_575 ?
C3 C6 1.505(5) . ?
F11 B1 1.340(5) . ?
F12 B1 1.370(3) . ?
F13 B1 1.371(6) . ?
B1 F12 1.370(3) 8_565 ?
F21 B2 1.373(3) . ?
F22 B2 1.373(5) . ?
F23 B2 1.367(5) . ?
B2 F21 1.373(3) 8_575 ?
F31 B3 1.372(5) . ?
F32 B3 1.383(3) . ?
F33 B3 1.360(5) . ?
B3 F32 1.383(3) 8_565 ?

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
N1 Ru N2 90.62(9) . 8_575 ?
N1 Ru N2 90.62(9) . . ?
N2 Ru N2 87.33(11) 8_575 . ?
N1 Ru N6 177.39(12) . . ?
N2 Ru N6 87.50(8) 8_575 . ?
N2 Ru N6 87.50(8) . . ?
N1 Ru N4 94.12(9) . . ?
N2 Ru N4 92.45(8) 8_575 . ?
N2 Ru N4 175.27(8) . . ?
N6 Ru N4 87.77(8) . . ?
N1 Ru N4 94.12(9) . 8_575 ?
N2 Ru N4 175.27(8) 8_575 8_575 ?
N2 Ru N4 92.45(8) . 8_575 ?
N6 Ru N4 87.77(8) . 8_575 ?
N4 Ru N4 87.37(11) . 8_575 ?
O1 N1 Ru 175.4(3) . . ?
Ru N2 H2A 109.5 . . ?
Ru N2 H2B 109.5 . . ?
H2A N2 H2B 109.5 . . ?
Ru N2 H2C 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?
Ru N4 H4A 109.5 . . ?
Ru N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
Ru N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
C1 N6 C1 117.8(3) . 8_575 ?
C1 N6 Ru 121.10(14) . . ?
C1 N6 Ru 121.10(14) 8_575 . ?
C6 N7 H7A 120.0 . . ?
C6 N7 H7B 120.0 . . ?
H7A N7 H7B 120.0 . . ?
N6 C1 C2 122.3(2) . . ?
N6 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C2 118.6(3) . 8_575 ?
C2 C3 C6 120.64(15) . . ?
C2 C3 C6 120.64(15) 8_575 . ?
O2 C6 N7 124.9(3) . . ?
O2 C6 C3 119.2(3) . . ?
N7 C6 C3 115.8(3) . . ?
F11 B1 F12 112.4(3) . . ?
F11 B1 F12 112.5(3) . 8_565 ?
F12 B1 F12 109.8(4) . 8_565 ?
F11 B1 F13 110.4(5) . . ?
F12 B1 F13 105.7(3) . . ?
F12 B1 F13 105.7(3) 8_565 . ?
F23 B2 F21 108.5(2) . . ?
F23 B2 F21 108.5(2) . 8_575 ?
F21 B2 F21 111.6(4) . 8_575 ?
F23 B2 F22 110.8(4) . . ?
F21 B2 F22 108.7(2) . . ?
F21 B2 F22 108.7(2) 8_575 . ?
F33 B3 F31 109.2(4) . . ?
F33 B3 F32 109.7(2) . 8_565 ?
F31 B3 F32 109.6(2) . 8_565 ?
F33 B3 F32 109.7(2) . . ?
F31 B3 F32 109.6(2) . . ?
F32 B3 F32 109.1(3) 8_565 . ?

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
C1 N6 C1 C2 -1.3(5) 8_575 . . . ?
Ru N6 C1 C2 -179.9(2) . . . . ?
N6 C1 C2 C3 1.5(5) . . . . ?
C1 C2 C3 C2 -1.6(6) . . . 8_575 ?
C1 C2 C3 C6 -178.1(3) . . . . ?
C2 C3 C6 O2 88.2(3) . . . . ?
C2 C3 C6 O2 -88.2(3) 8_575 . . . ?
C2 C3 C6 N7 -91.8(3) . . . . ?
C2 C3 C6 N7 91.8(3) 8_575 . . . ?

_refine_diff_density_max         2.190
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.105

_shelxl_version_number           2014/6



