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


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#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_mper22
_database_code_depnum_ccdc_archive 'CCDC 787101'
#TrackingRef 'final_version_MPER22_jan2013.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C55 H36 Br N11 Ru, 2(F6 P)'
_chemical_formula_sum            'C55 H36 Br F12 N11 P2 Ru'
_chemical_formula_weight         1321.87
_chemical_compound_source        'Synthesized by the authors. See text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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
_symmetry_space_group_name_hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   9.2589(12)
_cell_length_b                   14.846(3)
_cell_length_c                   21.138(4)
_cell_angle_alpha                108.121(8)
_cell_angle_beta                 98.105(8)
_cell_angle_gamma                93.990(8)
_cell_volume                     2713.9(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    5465
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      67.25
_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    4.562
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.6439
_exptl_absorpt_correction_T_max  0.9554
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2007)'
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker microstar diffractometer equiped with a Platinum 135 CCD Detector,
a Helios optics and a Kappa goniometer. The crystal-to-detector distance
was 4.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over three different parts of the reciprocal space
(99 frames total).
Due to geometrical constraints of the instrument and the use of copper
radiation, we obtain consistently a data completeness lower than 100%
in dependence of the crystal system and the orientation of the mounted crystal,
even with appropriate data collection routines. Typical values for data
completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98%
for all other crystal systems.
;
_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            29410
_diffrn_reflns_av_R_equivalents  0.087
_diffrn_reflns_av_unetI/netI     0.1072
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         54.61
_reflns_number_total             5922
_reflns_number_gt                3960
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_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.
Constraints and restraints (such as ISOR, DFIX, DANG, DELU, SIMU) were
used on PF6 and some C atoms of the cation.
;
_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^)+(0.1718P)^2^+68.3389P] 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     SHELXL
_refine_ls_extinction_coef       0.0030(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         5922
_refine_ls_number_parameters     384
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.2151
_refine_ls_R_factor_gt           0.1662
_refine_ls_wR_factor_ref         0.4348
_refine_ls_wR_factor_gt          0.3996
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_restrained_S_all      1.181
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru1 Ru 0.71341(17) 0.27096(15) 0.24989(9) 0.0689(10) Uani 1 1 d . . .
Br1 Br 1.0057(7) 0.9909(3) 0.6100(4) 0.204(3) Uani 1 1 d . . .
N1 N 0.5206(17) 0.3319(12) 0.2356(8) 0.051(5) Uani 1 1 d . . .
N2 N 0.7664(16) 0.3997(14) 0.3125(8) 0.061(6) Uani 1 1 d . . .
N3 N 0.9260(18) 0.2655(15) 0.2937(8) 0.070(7) Uani 1 1 d . . .
N4 N 0.702(2) 0.5575(17) 0.3638(11) 0.095(9) Uani 1 1 d . . .
N5 N 0.940(2) 0.5174(19) 0.3979(11) 0.099(9) Uani 1 1 d . . .
N6 N 0.7882(16) 0.2866(14) 0.1650(8) 0.054(5) Uani 1 1 d . . .
N7 N 0.6706(17) 0.1391(13) 0.1880(8) 0.051(5) Uani 1 1 d . . .
N8 N 0.6217(16) 0.2029(15) 0.3101(8) 0.057(6) Uani 1 1 d . . .
N9 N 0.216(3) -0.5909(17) -0.2135(12) 0.090(7) Uani 1 1 d . . .
N10 N 0.588(3) -0.625(2) -0.1606(13) 0.098(8) Uani 1 1 d . . .
N11 N 0.968(3) -0.578(2) -0.0877(14) 0.115(10) Uani 1 1 d . . .
C1 C 0.386(3) 0.2859(18) 0.1983(12) 0.062(6) Uiso 1 1 d . . .
H1 H 0.3790 0.2201 0.1729 0.075 Uiso 1 1 calc R . .
C2 C 0.264(2) 0.3320(16) 0.1968(11) 0.053(6) Uiso 1 1 d . . .
H2 H 0.1736 0.2985 0.1698 0.064 Uiso 1 1 calc R . .
C3 C 0.271(3) 0.4243(17) 0.2333(12) 0.061(6) Uiso 1 1 d . . .
H3 H 0.1858 0.4564 0.2327 0.073 Uiso 1 1 calc R . .
C4 C 0.404(2) 0.4728(17) 0.2722(11) 0.053(6) Uiso 1 1 d . . .
H4 H 0.4121 0.5390 0.2967 0.063 Uiso 1 1 calc R . .
C5 C 0.524(2) 0.4241(16) 0.2747(11) 0.049(5) Uiso 1 1 d . . .
C6 C 0.667(2) 0.4650(16) 0.3182(11) 0.052(6) Uiso 1 1 d . . .
C7 C 0.842(2) 0.5844(17) 0.4056(11) 0.055(6) Uiso 1 1 d . . .
C8 C 0.900(2) 0.4266(16) 0.3525(11) 0.050(6) Uiso 1 1 d . . .
C9 C 0.988(2) 0.3458(15) 0.3406(10) 0.044(5) Uiso 1 1 d . . .
C10 C 1.130(3) 0.3525(19) 0.3758(12) 0.064(7) Uiso 1 1 d . . .
H10 H 1.1720 0.4111 0.4093 0.077 Uiso 1 1 calc R . .
C11 C 1.208(4) 0.278(2) 0.3631(16) 0.093(9) Uiso 1 1 d . . .
H11 H 1.3068 0.2833 0.3854 0.112 Uiso 1 1 calc R . .
C12 C 1.138(3) 0.190(2) 0.3150(13) 0.073(7) Uiso 1 1 d . . .
H12 H 1.1837 0.1325 0.3067 0.087 Uiso 1 1 calc R . .
C13 C 0.997(3) 0.1924(19) 0.2805(12) 0.064(7) Uiso 1 1 d . . .
H13 H 0.9521 0.1365 0.2450 0.077 Uiso 1 1 calc R . .
C14 C 0.883(2) 0.6852(13) 0.4516(10) 0.076(7) Uiso 1 1 d G . .
C15 C 0.7812(19) 0.7506(16) 0.4605(10) 0.100(10) Uiso 1 1 d G . .
H15 H 0.6853 0.7334 0.4343 0.120 Uiso 1 1 calc R . .
C16 C 0.820(2) 0.8412(14) 0.5079(12) 0.112(11) Uiso 1 1 d G . .
H16 H 0.7499 0.8859 0.5140 0.135 Uiso 1 1 calc R . .
C17 C 0.960(3) 0.8664(14) 0.5463(11) 0.113(11) Uiso 1 1 d G . .
C18 C 1.062(2) 0.8010(19) 0.5373(12) 0.151(16) Uiso 1 1 d G . .
H18 H 1.1577 0.8182 0.5635 0.181 Uiso 1 1 calc R . .
C19 C 1.023(2) 0.7104(17) 0.4899(12) 0.131(13) Uiso 1 1 d G . .
H19 H 1.0930 0.6657 0.4838 0.157 Uiso 1 1 calc R . .
C20 C 0.604(3) 0.2416(19) 0.3738(12) 0.064(7) Uiso 1 1 d . . .
H20 H 0.6323 0.3081 0.3954 0.077 Uiso 1 1 calc R . .
C21 C 0.550(3) 0.192(2) 0.4080(16) 0.086(8) Uiso 1 1 d . . .
H21 H 0.5376 0.2237 0.4532 0.103 Uiso 1 1 calc R . .
C22 C 0.508(4) 0.092(3) 0.3787(17) 0.103(10) Uiso 1 1 d . . .
H22 H 0.4704 0.0542 0.4031 0.124 Uiso 1 1 calc R . .
C23 C 0.527(3) 0.051(2) 0.3100(16) 0.091(9) Uiso 1 1 d . . .
H23 H 0.4970 -0.0146 0.2870 0.109 Uiso 1 1 calc R . .
C24 C 0.587(2) 0.1055(17) 0.2772(11) 0.052(6) Uiso 1 1 d . . .
C25 C 0.615(2) 0.0704(17) 0.2084(11) 0.052(6) Uiso 1 1 d . . .
C26 C 0.590(2) -0.0247(16) 0.1664(10) 0.049(5) Uiso 1 1 d . . .
H26 H 0.5507 -0.0736 0.1815 0.059 Uiso 1 1 calc R . .
C27 C 0.626(2) -0.0461(16) 0.1011(11) 0.053(6) Uiso 1 1 d . . .
C28 C 0.686(2) 0.0223(15) 0.0817(11) 0.047(5) Uiso 1 1 d . . .
H28 H 0.7148 0.0070 0.0385 0.056 Uiso 1 1 calc R . .
C29 C 0.709(2) 0.1191(15) 0.1256(11) 0.048(5) Uiso 1 1 d . . .
C30 C 0.772(2) 0.2029(14) 0.1124(9) 0.036(5) Uiso 1 1 d . . .
C31 C 0.824(2) 0.2016(17) 0.0528(12) 0.056(6) Uiso 1 1 d . . .
H31 H 0.8161 0.1436 0.0165 0.068 Uiso 1 1 calc R . .
C32 C 0.883(3) 0.2831(18) 0.0481(13) 0.065(7) Uiso 1 1 d . . .
H32 H 0.9156 0.2828 0.0073 0.078 Uiso 1 1 calc R . .
C33 C 0.898(3) 0.366(2) 0.0995(13) 0.070(7) Uiso 1 1 d . . .
H33 H 0.9406 0.4243 0.0965 0.084 Uiso 1 1 calc R . .
C34 C 0.850(3) 0.3607(18) 0.1550(12) 0.057(6) Uiso 1 1 d . . .
H34 H 0.8632 0.4186 0.1918 0.068 Uiso 1 1 calc R . .
C35 C 0.6130(16) -0.1507(8) 0.0554(7) 0.053(6) Uiso 1 1 d G . .
C36 C 0.4956(14) -0.2166(10) 0.0522(7) 0.063(6) Uiso 1 1 d G . .
H36 H 0.4220 -0.1976 0.0790 0.075 Uiso 1 1 calc R . .
C37 C 0.4860(15) -0.3102(9) 0.0097(8) 0.074(7) Uiso 1 1 d G . .
H37 H 0.4058 -0.3553 0.0074 0.089 Uiso 1 1 calc R . .
C38 C 0.5938(17) -0.3380(8) -0.0296(7) 0.066(7) Uiso 1 1 d G . .
C39 C 0.7112(15) -0.2721(11) -0.0264(7) 0.064(7) Uiso 1 1 d G . .
H39 H 0.7848 -0.2911 -0.0532 0.077 Uiso 1 1 calc R . .
C40 C 0.7208(14) -0.1785(9) 0.0161(8) 0.070(7) Uiso 1 1 d G . .
H40 H 0.8010 -0.1334 0.0183 0.084 Uiso 1 1 calc R . .
C41 C 0.709(3) -0.575(2) -0.1191(14) 0.077(8) Uiso 1 1 d . . .
C42 C 0.721(3) -0.485(2) -0.0765(14) 0.082(8) Uiso 1 1 d . . .
H42 H 0.8110 -0.4493 -0.0504 0.099 Uiso 1 1 calc R . .
C43 C 0.576(3) -0.4459(18) -0.0753(12) 0.064(7) Uiso 1 1 d . . .
C44 C 0.472(3) -0.4857(19) -0.1095(12) 0.068(7) Uiso 1 1 d . . .
H44 H 0.3852 -0.4555 -0.1090 0.081 Uiso 1 1 calc R . .
C45 C 0.468(4) -0.584(2) -0.1553(16) 0.092(9) Uiso 1 1 d . . .
C46 C 0.845(4) -0.629(2) -0.1205(16) 0.085(8) Uiso 1 1 d . . .
C47 C 1.099(6) -0.621(4) -0.088(2) 0.152(16) Uiso 1 1 d . . .
H47 H 1.1916 -0.5844 -0.0670 0.182 Uiso 1 1 calc R . .
C48 C 1.087(5) -0.721(3) -0.123(2) 0.144(15) Uiso 1 1 d . . .
H48 H 1.1703 -0.7538 -0.1185 0.173 Uiso 1 1 calc R . .
C49 C 0.957(4) -0.771(3) -0.1612(19) 0.118(12) Uiso 1 1 d . . .
H49 H 0.9571 -0.8350 -0.1882 0.142 Uiso 1 1 calc R . .
C50 C 0.825(4) -0.730(2) -0.1625(16) 0.098(10) Uiso 1 1 d . . .
H50 H 0.7331 -0.7635 -0.1876 0.118 Uiso 1 1 calc R . .
C51 C 0.331(3) -0.638(2) -0.2085(15) 0.081(8) Uiso 1 1 d . . .
C52 C 0.339(4) -0.731(3) -0.2475(18) 0.112(11) Uiso 1 1 d . . .
H52 H 0.4288 -0.7579 -0.2439 0.134 Uiso 1 1 calc R . .
C53 C 0.216(5) -0.785(3) -0.292(2) 0.140(15) Uiso 1 1 d . . .
H53 H 0.2154 -0.8502 -0.3170 0.169 Uiso 1 1 calc R . .
C54 C 0.086(4) -0.733(3) -0.2975(18) 0.109(11) Uiso 1 1 d . . .
H54 H -0.0008 -0.7651 -0.3280 0.131 Uiso 1 1 calc R . .
C55 C 0.090(4) -0.640(3) -0.2595(17) 0.106(10) Uiso 1 1 d . . .
H55 H 0.0061 -0.6073 -0.2642 0.127 Uiso 1 1 calc R . .
P11 P 0.1612(7) 0.0152(5) 0.1263(3) 0.0620(18) Uiso 1 1 d D . .
F11 F 0.2760(17) 0.0633(11) 0.1938(7) 0.093(5) Uiso 1 1 d D . .
F12 F 0.2780(16) 0.0395(11) 0.0838(7) 0.086(4) Uiso 1 1 d D . .
F13 F 0.223(2) -0.0821(13) 0.1189(10) 0.132(7) Uiso 1 1 d D . .
F14 F 0.044(2) -0.0062(14) 0.1671(10) 0.118(6) Uiso 1 1 d D . .
F15 F 0.0996(17) 0.1142(11) 0.1342(8) 0.087(4) Uiso 1 1 d D . .
F16 F 0.046(2) -0.0341(15) 0.0588(10) 0.120(6) Uiso 1 1 d D . .
P21 P 0.390(3) 0.8148(19) 0.3845(14) 0.172(11) Uiso 0.50 1 d PD . .
F21 F 0.468(5) 0.727(3) 0.347(2) 0.169(19) Uiso 0.50 1 d PD . .
F22 F 0.331(6) 0.830(4) 0.315(2) 0.23(3) Uiso 0.50 1 d PD . .
F23 F 0.251(5) 0.746(4) 0.378(3) 0.29(4) Uiso 0.50 1 d PD . .
F24 F 0.458(7) 0.808(5) 0.454(2) 0.31(5) Uiso 0.50 1 d PD . .
F25 F 0.534(5) 0.885(4) 0.392(3) 0.30(4) Uiso 0.50 1 d PD . .
F26 F 0.312(7) 0.902(4) 0.424(3) 0.31(4) Uiso 0.50 1 d PD . .
P31 P 0.5000 0.5000 0.5000 0.074(3) Uiso 1 2 d SD . .
F31 F 0.6591(16) 0.4677(12) 0.4937(8) 0.103(5) Uiso 1 1 d D . .
F32 F 0.4565(16) 0.4649(11) 0.4200(7) 0.088(5) Uiso 1 1 d D . .
F33 F 0.4466(18) 0.3985(11) 0.5020(8) 0.099(5) Uiso 1 1 d 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 0.0249(9) 0.0825(16) 0.0571(13) -0.0325(10) -0.0061(7) 0.0110(8)
Br1 0.193(6) 0.081(3) 0.242(7) -0.041(3) -0.043(5) -0.018(3)
N1 0.037(9) 0.043(11) 0.048(10) -0.014(9) -0.008(8) 0.002(8)
N2 0.026(8) 0.078(14) 0.049(10) -0.020(10) 0.001(7) 0.016(9)
N3 0.044(10) 0.095(16) 0.037(10) -0.028(10) -0.012(8) 0.050(11)
N4 0.049(11) 0.099(17) 0.072(14) -0.051(13) -0.016(10) -0.001(11)
N5 0.040(11) 0.13(2) 0.083(16) -0.023(15) -0.002(10) -0.007(12)
N6 0.021(8) 0.086(14) 0.044(10) 0.009(10) -0.002(7) 0.005(9)
N7 0.032(8) 0.053(12) 0.048(10) -0.012(9) 0.001(8) 0.014(8)
N8 0.027(8) 0.110(17) 0.029(9) 0.011(10) 0.004(7) 0.033(9)
N9 0.077(15) 0.076(16) 0.091(17) 0.005(13) -0.014(13) -0.008(13)
N10 0.089(17) 0.11(2) 0.089(17) 0.030(16) 0.021(14) -0.003(15)
N11 0.10(2) 0.11(2) 0.12(2) 0.023(18) -0.008(17) 0.065(18)
_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_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru1 N2 . . 1.938(17) Y
Ru1 N7 . . 1.963(16) Y
Ru1 N3 . . 2.072(15) Y
Ru1 N1 . . 2.082(16) Y
Ru1 N6 . . 2.083(18) Y
Ru1 N8 . . 2.08(2) Y
Br1 C17 . . 1.896(17) Y
N1 C5 . . 1.36(3) Y
N1 C1 . . 1.38(3) Y
N2 C8 . . 1.35(3) Y
N2 C6 . . 1.37(3) Y
N3 C13 . . 1.29(3) Y
N3 C9 . . 1.32(3) Y
N4 C6 . . 1.39(3) Y
N4 C7 . . 1.41(3) Y
N5 C8 . . 1.38(3) Y
N5 C7 . . 1.38(3) Y
N6 C34 . . 1.29(3) Y
N6 C30 . . 1.37(3) Y
N7 C25 . . 1.33(3) Y
N7 C29 . . 1.36(3) Y
N8 C20 . . 1.33(3) Y
N8 C24 . . 1.39(3) Y
N9 C51 . . 1.33(4) Y
N9 C55 . . 1.40(4) Y
N10 C45 . . 1.31(4) Y
N10 C41 . . 1.33(4) Y
N11 C46 . . 1.29(4) Y
N11 C47 . . 1.41(5) Y
C1 C2 . . 1.37(3) Y
C1 H1 . . 0.9500 ?
C2 C3 . . 1.34(3) Y
C2 H2 . . 0.9500 ?
C3 C4 . . 1.39(3) Y
C3 H3 . . 0.9500 ?
C4 C5 . . 1.37(3) Y
C4 H4 . . 0.9500 ?
C5 C6 . . 1.47(3) Y
C7 C14 . . 1.50(3) Y
C8 C9 . . 1.47(3) Y
C9 C10 . . 1.40(3) Y
C10 C11 . . 1.35(4) Y
C10 H10 . . 0.9500 ?
C11 C12 . . 1.43(4) Y
C11 H11 . . 0.9500 ?
C12 C13 . . 1.41(3) Y
C12 H12 . . 0.9500 ?
C13 H13 . . 0.9500 ?
C14 C15 . . 1.3900 Y
C14 C19 . . 1.3900 Y
C15 C16 . . 1.3900 Y
C15 H15 . . 0.9500 ?
C16 C17 . . 1.3900 Y
C16 H16 . . 0.9500 ?
C17 C18 . . 1.3900 Y
C18 C19 . . 1.3900 Y
C18 H18 . . 0.9500 ?
C19 H19 . . 0.9500 ?
C20 C21 . . 1.30(3) Y
C20 H20 . . 0.9500 ?
C21 C22 . . 1.43(4) Y
C21 H21 . . 0.9500 ?
C22 C23 . . 1.43(4) Y
C22 H22 . . 0.9500 ?
C23 C24 . . 1.35(4) Y
C23 H23 . . 0.9500 ?
C24 C25 . . 1.45(3) Y
C25 C26 . . 1.40(3) Y
C26 C27 . . 1.41(3) Y
C26 H26 . . 0.9500 ?
C27 C28 . . 1.33(3) Y
C27 C35 . . 1.54(2) Y
C28 C29 . . 1.43(3) Y
C28 H28 . . 0.9500 ?
C29 C30 . . 1.46(3) Y
C30 C31 . . 1.40(3) Y
C31 C32 . . 1.33(3) Y
C31 H31 . . 0.9500 ?
C32 C33 . . 1.35(3) Y
C32 H32 . . 0.9500 ?
C33 C34 . . 1.33(3) Y
C33 H33 . . 0.9500 ?
C34 H34 . . 0.9500 ?
C35 C36 . . 1.3900 Y
C35 C40 . . 1.3900 Y
C36 C37 . . 1.3900 Y
C36 H36 . . 0.9500 ?
C37 C38 . . 1.3900 Y
C37 H37 . . 0.9500 ?
C38 C39 . . 1.3900 Y
C38 C43 . . 1.57(3) Y
C39 C40 . . 1.3900 Y
C39 H39 . . 0.9500 ?
C40 H40 . . 0.9500 ?
C41 C42 . . 1.35(4) Y
C41 C46 . . 1.53(4) Y
C42 C43 . . 1.50(4) Y
C42 H42 . . 0.9500 ?
C43 C44 . . 1.12(3) Y
C44 C45 . . 1.47(4) Y
C44 H44 . . 0.9500 ?
C45 C51 . . 1.55(4) Y
C46 C50 . . 1.47(4) Y
C47 C48 . . 1.42(6) Y
C47 H47 . . 0.9500 ?
C48 C49 . . 1.37(5) Y
C48 H48 . . 0.9500 ?
C49 C50 . . 1.41(5) Y
C49 H49 . . 0.9500 ?
C50 H50 . . 0.9500 ?
C51 C52 . . 1.38(4) Y
C52 C53 . . 1.38(5) Y
C52 H52 . . 0.9500 ?
C53 C54 . . 1.48(5) Y
C53 H53 . . 0.9500 ?
C54 C55 . . 1.36(4) Y
C54 H54 . . 0.9500 ?
C55 H55 . . 0.9500 ?
P11 F14 . . 1.55(2) Y
P11 F13 . . 1.561(17) Y
P11 F15 . . 1.583(17) Y
P11 F11 . . 1.584(14) Y
P11 F16 . . 1.59(2) Y
P11 F12 . . 1.589(14) Y
P21 F23 . . 1.55(2) Y
P21 F24 . . 1.55(3) Y
P21 F21 . . 1.578(19) Y
P21 F26 . . 1.58(3) Y
P21 F22 . . 1.584(19) Y
P21 F25 . . 1.59(2) Y
P31 F33 . . 1.568(15) Y
P31 F33 . 2_666 1.568(15) Y
P31 F32 . . 1.590(13) Y
P31 F32 . 2_666 1.590(13) Y
P31 F31 . . 1.591(14) Y
P31 F31 . 2_666 1.591(14) Y
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 RU1 N7 . . . 176.9(7) Y
N2 RU1 N3 . . . 78.1(7) Y
N7 RU1 N3 . . . 98.8(7) Y
N2 RU1 N1 . . . 78.3(6) Y
N7 RU1 N1 . . . 104.9(6) Y
N3 RU1 N1 . . . 156.3(6) Y
N2 RU1 N6 . . . 100.4(8) Y
N7 RU1 N6 . . . 79.4(8) Y
N3 RU1 N6 . . . 90.7(7) Y
N1 RU1 N6 . . . 95.2(7) Y
N2 RU1 N8 . . . 101.2(8) Y
N7 RU1 N8 . . . 79.0(8) Y
N3 RU1 N8 . . . 92.6(8) Y
N1 RU1 N8 . . . 90.3(7) Y
N6 RU1 N8 . . . 158.4(7) Y
C5 N1 C1 . . . 116.8(18) Y
C5 N1 RU1 . . . 115.3(12) Y
C1 N1 RU1 . . . 127.2(15) Y
C8 N2 C6 . . . 118.6(18) Y
C8 N2 RU1 . . . 121.1(14) Y
C6 N2 RU1 . . . 120.2(13) Y
C13 N3 C9 . . . 119.6(18) Y
C13 N3 RU1 . . . 126.3(16) Y
C9 N3 RU1 . . . 114.1(13) Y
C6 N4 C7 . . . 120(2) Y
C8 N5 C7 . . . 120.6(19) Y
C34 N6 C30 . . . 115.7(19) Y
C34 N6 RU1 . . . 130.9(16) Y
C30 N6 RU1 . . . 113.3(15) Y
C25 N7 C29 . . . 120.9(18) Y
C25 N7 RU1 . . . 120.4(14) Y
C29 N7 RU1 . . . 118.5(15) Y
C20 N8 C24 . . . 121(2) Y
C20 N8 RU1 . . . 127.4(18) Y
C24 N8 RU1 . . . 111.7(13) Y
C51 N9 C55 . . . 118(3) Y
C45 N10 C41 . . . 116(3) Y
C46 N11 C47 . . . 120(3) Y
C2 C1 N1 . . . 122(2) Y
C2 C1 H1 . . . 118.9 ?
N1 C1 H1 . . . 118.9 ?
C3 C2 C1 . . . 120(2) Y
C3 C2 H2 . . . 120.0 ?
C1 C2 H2 . . . 120.0 ?
C2 C3 C4 . . . 119(2) Y
C2 C3 H3 . . . 120.3 ?
C4 C3 H3 . . . 120.3 ?
C5 C4 C3 . . . 119(2) Y
C5 C4 H4 . . . 120.3 ?
C3 C4 H4 . . . 120.3 ?
N1 C5 C4 . . . 121.9(19) Y
N1 C5 C6 . . . 113.6(18) Y
C4 C5 C6 . . . 124(2) Y
N2 C6 N4 . . . 121.1(19) Y
N2 C6 C5 . . . 112.5(18) Y
N4 C6 C5 . . . 126(2) Y
N5 C7 N4 . . . 118(2) Y
N5 C7 C14 . . . 122(2) Y
N4 C7 C14 . . . 120(2) Y
N2 C8 N5 . . . 122(2) Y
N2 C8 C9 . . . 110.1(18) Y
N5 C8 C9 . . . 128(2) Y
N3 C9 C10 . . . 121(2) Y
N3 C9 C8 . . . 116.6(18) Y
C10 C9 C8 . . . 123(2) Y
C11 C10 C9 . . . 121(3) Y
C11 C10 H10 . . . 119.3 ?
C9 C10 H10 . . . 119.3 ?
C10 C11 C12 . . . 118(3) Y
C10 C11 H11 . . . 121.2 ?
C12 C11 H11 . . . 121.2 ?
C13 C12 C11 . . . 116(3) Y
C13 C12 H12 . . . 122.1 ?
C11 C12 H12 . . . 122.1 ?
N3 C13 C12 . . . 125(2) Y
N3 C13 H13 . . . 117.7 ?
C12 C13 H13 . . . 117.7 ?
C15 C14 C19 . . . 120.0 Y
C15 C14 C7 . . . 121.5(17) Y
C19 C14 C7 . . . 118.3(17) Y
C14 C15 C16 . . . 120.0 Y
C14 C15 H15 . . . 120.0 ?
C16 C15 H15 . . . 120.0 ?
C17 C16 C15 . . . 120.0 Y
C17 C16 H16 . . . 120.0 ?
C15 C16 H16 . . . 120.0 ?
C16 C17 C18 . . . 120.0 Y
C16 C17 BR1 . . . 118.0(15) Y
C18 C17 BR1 . . . 122.0(15) Y
C19 C18 C17 . . . 120.0 Y
C19 C18 H18 . . . 120.0 ?
C17 C18 H18 . . . 120.0 ?
C18 C19 C14 . . . 120.0 Y
C18 C19 H19 . . . 120.0 ?
C14 C19 H19 . . . 120.0 ?
C21 C20 N8 . . . 123(3) Y
C21 C20 H20 . . . 118.5 ?
N8 C20 H20 . . . 118.5 ?
C20 C21 C22 . . . 121(3) Y
C20 C21 H21 . . . 119.5 ?
C22 C21 H21 . . . 119.5 ?
C21 C22 C23 . . . 115(3) Y
C21 C22 H22 . . . 122.3 ?
C23 C22 H22 . . . 122.3 ?
C24 C23 C22 . . . 121(3) Y
C24 C23 H23 . . . 119.4 ?
C22 C23 H23 . . . 119.4 ?
C23 C24 N8 . . . 119(2) Y
C23 C24 C25 . . . 125(2) Y
N8 C24 C25 . . . 116(2) Y
N7 C25 C26 . . . 121(2) Y
N7 C25 C24 . . . 113(2) Y
C26 C25 C24 . . . 126(2) Y
C25 C26 C27 . . . 118(2) Y
C25 C26 H26 . . . 120.9 ?
C27 C26 H26 . . . 120.9 ?
C28 C27 C26 . . . 120(2) Y
C28 C27 C35 . . . 119.4(18) Y
C26 C27 C35 . . . 119.9(19) Y
C27 C28 C29 . . . 120(2) Y
C27 C28 H28 . . . 119.9 ?
C29 C28 H28 . . . 119.9 ?
N7 C29 C28 . . . 119(2) Y
N7 C29 C30 . . . 113.6(18) Y
C28 C29 C30 . . . 127.4(19) Y
N6 C30 C31 . . . 119.8(19) Y
N6 C30 C29 . . . 115.1(17) Y
C31 C30 C29 . . . 125.0(18) Y
C32 C31 C30 . . . 119(2) Y
C32 C31 H31 . . . 120.6 ?
C30 C31 H31 . . . 120.6 ?
C31 C32 C33 . . . 122(3) Y
C31 C32 H32 . . . 119.2 ?
C33 C32 H32 . . . 119.2 ?
C34 C33 C32 . . . 116(3) Y
C34 C33 H33 . . . 122.2 ?
C32 C33 H33 . . . 122.2 ?
N6 C34 C33 . . . 128(2) Y
N6 C34 H34 . . . 115.9 ?
C33 C34 H34 . . . 115.9 ?
C36 C35 C40 . . . 120.0 Y
C36 C35 C27 . . . 121.3(12) Y
C40 C35 C27 . . . 118.7(12) Y
C37 C36 C35 . . . 120.0 Y
C37 C36 H36 . . . 120.0 ?
C35 C36 H36 . . . 120.0 ?
C38 C37 C36 . . . 120.0 Y
C38 C37 H37 . . . 120.0 ?
C36 C37 H37 . . . 120.0 ?
C39 C38 C37 . . . 120.0 Y
C39 C38 C43 . . . 123.4(13) Y
C37 C38 C43 . . . 116.5(13) Y
C38 C39 C40 . . . 120.0 Y
C38 C39 H39 . . . 120.0 ?
C40 C39 H39 . . . 120.0 ?
C39 C40 C35 . . . 120.0 Y
C39 C40 H40 . . . 120.0 ?
C35 C40 H40 . . . 120.0 ?
N10 C41 C42 . . . 126(3) Y
N10 C41 C46 . . . 115(3) Y
C42 C41 C46 . . . 119(3) Y
C41 C42 C43 . . . 112(3) Y
C41 C42 H42 . . . 123.8 ?
C43 C42 H42 . . . 123.8 ?
C44 C43 C42 . . . 123(3) Y
C44 C43 C38 . . . 125(3) Y
C42 C43 C38 . . . 111(2) Y
C43 C44 C45 . . . 122(3) Y
C43 C44 H44 . . . 119.2 ?
C45 C44 H44 . . . 119.2 ?
N10 C45 C44 . . . 121(3) Y
N10 C45 C51 . . . 115(3) Y
C44 C45 C51 . . . 123(3) Y
N11 C46 C50 . . . 127(3) Y
N11 C46 C41 . . . 116(3) Y
C50 C46 C41 . . . 117(3) Y
N11 C47 C48 . . . 117(4) Y
N11 C47 H47 . . . 121.6 ?
C48 C47 H47 . . . 121.6 ?
C49 C48 C47 . . . 121(5) Y
C49 C48 H48 . . . 119.3 ?
C47 C48 H48 . . . 119.3 ?
C48 C49 C50 . . . 123(4) Y
C48 C49 H49 . . . 118.7 ?
C50 C49 H49 . . . 118.7 ?
C49 C50 C46 . . . 112(3) Y
C49 C50 H50 . . . 124.0 ?
C46 C50 H50 . . . 124.0 ?
N9 C51 C52 . . . 125(3) Y
N9 C51 C45 . . . 117(3) Y
C52 C51 C45 . . . 118(3) Y
C51 C52 C53 . . . 120(4) Y
C51 C52 H52 . . . 120.0 ?
C53 C52 H52 . . . 120.0 ?
C52 C53 C54 . . . 115(4) Y
C52 C53 H53 . . . 122.4 ?
C54 C53 H53 . . . 122.4 ?
C55 C54 C53 . . . 121(4) Y
C55 C54 H54 . . . 119.5 ?
C53 C54 H54 . . . 119.5 ?
C54 C55 N9 . . . 121(3) Y
C54 C55 H55 . . . 119.7 ?
N9 C55 H55 . . . 119.7 ?
F14 P11 F13 . . . 92.6(11) Y
F14 P11 F15 . . . 87.4(10) Y
F13 P11 F15 . . . 179.6(12) Y
F14 P11 F11 . . . 90.7(10) Y
F13 P11 F11 . . . 89.6(10) Y
F15 P11 F11 . . . 90.0(9) Y
F14 P11 F16 . . . 89.0(11) Y
F13 P11 F16 . . . 89.8(11) Y
F15 P11 F16 . . . 90.6(10) Y
F11 P11 F16 . . . 179.3(11) Y
F14 P11 F12 . . . 178.2(10) Y
F13 P11 F12 . . . 89.1(9) Y
F15 P11 F12 . . . 90.9(8) Y
F11 P11 F12 . . . 90.0(8) Y
F16 P11 F12 . . . 90.3(9) Y
F23 P21 F24 . . . 93(2) Y
F23 P21 F21 . . . 89.6(18) Y
F24 P21 F21 . . . 90(2) Y
F23 P21 F26 . . . 90(2) Y
F24 P21 F26 . . . 88(2) Y
F21 P21 F26 . . . 178(2) Y
F23 P21 F22 . . . 92.0(18) Y
F24 P21 F22 . . . 175(2) Y
F21 P21 F22 . . . 90.6(17) Y
F26 P21 F22 . . . 91(2) Y
F23 P21 F25 . . . 179(2) Y
F24 P21 F25 . . . 86(2) Y
F21 P21 F25 . . . 89.8(19) Y
F26 P21 F25 . . . 91(2) Y
F22 P21 F25 . . . 88.6(19) Y
F33 P31 F33 . . 2_666 179.998(4) Y
F33 P31 F32 . . . 91.1(8) Y
F33 P31 F32 2_666 . . 88.9(8) Y
F33 P31 F32 . . 2_666 88.9(8) Y
F33 P31 F32 2_666 . 2_666 91.1(8) Y
F32 P31 F32 . . 2_666 180.0(4) Y
F33 P31 F31 . . . 88.8(8) Y
F33 P31 F31 2_666 . . 91.2(8) Y
F32 P31 F31 . . . 90.2(8) Y
F32 P31 F31 2_666 . . 89.8(8) Y
F33 P31 F31 . . 2_666 91.2(8) Y
F33 P31 F31 2_666 . 2_666 88.8(8) Y
F32 P31 F31 . . 2_666 89.8(8) Y
F32 P31 F31 2_666 . 2_666 90.2(8) Y
F31 P31 F31 . . 2_666 180.0(3) Y
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N2 RU1 N1 C5 . . . . -1.0(16) Y
N7 RU1 N1 C5 . . . . 179.0(16) Y
N3 RU1 N1 C5 . . . . 3(3) Y
N6 RU1 N1 C5 . . . . -100.6(16) Y
N8 RU1 N1 C5 . . . . 100.4(16) Y
N2 RU1 N1 C1 . . . . -172(2) Y
N7 RU1 N1 C1 . . . . 8(2) Y
N3 RU1 N1 C1 . . . . -167(2) Y
N6 RU1 N1 C1 . . . . 89(2) Y
N8 RU1 N1 C1 . . . . -70(2) Y
N7 RU1 N2 C8 . . . . -2(17) Y
N3 RU1 N2 C8 . . . . -0.3(18) Y
N1 RU1 N2 C8 . . . . 178(2) Y
N6 RU1 N2 C8 . . . . -88.7(19) Y
N8 RU1 N2 C8 . . . . 90.1(18) Y
N7 RU1 N2 C6 . . . . 179(100) Y
N3 RU1 N2 C6 . . . . -178.8(19) Y
N1 RU1 N2 C6 . . . . -0.5(17) Y
N6 RU1 N2 C6 . . . . 92.7(18) Y
N8 RU1 N2 C6 . . . . -88.5(18) Y
N2 RU1 N3 C13 . . . . 180(2) Y
N7 RU1 N3 C13 . . . . -1(2) Y
N1 RU1 N3 C13 . . . . 175.4(19) Y
N6 RU1 N3 C13 . . . . -80(2) Y
N8 RU1 N3 C13 . . . . 79(2) Y
N2 RU1 N3 C9 . . . . 1.5(17) Y
N7 RU1 N3 C9 . . . . -178.6(17) Y
N1 RU1 N3 C9 . . . . -3(3) Y
N6 RU1 N3 C9 . . . . 102.0(18) Y
N8 RU1 N3 C9 . . . . -99.4(18) Y
N2 RU1 N6 C34 . . . . -1(2) Y
N7 RU1 N6 C34 . . . . -178(2) Y
N3 RU1 N6 C34 . . . . -79(2) Y
N1 RU1 N6 C34 . . . . 77.8(19) Y
N8 RU1 N6 C34 . . . . -178.0(18) Y
N2 RU1 N6 C30 . . . . 176.3(13) Y
N7 RU1 N6 C30 . . . . -0.5(13) Y
N3 RU1 N6 C30 . . . . 98.3(13) Y
N1 RU1 N6 C30 . . . . -104.7(13) Y
N8 RU1 N6 C30 . . . . -1(2) Y
N2 RU1 N7 C25 . . . . 90(16) Y
N3 RU1 N7 C25 . . . . 88.4(16) Y
N1 RU1 N7 C25 . . . . -89.9(16) Y
N6 RU1 N7 C25 . . . . 177.4(16) Y
N8 RU1 N7 C25 . . . . -2.6(15) Y
N2 RU1 N7 C29 . . . . -85(16) Y
N3 RU1 N7 C29 . . . . -87.3(16) Y
N1 RU1 N7 C29 . . . . 94.4(15) Y
N6 RU1 N7 C29 . . . . 1.8(14) Y
N8 RU1 N7 C29 . . . . -178.3(15) Y
N2 RU1 N8 C20 . . . . 1.3(18) Y
N7 RU1 N8 C20 . . . . 178.1(18) Y
N3 RU1 N8 C20 . . . . 79.7(18) Y
N1 RU1 N8 C20 . . . . -76.8(17) Y
N6 RU1 N8 C20 . . . . 178.1(17) Y
N2 RU1 N8 C24 . . . . -174.5(13) Y
N7 RU1 N8 C24 . . . . 2.3(13) Y
N3 RU1 N8 C24 . . . . -96.1(14) Y
N1 RU1 N8 C24 . . . . 107.4(13) Y
N6 RU1 N8 C24 . . . . 2(2) Y
C5 N1 C1 C2 . . . . 4(3) Y
RU1 N1 C1 C2 . . . . 174.7(17) Y
N1 C1 C2 C3 . . . . -1(4) Y
C1 C2 C3 C4 . . . . 1(4) Y
C2 C3 C4 C5 . . . . -3(3) Y
C1 N1 C5 C4 . . . . -7(3) Y
RU1 N1 C5 C4 . . . . -178.3(17) Y
C1 N1 C5 C6 . . . . 174(2) Y
RU1 N1 C5 C6 . . . . 2(2) Y
C3 C4 C5 N1 . . . . 6(3) Y
C3 C4 C5 C6 . . . . -174(2) Y
C8 N2 C6 N4 . . . . 0(3) Y
RU1 N2 C6 N4 . . . . 179.0(19) Y
C8 N2 C6 C5 . . . . -177(2) Y
RU1 N2 C6 C5 . . . . 2(3) Y
C7 N4 C6 N2 . . . . -1(4) Y
C7 N4 C6 C5 . . . . 176(2) Y
N1 C5 C6 N2 . . . . -3(3) Y
C4 C5 C6 N2 . . . . 178(2) Y
N1 C5 C6 N4 . . . . -180(2) Y
C4 C5 C6 N4 . . . . 1(4) Y
C8 N5 C7 N4 . . . . -2(4) Y
C8 N5 C7 C14 . . . . -177(2) Y
C6 N4 C7 N5 . . . . 2(4) Y
C6 N4 C7 C14 . . . . 176(2) Y
C6 N2 C8 N5 . . . . -1(3) Y
RU1 N2 C8 N5 . . . . -179.3(19) Y
C6 N2 C8 C9 . . . . 177.7(19) Y
RU1 N2 C8 C9 . . . . -1(3) Y
C7 N5 C8 N2 . . . . 2(4) Y
C7 N5 C8 C9 . . . . -177(2) Y
C13 N3 C9 C10 . . . . 0(4) Y
RU1 N3 C9 C10 . . . . 178.6(17) Y
C13 N3 C9 C8 . . . . 179(2) Y
RU1 N3 C9 C8 . . . . -2(3) Y
N2 C8 C9 N3 . . . . 2(3) Y
N5 C8 C9 N3 . . . . -179(2) Y
N2 C8 C9 C10 . . . . -179(2) Y
N5 C8 C9 C10 . . . . -1(4) Y
N3 C9 C10 C11 . . . . 0(4) Y
C8 C9 C10 C11 . . . . -179(2) Y
C9 C10 C11 C12 . . . . -3(4) Y
C10 C11 C12 C13 . . . . 6(4) Y
C9 N3 C13 C12 . . . . 3(4) Y
RU1 N3 C13 C12 . . . . -175(2) Y
C11 C12 C13 N3 . . . . -6(4) Y
N5 C7 C14 C15 . . . . -178(2) Y
N4 C7 C14 C15 . . . . 8(3) Y
N5 C7 C14 C19 . . . . -3(3) Y
N4 C7 C14 C19 . . . . -177.4(19) Y
C19 C14 C15 C16 . . . . 0.0 Y
C7 C14 C15 C16 . . . . 174(2) Y
C14 C15 C16 C17 . . . . 0.0 Y
C15 C16 C17 C18 . . . . 0.0 Y
C15 C16 C17 BR1 . . . . -180.0(17) Y
C16 C17 C18 C19 . . . . 0.0 Y
BR1 C17 C18 C19 . . . . 180.0(17) Y
C17 C18 C19 C14 . . . . 0.0 Y
C15 C14 C19 C18 . . . . 0.0 Y
C7 C14 C19 C18 . . . . -175(2) Y
C24 N8 C20 C21 . . . . -2(3) Y
RU1 N8 C20 C21 . . . . -178(2) Y
N8 C20 C21 C22 . . . . 1(4) Y
C20 C21 C22 C23 . . . . -2(4) Y
C21 C22 C23 C24 . . . . 3(4) Y
C22 C23 C24 N8 . . . . -4(4) Y
C22 C23 C24 C25 . . . . 178(3) Y
C20 N8 C24 C23 . . . . 4(3) Y
RU1 N8 C24 C23 . . . . 179.6(19) Y
C20 N8 C24 C25 . . . . -178.1(19) Y
RU1 N8 C24 C25 . . . . -2(2) Y
C29 N7 C25 C26 . . . . -1(3) Y
RU1 N7 C25 C26 . . . . -176.8(15) Y
C29 N7 C25 C24 . . . . 177.7(18) Y
RU1 N7 C25 C24 . . . . 2(2) Y
C23 C24 C25 N7 . . . . 178(2) Y
N8 C24 C25 N7 . . . . 0(3) Y
C23 C24 C25 C26 . . . . -3(4) Y
N8 C24 C25 C26 . . . . 179(2) Y
N7 C25 C26 C27 . . . . 0(3) Y
C24 C25 C26 C27 . . . . -179(2) Y
C25 C26 C27 C28 . . . . 3(3) Y
C25 C26 C27 C35 . . . . 174.7(18) Y
C26 C27 C28 C29 . . . . -3(3) Y
C35 C27 C28 C29 . . . . -175.4(18) Y
C25 N7 C29 C28 . . . . 1(3) Y
RU1 N7 C29 C28 . . . . 176.2(14) Y
C25 N7 C29 C30 . . . . -178.3(18) Y
RU1 N7 C29 C30 . . . . -3(2) Y
C27 C28 C29 N7 . . . . 2(3) Y
C27 C28 C29 C30 . . . . -180(2) Y
C34 N6 C30 C31 . . . . 1(3) Y
RU1 N6 C30 C31 . . . . -177.3(15) Y
C34 N6 C30 C29 . . . . 177.2(18) Y
RU1 N6 C30 C29 . . . . -1(2) Y
N7 C29 C30 N6 . . . . 2(2) Y
C28 C29 C30 N6 . . . . -176.6(19) Y
N7 C29 C30 C31 . . . . 178.5(18) Y
C28 C29 C30 C31 . . . . 0(3) Y
N6 C30 C31 C32 . . . . -2(3) Y
C29 C30 C31 C32 . . . . -178(2) Y
C30 C31 C32 C33 . . . . 2(4) Y
C31 C32 C33 C34 . . . . 0(4) Y
C30 N6 C34 C33 . . . . 1(3) Y
RU1 N6 C34 C33 . . . . 178.7(19) Y
C32 C33 C34 N6 . . . . -2(4) Y
C28 C27 C35 C36 . . . . -147.0(17) Y
C26 C27 C35 C36 . . . . 41(2) Y
C28 C27 C35 C40 . . . . 32(2) Y
C26 C27 C35 C40 . . . . -140.0(17) Y
C40 C35 C36 C37 . . . . 0.0 Y
C27 C35 C36 C37 . . . . 179.0(16) Y
C35 C36 C37 C38 . . . . 0.0 Y
C36 C37 C38 C39 . . . . 0.0 Y
C36 C37 C38 C43 . . . . 178.9(16) Y
C37 C38 C39 C40 . . . . 0.0 Y
C43 C38 C39 C40 . . . . -178.9(18) Y
C38 C39 C40 C35 . . . . 0.0 Y
C36 C35 C40 C39 . . . . 0.0 Y
C27 C35 C40 C39 . . . . -179.1(16) Y
C45 N10 C41 C42 . . . . -6(5) Y
C45 N10 C41 C46 . . . . 174(3) Y
N10 C41 C42 C43 . . . . 6(4) Y
C46 C41 C42 C43 . . . . -174(2) Y
C41 C42 C43 C44 . . . . -6(4) Y
C41 C42 C43 C38 . . . . -176(2) Y
C39 C38 C43 C44 . . . . -132(3) Y
C37 C38 C43 C44 . . . . 49(3) Y
C39 C38 C43 C42 . . . . 38(3) Y
C37 C38 C43 C42 . . . . -141.1(17) Y
C42 C43 C44 C45 . . . . 5(5) Y
C38 C43 C44 C45 . . . . 174(2) Y
C41 N10 C45 C44 . . . . 4(5) Y
C41 N10 C45 C51 . . . . 175(3) Y
C43 C44 C45 N10 . . . . -5(5) Y
C43 C44 C45 C51 . . . . -174(3) Y
C47 N11 C46 C50 . . . . -2(6) Y
C47 N11 C46 C41 . . . . -178(3) Y
N10 C41 C46 N11 . . . . 171(3) Y
C42 C41 C46 N11 . . . . -10(4) Y
N10 C41 C46 C50 . . . . -5(4) Y
C42 C41 C46 C50 . . . . 174(3) Y
C46 N11 C47 C48 . . . . -4(6) Y
N11 C47 C48 C49 . . . . 9(7) Y
C47 C48 C49 C50 . . . . -9(7) Y
C48 C49 C50 C46 . . . . 2(5) Y
N11 C46 C50 C49 . . . . 3(5) Y
C41 C46 C50 C49 . . . . 178(3) Y
C55 N9 C51 C52 . . . . 3(5) Y
C55 N9 C51 C45 . . . . -178(3) Y
N10 C45 C51 N9 . . . . -167(3) Y
C44 C45 C51 N9 . . . . 3(4) Y
N10 C45 C51 C52 . . . . 12(4) Y
C44 C45 C51 C52 . . . . -178(3) Y
N9 C51 C52 C53 . . . . -6(6) Y
C45 C51 C52 C53 . . . . 175(3) Y
C51 C52 C53 C54 . . . . 5(6) Y
C52 C53 C54 C55 . . . . -2(6) Y
C53 C54 C55 N9 . . . . -1(5) Y
C51 N9 C55 C54 . . . . 0(5) Y
_diffrn_measured_fraction_theta_max 0.882
_diffrn_reflns_theta_full        54.61
_diffrn_measured_fraction_theta_full 0.882
_refine_diff_density_max         2.052
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.239
_vrf_THETM01_mper22              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.5288
RESPONSE:
The best crystal was chosen and x-ray measurement proceeded at 100K.
The crystal (the largest available from several batches)
was a very small needle(.01 x .03 x .2mm) and diffracted weakly at
high angles.
Larger crystals were not obtainable, and since the crystals of this compound
are no longer available,
we can only rely on the current data set. Only 67% data was observed even if
theta full is 54.6deg.
The current solution is the best we could achieve, given the low current
ratio data/parameters (any use of OMIT, ACTA or SHEL to improve the
completness calculation was thus prevented).
;
_vrf_PLAT201_mper22              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 55
RESPONSE: not enough data to refine all the parameters.
;
_vrf_PLAT220_mper22              
;
PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.2 Ratio
RESPONSE: Disorder or thermal motions cannot be described due
to low number of data (we cannot increase anymore the number of
parameters to be refined than the one in the current description).
;
_vrf_PLAT082_mper22              
;
PROBLEM: High R1 Value .................................. 0.17
RESPONSE: Not enough data to fully refine anisotropically the model
nor describe eventual counter-ions disorder.
;
_vrf_PLAT084_mper22              
;
PROBLEM: High wR2 Value ................................. 0.43
RESPONSE: Not enough data to refine better the model nor describe
eventual counter-ions disorder.
;


data_mper24
_database_code_depnum_ccdc_archive 'CCDC 787467'
#TrackingRef 'final_version_MPER24_jan2013.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C74 H48 Br2 N16 Ru2'
_chemical_formula_sum            'C74 H48 Br2 N16 Ru2'
_chemical_formula_weight         1523.24
_chemical_compound_source        'Synthesized by the authors. See text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   8.7303(8)
_cell_length_b                   47.169(4)
_cell_length_c                   11.5648(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.399(4)
_cell_angle_gamma                90
_cell_volume                     4668.5(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150
_cell_measurement_reflns_used    5494
_cell_measurement_theta_min      4.01
_cell_measurement_theta_max      57.11
_exptl_crystal_description       Chunk
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1524
_exptl_absorpt_coefficient_mu    3.944
_exptl_absorpt_correction_Type   multi-scan
_exptl_absorpt_correction_T_min  0.6416
_exptl_absorpt_correction_T_max  0.8884
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_special_details           
;
X-ray crystallographic data for I were collected from a single crystal
sample, which was mounted on a loop fiber. Data were collected using
a Bruker microstar diffractometer equiped with a Platinum 135 CCD Detector,
a Helios optics and a Kappa goniometer. The crystal-to-detector distance
was 4.0 cm, and the data collection was carried out in 512 x 512 pixel mode.
The initial unit cell parameters were determined by a least-squares fit
of the angular setting of strong reflections, collected by a 10.0 degree
scan in 33 frames over three different parts of the reciprocal space
(99 frames total).
Due to geometrical constraints of the instrument and the use of copper
radiation, we obtain consistently a data completeness lower than 100%
in dependence of the crystal system and the orientation of the mounted crystal,
even with appropriate data collection routines. Typical values for data
completeness range from 83-92% for triclinic, 85-97% for monoclinic and 85-98%
for all other crystal systems.
;
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            24576
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         57.10
_reflns_number_total             6125
_reflns_number_gt                3911
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_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.
Constraints and restraints (such as ISOR, DFIX, DANG, DELU, SIMU) were
used on PF6 and some C atoms of the cation.
;
_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^)+(0.2000P)^2^] 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     SHELXL
_refine_ls_extinction_coef       0.00109(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         6125
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1357
_refine_ls_R_factor_gt           0.1076
_refine_ls_wR_factor_ref         0.3049
_refine_ls_wR_factor_gt          0.2875
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.017 0.000 0.002 770.8 260.3
2 -0.022 0.250 0.895 190.5 33.5
3 -0.008 0.500 0.963 770.8 260.4
4 0.022 0.750 0.549 190.5 33.7
_platon_squeeze_details          
;
Attempts to model disordered solvent and anions molecules
were unsuccessful. PLATON/SQUEEZE was used to correct
the data for the presence of the disordered solvent and anion.
A potential solvent volume of 1924.7 \%A^3^,
41.2 % of the total unit-cell volume, was found.
588 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density,
absorption coefficient, F(000) etc. may be incorrect.
Ref: Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
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
Br1 Br 0.5173(2) 0.61116(4) 0.0234(2) 0.1373(9) Uani 1 1 d . . .
Ru1 Ru 0.51460(8) 0.842129(16) 0.01516(7) 0.0516(4) Uani 1 1 d . . .
N1 N 0.7101(9) 0.85124(17) -0.0553(7) 0.053(2) Uani 1 1 d . . .
N2 N 0.5154(8) 0.88361(16) 0.0135(7) 0.055(2) Uani 1 1 d . . .
N3 N 0.3184(9) 0.85151(17) 0.0867(7) 0.052(2) Uani 1 1 d . . .
N4 N 0.6208(11) 0.92678(19) -0.0359(8) 0.074(3) Uani 1 1 d . . .
N5 N 0.3974(11) 0.9260(2) 0.0524(9) 0.083(3) Uani 1 1 d . . .
N6 N 0.6515(8) 0.83419(15) 0.1778(7) 0.046(2) Uani 1 1 d . . .
N7 N 0.5111(7) 0.80053(17) 0.0129(5) 0.0432(18) Uani 1 1 d . . .
N8 N 0.3929(10) 0.8332(2) -0.1480(8) 0.068(2) Uani 1 1 d . . .
C1 C 0.8106(11) 0.8335(2) -0.0905(8) 0.054(2) Uiso 1 1 d . . .
H1 H 0.7935 0.8137 -0.0835 0.064 Uiso 1 1 calc R . .
C2 C 0.9362(11) 0.84177(19) -0.1358(8) 0.050(2) Uiso 1 1 d . . .
H2 H 1.0067 0.8281 -0.1559 0.060 Uiso 1 1 calc R . .
C3 C 0.9592(13) 0.8707(2) -0.1520(9) 0.071(3) Uiso 1 1 d . . .
H3 H 1.0439 0.8769 -0.1859 0.085 Uiso 1 1 calc R . .
C4 C 0.8577(13) 0.8901(2) -0.1182(9) 0.070(3) Uiso 1 1 d . . .
H4 H 0.8701 0.9100 -0.1278 0.084 Uiso 1 1 calc R . .
C5 C 0.7397(11) 0.8795(2) -0.0707(8) 0.052(2) Uiso 1 1 d . . .
C6 C 0.6164(13) 0.8983(3) -0.0311(9) 0.067(3) Uiso 1 1 d . . .
C7 C 0.5054(12) 0.9397(2) 0.0171(8) 0.061(3) Uiso 1 1 d . . .
C8 C 0.3991(12) 0.8974(2) 0.0533(9) 0.064(3) Uiso 1 1 d . . .
C9 C 0.2917(11) 0.8798(2) 0.0966(8) 0.052(2) Uiso 1 1 d . . .
C10 C 0.1727(12) 0.8902(2) 0.1477(9) 0.066(3) Uiso 1 1 d . . .
H10 H 0.1613 0.9100 0.1591 0.079 Uiso 1 1 calc R . .
C11 C 0.0693(13) 0.8707(3) 0.1823(9) 0.074(3) Uiso 1 1 d . . .
H11 H -0.0162 0.8772 0.2147 0.088 Uiso 1 1 calc R . .
C12 C 0.0911(12) 0.8429(2) 0.1694(9) 0.060(3) Uiso 1 1 d . . .
H12 H 0.0210 0.8296 0.1923 0.073 Uiso 1 1 calc R . .
C13 C 0.2174(11) 0.8335(2) 0.1223(8) 0.050(2) Uiso 1 1 d . . .
H13 H 0.2327 0.8137 0.1152 0.060 Uiso 1 1 calc R . .
C14 C 0.4913(12) 0.9698(3) 0.0053(9) 0.074(3) Uiso 1 1 d . . .
C15 C 0.6112(15) 0.9844(3) -0.0489(11) 0.088(4) Uiso 1 1 d . . .
H15 H 0.6879 0.9743 -0.0801 0.106 Uiso 1 1 calc R . .
C16 C 0.3967(16) 0.9858(3) 0.0509(12) 0.099(4) Uiso 1 1 d . . .
H16 H 0.3252 0.9762 0.0897 0.118 Uiso 1 1 calc R . .
C17 C 0.7146(13) 0.8533(3) 0.2615(9) 0.071(3) Uiso 1 1 d . . .
H17 H 0.6951 0.8730 0.2480 0.085 Uiso 1 1 calc R . .
C18 C 0.8089(12) 0.8442(2) 0.3684(9) 0.065(3) Uiso 1 1 d . . .
H18 H 0.8585 0.8581 0.4227 0.078 Uiso 1 1 calc R . .
C19 C 0.8316(12) 0.8166(2) 0.3965(9) 0.069(3) Uiso 1 1 d . . .
H19 H 0.8906 0.8106 0.4704 0.082 Uiso 1 1 calc R . .
C20 C 0.7600(13) 0.7967(3) 0.3066(9) 0.074(3) Uiso 1 1 d . . .
H20 H 0.7767 0.7770 0.3192 0.089 Uiso 1 1 calc R . .
C21 C 0.6680(11) 0.8061(2) 0.2029(8) 0.052(2) Uiso 1 1 d . . .
C22 C 0.5967(11) 0.7867(2) 0.1050(8) 0.051(2) Uiso 1 1 d . . .
C23 C 0.6009(11) 0.7563(2) 0.1092(8) 0.054(2) Uiso 1 1 d . . .
H23 H 0.6601 0.7468 0.1758 0.065 Uiso 1 1 calc R . .
C24 C 0.5195(11) 0.7412(3) 0.0174(9) 0.063(3) Uiso 1 1 d . . .
C25 C 0.4427(11) 0.7571(2) -0.0841(8) 0.053(2) Uiso 1 1 d . . .
H25 H 0.3933 0.7473 -0.1531 0.063 Uiso 1 1 calc R . .
C26 C 0.4393(10) 0.78613(18) -0.0830(7) 0.039(2) Uiso 1 1 d . . .
C27 C 0.3592(10) 0.8048(2) -0.1733(7) 0.046(2) Uiso 1 1 d . . .
C28 C 0.2720(11) 0.7952(2) -0.2784(8) 0.056(2) Uiso 1 1 d . . .
H28 H 0.2613 0.7756 -0.2954 0.067 Uiso 1 1 calc R . .
C29 C 0.1982(14) 0.8159(3) -0.3610(11) 0.080(3) Uiso 1 1 d . . .
H29 H 0.1275 0.8102 -0.4304 0.097 Uiso 1 1 calc R . .
C30 C 0.2302(13) 0.8440(2) -0.3393(10) 0.068(3) Uiso 1 1 d . . .
H30 H 0.1894 0.8579 -0.3966 0.081 Uiso 1 1 calc R . .
C31 C 0.3203(11) 0.8518(2) -0.2353(8) 0.055(3) Uiso 1 1 d . . .
H31 H 0.3352 0.8715 -0.2207 0.066 Uiso 1 1 calc R . .
C32 C 0.5220(10) 0.7097(2) 0.0123(7) 0.046(2) Uiso 1 1 d . . .
C33 C 0.6141(12) 0.6949(2) 0.1052(9) 0.064(3) Uiso 1 1 d . . .
H33 H 0.6766 0.7052 0.1681 0.077 Uiso 1 1 calc R . .
C34 C 0.6157(13) 0.6653(2) 0.1070(10) 0.071(3) Uiso 1 1 d . . .
H34 H 0.6869 0.6549 0.1640 0.085 Uiso 1 1 calc R . .
C35 C 0.5033(13) 0.6518(3) 0.0174(10) 0.081(4) Uiso 1 1 d . . .
C36 C 0.4175(14) 0.6645(3) -0.0719(11) 0.079(3) Uiso 1 1 d . . .
H36 H 0.3527 0.6546 -0.1346 0.095 Uiso 1 1 calc R . .
C37 C 0.4288(13) 0.6939(2) -0.0678(9) 0.066(3) Uiso 1 1 d . . .
H37 H 0.3623 0.7040 -0.1293 0.080 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
Br1 0.195(2) 0.0481(9) 0.1843(19) 0.0072(9) 0.0758(17) 0.0009(10)
Ru1 0.0481(6) 0.0452(6) 0.0664(6) -0.0019(4) 0.0233(4) 0.0018(4)
N1 0.045(4) 0.051(5) 0.063(5) -0.001(4) 0.015(4) 0.006(4)
N2 0.045(5) 0.039(5) 0.085(6) 0.003(4) 0.025(4) -0.003(4)
N3 0.049(5) 0.054(5) 0.057(5) -0.009(4) 0.022(4) -0.002(4)
N4 0.086(6) 0.046(6) 0.101(7) -0.004(5) 0.046(6) 0.001(5)
N5 0.072(6) 0.066(7) 0.118(8) -0.005(6) 0.038(6) 0.005(5)
N6 0.040(4) 0.040(5) 0.069(5) -0.011(4) 0.036(4) 0.002(3)
N7 0.037(4) 0.058(5) 0.033(4) 0.014(3) 0.002(3) -0.001(3)
N8 0.067(6) 0.075(7) 0.067(6) 0.018(5) 0.020(5) 0.019(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.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Br1 C35 . . 1.921(14) Y
Ru1 N2 . . 1.957(8) Y
Ru1 N7 . . 1.962(8) Y
Ru1 N8 . . 2.018(9) Y
Ru1 N6 . . 2.054(8) Y
Ru1 N1 . . 2.076(7) Y
Ru1 N3 . . 2.092(7) Y
N1 C1 . . 1.333(12) Y
N1 C5 . . 1.375(12) Y
N2 C6 . . 1.305(12) Y
N2 C8 . . 1.361(12) Y
N3 C13 . . 1.346(11) Y
N3 C9 . . 1.366(12) Y
N4 C6 . . 1.346(13) Y
N4 C7 . . 1.417(12) Y
N5 C7 . . 1.274(12) Y
N5 C8 . . 1.349(14) Y
N6 C17 . . 1.359(13) Y
N6 C21 . . 1.359(11) Y
N7 C22 . . 1.344(11) Y
N7 C26 . . 1.345(11) Y
N8 C31 . . 1.391(12) Y
N8 C27 . . 1.393(12) Y
C1 C2 . . 1.362(12) Y
C1 H1 . . 0.9500 ?
C2 C3 . . 1.395(13) Y
C2 H2 . . 0.9500 ?
C3 C4 . . 1.385(14) Y
C3 H3 . . 0.9500 ?
C4 C5 . . 1.356(13) Y
C4 H4 . . 0.9500 ?
C5 C6 . . 1.534(14) Y
C7 C14 . . 1.428(17) Y
C8 C9 . . 1.417(13) Y
C9 C10 . . 1.382(13) Y
C10 C11 . . 1.404(14) Y
C10 H10 . . 0.9500 ?
C11 C12 . . 1.336(14) Y
C11 H11 . . 0.9500 ?
C12 C13 . . 1.394(13) Y
C12 H12 . . 0.9500 ?
C13 H13 . . 0.9500 ?
C14 C16 . . 1.305(16) Y
C14 C15 . . 1.492(15) Y
C15 C16 . 3_675 1.41(2) Y
C15 H15 . . 0.9500 ?
C16 C15 . 3_675 1.41(2) Y
C16 H16 . . 0.9500 ?
C17 C18 . . 1.410(15) Y
C17 H17 . . 0.9500 ?
C18 C19 . . 1.348(14) Y
C18 H18 . . 0.9500 ?
C19 C20 . . 1.447(15) Y
C19 H19 . . 0.9500 ?
C20 C21 . . 1.378(14) Y
C20 H20 . . 0.9500 ?
C21 C22 . . 1.492(13) Y
C22 C23 . . 1.436(13) Y
C23 C24 . . 1.357(14) Y
C23 H23 . . 0.9500 ?
C24 C25 . . 1.443(14) Y
C24 C32 . . 1.486(16) Y
C25 C26 . . 1.370(12) Y
C25 H25 . . 0.9500 ?
C26 C27 . . 1.437(12) Y
C27 C28 . . 1.377(12) Y
C28 C29 . . 1.426(15) Y
C28 H28 . . 0.9500 ?
C29 C30 . . 1.369(15) Y
C29 H29 . . 0.9500 ?
C30 C31 . . 1.351(14) Y
C30 H30 . . 0.9500 ?
C31 H31 . . 0.9500 ?
C32 C37 . . 1.332(14) Y
C32 C33 . . 1.394(13) Y
C33 C34 . . 1.397(14) Y
C33 H33 . . 0.9500 ?
C34 C35 . . 1.429(16) Y
C34 H34 . . 0.9500 ?
C35 C36 . . 1.296(17) Y
C36 C37 . . 1.394(15) Y
C36 H36 . . 0.9500 ?
C37 H37 . . 0.9500 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 RU1 N7 . . . 178.6(3) Y
N2 RU1 N8 . . . 101.6(3) Y
N7 RU1 N8 . . . 77.0(3) Y
N2 RU1 N6 . . . 100.9(3) Y
N7 RU1 N6 . . . 80.5(3) Y
N8 RU1 N6 . . . 157.2(3) Y
N2 RU1 N1 . . . 77.6(3) Y
N7 RU1 N1 . . . 102.3(3) Y
N8 RU1 N1 . . . 89.8(3) Y
N6 RU1 N1 . . . 91.3(3) Y
N2 RU1 N3 . . . 78.3(3) Y
N7 RU1 N3 . . . 101.8(3) Y
N8 RU1 N3 . . . 95.3(3) Y
N6 RU1 N3 . . . 92.9(3) Y
N1 RU1 N3 . . . 155.8(3) Y
C1 N1 C5 . . . 114.6(8) Y
C1 N1 RU1 . . . 129.2(7) Y
C5 N1 RU1 . . . 116.2(6) Y
C6 N2 C8 . . . 119.1(9) Y
C6 N2 RU1 . . . 122.6(7) Y
C8 N2 RU1 . . . 118.2(6) Y
C13 N3 C9 . . . 117.3(8) Y
C13 N3 RU1 . . . 128.7(7) Y
C9 N3 RU1 . . . 114.0(6) Y
C6 N4 C7 . . . 112.5(9) Y
C7 N5 C8 . . . 120.0(10) Y
C17 N6 C21 . . . 119.1(9) Y
C17 N6 RU1 . . . 127.7(7) Y
C21 N6 RU1 . . . 113.0(6) Y
C22 N7 C26 . . . 120.2(8) Y
C22 N7 RU1 . . . 118.1(6) Y
C26 N7 RU1 . . . 121.3(6) Y
C31 N8 C27 . . . 114.0(9) Y
C31 N8 RU1 . . . 128.9(8) Y
C27 N8 RU1 . . . 116.5(6) Y
N1 C1 C2 . . . 124.4(9) Y
N1 C1 H1 . . . 117.8 ?
C2 C1 H1 . . . 117.8 ?
C1 C2 C3 . . . 118.7(9) Y
C1 C2 H2 . . . 120.7 ?
C3 C2 H2 . . . 120.7 ?
C4 C3 C2 . . . 119.5(10) Y
C4 C3 H3 . . . 120.2 ?
C2 C3 H3 . . . 120.2 ?
C5 C4 C3 . . . 116.6(11) Y
C5 C4 H4 . . . 121.7 ?
C3 C4 H4 . . . 121.7 ?
C4 C5 N1 . . . 126.1(9) Y
C4 C5 C6 . . . 122.7(10) Y
N1 C5 C6 . . . 111.1(8) Y
N2 C6 N4 . . . 125.0(10) Y
N2 C6 C5 . . . 112.4(10) Y
N4 C6 C5 . . . 122.5(9) Y
N5 C7 N4 . . . 123.8(11) Y
N5 C7 C14 . . . 118.6(10) Y
N4 C7 C14 . . . 116.2(9) Y
N5 C8 N2 . . . 119.0(9) Y
N5 C8 C9 . . . 125.5(10) Y
N2 C8 C9 . . . 115.4(10) Y
N3 C9 C10 . . . 122.6(9) Y
N3 C9 C8 . . . 114.1(8) Y
C10 C9 C8 . . . 123.4(10) Y
C9 C10 C11 . . . 117.9(11) Y
C9 C10 H10 . . . 121.0 ?
C11 C10 H10 . . . 121.0 ?
C12 C11 C10 . . . 119.9(11) Y
C12 C11 H11 . . . 120.0 ?
C10 C11 H11 . . . 120.0 ?
C11 C12 C13 . . . 119.7(10) Y
C11 C12 H12 . . . 120.1 ?
C13 C12 H12 . . . 120.1 ?
N3 C13 C12 . . . 122.4(9) Y
N3 C13 H13 . . . 118.8 ?
C12 C13 H13 . . . 118.8 ?
C16 C14 C7 . . . 125.8(12) Y
C16 C14 C15 . . . 117.1(14) Y
C7 C14 C15 . . . 116.5(10) Y
C16 C15 C14 3_675 . . 115.7(10) Y
C16 C15 H15 3_675 . . 122.1 ?
C14 C15 H15 . . . 122.1 ?
C14 C16 C15 . . 3_675 127.1(13) Y
C14 C16 H16 . . . 116.4 ?
C15 C16 H16 3_675 . . 116.4 ?
N6 C17 C18 . . . 120.4(11) Y
N6 C17 H17 . . . 119.8 ?
C18 C17 H17 . . . 119.8 ?
C19 C18 C17 . . . 122.6(11) Y
C19 C18 H18 . . . 118.7 ?
C17 C18 H18 . . . 118.7 ?
C18 C19 C20 . . . 115.5(11) Y
C18 C19 H19 . . . 122.3 ?
C20 C19 H19 . . . 122.3 ?
C21 C20 C19 . . . 120.9(11) Y
C21 C20 H20 . . . 119.6 ?
C19 C20 H20 . . . 119.6 ?
N6 C21 C20 . . . 121.2(9) Y
N6 C21 C22 . . . 115.2(8) Y
C20 C21 C22 . . . 123.2(10) Y
N7 C22 C23 . . . 121.3(8) Y
N7 C22 C21 . . . 112.8(9) Y
C23 C22 C21 . . . 125.6(8) Y
C24 C23 C22 . . . 119.5(9) Y
C24 C23 H23 . . . 120.3 ?
C22 C23 H23 . . . 120.3 ?
C23 C24 C25 . . . 116.8(11) Y
C23 C24 C32 . . . 123.1(9) Y
C25 C24 C32 . . . 119.8(9) Y
C26 C25 C24 . . . 121.4(9) Y
C26 C25 H25 . . . 119.3 ?
C24 C25 H25 . . . 119.3 ?
N7 C26 C25 . . . 120.4(8) Y
N7 C26 C27 . . . 111.7(8) Y
C25 C26 C27 . . . 127.8(8) Y
C28 C27 N8 . . . 123.8(9) Y
C28 C27 C26 . . . 123.2(9) Y
N8 C27 C26 . . . 112.7(8) Y
C27 C28 C29 . . . 117.8(10) Y
C27 C28 H28 . . . 121.1 ?
C29 C28 H28 . . . 121.1 ?
C30 C29 C28 . . . 119.4(11) Y
C30 C29 H29 . . . 120.3 ?
C28 C29 H29 . . . 120.3 ?
C31 C30 C29 . . . 119.2(11) Y
C31 C30 H30 . . . 120.4 ?
C29 C30 H30 . . . 120.4 ?
C30 C31 N8 . . . 125.3(10) Y
C30 C31 H31 . . . 117.4 ?
N8 C31 H31 . . . 117.4 ?
C37 C32 C33 . . . 116.0(10) Y
C37 C32 C24 . . . 125.0(9) Y
C33 C32 C24 . . . 118.6(8) Y
C32 C33 C34 . . . 120.9(10) Y
C32 C33 H33 . . . 119.6 ?
C34 C33 H33 . . . 119.6 ?
C33 C34 C35 . . . 115.6(11) Y
C33 C34 H34 . . . 122.2 ?
C35 C34 H34 . . . 122.2 ?
C36 C35 C34 . . . 125.3(14) Y
C36 C35 BR1 . . . 120.8(11) Y
C34 C35 BR1 . . . 112.9(9) Y
C35 C36 C37 . . . 114.0(12) Y
C35 C36 H36 . . . 123.0 ?
C37 C36 H36 . . . 123.0 ?
C32 C37 C36 . . . 127.5(11) Y
C32 C37 H37 . . . 116.2 ?
C36 C37 H37 . . . 116.2 ?
_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        57.10
_diffrn_measured_fraction_theta_full 0.968
_refine_diff_density_max         2.198
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.187
_vrf_PLAT201_mper24              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 37
RESPONSE: not enough data to refine all the parameters.
;
_vrf_PLAT606_mper24              
;
PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure !
RESPONSE: Attempts to model disordered anions (NO3) and solvent molecules
were unsuccessful. A potential volume of 1924.7A^3^,
41.2 % of the total unit-cell volume, was found.
588 electrons per unit cell worth of scattering were located
in the void. PLATON/SQUEEZE was used to correct
the data for the presence of the anions and disordered solvent.
;
_vrf_THETM01_mper24              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
Calculated sin(theta_max)/wavelength = 0.5446
RESPONSE:
The best crystal was chosen and x-ray measurement proceeded at 150K.
The crystal (the largest available from several batches)
was very small (all dimensions smaller than 0.1 mm) and diffracted weakly at
high angles.
Larger crystals were not obtainable, and since the crystals of this compound
are no longer available,
we can only rely on the current data set. Only 63% data was observed even if
theta full is 57deg.
The current solution is the best we could achieve, given the low current
ratio data/parameters (any use of OMIT, ACTA or SHEL to improve the
completness calculation was thus prevented).
;
_vrf_PLAT082_mper24              
;
PROBLEM: High R1 Value .................................. 0.11
RESPONSE: Not enough data to fully refine anisotropically the model
nor describe eventual counter-ions disorder.
;
_vrf_PLAT084_mper24              
;
PROBLEM: High wR2 Value ................................. 0.30
RESPONSE: Not enough data to refine better the model nor describe
eventual counter-ions disorder.
;
_vrf_PLAT029_mper24              
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.968
RESPONSE: idem THETM01.
;