#------------------------------------------------------------------------------ #$Date: 2021-10-29 02:52:10 +0300 (Fri, 29 Oct 2021) $ #$Revision: 270127 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708637.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7708637 loop_ _publ_author_name 'Biancalana, Lorenzo' 'Zanda, Emanuele' 'Hadiji, Mouna' 'Zacchini, Stefano' 'Pratesi, Alessandro' 'Pampaloni, Guido' 'Dyson, Paul J.' 'Marchetti, Fabio' _publ_section_title ; Role of the (pseudo)halido ligand in ruthenium(II) p-cymene \a-amino acid complexes in speciation, protein reactivity and cytotoxicity. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt03274g _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_sum 'C15 H22 Br N O3 Ru' _chemical_formula_weight 445.31 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-08-23 deposited with the CCDC. 2021-10-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.108(9) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.8687(15) _cell_length_b 23.288(5) _cell_length_c 10.082(2) _cell_measurement_reflns_used 9682 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.7715 _cell_measurement_theta_min 2.207 _cell_volume 1612.4(6) _computing_cell_refinement 'APEX3 (Bruker AXS, 2015)' _computing_data_collection 'APEX3 (Bruker AXS, 2015)' _computing_data_reduction 'SAINT (Bruker AXS, 2015)' _computing_molecular_graphics 'ORTEPIII (Johnson, 1996)' _computing_publication_material 'XCIF 2014/2 (Bruker AXS, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_device_type 'PHOTON100 area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_unetI/netI 0.1012 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10106 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 25.005 _diffrn_reflns_theta_max 25.005 _diffrn_reflns_theta_min 2.020 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 3.459 _exptl_absorpt_correction_T_max 0.7467 _exptl_absorpt_correction_T_min 0.5070 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Data were corrected for Lorentz polarization and absorption effects (empirical absorption correction SADABS). R(int) = 0.1655 (selected reflections only, before parameter refinement) R(int) = 0.0905 (selected reflections only, after parameter refinement) ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.834 _exptl_crystal_description plate _exptl_crystal_F_000 888 _exptl_crystal_size_max 0.190 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _refine_diff_density_max 2.825 _refine_diff_density_min -2.798 _refine_diff_density_rms 0.268 _refine_ls_abs_structure_details ; Twinning involves inversion, so Flack parameter cannot be determined ; _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 384 _refine_ls_number_reflns 5346 _refine_ls_number_restraints 472 _refine_ls_restrained_S_all 1.111 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0723 _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/[\s^2^(Fo^2^)+(0.1251P)^2^+17.2487P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1959 _refine_ls_wR_factor_ref 0.2044 _reflns_Friedel_coverage 0.948 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.959 _reflns_number_gt 5084 _reflns_number_total 5346 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03274g2.cif _cod_data_source_block 2b _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7708637 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.559 _shelx_estimated_absorpt_t_max 0.702 _shelx_res_file ; p21_a.res created by SHELXL-2014/7 TITL p21_a.res in P2(1) CELL 0.71073 6.8687 23.2876 10.0821 90.000 91.108 90.000 ZERR 4.000 0.0015 0.0047 0.0023 0.000 0.009 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H Br N O Ru UNIT 60 88 4 4 12 4 OMIT -3 50.01 l.s. 16 ACTA BOND $H conf FMAP 2 PLAN 20 size 0.19 0.16 0.11 twin 1 0 0 0 -1 0 0 0 -1 -4 TEMP -173 simu .01 $c $n $o $ru isor .01 $c $o $n isor .001 ru1 ru2 isor .003 c12 c14 c20 n2 c54 eqiv $1 1-x, 0.5+y, 2-z eqiv $2 1-x, -0.5+y, 1-z dfix 1.9 0.1 h6 o1_$2 dfix 1.9 h3 o5_$1 dfix 1.43 c4 o3 htab EQIV $3 x+1, y, z EQIV $4 -x+1, y-1/2, -z+2 HTAB O3 O5_$1 HTAB N1 O5_$1 HTAB C3 O4_$1 HTAB C5 Br1_$3 HTAB C53 Br1_$4 HTAB O6 O1_$2 HTAB N2 O2_$2 WGHT 0.125100 17.248701 BASF 0.35234 0.07213 0.06089 FVAR 0.39329 RU1 6 0.840207 0.548513 0.856132 11.00000 0.00723 0.00375 = 0.02938 -0.00080 0.00208 0.00092 BR1 3 0.568981 0.553408 1.021283 11.00000 0.00849 0.01041 = 0.04425 -0.00129 0.00605 -0.00150 O1 5 0.701035 0.614652 0.747490 11.00000 0.00971 0.01448 = 0.01970 0.00126 0.00220 0.00241 O2 5 0.598154 0.705742 0.760666 11.00000 0.01957 0.01097 = 0.03100 0.00430 0.01761 -0.00120 O3 5 1.209108 0.708701 1.095497 11.00000 0.01547 0.01298 = 0.04300 -0.00376 0.00744 -0.01065 AFIX 147 H3 2 1.134495 0.687285 1.138238 11.00000 -1.50000 AFIX 0 N1 4 0.951571 0.624664 0.953717 11.00000 0.01048 0.00934 = 0.02826 0.00087 0.00502 0.00180 AFIX 13 H1 2 0.968429 0.616722 1.050735 11.00000 -1.20000 AFIX 0 C1 1 0.696342 0.664675 0.801651 11.00000 0.01268 0.01110 = 0.02361 0.00358 0.00292 0.00199 C2 1 0.805011 0.674640 0.934044 11.00000 0.01593 0.01246 = 0.02871 0.00351 0.00270 0.00468 AFIX 13 H2 2 0.709342 0.673865 1.007537 11.00000 -1.20000 AFIX 0 C3 1 0.928863 0.727932 0.947365 11.00000 0.01712 0.01251 = 0.02943 -0.00073 -0.00354 0.00093 AFIX 23 H3A 2 0.894608 0.749331 1.028489 11.00000 -1.20000 H3B 2 0.907024 0.753353 0.869792 11.00000 -1.20000 AFIX 0 C4 1 1.151572 0.708038 0.955688 11.00000 0.01533 0.01418 = 0.02892 0.00074 0.00832 -0.00509 AFIX 13 H4 2 1.237353 0.732902 0.900912 11.00000 -1.20000 AFIX 0 C5 1 1.136971 0.647683 0.901892 11.00000 0.01500 0.01342 = 0.03012 -0.00177 0.00886 0.00034 AFIX 23 H5A 2 1.134193 0.647936 0.803682 11.00000 -1.20000 H5B 2 1.248859 0.624206 0.933249 11.00000 -1.20000 AFIX 0 C11 1 0.951432 0.513354 0.678293 11.00000 0.01356 0.00912 = 0.02476 0.00296 0.00478 0.00126 C12 1 1.113557 0.520758 0.769463 11.00000 0.01114 0.01007 = 0.01471 -0.00064 0.00306 0.00099 AFIX 13 H12 2 1.217180 0.549563 0.750115 11.00000 -1.20000 AFIX 0 C13 1 1.095110 0.498558 0.900436 11.00000 0.01015 0.00575 = 0.02116 0.00329 0.00119 -0.00221 AFIX 13 H13 2 1.187443 0.512477 0.971286 11.00000 -1.20000 AFIX 0 C14 1 0.938860 0.463343 0.937205 11.00000 0.01093 0.01062 = 0.01561 0.00036 0.00019 0.00180 C15 1 0.782360 0.456958 0.842231 11.00000 0.00900 0.00563 = 0.02485 -0.00553 -0.00543 -0.00044 AFIX 13 H15 2 0.654620 0.442624 0.874765 11.00000 -1.20000 AFIX 0 C16 1 0.788895 0.478559 0.708387 11.00000 0.01359 0.01281 = 0.02382 -0.00238 0.00066 0.00215 AFIX 13 H16 2 0.669826 0.478482 0.649723 11.00000 -1.20000 AFIX 0 C17 1 0.954469 0.541117 0.539280 11.00000 0.01836 0.01465 = 0.04819 0.00912 0.00988 -0.00578 AFIX 33 H17A 2 1.073411 0.563949 0.530689 11.00000 -1.50000 H17B 2 0.951438 0.510981 0.471425 11.00000 -1.50000 H17C 2 0.840486 0.566042 0.527490 11.00000 -1.50000 AFIX 0 C18 1 0.925085 0.443287 1.074698 11.00000 0.01129 0.01640 = 0.02896 -0.00051 -0.00135 0.00626 AFIX 13 H18 2 0.782765 0.439272 1.091641 11.00000 -1.20000 AFIX 0 C19 1 1.006059 0.478505 1.187008 11.00000 0.02123 0.01878 = 0.02893 0.00029 0.00260 0.00310 AFIX 33 H19A 2 0.983973 0.458602 1.271029 11.00000 -1.50000 H19B 2 1.146162 0.484015 1.175467 11.00000 -1.50000 H19C 2 0.941065 0.515960 1.188073 11.00000 -1.50000 AFIX 0 C20 1 1.010257 0.381014 1.081139 11.00000 0.01703 0.01604 = 0.02591 0.00247 -0.00587 0.00516 AFIX 33 H20A 2 1.002929 0.366466 1.172115 11.00000 -1.50000 H20B 2 0.934736 0.355956 1.021389 11.00000 -1.50000 H20C 2 1.146452 0.381614 1.053948 11.00000 -1.50000 AFIX 0 C51 1 0.161122 0.190269 0.692766 11.00000 0.01049 0.01435 = 0.03254 0.00021 0.00205 0.00218 C52 1 0.309382 0.170164 0.590366 11.00000 0.01109 0.00985 = 0.02240 0.00088 -0.00143 -0.00275 AFIX 13 H52 2 0.234574 0.150879 0.516875 11.00000 -1.20000 AFIX 0 C53 1 0.449357 0.126279 0.648426 11.00000 0.01542 0.01904 = 0.03015 0.00257 -0.00444 0.00386 AFIX 23 H53A 2 0.392767 0.087191 0.645505 11.00000 -1.20000 H53B 2 0.486434 0.135850 0.741194 11.00000 -1.20000 AFIX 0 C54 1 0.622785 0.131269 0.557202 11.00000 0.01452 0.01664 = 0.02003 0.00110 -0.00101 0.00143 AFIX 13 H54 2 0.741619 0.118195 0.607491 11.00000 -1.20000 AFIX 0 C55 1 0.638291 0.196923 0.536798 11.00000 0.01487 0.01696 = 0.02239 -0.00122 0.00065 -0.00133 AFIX 23 H55A 2 0.709216 0.215309 0.611925 11.00000 -1.20000 H55B 2 0.705426 0.206062 0.453390 11.00000 -1.20000 AFIX 0 C61 1 0.468125 0.335746 0.779450 11.00000 0.01857 0.01622 = 0.02682 -0.00503 0.00499 0.00208 C62 1 0.622320 0.325448 0.702648 11.00000 0.01076 0.01485 = 0.02481 -0.00439 -0.00376 -0.00188 AFIX 13 H62 2 0.717355 0.295143 0.731244 11.00000 -1.20000 AFIX 0 C63 1 0.614108 0.342461 0.559090 11.00000 0.01718 0.01042 = 0.02534 -0.00170 0.00899 -0.00212 AFIX 13 H63 2 0.707175 0.326270 0.493828 11.00000 -1.20000 AFIX 0 C64 1 0.449911 0.376739 0.517003 11.00000 0.01706 0.01473 = 0.03132 0.00079 0.00443 -0.00024 C65 1 0.313135 0.390822 0.609034 11.00000 0.01836 0.01375 = 0.03183 -0.00220 0.00308 -0.00166 AFIX 13 H65 2 0.187293 0.407132 0.574649 11.00000 -1.20000 AFIX 0 C66 1 0.317665 0.371175 0.740915 11.00000 0.01801 0.01020 = 0.02327 0.00094 0.00152 -0.00101 AFIX 13 H66 2 0.200697 0.375378 0.797648 11.00000 -1.20000 AFIX 0 C67 1 0.481364 0.314359 0.922074 11.00000 0.02556 0.01982 = 0.02000 -0.00515 0.00553 -0.00335 AFIX 33 H67A 2 0.361451 0.324269 0.967958 11.00000 -1.50000 H67B 2 0.498393 0.272577 0.922450 11.00000 -1.50000 H67C 2 0.592766 0.332466 0.967598 11.00000 -1.50000 AFIX 0 C68 1 0.431707 0.398476 0.372147 11.00000 0.02268 0.02325 = 0.03059 -0.00325 -0.00015 -0.00055 AFIX 13 H68 2 0.290088 0.400399 0.347634 11.00000 -1.20000 AFIX 0 C69 1 0.531309 0.357908 0.272941 11.00000 0.03185 0.03268 = 0.02278 -0.01021 0.00999 -0.00411 AFIX 33 H69A 2 0.473032 0.319592 0.278484 11.00000 -1.50000 H69B 2 0.513327 0.372915 0.182723 11.00000 -1.50000 H69C 2 0.670743 0.355486 0.294696 11.00000 -1.50000 AFIX 0 C70 1 0.512252 0.459497 0.371311 11.00000 0.02826 0.03223 = 0.04146 0.00281 0.00712 -0.01192 AFIX 33 H70A 2 0.443134 0.482868 0.436109 11.00000 -1.50000 H70B 2 0.651399 0.458704 0.394629 11.00000 -1.50000 H70C 2 0.493983 0.476133 0.282657 11.00000 -1.50000 AFIX 0 RU2 6 0.342877 0.298144 0.606258 11.00000 0.00630 0.00461 = 0.02977 -0.00161 0.00407 0.00049 BR2 3 0.066049 0.288358 0.432013 11.00000 0.00927 0.00991 = 0.04428 -0.00111 0.00399 0.00028 O4 5 0.176678 0.244811 0.723129 11.00000 0.01839 0.01129 = 0.03398 0.00000 0.00665 0.00309 O5 5 0.060968 0.156363 0.751269 11.00000 0.00861 0.00356 = 0.03568 0.00053 0.00457 -0.00160 O6 5 0.605940 0.098645 0.442130 11.00000 0.02100 0.01780 = 0.05486 -0.00503 0.00859 0.01354 AFIX 147 H6 2 0.516018 0.111953 0.393564 11.00000 -1.50000 AFIX 0 N2 4 0.425081 0.216452 0.530276 11.00000 0.00688 0.00872 = 0.01283 -0.00120 -0.00167 0.00045 AFIX 13 H2A 2 0.387311 0.216891 0.433993 11.00000 -1.20000 AFIX 0 HKLF 4 REM p21_a.res in P2(1) REM R1 = 0.0723 for 5084 Fo > 4sig(Fo) and 0.0770 for all 5346 data REM 384 parameters refined using 472 restraints END WGHT 0.1252 17.2488 REM Instructions for potential hydrogen bonds HTAB O3 O5_$1 HTAB N1 O5_$1 HTAB C3 O4_$1 HTAB C5 Br1_$3 HTAB C53 Br1_$4 HTAB O6 O1_$2 HTAB N2 O2_$2 REM Highest difference peak 2.825, deepest hole -2.798, 1-sigma level 0.268 Q1 1 0.3453 0.2957 0.7340 11.00000 0.05 2.83 Q2 1 0.8551 0.5485 1.0015 11.00000 0.05 2.69 Q3 1 0.3335 0.2999 0.4613 11.00000 0.05 2.09 Q4 1 0.0723 0.2913 0.5726 11.00000 0.05 2.05 Q5 1 0.8194 0.5496 0.7050 11.00000 0.05 2.00 Q6 1 0.8518 0.5494 0.7339 11.00000 0.05 1.95 Q7 1 0.6023 0.5548 1.1740 11.00000 0.05 1.82 Q8 1 0.0672 0.2875 0.3204 11.00000 0.05 1.82 Q9 1 0.2457 0.2952 0.3464 11.00000 0.05 1.36 Q10 1 0.5472 0.5507 0.8827 11.00000 0.05 1.13 Q11 1 0.9377 0.5492 1.1248 11.00000 0.05 1.08 Q12 1 0.9313 0.7696 0.7534 11.00000 0.05 1.06 Q13 1 0.7978 0.8011 0.7579 11.00000 0.05 1.05 Q14 1 1.4525 0.5594 0.7537 11.00000 0.05 0.99 Q15 1 0.7572 0.5450 1.1062 11.00000 0.05 0.93 Q16 1 0.2931 0.0651 0.7183 11.00000 0.05 0.90 Q17 1 0.8527 0.7591 1.1182 11.00000 0.05 0.85 Q18 1 0.3546 0.0506 0.7015 11.00000 0.05 0.83 Q19 1 1.0756 0.5545 0.6559 11.00000 0.05 0.83 Q20 1 0.1890 0.3019 0.6416 11.00000 0.05 0.83 ; _shelx_res_checksum 71748 _shelx_hkl_file ; 1 0 0 13.40 2.70 1 0 0 17.10 2.60 1 0 0 18.70 3.50 -1 0 0 14.10 2.70 -1 0 0 14.10 2.40 2 0 0 904.51 83.79 2 0 0 916.91 84.39 -2 0 0 790.62 83.59 -2 0 0 872.81 84.29 3 0 0 6.60 3.60 3 0 0 9.20 4.20 4 0 0 1433.06 139.59 5 0 0 32.30 8.60 6 0 0 104.39 17.20 7 0 0 19.30 9.10 8 0 0 918.51 92.59 -8 0 0 863.41 88.69 9 0 0 48.40 16.00 -9 0 0 71.49 21.10 10 0 0 538.25 60.59 -10 0 0 489.55 55.29 -10 0 1 100.59 19.60 10 0 -1 79.69 21.30 -9 0 1 22.30 17.30 9 0 -1 8.40 9.80 -8 0 1 374.56 41.40 8 0 -1 396.36 44.90 -7 0 1 1196.38 121.99 7 0 -1 1302.27 125.19 6 0 -1 50.89 12.50 -5 0 1 353.46 36.80 5 0 -1 347.77 38.10 -4 0 1 199.08 22.00 4 0 -1 198.68 22.80 3 0 -1 3930.71 376.36 -2 0 1 863.71 98.49 -2 0 1 1157.18 98.39 2 0 -1 1046.70 98.89 -1 0 1 1159.08 112.79 -1 0 1 1218.88 112.89 1 0 -1 1183.18 113.09 1 0 -1 1160.08 112.79 0 0 1 17.90 2.10 0 0 1 24.30 3.20 0 0 -1 21.00 2.70 0 0 -1 16.80 2.20 1 0 1 1304.87 128.99 1 0 1 1390.76 129.19 2 0 1 1028.70 90.29 2 0 1 931.21 89.79 -2 0 -1 847.42 89.59 -2 0 -1 919.01 90.09 3 0 1 3452.25 341.57 3 0 1 3690.53 342.17 4 0 1 188.68 21.00 4 0 1 177.28 20.90 5 0 1 314.77 34.50 5 0 1 314.67 34.40 6 0 1 98.89 18.20 6 0 1 61.89 17.20 7 0 1 1167.08 125.89 -7 0 -1 1337.57 123.09 -7 0 -1 1262.67 123.29 8 0 1 418.26 44.60 -8 0 -1 340.07 39.10 -8 0 -1 377.76 40.60 9 0 1 1.20 9.80 -9 0 -1 29.30 17.60 10 0 1 115.19 25.80 -10 0 -1 108.09 21.70 10 0 -2 49.50 16.60 9 0 -2 150.88 25.40 -8 0 2 202.68 26.00 8 0 -2 225.78 29.60 7 0 -2 532.35 57.69 -6 0 2 536.95 57.29 6 0 -2 614.24 63.89 -5 0 2 2195.08 211.48 5 0 -2 2199.48 213.48 4 0 -2 242.48 27.30 -3 0 2 575.94 131.79 3 0 -2 628.84 133.29 -2 0 2 1051.09 97.09 2 0 -2 966.80 96.89 -1 0 2 1094.99 101.49 1 0 -2 1016.70 101.49 0 0 2 1048.50 99.99 0 0 2 1102.79 101.19 0 0 -2 990.60 101.09 1 0 2 2284.27 231.08 -1 0 -2 2349.46 231.18 -1 0 -2 2599.54 230.18 2 0 2 1478.95 139.39 -2 0 -2 1407.46 138.09 3 0 2 631.44 62.69 4 0 2 218.58 24.80 5 0 2 2085.89 202.78 6 0 2 547.05 56.59 -6 0 -2 523.75 53.59 7 0 2 512.25 53.09 -7 0 -2 457.45 48.80 8 0 2 209.88 28.50 -8 0 -2 185.98 24.10 9 0 2 166.68 26.80 -9 0 -2 149.59 21.90 -9 0 -2 133.19 21.90 10 0 2 108.19 26.40 9 0 -3 254.17 35.20 -8 0 3 111.59 18.00 -7 0 3 26.90 14.20 7 0 -3 5.10 8.70 6 0 -3 278.97 204.58 6 0 -3 217.78 139.09 5 0 -3 317.17 35.90 4 0 -3 55.19 11.70 -3 0 3 391.96 39.00 -2 0 3 4260.67 380.36 2 0 -3 3701.23 380.56 -1 0 3 1495.55 141.49 -1 0 3 1505.35 143.89 1 0 -3 1420.46 141.49 0 0 3 12.80 3.80 0 0 3 5.70 3.30 0 0 -3 12.20 3.90 0 0 -3 15.30 4.20 0 0 -3 6.20 4.90 1 0 3 1402.46 133.49 -1 0 -3 1530.75 133.29 -1 0 -3 1243.98 133.29 -2 0 -3 4795.12 457.15 -3 0 -3 465.95 45.90 4 0 3 23.80 7.80 -4 0 -3 38.90 8.00 5 0 3 291.97 36.50 -5 0 -3 360.76 34.60 -6 0 -3 154.28 20.90 7 0 3 31.00 12.40 -7 0 -3 10.60 8.90 8 0 3 191.78 27.70 -8 0 -3 158.98 22.10 9 0 3 311.77 41.00 -9 0 -3 273.37 33.70 -9 0 4 48.60 20.90 9 0 -4 53.69 16.80 8 0 -4 191.38 29.10 7 0 -4 79.89 17.80 6 0 -4 619.24 65.49 5 0 -4 10.30 9.50 -4 0 4 328.17 36.90 4 0 -4 407.26 39.70 -3 0 4 480.35 44.20 3 0 -4 391.86 44.90 -1 0 4 540.65 59.49 1 0 -4 677.83 59.59 0 0 -4 83.79 10.70 1 0 4 519.65 52.89 -1 0 -4 560.54 52.59 2 0 4 1946.41 178.98 -2 0 -4 1750.52 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23.00 -2 31 -4 431.76 59.99 -1 31 -4 238.18 45.30 0 31 -4 185.38 38.90 1 31 -4 122.79 36.40 2 31 -4 448.96 58.59 -2 -31 4 434.66 52.99 3 31 -4 78.59 35.20 -3 31 -3 365.96 46.90 3 -31 3 260.87 41.10 -2 31 -3 235.38 45.70 2 -31 3 238.08 35.90 2 -31 3 300.67 38.00 -1 31 -3 151.98 37.90 0 31 -3 183.68 36.30 -1 -31 3 199.08 40.90 2 31 -3 234.88 41.10 3 31 -3 233.48 42.90 -3 31 -2 461.25 55.79 3 -31 2 363.26 49.50 -2 31 -2 206.48 40.70 2 -31 2 190.18 32.40 2 -31 2 201.08 30.90 -1 31 -2 166.78 35.90 0 31 -2 216.28 37.80 0 -31 2 239.48 34.00 1 31 -2 207.48 36.80 -1 -31 2 224.58 33.90 2 31 -2 169.78 34.30 3 31 -2 336.87 48.00 4 -31 1 154.58 30.60 -3 31 -1 283.97 37.90 3 -31 1 185.28 33.80 -2 31 -1 308.27 48.50 2 -31 1 350.96 41.90 -1 31 -1 177.58 38.00 1 -31 1 192.08 31.20 1 -31 1 210.38 31.60 0 31 -1 139.79 32.20 0 -31 1 138.09 27.20 1 31 -1 152.28 32.20 2 31 -1 307.97 44.70 3 31 -1 205.18 37.60 4 31 -1 183.78 43.60 -4 -31 1 251.47 45.70 -4 31 0 655.93 70.59 4 -31 0 632.64 72.59 -3 31 0 85.19 31.70 -3 31 0 137.69 28.30 3 -31 0 96.19 23.90 -2 31 0 125.49 33.10 2 -31 0 97.69 23.50 -1 31 0 175.78 37.20 0 31 0 25.70 26.80 1 31 0 201.08 37.30 2 31 0 116.69 33.50 3 31 0 88.29 31.90 4 31 0 666.33 78.69 -4 31 1 230.18 41.90 4 -31 -1 130.19 29.90 -3 31 1 268.37 37.80 3 -31 -1 246.28 37.60 -2 31 1 294.07 40.00 -2 31 1 317.27 45.60 2 -31 -1 307.67 40.20 -1 31 1 200.18 36.90 1 -31 -1 149.99 27.70 0 31 1 138.59 34.80 0 -31 -1 170.68 29.80 1 31 1 162.68 35.90 2 31 1 305.57 46.50 3 31 1 240.38 43.50 4 31 1 156.78 42.90 -3 31 2 411.56 53.39 3 -31 -2 405.46 51.09 -2 31 2 207.38 37.20 2 -31 -2 153.98 29.30 -1 31 2 227.18 41.10 1 -31 -2 210.38 32.50 0 31 2 215.48 41.10 0 -31 -2 205.88 29.80 1 31 2 204.68 40.50 2 31 2 162.68 38.30 3 31 2 398.96 56.99 -3 31 3 310.87 47.20 3 -31 -3 293.87 40.80 -2 31 3 244.18 42.70 2 -31 -3 191.58 33.10 -1 31 3 120.19 35.10 1 -31 -3 112.89 24.20 0 31 3 203.08 42.30 0 -31 -3 172.68 29.90 1 31 3 173.08 41.70 -1 -31 -3 123.69 26.20 2 31 3 252.57 47.80 -2 -31 -3 302.27 38.60 3 31 3 336.67 53.39 -3 31 4 216.38 38.80 -2 31 4 432.06 56.79 2 -31 -4 376.36 47.20 -1 31 4 206.58 42.30 1 -31 -4 206.78 31.60 0 31 4 168.58 41.80 0 -31 -4 140.99 27.10 1 31 4 233.88 44.20 -1 -31 -4 178.28 33.60 2 31 4 407.26 62.19 -2 -31 -4 467.95 53.59 3 31 4 168.18 48.70 -3 -31 -4 227.68 34.10 -2 31 5 189.28 36.60 2 -31 -5 115.39 26.20 -1 31 5 220.58 42.40 1 -31 -5 155.78 31.30 0 31 5 442.66 60.39 0 -31 -5 417.16 51.19 1 31 5 177.28 42.30 -1 -31 -5 171.88 32.40 2 31 5 185.88 47.00 -2 -31 -5 241.58 39.30 0 31 6 133.59 38.60 0 -31 -6 69.29 24.30 0 32 -5 195.18 45.00 -2 32 -4 226.78 43.40 2 -32 4 153.58 32.90 -1 32 -4 44.60 35.30 1 -32 4 45.20 29.40 0 32 -4 373.36 54.19 0 -32 4 368.76 47.20 1 32 -4 28.80 30.80 2 32 -4 182.48 40.20 -2 32 -3 342.37 52.29 2 -32 3 289.17 42.20 -1 32 -3 296.67 44.70 1 -32 3 235.78 37.20 0 32 -3 42.00 29.50 0 -32 3 60.19 30.30 1 32 -3 236.28 40.50 2 32 -3 223.68 43.60 -2 -32 3 326.77 39.80 -3 32 -2 48.40 30.50 3 -32 2 39.50 19.20 -2 32 -2 86.59 33.80 2 -32 2 59.59 19.50 -1 32 -2 433.06 57.29 0 32 -2 33.00 26.70 1 32 -2 502.35 61.49 2 32 -2 59.99 28.20 -2 -32 2 74.29 32.60 3 32 -2 40.30 27.70 -3 32 -1 384.16 47.50 3 -32 1 328.07 45.90 -2 32 -1 315.97 46.90 2 -32 1 229.48 36.70 2 -32 1 245.48 36.00 -1 32 -1 111.09 35.10 1 -32 1 168.88 40.30 0 32 -1 225.38 39.00 1 32 -1 87.79 30.90 2 32 -1 232.18 42.40 -2 -32 1 329.77 40.50 3 32 -1 347.97 49.50 -3 32 0 183.58 33.20 3 -32 0 176.58 33.80 -2 32 0 221.28 39.30 2 -32 0 200.88 32.80 -1 32 0 196.88 40.10 1 -32 0 174.48 29.30 0 32 0 537.35 67.99 0 -32 0 609.64 64.29 1 32 0 161.08 36.00 2 32 0 221.18 39.90 3 32 0 191.48 43.80 -3 32 1 371.46 48.20 -3 32 1 311.47 46.20 3 -32 -1 399.96 47.40 -2 32 1 260.37 44.00 2 -32 -1 307.17 39.70 -1 32 1 102.49 32.10 1 -32 -1 81.69 21.80 0 32 1 242.68 42.50 0 -32 -1 269.97 35.40 1 32 1 111.09 34.50 2 32 1 286.87 47.30 3 32 1 418.46 58.09 2 -32 -2 37.40 19.60 -1 32 2 594.84 66.69 1 -32 -2 460.45 58.29 0 32 2 50.39 32.80 0 -32 -2 22.10 16.70 1 32 2 452.25 65.89 -1 -32 -2 581.04 58.49 2 32 2 74.99 34.80 3 32 2 69.79 35.20 -2 32 3 291.07 49.40 2 -32 -3 322.97 41.80 -1 32 3 260.67 47.20 1 -32 -3 268.07 36.80 0 32 3 89.09 36.40 0 -32 -3 69.29 21.00 1 32 3 297.37 48.20 -1 -32 -3 227.68 35.30 2 32 3 347.57 54.99 -2 32 4 222.78 43.80 -1 32 4 73.69 34.60 1 -32 -4 32.40 18.00 0 32 4 393.16 57.19 0 -32 -4 407.26 49.20 1 32 4 187.78 43.40 2 32 4 284.67 53.09 0 32 5 229.58 48.60 -1 33 -3 257.67 47.80 1 -33 3 273.37 39.70 0 33 -3 229.08 41.40 1 33 -3 196.48 38.40 -2 33 -2 244.18 43.20 2 -33 2 180.18 33.70 -1 33 -2 122.69 37.40 0 33 -2 278.77 46.40 0 -33 2 326.57 42.00 1 33 -2 54.79 29.60 2 33 -2 169.58 38.70 -2 33 -1 119.79 36.00 2 -33 1 111.79 24.70 -1 33 -1 209.68 43.10 1 -33 1 224.08 31.60 0 33 -1 270.07 45.90 0 -33 1 308.17 41.00 1 33 -1 193.18 37.60 2 33 -1 103.59 34.40 -2 33 0 505.25 65.19 2 -33 0 575.04 61.99 -1 33 0 270.97 47.10 0 33 0 38.30 30.90 1 33 0 280.47 45.70 2 33 0 605.64 72.89 -2 33 1 174.38 35.10 2 -33 -1 103.89 27.40 -1 33 1 186.18 40.00 1 -33 -1 198.88 31.60 0 33 1 281.27 47.30 1 33 1 179.98 38.60 2 33 1 99.39 36.40 -2 33 2 215.08 39.20 2 -33 -2 159.48 32.70 -1 33 2 109.59 34.20 1 -33 -2 68.19 21.20 0 33 2 330.87 52.09 0 -33 -2 294.77 40.20 1 33 2 74.89 35.20 2 33 2 227.48 49.40 -1 33 3 266.97 48.50 1 -33 -3 257.07 38.10 0 -33 -3 243.18 36.00 1 33 3 279.57 50.19 -1 -33 -3 256.97 37.70 0 34 0 216.78 44.60 0 -34 0 175.08 34.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6620 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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 Ru1 Ru 0.8402(3) 0.54851(7) 0.8561(2) 0.0134(4) Uani 1 1 d . U . . . Br1 Br 0.5690(4) 0.55341(11) 1.0213(3) 0.0210(6) Uani 1 1 d . . . . . O1 O 0.701(2) 0.6147(8) 0.7475(18) 0.015(4) Uani 1 1 d . U . . . O2 O 0.598(3) 0.7057(8) 0.761(2) 0.020(4) Uani 1 1 d . U . . . O3 O 1.209(3) 0.7087(8) 1.095(2) 0.024(4) Uani 1 1 d D U . . . H3 H 1.1345 0.6873 1.1382 0.036 Uiso 1 1 calc DR U . . . N1 N 0.952(3) 0.6247(10) 0.954(2) 0.016(4) Uani 1 1 d . U . . . H1 H 0.9684 0.6167 1.0507 0.019 Uiso 1 1 calc R U . . . C1 C 0.696(4) 0.6647(11) 0.802(3) 0.016(4) Uani 1 1 d . U . . . C2 C 0.805(4) 0.6746(12) 0.934(3) 0.019(4) Uani 1 1 d . U . . . H2 H 0.7093 0.6739 1.0075 0.023 Uiso 1 1 calc R U . . . C3 C 0.929(4) 0.7279(11) 0.947(3) 0.020(4) Uani 1 1 d . U . . . H3A H 0.8946 0.7493 1.0285 0.024 Uiso 1 1 calc R U . . . H3B H 0.9070 0.7534 0.8698 0.024 Uiso 1 1 calc R U . . . C4 C 1.152(4) 0.7080(11) 0.956(2) 0.019(4) Uani 1 1 d D U . . . H4 H 1.2374 0.7329 0.9009 0.023 Uiso 1 1 calc R U . . . C5 C 1.137(4) 0.6477(11) 0.902(3) 0.019(4) Uani 1 1 d . U . . . H5A H 1.1342 0.6479 0.8037 0.023 Uiso 1 1 calc R U . . . H5B H 1.2489 0.6242 0.9332 0.023 Uiso 1 1 calc R U . . . C11 C 0.951(4) 0.5134(11) 0.678(3) 0.016(4) Uani 1 1 d . U . . . C12 C 1.114(4) 0.5208(11) 0.769(2) 0.012(4) Uani 1 1 d . U . . . H12 H 1.2172 0.5496 0.7501 0.014 Uiso 1 1 calc R U . . . C13 C 1.095(4) 0.4986(10) 0.900(3) 0.012(4) Uani 1 1 d . U . . . H13 H 1.1874 0.5125 0.9713 0.015 Uiso 1 1 calc R U . . . C14 C 0.939(4) 0.4633(11) 0.937(3) 0.012(4) Uani 1 1 d . U . . . C15 C 0.782(4) 0.4570(12) 0.842(3) 0.013(4) Uani 1 1 d . U . . . H15 H 0.6546 0.4426 0.8748 0.016 Uiso 1 1 calc R U . . . C16 C 0.789(4) 0.4786(12) 0.708(3) 0.017(4) Uani 1 1 d . U . . . H16 H 0.6698 0.4785 0.6497 0.020 Uiso 1 1 calc R U . . . C17 C 0.954(4) 0.5411(12) 0.539(3) 0.027(6) Uani 1 1 d . U . . . H17A H 1.0734 0.5639 0.5307 0.040 Uiso 1 1 calc R U . . . H17B H 0.9514 0.5110 0.4714 0.040 Uiso 1 1 calc R U . . . H17C H 0.8405 0.5660 0.5275 0.040 Uiso 1 1 calc R U . . . C18 C 0.925(4) 0.4433(11) 1.075(3) 0.019(4) Uani 1 1 d . U . . . H18 H 0.7828 0.4393 1.0916 0.023 Uiso 1 1 calc R U . . . C19 C 1.006(5) 0.4785(13) 1.187(3) 0.023(6) Uani 1 1 d . U . . . H19A H 0.9840 0.4586 1.2710 0.034 Uiso 1 1 calc R U . . . H19B H 1.1462 0.4840 1.1755 0.034 Uiso 1 1 calc R U . . . H19C H 0.9411 0.5160 1.1881 0.034 Uiso 1 1 calc R U . . . C20 C 1.010(4) 0.3810(12) 1.081(3) 0.020(6) Uani 1 1 d . U . . . H20A H 1.0029 0.3665 1.1721 0.030 Uiso 1 1 calc R U . . . H20B H 0.9347 0.3560 1.0214 0.030 Uiso 1 1 calc R U . . . H20C H 1.1465 0.3816 1.0539 0.030 Uiso 1 1 calc R U . . . C51 C 0.161(4) 0.1903(11) 0.693(3) 0.019(4) Uani 1 1 d . U . . . C52 C 0.309(4) 0.1702(10) 0.590(3) 0.014(4) Uani 1 1 d . U . . . H52 H 0.2346 0.1509 0.5169 0.017 Uiso 1 1 calc R U . . . C53 C 0.449(4) 0.1263(12) 0.648(3) 0.022(5) Uani 1 1 d . U . . . H53A H 0.3928 0.0872 0.6455 0.026 Uiso 1 1 calc R U . . . H53B H 0.4864 0.1359 0.7412 0.026 Uiso 1 1 calc R U . . . C54 C 0.623(4) 0.1313(12) 0.557(3) 0.017(4) Uani 1 1 d . U . . . H54 H 0.7416 0.1182 0.6075 0.020 Uiso 1 1 calc R U . . . C55 C 0.638(4) 0.1969(11) 0.537(3) 0.018(4) Uani 1 1 d . U . . . H55A H 0.7092 0.2153 0.6119 0.022 Uiso 1 1 calc R U . . . H55B H 0.7054 0.2061 0.4534 0.022 Uiso 1 1 calc R U . . . C61 C 0.468(4) 0.3357(12) 0.779(3) 0.020(4) Uani 1 1 d . U . . . C62 C 0.622(4) 0.3254(12) 0.703(3) 0.017(4) Uani 1 1 d . U . . . H62 H 0.7174 0.2951 0.7312 0.020 Uiso 1 1 calc R U . . . C63 C 0.614(4) 0.3425(11) 0.559(3) 0.018(4) Uani 1 1 d . U . . . H63 H 0.7072 0.3263 0.4938 0.021 Uiso 1 1 calc R U . . . C64 C 0.450(5) 0.3767(12) 0.517(3) 0.021(4) Uani 1 1 d . U . . . C65 C 0.313(4) 0.3908(13) 0.609(3) 0.021(5) Uani 1 1 d . U . . . H65 H 0.1873 0.4071 0.5746 0.026 Uiso 1 1 calc R U . . . C66 C 0.318(4) 0.3712(11) 0.741(3) 0.017(4) Uani 1 1 d . U . . . H66 H 0.2007 0.3754 0.7976 0.021 Uiso 1 1 calc R U . . . C67 C 0.481(4) 0.3144(12) 0.922(3) 0.022(6) Uani 1 1 d . U . . . H67A H 0.3615 0.3243 0.9680 0.033 Uiso 1 1 calc R U . . . H67B H 0.4984 0.2726 0.9225 0.033 Uiso 1 1 calc R U . . . H67C H 0.5928 0.3325 0.9676 0.033 Uiso 1 1 calc R U . . . C68 C 0.432(5) 0.3985(13) 0.372(3) 0.026(5) Uani 1 1 d . U . . . H68 H 0.2901 0.4004 0.3476 0.031 Uiso 1 1 calc R U . . . C69 C 0.531(5) 0.3579(14) 0.273(3) 0.029(7) Uani 1 1 d . U . . . H69A H 0.4730 0.3196 0.2785 0.043 Uiso 1 1 calc R U . . . H69B H 0.5133 0.3729 0.1827 0.043 Uiso 1 1 calc R U . . . H69C H 0.6707 0.3555 0.2947 0.043 Uiso 1 1 calc R U . . . C70 C 0.512(5) 0.4595(15) 0.371(4) 0.034(7) Uani 1 1 d . U . . . H70A H 0.4431 0.4829 0.4361 0.051 Uiso 1 1 calc R U . . . H70B H 0.6514 0.4587 0.3946 0.051 Uiso 1 1 calc R U . . . H70C H 0.4940 0.4761 0.2827 0.051 Uiso 1 1 calc R U . . . Ru2 Ru 0.3429(3) 0.29814(7) 0.6063(2) 0.0135(4) Uani 1 1 d . U . . . Br2 Br 0.0660(4) 0.28836(10) 0.4320(3) 0.0211(6) Uani 1 1 d . . . . . O4 O 0.177(3) 0.2448(7) 0.723(2) 0.021(4) Uani 1 1 d . U . . . O5 O 0.061(3) 0.1564(7) 0.751(2) 0.016(4) Uani 1 1 d . U . . . O6 O 0.606(3) 0.0986(8) 0.442(2) 0.031(5) Uani 1 1 d . U . . . H6 H 0.5160 0.1120 0.3936 0.047 Uiso 1 1 calc DR U . . . N2 N 0.425(3) 0.2165(9) 0.530(2) 0.009(4) Uani 1 1 d . U . . . H2A H 0.3873 0.2169 0.4340 0.011 Uiso 1 1 calc R U . . . 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 0.0072(7) 0.0038(7) 0.0294(8) -0.0008(7) 0.0021(7) 0.0009(8) Br1 0.0085(11) 0.0104(12) 0.0442(16) -0.0013(12) 0.0060(11) -0.0015(13) O1 0.010(7) 0.014(7) 0.020(7) 0.001(6) 0.002(6) 0.002(6) O2 0.020(9) 0.011(8) 0.031(10) 0.004(7) 0.018(8) -0.001(7) O3 0.015(9) 0.013(8) 0.043(10) -0.004(8) 0.007(8) -0.011(7) N1 0.010(7) 0.009(7) 0.028(8) 0.001(6) 0.005(7) 0.002(6) C1 0.013(8) 0.011(7) 0.024(7) 0.004(6) 0.003(7) 0.002(7) C2 0.016(7) 0.012(7) 0.029(7) 0.004(6) 0.003(7) 0.005(6) C3 0.017(8) 0.013(8) 0.029(8) -0.001(7) -0.004(7) 0.001(7) C4 0.015(7) 0.014(7) 0.029(8) 0.001(7) 0.008(7) -0.005(7) C5 0.015(8) 0.013(7) 0.030(8) -0.002(7) 0.009(7) 0.000(7) C11 0.014(7) 0.009(7) 0.025(8) 0.003(7) 0.005(7) 0.001(7) C12 0.011(5) 0.010(5) 0.015(5) -0.001(4) 0.003(4) 0.001(4) C13 0.010(7) 0.006(7) 0.021(7) 0.003(6) 0.001(7) -0.002(6) C14 0.011(5) 0.011(5) 0.016(5) 0.000(4) 0.000(4) 0.002(4) C15 0.009(7) 0.006(7) 0.025(8) -0.006(7) -0.005(7) 0.000(6) C16 0.014(8) 0.013(7) 0.024(8) -0.002(7) 0.001(7) 0.002(7) C17 0.018(11) 0.015(12) 0.048(13) 0.009(11) 0.010(11) -0.006(10) C18 0.011(8) 0.016(8) 0.029(8) -0.001(7) -0.001(7) 0.006(7) C19 0.021(12) 0.019(12) 0.029(12) 0.000(10) 0.003(11) 0.003(10) C20 0.017(8) 0.016(8) 0.026(8) 0.002(7) -0.006(7) 0.005(7) C51 0.010(7) 0.014(7) 0.033(8) 0.000(7) 0.002(7) 0.002(7) C52 0.011(7) 0.010(6) 0.022(7) 0.001(6) -0.001(6) -0.003(6) C53 0.015(8) 0.019(8) 0.030(8) 0.003(7) -0.004(7) 0.004(7) C54 0.015(5) 0.017(5) 0.020(5) 0.001(4) -0.001(4) 0.001(4) C55 0.015(7) 0.017(7) 0.022(7) -0.001(7) 0.001(7) -0.001(7) C61 0.019(8) 0.016(7) 0.027(8) -0.005(7) 0.005(7) 0.002(7) C62 0.011(8) 0.015(7) 0.025(8) -0.004(7) -0.004(7) -0.002(7) C63 0.017(8) 0.010(7) 0.025(8) -0.002(7) 0.009(7) -0.002(7) C64 0.017(7) 0.015(7) 0.031(8) 0.001(6) 0.004(7) 0.000(7) C65 0.018(8) 0.014(8) 0.032(8) -0.002(7) 0.003(7) -0.002(7) C66 0.018(8) 0.010(7) 0.023(8) 0.001(7) 0.002(7) -0.001(7) C67 0.026(12) 0.020(12) 0.020(11) -0.005(9) 0.006(10) -0.003(10) C68 0.023(8) 0.023(8) 0.031(9) -0.003(8) 0.000(8) -0.001(8) C69 0.032(13) 0.033(14) 0.023(12) -0.010(11) 0.010(11) -0.004(12) C70 0.028(13) 0.032(14) 0.041(14) 0.003(12) 0.007(13) -0.012(12) Ru2 0.0063(7) 0.0046(8) 0.0298(9) -0.0016(7) 0.0041(7) 0.0005(8) Br2 0.0093(12) 0.0099(12) 0.0443(16) -0.0011(11) 0.0040(11) 0.0003(11) O4 0.018(7) 0.011(7) 0.034(8) 0.000(6) 0.007(7) 0.003(7) O5 0.009(8) 0.004(7) 0.036(10) 0.001(7) 0.005(8) -0.002(7) O6 0.021(9) 0.018(9) 0.055(12) -0.005(9) 0.009(9) 0.014(7) N2 0.007(5) 0.009(5) 0.013(5) -0.001(4) -0.002(4) 0.000(4) 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' Br Br -0.2901 2.4595 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ru1 C11 90.6(9) . . ? O1 Ru1 C13 150.0(8) . . ? C11 Ru1 C13 70.2(10) . . ? O1 Ru1 N1 77.9(8) . . ? C11 Ru1 N1 124.8(10) . . ? C13 Ru1 N1 94.0(9) . . ? O1 Ru1 C15 127.1(9) . . ? C11 Ru1 C15 68.7(10) . . ? C13 Ru1 C15 68.2(9) . . ? N1 Ru1 C15 153.8(10) . . ? O1 Ru1 C12 113.1(8) . . ? C11 Ru1 C12 39.0(10) . . ? C13 Ru1 C12 38.5(9) . . ? N1 Ru1 C12 97.2(9) . . ? C15 Ru1 C12 80.9(10) . . ? O1 Ru1 C16 97.0(9) . . ? C11 Ru1 C16 37.9(10) . . ? C13 Ru1 C16 82.0(10) . . ? N1 Ru1 C16 162.4(10) . . ? C15 Ru1 C16 38.2(10) . . ? C12 Ru1 C16 69.1(10) . . ? O1 Ru1 C14 164.8(9) . . ? C11 Ru1 C14 81.7(10) . . ? C13 Ru1 C14 37.3(9) . . ? N1 Ru1 C14 117.2(9) . . ? C15 Ru1 C14 37.8(10) . . ? C12 Ru1 C14 68.2(9) . . ? C16 Ru1 C14 68.9(10) . . ? O1 Ru1 Br1 88.7(5) . . ? C11 Ru1 Br1 148.8(8) . . ? C13 Ru1 Br1 119.8(7) . . ? N1 Ru1 Br1 85.5(6) . . ? C15 Ru1 Br1 87.2(8) . . ? C12 Ru1 Br1 158.1(7) . . ? C16 Ru1 Br1 111.4(7) . . ? C14 Ru1 Br1 91.2(7) . . ? C1 O1 Ru1 117.1(16) . . ? C4 O3 H3 109.5 . . ? C5 N1 C2 104(2) . . ? C5 N1 Ru1 115.7(17) . . ? C2 N1 Ru1 109.6(17) . . ? C5 N1 H1 109.1 . . ? C2 N1 H1 109.1 . . ? Ru1 N1 H1 109.1 . . ? O2 C1 O1 125(3) . . ? O2 C1 C2 115(2) . . ? O1 C1 C2 119(2) . . ? C3 C2 C1 118(2) . . ? C3 C2 N1 104(2) . . ? C1 C2 N1 108(2) . . ? C3 C2 H2 109.0 . . ? C1 C2 H2 109.0 . . ? N1 C2 H2 109.0 . . ? C2 C3 C4 108(2) . . ? C2 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? C2 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? O3 C4 C5 112(2) . . ? O3 C4 C3 107(2) . . ? C5 C4 C3 101(2) . . ? O3 C4 H4 112.1 . . ? C5 C4 H4 112.1 . . ? C3 C4 H4 112.1 . . ? N1 C5 C4 105(2) . . ? N1 C5 H5A 110.7 . . ? C4 C5 H5A 110.7 . . ? N1 C5 H5B 110.7 . . ? C4 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C16 C11 C12 122(2) . . ? C16 C11 C17 117(3) . . ? C12 C11 C17 120(2) . . ? C16 C11 Ru1 75.1(16) . . ? C12 C11 Ru1 72.6(15) . . ? C17 C11 Ru1 128.0(19) . . ? C13 C12 C11 118(2) . . ? C13 C12 Ru1 69.2(14) . . ? C11 C12 Ru1 68.3(14) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? Ru1 C12 H12 120.0 . . ? C14 C13 C12 123(2) . . ? C14 C13 Ru1 75.3(15) . . ? C12 C13 Ru1 72.4(14) . . ? C14 C13 H13 118.5 . . ? C12 C13 H13 118.5 . . ? Ru1 C13 H13 118.5 . . ? C13 C14 C15 117(2) . . ? C13 C14 C18 120(3) . . ? C15 C14 C18 122(3) . . ? C13 C14 Ru1 67.4(14) . . ? C15 C14 Ru1 68.4(15) . . ? C18 C14 Ru1 126.9(19) . . ? C14 C15 C16 124(3) . . ? C14 C15 Ru1 73.8(15) . . ? C16 C15 Ru1 73.1(16) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? Ru1 C15 H15 117.8 . . ? C11 C16 C15 116(3) . . ? C11 C16 Ru1 67.1(15) . . ? C15 C16 Ru1 68.7(15) . . ? C11 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? Ru1 C16 H16 120.9 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 121(3) . . ? C14 C18 C20 108(2) . . ? C19 C18 C20 110(2) . . ? C14 C18 H18 105.8 . . ? C19 C18 H18 105.8 . . ? C20 C18 H18 105.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C51 O4 124(3) . . ? O5 C51 C52 121(2) . . ? O4 C51 C52 114(2) . . ? N2 C52 C53 108(2) . . ? N2 C52 C51 115(2) . . ? C53 C52 C51 112(2) . . ? N2 C52 H52 107.3 . . ? C53 C52 H52 107.3 . . ? C51 C52 H52 107.3 . . ? C52 C53 C54 102(2) . . ? C52 C53 H53A 111.3 . . ? C54 C53 H53A 111.3 . . ? C52 C53 H53B 111.3 . . ? C54 C53 H53B 111.3 . . ? H53A C53 H53B 109.2 . . ? O6 C54 C53 114(2) . . ? O6 C54 C55 116(2) . . ? C53 C54 C55 102(2) . . ? O6 C54 H54 108.1 . . ? C53 C54 H54 108.1 . . ? C55 C54 H54 108.1 . . ? N2 C55 C54 103(2) . . ? N2 C55 H55A 111.1 . . ? C54 C55 H55A 111.1 . . ? N2 C55 H55B 111.1 . . ? C54 C55 H55B 111.1 . . ? H55A C55 H55B 109.1 . . ? C62 C61 C66 123(3) . . ? C62 C61 C67 117(3) . . ? C66 C61 C67 120(3) . . ? C62 C61 Ru2 76.3(16) . . ? C66 C61 Ru2 74.0(17) . . ? C67 C61 Ru2 131(2) . . ? C61 C62 C63 120(2) . . ? C61 C62 Ru2 67.7(17) . . ? C63 C62 Ru2 68.8(14) . . ? C61 C62 H62 118.5 . . ? C63 C62 H62 118.5 . . ? Ru2 C62 H62 118.5 . . ? C64 C63 C62 116(2) . . ? C64 C63 Ru2 70.1(16) . . ? C62 C63 Ru2 71.5(14) . . ? C64 C63 H63 121.5 . . ? C62 C63 H63 121.5 . . ? Ru2 C63 H63 121.5 . . ? C65 C64 C63 118(3) . . ? C65 C64 C68 121(3) . . ? C63 C64 C68 121(3) . . ? C65 C64 Ru2 71.3(17) . . ? C63 C64 Ru2 71.4(15) . . ? C68 C64 Ru2 130(2) . . ? C64 C65 C66 124(3) . . ? C64 C65 Ru2 71.8(17) . . ? C66 C65 Ru2 71.8(17) . . ? C64 C65 H65 117.0 . . ? C66 C65 H65 117.0 . . ? Ru2 C65 H65 117.0 . . ? C61 C66 C65 118(3) . . ? C61 C66 Ru2 68.9(16) . . ? C65 C66 Ru2 70.5(16) . . ? C61 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? Ru2 C66 H66 120.4 . . ? C61 C67 H67A 109.5 . . ? C61 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C61 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C70 C68 C69 114(3) . . ? C70 C68 C64 107(3) . . ? C69 C68 C64 112(3) . . ? C70 C68 H68 107.9 . . ? C69 C68 H68 107.9 . . ? C64 C68 H68 107.9 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O4 Ru2 C61 89.9(10) . . ? O4 Ru2 N2 79.7(8) . . ? C61 Ru2 N2 124.0(10) . . ? O4 Ru2 C65 122.5(9) . . ? C61 Ru2 C65 67.4(11) . . ? N2 Ru2 C65 156.8(10) . . ? O4 Ru2 C64 159.3(9) . . ? C61 Ru2 C64 81.8(11) . . ? N2 Ru2 C64 120.6(9) . . ? C65 Ru2 C64 36.9(11) . . ? O4 Ru2 C66 93.6(9) . . ? C61 Ru2 C66 37.1(11) . . ? N2 Ru2 C66 160.5(9) . . ? C65 Ru2 C66 37.7(11) . . ? C64 Ru2 C66 68.5(10) . . ? O4 Ru2 C63 152.5(10) . . ? C61 Ru2 C63 69.6(11) . . ? N2 Ru2 C63 96.3(9) . . ? C65 Ru2 C63 67.3(11) . . ? C64 Ru2 C63 38.5(11) . . ? C66 Ru2 C63 81.1(10) . . ? O4 Ru2 C62 113.8(9) . . ? C61 Ru2 C62 35.9(10) . . ? N2 Ru2 C62 100.3(9) . . ? C65 Ru2 C62 77.9(11) . . ? C64 Ru2 C62 69.2(11) . . ? C66 Ru2 C62 65.5(10) . . ? C63 Ru2 C62 39.7(10) . . ? O4 Ru2 Br2 85.8(6) . . ? C61 Ru2 Br2 151.8(8) . . ? N2 Ru2 Br2 82.7(6) . . ? C65 Ru2 Br2 91.6(8) . . ? C64 Ru2 Br2 92.5(8) . . ? C66 Ru2 Br2 115.3(8) . . ? C63 Ru2 Br2 120.9(8) . . ? C62 Ru2 Br2 160.4(7) . . ? C51 O4 Ru2 119.5(18) . . ? C54 O6 H6 109.5 . . ? C52 N2 C55 107(2) . . ? C52 N2 Ru2 110.8(16) . . ? C55 N2 Ru2 120.6(16) . . ? C52 N2 H2A 105.9 . . ? C55 N2 H2A 105.9 . . ? Ru2 N2 H2A 105.9 . . ? 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 O1 2.108(18) . ? Ru1 C11 2.13(3) . ? Ru1 C13 2.14(2) . ? Ru1 N1 2.16(2) . ? Ru1 C15 2.17(3) . ? Ru1 C12 2.18(2) . ? Ru1 C16 2.23(3) . ? Ru1 C14 2.24(3) . ? Ru1 Br1 2.525(3) . ? O1 C1 1.29(3) . ? O2 C1 1.24(3) . ? O3 C4 1.46(2) . ? O3 H3 0.8400 . ? N1 C5 1.49(4) . ? N1 C2 1.55(3) . ? N1 H1 1.0000 . ? C1 C2 1.53(4) . ? C2 C3 1.51(4) . ? C2 H2 1.0000 . ? C3 C4 1.60(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.51(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C11 C16 1.42(4) . ? C11 C12 1.44(4) . ? C11 C17 1.54(4) . ? C12 C13 1.43(4) . ? C12 H12 1.0000 . ? C13 C14 1.41(4) . ? C13 H13 1.0000 . ? C14 C15 1.43(4) . ? C14 C18 1.47(4) . ? C15 C16 1.44(4) . ? C15 H15 1.0000 . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.50(4) . ? C18 C20 1.56(4) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C51 O5 1.21(3) . ? C51 O4 1.31(3) . ? C51 C52 1.54(4) . ? C52 N2 1.48(3) . ? C52 C53 1.51(4) . ? C52 H52 1.0000 . ? C53 C54 1.52(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 O6 1.39(3) . ? C54 C55 1.55(4) . ? C54 H54 1.0000 . ? C55 N2 1.53(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C61 C62 1.35(4) . ? C61 C66 1.37(4) . ? C61 C67 1.52(4) . ? C61 Ru2 2.12(3) . ? C62 C63 1.50(4) . ? C62 Ru2 2.23(3) . ? C62 H62 1.0000 . ? C63 C64 1.44(4) . ? C63 Ru2 2.19(3) . ? C63 H63 1.0000 . ? C64 C65 1.37(4) . ? C64 C68 1.55(4) . ? C64 Ru2 2.17(3) . ? C65 C66 1.41(4) . ? C65 Ru2 2.17(3) . ? C65 H65 1.0000 . ? C66 Ru2 2.19(3) . ? C66 H66 1.0000 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 C70 1.53(5) . ? C68 C69 1.55(4) . ? C68 H68 1.0000 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? Ru2 O4 2.07(2) . ? Ru2 N2 2.13(2) . ? Ru2 Br2 2.574(3) . ? O6 H6 0.8400 . ? N2 H2A 1.0000 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O5 0.84 1.90 2.72(2) 165.8 2_657 N1 H1 O5 1.00 2.21 3.07(3) 142.6 2_657 C3 H3A O4 0.99 2.56 3.44(4) 147.1 2_657 C5 H5B Br1 0.99 2.87 3.86(3) 178.5 1_655 C53 H53B Br1 0.99 3.10 3.74(3) 123.9 2_647 O6 H6 O1 0.84 2.04 2.84(3) 159.4 2_646 N2 H2A O2 1.00 1.98 2.95(3) 160.4 2_646 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 Ru1 O1 C1 O2 -169(2) . . . . ? Ru1 O1 C1 C2 5(3) . . . . ? O2 C1 C2 C3 -51(3) . . . . ? O1 C1 C2 C3 134(3) . . . . ? O2 C1 C2 N1 -168(2) . . . . ? O1 C1 C2 N1 17(3) . . . . ? C5 N1 C2 C3 -31(3) . . . . ? Ru1 N1 C2 C3 -155.0(18) . . . . ? C5 N1 C2 C1 95(2) . . . . ? Ru1 N1 C2 C1 -29(2) . . . . ? C1 C2 C3 C4 -112(3) . . . . ? N1 C2 C3 C4 7(3) . . . . ? C2 C3 C4 O3 -99(2) . . . . ? C2 C3 C4 C5 18(3) . . . . ? C2 N1 C5 C4 44(3) . . . . ? Ru1 N1 C5 C4 163.8(16) . . . . ? O3 C4 C5 N1 76(3) . . . . ? C3 C4 C5 N1 -37(2) . . . . ? C16 C11 C12 C13 -9(4) . . . . ? C17 C11 C12 C13 174(2) . . . . ? Ru1 C11 C12 C13 50(2) . . . . ? C16 C11 C12 Ru1 -59(2) . . . . ? C17 C11 C12 Ru1 124(2) . . . . ? C11 C12 C13 C14 9(4) . . . . ? Ru1 C12 C13 C14 59(2) . . . . ? C11 C12 C13 Ru1 -50(2) . . . . ? C12 C13 C14 C15 -9(4) . . . . ? Ru1 C13 C14 C15 49(2) . . . . ? C12 C13 C14 C18 -178(2) . . . . ? Ru1 C13 C14 C18 -121(2) . . . . ? C12 C13 C14 Ru1 -57(2) . . . . ? C13 C14 C15 C16 8(4) . . . . ? C18 C14 C15 C16 177(2) . . . . ? Ru1 C14 C15 C16 56(2) . . . . ? C13 C14 C15 Ru1 -48(2) . . . . ? C18 C14 C15 Ru1 121(3) . . . . ? C12 C11 C16 C15 8(4) . . . . ? C17 C11 C16 C15 -175(2) . . . . ? Ru1 C11 C16 C15 -50(2) . . . . ? C12 C11 C16 Ru1 58(2) . . . . ? C17 C11 C16 Ru1 -125(2) . . . . ? C14 C15 C16 C11 -8(4) . . . . ? Ru1 C15 C16 C11 49(2) . . . . ? C14 C15 C16 Ru1 -57(2) . . . . ? C13 C14 C18 C19 30(4) . . . . ? C15 C14 C18 C19 -139(3) . . . . ? Ru1 C14 C18 C19 -53(4) . . . . ? C13 C14 C18 C20 -98(3) . . . . ? C15 C14 C18 C20 93(3) . . . . ? Ru1 C14 C18 C20 179.2(19) . . . . ? O5 C51 C52 N2 -178(2) . . . . ? O4 C51 C52 N2 -8(3) . . . . ? O5 C51 C52 C53 -55(4) . . . . ? O4 C51 C52 C53 116(3) . . . . ? N2 C52 C53 C54 -30(3) . . . . ? C51 C52 C53 C54 -158(2) . . . . ? C52 C53 C54 O6 -85(3) . . . . ? C52 C53 C54 C55 41(3) . . . . ? O6 C54 C55 N2 88(3) . . . . ? C53 C54 C55 N2 -37(2) . . . . ? C66 C61 C62 C63 -13(4) . . . . ? C67 C61 C62 C63 177(2) . . . . ? Ru2 C61 C62 C63 47(2) . . . . ? C66 C61 C62 Ru2 -60(3) . . . . ? C67 C61 C62 Ru2 130(3) . . . . ? C61 C62 C63 C64 9(4) . . . . ? Ru2 C62 C63 C64 55(2) . . . . ? C61 C62 C63 Ru2 -47(2) . . . . ? C62 C63 C64 C65 -1(4) . . . . ? Ru2 C63 C64 C65 55(2) . . . . ? C62 C63 C64 C68 178(3) . . . . ? Ru2 C63 C64 C68 -126(3) . . . . ? C62 C63 C64 Ru2 -56(2) . . . . ? C63 C64 C65 C66 -4(4) . . . . ? C68 C64 C65 C66 178(3) . . . . ? Ru2 C64 C65 C66 52(3) . . . . ? C63 C64 C65 Ru2 -55(2) . . . . ? C68 C64 C65 Ru2 126(3) . . . . ? C62 C61 C66 C65 9(4) . . . . ? C67 C61 C66 C65 179(3) . . . . ? Ru2 C61 C66 C65 -53(2) . . . . ? C62 C61 C66 Ru2 62(3) . . . . ? C67 C61 C66 Ru2 -129(3) . . . . ? C64 C65 C66 C61 0(4) . . . . ? Ru2 C65 C66 C61 52(2) . . . . ? C64 C65 C66 Ru2 -52(3) . . . . ? C65 C64 C68 C70 82(4) . . . . ? C63 C64 C68 C70 -96(3) . . . . ? Ru2 C64 C68 C70 173(2) . . . . ? C65 C64 C68 C69 -153(3) . . . . ? C63 C64 C68 C69 29(4) . . . . ? Ru2 C64 C68 C69 -62(4) . . . . ? O5 C51 O4 Ru2 -177(2) . . . . ? C52 C51 O4 Ru2 13(3) . . . . ? C53 C52 N2 C55 7(3) . . . . ? C51 C52 N2 C55 132(2) . . . . ? C53 C52 N2 Ru2 -126.2(19) . . . . ? C51 C52 N2 Ru2 -1(3) . . . . ? C54 C55 N2 C52 19(3) . . . . ? C54 C55 N2 Ru2 146.4(16) . . . . ?