#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:55:54 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257548 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705307.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_7705307 loop_ _publ_author_name 'Gallardo-Villagr\'an, Manuel' 'Rivada-Wheelaghan, Orestes' 'Rahaman, S. M. Wahidur' 'Fayzullin, Robert R.' 'Khusnutdinova, Julia R.' _publ_section_title ; Proton-responsive naphthyridinone-based RuII complexes and their reactivity with water and alcohols. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12756 _journal_page_last 12766 _journal_paper_doi 10.1039/d0dt02505d _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C30 H42 Cl2 N4 O2 P2 Ru, 1.5(C6 H6)' _chemical_formula_sum 'C39 H51 Cl2 N4 O2 P2 Ru' _chemical_formula_weight 841.74 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-06-14 deposited with the CCDC. 2020-08-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.6750(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.65544(11) _cell_length_b 16.40142(13) _cell_length_c 16.48977(14) _cell_measurement_reflns_used 117037 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 32.5250 _cell_measurement_theta_min 2.3110 _cell_volume 3950.46(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.20a (Rigaku OD, 2015)' _computing_molecular_graphics ; WinGX (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009); enCIFer (Allen, 2004) ; _computing_publication_material ; WinGX (Farrugia, 2012); PLATON (Spek, 2009); ORTEP-3 (Farrugia, 2012); Olex2 (Dolomanov et al., 2009); enCIFer (Allen, 2004) ; _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'XtaLAB Pro: Kappa dual offset/far' _diffrn_measurement_method '\w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_unetI/netI 0.0136 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 237734 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.355 _diffrn_reflns_theta_min 2.177 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.20a (Rigaku Oxford Diffraction, 2015). Numerical absorption correction based on gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics, frame scaling and detector area scaling, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.415 _exptl_crystal_description prism _exptl_crystal_F_000 1748 _exptl_crystal_recrystallization_method 'from a concentrated benzene solution at -20 \%C' _exptl_crystal_size_max 0.256 _exptl_crystal_size_mid 0.166 _exptl_crystal_size_min 0.098 _refine_diff_density_max 0.804 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 488 _refine_ls_number_reflns 13567 _refine_ls_number_restraints 80 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0202 _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^)+(0.0197P)^2^+2.3325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.0494 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12713 _reflns_number_total 13567 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02505d2.cif _cod_data_source_block jk337 _cod_depositor_comments 'Adding full bibliography for 7705307--7705310.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705307 _shelx_shelxl_version_number 2018/3 _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 0.851 _shelx_estimated_absorpt_t_max 0.939 _shelx_res_file ; TITL jk337 in P2(1)/n shelx.res created by SHELXL-2018/3 at 16:41:38 on 10-Apr-2020 CELL 0.71073 14.655444 16.401417 16.489765 90.0000 94.6750 90.0000 ZERR 4.00 0.000112 0.000126 0.000137 0.0000 0.0007 0.0000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL RU UNIT 156 204 16 8 8 8 4 MERG 2 OMIT -2 0 8 OMIT -7 3 1 OMIT -7 0 1 OMIT 3 0 7 HTAB N12 CL1 HTAB N22 CL2 SADI N12 H12 N22 H22 DFIX 1.39 0.012 C81 C82 C82 C83 C83 C84 C84 C85 C85 C86 C86 C81 DFIX 1.39 0.012 C91 C92 C92 C93 C93 C94 C94 C95 C95 C96 C96 C91 SIMU 0.02 C81 > C96 MORE -1 FMAP 2 PLAN 20 SIZE 0.098 0.166 0.256 ACTA BOND $H CONF LIST 4 L.S. 40 TEMP -180.15 WGHT 0.019700 2.332500 FVAR 0.27741 RU1 7 0.589597 0.395952 0.755989 11.00000 0.00936 0.00793 = 0.00583 0.00014 0.00070 0.00120 CL1 6 0.688920 0.471760 0.671926 11.00000 0.01384 0.01246 = 0.01095 0.00110 0.00393 0.00059 CL2 6 0.477848 0.336746 0.840261 11.00000 0.01238 0.01299 = 0.00883 0.00136 0.00135 -0.00018 P1 5 0.695987 0.358822 0.858326 11.00000 0.01048 0.01028 = 0.00847 0.00070 -0.00020 0.00134 P2 5 0.586681 0.292526 0.662591 11.00000 0.01380 0.00927 = 0.00798 -0.00075 0.00085 0.00173 O1 4 0.503957 0.674265 0.620461 11.00000 0.02398 0.01646 = 0.01005 0.00221 0.00055 0.00514 O2 4 0.320153 0.560849 0.866114 11.00000 0.02198 0.02375 = 0.01065 -0.00253 0.00334 0.00610 N11 3 0.589889 0.505710 0.835860 11.00000 0.01120 0.00977 = 0.00764 -0.00012 0.00084 0.00024 N12 3 0.550393 0.596875 0.730119 11.00000 0.01494 0.00993 = 0.00778 -0.00031 0.00161 0.00180 H12 2 0.574561 0.563071 0.699073 11.00000 0.02282 N21 3 0.470989 0.432825 0.667884 11.00000 0.01102 0.01054 = 0.00745 0.00040 0.00104 0.00018 N22 3 0.388437 0.497297 0.764949 11.00000 0.01162 0.01378 = 0.00723 0.00039 0.00075 0.00243 H22 2 0.419589 0.467730 0.799741 11.00000 0.02060 C11 1 0.651627 0.414302 0.943862 11.00000 0.01448 0.01201 = 0.00829 0.00072 -0.00024 0.00182 AFIX 23 H11A 2 0.604025 0.381016 0.967440 11.00000 -1.20000 H11B 2 0.701909 0.423341 0.986745 11.00000 -1.20000 AFIX 0 C12 1 0.611628 0.494766 0.916638 11.00000 0.01074 0.01194 = 0.00864 0.00003 0.00053 -0.00058 C13 1 0.596826 0.554834 0.974552 11.00000 0.01470 0.01339 = 0.00831 -0.00100 0.00090 -0.00076 AFIX 43 H13 2 0.614594 0.545633 1.030499 11.00000 -1.20000 AFIX 0 C14 1 0.556174 0.627522 0.949537 11.00000 0.01478 0.01260 = 0.01013 -0.00259 0.00206 -0.00054 AFIX 43 H14 2 0.541687 0.667237 0.988412 11.00000 -1.20000 AFIX 0 C15 1 0.536552 0.642072 0.866412 11.00000 0.01236 0.01050 = 0.01020 -0.00142 0.00183 -0.00005 C16 1 0.494128 0.714876 0.832890 11.00000 0.01798 0.01144 = 0.01321 -0.00187 0.00204 0.00277 AFIX 43 H16 2 0.475872 0.756120 0.868644 11.00000 -1.20000 AFIX 0 C17 1 0.479569 0.726096 0.751729 11.00000 0.01856 0.01183 = 0.01378 -0.00051 0.00103 0.00415 AFIX 43 H17 2 0.448727 0.773751 0.731441 11.00000 -1.20000 AFIX 0 C18 1 0.510498 0.666154 0.694927 11.00000 0.01308 0.01069 = 0.01164 0.00060 0.00076 0.00047 C19 1 0.559941 0.581097 0.811894 11.00000 0.01032 0.01042 = 0.00858 -0.00003 0.00100 -0.00056 C21 1 0.545997 0.349017 0.570374 11.00000 0.01574 0.01275 = 0.00811 -0.00047 0.00162 0.00296 AFIX 23 H21A 2 0.597963 0.378017 0.548574 11.00000 -1.20000 H21B 2 0.520480 0.310375 0.528322 11.00000 -1.20000 AFIX 0 C22 1 0.473881 0.409258 0.589271 11.00000 0.01254 0.01067 = 0.00806 -0.00007 0.00114 -0.00022 C23 1 0.411482 0.437239 0.526487 11.00000 0.01438 0.01520 = 0.00764 0.00011 0.00010 0.00017 AFIX 43 H23 2 0.415182 0.418536 0.472328 11.00000 -1.20000 AFIX 0 C24 1 0.344661 0.492187 0.544096 11.00000 0.01340 0.01597 = 0.00908 0.00189 -0.00099 0.00082 AFIX 43 H24 2 0.303980 0.513985 0.501773 11.00000 -1.20000 AFIX 0 C25 1 0.337417 0.515448 0.624750 11.00000 0.01100 0.01346 = 0.00986 0.00142 0.00050 0.00085 C26 1 0.270940 0.572297 0.650195 11.00000 0.01475 0.01872 = 0.01313 0.00117 0.00005 0.00559 AFIX 43 H26 2 0.229647 0.597427 0.610375 11.00000 -1.20000 AFIX 0 C27 1 0.265823 0.590810 0.729375 11.00000 0.01572 0.01929 = 0.01488 -0.00023 0.00172 0.00689 AFIX 43 H27 2 0.223236 0.630762 0.744091 11.00000 -1.20000 AFIX 0 C28 1 0.324595 0.550494 0.792720 11.00000 0.01261 0.01433 = 0.01174 -0.00100 0.00224 0.00155 C29 1 0.399544 0.481047 0.684807 11.00000 0.01060 0.01047 = 0.00833 -0.00021 0.00068 -0.00055 C31 1 0.817978 0.391958 0.862967 11.00000 0.01174 0.01852 = 0.01546 0.00095 -0.00008 -0.00013 AFIX 13 H31 2 0.845170 0.369056 0.814157 11.00000 -1.20000 AFIX 0 C32 1 0.877841 0.363509 0.938729 11.00000 0.01538 0.02626 = 0.02509 0.00527 -0.00618 -0.00055 AFIX 137 H32A 2 0.850655 0.382094 0.987852 11.00000 -1.50000 H32B 2 0.939459 0.386473 0.937611 11.00000 -1.50000 H32C 2 0.881519 0.303848 0.938958 11.00000 -1.50000 AFIX 0 C33 1 0.822874 0.485463 0.857222 11.00000 0.01674 0.02021 = 0.02272 0.00431 -0.00240 -0.00513 AFIX 137 H33A 2 0.784925 0.504027 0.809073 11.00000 -1.50000 H33B 2 0.886470 0.502210 0.852825 11.00000 -1.50000 H33C 2 0.800344 0.509711 0.906108 11.00000 -1.50000 AFIX 0 C41 1 0.693470 0.250703 0.891968 11.00000 0.01599 0.01181 = 0.01422 0.00237 -0.00206 0.00212 AFIX 13 H41 2 0.630823 0.230465 0.873541 11.00000 -1.20000 AFIX 0 C42 1 0.704640 0.234997 0.984104 11.00000 0.02759 0.01724 = 0.01588 0.00621 -0.00059 0.00209 AFIX 137 H42A 2 0.765463 0.253107 1.005966 11.00000 -1.50000 H42B 2 0.697911 0.176570 0.994534 11.00000 -1.50000 H42C 2 0.657668 0.265298 1.010576 11.00000 -1.50000 AFIX 0 C43 1 0.759592 0.197287 0.847771 11.00000 0.02810 0.01630 = 0.02076 -0.00018 -0.00024 0.00913 AFIX 137 H43A 2 0.756189 0.212320 0.790084 11.00000 -1.50000 H43B 2 0.742642 0.139834 0.852951 11.00000 -1.50000 H43C 2 0.822189 0.205578 0.872039 11.00000 -1.50000 AFIX 0 C51 1 0.688641 0.238405 0.628213 11.00000 0.01998 0.01495 = 0.01465 -0.00231 0.00181 0.00671 AFIX 13 H51 2 0.701653 0.191566 0.666228 11.00000 -1.20000 AFIX 0 C52 1 0.774437 0.291716 0.633226 11.00000 0.01763 0.02427 = 0.03101 -0.00649 0.00643 0.00573 AFIX 137 H52A 2 0.765601 0.336939 0.594541 11.00000 -1.50000 H52B 2 0.827077 0.258945 0.619854 11.00000 -1.50000 H52C 2 0.785653 0.313451 0.688499 11.00000 -1.50000 AFIX 0 C53 1 0.673634 0.202595 0.542044 11.00000 0.02795 0.02921 = 0.01774 -0.00894 0.00348 0.01014 AFIX 137 H53A 2 0.619515 0.167282 0.538619 11.00000 -1.50000 H53B 2 0.727445 0.170663 0.530093 11.00000 -1.50000 H53C 2 0.664371 0.247002 0.502466 11.00000 -1.50000 AFIX 0 C61 1 0.504127 0.206607 0.662899 11.00000 0.02297 0.01207 = 0.01257 -0.00184 0.00072 -0.00321 AFIX 13 H61 2 0.513427 0.172356 0.614083 11.00000 -1.20000 AFIX 0 C62 1 0.404218 0.234535 0.655047 11.00000 0.02009 0.02197 = 0.01598 -0.00005 -0.00104 -0.00664 AFIX 137 H62A 2 0.391397 0.265763 0.703497 11.00000 -1.50000 H62B 2 0.363964 0.186783 0.649962 11.00000 -1.50000 H62C 2 0.393282 0.268954 0.606650 11.00000 -1.50000 AFIX 0 C63 1 0.522626 0.151785 0.737848 11.00000 0.03137 0.01255 = 0.01899 0.00228 0.00136 -0.00228 AFIX 137 H63A 2 0.586592 0.133777 0.741645 11.00000 -1.50000 H63B 2 0.482219 0.104133 0.732824 11.00000 -1.50000 H63C 2 0.510881 0.182435 0.786942 11.00000 -1.50000 AFIX 0 C71 1 0.227521 0.360028 0.784935 11.00000 0.01572 0.03177 = 0.03535 0.00710 -0.00252 -0.00450 AFIX 43 H71 2 0.281884 0.331579 0.802995 11.00000 -1.20000 AFIX 0 C72 1 0.198757 0.362443 0.702537 11.00000 0.02056 0.02680 = 0.02956 0.00021 0.00647 -0.00534 AFIX 43 H72 2 0.233758 0.336022 0.664241 11.00000 -1.20000 AFIX 0 C73 1 0.119239 0.403270 0.676265 11.00000 0.02923 0.01737 = 0.02060 0.00279 -0.00103 -0.00625 AFIX 43 H73 2 0.100091 0.405479 0.619864 11.00000 -1.20000 AFIX 0 C74 1 0.067274 0.441090 0.732281 11.00000 0.02894 0.01475 = 0.02832 0.00198 -0.00217 0.00162 AFIX 43 H74 2 0.011791 0.467872 0.714329 11.00000 -1.20000 AFIX 0 C75 1 0.096564 0.439672 0.814511 11.00000 0.03144 0.02120 = 0.02510 -0.00153 0.00578 -0.00375 AFIX 43 H75 2 0.061737 0.466379 0.852753 11.00000 -1.20000 AFIX 0 C76 1 0.176803 0.399187 0.840796 11.00000 0.02872 0.03016 = 0.02043 0.00565 -0.00281 -0.01067 AFIX 43 H76 2 0.196965 0.398304 0.897023 11.00000 -1.20000 AFIX 0 PART -1 SAME C71 > C76 C81 1 -0.070078 0.498089 0.545218 10.25000 0.02653 AFIX 43 H81 2 -0.119598 0.490563 0.578221 10.25000 -1.20000 AFIX 0 C82 1 -0.043083 0.434670 0.491899 10.25000 0.02334 AFIX 43 H82 2 -0.074690 0.384181 0.485958 10.25000 -1.20000 AFIX 0 C83 1 0.031833 0.452562 0.450197 10.25000 0.02079 AFIX 43 H83 2 0.051831 0.411363 0.415229 10.25000 -1.20000 AFIX 0 C84 1 0.081270 0.524985 0.454105 10.25000 0.01642 AFIX 43 H84 2 0.133457 0.531629 0.424144 10.25000 -1.20000 AFIX 0 C85 1 0.053506 0.585104 0.501124 10.25000 0.03483 AFIX 43 H85 2 0.084123 0.636207 0.503151 10.25000 -1.20000 AFIX 0 C86 1 -0.020374 0.572011 0.546817 10.25000 0.02007 AFIX 43 H86 2 -0.038511 0.614782 0.580875 10.25000 -1.20000 AFIX 0 PART -2 SAME C71 > C76 C91 1 -0.064653 0.517187 0.551732 10.25000 0.02273 AFIX 43 H91 2 -0.109181 0.535701 0.586245 10.25000 -1.20000 AFIX 0 C92 1 -0.069154 0.438624 0.517038 10.25000 0.02148 AFIX 43 H92 2 -0.116495 0.403412 0.531885 10.25000 -1.20000 AFIX 0 C93 1 -0.011634 0.409801 0.464625 10.25000 0.03485 AFIX 43 H93 2 -0.018961 0.356023 0.443704 10.25000 -1.20000 AFIX 0 C94 1 0.057083 0.457898 0.441656 10.25000 0.01839 AFIX 43 H94 2 0.096948 0.439920 0.402682 10.25000 -1.20000 AFIX 0 C95 1 0.066917 0.535094 0.477674 10.25000 0.02328 AFIX 43 H95 2 0.116647 0.567745 0.463279 10.25000 -1.20000 AFIX 0 C96 1 0.010242 0.567795 0.532488 10.25000 0.02954 AFIX 43 H96 2 0.020363 0.620319 0.555791 10.25000 -1.20000 PART 0 AFIX 0 HKLF 4 REM jk337 in P2(1)/n REM wR2 = 0.0494, GooF = S = 1.030, Restrained GooF = 1.034 for all data REM R1 = 0.0202 for 12713 Fo > 4sig(Fo) and 0.0224 for all 13567 data REM 488 parameters refined using 80 restraints END WGHT 0.0197 2.3326 REM Highest difference peak 0.804, deepest hole -0.717, 1-sigma level 0.057 Q1 1 -0.0348 0.4185 0.4724 11.00000 0.05 0.80 Q2 1 0.0135 0.3977 0.4573 11.00000 0.05 0.66 Q3 1 0.0778 0.5966 0.4869 11.00000 0.05 0.59 Q4 1 0.4401 0.4219 0.5593 11.00000 0.05 0.52 Q5 1 0.5191 0.6781 0.8497 11.00000 0.05 0.50 Q6 1 0.3434 0.5016 0.5855 11.00000 0.05 0.47 Q7 1 0.3774 0.4638 0.5379 11.00000 0.05 0.47 Q8 1 0.5443 0.6348 0.9050 11.00000 0.05 0.47 Q9 1 0.3657 0.4971 0.6533 11.00000 0.05 0.46 Q10 1 0.5772 0.4389 0.7430 11.00000 0.05 0.46 Q11 1 0.4951 0.6977 0.7243 11.00000 0.05 0.46 Q12 1 0.5423 0.6080 0.8416 11.00000 0.05 0.45 Q13 1 0.0477 0.5380 0.4959 11.00000 0.05 0.44 Q14 1 0.6077 0.5244 0.9448 11.00000 0.05 0.44 Q15 1 0.3040 0.5374 0.6356 11.00000 0.05 0.44 Q16 1 0.1574 0.3822 0.6924 11.00000 0.05 0.44 Q17 1 0.6018 0.3529 0.7758 11.00000 0.05 0.43 Q18 1 0.5823 0.5928 0.9628 11.00000 0.05 0.42 Q19 1 0.5722 0.5408 0.8250 11.00000 0.05 0.41 Q20 1 0.6344 0.4555 0.9287 11.00000 0.05 0.40 ; _shelx_res_checksum 45699 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.58960(2) 0.39595(2) 0.75599(2) 0.00770(2) Uani 1 1 d . . . . . Cl1 Cl 0.68892(2) 0.47176(2) 0.67193(2) 0.01226(4) Uani 1 1 d . . . . . Cl2 Cl 0.47785(2) 0.33675(2) 0.84026(2) 0.01138(4) Uani 1 1 d . . . . . P1 P 0.69599(2) 0.35882(2) 0.85833(2) 0.00980(4) Uani 1 1 d . . . . . P2 P 0.58668(2) 0.29253(2) 0.66259(2) 0.01035(4) Uani 1 1 d . . . . . O1 O 0.50396(5) 0.67427(5) 0.62046(4) 0.01687(14) Uani 1 1 d . . . . . O2 O 0.32015(5) 0.56085(5) 0.86611(4) 0.01869(14) Uani 1 1 d . . . . . N11 N 0.58989(5) 0.50571(5) 0.83586(5) 0.00953(13) Uani 1 1 d . . . . . N12 N 0.55039(6) 0.59688(5) 0.73012(5) 0.01085(13) Uani 1 1 d D . . . . H12 H 0.5746(10) 0.5631(9) 0.6991(9) 0.023(4) Uiso 1 1 d D . . . . N21 N 0.47099(5) 0.43283(5) 0.66788(4) 0.00965(13) Uani 1 1 d . . . . . N22 N 0.38844(5) 0.49730(5) 0.76495(5) 0.01088(13) Uani 1 1 d D . . . . H22 H 0.4196(10) 0.4677(9) 0.7997(8) 0.021(3) Uiso 1 1 d D . . . . C11 C 0.65163(6) 0.41430(6) 0.94386(5) 0.01166(15) Uani 1 1 d . . . . . H11A H 0.604025 0.381016 0.967440 0.014 Uiso 1 1 calc R U . . . H11B H 0.701909 0.423341 0.986745 0.014 Uiso 1 1 calc R U . . . C12 C 0.61163(6) 0.49477(6) 0.91664(5) 0.01045(15) Uani 1 1 d . . . . . C13 C 0.59683(6) 0.55483(6) 0.97455(5) 0.01213(15) Uani 1 1 d . . . . . H13 H 0.614594 0.545633 1.030499 0.015 Uiso 1 1 calc R U . . . C14 C 0.55617(6) 0.62752(6) 0.94954(6) 0.01245(16) Uani 1 1 d . . . . . H14 H 0.541687 0.667237 0.988412 0.015 Uiso 1 1 calc R U . . . C15 C 0.53655(6) 0.64207(5) 0.86641(5) 0.01097(15) Uani 1 1 d . . . . . C16 C 0.49413(7) 0.71488(6) 0.83289(6) 0.01417(16) Uani 1 1 d . . . . . H16 H 0.475872 0.756120 0.868644 0.017 Uiso 1 1 calc R U . . . C17 C 0.47957(7) 0.72610(6) 0.75173(6) 0.01474(17) Uani 1 1 d . . . . . H17 H 0.448727 0.773751 0.731441 0.018 Uiso 1 1 calc R U . . . C18 C 0.51050(6) 0.66615(6) 0.69493(6) 0.01182(15) Uani 1 1 d . . . . . C19 C 0.55994(6) 0.58110(5) 0.81189(5) 0.00976(14) Uani 1 1 d . . . . . C21 C 0.54600(6) 0.34902(6) 0.57037(5) 0.01216(15) Uani 1 1 d . . . . . H21A H 0.597963 0.378017 0.548574 0.015 Uiso 1 1 calc R U . . . H21B H 0.520480 0.310375 0.528322 0.015 Uiso 1 1 calc R U . . . C22 C 0.47388(6) 0.40926(5) 0.58927(5) 0.01041(15) Uani 1 1 d . . . . . C23 C 0.41148(6) 0.43724(6) 0.52649(5) 0.01245(16) Uani 1 1 d . . . . . H23 H 0.415182 0.418536 0.472328 0.015 Uiso 1 1 calc R U . . . C24 C 0.34466(6) 0.49219(6) 0.54410(6) 0.01292(16) Uani 1 1 d . . . . . H24 H 0.303980 0.513985 0.501773 0.016 Uiso 1 1 calc R U . . . C25 C 0.33742(6) 0.51545(6) 0.62475(5) 0.01146(15) Uani 1 1 d . . . . . C26 C 0.27094(7) 0.57230(6) 0.65020(6) 0.01560(17) Uani 1 1 d . . . . . H26 H 0.229647 0.597427 0.610375 0.019 Uiso 1 1 calc R U . . . C27 C 0.26582(7) 0.59081(6) 0.72938(6) 0.01660(18) Uani 1 1 d . . . . . H27 H 0.223236 0.630762 0.744091 0.020 Uiso 1 1 calc R U . . . C28 C 0.32460(6) 0.55049(6) 0.79272(6) 0.01283(16) Uani 1 1 d . . . . . C29 C 0.39954(6) 0.48105(5) 0.68481(5) 0.00980(14) Uani 1 1 d . . . . . C31 C 0.81798(6) 0.39196(6) 0.86297(6) 0.01530(17) Uani 1 1 d . . . . . H31 H 0.845170 0.369056 0.814157 0.018 Uiso 1 1 calc R U . . . C32 C 0.87784(7) 0.36351(7) 0.93873(7) 0.0227(2) Uani 1 1 d . . . . . H32A H 0.850655 0.382094 0.987852 0.034 Uiso 1 1 calc R U . . . H32B H 0.939459 0.386473 0.937611 0.034 Uiso 1 1 calc R U . . . H32C H 0.881519 0.303848 0.938958 0.034 Uiso 1 1 calc R U . . . C33 C 0.82287(7) 0.48546(7) 0.85722(7) 0.02011(19) Uani 1 1 d . . . . . H33A H 0.784925 0.504027 0.809073 0.030 Uiso 1 1 calc R U . . . H33B H 0.886470 0.502210 0.852825 0.030 Uiso 1 1 calc R U . . . H33C H 0.800344 0.509711 0.906108 0.030 Uiso 1 1 calc R U . . . C41 C 0.69347(7) 0.25070(6) 0.89197(6) 0.01419(16) Uani 1 1 d . . . . . H41 H 0.630823 0.230465 0.873541 0.017 Uiso 1 1 calc R U . . . C42 C 0.70464(8) 0.23500(7) 0.98410(6) 0.0204(2) Uani 1 1 d . . . . . H42A H 0.765463 0.253107 1.005966 0.031 Uiso 1 1 calc R U . . . H42B H 0.697911 0.176570 0.994534 0.031 Uiso 1 1 calc R U . . . H42C H 0.657668 0.265298 1.010576 0.031 Uiso 1 1 calc R U . . . C43 C 0.75959(8) 0.19729(7) 0.84777(7) 0.0218(2) Uani 1 1 d . . . . . H43A H 0.756189 0.212320 0.790084 0.033 Uiso 1 1 calc R U . . . H43B H 0.742642 0.139834 0.852951 0.033 Uiso 1 1 calc R U . . . H43C H 0.822189 0.205578 0.872039 0.033 Uiso 1 1 calc R U . . . C51 C 0.68864(7) 0.23841(6) 0.62821(6) 0.01651(17) Uani 1 1 d . . . . . H51 H 0.701653 0.191566 0.666228 0.020 Uiso 1 1 calc R U . . . C52 C 0.77444(8) 0.29172(7) 0.63323(8) 0.0241(2) Uani 1 1 d . . . . . H52A H 0.765601 0.336939 0.594541 0.036 Uiso 1 1 calc R U . . . H52B H 0.827077 0.258945 0.619854 0.036 Uiso 1 1 calc R U . . . H52C H 0.785653 0.313451 0.688499 0.036 Uiso 1 1 calc R U . . . C53 C 0.67363(8) 0.20259(8) 0.54204(7) 0.0249(2) Uani 1 1 d . . . . . H53A H 0.619515 0.167282 0.538619 0.037 Uiso 1 1 calc R U . . . H53B H 0.727445 0.170663 0.530093 0.037 Uiso 1 1 calc R U . . . H53C H 0.664371 0.247002 0.502466 0.037 Uiso 1 1 calc R U . . . C61 C 0.50413(7) 0.20661(6) 0.66290(6) 0.01591(17) Uani 1 1 d . . . . . H61 H 0.513427 0.172356 0.614083 0.019 Uiso 1 1 calc R U . . . C62 C 0.40422(7) 0.23454(7) 0.65505(6) 0.01948(19) Uani 1 1 d . . . . . H62A H 0.391397 0.265763 0.703497 0.029 Uiso 1 1 calc R U . . . H62B H 0.363964 0.186783 0.649962 0.029 Uiso 1 1 calc R U . . . H62C H 0.393282 0.268954 0.606650 0.029 Uiso 1 1 calc R U . . . C63 C 0.52263(8) 0.15179(6) 0.73785(7) 0.0210(2) Uani 1 1 d . . . . . H63A H 0.586592 0.133777 0.741645 0.032 Uiso 1 1 calc R U . . . H63B H 0.482219 0.104133 0.732824 0.032 Uiso 1 1 calc R U . . . H63C H 0.510881 0.182435 0.786942 0.032 Uiso 1 1 calc R U . . . C71 C 0.22752(8) 0.36003(8) 0.78493(8) 0.0279(2) Uani 1 1 d D . . . . H71 H 0.281884 0.331579 0.802995 0.033 Uiso 1 1 calc R U . . . C72 C 0.19876(8) 0.36244(8) 0.70254(8) 0.0254(2) Uani 1 1 d D . . . . H72 H 0.233758 0.336022 0.664241 0.030 Uiso 1 1 calc R U . . . C73 C 0.11924(8) 0.40327(7) 0.67626(7) 0.0226(2) Uani 1 1 d D . . . . H73 H 0.100091 0.405479 0.619864 0.027 Uiso 1 1 calc R U . . . C74 C 0.06727(9) 0.44109(7) 0.73228(8) 0.0242(2) Uani 1 1 d D . . . . H74 H 0.011791 0.467872 0.714329 0.029 Uiso 1 1 calc R U . . . C75 C 0.09656(9) 0.43967(7) 0.81451(8) 0.0257(2) Uani 1 1 d D . . . . H75 H 0.061737 0.466379 0.852753 0.031 Uiso 1 1 calc R U . . . C76 C 0.17680(9) 0.39919(8) 0.84080(7) 0.0267(2) Uani 1 1 d D . . . . H76 H 0.196965 0.398304 0.897023 0.032 Uiso 1 1 calc R U . . . C81 C -0.0701(5) 0.4981(5) 0.5452(5) 0.0265(16) Uiso 0.25 1 d D U P A -1 H81 H -0.119598 0.490563 0.578221 0.032 Uiso 0.25 1 calc R U P A -1 C82 C -0.0431(5) 0.4347(4) 0.4919(4) 0.0233(11) Uiso 0.25 1 d D U P A -1 H82 H -0.074690 0.384181 0.485958 0.028 Uiso 0.25 1 calc R U P A -1 C83 C 0.0318(5) 0.4526(4) 0.4502(4) 0.0208(11) Uiso 0.25 1 d D U P A -1 H83 H 0.051831 0.411363 0.415229 0.025 Uiso 0.25 1 calc R U P A -1 C84 C 0.0813(3) 0.5250(4) 0.4541(3) 0.0164(9) Uiso 0.25 1 d D U P A -1 H84 H 0.133457 0.531629 0.424144 0.020 Uiso 0.25 1 calc R U P A -1 C85 C 0.0535(5) 0.5851(5) 0.5011(5) 0.0348(15) Uiso 0.25 1 d D U P A -1 H85 H 0.084123 0.636207 0.503151 0.042 Uiso 0.25 1 calc R U P A -1 C86 C -0.0204(5) 0.5720(4) 0.5468(3) 0.0201(10) Uiso 0.25 1 d D U P A -1 H86 H -0.038511 0.614782 0.580875 0.024 Uiso 0.25 1 calc R U P A -1 C91 C -0.0647(5) 0.5172(5) 0.5517(4) 0.0227(13) Uiso 0.25 1 d D U P B -2 H91 H -0.109181 0.535701 0.586245 0.027 Uiso 0.25 1 calc R U P B -2 C92 C -0.0692(4) 0.4386(4) 0.5170(4) 0.0215(10) Uiso 0.25 1 d D U P B -2 H92 H -0.116495 0.403412 0.531885 0.026 Uiso 0.25 1 calc R U P B -2 C93 C -0.0116(5) 0.4098(5) 0.4646(4) 0.0348(16) Uiso 0.25 1 d D U P B -2 H93 H -0.018961 0.356023 0.443704 0.042 Uiso 0.25 1 calc R U P B -2 C94 C 0.0571(4) 0.4579(4) 0.4417(3) 0.0184(10) Uiso 0.25 1 d D U P B -2 H94 H 0.096948 0.439920 0.402682 0.022 Uiso 0.25 1 calc R U P B -2 C95 C 0.0669(4) 0.5351(4) 0.4777(4) 0.0233(11) Uiso 0.25 1 d D U P B -2 H95 H 0.116647 0.567745 0.463279 0.028 Uiso 0.25 1 calc R U P B -2 C96 C 0.0102(5) 0.5678(4) 0.5325(4) 0.0295(14) Uiso 0.25 1 d D U P B -2 H96 H 0.020363 0.620319 0.555791 0.035 Uiso 0.25 1 calc R U P B -2 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 0.00936(3) 0.00793(3) 0.00583(3) 0.00014(2) 0.00070(2) 0.00120(2) Cl1 0.01384(9) 0.01246(9) 0.01095(9) 0.00110(7) 0.00393(7) 0.00059(7) Cl2 0.01238(9) 0.01299(9) 0.00883(8) 0.00136(7) 0.00135(7) -0.00018(7) P1 0.01048(9) 0.01028(9) 0.00847(9) 0.00070(7) -0.00020(7) 0.00134(7) P2 0.01380(10) 0.00927(9) 0.00798(9) -0.00075(7) 0.00085(7) 0.00173(8) O1 0.0240(4) 0.0165(3) 0.0101(3) 0.0022(2) 0.0006(3) 0.0051(3) O2 0.0220(4) 0.0237(4) 0.0107(3) -0.0025(3) 0.0033(3) 0.0061(3) N11 0.0112(3) 0.0098(3) 0.0076(3) -0.0001(2) 0.0008(2) 0.0002(2) N12 0.0149(3) 0.0099(3) 0.0078(3) -0.0003(3) 0.0016(3) 0.0018(3) N21 0.0110(3) 0.0105(3) 0.0075(3) 0.0004(2) 0.0010(2) 0.0002(2) N22 0.0116(3) 0.0138(3) 0.0072(3) 0.0004(3) 0.0008(3) 0.0024(3) C11 0.0145(4) 0.0120(4) 0.0083(4) 0.0007(3) -0.0002(3) 0.0018(3) C12 0.0107(3) 0.0119(4) 0.0086(4) 0.0000(3) 0.0005(3) -0.0006(3) C13 0.0147(4) 0.0134(4) 0.0083(4) -0.0010(3) 0.0009(3) -0.0008(3) C14 0.0148(4) 0.0126(4) 0.0101(4) -0.0026(3) 0.0021(3) -0.0005(3) C15 0.0124(4) 0.0105(4) 0.0102(4) -0.0014(3) 0.0018(3) -0.0001(3) C16 0.0180(4) 0.0114(4) 0.0132(4) -0.0019(3) 0.0020(3) 0.0028(3) C17 0.0186(4) 0.0118(4) 0.0138(4) -0.0005(3) 0.0010(3) 0.0041(3) C18 0.0131(4) 0.0107(4) 0.0116(4) 0.0006(3) 0.0008(3) 0.0005(3) C19 0.0103(3) 0.0104(3) 0.0086(4) 0.0000(3) 0.0010(3) -0.0006(3) C21 0.0157(4) 0.0127(4) 0.0081(4) -0.0005(3) 0.0016(3) 0.0030(3) C22 0.0125(4) 0.0107(4) 0.0081(4) -0.0001(3) 0.0011(3) -0.0002(3) C23 0.0144(4) 0.0152(4) 0.0076(4) 0.0001(3) 0.0001(3) 0.0002(3) C24 0.0134(4) 0.0160(4) 0.0091(4) 0.0019(3) -0.0010(3) 0.0008(3) C25 0.0110(4) 0.0135(4) 0.0099(4) 0.0014(3) 0.0005(3) 0.0009(3) C26 0.0148(4) 0.0187(4) 0.0131(4) 0.0012(3) 0.0001(3) 0.0056(3) C27 0.0157(4) 0.0193(4) 0.0149(4) -0.0002(3) 0.0017(3) 0.0069(3) C28 0.0126(4) 0.0143(4) 0.0117(4) -0.0010(3) 0.0022(3) 0.0016(3) C29 0.0106(3) 0.0105(3) 0.0083(4) -0.0002(3) 0.0007(3) -0.0006(3) C31 0.0117(4) 0.0185(4) 0.0155(4) 0.0009(3) -0.0001(3) -0.0001(3) C32 0.0154(4) 0.0263(5) 0.0251(5) 0.0053(4) -0.0062(4) -0.0005(4) C33 0.0167(4) 0.0202(5) 0.0227(5) 0.0043(4) -0.0024(4) -0.0051(4) C41 0.0160(4) 0.0118(4) 0.0142(4) 0.0024(3) -0.0021(3) 0.0021(3) C42 0.0276(5) 0.0172(4) 0.0159(4) 0.0062(4) -0.0006(4) 0.0021(4) C43 0.0281(5) 0.0163(4) 0.0208(5) -0.0002(4) -0.0002(4) 0.0091(4) C51 0.0200(4) 0.0150(4) 0.0147(4) -0.0023(3) 0.0018(3) 0.0067(3) C52 0.0176(5) 0.0243(5) 0.0310(6) -0.0065(4) 0.0064(4) 0.0057(4) C53 0.0280(5) 0.0292(6) 0.0177(5) -0.0089(4) 0.0035(4) 0.0101(4) C61 0.0230(5) 0.0121(4) 0.0126(4) -0.0018(3) 0.0007(3) -0.0032(3) C62 0.0201(5) 0.0220(5) 0.0160(4) -0.0001(4) -0.0010(4) -0.0066(4) C63 0.0314(5) 0.0126(4) 0.0190(5) 0.0023(4) 0.0014(4) -0.0023(4) C71 0.0157(5) 0.0318(6) 0.0353(6) 0.0071(5) -0.0025(4) -0.0045(4) C72 0.0206(5) 0.0268(6) 0.0296(6) 0.0002(5) 0.0065(4) -0.0053(4) C73 0.0292(5) 0.0174(5) 0.0206(5) 0.0028(4) -0.0010(4) -0.0063(4) C74 0.0289(5) 0.0148(4) 0.0283(6) 0.0020(4) -0.0022(4) 0.0016(4) C75 0.0314(6) 0.0212(5) 0.0251(5) -0.0015(4) 0.0058(4) -0.0038(4) C76 0.0287(6) 0.0302(6) 0.0204(5) 0.0057(4) -0.0028(4) -0.0107(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N11 Ru1 N21 97.37(3) . . ? N11 Ru1 P1 79.09(2) . . ? N21 Ru1 P1 172.29(2) . . ? N11 Ru1 P2 173.93(2) . . ? N21 Ru1 P2 78.12(2) . . ? P1 Ru1 P2 105.877(9) . . ? N11 Ru1 Cl1 87.22(2) . . ? N21 Ru1 Cl1 87.79(2) . . ? P1 Ru1 Cl1 98.807(8) . . ? P2 Ru1 Cl1 88.545(8) . . ? N11 Ru1 Cl2 87.36(2) . . ? N21 Ru1 Cl2 87.46(2) . . ? P1 Ru1 Cl2 85.552(8) . . ? P2 Ru1 Cl2 96.426(8) . . ? Cl1 Ru1 Cl2 172.276(8) . . ? C11 P1 C41 103.06(4) . . ? C11 P1 C31 102.82(4) . . ? C41 P1 C31 107.94(4) . . ? C11 P1 Ru1 99.89(3) . . ? C41 P1 Ru1 116.46(3) . . ? C31 P1 Ru1 123.16(3) . . ? C21 P2 C61 102.55(4) . . ? C21 P2 C51 101.67(4) . . ? C61 P2 C51 100.25(5) . . ? C21 P2 Ru1 99.79(3) . . ? C61 P2 Ru1 122.46(3) . . ? C51 P2 Ru1 125.84(3) . . ? C12 N11 C19 116.76(8) . . ? C12 N11 Ru1 117.53(6) . . ? C19 N11 Ru1 125.26(6) . . ? C19 N12 C18 125.04(8) . . ? C19 N12 H12 117.1(10) . . ? C18 N12 H12 117.7(10) . . ? C22 N21 C29 116.52(8) . . ? C22 N21 Ru1 117.17(6) . . ? C29 N21 Ru1 126.16(6) . . ? C29 N22 C28 125.31(8) . . ? C29 N22 H22 116.0(10) . . ? C28 N22 H22 118.3(10) . . ? C12 C11 P1 111.09(6) . . ? C12 C11 H11A 109.4 . . ? P1 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? P1 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N11 C12 C13 122.64(8) . . ? N11 C12 C11 117.77(8) . . ? C13 C12 C11 119.59(8) . . ? C14 C13 C12 119.37(8) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 119.32(8) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C19 117.66(8) . . ? C14 C15 C16 124.57(8) . . ? C19 C15 C16 117.77(8) . . ? C17 C16 C15 121.55(9) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 120.89(9) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? O1 C18 N12 120.20(8) . . ? O1 C18 C17 124.46(9) . . ? N12 C18 C17 115.34(8) . . ? N11 C19 N12 117.57(8) . . ? N11 C19 C15 123.42(8) . . ? N12 C19 C15 119.00(8) . . ? C22 C21 P2 110.31(6) . . ? C22 C21 H21A 109.6 . . ? P2 C21 H21A 109.6 . . ? C22 C21 H21B 109.6 . . ? P2 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? N21 C22 C23 122.90(8) . . ? N21 C22 C21 117.66(8) . . ? C23 C22 C21 119.42(8) . . ? C24 C23 C22 119.35(8) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C23 C24 C25 119.32(8) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C29 117.76(8) . . ? C24 C25 C26 124.20(8) . . ? C29 C25 C26 118.05(8) . . ? C27 C26 C25 121.45(9) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 121.04(9) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? O2 C28 N22 120.29(9) . . ? O2 C28 C27 124.57(9) . . ? N22 C28 C27 115.14(8) . . ? N21 C29 N22 117.71(8) . . ? N21 C29 C25 123.63(8) . . ? N22 C29 C25 118.66(8) . . ? C33 C31 C32 109.01(9) . . ? C33 C31 P1 109.72(7) . . ? C32 C31 P1 115.23(7) . . ? C33 C31 H31 107.5 . . ? C32 C31 H31 107.5 . . ? P1 C31 H31 107.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C43 C41 C42 110.70(8) . . ? C43 C41 P1 111.98(7) . . ? C42 C41 P1 116.86(7) . . ? C43 C41 H41 105.4 . . ? C42 C41 H41 105.4 . . ? P1 C41 H41 105.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C52 C51 C53 108.89(9) . . ? C52 C51 P2 112.78(7) . . ? C53 C51 P2 113.89(7) . . ? C52 C51 H51 107.0 . . ? C53 C51 H51 107.0 . . ? P2 C51 H51 107.0 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C62 C61 C63 110.41(9) . . ? C62 C61 P2 113.07(7) . . ? C63 C61 P2 111.98(7) . . ? C62 C61 H61 107.0 . . ? C63 C61 H61 107.0 . . ? P2 C61 H61 107.0 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C76 C71 C72 119.97(11) . . ? C76 C71 H71 120.0 . . ? C72 C71 H71 120.0 . . ? C73 C72 C71 120.05(12) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.08(11) . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C75 C74 C73 119.92(11) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C76 C75 C74 119.95(11) . . ? C76 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C71 C76 C75 120.00(11) . . ? C71 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C86 C81 C82 117.7(6) . . ? C86 C81 H81 121.2 . . ? C82 C81 H81 121.2 . . ? C83 C82 C81 115.0(6) . . ? C83 C82 H82 122.5 . . ? C81 C82 H82 122.5 . . ? C82 C83 C84 126.4(5) . . ? C82 C83 H83 116.8 . . ? C84 C83 H83 116.8 . . ? C85 C84 C83 118.3(6) . . ? C85 C84 H84 120.8 . . ? C83 C84 H84 120.8 . . ? C84 C85 C86 119.3(6) . . ? C84 C85 H85 120.4 . . ? C86 C85 H85 120.4 . . ? C85 C86 C81 123.2(6) . . ? C85 C86 H86 118.4 . . ? C81 C86 H86 118.4 . . ? C92 C91 C96 116.8(6) . . ? C92 C91 H91 121.6 . . ? C96 C91 H91 121.6 . . ? C93 C92 C91 124.9(6) . . ? C93 C92 H92 117.5 . . ? C91 C92 H92 117.5 . . ? C92 C93 C94 119.6(6) . . ? C92 C93 H93 120.2 . . ? C94 C93 H93 120.2 . . ? C93 C94 C95 117.4(6) . . ? C93 C94 H94 121.3 . . ? C95 C94 H94 121.3 . . ? C96 C95 C94 125.5(6) . . ? C96 C95 H95 117.3 . . ? C94 C95 H95 117.3 . . ? C95 C96 C91 115.6(6) . . ? C95 C96 H96 122.2 . . ? C91 C96 H96 122.2 . . ? 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 N11 2.2303(8) . ? Ru1 N21 2.2553(8) . ? Ru1 P1 2.2849(2) . ? Ru1 P2 2.2892(2) . ? Ru1 Cl1 2.4321(2) . ? Ru1 Cl2 2.4346(2) . ? P1 C11 1.8411(9) . ? P1 C41 1.8593(10) . ? P1 C31 1.8642(10) . ? P2 C21 1.8381(9) . ? P2 C61 1.8576(10) . ? P2 C51 1.8655(10) . ? O1 C18 1.2311(11) . ? O2 C28 1.2291(11) . ? N11 C12 1.3560(11) . ? N11 C19 1.3599(11) . ? N12 C19 1.3690(11) . ? N12 C18 1.3836(12) . ? N12 H12 0.851(13) . ? N21 C22 1.3567(11) . ? N21 C29 1.3592(11) . ? N22 C29 1.3708(11) . ? N22 C28 1.3843(12) . ? N22 H22 0.854(13) . ? C11 C12 1.4980(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.4012(12) . ? C13 C14 1.3807(13) . ? C13 H13 0.9500 . ? C14 C15 1.3979(12) . ? C14 H14 0.9500 . ? C15 C19 1.4057(12) . ? C15 C16 1.4359(13) . ? C16 C17 1.3505(13) . ? C16 H16 0.9500 . ? C17 C18 1.4555(13) . ? C17 H17 0.9500 . ? C21 C22 1.4980(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.4016(12) . ? C23 C24 1.3791(13) . ? C23 H23 0.9500 . ? C24 C25 1.3959(13) . ? C24 H24 0.9500 . ? C25 C29 1.4075(12) . ? C25 C26 1.4357(13) . ? C26 C27 1.3485(14) . ? C26 H26 0.9500 . ? C27 C28 1.4572(13) . ? C27 H27 0.9500 . ? C31 C33 1.5386(15) . ? C31 C32 1.5393(14) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C43 1.5339(14) . ? C41 C42 1.5365(14) . ? C41 H41 1.0000 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 C52 1.5282(16) . ? C51 C53 1.5367(15) . ? C51 H51 1.0000 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C62 1.5296(15) . ? C61 C63 1.5345(14) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C71 C76 1.3875(19) . ? C71 C72 1.3900(18) . ? C71 H71 0.9500 . ? C72 C73 1.3827(17) . ? C72 H72 0.9500 . ? C73 C74 1.3902(17) . ? C73 H73 0.9500 . ? C74 C75 1.3887(17) . ? C74 H74 0.9500 . ? C75 C76 1.3887(18) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.414(7) . ? C81 C82 1.438(7) . ? C81 H81 0.9500 . ? C82 C83 1.374(7) . ? C82 H82 0.9500 . ? C83 C84 1.390(7) . ? C83 H83 0.9500 . ? C84 C85 1.338(7) . ? C84 H84 0.9500 . ? C85 C86 1.385(7) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 C92 1.409(7) . ? C91 C96 1.432(7) . ? C91 H91 0.9500 . ? C92 C93 1.342(7) . ? C92 H92 0.9500 . ? C93 C94 1.357(7) . ? C93 H93 0.9500 . ? C94 C95 1.401(7) . ? C94 H94 0.9500 . ? C95 C96 1.385(7) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? 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 _geom_hbond_publ_flag N12 H12 Cl1 0.851(13) 2.318(14) 3.0937(8) 151.6(14) . yes N22 H22 Cl2 0.854(13) 2.387(14) 3.1509(8) 149.1(13) . yes 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 C41 P1 C11 C12 -156.19(6) . . . . ? C31 P1 C11 C12 91.65(7) . . . . ? Ru1 P1 C11 C12 -35.88(7) . . . . ? C19 N11 C12 C13 5.62(13) . . . . ? Ru1 N11 C12 C13 -167.04(7) . . . . ? C19 N11 C12 C11 -175.36(8) . . . . ? Ru1 N11 C12 C11 11.98(10) . . . . ? P1 C11 C12 N11 17.95(10) . . . . ? P1 C11 C12 C13 -163.00(7) . . . . ? N11 C12 C13 C14 1.88(14) . . . . ? C11 C12 C13 C14 -177.12(8) . . . . ? C12 C13 C14 C15 -4.53(14) . . . . ? C13 C14 C15 C19 -0.24(13) . . . . ? C13 C14 C15 C16 179.70(9) . . . . ? C14 C15 C16 C17 177.97(10) . . . . ? C19 C15 C16 C17 -2.09(14) . . . . ? C15 C16 C17 C18 -2.98(15) . . . . ? C19 N12 C18 O1 -179.00(9) . . . . ? C19 N12 C18 C17 1.72(13) . . . . ? C16 C17 C18 O1 -176.00(10) . . . . ? C16 C17 C18 N12 3.24(14) . . . . ? C12 N11 C19 N12 170.73(8) . . . . ? Ru1 N11 C19 N12 -17.25(11) . . . . ? C12 N11 C19 C15 -10.85(13) . . . . ? Ru1 N11 C19 C15 161.18(7) . . . . ? C18 N12 C19 N11 171.70(8) . . . . ? C18 N12 C19 C15 -6.80(14) . . . . ? C14 C15 C19 N11 8.30(13) . . . . ? C16 C15 C19 N11 -171.64(8) . . . . ? C14 C15 C19 N12 -173.30(8) . . . . ? C16 C15 C19 N12 6.76(13) . . . . ? C61 P2 C21 C22 87.10(7) . . . . ? C51 P2 C21 C22 -169.48(7) . . . . ? Ru1 P2 C21 C22 -39.52(7) . . . . ? C29 N21 C22 C23 4.79(13) . . . . ? Ru1 N21 C22 C23 -171.03(7) . . . . ? C29 N21 C22 C21 -173.62(8) . . . . ? Ru1 N21 C22 C21 10.55(10) . . . . ? P2 C21 C22 N21 21.14(10) . . . . ? P2 C21 C22 C23 -157.33(7) . . . . ? N21 C22 C23 C24 1.08(14) . . . . ? C21 C22 C23 C24 179.47(9) . . . . ? C22 C23 C24 C25 -3.44(14) . . . . ? C23 C24 C25 C29 -0.06(13) . . . . ? C23 C24 C25 C26 179.74(9) . . . . ? C24 C25 C26 C27 178.29(10) . . . . ? C29 C25 C26 C27 -1.92(15) . . . . ? C25 C26 C27 C28 -3.25(16) . . . . ? C29 N22 C28 O2 -179.99(9) . . . . ? C29 N22 C28 C27 0.21(14) . . . . ? C26 C27 C28 O2 -175.67(10) . . . . ? C26 C27 C28 N22 4.12(15) . . . . ? C22 N21 C29 N22 171.95(8) . . . . ? Ru1 N21 C29 N22 -12.65(11) . . . . ? C22 N21 C29 C25 -8.64(13) . . . . ? Ru1 N21 C29 C25 166.76(7) . . . . ? C28 N22 C29 N21 174.15(8) . . . . ? C28 N22 C29 C25 -5.29(14) . . . . ? C24 C25 C29 N21 6.42(14) . . . . ? C26 C25 C29 N21 -173.39(9) . . . . ? C24 C25 C29 N22 -174.18(8) . . . . ? C26 C25 C29 N22 6.01(13) . . . . ? C11 P1 C31 C33 -57.06(8) . . . . ? C41 P1 C31 C33 -165.55(7) . . . . ? Ru1 P1 C31 C33 53.99(8) . . . . ? C11 P1 C31 C32 66.41(9) . . . . ? C41 P1 C31 C32 -42.09(9) . . . . ? Ru1 P1 C31 C32 177.45(6) . . . . ? C11 P1 C41 C43 -158.06(7) . . . . ? C31 P1 C41 C43 -49.73(8) . . . . ? Ru1 P1 C41 C43 93.73(7) . . . . ? C11 P1 C41 C42 -28.88(9) . . . . ? C31 P1 C41 C42 79.45(8) . . . . ? Ru1 P1 C41 C42 -137.09(7) . . . . ? C21 P2 C51 C52 82.87(8) . . . . ? C61 P2 C51 C52 -171.89(8) . . . . ? Ru1 P2 C51 C52 -28.44(9) . . . . ? C21 P2 C51 C53 -41.89(9) . . . . ? C61 P2 C51 C53 63.35(9) . . . . ? Ru1 P2 C51 C53 -153.20(7) . . . . ? C21 P2 C61 C62 -52.25(8) . . . . ? C51 P2 C61 C62 -156.78(7) . . . . ? Ru1 P2 C61 C62 58.12(8) . . . . ? C21 P2 C61 C63 -177.75(7) . . . . ? C51 P2 C61 C63 77.73(8) . . . . ? Ru1 P2 C61 C63 -67.38(8) . . . . ? C76 C71 C72 C73 -0.53(18) . . . . ? C71 C72 C73 C74 -0.83(17) . . . . ? C72 C73 C74 C75 1.70(17) . . . . ? C73 C74 C75 C76 -1.20(18) . . . . ? C72 C71 C76 C75 1.02(18) . . . . ? C74 C75 C76 C71 -0.15(18) . . . . ? C86 C81 C82 C83 2.5(9) . . . . ? C81 C82 C83 C84 -1.1(9) . . . . ? C82 C83 C84 C85 -1.7(9) . . . . ? C83 C84 C85 C86 2.9(9) . . . . ? C84 C85 C86 C81 -1.4(10) . . . . ? C82 C81 C86 C85 -1.4(9) . . . . ? C96 C91 C92 C93 -3.6(9) . . . . ? C91 C92 C93 C94 0.0(10) . . . . ? C92 C93 C94 C95 3.0(9) . . . . ? C93 C94 C95 C96 -2.6(9) . . . . ? C94 C95 C96 C91 -0.9(9) . . . . ? C92 C91 C96 C95 3.7(9) . . . . ?