#------------------------------------------------------------------------------ #$Date: 2026-05-07 23:59:01 +0100 (Thu, 07 May 2026) $ #$Revision: 305893 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720997.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_7720997 loop_ _publ_author_name 'Bera, Jitendra K.' 'Yadav, Sudhir' 'Chourasia, Vishal' 'Ranjan, Prabodh' 'De, Subhabrata' 'Saptal, Vitthal Bhimrao' _publ_section_title ; Cooperative Ruthenium Catalyst for Deaminative Coupling of Primary Amines to Symmetrical Secondary Amines ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00770H _journal_year 2026 _chemical_formula_moiety 'C H2 Cl1.95, C49 H46 N3 O P2 Ru, Cl' _chemical_formula_sum 'C50 H48 Cl2.95 N3 O P2 Ru' _chemical_formula_weight 974.50 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2023-04-25 _audit_creation_method ; Olex2 1.5 (compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410) ; _audit_update_record ; 2023-04-27 deposited with the CCDC. 2026-05-05 downloaded from the CCDC. ; _cell_angle_alpha 93.4510(10) _cell_angle_beta 104.7600(10) _cell_angle_gamma 109.2980(10) _cell_formula_units_Z 2 _cell_length_a 10.3020(2) _cell_length_b 14.3537(3) _cell_length_c 17.0125(4) _cell_measurement_reflns_used 9984 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.25 _cell_measurement_theta_min 2.51 _cell_volume 2267.05(9) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.0280 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 38910 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.255 _diffrn_reflns_theta_min 2.120 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1047 before and 0.0418 after correction. The Ratio of minimum to maximum transmission is 0.9051. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.428 _exptl_crystal_description block _exptl_crystal_F_000 1002 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.989 _refine_diff_density_min -1.621 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 574 _refine_ls_number_reflns 11227 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0308 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+2.8074P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.0790 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10285 _reflns_number_total 11227 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00770h2.cif _cod_data_source_block 24aprc_o_0m_a _cod_database_code 7720997 _shelx_shelxl_version_number 2019/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.895 _shelx_estimated_absorpt_t_min 0.853 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C3-Cl2 \\sim C3-Cl3 \\sim C3-Cl5 with sigma of 0.02 3. Rigid body (RIGU) restrains C3, Cl2, Cl3, Cl5 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: Cl2(0.2) Cl3(0.55) Cl1(0.2) 5.a Aromatic/amide H refined with riding coordinates: N3(H3), C2(H2), C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45) 5.b Idealised Me refined as rotating group: C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C) ; _shelx_res_file ; TITL 24aprc_O_0m_a.res in P-1 24aprc_o_0m_a.res created by SHELXL-2019/1 at 18:33:18 on 25-Apr-2023 REM Old TITL 24aprc_O_0m in P-1 REM SHELXT solution in P-1: R1 0.095, Rweak 0.007, Alpha 0.034 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C50 Cl4 N3 O2 Ru CELL 0.71073 10.302 14.3537 17.0125 93.451 104.76 109.298 ZERR 2 0.0002 0.0003 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H Cl N O P Ru UNIT 100 96 5.9 6 2 4 2 SADI C3 Cl2 C3 Cl3 C3 Cl5 RIGU C3 Cl2 Cl3 Cl5 L.S. 30 PLAN 8 SIZE 0.26 0.22 0.18 TEMP -173.15 CONF BOND LIST 6 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.032100 2.807400 FVAR 0.40366 PART 1 CL2 3 1.323215 0.707935 0.712613 10.20000 0.06976 0.06672 = 0.04402 -0.02096 0.04109 -0.02547 PART 0 C3 1 1.187660 0.585582 0.678913 11.00000 0.05279 0.04234 = 0.03538 0.01213 0.02580 0.02384 PART -1 CL3 3 1.291116 0.715796 0.697304 10.55000 0.08836 0.03602 = 0.05762 0.00955 0.05284 0.00175 PART 0 CL5 3 1.062912 0.559566 0.735347 11.00000 0.03903 0.05168 = 0.03928 -0.00664 0.01713 -0.00048 H 2 0.530191 0.083017 0.661082 11.00000 0.00554 PART -2 CL1 3 1.216359 0.698838 0.655672 10.20000 0.13599 0.04241 = 0.12880 0.05020 0.11087 0.05092 PART 0 H3A 2 1.250404 0.554547 0.697916 11.00000 0.06092 H3B 2 1.127199 0.564624 0.620398 11.00000 0.06078 RESI M001 1 RU1 7 0.589695 0.207270 0.715686 11.00000 0.00873 0.00939 = 0.00966 0.00123 0.00260 0.00261 P1 6 0.542483 0.128642 0.828367 11.00000 0.00906 0.01099 = 0.01084 0.00217 0.00299 0.00303 P2 6 0.621704 0.259306 0.590740 11.00000 0.01250 0.01241 = 0.01034 0.00222 0.00338 0.00438 O1 5 0.285227 0.201216 0.669618 11.00000 0.01611 0.02959 = 0.02636 0.00273 0.00444 0.01022 N1 4 0.807317 0.209698 0.751003 11.00000 0.01110 0.01270 = 0.01114 0.00332 0.00370 0.00452 N2 4 0.716040 0.352973 0.788499 11.00000 0.01180 0.01102 = 0.01242 0.00112 0.00448 0.00396 N3 4 0.695101 0.436350 0.812956 11.00000 0.01203 0.01139 = 0.01491 0.00031 0.00414 0.00491 AFIX 43 H3 2 0.611127 0.443725 0.799919 11.00000 -1.20000 AFIX 0 C1 1 0.358182 0.042250 0.812851 11.00000 0.01016 0.01391 = 0.01627 0.00461 0.00323 0.00407 C2 1 0.279631 -0.018081 0.736783 11.00000 0.01678 0.02345 = 0.01653 0.00330 0.00458 0.00054 AFIX 43 H2 2 0.316872 -0.008223 0.691034 11.00000 -1.20000 AFIX 0 C3 1 0.147019 -0.092643 0.727478 11.00000 0.01757 0.02539 = 0.02138 0.00295 0.00228 -0.00262 AFIX 43 H3A 2 0.094109 -0.133282 0.675457 11.00000 -1.20000 AFIX 0 C4 1 0.092024 -0.107686 0.794057 11.00000 0.01163 0.02180 = 0.02926 0.01129 0.00456 0.00143 AFIX 43 H4 2 0.002238 -0.159206 0.787880 11.00000 -1.20000 AFIX 0 C5 1 0.168120 -0.047601 0.869250 11.00000 0.01616 0.02609 = 0.02334 0.01259 0.01018 0.00818 AFIX 43 H5 2 0.129711 -0.057312 0.914574 11.00000 -1.20000 AFIX 0 C6 1 0.300700 0.027110 0.879189 11.00000 0.01357 0.01980 = 0.01834 0.00499 0.00540 0.00579 AFIX 43 H6 2 0.352374 0.067993 0.931233 11.00000 -1.20000 AFIX 0 C7 1 0.771747 0.237232 0.564786 11.00000 0.01569 0.01649 = 0.01250 0.00499 0.00566 0.00614 C8 1 0.749905 0.154462 0.508491 11.00000 0.01950 0.02085 = 0.01502 0.00309 0.00536 0.00865 AFIX 43 H8 2 0.655123 0.109973 0.480471 11.00000 -1.20000 AFIX 0 C9 1 0.867933 0.137558 0.493692 11.00000 0.02570 0.02722 = 0.01780 0.00290 0.00888 0.01430 AFIX 43 H9 2 0.852907 0.081817 0.454882 11.00000 -1.20000 AFIX 0 C10 1 1.006803 0.201020 0.534867 11.00000 0.02224 0.03263 = 0.02185 0.01102 0.01224 0.01609 AFIX 43 H10 2 1.086343 0.189011 0.523967 11.00000 -1.20000 AFIX 0 C11 1 1.029575 0.282224 0.592105 11.00000 0.01604 0.02641 = 0.01943 0.00990 0.00657 0.00674 AFIX 43 H11 2 1.124699 0.325203 0.621214 11.00000 -1.20000 AFIX 0 C12 1 0.912814 0.300345 0.606615 11.00000 0.01764 0.01895 = 0.01482 0.00546 0.00659 0.00616 AFIX 43 H12 2 0.928726 0.356313 0.645444 11.00000 -1.20000 AFIX 0 C13 1 0.573990 0.211770 0.922375 11.00000 0.01165 0.01360 = 0.01400 0.00112 0.00571 0.00210 C14 1 0.521054 0.289792 0.913227 11.00000 0.01650 0.01708 = 0.01940 0.00445 0.00978 0.00570 AFIX 43 H14 2 0.475116 0.298938 0.859841 11.00000 -1.20000 AFIX 0 C15 1 0.535483 0.353902 0.981980 11.00000 0.02669 0.01765 = 0.02833 0.00310 0.01763 0.00882 AFIX 43 H15 2 0.498632 0.406411 0.975324 11.00000 -1.20000 AFIX 0 C16 1 0.603498 0.341904 1.060603 11.00000 0.02322 0.02289 = 0.02209 -0.00525 0.01246 0.00242 AFIX 43 H16 2 0.614618 0.386588 1.107428 11.00000 -1.20000 AFIX 0 C17 1 0.654894 0.263905 1.069811 11.00000 0.01823 0.02916 = 0.01381 -0.00027 0.00492 0.00398 AFIX 43 H17 2 0.700626 0.254911 1.123296 11.00000 -1.20000 AFIX 0 C18 1 0.639935 0.198817 1.001309 11.00000 0.01451 0.02043 = 0.01511 0.00143 0.00456 0.00509 AFIX 43 H18 2 0.674744 0.145365 1.008303 11.00000 -1.20000 AFIX 0 C19 1 0.645034 0.048336 0.862197 11.00000 0.01375 0.01419 = 0.01090 0.00219 0.00393 0.00586 C20 1 0.794975 0.091448 0.895417 11.00000 0.01452 0.01497 = 0.01215 0.00269 0.00310 0.00356 AFIX 43 H20 2 0.840788 0.162077 0.904128 11.00000 -1.20000 AFIX 0 C21 1 0.876899 0.032033 0.915645 11.00000 0.01339 0.02265 = 0.01410 0.00318 0.00114 0.00749 AFIX 43 H21 2 0.978520 0.061954 0.936928 11.00000 -1.20000 AFIX 0 C22 1 0.810665 -0.071198 0.904851 11.00000 0.02135 0.02033 = 0.01784 0.00336 0.00453 0.01241 AFIX 43 H22 2 0.866984 -0.111835 0.918595 11.00000 -1.20000 AFIX 0 C23 1 0.662471 -0.114842 0.874039 11.00000 0.02252 0.01431 = 0.02454 0.00337 0.00647 0.00773 AFIX 43 H23 2 0.617091 -0.185315 0.867886 11.00000 -1.20000 AFIX 0 C24 1 0.579756 -0.055659 0.852039 11.00000 0.01582 0.01546 = 0.02011 0.00275 0.00497 0.00557 AFIX 43 H24 2 0.478320 -0.086159 0.829988 11.00000 -1.20000 AFIX 0 C25 1 0.402936 0.206850 0.687154 11.00000 0.01885 0.01444 = 0.01370 0.00198 0.00453 0.00412 C26 1 0.910275 0.294529 0.798474 11.00000 0.01194 0.01325 = 0.01349 0.00303 0.00378 0.00490 C27 1 1.055560 0.306831 0.821047 11.00000 0.01355 0.01850 = 0.01755 0.00216 0.00400 0.00560 AFIX 43 H27 2 1.125898 0.367155 0.853405 11.00000 -1.20000 AFIX 0 C28 1 1.095866 0.229923 0.795651 11.00000 0.01422 0.02562 = 0.02190 0.00601 0.00627 0.01077 AFIX 43 H28 2 1.194327 0.236839 0.810327 11.00000 -1.20000 AFIX 0 C29 1 0.990951 0.142650 0.748546 11.00000 0.01973 0.02043 = 0.01981 0.00508 0.00913 0.01252 AFIX 43 H29 2 1.016283 0.088611 0.731182 11.00000 -1.20000 AFIX 0 C30 1 0.848071 0.135540 0.727147 11.00000 0.01821 0.01491 = 0.01417 0.00315 0.00689 0.00742 AFIX 43 H30 2 0.776500 0.075933 0.694389 11.00000 -1.20000 AFIX 0 C31 1 0.819142 0.507700 0.860161 11.00000 0.01386 0.01237 = 0.01456 -0.00019 0.00269 0.00270 C32 1 0.925986 0.468066 0.867084 11.00000 0.01252 0.01456 = 0.01814 -0.00166 0.00055 0.00290 AFIX 43 H32 2 1.024777 0.499182 0.896991 11.00000 -1.20000 AFIX 0 C33 1 0.857322 0.371805 0.820408 11.00000 0.01005 0.01375 = 0.01363 0.00194 0.00280 0.00379 C34 1 0.657842 0.392114 0.583446 11.00000 0.01840 0.01253 = 0.01290 0.00376 0.00225 0.00508 C35 1 0.753398 0.446292 0.542946 11.00000 0.02484 0.02060 = 0.02037 0.00734 0.00924 0.00790 AFIX 43 H35 2 0.806193 0.415032 0.519734 11.00000 -1.20000 AFIX 0 C36 1 0.771699 0.545389 0.536402 11.00000 0.03218 0.02188 = 0.02638 0.01226 0.01013 0.00700 AFIX 43 H36 2 0.837666 0.581931 0.509310 11.00000 -1.20000 AFIX 0 C37 1 0.693905 0.591187 0.569324 11.00000 0.03709 0.01529 = 0.02301 0.00560 0.00375 0.00705 AFIX 43 H37 2 0.706973 0.659181 0.565069 11.00000 -1.20000 AFIX 0 C38 1 0.597079 0.537805 0.608439 11.00000 0.03104 0.01805 = 0.01788 0.00229 0.00338 0.01201 AFIX 43 H38 2 0.542536 0.568923 0.630093 11.00000 -1.20000 AFIX 0 C39 1 0.579468 0.438484 0.616109 11.00000 0.02192 0.01692 = 0.01333 0.00305 0.00298 0.00758 AFIX 43 H39 2 0.513952 0.402387 0.643638 11.00000 -1.20000 AFIX 0 C40 1 0.471967 0.200400 0.496624 11.00000 0.01845 0.01500 = 0.01226 0.00053 0.00187 0.00918 C41 1 0.484690 0.235444 0.423084 11.00000 0.02590 0.02220 = 0.01555 0.00321 0.00136 0.00605 AFIX 43 H41 2 0.569742 0.288066 0.422901 11.00000 -1.20000 AFIX 0 C42 1 0.374104 0.194084 0.350116 11.00000 0.03800 0.02669 = 0.01506 0.00319 -0.00011 0.01538 AFIX 43 H42 2 0.384665 0.217447 0.300206 11.00000 -1.20000 AFIX 0 C43 1 0.249088 0.119114 0.350288 11.00000 0.02830 0.02214 = 0.01933 -0.00506 -0.00723 0.01392 AFIX 43 H43 2 0.172843 0.091759 0.300650 11.00000 -1.20000 AFIX 0 C44 1 0.234600 0.083818 0.422361 11.00000 0.02036 0.02524 = 0.02429 -0.00291 -0.00055 0.00415 AFIX 43 H44 2 0.148139 0.032465 0.422333 11.00000 -1.20000 AFIX 0 C45 1 0.346851 0.123403 0.495537 11.00000 0.01978 0.02144 = 0.01738 0.00057 0.00176 0.00673 AFIX 43 H45 2 0.337415 0.097479 0.544702 11.00000 -1.20000 AFIX 0 C46 1 0.824977 0.610562 0.890709 11.00000 0.01508 0.01295 = 0.01996 -0.00239 0.00282 0.00358 C47 1 0.767269 0.656434 0.816337 11.00000 0.02175 0.01343 = 0.02453 -0.00104 0.00236 0.00527 AFIX 137 H47A 2 0.819869 0.654703 0.776040 11.00000 -1.50000 H47B 2 0.780404 0.725859 0.834650 11.00000 -1.50000 H47C 2 0.664747 0.617980 0.790915 11.00000 -1.50000 AFIX 0 C48 1 0.980947 0.675963 0.935355 11.00000 0.01775 0.01601 = 0.03017 -0.00643 -0.00133 0.00372 AFIX 137 H48A 2 1.018283 0.645658 0.981873 11.00000 -1.50000 H48B 2 0.985459 0.742658 0.955646 11.00000 -1.50000 H48C 2 1.039122 0.681516 0.897176 11.00000 -1.50000 AFIX 0 C49 1 0.732826 0.603212 0.949450 11.00000 0.02790 0.02126 = 0.02488 -0.00426 0.01020 0.00770 AFIX 137 H49A 2 0.632172 0.563906 0.919818 11.00000 -1.50000 H49B 2 0.740962 0.670465 0.970880 11.00000 -1.50000 H49C 2 0.766321 0.570557 0.995276 11.00000 -1.50000 AFIX 0 RESI M003 3 CL1 3 0.392150 0.449264 0.775928 11.00000 0.01454 0.02111 = 0.02970 0.00082 0.00565 0.00772 HKLF 4 REM 24aprc_O_0m_a.res in P-1 REM wR2 = 0.0790, GooF = S = 1.039, Restrained GooF = 1.039 for all data REM R1 = 0.0308 for 10285 Fo > 4sig(Fo) and 0.0347 for all 11227 data REM 574 parameters refined using 15 restraints END WGHT 0.0321 2.8082 REM Highest difference peak 0.989, deepest hole -1.621, 1-sigma level 0.073 Q1 1 1.0376 0.6034 0.7023 11.00000 0.05 0.99 Q2 1 0.5140 0.0342 0.6388 11.00000 0.05 0.83 Q3 1 0.5024 0.0084 0.6327 11.00000 0.05 0.82 Q4 1 0.6384 0.3379 0.5836 11.00000 0.05 0.44 Q5 1 0.8904 0.3390 0.8103 11.00000 0.05 0.44 Q6 1 1.3193 0.6329 0.7181 11.00000 0.05 0.43 Q7 1 0.9793 0.2987 0.8116 11.00000 0.05 0.43 Q8 1 0.2588 0.1052 0.3900 11.00000 0.05 0.42 ; _shelx_res_checksum 26188 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Cl2 Cl 1.323(2) 0.7079(9) 0.7126(11) 0.070(5) Uani 0.2 1 d D . P A 1 C3 C 1.1877(3) 0.5856(2) 0.67891(18) 0.0389(6) Uani 1 1 d D . . . . Cl3 Cl 1.2911(8) 0.7158(3) 0.6973(4) 0.0597(16) Uani 0.55 1 d D . P A -1 Cl5 Cl 1.06291(8) 0.55957(6) 0.73535(4) 0.04721(18) Uani 1 1 d D . . . . H H 0.530(2) 0.0830(15) 0.6611(12) 0.006(5) Uiso 1 1 d . . . . . Cl1 Cl 1.2164(10) 0.6988(5) 0.6557(5) 0.082(3) Uani 0.2 1 d . . P A -2 H3A H 1.250(4) 0.555(3) 0.698(2) 0.061(11) Uiso 1 1 d . . . . . H3B H 1.127(4) 0.565(3) 0.620(2) 0.061(10) Uiso 1 1 d . . . . . Ru1_1 Ru 0.58969(2) 0.20727(2) 0.71569(2) 0.00945(4) Uani 1 1 d . . . . . P1_1 P 0.54248(5) 0.12864(3) 0.82837(3) 0.01041(9) Uani 1 1 d . . . . . P2_1 P 0.62170(5) 0.25931(3) 0.59074(3) 0.01174(9) Uani 1 1 d . . . . . O1_1 O 0.28523(15) 0.20122(12) 0.66962(9) 0.0239(3) Uani 1 1 d . . . . . N1_1 N 0.80732(16) 0.20970(11) 0.75100(9) 0.0114(3) Uani 1 1 d . . . . . N2_1 N 0.71604(16) 0.35297(11) 0.78850(9) 0.0116(3) Uani 1 1 d . . . . . N3_1 N 0.69510(16) 0.43635(11) 0.81296(9) 0.0126(3) Uani 1 1 d . . . . . H3_1 H 0.611127 0.443725 0.799919 0.015 Uiso 1 1 calc R U . . . C1_1 C 0.35818(19) 0.04225(14) 0.81285(11) 0.0135(3) Uani 1 1 d . . . . . C2_1 C 0.2796(2) -0.01808(16) 0.73678(12) 0.0207(4) Uani 1 1 d . . . . . H2_1 H 0.316872 -0.008223 0.691034 0.025 Uiso 1 1 calc R U . . . C3_1 C 0.1470(2) -0.09264(17) 0.72748(13) 0.0248(4) Uani 1 1 d . . . . . H3A_1 H 0.094109 -0.133282 0.675457 0.030 Uiso 1 1 calc R U . . . C4_1 C 0.0920(2) -0.10769(16) 0.79406(13) 0.0220(4) Uani 1 1 d . . . . . H4_1 H 0.002238 -0.159206 0.787880 0.026 Uiso 1 1 calc R U . . . C5_1 C 0.1681(2) -0.04760(16) 0.86925(13) 0.0204(4) Uani 1 1 d . . . . . H5_1 H 0.129711 -0.057312 0.914574 0.025 Uiso 1 1 calc R U . . . C6_1 C 0.3007(2) 0.02711(15) 0.87919(12) 0.0171(4) Uani 1 1 d . . . . . H6_1 H 0.352374 0.067993 0.931233 0.020 Uiso 1 1 calc R U . . . C7_1 C 0.7717(2) 0.23723(14) 0.56479(11) 0.0144(3) Uani 1 1 d . . . . . C8_1 C 0.7499(2) 0.15446(15) 0.50849(12) 0.0180(4) Uani 1 1 d . . . . . H8_1 H 0.655123 0.109973 0.480471 0.022 Uiso 1 1 calc R U . . . C9_1 C 0.8679(2) 0.13756(16) 0.49369(13) 0.0218(4) Uani 1 1 d . . . . . H9_1 H 0.852907 0.081817 0.454882 0.026 Uiso 1 1 calc R U . . . C10_1 C 1.0068(2) 0.20102(17) 0.53487(13) 0.0225(4) Uani 1 1 d . . . . . H10_1 H 1.086343 0.189011 0.523967 0.027 Uiso 1 1 calc R U . . . C11_1 C 1.0296(2) 0.28222(16) 0.59210(13) 0.0203(4) Uani 1 1 d . . . . . H11_1 H 1.124699 0.325203 0.621214 0.024 Uiso 1 1 calc R U . . . C12_1 C 0.9128(2) 0.30035(15) 0.60661(12) 0.0167(4) Uani 1 1 d . . . . . H12_1 H 0.928726 0.356313 0.645444 0.020 Uiso 1 1 calc R U . . . C13_1 C 0.57399(19) 0.21177(13) 0.92237(11) 0.0134(3) Uani 1 1 d . . . . . C14_1 C 0.5211(2) 0.28979(14) 0.91323(12) 0.0168(4) Uani 1 1 d . . . . . H14_1 H 0.475116 0.298938 0.859841 0.020 Uiso 1 1 calc R U . . . C15_1 C 0.5355(2) 0.35390(15) 0.98198(14) 0.0221(4) Uani 1 1 d . . . . . H15_1 H 0.498632 0.406411 0.975324 0.027 Uiso 1 1 calc R U . . . C16_1 C 0.6035(2) 0.34190(16) 1.06060(13) 0.0235(4) Uani 1 1 d . . . . . H16_1 H 0.614618 0.386588 1.107428 0.028 Uiso 1 1 calc R U . . . C17_1 C 0.6549(2) 0.26391(16) 1.06981(12) 0.0217(4) Uani 1 1 d . . . . . H17_1 H 0.700626 0.254911 1.123296 0.026 Uiso 1 1 calc R U . . . C18_1 C 0.6399(2) 0.19882(15) 1.00131(12) 0.0170(4) Uani 1 1 d . . . . . H18_1 H 0.674744 0.145365 1.008303 0.020 Uiso 1 1 calc R U . . . C19_1 C 0.64503(19) 0.04834(13) 0.86220(11) 0.0127(3) Uani 1 1 d . . . . . C20_1 C 0.7950(2) 0.09145(14) 0.89542(11) 0.0145(3) Uani 1 1 d . . . . . H20_1 H 0.840788 0.162077 0.904128 0.017 Uiso 1 1 calc R U . . . C21_1 C 0.8769(2) 0.03203(15) 0.91564(12) 0.0170(4) Uani 1 1 d . . . . . H21_1 H 0.978520 0.061954 0.936928 0.020 Uiso 1 1 calc R U . . . C22_1 C 0.8107(2) -0.07120(15) 0.90485(12) 0.0188(4) Uani 1 1 d . . . . . H22_1 H 0.866984 -0.111835 0.918595 0.023 Uiso 1 1 calc R U . . . C23_1 C 0.6625(2) -0.11484(15) 0.87404(13) 0.0202(4) Uani 1 1 d . . . . . H23_1 H 0.617091 -0.185315 0.867886 0.024 Uiso 1 1 calc R U . . . C24_1 C 0.5798(2) -0.05566(14) 0.85204(12) 0.0172(4) Uani 1 1 d . . . . . H24_1 H 0.478320 -0.086159 0.829988 0.021 Uiso 1 1 calc R U . . . C25_1 C 0.4029(2) 0.20685(14) 0.68715(11) 0.0162(4) Uani 1 1 d . . . . . C26_1 C 0.91027(19) 0.29453(13) 0.79847(11) 0.0127(3) Uani 1 1 d . . . . . C27_1 C 1.0556(2) 0.30683(15) 0.82105(12) 0.0167(4) Uani 1 1 d . . . . . H27_1 H 1.125898 0.367155 0.853405 0.020 Uiso 1 1 calc R U . . . C28_1 C 1.0959(2) 0.22992(16) 0.79565(13) 0.0193(4) Uani 1 1 d . . . . . H28_1 H 1.194327 0.236839 0.810327 0.023 Uiso 1 1 calc R U . . . C29_1 C 0.9910(2) 0.14265(15) 0.74855(12) 0.0178(4) Uani 1 1 d . . . . . H29_1 H 1.016283 0.088611 0.731182 0.021 Uiso 1 1 calc R U . . . C30_1 C 0.8481(2) 0.13554(14) 0.72715(11) 0.0149(3) Uani 1 1 d . . . . . H30_1 H 0.776500 0.075933 0.694389 0.018 Uiso 1 1 calc R U . . . C31_1 C 0.8191(2) 0.50770(14) 0.86016(11) 0.0145(3) Uani 1 1 d . . . . . C32_1 C 0.9260(2) 0.46807(14) 0.86708(12) 0.0166(4) Uani 1 1 d . . . . . H32_1 H 1.024777 0.499182 0.896991 0.020 Uiso 1 1 calc R U . . . C33_1 C 0.85732(19) 0.37180(13) 0.82041(11) 0.0127(3) Uani 1 1 d . . . . . C34_1 C 0.6578(2) 0.39211(14) 0.58345(11) 0.0151(4) Uani 1 1 d . . . . . C35_1 C 0.7534(2) 0.44629(16) 0.54295(13) 0.0213(4) Uani 1 1 d . . . . . H35_1 H 0.806193 0.415032 0.519734 0.026 Uiso 1 1 calc R U . . . C36_1 C 0.7717(3) 0.54539(16) 0.53640(14) 0.0268(5) Uani 1 1 d . . . . . H36_1 H 0.837666 0.581931 0.509310 0.032 Uiso 1 1 calc R U . . . C37_1 C 0.6939(3) 0.59119(16) 0.56932(14) 0.0266(5) Uani 1 1 d . . . . . H37_1 H 0.706973 0.659181 0.565069 0.032 Uiso 1 1 calc R U . . . C38_1 C 0.5971(2) 0.53781(15) 0.60844(12) 0.0222(4) Uani 1 1 d . . . . . H38_1 H 0.542536 0.568923 0.630093 0.027 Uiso 1 1 calc R U . . . C39_1 C 0.5795(2) 0.43848(14) 0.61611(12) 0.0176(4) Uani 1 1 d . . . . . H39_1 H 0.513952 0.402387 0.643638 0.021 Uiso 1 1 calc R U . . . C40_1 C 0.4720(2) 0.20040(14) 0.49662(11) 0.0150(3) Uani 1 1 d . . . . . C41_1 C 0.4847(2) 0.23544(16) 0.42308(12) 0.0228(4) Uani 1 1 d . . . . . H41_1 H 0.569742 0.288066 0.422901 0.027 Uiso 1 1 calc R U . . . C42_1 C 0.3741(3) 0.19408(17) 0.35012(13) 0.0271(5) Uani 1 1 d . . . . . H42_1 H 0.384665 0.217447 0.300206 0.033 Uiso 1 1 calc R U . . . C43_1 C 0.2491(2) 0.11911(16) 0.35029(13) 0.0251(5) Uani 1 1 d . . . . . H43_1 H 0.172843 0.091759 0.300650 0.030 Uiso 1 1 calc R U . . . C44_1 C 0.2346(2) 0.08382(17) 0.42236(14) 0.0261(5) Uani 1 1 d . . . . . H44_1 H 0.148139 0.032465 0.422333 0.031 Uiso 1 1 calc R U . . . C45_1 C 0.3469(2) 0.12340(15) 0.49554(13) 0.0205(4) Uani 1 1 d . . . . . H45_1 H 0.337415 0.097479 0.544702 0.025 Uiso 1 1 calc R U . . . C46_1 C 0.8250(2) 0.61056(14) 0.89071(12) 0.0170(4) Uani 1 1 d . . . . . C47_1 C 0.7673(2) 0.65643(15) 0.81634(13) 0.0212(4) Uani 1 1 d . . . . . H47A_1 H 0.819869 0.654703 0.776040 0.032 Uiso 1 1 calc R U . . . H47B_1 H 0.780404 0.725859 0.834650 0.032 Uiso 1 1 calc R U . . . H47C_1 H 0.664747 0.617980 0.790915 0.032 Uiso 1 1 calc R U . . . C48_1 C 0.9809(2) 0.67596(15) 0.93535(14) 0.0240(4) Uani 1 1 d . . . . . H48A_1 H 1.018283 0.645658 0.981873 0.036 Uiso 1 1 calc R U . . . H48B_1 H 0.985459 0.742658 0.955646 0.036 Uiso 1 1 calc R U . . . H48C_1 H 1.039122 0.681516 0.897176 0.036 Uiso 1 1 calc R U . . . C49_1 C 0.7328(2) 0.60321(16) 0.94945(14) 0.0248(4) Uani 1 1 d . . . . . H49A_1 H 0.632172 0.563906 0.919818 0.037 Uiso 1 1 calc R U . . . H49B_1 H 0.740962 0.670465 0.970880 0.037 Uiso 1 1 calc R U . . . H49C_1 H 0.766321 0.570557 0.995276 0.037 Uiso 1 1 calc R U . . . Cl1_3 Cl 0.39215(5) 0.44926(4) 0.77593(3) 0.02173(10) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl2 0.070(6) 0.067(7) 0.044(5) -0.021(5) 0.041(5) -0.025(6) C3 0.0528(17) 0.0423(15) 0.0354(14) 0.0121(12) 0.0258(13) 0.0238(14) Cl3 0.088(4) 0.0360(12) 0.058(3) 0.0095(15) 0.053(3) 0.0017(17) Cl5 0.0390(4) 0.0517(4) 0.0393(4) -0.0066(3) 0.0171(3) -0.0005(3) Cl1 0.136(7) 0.042(3) 0.129(7) 0.050(4) 0.111(6) 0.051(4) Ru1_1 0.00873(7) 0.00939(7) 0.00966(7) 0.00123(5) 0.00260(5) 0.00261(5) P1_1 0.0091(2) 0.0110(2) 0.0108(2) 0.00217(16) 0.00299(16) 0.00303(16) P2_1 0.0125(2) 0.0124(2) 0.0103(2) 0.00222(16) 0.00338(17) 0.00438(17) O1_1 0.0161(7) 0.0296(8) 0.0264(8) 0.0027(6) 0.0044(6) 0.0102(6) N1_1 0.0111(7) 0.0127(7) 0.0111(7) 0.0033(5) 0.0037(6) 0.0045(6) N2_1 0.0118(7) 0.0110(7) 0.0124(7) 0.0011(5) 0.0045(6) 0.0040(6) N3_1 0.0120(7) 0.0114(7) 0.0149(7) 0.0003(6) 0.0041(6) 0.0049(6) C1_1 0.0102(8) 0.0139(8) 0.0163(9) 0.0046(7) 0.0032(7) 0.0041(7) C2_1 0.0168(9) 0.0235(10) 0.0165(9) 0.0033(8) 0.0046(8) 0.0005(8) C3_1 0.0176(10) 0.0254(11) 0.0214(10) 0.0029(8) 0.0023(8) -0.0026(8) C4_1 0.0116(9) 0.0218(10) 0.0293(11) 0.0113(8) 0.0046(8) 0.0014(7) C5_1 0.0162(9) 0.0261(10) 0.0233(10) 0.0126(8) 0.0102(8) 0.0082(8) C6_1 0.0136(9) 0.0198(9) 0.0183(9) 0.0050(7) 0.0054(7) 0.0058(7) C7_1 0.0157(9) 0.0165(9) 0.0125(8) 0.0050(7) 0.0057(7) 0.0061(7) C8_1 0.0195(9) 0.0208(9) 0.0150(9) 0.0031(7) 0.0054(7) 0.0087(8) C9_1 0.0257(11) 0.0272(11) 0.0178(9) 0.0029(8) 0.0089(8) 0.0143(9) C10_1 0.0222(10) 0.0326(11) 0.0219(10) 0.0110(9) 0.0122(8) 0.0161(9) C11_1 0.0160(9) 0.0264(10) 0.0194(9) 0.0099(8) 0.0066(8) 0.0067(8) C12_1 0.0176(9) 0.0189(9) 0.0148(8) 0.0055(7) 0.0066(7) 0.0062(7) C13_1 0.0117(8) 0.0136(8) 0.0140(8) 0.0011(6) 0.0057(7) 0.0021(7) C14_1 0.0165(9) 0.0171(9) 0.0194(9) 0.0045(7) 0.0098(7) 0.0057(7) C15_1 0.0267(11) 0.0176(9) 0.0283(11) 0.0031(8) 0.0176(9) 0.0088(8) C16_1 0.0232(10) 0.0229(10) 0.0221(10) -0.0052(8) 0.0125(8) 0.0024(8) C17_1 0.0182(10) 0.0292(11) 0.0138(9) -0.0003(8) 0.0049(7) 0.0040(8) C18_1 0.0145(9) 0.0204(9) 0.0151(9) 0.0014(7) 0.0046(7) 0.0051(7) C19_1 0.0138(8) 0.0142(8) 0.0109(8) 0.0022(6) 0.0039(7) 0.0059(7) C20_1 0.0145(9) 0.0150(8) 0.0122(8) 0.0027(7) 0.0031(7) 0.0036(7) C21_1 0.0134(9) 0.0227(10) 0.0141(8) 0.0032(7) 0.0011(7) 0.0075(7) C22_1 0.0213(10) 0.0203(9) 0.0178(9) 0.0034(7) 0.0045(8) 0.0124(8) C23_1 0.0225(10) 0.0143(9) 0.0245(10) 0.0034(7) 0.0065(8) 0.0077(8) C24_1 0.0158(9) 0.0155(9) 0.0201(9) 0.0028(7) 0.0050(7) 0.0056(7) C25_1 0.0189(9) 0.0144(8) 0.0137(8) 0.0020(7) 0.0045(7) 0.0041(7) C26_1 0.0119(8) 0.0133(8) 0.0135(8) 0.0030(7) 0.0038(7) 0.0049(7) C27_1 0.0135(9) 0.0185(9) 0.0175(9) 0.0022(7) 0.0040(7) 0.0056(7) C28_1 0.0142(9) 0.0256(10) 0.0219(10) 0.0060(8) 0.0063(8) 0.0108(8) C29_1 0.0197(9) 0.0204(9) 0.0198(9) 0.0051(7) 0.0091(8) 0.0125(8) C30_1 0.0182(9) 0.0149(8) 0.0142(8) 0.0031(7) 0.0069(7) 0.0074(7) C31_1 0.0139(8) 0.0124(8) 0.0146(8) -0.0002(7) 0.0027(7) 0.0027(7) C32_1 0.0125(8) 0.0146(9) 0.0181(9) -0.0017(7) 0.0006(7) 0.0029(7) C33_1 0.0101(8) 0.0137(8) 0.0136(8) 0.0019(6) 0.0028(6) 0.0038(7) C34_1 0.0184(9) 0.0125(8) 0.0129(8) 0.0038(7) 0.0022(7) 0.0051(7) C35_1 0.0248(10) 0.0206(10) 0.0204(10) 0.0073(8) 0.0092(8) 0.0079(8) C36_1 0.0322(12) 0.0219(10) 0.0264(11) 0.0123(9) 0.0101(9) 0.0070(9) C37_1 0.0371(13) 0.0153(9) 0.0230(10) 0.0056(8) 0.0038(9) 0.0070(9) C38_1 0.0310(11) 0.0180(9) 0.0179(9) 0.0023(7) 0.0034(8) 0.0120(8) C39_1 0.0219(10) 0.0169(9) 0.0133(8) 0.0031(7) 0.0030(7) 0.0076(8) C40_1 0.0184(9) 0.0150(8) 0.0123(8) 0.0005(7) 0.0019(7) 0.0092(7) C41_1 0.0259(11) 0.0222(10) 0.0155(9) 0.0032(8) 0.0014(8) 0.0061(8) C42_1 0.0380(13) 0.0267(11) 0.0151(9) 0.0032(8) -0.0001(9) 0.0154(10) C43_1 0.0283(11) 0.0221(10) 0.0193(10) -0.0051(8) -0.0072(8) 0.0139(9) C44_1 0.0204(10) 0.0252(11) 0.0243(11) -0.0029(8) -0.0005(8) 0.0041(8) C45_1 0.0198(10) 0.0214(10) 0.0174(9) 0.0006(8) 0.0018(8) 0.0067(8) C46_1 0.0151(9) 0.0130(8) 0.0200(9) -0.0024(7) 0.0028(7) 0.0036(7) C47_1 0.0217(10) 0.0134(9) 0.0245(10) -0.0010(7) 0.0024(8) 0.0053(8) C48_1 0.0177(10) 0.0160(9) 0.0302(11) -0.0064(8) -0.0013(8) 0.0037(8) C49_1 0.0279(11) 0.0213(10) 0.0249(11) -0.0043(8) 0.0102(9) 0.0077(9) Cl1_3 0.0145(2) 0.0211(2) 0.0297(3) 0.00082(19) 0.00565(19) 0.00772(18) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Cl2 C3 H3A 93(2) . . ? Cl2 C3 H3B 121(2) . . ? Cl3 C3 Cl2 13.4(9) . . ? Cl3 C3 H3A 106(2) . . ? Cl3 C3 H3B 110(2) . . ? Cl5 C3 Cl2 113.0(7) . . ? Cl5 C3 Cl3 110.7(3) . . ? Cl5 C3 H3A 108(2) . . ? Cl5 C3 H3B 104(2) . . ? Cl1 C3 Cl5 109.1(3) . . ? Cl1 C3 H3A 130(2) . . ? Cl1 C3 H3B 83(2) . . ? H3A C3 H3B 118(3) . . ? P1_1 Ru1_1 H 85.4(6) . . ? P1_1 Ru1_1 P2_1 170.645(17) . . ? P2_1 Ru1_1 H 85.3(6) . . ? N1_1 Ru1_1 H 89.6(6) . . ? N1_1 Ru1_1 P1_1 91.35(4) . . ? N1_1 Ru1_1 P2_1 89.19(4) . . ? N1_1 Ru1_1 N2_1 75.26(6) . . ? N2_1 Ru1_1 H 164.9(7) . . ? N2_1 Ru1_1 P1_1 94.92(4) . . ? N2_1 Ru1_1 P2_1 94.25(4) . . ? C25_1 Ru1_1 H 91.3(7) . . ? C25_1 Ru1_1 P1_1 88.16(6) . . ? C25_1 Ru1_1 P2_1 91.46(6) . . ? C25_1 Ru1_1 N1_1 178.87(7) . . ? C25_1 Ru1_1 N2_1 103.77(7) . . ? C1_1 P1_1 Ru1_1 116.51(6) . . ? C13_1 P1_1 Ru1_1 115.96(6) . . ? C13_1 P1_1 C1_1 102.11(8) . . ? C13_1 P1_1 C19_1 104.08(8) . . ? C19_1 P1_1 Ru1_1 115.04(6) . . ? C19_1 P1_1 C1_1 101.07(8) . . ? C7_1 P2_1 Ru1_1 113.48(6) . . ? C7_1 P2_1 C34_1 103.26(9) . . ? C7_1 P2_1 C40_1 102.65(9) . . ? C34_1 P2_1 Ru1_1 117.07(6) . . ? C34_1 P2_1 C40_1 100.78(8) . . ? C40_1 P2_1 Ru1_1 117.46(6) . . ? C26_1 N1_1 Ru1_1 116.78(12) . . ? C30_1 N1_1 Ru1_1 124.76(13) . . ? C30_1 N1_1 C26_1 118.41(16) . . ? N3_1 N2_1 Ru1_1 138.02(12) . . ? C33_1 N2_1 Ru1_1 116.20(12) . . ? C33_1 N2_1 N3_1 105.78(14) . . ? N2_1 N3_1 H3_1 124.1 . . ? N2_1 N3_1 C31_1 111.79(15) . . ? C31_1 N3_1 H3_1 124.1 . . ? C2_1 C1_1 P1_1 120.17(14) . . ? C2_1 C1_1 C6_1 118.83(17) . . ? C6_1 C1_1 P1_1 120.56(14) . . ? C1_1 C2_1 H2_1 119.8 . . ? C3_1 C2_1 C1_1 120.46(19) . . ? C3_1 C2_1 H2_1 119.8 . . ? C2_1 C3_1 H3A_1 119.9 . . ? C4_1 C3_1 C2_1 120.1(2) . . ? C4_1 C3_1 H3A_1 119.9 . . ? C3_1 C4_1 H4_1 120.1 . . ? C5_1 C4_1 C3_1 119.82(18) . . ? C5_1 C4_1 H4_1 120.1 . . ? C4_1 C5_1 H5_1 119.8 . . ? C4_1 C5_1 C6_1 120.50(18) . . ? C6_1 C5_1 H5_1 119.8 . . ? C1_1 C6_1 H6_1 119.9 . . ? C5_1 C6_1 C1_1 120.26(18) . . ? C5_1 C6_1 H6_1 119.9 . . ? C8_1 C7_1 P2_1 121.54(15) . . ? C8_1 C7_1 C12_1 118.94(18) . . ? C12_1 C7_1 P2_1 119.35(14) . . ? C7_1 C8_1 H8_1 120.2 . . ? C9_1 C8_1 C7_1 119.67(19) . . ? C9_1 C8_1 H8_1 120.2 . . ? C8_1 C9_1 H9_1 119.6 . . ? C10_1 C9_1 C8_1 120.82(19) . . ? C10_1 C9_1 H9_1 119.6 . . ? C9_1 C10_1 H10_1 120.1 . . ? C9_1 C10_1 C11_1 119.89(19) . . ? C11_1 C10_1 H10_1 120.1 . . ? C10_1 C11_1 H11_1 120.1 . . ? C12_1 C11_1 C10_1 119.73(19) . . ? C12_1 C11_1 H11_1 120.1 . . ? C7_1 C12_1 H12_1 119.5 . . ? C11_1 C12_1 C7_1 120.92(19) . . ? C11_1 C12_1 H12_1 119.5 . . ? C14_1 C13_1 P1_1 116.59(14) . . ? C18_1 C13_1 P1_1 124.17(15) . . ? C18_1 C13_1 C14_1 119.16(17) . . ? C13_1 C14_1 H14_1 119.9 . . ? C15_1 C14_1 C13_1 120.17(19) . . ? C15_1 C14_1 H14_1 119.9 . . ? C14_1 C15_1 H15_1 119.7 . . ? C14_1 C15_1 C16_1 120.59(19) . . ? C16_1 C15_1 H15_1 119.7 . . ? C15_1 C16_1 H16_1 120.4 . . ? C17_1 C16_1 C15_1 119.28(19) . . ? C17_1 C16_1 H16_1 120.4 . . ? C16_1 C17_1 H17_1 119.7 . . ? C16_1 C17_1 C18_1 120.53(19) . . ? C18_1 C17_1 H17_1 119.7 . . ? C13_1 C18_1 H18_1 119.9 . . ? C17_1 C18_1 C13_1 120.26(19) . . ? C17_1 C18_1 H18_1 119.9 . . ? C20_1 C19_1 P1_1 119.25(14) . . ? C24_1 C19_1 P1_1 122.10(14) . . ? C24_1 C19_1 C20_1 118.56(17) . . ? C19_1 C20_1 H20_1 119.7 . . ? C21_1 C20_1 C19_1 120.68(17) . . ? C21_1 C20_1 H20_1 119.7 . . ? C20_1 C21_1 H21_1 119.9 . . ? C20_1 C21_1 C22_1 120.12(18) . . ? C22_1 C21_1 H21_1 119.9 . . ? C21_1 C22_1 H22_1 120.0 . . ? C23_1 C22_1 C21_1 119.96(18) . . ? C23_1 C22_1 H22_1 120.0 . . ? C22_1 C23_1 H23_1 119.9 . . ? C22_1 C23_1 C24_1 120.18(18) . . ? C24_1 C23_1 H23_1 119.9 . . ? C19_1 C24_1 H24_1 119.8 . . ? C23_1 C24_1 C19_1 120.47(18) . . ? C23_1 C24_1 H24_1 119.8 . . ? O1_1 C25_1 Ru1_1 176.35(17) . . ? N1_1 C26_1 C27_1 121.82(17) . . ? N1_1 C26_1 C33_1 114.90(15) . . ? C27_1 C26_1 C33_1 123.24(17) . . ? C26_1 C27_1 H27_1 120.5 . . ? C28_1 C27_1 C26_1 119.05(18) . . ? C28_1 C27_1 H27_1 120.5 . . ? C27_1 C28_1 H28_1 120.4 . . ? C27_1 C28_1 C29_1 119.26(18) . . ? C29_1 C28_1 H28_1 120.4 . . ? C28_1 C29_1 H29_1 120.6 . . ? C28_1 C29_1 C30_1 118.90(18) . . ? C30_1 C29_1 H29_1 120.6 . . ? N1_1 C30_1 C29_1 122.54(18) . . ? N1_1 C30_1 H30_1 118.7 . . ? C29_1 C30_1 H30_1 118.7 . . ? N3_1 C31_1 C32_1 106.86(16) . . ? N3_1 C31_1 C46_1 121.69(17) . . ? C32_1 C31_1 C46_1 131.34(17) . . ? C31_1 C32_1 H32_1 127.4 . . ? C31_1 C32_1 C33_1 105.24(16) . . ? C33_1 C32_1 H32_1 127.4 . . ? N2_1 C33_1 C26_1 116.78(16) . . ? N2_1 C33_1 C32_1 110.32(16) . . ? C32_1 C33_1 C26_1 132.84(17) . . ? C35_1 C34_1 P2_1 123.07(15) . . ? C39_1 C34_1 P2_1 117.68(14) . . ? C39_1 C34_1 C35_1 119.14(18) . . ? C34_1 C35_1 H35_1 119.8 . . ? C36_1 C35_1 C34_1 120.5(2) . . ? C36_1 C35_1 H35_1 119.8 . . ? C35_1 C36_1 H36_1 119.9 . . ? C37_1 C36_1 C35_1 120.1(2) . . ? C37_1 C36_1 H36_1 119.9 . . ? C36_1 C37_1 H37_1 120.0 . . ? C38_1 C37_1 C36_1 120.0(2) . . ? C38_1 C37_1 H37_1 120.0 . . ? C37_1 C38_1 H38_1 119.9 . . ? C37_1 C38_1 C39_1 120.2(2) . . ? C39_1 C38_1 H38_1 119.9 . . ? C34_1 C39_1 C38_1 120.11(19) . . ? C34_1 C39_1 H39_1 119.9 . . ? C38_1 C39_1 H39_1 119.9 . . ? C41_1 C40_1 P2_1 118.27(15) . . ? C45_1 C40_1 P2_1 122.98(15) . . ? C45_1 C40_1 C41_1 118.74(18) . . ? C40_1 C41_1 H41_1 119.7 . . ? C42_1 C41_1 C40_1 120.7(2) . . ? C42_1 C41_1 H41_1 119.7 . . ? C41_1 C42_1 H42_1 120.0 . . ? C43_1 C42_1 C41_1 119.9(2) . . ? C43_1 C42_1 H42_1 120.0 . . ? C42_1 C43_1 H43_1 119.9 . . ? C44_1 C43_1 C42_1 120.1(2) . . ? C44_1 C43_1 H43_1 119.9 . . ? C43_1 C44_1 H44_1 119.9 . . ? C43_1 C44_1 C45_1 120.2(2) . . ? C45_1 C44_1 H44_1 119.9 . . ? C40_1 C45_1 C44_1 120.3(2) . . ? C40_1 C45_1 H45_1 119.9 . . ? C44_1 C45_1 H45_1 119.9 . . ? C31_1 C46_1 C47_1 108.71(16) . . ? C31_1 C46_1 C48_1 109.03(16) . . ? C31_1 C46_1 C49_1 110.14(16) . . ? C48_1 C46_1 C47_1 109.62(17) . . ? C48_1 C46_1 C49_1 109.80(17) . . ? C49_1 C46_1 C47_1 109.52(17) . . ? C46_1 C47_1 H47A_1 109.5 . . ? C46_1 C47_1 H47B_1 109.5 . . ? C46_1 C47_1 H47C_1 109.5 . . ? H47A_1 C47_1 H47B_1 109.5 . . ? H47A_1 C47_1 H47C_1 109.5 . . ? H47B_1 C47_1 H47C_1 109.5 . . ? C46_1 C48_1 H48A_1 109.5 . . ? C46_1 C48_1 H48B_1 109.5 . . ? C46_1 C48_1 H48C_1 109.5 . . ? H48A_1 C48_1 H48B_1 109.5 . . ? H48A_1 C48_1 H48C_1 109.5 . . ? H48B_1 C48_1 H48C_1 109.5 . . ? C46_1 C49_1 H49A_1 109.5 . . ? C46_1 C49_1 H49B_1 109.5 . . ? C46_1 C49_1 H49C_1 109.5 . . ? H49A_1 C49_1 H49B_1 109.5 . . ? H49A_1 C49_1 H49C_1 109.5 . . ? H49B_1 C49_1 H49C_1 109.5 . . ? 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 Cl2 C3 1.792(12) . ? C3 Cl3 1.781(5) . ? C3 Cl5 1.751(3) . ? C3 Cl1 1.645(6) . ? C3 H3A 0.91(4) . ? C3 H3B 1.00(4) . ? Ru1_1 H 1.79(2) . ? Ru1_1 P1_1 2.3575(5) . ? Ru1_1 P2_1 2.3602(5) . ? Ru1_1 N1_1 2.1559(15) . ? Ru1_1 N2_1 2.1610(15) . ? Ru1_1 C25_1 1.858(2) . ? P1_1 C1_1 1.8334(19) . ? P1_1 C13_1 1.8266(19) . ? P1_1 C19_1 1.8306(18) . ? P2_1 C7_1 1.8274(19) . ? P2_1 C34_1 1.8360(19) . ? P2_1 C40_1 1.8370(19) . ? O1_1 C25_1 1.146(2) . ? N1_1 C26_1 1.361(2) . ? N1_1 C30_1 1.343(2) . ? N2_1 N3_1 1.345(2) . ? N2_1 C33_1 1.344(2) . ? N3_1 H3_1 0.8800 . ? N3_1 C31_1 1.356(2) . ? C1_1 C2_1 1.396(3) . ? C1_1 C6_1 1.399(3) . ? C2_1 H2_1 0.9500 . ? C2_1 C3_1 1.393(3) . ? C3_1 H3A_1 0.9500 . ? C3_1 C4_1 1.388(3) . ? C4_1 H4_1 0.9500 . ? C4_1 C5_1 1.380(3) . ? C5_1 H5_1 0.9500 . ? C5_1 C6_1 1.392(3) . ? C6_1 H6_1 0.9500 . ? C7_1 C8_1 1.399(3) . ? C7_1 C12_1 1.402(3) . ? C8_1 H8_1 0.9500 . ? C8_1 C9_1 1.394(3) . ? C9_1 H9_1 0.9500 . ? C9_1 C10_1 1.385(3) . ? C10_1 H10_1 0.9500 . ? C10_1 C11_1 1.389(3) . ? C11_1 H11_1 0.9500 . ? C11_1 C12_1 1.388(3) . ? C12_1 H12_1 0.9500 . ? C13_1 C14_1 1.399(3) . ? C13_1 C18_1 1.396(3) . ? C14_1 H14_1 0.9500 . ? C14_1 C15_1 1.389(3) . ? C15_1 H15_1 0.9500 . ? C15_1 C16_1 1.393(3) . ? C16_1 H16_1 0.9500 . ? C16_1 C17_1 1.389(3) . ? C17_1 H17_1 0.9500 . ? C17_1 C18_1 1.392(3) . ? C18_1 H18_1 0.9500 . ? C19_1 C20_1 1.403(3) . ? C19_1 C24_1 1.399(3) . ? C20_1 H20_1 0.9500 . ? C20_1 C21_1 1.386(3) . ? C21_1 H21_1 0.9500 . ? C21_1 C22_1 1.389(3) . ? C22_1 H22_1 0.9500 . ? C22_1 C23_1 1.385(3) . ? C23_1 H23_1 0.9500 . ? C23_1 C24_1 1.394(3) . ? C24_1 H24_1 0.9500 . ? C26_1 C27_1 1.394(3) . ? C26_1 C33_1 1.456(2) . ? C27_1 H27_1 0.9500 . ? C27_1 C28_1 1.384(3) . ? C28_1 H28_1 0.9500 . ? C28_1 C29_1 1.387(3) . ? C29_1 H29_1 0.9500 . ? C29_1 C30_1 1.390(3) . ? C30_1 H30_1 0.9500 . ? C31_1 C32_1 1.380(3) . ? C31_1 C46_1 1.512(3) . ? C32_1 H32_1 0.9500 . ? C32_1 C33_1 1.406(3) . ? C34_1 C35_1 1.397(3) . ? C34_1 C39_1 1.394(3) . ? C35_1 H35_1 0.9500 . ? C35_1 C36_1 1.387(3) . ? C36_1 H36_1 0.9500 . ? C36_1 C37_1 1.386(3) . ? C37_1 H37_1 0.9500 . ? C37_1 C38_1 1.385(3) . ? C38_1 H38_1 0.9500 . ? C38_1 C39_1 1.395(3) . ? C39_1 H39_1 0.9500 . ? C40_1 C41_1 1.397(3) . ? C40_1 C45_1 1.388(3) . ? C41_1 H41_1 0.9500 . ? C41_1 C42_1 1.391(3) . ? C42_1 H42_1 0.9500 . ? C42_1 C43_1 1.379(3) . ? C43_1 H43_1 0.9500 . ? C43_1 C44_1 1.379(3) . ? C44_1 H44_1 0.9500 . ? C44_1 C45_1 1.399(3) . ? C45_1 H45_1 0.9500 . ? C46_1 C47_1 1.537(3) . ? C46_1 C48_1 1.528(3) . ? C46_1 C49_1 1.530(3) . ? C47_1 H47A_1 0.9800 . ? C47_1 H47B_1 0.9800 . ? C47_1 H47C_1 0.9800 . ? C48_1 H48A_1 0.9800 . ? C48_1 H48B_1 0.9800 . ? C48_1 H48C_1 0.9800 . ? C49_1 H49A_1 0.9800 . ? C49_1 H49B_1 0.9800 . ? C49_1 H49C_1 0.9800 . ? 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_1 P1_1 C1_1 C2_1 36.65(18) . . . . ? Ru1_1 P1_1 C1_1 C6_1 -151.04(13) . . . . ? Ru1_1 P1_1 C13_1 C14_1 45.49(16) . . . . ? Ru1_1 P1_1 C13_1 C18_1 -137.88(14) . . . . ? Ru1_1 P1_1 C19_1 C20_1 65.31(15) . . . . ? Ru1_1 P1_1 C19_1 C24_1 -111.21(15) . . . . ? Ru1_1 P2_1 C7_1 C8_1 99.39(15) . . . . ? Ru1_1 P2_1 C7_1 C12_1 -75.79(15) . . . . ? Ru1_1 P2_1 C34_1 C35_1 142.21(15) . . . . ? Ru1_1 P2_1 C34_1 C39_1 -41.50(17) . . . . ? Ru1_1 P2_1 C40_1 C41_1 175.30(14) . . . . ? Ru1_1 P2_1 C40_1 C45_1 -4.22(19) . . . . ? Ru1_1 N1_1 C26_1 C27_1 -176.24(14) . . . . ? Ru1_1 N1_1 C26_1 C33_1 1.3(2) . . . . ? Ru1_1 N1_1 C30_1 C29_1 176.94(14) . . . . ? Ru1_1 N2_1 N3_1 C31_1 179.95(14) . . . . ? Ru1_1 N2_1 C33_1 C26_1 3.4(2) . . . . ? Ru1_1 N2_1 C33_1 C32_1 -179.15(12) . . . . ? P1_1 C1_1 C2_1 C3_1 171.81(17) . . . . ? P1_1 C1_1 C6_1 C5_1 -171.78(15) . . . . ? P1_1 C13_1 C14_1 C15_1 177.43(15) . . . . ? P1_1 C13_1 C18_1 C17_1 -177.67(15) . . . . ? P1_1 C19_1 C20_1 C21_1 -174.94(14) . . . . ? P1_1 C19_1 C24_1 C23_1 176.13(15) . . . . ? P2_1 C7_1 C8_1 C9_1 -176.64(15) . . . . ? P2_1 C7_1 C12_1 C11_1 176.04(15) . . . . ? P2_1 C34_1 C35_1 C36_1 177.22(17) . . . . ? P2_1 C34_1 C39_1 C38_1 -176.64(15) . . . . ? P2_1 C40_1 C41_1 C42_1 -179.49(17) . . . . ? P2_1 C40_1 C45_1 C44_1 177.88(16) . . . . ? N1_1 C26_1 C27_1 C28_1 -1.1(3) . . . . ? N1_1 C26_1 C33_1 N2_1 -3.1(2) . . . . ? N1_1 C26_1 C33_1 C32_1 -179.83(19) . . . . ? N2_1 N3_1 C31_1 C32_1 -0.4(2) . . . . ? N2_1 N3_1 C31_1 C46_1 176.13(16) . . . . ? N3_1 N2_1 C33_1 C26_1 -176.27(15) . . . . ? N3_1 N2_1 C33_1 C32_1 1.1(2) . . . . ? N3_1 C31_1 C32_1 C33_1 1.1(2) . . . . ? N3_1 C31_1 C46_1 C47_1 -55.6(2) . . . . ? N3_1 C31_1 C46_1 C48_1 -175.04(18) . . . . ? N3_1 C31_1 C46_1 C49_1 64.4(2) . . . . ? C1_1 P1_1 C13_1 C14_1 -82.26(15) . . . . ? C1_1 P1_1 C13_1 C18_1 94.38(17) . . . . ? C1_1 P1_1 C19_1 C20_1 -168.29(15) . . . . ? C1_1 P1_1 C19_1 C24_1 15.19(17) . . . . ? C1_1 C2_1 C3_1 C4_1 -0.2(3) . . . . ? C2_1 C1_1 C6_1 C5_1 0.6(3) . . . . ? C2_1 C3_1 C4_1 C5_1 0.9(3) . . . . ? C3_1 C4_1 C5_1 C6_1 -0.9(3) . . . . ? C4_1 C5_1 C6_1 C1_1 0.1(3) . . . . ? C6_1 C1_1 C2_1 C3_1 -0.6(3) . . . . ? C7_1 P2_1 C34_1 C35_1 16.75(19) . . . . ? C7_1 P2_1 C34_1 C39_1 -166.95(15) . . . . ? C7_1 P2_1 C40_1 C41_1 -59.48(17) . . . . ? C7_1 P2_1 C40_1 C45_1 121.00(17) . . . . ? C7_1 C8_1 C9_1 C10_1 0.9(3) . . . . ? C8_1 C7_1 C12_1 C11_1 0.7(3) . . . . ? C8_1 C9_1 C10_1 C11_1 0.5(3) . . . . ? C9_1 C10_1 C11_1 C12_1 -1.2(3) . . . . ? C10_1 C11_1 C12_1 C7_1 0.6(3) . . . . ? C12_1 C7_1 C8_1 C9_1 -1.4(3) . . . . ? C13_1 P1_1 C1_1 C2_1 164.04(16) . . . . ? C13_1 P1_1 C1_1 C6_1 -23.65(17) . . . . ? C13_1 P1_1 C19_1 C20_1 -62.66(16) . . . . ? C13_1 P1_1 C19_1 C24_1 120.82(16) . . . . ? C13_1 C14_1 C15_1 C16_1 0.5(3) . . . . ? C14_1 C13_1 C18_1 C17_1 -1.1(3) . . . . ? C14_1 C15_1 C16_1 C17_1 -1.1(3) . . . . ? C15_1 C16_1 C17_1 C18_1 0.6(3) . . . . ? C16_1 C17_1 C18_1 C13_1 0.5(3) . . . . ? C18_1 C13_1 C14_1 C15_1 0.6(3) . . . . ? C19_1 P1_1 C1_1 C2_1 -88.77(17) . . . . ? C19_1 P1_1 C1_1 C6_1 83.54(16) . . . . ? C19_1 P1_1 C13_1 C14_1 172.89(14) . . . . ? C19_1 P1_1 C13_1 C18_1 -10.48(18) . . . . ? C19_1 C20_1 C21_1 C22_1 -1.4(3) . . . . ? C20_1 C19_1 C24_1 C23_1 -0.4(3) . . . . ? C20_1 C21_1 C22_1 C23_1 -0.2(3) . . . . ? C21_1 C22_1 C23_1 C24_1 1.5(3) . . . . ? C22_1 C23_1 C24_1 C19_1 -1.2(3) . . . . ? C24_1 C19_1 C20_1 C21_1 1.7(3) . . . . ? C26_1 N1_1 C30_1 C29_1 -0.5(3) . . . . ? C26_1 C27_1 C28_1 C29_1 -0.1(3) . . . . ? C27_1 C26_1 C33_1 N2_1 174.37(17) . . . . ? C27_1 C26_1 C33_1 C32_1 -2.3(3) . . . . ? C27_1 C28_1 C29_1 C30_1 0.9(3) . . . . ? C28_1 C29_1 C30_1 N1_1 -0.6(3) . . . . ? C30_1 N1_1 C26_1 C27_1 1.4(3) . . . . ? C30_1 N1_1 C26_1 C33_1 178.98(16) . . . . ? C31_1 C32_1 C33_1 N2_1 -1.4(2) . . . . ? C31_1 C32_1 C33_1 C26_1 175.45(19) . . . . ? C32_1 C31_1 C46_1 C47_1 120.0(2) . . . . ? C32_1 C31_1 C46_1 C48_1 0.6(3) . . . . ? C32_1 C31_1 C46_1 C49_1 -120.0(2) . . . . ? C33_1 N2_1 N3_1 C31_1 -0.4(2) . . . . ? C33_1 C26_1 C27_1 C28_1 -178.48(18) . . . . ? C34_1 P2_1 C7_1 C8_1 -132.86(16) . . . . ? C34_1 P2_1 C7_1 C12_1 51.95(16) . . . . ? C34_1 P2_1 C40_1 C41_1 46.91(17) . . . . ? C34_1 P2_1 C40_1 C45_1 -132.61(17) . . . . ? C34_1 C35_1 C36_1 C37_1 -0.7(3) . . . . ? C35_1 C34_1 C39_1 C38_1 -0.2(3) . . . . ? C35_1 C36_1 C37_1 C38_1 -0.4(3) . . . . ? C36_1 C37_1 C38_1 C39_1 1.1(3) . . . . ? C37_1 C38_1 C39_1 C34_1 -0.9(3) . . . . ? C39_1 C34_1 C35_1 C36_1 1.0(3) . . . . ? C40_1 P2_1 C7_1 C8_1 -28.39(17) . . . . ? C40_1 P2_1 C7_1 C12_1 156.42(15) . . . . ? C40_1 P2_1 C34_1 C35_1 -89.15(18) . . . . ? C40_1 P2_1 C34_1 C39_1 87.15(16) . . . . ? C40_1 C41_1 C42_1 C43_1 1.4(3) . . . . ? C41_1 C40_1 C45_1 C44_1 -1.6(3) . . . . ? C41_1 C42_1 C43_1 C44_1 -1.2(3) . . . . ? C42_1 C43_1 C44_1 C45_1 -0.4(3) . . . . ? C43_1 C44_1 C45_1 C40_1 1.8(3) . . . . ? C45_1 C40_1 C41_1 C42_1 0.1(3) . . . . ? C46_1 C31_1 C32_1 C33_1 -175.02(19) . . . . ?