# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_bj254 _database_code_depnum_ccdc_archive 'CCDC 913686' #TrackingRef 'bj254_bj255.cif' _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H49 Cl2 N O P2 Ru' _chemical_formula_weight 913.81 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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; 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' _cell_length_a 10.5773(6) _cell_length_b 16.979(2) _cell_length_c 24.2616(6) _cell_angle_alpha 90 _cell_angle_beta 90.7060(10) _cell_angle_gamma 90 _cell_volume 4356.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17613 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.05 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.393 _exptl_crystal_F_000 1888 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_absorpt_coefficient_mu 0.594 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38191 _diffrn_reflns_av_unetI/netI 0.0672 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.063 _diffrn_reflns_theta_max 30.035 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.841 _diffrn_measured_fraction_theta_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.841 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.841 _diffrn_reflns_point_group_measured_fraction_full 0.983 _reflns_number_total 10710 _reflns_number_gt 6767 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Giacovazzo, 1999)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0801P)^2^+17.5926P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10710 _refine_ls_number_parameters 597 _refine_ls_number_restraints 1150 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1670 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.43566(4) 0.53472(2) 0.37007(2) 0.02550(13) Uani 1 1 d . U . . . Cl1 Cl 0.27183(11) 0.61621(8) 0.33182(6) 0.0324(3) Uani 1 1 d . U . . . Cl2 Cl 0.58436(11) 0.46822(8) 0.43068(5) 0.0304(3) Uani 1 1 d . U . . . P1 P 0.57871(11) 0.52745(8) 0.30348(6) 0.0262(3) Uani 1 1 d . U . . . P2 P 0.31151(12) 0.42789(8) 0.34530(6) 0.0274(3) Uani 1 1 d . U . . . O1 O 0.3258(4) 0.5510(2) 0.44719(16) 0.0345(9) Uani 1 1 d D U . . . N1 N 0.5544(4) 0.6443(3) 0.39354(18) 0.0292(9) Uani 1 1 d . U . . . C1 C 0.7107(5) 0.5849(3) 0.3318(2) 0.0320(12) Uani 1 1 d . U . . . C2 C 0.6869(5) 0.6318(3) 0.3773(2) 0.0310(12) Uani 1 1 d . U . . . C3 C 0.7858(5) 0.6725(4) 0.4029(3) 0.0423(15) Uani 1 1 d . U . . . H3 H 0.7703 0.7045 0.4343 0.051 Uiso 1 1 calc R U . . . C4 C 0.9073(6) 0.6659(4) 0.3821(3) 0.0491(17) Uani 1 1 d . U . . . H4 H 0.9752 0.6927 0.4000 0.059 Uiso 1 1 calc R U . . . C5 C 0.9305(5) 0.6215(4) 0.3365(3) 0.0467(17) Uani 1 1 d . U . . . H5 H 1.0137 0.6185 0.3223 0.056 Uiso 1 1 calc R U . . . C6 C 0.8319(5) 0.5805(4) 0.3104(3) 0.0401(14) Uani 1 1 d . U . . . H6 H 0.8475 0.5500 0.2784 0.048 Uiso 1 1 calc R U . . . C7 C 0.5440(6) 0.6606(4) 0.4535(3) 0.0423(14) Uani 1 1 d . U . . . H7A H 0.5821 0.6171 0.4745 0.063 Uiso 1 1 calc R U . . . H7B H 0.4546 0.6656 0.4631 0.063 Uiso 1 1 calc R U . . . H7C H 0.5883 0.7097 0.4624 0.063 Uiso 1 1 calc R U . . . C8 C 0.5112(6) 0.7165(3) 0.3637(3) 0.0400(14) Uani 1 1 d . U . . . H8A H 0.5651 0.7611 0.3744 0.060 Uiso 1 1 calc R U . . . H8B H 0.4234 0.7280 0.3734 0.060 Uiso 1 1 calc R U . . . H8C H 0.5167 0.7079 0.3239 0.060 Uiso 1 1 calc R U . . . C9 C 0.5663(5) 0.5703(3) 0.2336(2) 0.0339(12) Uani 1 1 d . U . . . C10 C 0.4762(5) 0.6281(3) 0.2216(2) 0.0350(12) Uani 1 1 d . U . . . H10 H 0.4173 0.6431 0.2489 0.042 Uiso 1 1 calc R U . . . C11 C 0.4719(6) 0.6636(4) 0.1705(3) 0.0441(15) Uani 1 1 d . U . . . H11 H 0.4093 0.7024 0.1628 0.053 Uiso 1 1 calc R U . . . C12 C 0.5572(6) 0.6434(4) 0.1304(3) 0.0500(16) Uani 1 1 d . U . . . H12 H 0.5528 0.6680 0.0952 0.060 Uiso 1 1 calc R U . . . C13 C 0.6490(7) 0.5877(5) 0.1410(3) 0.0569(19) Uani 1 1 d . U . . . H13 H 0.7090 0.5746 0.1137 0.068 Uiso 1 1 calc R U . . . C14 C 0.6532(6) 0.5506(4) 0.1922(3) 0.0455(15) Uani 1 1 d . U . . . H14 H 0.7155 0.5114 0.1994 0.055 Uiso 1 1 calc R U . . . C15 C 0.6505(5) 0.4306(3) 0.2894(2) 0.0336(12) Uani 1 1 d . U . . . C16 C 0.6023(6) 0.3838(4) 0.2470(3) 0.0431(14) Uani 1 1 d . U . . . H16 H 0.5356 0.4031 0.2242 0.052 Uiso 1 1 calc R U . . . C17 C 0.6507(7) 0.3094(4) 0.2379(3) 0.0551(18) Uani 1 1 d . U . . . H17 H 0.6187 0.2783 0.2083 0.066 Uiso 1 1 calc R U . . . C18 C 0.7461(7) 0.2805(4) 0.2718(4) 0.060(2) Uani 1 1 d . U . . . H18 H 0.7797 0.2294 0.2655 0.071 Uiso 1 1 calc R U . . . C19 C 0.7922(6) 0.3254(4) 0.3147(3) 0.0473(16) Uani 1 1 d . U . . . H19 H 0.8558 0.3047 0.3387 0.057 Uiso 1 1 calc R U . . . C20 C 0.7459(5) 0.4010(4) 0.3230(3) 0.0385(13) Uani 1 1 d . U . . . H20 H 0.7800 0.4326 0.3519 0.046 Uiso 1 1 calc R U . . . C21 C 0.3778(5) 0.3279(3) 0.3368(2) 0.0322(12) Uani 1 1 d . U . . . C22 C 0.4720(6) 0.3023(4) 0.3726(3) 0.0441(15) Uani 1 1 d . U . . . H22 H 0.5032 0.3370 0.4004 0.053 Uiso 1 1 calc R U . . . C23 C 0.5215(6) 0.2272(4) 0.3687(3) 0.0496(17) Uani 1 1 d . U . . . H23 H 0.5873 0.2108 0.3931 0.060 Uiso 1 1 calc R U . . . C24 C 0.4746(6) 0.1760(4) 0.3290(3) 0.0505(17) Uani 1 1 d . U . . . H24 H 0.5072 0.1240 0.3266 0.061 Uiso 1 1 calc R U . . . C25 C 0.3812(6) 0.2002(4) 0.2930(3) 0.0479(16) Uani 1 1 d . U . . . H25 H 0.3494 0.1650 0.2657 0.057 Uiso 1 1 calc R U . . . C26 C 0.3332(5) 0.2760(4) 0.2965(3) 0.0390(13) Uani 1 1 d . U . . . H26 H 0.2693 0.2927 0.2713 0.047 Uiso 1 1 calc R U . . . C27 C 0.1829(5) 0.4092(3) 0.3949(2) 0.0313(12) Uani 1 1 d . U . . . C28 C 0.1730(6) 0.3400(4) 0.4261(3) 0.0394(14) Uani 1 1 d . U . . . H28 H 0.2366 0.3007 0.4240 0.047 Uiso 1 1 calc R U . . . C29 C 0.0693(6) 0.3294(4) 0.4601(3) 0.0474(16) Uani 1 1 d . U . . . H29 H 0.0621 0.2823 0.4810 0.057 Uiso 1 1 calc R U . . . C30 C -0.0238(6) 0.3868(4) 0.4640(3) 0.0472(16) Uani 1 1 d . U . . . H30 H -0.0945 0.3785 0.4871 0.057 Uiso 1 1 calc R U . . . C31 C -0.0134(5) 0.4560(4) 0.4342(3) 0.0411(14) Uani 1 1 d . U . . . H31 H -0.0761 0.4958 0.4371 0.049 Uiso 1 1 calc R U . . . C32 C 0.0895(5) 0.4663(3) 0.4002(2) 0.0333(12) Uani 1 1 d . U . . . H32 H 0.0965 0.5139 0.3799 0.040 Uiso 1 1 calc R U . . . C33 C 0.2152(5) 0.4376(3) 0.2819(2) 0.0311(12) Uani 1 1 d . U . . . C34 C 0.0961(5) 0.4042(4) 0.2756(3) 0.0423(15) Uani 1 1 d . U . . . H34 H 0.0609 0.3755 0.3053 0.051 Uiso 1 1 calc R U . . . C35 C 0.0278(6) 0.4119(4) 0.2270(3) 0.0500(17) Uani 1 1 d . U . . . H35 H -0.0536 0.3887 0.2235 0.060 Uiso 1 1 calc R U . . . C36 C 0.0780(7) 0.4534(5) 0.1833(3) 0.0551(18) Uani 1 1 d . U . . . H36 H 0.0314 0.4586 0.1498 0.066 Uiso 1 1 calc R U . . . C37 C 0.1960(6) 0.4872(4) 0.1888(3) 0.0470(16) Uani 1 1 d . U . . . H37 H 0.2305 0.5162 0.1591 0.056 Uiso 1 1 calc R U . . . C38 C 0.2642(6) 0.4789(4) 0.2373(3) 0.0405(14) Uani 1 1 d . U . . . H38 H 0.3460 0.5017 0.2404 0.049 Uiso 1 1 calc R U . . . C39 C 0.2643(16) 0.1256(6) 0.4682(5) 0.113(5) Uani 1 1 d . U . . . H39 H 0.2461 0.1371 0.4306 0.135 Uiso 1 1 calc R U . . . C40 C 0.3864(13) 0.1097(7) 0.4851(5) 0.104(4) Uani 1 1 d . U . . . H40 H 0.4526 0.1085 0.4591 0.125 Uiso 1 1 calc R U . . . C41 C 0.4117(11) 0.0959(6) 0.5395(5) 0.093(3) Uani 1 1 d . U . . . H41 H 0.4962 0.0866 0.5515 0.111 Uiso 1 1 calc R U . . . C42 C 0.3162(10) 0.0951(6) 0.5767(5) 0.085(3) Uani 1 1 d . U . . . H42 H 0.3340 0.0844 0.6144 0.102 Uiso 1 1 calc R U . . . C43 C 0.1963(10) 0.1098(6) 0.5600(5) 0.097(3) Uani 1 1 d . U . . . H43 H 0.1304 0.1095 0.5862 0.116 Uiso 1 1 calc R U . . . C44 C 0.1686(13) 0.1248(6) 0.5064(6) 0.110(4) Uani 1 1 d . U . . . H44 H 0.0838 0.1347 0.4952 0.132 Uiso 1 1 calc R U . . . C45 C 0.7726(17) 0.1826(12) 0.5114(8) 0.070(5) Uani 0.449(19) 1 d G U P A 1 H45 H 0.7382 0.2056 0.4788 0.084 Uiso 0.449(19) 1 calc R U P A 1 C46 C 0.789(2) 0.2279(8) 0.5587(12) 0.062(6) Uani 0.449(19) 1 d G U P A 1 H46 H 0.7653 0.2819 0.5584 0.074 Uiso 0.449(19) 1 calc R U P A 1 C47 C 0.839(2) 0.1942(12) 0.6063(8) 0.072(6) Uani 0.449(19) 1 d G U P A 1 H47 H 0.8501 0.2251 0.6386 0.086 Uiso 0.449(19) 1 calc R U P A 1 C48 C 0.873(2) 0.1151(13) 0.6066(6) 0.078(6) Uani 0.449(19) 1 d G U P A 1 H48 H 0.9079 0.0921 0.6392 0.094 Uiso 0.449(19) 1 calc R U P A 1 C49 C 0.857(2) 0.0698(7) 0.5594(8) 0.084(6) Uani 0.449(19) 1 d G U P A 1 H49 H 0.8809 0.0158 0.5596 0.101 Uiso 0.449(19) 1 calc R U P A 1 C50 C 0.807(2) 0.1035(11) 0.5117(6) 0.072(6) Uani 0.449(19) 1 d G U P A 1 H50 H 0.7960 0.0726 0.4794 0.086 Uiso 0.449(19) 1 calc R U P A 1 C45B C 0.749(3) 0.2319(17) 0.5043(13) 0.057(6) Uani 0.32(3) 1 d G U P B 2 H45B H 0.7230 0.2733 0.4803 0.068 Uiso 0.32(3) 1 calc R U P B 2 C46B C 0.745(3) 0.1543(18) 0.4861(10) 0.069(7) Uani 0.32(3) 1 d G U P B 2 H46B H 0.7169 0.1426 0.4497 0.083 Uiso 0.32(3) 1 calc R U P B 2 C47B C 0.783(4) 0.0937(15) 0.5212(12) 0.084(7) Uani 0.32(3) 1 d G U P B 2 H47B H 0.7803 0.0407 0.5088 0.101 Uiso 0.32(3) 1 calc R U P B 2 C48B C 0.824(3) 0.1108(18) 0.5745(11) 0.080(7) Uani 0.32(3) 1 d G U P B 2 H48B H 0.8498 0.0694 0.5985 0.095 Uiso 0.32(3) 1 calc R U P B 2 C49B C 0.828(3) 0.188(2) 0.5927(10) 0.062(7) Uani 0.32(3) 1 d G U P B 2 H49B H 0.8559 0.2000 0.6291 0.075 Uiso 0.32(3) 1 calc R U P B 2 C50B C 0.790(3) 0.2489(17) 0.5576(14) 0.058(7) Uani 0.32(3) 1 d G U P B 2 H50B H 0.7925 0.3019 0.5700 0.069 Uiso 0.32(3) 1 calc R U P B 2 C45C C 0.754(5) 0.218(3) 0.527(3) 0.060(8) Uani 0.22(3) 1 d G U P C 3 H45C H 0.7166 0.2642 0.5111 0.073 Uiso 0.22(3) 1 calc R U P C 3 C46C C 0.801(5) 0.219(3) 0.580(3) 0.062(7) Uani 0.22(3) 1 d G U P C 3 H46C H 0.7959 0.2663 0.6016 0.075 Uiso 0.22(3) 1 calc R U P C 3 C47C C 0.856(5) 0.152(4) 0.6029(15) 0.076(8) Uani 0.22(3) 1 d G U P C 3 H47C H 0.8880 0.1531 0.6396 0.091 Uiso 0.22(3) 1 calc R U P C 3 C48C C 0.863(6) 0.084(3) 0.572(2) 0.080(8) Uani 0.22(3) 1 d G U P C 3 H48C H 0.9008 0.0377 0.5873 0.096 Uiso 0.22(3) 1 calc R U P C 3 C49C C 0.816(6) 0.082(2) 0.518(2) 0.074(8) Uani 0.22(3) 1 d G U P C 3 H49C H 0.8214 0.0356 0.4968 0.089 Uiso 0.22(3) 1 calc R U P C 3 C50C C 0.762(5) 0.150(4) 0.4955(15) 0.064(8) Uani 0.22(3) 1 d G U P C 3 H50C H 0.7293 0.1488 0.4588 0.077 Uiso 0.22(3) 1 calc R U P C 3 H1 H 0.363(7) 0.540(5) 0.4784(19) 0.096 Uiso 1 1 d D U . . . H2 H 0.253(4) 0.527(5) 0.447(3) 0.096 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.0218(2) 0.0285(2) 0.0261(2) -0.00070(18) -0.00470(14) -0.00073(15) Cl1 0.0239(6) 0.0362(7) 0.0371(7) 0.0011(6) -0.0048(5) 0.0029(5) Cl2 0.0300(6) 0.0349(7) 0.0262(7) 0.0007(6) -0.0083(5) 0.0016(5) P1 0.0200(6) 0.0310(7) 0.0276(7) -0.0006(6) -0.0019(5) -0.0011(5) P2 0.0256(6) 0.0290(7) 0.0276(7) 0.0003(6) -0.0037(5) -0.0035(5) O1 0.033(2) 0.045(2) 0.026(2) 0.0018(18) 0.0014(15) 0.0040(16) N1 0.028(2) 0.031(2) 0.028(2) -0.0010(19) -0.0040(17) -0.0026(17) C1 0.024(2) 0.030(3) 0.042(3) 0.006(2) -0.005(2) 0.0005(19) C2 0.028(3) 0.031(3) 0.034(3) 0.004(2) -0.007(2) -0.004(2) C3 0.035(3) 0.042(3) 0.050(4) -0.003(3) -0.014(3) -0.009(2) C4 0.039(3) 0.044(4) 0.063(5) 0.009(3) -0.024(3) -0.012(3) C5 0.021(3) 0.056(4) 0.063(4) 0.022(4) -0.004(3) -0.001(2) C6 0.029(3) 0.040(3) 0.051(4) 0.013(3) -0.003(2) -0.008(2) C7 0.041(3) 0.043(4) 0.042(4) -0.012(3) -0.004(3) -0.008(3) C8 0.040(3) 0.031(3) 0.049(4) -0.002(3) -0.008(3) -0.002(2) C9 0.033(3) 0.035(3) 0.034(3) -0.001(2) -0.004(2) -0.007(2) C10 0.032(3) 0.037(3) 0.036(3) 0.005(3) -0.003(2) -0.007(2) C11 0.042(3) 0.042(4) 0.048(4) 0.013(3) -0.008(3) -0.002(3) C12 0.055(4) 0.057(4) 0.038(4) 0.007(3) -0.004(3) 0.001(3) C13 0.060(4) 0.068(5) 0.043(4) 0.006(4) 0.012(3) 0.009(4) C14 0.045(4) 0.060(4) 0.031(3) -0.001(3) 0.000(3) 0.009(3) C15 0.026(3) 0.034(3) 0.040(3) -0.004(3) 0.006(2) 0.000(2) C16 0.042(3) 0.043(4) 0.044(4) -0.004(3) 0.001(3) -0.001(3) C17 0.061(4) 0.043(4) 0.062(5) -0.016(3) 0.015(4) -0.003(3) C18 0.051(4) 0.038(4) 0.090(6) -0.007(4) 0.015(4) 0.008(3) C19 0.037(3) 0.035(3) 0.070(5) 0.005(3) 0.013(3) 0.009(2) C20 0.031(3) 0.036(3) 0.049(4) 0.005(3) 0.003(2) 0.000(2) C21 0.027(3) 0.036(3) 0.034(3) 0.004(2) 0.001(2) 0.000(2) C22 0.043(3) 0.044(4) 0.045(4) -0.004(3) -0.010(3) -0.002(3) C23 0.052(4) 0.031(3) 0.065(5) -0.001(3) -0.016(3) 0.005(3) C24 0.044(4) 0.033(3) 0.074(5) -0.006(3) 0.004(3) -0.001(3) C25 0.040(3) 0.038(4) 0.065(4) -0.021(3) 0.002(3) -0.003(3) C26 0.037(3) 0.043(3) 0.037(3) -0.009(3) -0.003(2) -0.004(2) C27 0.027(3) 0.035(3) 0.032(3) 0.000(2) -0.008(2) -0.010(2) C28 0.041(3) 0.034(3) 0.043(4) -0.004(3) -0.010(3) -0.006(2) C29 0.054(4) 0.045(4) 0.043(4) 0.005(3) 0.008(3) -0.011(3) C30 0.042(3) 0.058(4) 0.042(4) -0.002(3) 0.006(3) -0.013(3) C31 0.028(3) 0.053(4) 0.043(4) -0.004(3) 0.002(2) -0.001(2) C32 0.028(3) 0.035(3) 0.036(3) 0.008(3) 0.000(2) -0.001(2) C33 0.025(2) 0.034(3) 0.034(3) -0.003(2) -0.007(2) -0.001(2) C34 0.036(3) 0.052(4) 0.038(3) 0.002(3) -0.013(3) -0.013(3) C35 0.034(3) 0.069(5) 0.047(4) -0.008(3) -0.015(3) -0.010(3) C36 0.058(4) 0.071(5) 0.036(4) 0.002(3) -0.022(3) -0.008(3) C37 0.051(4) 0.059(4) 0.030(3) 0.005(3) -0.011(3) -0.013(3) C38 0.038(3) 0.048(4) 0.035(3) 0.001(3) -0.008(2) -0.012(2) C39 0.190(13) 0.049(6) 0.097(9) 0.025(6) -0.075(9) -0.016(7) C40 0.144(10) 0.081(7) 0.087(8) 0.013(6) -0.010(7) -0.021(7) C41 0.106(8) 0.085(7) 0.086(7) 0.028(6) -0.033(6) -0.026(6) C42 0.088(7) 0.080(6) 0.086(7) 0.002(5) -0.028(6) -0.013(5) C43 0.090(7) 0.071(6) 0.128(9) -0.004(6) -0.041(7) 0.009(5) C44 0.123(9) 0.062(6) 0.143(11) 0.001(7) -0.073(8) 0.002(6) C45 0.075(10) 0.067(12) 0.068(11) -0.010(10) 0.009(9) -0.001(10) C46 0.059(10) 0.063(11) 0.064(13) 0.003(10) 0.009(10) -0.015(9) C47 0.078(11) 0.072(12) 0.067(12) -0.013(10) 0.019(10) -0.026(10) C48 0.112(13) 0.069(12) 0.053(10) -0.014(10) 0.011(9) -0.041(11) C49 0.120(13) 0.069(11) 0.064(12) -0.018(9) 0.000(10) -0.030(10) C50 0.097(13) 0.062(11) 0.057(10) -0.015(9) 0.009(9) -0.018(10) C45B 0.056(11) 0.048(12) 0.067(14) -0.010(12) 0.017(11) 0.006(9) C46B 0.069(13) 0.063(13) 0.076(13) -0.029(11) 0.009(11) 0.006(11) C47B 0.097(15) 0.071(13) 0.084(13) -0.010(12) 0.003(12) -0.015(12) C48B 0.094(13) 0.068(13) 0.077(12) 0.004(12) 0.002(11) -0.016(11) C49B 0.069(12) 0.063(13) 0.055(12) -0.005(11) 0.018(11) -0.011(11) C50B 0.053(11) 0.056(13) 0.065(14) -0.003(12) 0.014(11) 0.000(10) C45C 0.067(13) 0.054(14) 0.061(16) -0.010(14) 0.017(14) 0.004(12) C46C 0.063(13) 0.062(14) 0.062(15) -0.007(13) 0.020(13) -0.022(12) C47C 0.092(14) 0.064(16) 0.072(14) -0.021(14) 0.014(13) -0.020(14) C48C 0.108(15) 0.065(14) 0.068(14) -0.011(13) 0.018(13) -0.015(13) C49C 0.085(15) 0.063(14) 0.074(14) -0.004(13) 0.000(13) 0.000(13) C50C 0.071(14) 0.055(15) 0.067(15) -0.020(14) 0.007(13) 0.012(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 P1 2.2305(14) . ? Ru1 O1 2.232(4) . ? Ru1 N1 2.312(4) . ? Ru1 P2 2.3143(14) . ? Ru1 Cl1 2.3957(13) . ? Ru1 Cl2 2.4195(13) . ? P1 C1 1.830(5) . ? P1 C15 1.844(6) . ? P1 C9 1.848(6) . ? P2 C33 1.842(5) . ? P2 C21 1.849(6) . ? P2 C27 1.855(6) . ? O1 H1 0.870(10) . ? O1 H2 0.870(10) . ? N1 C2 1.475(7) . ? N1 C7 1.486(7) . ? N1 C8 1.493(7) . ? C1 C2 1.388(8) . ? C1 C6 1.390(8) . ? C2 C3 1.393(7) . ? C3 C4 1.392(9) . ? C3 H3 0.9500 . ? C4 C5 1.364(10) . ? C4 H4 0.9500 . ? C5 C6 1.398(8) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.396(8) . ? C9 C14 1.410(8) . ? C10 C11 1.380(8) . ? C10 H10 0.9500 . ? C11 C12 1.379(9) . ? C11 H11 0.9500 . ? C12 C13 1.378(10) . ? C12 H12 0.9500 . ? C13 C14 1.393(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.383(8) . ? C15 C16 1.392(8) . ? C16 C17 1.381(9) . ? C16 H16 0.9500 . ? C17 C18 1.386(11) . ? C17 H17 0.9500 . ? C18 C19 1.374(10) . ? C18 H18 0.9500 . ? C19 C20 1.390(8) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.384(8) . ? C21 C26 1.395(8) . ? C22 C23 1.382(9) . ? C22 H22 0.9500 . ? C23 C24 1.386(9) . ? C23 H23 0.9500 . ? C24 C25 1.373(10) . ? C24 H24 0.9500 . ? C25 C26 1.386(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.391(8) . ? C27 C28 1.402(8) . ? C28 C29 1.394(9) . ? C28 H28 0.9500 . ? C29 C30 1.389(10) . ? C29 H29 0.9500 . ? C30 C31 1.385(9) . ? C30 H30 0.9500 . ? C31 C32 1.385(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.387(7) . ? C33 C38 1.394(8) . ? C34 C35 1.382(8) . ? C34 H34 0.9500 . ? C35 C36 1.383(10) . ? C35 H35 0.9500 . ? C36 C37 1.379(9) . ? C36 H36 0.9500 . ? C37 C38 1.380(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.377(17) . ? C39 C44 1.382(18) . ? C39 H39 0.9500 . ? C40 C41 1.364(14) . ? C40 H40 0.9500 . ? C41 C42 1.362(15) . ? C41 H41 0.9500 . ? C42 C43 1.350(13) . ? C42 H42 0.9500 . ? C43 C44 1.352(16) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 C50 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 C50 1.3900 . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C45B C46B 1.3900 . ? C45B C50B 1.3900 . ? C45B H45B 0.9500 . ? C46B C47B 1.3900 . ? C46B H46B 0.9500 . ? C47B C48B 1.3900 . ? C47B H47B 0.9500 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B C50B 1.3900 . ? C49B H49B 0.9500 . ? C50B H50B 0.9500 . ? C45C C46C 1.3900 . ? C45C C50C 1.3900 . ? C45C H45C 0.9500 . ? C46C C47C 1.3900 . ? C46C H46C 0.9500 . ? C47C C48C 1.3900 . ? C47C H47C 0.9500 . ? C48C C49C 1.3900 . ? C48C H48C 0.9500 . ? C49C C50C 1.3900 . ? C49C H49C 0.9500 . ? C50C H50C 0.9500 . ? 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 P1 Ru1 O1 168.22(11) . . ? P1 Ru1 N1 81.46(12) . . ? O1 Ru1 N1 88.90(16) . . ? P1 Ru1 P2 98.99(5) . . ? O1 Ru1 P2 90.87(11) . . ? N1 Ru1 P2 178.03(12) . . ? P1 Ru1 Cl1 104.20(5) . . ? O1 Ru1 Cl1 82.62(11) . . ? N1 Ru1 Cl1 91.09(11) . . ? P2 Ru1 Cl1 86.94(5) . . ? P1 Ru1 Cl2 88.43(5) . . ? O1 Ru1 Cl2 83.67(11) . . ? N1 Ru1 Cl2 83.03(11) . . ? P2 Ru1 Cl2 98.89(5) . . ? Cl1 Ru1 Cl2 165.17(5) . . ? C1 P1 C15 103.3(2) . . ? C1 P1 C9 100.3(3) . . ? C15 P1 C9 101.9(3) . . ? C1 P1 Ru1 102.70(19) . . ? C15 P1 Ru1 117.89(19) . . ? C9 P1 Ru1 126.97(19) . . ? C33 P2 C21 101.3(3) . . ? C33 P2 C27 98.9(2) . . ? C21 P2 C27 101.4(3) . . ? C33 P2 Ru1 116.94(19) . . ? C21 P2 Ru1 122.25(18) . . ? C27 P2 Ru1 112.55(18) . . ? Ru1 O1 H1 118(6) . . ? Ru1 O1 H2 114(6) . . ? H1 O1 H2 107(3) . . ? C2 N1 C7 111.7(4) . . ? C2 N1 C8 106.0(4) . . ? C7 N1 C8 107.2(5) . . ? C2 N1 Ru1 109.5(3) . . ? C7 N1 Ru1 110.1(3) . . ? C8 N1 Ru1 112.3(3) . . ? C2 C1 C6 120.3(5) . . ? C2 C1 P1 117.4(4) . . ? C6 C1 P1 122.3(5) . . ? C1 C2 C3 119.8(5) . . ? C1 C2 N1 118.5(4) . . ? C3 C2 N1 121.3(5) . . ? C4 C3 C2 119.3(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 121.0(6) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.5(6) . . ? C1 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C14 118.0(6) . . ? C10 C9 P1 120.6(4) . . ? C14 C9 P1 121.3(5) . . ? C11 C10 C9 120.6(6) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 120.8(6) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 120.3(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C14 119.5(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C9 120.9(6) . . ? C13 C14 H14 119.6 . . ? C9 C14 H14 119.6 . . ? C20 C15 C16 119.0(6) . . ? C20 C15 P1 121.0(5) . . ? C16 C15 P1 119.8(4) . . ? C17 C16 C15 120.6(6) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 119.8(7) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C19 C18 C17 120.2(6) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.0(7) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C15 C20 C19 120.4(6) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C26 118.4(6) . . ? C22 C21 P2 119.3(5) . . ? C26 C21 P2 122.2(4) . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.6(6) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.0(6) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.6(6) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C32 C27 C28 118.5(5) . . ? C32 C27 P2 117.9(4) . . ? C28 C27 P2 123.6(5) . . ? C29 C28 C27 119.5(6) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C30 C29 C28 120.9(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 120.0(6) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 119.1(6) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C31 C32 C27 122.1(5) . . ? C31 C32 H32 119.0 . . ? C27 C32 H32 119.0 . . ? C34 C33 C38 117.7(5) . . ? C34 C33 P2 123.2(5) . . ? C38 C33 P2 119.0(4) . . ? C35 C34 C33 121.3(6) . . ? C35 C34 H34 119.3 . . ? C33 C34 H34 119.3 . . ? C34 C35 C36 120.0(6) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 119.6(6) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 120.2(6) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 121.1(5) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C40 C39 C44 119.3(11) . . ? C40 C39 H39 120.4 . . ? C44 C39 H39 120.4 . . ? C41 C40 C39 119.7(13) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C42 C41 C40 120.2(11) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C43 C42 C41 120.1(11) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 121.0(13) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C43 C44 C39 119.7(12) . . ? C43 C44 H44 120.1 . . ? C39 C44 H44 120.1 . . ? C46 C45 C50 120.0 . . ? C46 C45 H45 120.0 . . ? C50 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C45 120.0 . . ? C49 C50 H50 120.0 . . ? C45 C50 H50 120.0 . . ? C46B C45B C50B 120.0 . . ? C46B C45B H45B 120.0 . . ? C50B C45B H45B 120.0 . . ? C45B C46B C47B 120.0 . . ? C45B C46B H46B 120.0 . . ? C47B C46B H46B 120.0 . . ? C46B C47B C48B 120.0 . . ? C46B C47B H47B 120.0 . . ? C48B C47B H47B 120.0 . . ? C49B C48B C47B 120.0 . . ? C49B C48B H48B 120.0 . . ? C47B C48B H48B 120.0 . . ? C48B C49B C50B 120.0 . . ? C48B C49B H49B 120.0 . . ? C50B C49B H49B 120.0 . . ? C49B C50B C45B 120.0 . . ? C49B C50B H50B 120.0 . . ? C45B C50B H50B 120.0 . . ? C46C C45C C50C 120.0 . . ? C46C C45C H45C 120.0 . . ? C50C C45C H45C 120.0 . . ? C45C C46C C47C 120.0 . . ? C45C C46C H46C 120.0 . . ? C47C C46C H46C 120.0 . . ? C48C C47C C46C 120.0 . . ? C48C C47C H47C 120.0 . . ? C46C C47C H47C 120.0 . . ? C49C C48C C47C 120.0 . . ? C49C C48C H48C 120.0 . . ? C47C C48C H48C 120.0 . . ? C48C C49C C50C 120.0 . . ? C48C C49C H49C 120.0 . . ? C50C C49C H49C 120.0 . . ? C49C C50C C45C 120.0 . . ? C49C C50C H50C 120.0 . . ? C45C C50C H50C 120.0 . . ? 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 P1 C1 C2 -137.0(4) . . . . ? C9 P1 C1 C2 118.0(5) . . . . ? Ru1 P1 C1 C2 -13.9(5) . . . . ? C15 P1 C1 C6 40.8(5) . . . . ? C9 P1 C1 C6 -64.2(5) . . . . ? Ru1 P1 C1 C6 163.9(4) . . . . ? C6 C1 C2 C3 -2.3(8) . . . . ? P1 C1 C2 C3 175.6(4) . . . . ? C6 C1 C2 N1 170.9(5) . . . . ? P1 C1 C2 N1 -11.3(7) . . . . ? C7 N1 C2 C1 152.8(5) . . . . ? C8 N1 C2 C1 -90.8(6) . . . . ? Ru1 N1 C2 C1 30.5(6) . . . . ? C7 N1 C2 C3 -34.2(7) . . . . ? C8 N1 C2 C3 82.2(6) . . . . ? Ru1 N1 C2 C3 -156.5(5) . . . . ? C1 C2 C3 C4 0.4(9) . . . . ? N1 C2 C3 C4 -172.5(5) . . . . ? C2 C3 C4 C5 1.4(10) . . . . ? C3 C4 C5 C6 -1.3(10) . . . . ? C2 C1 C6 C5 2.4(9) . . . . ? P1 C1 C6 C5 -175.4(4) . . . . ? C4 C5 C6 C1 -0.6(9) . . . . ? C1 P1 C9 C10 -98.7(5) . . . . ? C15 P1 C9 C10 155.2(4) . . . . ? Ru1 P1 C9 C10 15.9(5) . . . . ? C1 P1 C9 C14 76.2(5) . . . . ? C15 P1 C9 C14 -29.9(5) . . . . ? Ru1 P1 C9 C14 -169.1(4) . . . . ? C14 C9 C10 C11 1.0(8) . . . . ? P1 C9 C10 C11 176.0(4) . . . . ? C9 C10 C11 C12 -0.7(9) . . . . ? C10 C11 C12 C13 -0.5(11) . . . . ? C11 C12 C13 C14 1.4(11) . . . . ? C12 C13 C14 C9 -1.2(11) . . . . ? C10 C9 C14 C13 0.0(9) . . . . ? P1 C9 C14 C13 -175.0(5) . . . . ? C1 P1 C15 C20 33.8(5) . . . . ? C9 P1 C15 C20 137.6(5) . . . . ? Ru1 P1 C15 C20 -78.5(5) . . . . ? C1 P1 C15 C16 -151.0(5) . . . . ? C9 P1 C15 C16 -47.2(5) . . . . ? Ru1 P1 C15 C16 96.6(5) . . . . ? C20 C15 C16 C17 -1.3(9) . . . . ? P1 C15 C16 C17 -176.6(5) . . . . ? C15 C16 C17 C18 1.4(10) . . . . ? C16 C17 C18 C19 0.2(11) . . . . ? C17 C18 C19 C20 -2.0(11) . . . . ? C16 C15 C20 C19 -0.4(9) . . . . ? P1 C15 C20 C19 174.8(5) . . . . ? C18 C19 C20 C15 2.1(10) . . . . ? C33 P2 C21 C22 170.4(5) . . . . ? C27 P2 C21 C22 -88.0(5) . . . . ? Ru1 P2 C21 C22 38.1(6) . . . . ? C33 P2 C21 C26 -11.8(5) . . . . ? C27 P2 C21 C26 89.8(5) . . . . ? Ru1 P2 C21 C26 -144.1(4) . . . . ? C26 C21 C22 C23 0.2(10) . . . . ? P2 C21 C22 C23 178.1(5) . . . . ? C21 C22 C23 C24 -1.2(11) . . . . ? C22 C23 C24 C25 1.2(11) . . . . ? C23 C24 C25 C26 -0.2(11) . . . . ? C24 C25 C26 C21 -0.8(10) . . . . ? C22 C21 C26 C25 0.8(9) . . . . ? P2 C21 C26 C25 -177.0(5) . . . . ? C33 P2 C27 C32 -59.5(5) . . . . ? C21 P2 C27 C32 -163.0(4) . . . . ? Ru1 P2 C27 C32 64.7(4) . . . . ? C33 P2 C27 C28 118.7(5) . . . . ? C21 P2 C27 C28 15.2(5) . . . . ? Ru1 P2 C27 C28 -117.1(4) . . . . ? C32 C27 C28 C29 1.7(8) . . . . ? P2 C27 C28 C29 -176.5(5) . . . . ? C27 C28 C29 C30 -0.7(9) . . . . ? C28 C29 C30 C31 -0.7(10) . . . . ? C29 C30 C31 C32 0.9(10) . . . . ? C30 C31 C32 C27 0.2(9) . . . . ? C28 C27 C32 C31 -1.5(8) . . . . ? P2 C27 C32 C31 176.8(5) . . . . ? C21 P2 C33 C34 79.5(6) . . . . ? C27 P2 C33 C34 -24.1(6) . . . . ? Ru1 P2 C33 C34 -145.1(5) . . . . ? C21 P2 C33 C38 -99.1(5) . . . . ? C27 P2 C33 C38 157.3(5) . . . . ? Ru1 P2 C33 C38 36.3(5) . . . . ? C38 C33 C34 C35 -0.4(10) . . . . ? P2 C33 C34 C35 -179.0(5) . . . . ? C33 C34 C35 C36 0.1(11) . . . . ? C34 C35 C36 C37 -0.3(12) . . . . ? C35 C36 C37 C38 0.7(12) . . . . ? C36 C37 C38 C33 -1.0(11) . . . . ? C34 C33 C38 C37 0.8(10) . . . . ? P2 C33 C38 C37 179.5(5) . . . . ? C44 C39 C40 C41 -2.0(17) . . . . ? C39 C40 C41 C42 2.1(17) . . . . ? C40 C41 C42 C43 -1.3(16) . . . . ? C41 C42 C43 C44 0.4(16) . . . . ? C42 C43 C44 C39 -0.4(17) . . . . ? C40 C39 C44 C43 1.2(17) . . . . ? C50 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C45 0.0 . . . . ? C46 C45 C50 C49 0.0 . . . . ? C50B C45B C46B C47B 0.0 . . . . ? C45B C46B C47B C48B 0.0 . . . . ? C46B C47B C48B C49B 0.0 . . . . ? C47B C48B C49B C50B 0.0 . . . . ? C48B C49B C50B C45B 0.0 . . . . ? C46B C45B C50B C49B 0.0 . . . . ? C50C C45C C46C C47C 0.0 . . . . ? C45C C46C C47C C48C 0.0 . . . . ? C46C C47C C48C C49C 0.0 . . . . ? C47C C48C C49C C50C 0.0 . . . . ? C48C C49C C50C C45C 0.0 . . . . ? C46C C45C C50C C49C 0.0 . . . . ? _refine_diff_density_max 2.034 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.140 _shelxl_version_number 2012-9 _shelx_res_file ; TITL bj254 CELL 0.71070 10.5773 16.9790 24.2616 90.000 90.706 90.000 ZERR 4.00 0.0006 0.0020 0.0006 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O P CL RU UNIT 200 196 4 4 8 8 4 MERG 2 DFIX 0.87 0.01 O1 H1 O1 H2 SIMU ISOR SUMP 1 0.005 1 2 1 3 1 4 DFIX -1.400 0.020 H1 H2 FMAP 2 PLAN 20 ACTA 50.00 BOND $H CONF L.S. 20 TEMP -93.00 WGHT 0.080100 17.592602 FVAR 0.50586 0.44946 0.31643 0.22071 RU1 7 0.435657 0.534719 0.370071 11.00000 0.02182 0.02849 = 0.02606 -0.00070 -0.00470 -0.00073 CL1 6 0.271827 0.616215 0.331819 11.00000 0.02389 0.03615 = 0.03710 0.00111 -0.00482 0.00293 CL2 6 0.584359 0.468217 0.430679 11.00000 0.03002 0.03494 = 0.02616 0.00072 -0.00833 0.00162 P1 5 0.578706 0.527447 0.303480 11.00000 0.01996 0.03104 = 0.02765 -0.00059 -0.00193 -0.00111 P2 5 0.311507 0.427892 0.345297 11.00000 0.02559 0.02901 = 0.02762 0.00032 -0.00374 -0.00349 O1 4 0.325779 0.551015 0.447193 11.00000 0.03281 0.04483 = 0.02584 0.00177 0.00140 0.00400 N1 3 0.554433 0.644273 0.393540 11.00000 0.02838 0.03091 = 0.02833 -0.00101 -0.00403 -0.00258 C1 1 0.710721 0.584867 0.331793 11.00000 0.02393 0.02952 = 0.04236 0.00605 -0.00462 0.00048 C2 1 0.686919 0.631787 0.377343 11.00000 0.02768 0.03085 = 0.03435 0.00450 -0.00712 -0.00363 C3 1 0.785755 0.672528 0.402932 11.00000 0.03467 0.04182 = 0.04999 -0.00253 -0.01409 -0.00897 AFIX 43 H3 2 0.770342 0.704509 0.434269 11.00000 -1.20000 AFIX 0 C4 1 0.907325 0.665887 0.382107 11.00000 0.03947 0.04446 = 0.06264 0.00877 -0.02375 -0.01161 AFIX 43 H4 2 0.975221 0.692657 0.399969 11.00000 -1.20000 AFIX 0 C5 1 0.930495 0.621540 0.336451 11.00000 0.02074 0.05649 = 0.06283 0.02228 -0.00382 -0.00057 AFIX 43 H5 2 1.013713 0.618506 0.322315 11.00000 -1.20000 AFIX 0 C6 1 0.831862 0.580549 0.310444 11.00000 0.02905 0.04011 = 0.05115 0.01303 -0.00297 -0.00825 AFIX 43 H6 2 0.847514 0.549995 0.278443 11.00000 -1.20000 AFIX 0 C7 1 0.543973 0.660553 0.453488 11.00000 0.04116 0.04346 = 0.04215 -0.01230 -0.00364 -0.00758 AFIX 137 H7A 2 0.582076 0.617117 0.474470 11.00000 -1.50000 H7B 2 0.454631 0.665586 0.463123 11.00000 -1.50000 H7C 2 0.588313 0.709691 0.462409 11.00000 -1.50000 AFIX 0 C8 1 0.511223 0.716521 0.363735 11.00000 0.03950 0.03119 = 0.04904 -0.00156 -0.00800 -0.00151 AFIX 137 H8A 2 0.565137 0.761081 0.374356 11.00000 -1.50000 H8B 2 0.423441 0.728021 0.373384 11.00000 -1.50000 H8C 2 0.516725 0.707891 0.323897 11.00000 -1.50000 AFIX 0 C9 1 0.566299 0.570343 0.233600 11.00000 0.03295 0.03497 = 0.03379 -0.00114 -0.00393 -0.00700 C10 1 0.476154 0.628115 0.221624 11.00000 0.03186 0.03725 = 0.03567 0.00471 -0.00304 -0.00693 AFIX 43 H10 2 0.417253 0.643142 0.248936 11.00000 -1.20000 AFIX 0 C11 1 0.471862 0.663579 0.170466 11.00000 0.04170 0.04191 = 0.04841 0.01276 -0.00834 -0.00194 AFIX 43 H11 2 0.409338 0.702352 0.162780 11.00000 -1.20000 AFIX 0 C12 1 0.557245 0.643408 0.130372 11.00000 0.05507 0.05731 = 0.03758 0.00737 -0.00402 0.00081 AFIX 43 H12 2 0.552785 0.668040 0.095244 11.00000 -1.20000 AFIX 0 C13 1 0.649033 0.587666 0.141037 11.00000 0.05964 0.06823 = 0.04304 0.00562 0.01177 0.00858 AFIX 43 H13 2 0.709002 0.574631 0.113671 11.00000 -1.20000 AFIX 0 C14 1 0.653232 0.550582 0.192227 11.00000 0.04462 0.06038 = 0.03148 -0.00125 -0.00032 0.00911 AFIX 43 H14 2 0.715500 0.511448 0.199369 11.00000 -1.20000 AFIX 0 C15 1 0.650540 0.430631 0.289445 11.00000 0.02649 0.03430 = 0.04016 -0.00431 0.00649 0.00028 C16 1 0.602317 0.383776 0.247041 11.00000 0.04230 0.04298 = 0.04403 -0.00426 0.00126 -0.00064 AFIX 43 H16 2 0.535570 0.403100 0.224239 11.00000 -1.20000 AFIX 0 C17 1 0.650702 0.309445 0.237852 11.00000 0.06068 0.04250 = 0.06237 -0.01623 0.01476 -0.00326 AFIX 43 H17 2 0.618660 0.278271 0.208316 11.00000 -1.20000 AFIX 0 C18 1 0.746115 0.280468 0.271834 11.00000 0.05098 0.03782 = 0.09019 -0.00717 0.01513 0.00849 AFIX 43 H18 2 0.779732 0.229430 0.265479 11.00000 -1.20000 AFIX 0 C19 1 0.792248 0.325359 0.314707 11.00000 0.03665 0.03527 = 0.07038 0.00527 0.01316 0.00930 AFIX 43 H19 2 0.855764 0.304709 0.338664 11.00000 -1.20000 AFIX 0 C20 1 0.745927 0.401002 0.323003 11.00000 0.03110 0.03576 = 0.04857 0.00498 0.00341 -0.00012 AFIX 43 H20 2 0.780003 0.432555 0.351909 11.00000 -1.20000 AFIX 0 C21 1 0.377806 0.327916 0.336830 11.00000 0.02652 0.03566 = 0.03439 0.00368 0.00096 -0.00022 C22 1 0.472040 0.302331 0.372649 11.00000 0.04277 0.04427 = 0.04509 -0.00447 -0.00961 -0.00185 AFIX 43 H22 2 0.503217 0.336967 0.400403 11.00000 -1.20000 AFIX 0 C23 1 0.521533 0.227222 0.368708 11.00000 0.05196 0.03144 = 0.06497 -0.00121 -0.01646 0.00477 AFIX 43 H23 2 0.587338 0.210811 0.393111 11.00000 -1.20000 AFIX 0 C24 1 0.474634 0.175983 0.328961 11.00000 0.04444 0.03299 = 0.07401 -0.00583 0.00392 -0.00095 AFIX 43 H24 2 0.507248 0.123978 0.326585 11.00000 -1.20000 AFIX 0 C25 1 0.381160 0.200169 0.293003 11.00000 0.04036 0.03847 = 0.06489 -0.02075 0.00182 -0.00251 AFIX 43 H25 2 0.349389 0.164983 0.265721 11.00000 -1.20000 AFIX 0 C26 1 0.333194 0.275953 0.296539 11.00000 0.03709 0.04252 = 0.03719 -0.00929 -0.00335 -0.00410 AFIX 43 H26 2 0.269316 0.292658 0.271273 11.00000 -1.20000 AFIX 0 C27 1 0.182869 0.409240 0.394937 11.00000 0.02674 0.03535 = 0.03151 -0.00007 -0.00795 -0.01042 C28 1 0.173046 0.340020 0.426100 11.00000 0.04085 0.03400 = 0.04301 -0.00357 -0.00984 -0.00583 AFIX 43 H28 2 0.236644 0.300660 0.424026 11.00000 -1.20000 AFIX 0 C29 1 0.069267 0.329408 0.460142 11.00000 0.05447 0.04535 = 0.04267 0.00548 0.00781 -0.01093 AFIX 43 H29 2 0.062072 0.282288 0.480983 11.00000 -1.20000 AFIX 0 C30 1 -0.023776 0.386773 0.464013 11.00000 0.04153 0.05813 = 0.04217 -0.00233 0.00595 -0.01251 AFIX 43 H30 2 -0.094478 0.378541 0.487087 11.00000 -1.20000 AFIX 0 C31 1 -0.013429 0.455976 0.434222 11.00000 0.02754 0.05295 = 0.04275 -0.00430 0.00193 -0.00106 AFIX 43 H31 2 -0.076080 0.495814 0.437054 11.00000 -1.20000 AFIX 0 C32 1 0.089462 0.466331 0.400247 11.00000 0.02836 0.03533 = 0.03629 0.00802 0.00027 -0.00113 AFIX 43 H32 2 0.096501 0.513919 0.379921 11.00000 -1.20000 AFIX 0 C33 1 0.215168 0.437586 0.281873 11.00000 0.02527 0.03431 = 0.03357 -0.00289 -0.00740 -0.00140 C34 1 0.096125 0.404232 0.275567 11.00000 0.03617 0.05221 = 0.03816 0.00212 -0.01345 -0.01322 AFIX 43 H34 2 0.060882 0.375524 0.305270 11.00000 -1.20000 AFIX 0 C35 1 0.027792 0.411920 0.226964 11.00000 0.03352 0.06912 = 0.04700 -0.00789 -0.01454 -0.01025 AFIX 43 H35 2 -0.053646 0.388709 0.223525 11.00000 -1.20000 AFIX 0 C36 1 0.077950 0.453406 0.183319 11.00000 0.05778 0.07082 = 0.03625 0.00235 -0.02174 -0.00850 AFIX 43 H36 2 0.031377 0.458617 0.149787 11.00000 -1.20000 AFIX 0 C37 1 0.196022 0.487159 0.188802 11.00000 0.05150 0.05925 = 0.02986 0.00546 -0.01091 -0.01318 AFIX 43 H37 2 0.230506 0.516219 0.159093 11.00000 -1.20000 AFIX 0 C38 1 0.264227 0.478862 0.237291 11.00000 0.03801 0.04824 = 0.03511 0.00071 -0.00791 -0.01193 AFIX 43 H38 2 0.346029 0.501666 0.240359 11.00000 -1.20000 AFIX 0 C39 1 0.264328 0.125643 0.468160 11.00000 0.18970 0.04924 = 0.09687 0.02543 -0.07544 -0.01643 AFIX 43 H39 2 0.246108 0.137075 0.430563 11.00000 -1.20000 AFIX 0 C40 1 0.386354 0.109747 0.485136 11.00000 0.14441 0.08091 = 0.08741 0.01257 -0.00956 -0.02149 AFIX 43 H40 2 0.452623 0.108464 0.459075 11.00000 -1.20000 AFIX 0 C41 1 0.411698 0.095853 0.539514 11.00000 0.10563 0.08520 = 0.08620 0.02777 -0.03304 -0.02598 AFIX 43 H41 2 0.496234 0.086632 0.551522 11.00000 -1.20000 AFIX 0 C42 1 0.316198 0.095149 0.576683 11.00000 0.08788 0.07988 = 0.08569 0.00207 -0.02787 -0.01302 AFIX 43 H42 2 0.334005 0.084354 0.614408 11.00000 -1.20000 AFIX 0 C43 1 0.196310 0.109776 0.559956 11.00000 0.09032 0.07092 = 0.12826 -0.00444 -0.04076 0.00892 AFIX 43 H43 2 0.130379 0.109523 0.586193 11.00000 -1.20000 AFIX 0 C44 1 0.168629 0.124782 0.506433 11.00000 0.12290 0.06167 = 0.14284 0.00082 -0.07303 0.00182 AFIX 43 H44 2 0.083770 0.134691 0.495177 11.00000 -1.20000 PART 1 AFIX 66 C45 1 0.772649 0.182555 0.511384 21.00000 0.07539 0.06673 = 0.06820 -0.01016 0.00928 -0.00071 AFIX 43 H45 2 0.738197 0.205593 0.478831 21.00000 -1.20000 AFIX 65 C46 1 0.788722 0.227870 0.558668 21.00000 0.05884 0.06324 = 0.06431 0.00255 0.00946 -0.01549 AFIX 43 H46 2 0.765255 0.281878 0.558431 21.00000 -1.20000 AFIX 65 C47 1 0.839130 0.194162 0.606300 21.00000 0.07768 0.07216 = 0.06653 -0.01268 0.01937 -0.02604 AFIX 43 H47 2 0.850115 0.225132 0.638616 21.00000 -1.20000 AFIX 65 C48 1 0.873465 0.115140 0.606647 21.00000 0.11182 0.06900 = 0.05346 -0.01439 0.01087 -0.04114 AFIX 43 H48 2 0.907917 0.092103 0.639201 21.00000 -1.20000 AFIX 65 C49 1 0.857393 0.069825 0.559364 21.00000 0.12011 0.06870 = 0.06414 -0.01755 -0.00021 -0.03034 AFIX 43 H49 2 0.880860 0.015817 0.559602 21.00000 -1.20000 AFIX 65 C50 1 0.806985 0.103532 0.511732 21.00000 0.09677 0.06232 = 0.05724 -0.01453 0.00925 -0.01848 AFIX 43 H50 2 0.796001 0.072561 0.479416 21.00000 -1.20000 PART 2 AFIX 66 C45B 1 0.748730 0.231870 0.504318 31.00000 0.05582 0.04788 = 0.06683 -0.00990 0.01708 0.00637 AFIX 43 H45B 2 0.722986 0.273259 0.480341 31.00000 -1.20000 AFIX 65 C46B 1 0.745087 0.154270 0.486113 31.00000 0.06863 0.06260 = 0.07567 -0.02919 0.00861 0.00570 AFIX 43 H46B 2 0.716853 0.142624 0.449695 31.00000 -1.20000 AFIX 65 C47B 1 0.782754 0.093711 0.521195 31.00000 0.09747 0.07092 = 0.08383 -0.01026 0.00337 -0.01539 AFIX 43 H47B 2 0.780264 0.040676 0.508753 31.00000 -1.20000 AFIX 65 C48B 1 0.824065 0.110751 0.574482 31.00000 0.09405 0.06750 = 0.07701 0.00369 0.00241 -0.01582 AFIX 43 H48B 2 0.849809 0.069361 0.598459 31.00000 -1.20000 AFIX 65 C49B 1 0.827708 0.188350 0.592687 31.00000 0.06931 0.06275 = 0.05467 -0.00456 0.01788 -0.01086 AFIX 43 H49B 2 0.855942 0.199995 0.629106 31.00000 -1.20000 AFIX 65 C50B 1 0.790042 0.248909 0.557606 31.00000 0.05255 0.05610 = 0.06543 -0.00342 0.01402 -0.00025 AFIX 43 H50B 2 0.792532 0.301945 0.570048 31.00000 -1.20000 PART 3 AFIX 66 C45C 1 0.753949 0.218198 0.526584 41.00000 0.06680 0.05360 = 0.06144 -0.00977 0.01719 0.00418 AFIX 43 H45C 2 0.716554 0.264163 0.511128 41.00000 -1.20000 AFIX 65 C46C 1 0.801082 0.219486 0.580310 41.00000 0.06286 0.06201 = 0.06245 -0.00749 0.02022 -0.02240 AFIX 43 H46C 2 0.795901 0.266332 0.601574 41.00000 -1.20000 AFIX 65 C47C 1 0.855797 0.152232 0.602925 41.00000 0.09238 0.06370 = 0.07162 -0.02079 0.01359 -0.01973 AFIX 43 H47C 2 0.888010 0.153113 0.639644 41.00000 -1.20000 AFIX 65 C48C 1 0.863379 0.083690 0.571813 41.00000 0.10782 0.06516 = 0.06830 -0.01105 0.01758 -0.01475 AFIX 43 H48C 2 0.900774 0.037725 0.587269 41.00000 -1.20000 AFIX 65 C49C 1 0.816247 0.082400 0.518086 41.00000 0.08538 0.06267 = 0.07417 -0.00407 -0.00045 -0.00009 AFIX 43 H49C 2 0.821429 0.035554 0.496823 41.00000 -1.20000 AFIX 65 C50C 1 0.761532 0.149654 0.495471 41.00000 0.07069 0.05490 = 0.06677 -0.01957 0.00662 0.01226 AFIX 43 H50C 2 0.729318 0.148773 0.458752 41.00000 -1.20000 AFIX 0 PART 0 H1 2 0.362694 0.539748 0.478445 11.00000 -1.50000 H2 2 0.253488 0.526593 0.447020 11.00000 -1.50000 HKLF 4 REM bj254 REM R1 = 0.0759 for 6767 Fo > 4sig(Fo) and 0.1357 for all 10710 data REM 597 parameters refined using 1150 restraints END WGHT 0.0804 17.7144 REM Highest difference peak 2.034, deepest hole -1.392, 1-sigma level 0.140 Q1 1 0.4365 0.3999 0.3704 11.00000 0.05 2.03 Q2 1 0.8086 0.0352 0.6114 11.00000 0.05 1.68 Q3 1 0.2827 0.4624 0.3143 11.00000 0.05 1.32 Q4 1 0.4584 0.5337 0.1710 11.00000 0.05 1.31 Q5 1 0.3263 0.5046 0.3473 11.00000 0.05 1.26 Q6 1 0.5538 0.4273 0.3926 11.00000 0.05 1.14 Q7 1 0.6435 0.1154 0.5712 11.00000 0.05 1.02 Q8 1 0.2685 0.3171 0.3330 11.00000 0.05 1.00 Q9 1 0.3179 0.0665 0.4147 11.00000 0.05 0.94 Q10 1 0.5839 0.6003 0.4251 11.00000 0.05 0.92 Q11 1 0.9541 0.0312 0.5434 11.00000 0.05 0.91 Q12 1 0.3122 0.6448 0.3435 11.00000 0.05 0.87 Q13 1 0.6019 0.5290 0.1076 11.00000 0.05 0.74 Q14 1 0.5793 0.4077 0.3033 11.00000 0.05 0.73 Q15 1 0.4829 0.4589 0.3639 11.00000 0.05 0.62 Q16 1 0.3602 0.5862 0.3370 11.00000 0.05 0.61 Q17 1 0.4421 0.4669 0.4934 11.00000 0.05 0.60 Q18 1 0.3365 0.6528 0.2928 11.00000 0.05 0.60 Q19 1 0.7317 0.4685 0.3653 11.00000 0.05 0.60 Q20 1 0.2928 0.5356 0.4364 11.00000 0.05 0.60 ; _shelx_res_checksum 33753 _shelx_hkl_checksum 35083 data_bj255 _database_code_depnum_ccdc_archive 'CCDC 913687' #TrackingRef 'bj254_bj255.cif' _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H46 Cl2 N O P2 Ru' _chemical_formula_weight 874.76 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9020(8) _cell_length_b 12.7647(13) _cell_length_c 15.590(2) _cell_angle_alpha 106.371(5) _cell_angle_beta 94.400(3) _cell_angle_gamma 113.7900(10) _cell_volume 2029.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 11863 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.431 _exptl_crystal_F_000 902 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_absorpt_coefficient_mu 0.634 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.620 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Rigaku/ADSC CCD' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18577 _diffrn_reflns_av_unetI/netI 0.0625 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.856 _diffrn_reflns_theta_max 30.024 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.773 _diffrn_measured_fraction_theta_full 0.965 _diffrn_reflns_Laue_measured_fraction_max 0.773 _diffrn_reflns_Laue_measured_fraction_full 0.965 _diffrn_reflns_point_group_measured_fraction_max 0.773 _diffrn_reflns_point_group_measured_fraction_full 0.965 _reflns_number_total 9156 _reflns_number_gt 6959 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR97 (Giacovazzo, 1999)' _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0563P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9156 _refine_ls_number_parameters 497 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 C1 C 0.2975(2) 0.4150(3) 0.07483(18) 0.0188(6) Uani 1 1 d . . . . . C2 C 0.3050(2) 0.3143(3) 0.01753(19) 0.0203(6) Uani 1 1 d . . . . . C3 C 0.3219(3) 0.3082(3) -0.0708(2) 0.0317(7) Uani 1 1 d . . . . . H3 H 0.3297 0.2404 -0.1096 0.038 Uiso 1 1 calc R U . . . C4 C 0.3274(3) 0.4012(3) -0.1023(2) 0.0372(8) Uani 1 1 d . . . . . H4 H 0.3370 0.3959 -0.1631 0.045 Uiso 1 1 calc R U . . . C5 C 0.3189(3) 0.5010(3) -0.0458(2) 0.0297(7) Uani 1 1 d . . . . . H5 H 0.3226 0.5645 -0.0676 0.036 Uiso 1 1 calc R U . . . C6 C 0.3052(2) 0.5090(3) 0.0427(2) 0.0248(6) Uani 1 1 d . . . . . H6 H 0.3009 0.5787 0.0819 0.030 Uiso 1 1 calc R U . . . C7 C 0.2465(3) 0.0969(3) -0.0178(2) 0.0283(7) Uani 1 1 d . . . . . H7A H 0.1585 0.0752 -0.0418 0.042 Uiso 1 1 calc R U . . . H7B H 0.2501 0.0368 0.0085 0.042 Uiso 1 1 calc R U . . . H7C H 0.2919 0.0977 -0.0676 0.042 Uiso 1 1 calc R U . . . C8 C 0.4403(3) 0.2489(3) 0.0849(2) 0.0281(7) Uani 1 1 d . . . . . H8A H 0.4809 0.2477 0.0325 0.042 Uiso 1 1 calc R U . . . H8B H 0.4446 0.1880 0.1100 0.042 Uiso 1 1 calc R U . . . H8C H 0.4837 0.3300 0.1322 0.042 Uiso 1 1 calc R U . . . C9 C 0.4260(2) 0.5421(3) 0.25908(18) 0.0175(6) Uani 1 1 d . . . . . C10 C 0.5203(2) 0.5189(3) 0.29657(18) 0.0210(6) Uani 1 1 d . . . . . H10 H 0.5028 0.4379 0.2922 0.025 Uiso 1 1 calc R U . . . C11 C 0.6393(3) 0.6131(3) 0.3401(2) 0.0263(7) Uani 1 1 d . . . . . H11 H 0.7025 0.5960 0.3653 0.032 Uiso 1 1 calc R U . . . C12 C 0.6661(3) 0.7313(3) 0.3468(2) 0.0290(7) Uani 1 1 d . . . . . H12 H 0.7479 0.7954 0.3759 0.035 Uiso 1 1 calc R U . . . C13 C 0.5734(3) 0.7558(3) 0.3109(2) 0.0325(7) Uani 1 1 d . . . . . H13 H 0.5914 0.8372 0.3159 0.039 Uiso 1 1 calc R U . . . C14 C 0.4546(3) 0.6627(3) 0.2678(2) 0.0260(7) Uani 1 1 d . . . . . H14 H 0.3916 0.6808 0.2438 0.031 Uiso 1 1 calc R U . . . C15 C 0.1672(2) 0.4875(2) 0.21093(19) 0.0168(6) Uani 1 1 d . . . . . C16 C 0.0754(3) 0.4704(3) 0.1405(2) 0.0229(6) Uani 1 1 d . . . . . H16 H 0.0735 0.4292 0.0788 0.028 Uiso 1 1 calc R U . . . C17 C -0.0139(3) 0.5134(3) 0.1596(2) 0.0328(8) Uani 1 1 d . . . . . H17 H -0.0755 0.5022 0.1110 0.039 Uiso 1 1 calc R U . . . C18 C -0.0130(3) 0.5719(3) 0.2487(3) 0.0353(8) Uani 1 1 d . . . . . H18 H -0.0756 0.5988 0.2617 0.042 Uiso 1 1 calc R U . . . C19 C 0.0789(3) 0.5916(3) 0.3194(2) 0.0315(7) Uani 1 1 d . . . . . H19 H 0.0803 0.6332 0.3808 0.038 Uiso 1 1 calc R U . . . C20 C 0.1690(3) 0.5507(3) 0.3009(2) 0.0232(6) Uani 1 1 d . . . . . H20 H 0.2327 0.5657 0.3497 0.028 Uiso 1 1 calc R U . . . C21 C 0.1731(2) 0.3499(2) 0.39924(18) 0.0171(6) Uani 1 1 d . . . . . C22 C 0.3035(2) 0.4192(3) 0.42022(18) 0.0185(6) Uani 1 1 d . . . . . H22 H 0.3527 0.3912 0.3836 0.022 Uiso 1 1 calc R U . . . C23 C 0.3623(3) 0.5277(3) 0.49308(19) 0.0235(6) Uani 1 1 d . . . . . H23 H 0.4511 0.5736 0.5057 0.028 Uiso 1 1 calc R U . . . C24 C 0.2928(3) 0.5700(3) 0.5478(2) 0.0274(7) Uani 1 1 d . . . . . H24 H 0.3330 0.6455 0.5971 0.033 Uiso 1 1 calc R U . . . C25 C 0.1632(3) 0.5001(3) 0.5297(2) 0.0277(7) Uani 1 1 d . . . . . H25 H 0.1149 0.5270 0.5680 0.033 Uiso 1 1 calc R U . . . C26 C 0.1043(3) 0.3922(3) 0.4566(2) 0.0234(6) Uani 1 1 d . . . . . H26 H 0.0156 0.3459 0.4450 0.028 Uiso 1 1 calc R U . . . C27 C -0.0654(2) 0.1929(3) 0.28044(18) 0.0176(6) Uani 1 1 d . . . . . C28 C -0.1051(2) 0.2530(3) 0.23310(19) 0.0213(6) Uani 1 1 d . . . . . H28 H -0.0492 0.2999 0.2032 0.026 Uiso 1 1 calc R U . . . C29 C -0.2251(3) 0.2461(3) 0.2284(2) 0.0299(7) Uani 1 1 d . . . . . H29 H -0.2498 0.2891 0.1962 0.036 Uiso 1 1 calc R U . . . C30 C -0.3089(3) 0.1770(3) 0.2704(2) 0.0306(8) Uani 1 1 d . . . . . H30 H -0.3917 0.1705 0.2657 0.037 Uiso 1 1 calc R U . . . C31 C -0.2706(3) 0.1180(3) 0.3190(2) 0.0325(8) Uani 1 1 d . . . . . H31 H -0.3268 0.0720 0.3493 0.039 Uiso 1 1 calc R U . . . C32 C -0.1505(3) 0.1250(3) 0.3242(2) 0.0271(7) Uani 1 1 d . . . . . H32 H -0.1257 0.0834 0.3577 0.033 Uiso 1 1 calc R U . . . C33 C 0.0839(2) 0.0881(3) 0.33274(19) 0.0179(6) Uani 1 1 d . . . . . C34 C 0.1522(3) 0.1046(3) 0.4158(2) 0.0258(7) Uani 1 1 d . . . . . H34 H 0.2117 0.1842 0.4542 0.031 Uiso 1 1 calc R U . . . C35 C 0.1337(3) 0.0049(3) 0.4429(2) 0.0345(8) Uani 1 1 d . . . . . H35 H 0.1801 0.0169 0.5001 0.041 Uiso 1 1 calc R U . . . C36 C 0.0487(3) -0.1109(3) 0.3874(2) 0.0344(8) Uani 1 1 d . . . . . H36 H 0.0363 -0.1785 0.4065 0.041 Uiso 1 1 calc R U . . . C37 C -0.0188(3) -0.1289(3) 0.3038(2) 0.0311(7) Uani 1 1 d . . . . . H37 H -0.0768 -0.2088 0.2650 0.037 Uiso 1 1 calc R U . . . C38 C -0.0015(3) -0.0301(3) 0.2772(2) 0.0245(6) Uani 1 1 d . . . . . H38 H -0.0484 -0.0427 0.2201 0.029 Uiso 1 1 calc R U . . . C39 C 0.2546(3) -0.1825(3) 0.1786(3) 0.0418(9) Uani 1 1 d . . . . . H39 H 0.2195 -0.1987 0.2289 0.050 Uiso 1 1 calc R U . . . C40 C 0.1786(3) -0.2295(3) 0.0927(3) 0.0388(8) Uani 1 1 d . . . . . H40 H 0.0907 -0.2774 0.0838 0.047 Uiso 1 1 calc R U . . . C41 C 0.2299(3) -0.2072(3) 0.0193(2) 0.0342(8) Uani 1 1 d . . . . . H41 H 0.1774 -0.2403 -0.0400 0.041 Uiso 1 1 calc R U . . . C42 C 0.3573(3) -0.1370(3) 0.0325(2) 0.0355(8) Uani 1 1 d . . . . . H42 H 0.3926 -0.1208 -0.0177 0.043 Uiso 1 1 calc R U . . . C43 C 0.4333(3) -0.0905(3) 0.1181(2) 0.0392(9) Uani 1 1 d . . . . . H43 H 0.5214 -0.0436 0.1268 0.047 Uiso 1 1 calc R U . . . C44 C 0.3824(3) -0.1115(4) 0.1913(3) 0.0448(9) Uani 1 1 d . . . . . H44 H 0.4350 -0.0772 0.2507 0.054 Uiso 1 1 calc R U . . . C45 C 0.5561(4) 0.1209(4) 0.5081(3) 0.0583(12) Uani 1 1 d . . . . . H45 H 0.5949 0.2044 0.5135 0.070 Uiso 1 1 calc R U . . . C46 C 0.6110(4) 0.0779(5) 0.5604(3) 0.0611(13) Uani 1 1 d . . . . . H46 H 0.6886 0.1324 0.6028 0.073 Uiso 1 1 calc R U . . . C47 C 0.5572(4) -0.0411(5) 0.5531(3) 0.0576(12) Uani 1 1 d . . . . . H47 H 0.5972 -0.0695 0.5899 0.069 Uiso 1 1 calc R U . . . N1 N 0.3057(2) 0.2201(2) 0.05450(15) 0.0174(5) Uani 1 1 d . . . . . O1 O 0.12792(19) 0.02075(18) 0.13210(14) 0.0216(4) Uani 1 1 d D . . . . P1 P 0.27393(6) 0.41610(6) 0.19004(5) 0.01372(15) Uani 1 1 d . . . . . P2 P 0.09923(6) 0.21505(6) 0.29357(5) 0.01399(15) Uani 1 1 d . . . . . Cl1 Cl 0.36591(6) 0.20752(6) 0.26851(5) 0.02083(15) Uani 1 1 d . . . . . Cl2 Cl 0.02677(6) 0.17787(6) 0.06158(4) 0.01883(15) Uani 1 1 d . . . . . Ru1 Ru 0.20217(2) 0.21925(2) 0.17401(2) 0.01265(7) Uani 1 1 d . . . . . H1 H 0.090(3) -0.025(3) 0.0762(10) 0.034(10) Uiso 1 1 d D . . . . H2 H 0.179(3) -0.005(3) 0.151(2) 0.057(12) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0129(13) 0.0200(16) 0.0179(15) 0.0049(12) 0.0015(10) 0.0034(11) C2 0.0141(13) 0.0199(16) 0.0192(15) 0.0046(13) 0.0021(11) 0.0020(11) C3 0.0404(18) 0.032(2) 0.0195(16) 0.0064(15) 0.0119(14) 0.0134(15) C4 0.0407(19) 0.044(2) 0.0239(18) 0.0156(17) 0.0126(14) 0.0123(17) C5 0.0277(16) 0.035(2) 0.0283(18) 0.0227(16) 0.0049(13) 0.0075(14) C6 0.0197(14) 0.0210(17) 0.0288(17) 0.0107(14) 0.0030(12) 0.0033(12) C7 0.0320(17) 0.0213(18) 0.0254(17) 0.0003(14) 0.0133(13) 0.0098(14) C8 0.0212(15) 0.035(2) 0.0306(17) 0.0095(15) 0.0103(13) 0.0148(14) C9 0.0166(13) 0.0146(15) 0.0134(14) 0.0000(11) 0.0030(10) 0.0026(11) C10 0.0201(14) 0.0237(17) 0.0172(15) 0.0096(13) 0.0037(11) 0.0062(12) C11 0.0181(14) 0.033(2) 0.0190(16) 0.0081(14) -0.0001(11) 0.0043(13) C12 0.0221(15) 0.0280(19) 0.0161(16) 0.0014(14) -0.0012(12) -0.0036(13) C13 0.0309(17) 0.0162(18) 0.039(2) 0.0068(15) 0.0055(14) 0.0012(13) C14 0.0221(15) 0.0150(16) 0.0317(18) 0.0037(14) 0.0009(12) 0.0033(12) C15 0.0152(13) 0.0105(14) 0.0239(15) 0.0070(12) 0.0032(11) 0.0043(11) C16 0.0217(15) 0.0174(16) 0.0285(17) 0.0102(13) 0.0014(12) 0.0066(12) C17 0.0216(16) 0.0244(19) 0.056(2) 0.0197(17) 0.0031(15) 0.0111(14) C18 0.0316(18) 0.0268(19) 0.059(2) 0.0174(17) 0.0183(16) 0.0208(15) C19 0.0387(19) 0.0169(17) 0.041(2) 0.0061(15) 0.0157(15) 0.0151(14) C20 0.0256(15) 0.0128(16) 0.0317(17) 0.0064(13) 0.0072(12) 0.0096(12) C21 0.0215(14) 0.0126(15) 0.0170(14) 0.0061(12) 0.0031(11) 0.0069(11) C22 0.0193(14) 0.0168(16) 0.0196(15) 0.0066(12) 0.0044(11) 0.0081(12) C23 0.0214(15) 0.0177(16) 0.0228(16) 0.0009(13) -0.0001(12) 0.0054(12) C24 0.0354(17) 0.0199(17) 0.0203(16) -0.0038(13) -0.0007(13) 0.0142(14) C25 0.0332(17) 0.0292(19) 0.0239(16) 0.0049(14) 0.0098(13) 0.0193(15) C26 0.0224(14) 0.0207(17) 0.0248(16) 0.0044(13) 0.0056(12) 0.0095(12) C27 0.0121(13) 0.0143(15) 0.0201(15) 0.0015(12) 0.0011(10) 0.0030(11) C28 0.0172(14) 0.0211(17) 0.0195(15) 0.0025(13) 0.0020(11) 0.0061(12) C29 0.0242(16) 0.032(2) 0.0279(17) -0.0021(15) -0.0031(13) 0.0170(14) C30 0.0141(14) 0.0252(18) 0.0365(19) -0.0074(15) 0.0023(13) 0.0063(13) C31 0.0196(15) 0.0249(19) 0.046(2) 0.0071(16) 0.0162(14) 0.0052(13) C32 0.0215(15) 0.0219(17) 0.0377(19) 0.0110(14) 0.0119(13) 0.0080(13) C33 0.0179(13) 0.0141(15) 0.0203(15) 0.0044(12) 0.0057(11) 0.0064(11) C34 0.0278(16) 0.0185(17) 0.0293(17) 0.0060(14) 0.0041(13) 0.0105(13) C35 0.048(2) 0.033(2) 0.0327(19) 0.0169(17) 0.0088(15) 0.0235(17) C36 0.054(2) 0.0208(19) 0.038(2) 0.0164(16) 0.0175(17) 0.0205(17) C37 0.0388(18) 0.0150(17) 0.0356(19) 0.0063(14) 0.0122(14) 0.0088(14) C38 0.0232(15) 0.0206(17) 0.0270(17) 0.0080(14) 0.0045(12) 0.0074(13) C39 0.045(2) 0.042(2) 0.042(2) 0.0221(19) 0.0097(17) 0.0182(18) C40 0.0254(17) 0.034(2) 0.052(2) 0.0156(18) -0.0025(16) 0.0098(15) C41 0.0358(19) 0.037(2) 0.0317(19) 0.0070(16) -0.0032(14) 0.0229(16) C42 0.0364(19) 0.042(2) 0.0335(19) 0.0088(17) 0.0095(15) 0.0254(17) C43 0.0322(18) 0.035(2) 0.038(2) -0.0012(17) 0.0017(15) 0.0127(16) C44 0.042(2) 0.045(3) 0.036(2) 0.0047(18) -0.0063(16) 0.0170(19) C45 0.077(3) 0.046(3) 0.057(3) 0.016(2) 0.034(3) 0.029(3) C46 0.050(3) 0.073(4) 0.036(2) 0.003(2) 0.0019(19) 0.016(2) C47 0.065(3) 0.089(4) 0.044(3) 0.029(3) 0.023(2) 0.052(3) N1 0.0152(11) 0.0144(13) 0.0196(12) 0.0026(10) 0.0064(9) 0.0056(9) O1 0.0268(11) 0.0122(11) 0.0201(12) 0.0001(9) -0.0018(9) 0.0082(9) P1 0.0134(3) 0.0107(4) 0.0141(4) 0.0021(3) 0.0016(3) 0.0042(3) P2 0.0126(3) 0.0114(4) 0.0156(4) 0.0032(3) 0.0022(3) 0.0042(3) Cl1 0.0181(3) 0.0219(4) 0.0241(4) 0.0077(3) 0.0017(3) 0.0110(3) Cl2 0.0166(3) 0.0162(4) 0.0177(3) 0.0013(3) -0.0022(2) 0.0056(3) Ru1 0.01242(11) 0.00961(12) 0.01318(12) 0.00143(9) 0.00123(8) 0.00420(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(4) . ? C1 C6 1.398(4) . ? C1 P1 1.836(3) . ? C2 C3 1.393(4) . ? C2 N1 1.475(4) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.376(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.492(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.496(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C14 1.398(4) . ? C9 C10 1.398(4) . ? C9 P1 1.843(3) . ? C10 C11 1.389(4) . ? C10 H10 0.9500 . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 C13 1.383(4) . ? C12 H12 0.9500 . ? C13 C14 1.382(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.392(4) . ? C15 C20 1.401(4) . ? C15 P1 1.839(2) . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C17 C18 1.376(5) . ? C17 H17 0.9500 . ? C18 C19 1.383(5) . ? C18 H18 0.9500 . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.395(4) . ? C21 C26 1.400(3) . ? C21 P2 1.846(3) . ? C22 C23 1.381(4) . ? C22 H22 0.9500 . ? C23 C24 1.383(4) . ? C23 H23 0.9500 . ? C24 C25 1.391(4) . ? C24 H24 0.9500 . ? C25 C26 1.378(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.384(4) . ? C27 C32 1.404(4) . ? C27 P2 1.849(2) . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.384(5) . ? C29 H29 0.9500 . ? C30 C31 1.378(5) . ? C30 H30 0.9500 . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C34 1.388(4) . ? C33 C38 1.397(4) . ? C33 P2 1.835(3) . ? C34 C35 1.393(4) . ? C34 H34 0.9500 . ? C35 C36 1.377(5) . ? C35 H35 0.9500 . ? C36 C37 1.385(5) . ? C36 H36 0.9500 . ? C37 C38 1.379(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.377(5) . ? C39 C44 1.384(5) . ? C39 H39 0.9500 . ? C40 C41 1.383(5) . ? C40 H40 0.9500 . ? C41 C42 1.378(5) . ? C41 H41 0.9500 . ? C42 C43 1.374(5) . ? C42 H42 0.9500 . ? C43 C44 1.375(5) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.362(6) . ? C45 C47 1.383(6) 2_656 ? C45 H45 0.9500 . ? C46 C47 1.355(7) . ? C46 H46 0.9500 . ? C47 C45 1.383(6) 2_656 ? C47 H47 0.9500 . ? N1 Ru1 2.311(2) . ? O1 Ru1 2.191(2) . ? O1 H1 0.863(10) . ? O1 H2 0.866(10) . ? P1 Ru1 2.2333(8) . ? P2 Ru1 2.3091(7) . ? Cl1 Ru1 2.4311(7) . ? Cl2 Ru1 2.3951(7) . ? 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 C2 C1 C6 119.5(3) . . ? C2 C1 P1 117.4(2) . . ? C6 C1 P1 123.1(2) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 N1 118.8(2) . . ? C3 C2 N1 121.2(3) . . ? C4 C3 C2 120.1(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.0(3) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 120.3(3) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C14 C9 C10 118.0(3) . . ? C14 C9 P1 120.8(2) . . ? C10 C9 P1 120.9(2) . . ? C11 C10 C9 120.7(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 119.6(3) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C9 120.9(3) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? C16 C15 C20 118.4(2) . . ? C16 C15 P1 121.7(2) . . ? C20 C15 P1 119.6(2) . . ? C15 C16 C17 120.5(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C15 120.7(3) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C22 C21 C26 117.6(3) . . ? C22 C21 P2 118.96(19) . . ? C26 C21 P2 123.3(2) . . ? C23 C22 C21 121.4(2) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C25 118.9(3) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 120.7(2) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 120.9(3) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C28 C27 C32 117.6(2) . . ? C28 C27 P2 120.0(2) . . ? C32 C27 P2 122.1(2) . . ? C27 C28 C29 121.3(3) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C29 119.1(3) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 120.6(3) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C27 120.9(3) . . ? C31 C32 H32 119.6 . . ? C27 C32 H32 119.6 . . ? C34 C33 C38 118.6(3) . . ? C34 C33 P2 122.8(2) . . ? C38 C33 P2 118.6(2) . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.5(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 120.0(3) . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C33 121.2(3) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C40 C39 C44 119.5(3) . . ? C40 C39 H39 120.3 . . ? C44 C39 H39 120.3 . . ? C39 C40 C41 120.3(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 119.8(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C41 120.0(3) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.1(3) . . ? C43 C44 H44 119.9 . . ? C39 C44 H44 119.9 . . ? C46 C45 C47 118.9(4) . 2_656 ? C46 C45 H45 120.5 . . ? C47 C45 H45 120.5 2_656 . ? C47 C46 C45 121.3(4) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C45 119.8(4) . 2_656 ? C46 C47 H47 120.1 . . ? C45 C47 H47 120.1 2_656 . ? C2 N1 C7 111.4(2) . . ? C2 N1 C8 107.1(2) . . ? C7 N1 C8 106.4(2) . . ? C2 N1 Ru1 109.98(15) . . ? C7 N1 Ru1 110.05(16) . . ? C8 N1 Ru1 111.75(17) . . ? Ru1 O1 H1 121(2) . . ? Ru1 O1 H2 115(3) . . ? H1 O1 H2 109(3) . . ? C1 P1 C15 103.42(12) . . ? C1 P1 C9 99.78(12) . . ? C15 P1 C9 101.70(12) . . ? C1 P1 Ru1 102.13(9) . . ? C15 P1 Ru1 118.65(9) . . ? C9 P1 Ru1 127.18(10) . . ? C33 P2 C21 103.74(12) . . ? C33 P2 C27 99.61(12) . . ? C21 P2 C27 100.03(12) . . ? C33 P2 Ru1 112.01(8) . . ? C21 P2 Ru1 116.77(9) . . ? C27 P2 Ru1 121.93(9) . . ? O1 Ru1 P1 169.78(6) . . ? O1 Ru1 P2 88.69(6) . . ? P1 Ru1 P2 99.71(3) . . ? O1 Ru1 N1 90.32(8) . . ? P1 Ru1 N1 81.33(6) . . ? P2 Ru1 N1 178.85(6) . . ? O1 Ru1 Cl2 85.26(6) . . ? P1 Ru1 Cl2 88.04(3) . . ? P2 Ru1 Cl2 96.26(2) . . ? N1 Ru1 Cl2 84.25(6) . . ? O1 Ru1 Cl1 80.76(6) . . ? P1 Ru1 Cl1 105.31(3) . . ? P2 Ru1 Cl1 86.98(2) . . ? N1 Ru1 Cl1 92.27(6) . . ? Cl2 Ru1 Cl1 165.58(2) . . ? 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 C6 C1 C2 C3 0.9(4) . . . . ? P1 C1 C2 C3 179.5(2) . . . . ? C6 C1 C2 N1 175.8(2) . . . . ? P1 C1 C2 N1 -5.7(3) . . . . ? C1 C2 C3 C4 -2.0(5) . . . . ? N1 C2 C3 C4 -176.6(3) . . . . ? C2 C3 C4 C5 1.4(5) . . . . ? C3 C4 C5 C6 0.1(5) . . . . ? C4 C5 C6 C1 -1.1(4) . . . . ? C2 C1 C6 C5 0.6(4) . . . . ? P1 C1 C6 C5 -177.9(2) . . . . ? C14 C9 C10 C11 -0.8(4) . . . . ? P1 C9 C10 C11 173.0(2) . . . . ? C9 C10 C11 C12 -0.1(4) . . . . ? C10 C11 C12 C13 0.8(4) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? C12 C13 C14 C9 -0.4(5) . . . . ? C10 C9 C14 C13 1.1(4) . . . . ? P1 C9 C14 C13 -172.8(2) . . . . ? C20 C15 C16 C17 -1.2(4) . . . . ? P1 C15 C16 C17 172.3(2) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C16 C17 C18 C19 2.0(5) . . . . ? C17 C18 C19 C20 -1.1(5) . . . . ? C18 C19 C20 C15 -1.0(5) . . . . ? C16 C15 C20 C19 2.1(4) . . . . ? P1 C15 C20 C19 -171.5(2) . . . . ? C26 C21 C22 C23 -2.1(4) . . . . ? P2 C21 C22 C23 173.2(2) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C22 C23 C24 C25 1.5(5) . . . . ? C23 C24 C25 C26 -1.9(5) . . . . ? C24 C25 C26 C21 0.4(5) . . . . ? C22 C21 C26 C25 1.7(4) . . . . ? P2 C21 C26 C25 -173.5(2) . . . . ? C32 C27 C28 C29 -0.4(4) . . . . ? P2 C27 C28 C29 -174.7(2) . . . . ? C27 C28 C29 C30 -0.8(4) . . . . ? C28 C29 C30 C31 1.8(5) . . . . ? C29 C30 C31 C32 -1.5(5) . . . . ? C30 C31 C32 C27 0.3(5) . . . . ? C28 C27 C32 C31 0.6(4) . . . . ? P2 C27 C32 C31 174.8(2) . . . . ? C38 C33 C34 C35 -0.9(4) . . . . ? P2 C33 C34 C35 178.1(2) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? C34 C35 C36 C37 0.2(5) . . . . ? C35 C36 C37 C38 -0.8(4) . . . . ? C36 C37 C38 C33 0.5(4) . . . . ? C34 C33 C38 C37 0.4(4) . . . . ? P2 C33 C38 C37 -178.7(2) . . . . ? C44 C39 C40 C41 0.9(5) . . . . ? C39 C40 C41 C42 -0.5(5) . . . . ? C40 C41 C42 C43 0.8(5) . . . . ? C41 C42 C43 C44 -1.4(5) . . . . ? C42 C43 C44 C39 1.8(6) . . . . ? C40 C39 C44 C43 -1.5(6) . . . . ? C47 C45 C46 C47 0.4(7) 2_656 . . . ? C45 C46 C47 C45 -0.4(7) . . . 2_656 ? C1 C2 N1 C7 149.3(2) . . . . ? C3 C2 N1 C7 -36.0(3) . . . . ? C1 C2 N1 C8 -94.7(3) . . . . ? C3 C2 N1 C8 80.1(3) . . . . ? C1 C2 N1 Ru1 27.0(3) . . . . ? C3 C2 N1 Ru1 -158.3(2) . . . . ? C2 C1 P1 C15 -142.2(2) . . . . ? C6 C1 P1 C15 36.3(3) . . . . ? C2 C1 P1 C9 113.1(2) . . . . ? C6 C1 P1 C9 -68.3(2) . . . . ? C2 C1 P1 Ru1 -18.5(2) . . . . ? C6 C1 P1 Ru1 160.0(2) . . . . ? C16 C15 P1 C1 33.8(3) . . . . ? C20 C15 P1 C1 -152.8(2) . . . . ? C16 C15 P1 C9 137.0(2) . . . . ? C20 C15 P1 C9 -49.6(2) . . . . ? C16 C15 P1 Ru1 -78.3(2) . . . . ? C20 C15 P1 Ru1 95.1(2) . . . . ? C14 C9 P1 C1 71.1(2) . . . . ? C10 C9 P1 C1 -102.6(2) . . . . ? C14 C9 P1 C15 -34.9(3) . . . . ? C10 C9 P1 C15 151.4(2) . . . . ? C14 C9 P1 Ru1 -175.44(18) . . . . ? C10 C9 P1 Ru1 10.9(3) . . . . ? C34 C33 P2 C21 -18.3(2) . . . . ? C38 C33 P2 C21 160.7(2) . . . . ? C34 C33 P2 C27 -121.2(2) . . . . ? C38 C33 P2 C27 57.8(2) . . . . ? C34 C33 P2 Ru1 108.5(2) . . . . ? C38 C33 P2 Ru1 -72.5(2) . . . . ? C22 C21 P2 C33 95.6(2) . . . . ? C26 C21 P2 C33 -89.3(3) . . . . ? C22 C21 P2 C27 -161.8(2) . . . . ? C26 C21 P2 C27 13.3(3) . . . . ? C22 C21 P2 Ru1 -28.1(2) . . . . ? C26 C21 P2 Ru1 147.0(2) . . . . ? C28 C27 P2 C33 -166.2(2) . . . . ? C32 C27 P2 C33 19.8(3) . . . . ? C28 C27 P2 C21 87.9(2) . . . . ? C32 C27 P2 C21 -86.1(3) . . . . ? C28 C27 P2 Ru1 -42.6(3) . . . . ? C32 C27 P2 Ru1 143.4(2) . . . . ? _refine_diff_density_max 0.730 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.099 _shelxl_version_number 2012-9 _shelx_res_file ; TITL bj255/EM03043b CELL 0.71070 11.9020 12.7647 15.5900 106.371 94.400 113.790 ZERR 2.00 0.0008 0.0013 0.0020 0.005 0.003 0.001 LATT 1 SFAC C H N O P CL RU UNIT 94 92 2 2 4 4 2 MERG 2 DFIX -1.400 0.020 H1 H2 DFIX 0.87 0.01 O1 H1 O1 H2 FMAP 2 PLAN 20 ACTA 50.00 BOND $H CONF L.S. 99 TEMP -93.00 WGHT 0.056300 FVAR 0.94099 C1 1 0.297505 0.415011 0.074831 11.00000 0.01287 0.02003 = 0.01785 0.00490 0.00154 0.00337 C2 1 0.304994 0.314264 0.017532 11.00000 0.01410 0.01987 = 0.01922 0.00456 0.00207 0.00195 C3 1 0.321887 0.308224 -0.070839 11.00000 0.04035 0.03167 = 0.01954 0.00637 0.01188 0.01338 AFIX 43 H3 2 0.329667 0.240356 -0.109605 11.00000 -1.20000 AFIX 0 C4 1 0.327365 0.401191 -0.102321 11.00000 0.04071 0.04391 = 0.02387 0.01558 0.01255 0.01226 AFIX 43 H4 2 0.336963 0.395922 -0.163107 11.00000 -1.20000 AFIX 0 C5 1 0.318949 0.501018 -0.045820 11.00000 0.02766 0.03473 = 0.02832 0.02272 0.00491 0.00752 AFIX 43 H5 2 0.322607 0.564452 -0.067648 11.00000 -1.20000 AFIX 0 C6 1 0.305169 0.508996 0.042710 11.00000 0.01970 0.02097 = 0.02885 0.01070 0.00305 0.00329 AFIX 43 H6 2 0.300884 0.578682 0.081929 11.00000 -1.20000 AFIX 0 C7 1 0.246458 0.096873 -0.017801 11.00000 0.03201 0.02126 = 0.02540 0.00029 0.01327 0.00985 AFIX 137 H7A 2 0.158494 0.075206 -0.041777 11.00000 -1.50000 H7B 2 0.250075 0.036752 0.008508 11.00000 -1.50000 H7C 2 0.291887 0.097716 -0.067630 11.00000 -1.50000 AFIX 0 C8 1 0.440331 0.248948 0.084924 11.00000 0.02118 0.03467 = 0.03061 0.00954 0.01034 0.01482 AFIX 137 H8A 2 0.480909 0.247743 0.032519 11.00000 -1.50000 H8B 2 0.444578 0.188032 0.110018 11.00000 -1.50000 H8C 2 0.483723 0.329984 0.132172 11.00000 -1.50000 AFIX 0 C9 1 0.425980 0.542137 0.259084 11.00000 0.01656 0.01457 = 0.01340 -0.00002 0.00296 0.00257 C10 1 0.520296 0.518911 0.296567 11.00000 0.02006 0.02375 = 0.01724 0.00963 0.00368 0.00615 AFIX 43 H10 2 0.502817 0.437887 0.292249 11.00000 -1.20000 AFIX 0 C11 1 0.639315 0.613069 0.340062 11.00000 0.01814 0.03311 = 0.01896 0.00809 -0.00006 0.00429 AFIX 43 H11 2 0.702519 0.596044 0.365292 11.00000 -1.20000 AFIX 0 C12 1 0.666138 0.731258 0.346780 11.00000 0.02215 0.02797 = 0.01610 0.00141 -0.00120 -0.00362 AFIX 43 H12 2 0.747865 0.795369 0.375884 11.00000 -1.20000 AFIX 0 C13 1 0.573388 0.755822 0.310910 11.00000 0.03093 0.01619 = 0.03857 0.00684 0.00551 0.00124 AFIX 43 H13 2 0.591398 0.837172 0.315916 11.00000 -1.20000 AFIX 0 C14 1 0.454633 0.662680 0.267817 11.00000 0.02206 0.01498 = 0.03169 0.00369 0.00093 0.00328 AFIX 43 H14 2 0.391623 0.680847 0.243805 11.00000 -1.20000 AFIX 0 C15 1 0.167200 0.487516 0.210927 11.00000 0.01523 0.01046 = 0.02390 0.00699 0.00322 0.00425 C16 1 0.075353 0.470442 0.140467 11.00000 0.02174 0.01737 = 0.02850 0.01024 0.00141 0.00665 AFIX 43 H16 2 0.073458 0.429214 0.078844 11.00000 -1.20000 AFIX 0 C17 1 -0.013881 0.513388 0.159648 11.00000 0.02155 0.02438 = 0.05637 0.01972 0.00310 0.01107 AFIX 43 H17 2 -0.075527 0.502204 0.111024 11.00000 -1.20000 AFIX 0 C18 1 -0.013015 0.571906 0.248727 11.00000 0.03163 0.02676 = 0.05907 0.01745 0.01831 0.02075 AFIX 43 H18 2 -0.075559 0.598781 0.261653 11.00000 -1.20000 AFIX 0 C19 1 0.078908 0.591584 0.319421 11.00000 0.03866 0.01689 = 0.04054 0.00607 0.01566 0.01514 AFIX 43 H19 2 0.080275 0.633205 0.380811 11.00000 -1.20000 AFIX 0 C20 1 0.169049 0.550719 0.300907 11.00000 0.02555 0.01280 = 0.03174 0.00640 0.00718 0.00963 AFIX 43 H20 2 0.232725 0.565718 0.349723 11.00000 -1.20000 AFIX 0 C21 1 0.173137 0.349920 0.399241 11.00000 0.02154 0.01255 = 0.01702 0.00614 0.00307 0.00691 C22 1 0.303454 0.419224 0.420220 11.00000 0.01932 0.01684 = 0.01960 0.00656 0.00440 0.00813 AFIX 43 H22 2 0.352712 0.391199 0.383634 11.00000 -1.20000 AFIX 0 C23 1 0.362280 0.527714 0.493077 11.00000 0.02139 0.01768 = 0.02279 0.00091 -0.00010 0.00539 AFIX 43 H23 2 0.451074 0.573615 0.505657 11.00000 -1.20000 AFIX 0 C24 1 0.292827 0.569985 0.547838 11.00000 0.03538 0.01992 = 0.02030 -0.00382 -0.00074 0.01421 AFIX 43 H24 2 0.332957 0.645547 0.597084 11.00000 -1.20000 AFIX 0 C25 1 0.163225 0.500085 0.529664 11.00000 0.03323 0.02924 = 0.02393 0.00486 0.00982 0.01933 AFIX 43 H25 2 0.114888 0.526990 0.567995 11.00000 -1.20000 AFIX 0 C26 1 0.104261 0.392196 0.456607 11.00000 0.02238 0.02069 = 0.02479 0.00437 0.00556 0.00951 AFIX 43 H26 2 0.015625 0.345858 0.445011 11.00000 -1.20000 AFIX 0 C27 1 -0.065374 0.192866 0.280440 11.00000 0.01205 0.01427 = 0.02006 0.00150 0.00107 0.00301 C28 1 -0.105065 0.253006 0.233096 11.00000 0.01725 0.02108 = 0.01947 0.00254 0.00199 0.00608 AFIX 43 H28 2 -0.049170 0.299949 0.203189 11.00000 -1.20000 AFIX 0 C29 1 -0.225099 0.246084 0.228438 11.00000 0.02420 0.03210 = 0.02785 -0.00210 -0.00310 0.01704 AFIX 43 H29 2 -0.249772 0.289074 0.196215 11.00000 -1.20000 AFIX 0 C30 1 -0.308910 0.177049 0.270380 11.00000 0.01412 0.02519 = 0.03654 -0.00744 0.00230 0.00626 AFIX 43 H30 2 -0.391713 0.170483 0.265711 11.00000 -1.20000 AFIX 0 C31 1 -0.270581 0.117974 0.319004 11.00000 0.01961 0.02488 = 0.04620 0.00711 0.01616 0.00520 AFIX 43 H31 2 -0.326759 0.071985 0.349284 11.00000 -1.20000 AFIX 0 C32 1 -0.150477 0.125029 0.324175 11.00000 0.02146 0.02191 = 0.03772 0.01100 0.01187 0.00795 AFIX 43 H32 2 -0.125654 0.083421 0.357728 11.00000 -1.20000 AFIX 0 C33 1 0.083911 0.088103 0.332744 11.00000 0.01787 0.01410 = 0.02032 0.00441 0.00571 0.00642 C34 1 0.152221 0.104644 0.415792 11.00000 0.02779 0.01854 = 0.02932 0.00603 0.00406 0.01050 AFIX 43 H34 2 0.211698 0.184158 0.454196 11.00000 -1.20000 AFIX 0 C35 1 0.133727 0.004913 0.442908 11.00000 0.04752 0.03304 = 0.03270 0.01689 0.00885 0.02352 AFIX 43 H35 2 0.180110 0.016869 0.500087 11.00000 -1.20000 AFIX 0 C36 1 0.048677 -0.110909 0.387416 11.00000 0.05445 0.02084 = 0.03780 0.01643 0.01753 0.02051 AFIX 43 H36 2 0.036311 -0.178478 0.406469 11.00000 -1.20000 AFIX 0 C37 1 -0.018845 -0.128913 0.303828 11.00000 0.03877 0.01499 = 0.03555 0.00634 0.01217 0.00884 AFIX 43 H37 2 -0.076784 -0.208828 0.265045 11.00000 -1.20000 AFIX 0 C38 1 -0.001458 -0.030107 0.277228 11.00000 0.02316 0.02064 = 0.02702 0.00802 0.00451 0.00737 AFIX 43 H38 2 -0.048435 -0.042710 0.220078 11.00000 -1.20000 AFIX 0 C39 1 0.254550 -0.182519 0.178649 11.00000 0.04474 0.04241 = 0.04237 0.02206 0.00967 0.01823 AFIX 43 H39 2 0.219469 -0.198740 0.228888 11.00000 -1.20000 AFIX 0 C40 1 0.178629 -0.229490 0.092693 11.00000 0.02544 0.03418 = 0.05162 0.01559 -0.00246 0.00976 AFIX 43 H40 2 0.090666 -0.277380 0.083766 11.00000 -1.20000 AFIX 0 C41 1 0.229889 -0.207244 0.019313 11.00000 0.03581 0.03694 = 0.03165 0.00701 -0.00322 0.02285 AFIX 43 H41 2 0.177379 -0.240294 -0.040007 11.00000 -1.20000 AFIX 0 C42 1 0.357317 -0.137020 0.032477 11.00000 0.03645 0.04224 = 0.03349 0.00883 0.00949 0.02543 AFIX 43 H42 2 0.392643 -0.120771 -0.017671 11.00000 -1.20000 AFIX 0 C43 1 0.433340 -0.090470 0.118109 11.00000 0.03222 0.03453 = 0.03801 -0.00124 0.00172 0.01268 AFIX 43 H43 2 0.521449 -0.043589 0.126768 11.00000 -1.20000 AFIX 0 C44 1 0.382358 -0.111495 0.191294 11.00000 0.04213 0.04458 = 0.03607 0.00465 -0.00626 0.01696 AFIX 43 H44 2 0.434973 -0.077195 0.250687 11.00000 -1.20000 AFIX 0 C45 1 0.556075 0.120900 0.508064 11.00000 0.07666 0.04550 = 0.05722 0.01636 0.03370 0.02879 AFIX 43 H45 2 0.594947 0.204399 0.513499 11.00000 -1.20000 AFIX 0 C46 1 0.611018 0.077902 0.560389 11.00000 0.04994 0.07253 = 0.03640 0.00341 0.00190 0.01555 AFIX 43 H46 2 0.688583 0.132379 0.602822 11.00000 -1.20000 AFIX 0 C47 1 0.557231 -0.041057 0.553121 11.00000 0.06528 0.08874 = 0.04410 0.02914 0.02342 0.05214 AFIX 43 H47 2 0.597202 -0.069517 0.589922 11.00000 -1.20000 AFIX 0 N1 3 0.305700 0.220083 0.054495 11.00000 0.01524 0.01442 = 0.01964 0.00264 0.00638 0.00560 O1 4 0.127916 0.020753 0.132100 11.00000 0.02680 0.01223 = 0.02011 0.00005 -0.00180 0.00823 P1 5 0.273930 0.416102 0.190042 11.00000 0.01337 0.01073 = 0.01407 0.00211 0.00158 0.00419 P2 5 0.099234 0.215046 0.293574 11.00000 0.01262 0.01143 = 0.01558 0.00319 0.00220 0.00423 CL1 6 0.365913 0.207516 0.268508 11.00000 0.01806 0.02188 = 0.02412 0.00769 0.00167 0.01100 CL2 6 0.026771 0.177873 0.061577 11.00000 0.01659 0.01618 = 0.01769 0.00129 -0.00222 0.00558 RU1 7 0.202166 0.219246 0.174009 11.00000 0.01242 0.00961 = 0.01318 0.00143 0.00123 0.00420 H1 2 0.090069 -0.024854 0.076164 11.00000 0.03421 H2 2 0.178769 -0.004849 0.151401 11.00000 0.05725 HKLF 4 REM bj255/EM03043b REM R1 = 0.0371 for 6959 Fo > 4sig(Fo) and 0.0622 for all 9156 data REM 497 parameters refined using 2 restraints END WGHT 0.0565 0.0000 REM Highest difference peak 0.730, deepest hole -0.864, 1-sigma level 0.099 Q1 1 0.2524 0.3013 0.1705 11.00000 0.05 0.73 Q2 1 0.1552 0.1530 0.1795 11.00000 0.05 0.59 Q3 1 0.2214 0.3383 0.1816 11.00000 0.05 0.48 Q4 1 0.3587 0.4142 0.0689 11.00000 0.05 0.46 Q5 1 0.1700 0.1108 0.1109 11.00000 0.05 0.43 Q6 1 0.2238 0.3144 0.2370 11.00000 0.05 0.43 Q7 1 0.3070 0.2292 0.2340 11.00000 0.05 0.41 Q8 1 0.2703 0.2180 0.0895 11.00000 0.05 0.41 Q9 1 0.0639 0.1332 0.3009 11.00000 0.05 0.40 Q10 1 0.0623 0.0372 0.2908 11.00000 0.05 0.40 Q11 1 0.1578 0.5173 0.2571 11.00000 0.05 0.40 Q12 1 0.6031 0.6577 0.5198 11.00000 0.05 0.39 Q13 1 0.2982 0.1183 0.2684 11.00000 0.05 0.39 Q14 1 0.3192 0.1500 0.4586 11.00000 0.05 0.39 Q15 1 0.4830 0.6176 0.4911 11.00000 0.05 0.38 Q16 1 -0.0001 0.1889 -0.0057 11.00000 0.05 0.38 Q17 1 0.5704 -0.2204 0.5945 11.00000 0.05 0.38 Q18 1 0.4155 0.2098 0.2464 11.00000 0.05 0.38 Q19 1 0.4292 0.6113 0.4020 11.00000 0.05 0.37 Q20 1 0.2136 0.4577 0.1939 11.00000 0.05 0.37 ; _shelx_res_checksum 13115 _shelx_hkl_checksum 69824