#------------------------------------------------------------------------------ #$Date: 2024-11-22 00:36:26 +0200 (Fri, 22 Nov 2024) $ #$Revision: 296048 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573244.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_1573244 _journal_paper_doi 10.1039/D4CY01032A _chemical_formula_moiety 'C34 H38 P2 Ru' _chemical_formula_sum 'C34 H38 P2 Ru' _chemical_formula_weight 609.65 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-09-20 deposited with the CCDC. 2024-11-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.7984(12) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.4141(3) _cell_length_b 13.33648(14) _cell_length_c 22.5810(3) _cell_measurement_reflns_used 52659 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 30.1330 _cell_measurement_theta_min 3.3780 _cell_volume 5943.81(14) _computing_cell_refinement 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)' _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _computing_structure_refinement ; SHELXL-2018/3 (Sheldrick, 2018) Sheldrick GM (2008) Acta Crystallogr A64:112--122 and C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich ShelXle: a Qt graphical user interface for SHELXL J. Appl. Cryst., 44, (2011) 1281-1284. ; _computing_structure_solution ; SHELXT Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 149.9(6) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0734 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'New Xcalibur, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0148 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.942 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 85135 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.942 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.275 _diffrn_reflns_theta_min 3.055 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'pale yellow' _exptl_crystal_density_diffrn 1.363 _exptl_crystal_description block _exptl_crystal_F_000 2528 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: acetone' _exptl_crystal_size_max 0.761 _exptl_crystal_size_mid 0.643 _exptl_crystal_size_min 0.397 _refine_diff_density_max 0.382 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.058 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 368 _refine_ls_number_reflns 8371 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.101 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0210 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+7.3888P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0502 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7521 _reflns_number_total 8371 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cy01032a2.cif _cod_data_source_block e22uh2 _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 1573244 _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 0.635 _shelx_estimated_absorpt_t_max 0.781 _oxdiff_exptl_absorpt_empirical_full_min 0.881 _oxdiff_exptl_absorpt_empirical_full_max 1.185 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL shelxt_a.res in I2/a e22uh2.res created by SHELXL-2018/3 at 14:57:40 on 22-Aug-2022 CELL 0.71073 20.4141 13.33648 22.5810 90.000 104.7984 90.000 ZERR 8 0.0003 0.00014 0.0003 0.000 0.0012 0.000 LATT 2 SYMM 1/2 - X, Y, - Z SFAC C H P RU UNIT 272 304 16 8 ACTA FMAP 2 PLAN 5 BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 SIZE 0.397 0.643 0.761 WGHT 0.016500 7.388800 FVAR 2.22262 RU 4 0.446237 0.677716 0.605886 11.00000 0.01425 0.01168 = 0.01200 0.00042 0.00323 -0.00036 P1 3 0.556415 0.732272 0.627098 11.00000 0.01343 0.01410 = 0.01505 0.00061 0.00254 0.00151 P2 3 0.432063 0.797251 0.674613 11.00000 0.01470 0.01650 = 0.01233 -0.00031 0.00297 0.00129 C1 1 0.507375 0.880033 0.693736 11.00000 0.01859 0.01941 = 0.02310 -0.00699 0.00510 -0.00067 AFIX 23 H1A 2 0.500865 0.936070 0.664047 11.00000 -1.20000 H1B 2 0.512479 0.908829 0.735077 11.00000 -1.20000 AFIX 0 C2 1 0.571736 0.822237 0.692208 11.00000 0.01621 0.02404 = 0.02103 -0.00668 0.00204 -0.00107 AFIX 23 H2A 2 0.588201 0.785147 0.731155 11.00000 -1.20000 H2B 2 0.607434 0.870321 0.688529 11.00000 -1.20000 AFIX 0 C3 1 0.587541 0.801947 0.569443 11.00000 0.01309 0.01945 = 0.01945 0.00177 0.00175 -0.00277 C4 1 0.570810 0.903144 0.558002 11.00000 0.01745 0.02058 = 0.03285 0.00514 0.00565 -0.00136 AFIX 43 H4 2 0.546192 0.937140 0.582381 11.00000 -1.20000 AFIX 0 C5 1 0.589709 0.954453 0.511522 11.00000 0.02495 0.02522 = 0.03931 0.01283 0.00214 -0.00621 AFIX 43 H5 2 0.577649 1.022990 0.504227 11.00000 -1.20000 AFIX 0 C6 1 0.625807 0.906844 0.475875 11.00000 0.03110 0.04099 = 0.02683 0.00984 0.00515 -0.01478 AFIX 43 H6 2 0.638857 0.942381 0.444258 11.00000 -1.20000 AFIX 0 C7 1 0.642953 0.806643 0.486492 11.00000 0.03221 0.04157 = 0.02558 -0.00247 0.01310 -0.00861 AFIX 43 H7 2 0.668014 0.773474 0.462173 11.00000 -1.20000 AFIX 0 C8 1 0.623584 0.754511 0.532635 11.00000 0.02424 0.02458 = 0.02383 -0.00068 0.00821 -0.00210 AFIX 43 H8 2 0.635071 0.685647 0.539157 11.00000 -1.20000 AFIX 0 C9 1 0.628176 0.646417 0.652720 11.00000 0.02262 0.02537 = 0.01746 0.00341 0.00534 0.01042 C10 1 0.693229 0.684391 0.678116 11.00000 0.02130 0.04901 = 0.02770 -0.00328 0.00237 0.01190 AFIX 43 H10 2 0.700083 0.754764 0.682270 11.00000 -1.20000 AFIX 0 C11 1 0.747736 0.619610 0.697243 11.00000 0.03009 0.08675 = 0.03124 -0.00576 -0.00053 0.03191 AFIX 43 H11 2 0.791821 0.645942 0.714004 11.00000 -1.20000 AFIX 0 C12 1 0.738395 0.517782 0.692114 11.00000 0.06267 0.08293 = 0.02629 0.00627 0.00869 0.05732 AFIX 43 H12 2 0.775778 0.473891 0.706257 11.00000 -1.20000 AFIX 0 C13 1 0.674947 0.479097 0.666509 11.00000 0.08739 0.03826 = 0.03169 0.01080 0.02848 0.03914 AFIX 43 H13 2 0.668703 0.408561 0.662906 11.00000 -1.20000 AFIX 0 C14 1 0.619457 0.543518 0.645711 11.00000 0.04701 0.02464 = 0.02554 0.00447 0.01703 0.01331 AFIX 43 H14 2 0.576012 0.516724 0.626871 11.00000 -1.20000 AFIX 0 C15 1 0.362637 0.888401 0.652960 11.00000 0.01726 0.02114 = 0.01416 0.00212 0.00597 0.00369 C16 1 0.365591 0.980345 0.683061 11.00000 0.02596 0.02750 = 0.01848 -0.00389 0.00282 0.00661 AFIX 43 H16 2 0.404391 0.996680 0.714972 11.00000 -1.20000 AFIX 0 C17 1 0.312388 1.048219 0.666845 11.00000 0.03426 0.02743 = 0.02765 -0.00467 0.00849 0.01056 AFIX 43 H17 2 0.315032 1.110651 0.687581 11.00000 -1.20000 AFIX 0 C18 1 0.255394 1.025006 0.620423 11.00000 0.02437 0.03154 = 0.03094 0.00466 0.00925 0.01197 AFIX 43 H18 2 0.219175 1.071643 0.609046 11.00000 -1.20000 AFIX 0 C19 1 0.251598 0.933503 0.590774 11.00000 0.01615 0.03372 = 0.02626 0.00238 0.00386 0.00322 AFIX 43 H19 2 0.212421 0.917147 0.559275 11.00000 -1.20000 AFIX 0 C20 1 0.304821 0.865328 0.606827 11.00000 0.01861 0.02213 = 0.02129 0.00043 0.00600 0.00043 AFIX 43 H20 2 0.301743 0.802714 0.586237 11.00000 -1.20000 AFIX 0 C21 1 0.420886 0.760113 0.750037 11.00000 0.02590 0.02112 = 0.01346 -0.00113 0.00591 0.00301 C22 1 0.475797 0.746530 0.800678 11.00000 0.03051 0.04611 = 0.01838 0.00331 0.00118 -0.00088 AFIX 43 H22 2 0.520121 0.763145 0.797769 11.00000 -1.20000 AFIX 0 C23 1 0.466499 0.708827 0.855613 11.00000 0.04916 0.05785 = 0.01716 0.00723 -0.00077 0.00145 AFIX 43 H23 2 0.504306 0.701585 0.890027 11.00000 -1.20000 AFIX 0 C24 1 0.402803 0.682053 0.860216 11.00000 0.05852 0.04136 = 0.01890 0.00661 0.01563 0.00399 AFIX 43 H24 2 0.396808 0.655266 0.897461 11.00000 -1.20000 AFIX 0 C25 1 0.347615 0.694307 0.810426 11.00000 0.04085 0.03641 = 0.02718 0.00424 0.01879 0.00243 AFIX 43 H25 2 0.303645 0.675555 0.813320 11.00000 -1.20000 AFIX 0 C26 1 0.356603 0.734169 0.756056 11.00000 0.02712 0.02992 = 0.01928 0.00234 0.00886 0.00379 AFIX 43 H26 2 0.318283 0.743909 0.722408 11.00000 -1.20000 AFIX 0 C27 1 0.465280 0.559490 0.678541 11.00000 0.03430 0.01817 = 0.02106 0.00757 0.00934 0.00308 H27A 2 0.504245 0.516559 0.685987 11.00000 0.02932 H27B 2 0.459237 0.587357 0.714237 11.00000 0.02659 C28 1 0.408235 0.535029 0.630424 11.00000 0.03228 0.01548 = 0.02501 0.00255 0.01269 -0.00505 C29 1 0.352547 0.602028 0.618239 11.00000 0.02323 0.02365 = 0.02583 -0.00101 0.00961 -0.00808 H29A 2 0.339040 0.633373 0.651065 11.00000 0.02674 H29B 2 0.315577 0.589547 0.585008 11.00000 0.02926 C30 1 0.407475 0.441057 0.592767 11.00000 0.05089 0.01664 = 0.04119 -0.00366 0.01575 -0.00687 AFIX 137 H30A 2 0.378805 0.451860 0.551293 11.00000 -1.50000 H30B 2 0.389408 0.385151 0.611918 11.00000 -1.50000 H30C 2 0.453720 0.425264 0.590690 11.00000 -1.50000 AFIX 0 C31 1 0.417591 0.781825 0.527012 11.00000 0.01527 0.02121 = 0.01501 0.00499 0.00319 0.00247 H31A 2 0.379503 0.825637 0.521963 11.00000 0.02027 H31B 2 0.456375 0.812097 0.522554 11.00000 0.01919 C32 1 0.404695 0.681771 0.506820 11.00000 0.01796 0.02617 = 0.01163 -0.00115 0.00385 -0.00153 C33 1 0.460389 0.614733 0.517021 11.00000 0.02368 0.02086 = 0.01940 -0.00499 0.00781 -0.00066 H33A 2 0.503325 0.638103 0.512527 11.00000 0.03109 H33B 2 0.450808 0.545983 0.507384 11.00000 0.02779 C34 1 0.333497 0.649426 0.476178 11.00000 0.02198 0.04263 = 0.02038 -0.00608 0.00101 -0.00587 AFIX 137 H34A 2 0.324106 0.662077 0.432054 11.00000 -1.50000 H34B 2 0.301507 0.687462 0.493226 11.00000 -1.50000 H34C 2 0.328501 0.577670 0.483296 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in I2/a REM wR2 = 0.0502, GooF = S = 1.101, Restrained GooF = 1.101 for all data REM R1 = 0.0210 for 7521 Fo > 4sig(Fo) and 0.0266 for all 8371 data REM 368 parameters refined using 0 restraints END WGHT 0.0165 7.3885 REM Highest difference peak 0.382, deepest hole -0.450, 1-sigma level 0.058 Q1 1 0.3912 0.8490 0.6614 11.00000 0.05 0.38 Q2 1 0.4254 0.7656 0.7176 11.00000 0.05 0.37 Q3 1 0.5419 0.8526 0.6939 11.00000 0.05 0.37 Q4 1 0.6587 0.8235 0.6824 11.00000 0.05 0.36 Q5 1 0.5805 0.8512 0.5634 11.00000 0.05 0.35 ; _shelx_res_checksum 33545 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -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 Ru Ru 0.44624(2) 0.67772(2) 0.60589(2) 0.01266(3) Uani 1 1 d . . . . . P1 P 0.55642(2) 0.73227(2) 0.62710(2) 0.01439(6) Uani 1 1 d . . . . . P2 P 0.43206(2) 0.79725(2) 0.67461(2) 0.01460(6) Uani 1 1 d . . . . . C1 C 0.50737(6) 0.88003(10) 0.69374(6) 0.0204(3) Uani 1 1 d . . . . . H1A H 0.500865 0.936070 0.664047 0.024 Uiso 1 1 calc R U . . . H1B H 0.512479 0.908829 0.735077 0.024 Uiso 1 1 calc R U . . . C2 C 0.57174(7) 0.82224(10) 0.69221(6) 0.0209(3) Uani 1 1 d . . . . . H2A H 0.588201 0.785147 0.731155 0.025 Uiso 1 1 calc R U . . . H2B H 0.607434 0.870321 0.688529 0.025 Uiso 1 1 calc R U . . . C3 C 0.58754(6) 0.80195(10) 0.56944(6) 0.0178(2) Uani 1 1 d . . . . . C4 C 0.57081(7) 0.90314(10) 0.55800(7) 0.0238(3) Uani 1 1 d . . . . . H4 H 0.546192 0.937140 0.582381 0.029 Uiso 1 1 calc R U . . . C5 C 0.58971(8) 0.95445(12) 0.51152(7) 0.0309(3) Uani 1 1 d . . . . . H5 H 0.577649 1.022990 0.504227 0.037 Uiso 1 1 calc R U . . . C6 C 0.62581(8) 0.90684(13) 0.47588(7) 0.0334(4) Uani 1 1 d . . . . . H6 H 0.638857 0.942381 0.444258 0.040 Uiso 1 1 calc R U . . . C7 C 0.64295(8) 0.80664(13) 0.48649(7) 0.0321(3) Uani 1 1 d . . . . . H7 H 0.668014 0.773474 0.462173 0.038 Uiso 1 1 calc R U . . . C8 C 0.62358(7) 0.75451(11) 0.53263(6) 0.0238(3) Uani 1 1 d . . . . . H8 H 0.635071 0.685647 0.539157 0.029 Uiso 1 1 calc R U . . . C9 C 0.62818(7) 0.64642(11) 0.65272(6) 0.0218(3) Uani 1 1 d . . . . . C10 C 0.69323(8) 0.68439(14) 0.67812(7) 0.0334(4) Uani 1 1 d . . . . . H10 H 0.700083 0.754764 0.682270 0.040 Uiso 1 1 calc R U . . . C11 C 0.74774(9) 0.61961(19) 0.69724(8) 0.0509(6) Uani 1 1 d . . . . . H11 H 0.791821 0.645942 0.714004 0.061 Uiso 1 1 calc R U . . . C12 C 0.73839(11) 0.51778(19) 0.69211(8) 0.0578(7) Uani 1 1 d . . . . . H12 H 0.775778 0.473891 0.706257 0.069 Uiso 1 1 calc R U . . . C13 C 0.67495(12) 0.47910(15) 0.66651(8) 0.0500(6) Uani 1 1 d . . . . . H13 H 0.668703 0.408561 0.662906 0.060 Uiso 1 1 calc R U . . . C14 C 0.61946(9) 0.54352(11) 0.64571(7) 0.0310(3) Uani 1 1 d . . . . . H14 H 0.576012 0.516724 0.626871 0.037 Uiso 1 1 calc R U . . . C15 C 0.36264(6) 0.88840(10) 0.65296(6) 0.0172(2) Uani 1 1 d . . . . . C16 C 0.36559(7) 0.98035(11) 0.68306(6) 0.0245(3) Uani 1 1 d . . . . . H16 H 0.404391 0.996680 0.714972 0.029 Uiso 1 1 calc R U . . . C17 C 0.31239(8) 1.04822(12) 0.66685(7) 0.0297(3) Uani 1 1 d . . . . . H17 H 0.315032 1.110651 0.687581 0.036 Uiso 1 1 calc R U . . . C18 C 0.25539(7) 1.02501(12) 0.62042(7) 0.0286(3) Uani 1 1 d . . . . . H18 H 0.219175 1.071643 0.609046 0.034 Uiso 1 1 calc R U . . . C19 C 0.25160(7) 0.93350(12) 0.59077(7) 0.0257(3) Uani 1 1 d . . . . . H19 H 0.212421 0.917147 0.559275 0.031 Uiso 1 1 calc R U . . . C20 C 0.30482(7) 0.86533(10) 0.60683(6) 0.0205(3) Uani 1 1 d . . . . . H20 H 0.301743 0.802714 0.586237 0.025 Uiso 1 1 calc R U . . . C21 C 0.42089(7) 0.76011(10) 0.75004(6) 0.0200(2) Uani 1 1 d . . . . . C22 C 0.47580(8) 0.74653(13) 0.80068(7) 0.0326(3) Uani 1 1 d . . . . . H22 H 0.520121 0.763145 0.797769 0.039 Uiso 1 1 calc R U . . . C23 C 0.46650(10) 0.70883(16) 0.85561(7) 0.0431(4) Uani 1 1 d . . . . . H23 H 0.504306 0.701585 0.890027 0.052 Uiso 1 1 calc R U . . . C24 C 0.40280(10) 0.68205(13) 0.86022(7) 0.0385(4) Uani 1 1 d . . . . . H24 H 0.396808 0.655266 0.897461 0.046 Uiso 1 1 calc R U . . . C25 C 0.34762(9) 0.69431(13) 0.81043(7) 0.0330(3) Uani 1 1 d . . . . . H25 H 0.303645 0.675555 0.813320 0.040 Uiso 1 1 calc R U . . . C26 C 0.35660(7) 0.73417(11) 0.75606(6) 0.0249(3) Uani 1 1 d . . . . . H26 H 0.318283 0.743909 0.722408 0.030 Uiso 1 1 calc R U . . . C27 C 0.46528(8) 0.55949(10) 0.67854(6) 0.0241(3) Uani 1 1 d . . . . . H27A H 0.5042(9) 0.5166(14) 0.6860(8) 0.029(5) Uiso 1 1 d . . . . . H27B H 0.4592(9) 0.5874(13) 0.7142(8) 0.027(4) Uiso 1 1 d . . . . . C28 C 0.40824(8) 0.53503(10) 0.63042(6) 0.0233(3) Uani 1 1 d . . . . . C29 C 0.35255(7) 0.60203(11) 0.61824(7) 0.0236(3) Uani 1 1 d . . . . . H29A H 0.3390(9) 0.6334(13) 0.6511(8) 0.027(4) Uiso 1 1 d . . . . . H29B H 0.3156(9) 0.5895(13) 0.5850(8) 0.029(4) Uiso 1 1 d . . . . . C30 C 0.40748(10) 0.44106(11) 0.59277(8) 0.0355(4) Uani 1 1 d . . . . . H30A H 0.378805 0.451860 0.551293 0.053 Uiso 1 1 calc R U . . . H30B H 0.389408 0.385151 0.611918 0.053 Uiso 1 1 calc R U . . . H30C H 0.453720 0.425264 0.590690 0.053 Uiso 1 1 calc R U . . . C31 C 0.41759(7) 0.78182(10) 0.52701(6) 0.0173(2) Uani 1 1 d . . . . . H31A H 0.3795(8) 0.8256(12) 0.5220(7) 0.020(4) Uiso 1 1 d . . . . . H31B H 0.4564(8) 0.8121(12) 0.5226(7) 0.019(4) Uiso 1 1 d . . . . . C32 C 0.40469(6) 0.68177(10) 0.50682(6) 0.0186(2) Uani 1 1 d . . . . . C33 C 0.46039(7) 0.61473(11) 0.51702(6) 0.0209(3) Uani 1 1 d . . . . . H33A H 0.5033(10) 0.6381(14) 0.5125(8) 0.031(5) Uiso 1 1 d . . . . . H33B H 0.4508(9) 0.5460(14) 0.5074(8) 0.028(4) Uiso 1 1 d . . . . . C34 C 0.33350(7) 0.64943(13) 0.47618(7) 0.0291(3) Uani 1 1 d . . . . . H34A H 0.324106 0.662077 0.432054 0.044 Uiso 1 1 calc R U . . . H34B H 0.301507 0.687462 0.493226 0.044 Uiso 1 1 calc R U . . . H34C H 0.328501 0.577670 0.483296 0.044 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 Ru 0.01425(5) 0.01168(5) 0.01200(5) 0.00042(3) 0.00323(3) -0.00036(3) P1 0.01343(14) 0.01410(14) 0.01505(14) 0.00061(11) 0.00254(11) 0.00151(11) P2 0.01470(14) 0.01650(14) 0.01233(13) -0.00031(11) 0.00297(11) 0.00129(11) C1 0.0186(6) 0.0194(6) 0.0231(6) -0.0070(5) 0.0051(5) -0.0007(5) C2 0.0162(6) 0.0240(6) 0.0210(6) -0.0067(5) 0.0020(5) -0.0011(5) C3 0.0131(5) 0.0195(6) 0.0195(6) 0.0018(5) 0.0017(4) -0.0028(4) C4 0.0175(6) 0.0206(6) 0.0329(7) 0.0051(5) 0.0057(5) -0.0014(5) C5 0.0250(7) 0.0252(7) 0.0393(8) 0.0128(6) 0.0021(6) -0.0062(6) C6 0.0311(8) 0.0410(9) 0.0268(7) 0.0098(6) 0.0051(6) -0.0148(7) C7 0.0322(8) 0.0416(9) 0.0256(7) -0.0025(6) 0.0131(6) -0.0086(7) C8 0.0242(7) 0.0246(7) 0.0238(6) -0.0007(5) 0.0082(5) -0.0021(5) C9 0.0226(6) 0.0254(7) 0.0175(6) 0.0034(5) 0.0053(5) 0.0104(5) C10 0.0213(7) 0.0490(10) 0.0277(7) -0.0033(7) 0.0024(6) 0.0119(7) C11 0.0301(9) 0.0868(16) 0.0312(9) -0.0058(9) -0.0005(7) 0.0319(10) C12 0.0627(13) 0.0829(16) 0.0263(8) 0.0063(9) 0.0087(8) 0.0573(13) C13 0.0874(16) 0.0383(10) 0.0317(9) 0.0108(7) 0.0285(10) 0.0391(10) C14 0.0470(9) 0.0246(7) 0.0255(7) 0.0045(6) 0.0170(7) 0.0133(7) C15 0.0173(6) 0.0211(6) 0.0142(5) 0.0021(4) 0.0060(4) 0.0037(5) C16 0.0260(7) 0.0275(7) 0.0185(6) -0.0039(5) 0.0028(5) 0.0066(6) C17 0.0343(8) 0.0274(7) 0.0276(7) -0.0047(6) 0.0085(6) 0.0106(6) C18 0.0244(7) 0.0315(8) 0.0309(7) 0.0047(6) 0.0092(6) 0.0120(6) C19 0.0161(6) 0.0337(8) 0.0263(7) 0.0024(6) 0.0039(5) 0.0032(5) C20 0.0186(6) 0.0221(6) 0.0213(6) 0.0004(5) 0.0060(5) 0.0004(5) C21 0.0259(7) 0.0211(6) 0.0135(5) -0.0011(5) 0.0059(5) 0.0030(5) C22 0.0305(8) 0.0461(9) 0.0184(7) 0.0033(6) 0.0012(6) -0.0009(7) C23 0.0492(11) 0.0578(12) 0.0172(7) 0.0072(7) -0.0008(7) 0.0014(9) C24 0.0585(11) 0.0414(9) 0.0189(7) 0.0066(6) 0.0156(7) 0.0040(8) C25 0.0409(9) 0.0364(8) 0.0272(7) 0.0042(6) 0.0188(7) 0.0024(7) C26 0.0271(7) 0.0299(7) 0.0193(6) 0.0023(5) 0.0089(5) 0.0038(6) C27 0.0343(8) 0.0182(6) 0.0211(6) 0.0076(5) 0.0093(6) 0.0031(6) C28 0.0323(7) 0.0155(6) 0.0250(6) 0.0026(5) 0.0127(6) -0.0051(5) C29 0.0232(7) 0.0236(7) 0.0258(7) -0.0010(5) 0.0096(5) -0.0081(5) C30 0.0509(10) 0.0166(7) 0.0412(9) -0.0037(6) 0.0158(8) -0.0069(7) C31 0.0153(6) 0.0212(6) 0.0150(5) 0.0050(5) 0.0032(4) 0.0025(5) C32 0.0180(6) 0.0262(7) 0.0116(5) -0.0012(5) 0.0039(4) -0.0015(5) C33 0.0237(6) 0.0209(6) 0.0194(6) -0.0050(5) 0.0078(5) -0.0007(5) C34 0.0220(7) 0.0426(9) 0.0204(6) -0.0061(6) 0.0010(5) -0.0059(6) 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' 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 C28 Ru C32 102.24(5) . . ? C28 Ru C31 135.52(5) . . ? C32 Ru C31 37.48(5) . . ? C28 Ru C27 37.29(5) . . ? C32 Ru C27 135.97(5) . . ? C31 Ru C27 172.76(5) . . ? C28 Ru C29 37.34(5) . . ? C32 Ru C29 91.04(5) . . ? C31 Ru C29 108.89(5) . . ? C27 Ru C29 65.50(6) . . ? C28 Ru C33 92.05(5) . . ? C32 Ru C33 37.18(5) . . ? C31 Ru C33 65.59(5) . . ? C27 Ru C33 110.58(5) . . ? C29 Ru C33 104.45(5) . . ? C28 Ru P2 108.67(4) . . ? C32 Ru P2 126.40(4) . . ? C31 Ru P2 93.17(4) . . ? C27 Ru P2 91.26(4) . . ? C29 Ru P2 88.26(4) . . ? C33 Ru P2 157.72(4) . . ? C28 Ru P1 128.12(4) . . ? C32 Ru P1 108.05(4) . . ? C31 Ru P1 90.72(4) . . ? C27 Ru P1 95.33(4) . . ? C29 Ru P1 159.78(4) . . ? C33 Ru P1 87.85(4) . . ? P2 Ru P1 85.684(12) . . ? C9 P1 C3 98.41(6) . . ? C9 P1 C2 101.18(6) . . ? C3 P1 C2 102.40(6) . . ? C9 P1 Ru 121.97(5) . . ? C3 P1 Ru 120.64(4) . . ? C2 P1 Ru 109.10(4) . . ? C15 P2 C21 98.90(6) . . ? C15 P2 C1 101.87(6) . . ? C21 P2 C1 103.66(6) . . ? C15 P2 Ru 120.14(4) . . ? C21 P2 Ru 120.34(4) . . ? C1 P2 Ru 109.35(4) . . ? C2 C1 P2 111.14(9) . . ? C2 C1 H1A 109.4 . . ? P2 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 P1 111.73(9) . . ? C1 C2 H2A 109.3 . . ? P1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? P1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? C8 C3 C4 117.93(12) . . ? C8 C3 P1 121.52(10) . . ? C4 C3 P1 120.36(10) . . ? C5 C4 C3 120.87(14) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 120.55(15) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 119.49(14) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 120.24(15) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C3 120.91(14) . . ? C7 C8 H8 119.5 . . ? C3 C8 H8 119.5 . . ? C14 C9 C10 119.02(14) . . ? C14 C9 P1 120.86(12) . . ? C10 C9 P1 120.09(12) . . ? C11 C10 C9 120.24(18) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 120.5(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.12(16) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 120.23(19) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C9 C14 C13 119.88(18) . . ? C9 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C20 C15 C16 118.73(12) . . ? C20 C15 P2 120.08(10) . . ? C16 C15 P2 121.17(10) . . ? C17 C16 C15 120.69(13) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C18 C17 C16 120.13(14) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.64(13) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.41(13) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.39(13) . . ? C19 C20 H20 119.8 . . ? C15 C20 H20 119.8 . . ? C22 C21 C26 117.82(13) . . ? C22 C21 P2 121.99(11) . . ? C26 C21 P2 119.84(10) . . ? C21 C22 C23 120.84(16) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 120.37(16) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.77(15) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 119.90(16) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C21 121.26(14) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C28 C27 Ru 69.15(7) . . ? C28 C27 H27A 118.7(11) . . ? Ru C27 H27A 122.0(11) . . ? C28 C27 H27B 119.7(11) . . ? Ru C27 H27B 108.6(11) . . ? H27A C27 H27B 112.1(15) . . ? C27 C28 C29 117.81(13) . . ? C27 C28 C30 120.78(14) . . ? C29 C28 C30 121.40(14) . . ? C27 C28 Ru 73.56(8) . . ? C29 C28 Ru 73.74(8) . . ? C30 C28 Ru 122.26(10) . . ? C28 C29 Ru 68.92(8) . . ? C28 C29 H29A 120.3(11) . . ? Ru C29 H29A 109.0(11) . . ? C28 C29 H29B 119.2(11) . . ? Ru C29 H29B 121.4(11) . . ? H29A C29 H29B 111.7(15) . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 Ru 69.93(7) . . ? C32 C31 H31A 117.4(10) . . ? Ru C31 H31A 121.2(10) . . ? C32 C31 H31B 118.4(10) . . ? Ru C31 H31B 107.8(10) . . ? H31A C31 H31B 114.6(14) . . ? C31 C32 C33 117.86(12) . . ? C31 C32 C34 119.85(12) . . ? C33 C32 C34 122.29(13) . . ? C31 C32 Ru 72.59(7) . . ? C33 C32 Ru 74.47(7) . . ? C34 C32 Ru 122.78(9) . . ? C32 C33 Ru 68.35(7) . . ? C32 C33 H33A 119.6(11) . . ? Ru C33 H33A 107.5(11) . . ? C32 C33 H33B 117.5(11) . . ? Ru C33 H33B 119.7(10) . . ? H33A C33 H33B 115.4(15) . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 Ru C28 2.1794(13) . ? Ru C32 2.1811(12) . ? Ru C31 2.2158(12) . ? Ru C27 2.2367(13) . ? Ru C29 2.2422(13) . ? Ru C33 2.2610(13) . ? Ru P2 2.2941(3) . ? Ru P1 2.2951(3) . ? P1 C9 1.8327(13) . ? P1 C3 1.8398(13) . ? P1 C2 1.8612(13) . ? P2 C15 1.8362(13) . ? P2 C21 1.8430(13) . ? P2 C1 1.8520(13) . ? C1 C2 1.5313(18) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.3946(19) . ? C3 C4 1.3999(18) . ? C4 C5 1.388(2) . ? C4 H4 0.9500 . ? C5 C6 1.377(2) . ? C5 H5 0.9500 . ? C6 C7 1.387(2) . ? C6 H6 0.9500 . ? C7 C8 1.391(2) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.388(2) . ? C9 C10 1.400(2) . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C11 C12 1.372(3) . ? C11 H11 0.9500 . ? C12 C13 1.377(3) . ? C12 H12 0.9500 . ? C13 C14 1.404(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.3946(18) . ? C15 C16 1.3958(19) . ? C16 C17 1.389(2) . ? C16 H16 0.9500 . ? C17 C18 1.388(2) . ? C17 H17 0.9500 . ? C18 C19 1.385(2) . ? C18 H18 0.9500 . ? C19 C20 1.3919(19) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.3936(19) . ? C21 C26 1.397(2) . ? C22 C23 1.396(2) . ? C22 H22 0.9500 . ? C23 C24 1.378(3) . ? C23 H23 0.9500 . ? C24 C25 1.383(2) . ? C24 H24 0.9500 . ? C25 C26 1.392(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.413(2) . ? C27 H27A 0.959(18) . ? C27 H27B 0.924(18) . ? C28 C29 1.417(2) . ? C28 C30 1.512(2) . ? C29 H29A 0.951(18) . ? C29 H29B 0.933(18) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.4129(19) . ? C31 H31A 0.956(16) . ? C31 H31B 0.917(17) . ? C32 C33 1.4182(19) . ? C32 C34 1.5045(18) . ? C33 H33A 0.960(19) . ? C33 H33B 0.951(18) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 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 C15 P2 C1 C2 -160.70(9) . . . . ? C21 P2 C1 C2 96.96(10) . . . . ? Ru P2 C1 C2 -32.56(10) . . . . ? P2 C1 C2 P1 39.97(12) . . . . ? C9 P1 C2 C1 -160.09(10) . . . . ? C3 P1 C2 C1 98.60(10) . . . . ? Ru P1 C2 C1 -30.33(11) . . . . ? C9 P1 C3 C8 37.10(12) . . . . ? C2 P1 C3 C8 140.58(11) . . . . ? Ru P1 C3 C8 -98.11(11) . . . . ? C9 P1 C3 C4 -148.05(11) . . . . ? C2 P1 C3 C4 -44.57(12) . . . . ? Ru P1 C3 C4 76.73(11) . . . . ? C8 C3 C4 C5 -0.1(2) . . . . ? P1 C3 C4 C5 -175.15(11) . . . . ? C3 C4 C5 C6 -0.4(2) . . . . ? C4 C5 C6 C7 0.4(2) . . . . ? C5 C6 C7 C8 0.3(2) . . . . ? C6 C7 C8 C3 -0.8(2) . . . . ? C4 C3 C8 C7 0.8(2) . . . . ? P1 C3 C8 C7 175.72(11) . . . . ? C3 P1 C9 C14 -118.19(12) . . . . ? C2 P1 C9 C14 137.31(12) . . . . ? Ru P1 C9 C14 16.20(14) . . . . ? C3 P1 C9 C10 59.91(12) . . . . ? C2 P1 C9 C10 -44.59(13) . . . . ? Ru P1 C9 C10 -165.70(10) . . . . ? C14 C9 C10 C11 -1.5(2) . . . . ? P1 C9 C10 C11 -179.64(13) . . . . ? C9 C10 C11 C12 -0.7(3) . . . . ? C10 C11 C12 C13 1.6(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C10 C9 C14 C13 2.8(2) . . . . ? P1 C9 C14 C13 -179.04(11) . . . . ? C12 C13 C14 C9 -2.0(2) . . . . ? C21 P2 C15 C20 -108.59(11) . . . . ? C1 P2 C15 C20 145.32(11) . . . . ? Ru P2 C15 C20 24.42(12) . . . . ? C21 P2 C15 C16 69.66(12) . . . . ? C1 P2 C15 C16 -36.43(12) . . . . ? Ru P2 C15 C16 -157.33(9) . . . . ? C20 C15 C16 C17 -0.9(2) . . . . ? P2 C15 C16 C17 -179.15(11) . . . . ? C15 C16 C17 C18 0.2(2) . . . . ? C16 C17 C18 C19 0.6(2) . . . . ? C17 C18 C19 C20 -0.7(2) . . . . ? C18 C19 C20 C15 0.0(2) . . . . ? C16 C15 C20 C19 0.8(2) . . . . ? P2 C15 C20 C19 179.09(10) . . . . ? C15 P2 C21 C22 -138.44(13) . . . . ? C1 P2 C21 C22 -33.82(14) . . . . ? Ru P2 C21 C22 88.68(13) . . . . ? C15 P2 C21 C26 48.53(12) . . . . ? C1 P2 C21 C26 153.15(11) . . . . ? Ru P2 C21 C26 -84.35(12) . . . . ? C26 C21 C22 C23 -0.4(2) . . . . ? P2 C21 C22 C23 -173.57(14) . . . . ? C21 C22 C23 C24 1.6(3) . . . . ? C22 C23 C24 C25 -1.2(3) . . . . ? C23 C24 C25 C26 -0.4(3) . . . . ? C24 C25 C26 C21 1.6(2) . . . . ? C22 C21 C26 C25 -1.2(2) . . . . ? P2 C21 C26 C25 172.16(12) . . . . ? Ru C27 C28 C29 -60.94(11) . . . . ? Ru C27 C28 C30 118.17(13) . . . . ? C27 C28 C29 Ru 60.84(11) . . . . ? C30 C28 C29 Ru -118.26(13) . . . . ? Ru C31 C32 C33 -61.11(10) . . . . ? Ru C31 C32 C34 118.31(12) . . . . ? C31 C32 C33 Ru 60.12(10) . . . . ? C34 C32 C33 Ru -119.28(12) . . . . ?