# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Reto Dorta' _publ_contact_author_email DORTA@OCI.UZH.CH _publ_section_title ; Improving Grubbs II Type Ruthenium Catalysts by Appropriately Modifying the N-Heterocyclic Carbene Ligand. ; loop_ _publ_author_name 'Reto Dorta' 'Sascha Blumentritt' 'Fabien Boeda' 'Herve Clavier' 'Michele Gatti' 'Anthony Linden' ; X.Luan ; 'Steven Nolan' 'Ludovic Vieille-Petit' # Attachment 'dorta_revised3.cif' data_2a _database_code_depnum_ccdc_archive 'CCDC 707353' # DT0824 _audit_creation_method SHELXL-97 _audit_creation_date 08-08-12 # CLIENT : R. Dorta # JOURNAL COMPOUND IDENTIFIER : 2a # ABSOLUTE CONFIGURATION : # POLYMORPH : # NEUTRON STUDY : # BIOLOGICAL ACTIVITY : # COMMENTS : solvent: dichloromethane / MeOH. # The asymmetric unit contains one molecule of the Ru-complex plus one # half of a molecule of MeOH. The MeOH molecule is disordered about a # centre of inversion. The H-atoms of the MeOH molecule were not # included in the model. # deposition numbers 707353-707357 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C54 H69 Cl2 N2 P Ru, 0.5(C H4 O)' _chemical_formula_sum 'C54.50 H71 Cl2 N2 O0.50 P Ru' _chemical_formula_weight 965.05 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 109 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 142 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cl Cl 4 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 1 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 2 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 2 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9635(1) _cell_length_b 12.3613(2) _cell_length_c 17.5395(2) _cell_angle_alpha 78.1999(7) _cell_angle_beta 77.4826(8) _cell_angle_gamma 76.6149(8) _cell_volume 2430.64(5) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 61255 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 0.505 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.943 _exptl_special_details ; Solvent used: dichloromethane / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.515(1) Frames collected: 541 Seconds exposure per frame: 45 Degrees rotation per frame: 1.5 Crystal-Detector distance (mm): 33.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 66892 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 30.05 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 14117 _reflns_number_gt 12127 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The asymmetric unit contains one molecule of the Ru-complex plus one half of a molecule of MeOH. The MeOH molecule is disordered about a centre of inversion. The O and C atoms of the solvent molecule have elongated displacement ellipsoids, there are no potential acceptor atoms close to either atom and test refinements were unconvincing as to the correct assignment of the O and C atoms. For these resaons, the H-atoms of the MeOH molecule were not included in the model. ; _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^)+(0.0438P)^2^+2.7461P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14114 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.209 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.080 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.767741(13) 0.229732(13) 0.745507(9) 0.01914(5) Uani 1 1 d . . . Cl1 Cl 0.93428(4) 0.22255(4) 0.64247(3) 0.02753(11) Uani 1 1 d . . . Cl2 Cl 0.62455(5) 0.24951(5) 0.86391(3) 0.02937(11) Uani 1 1 d . . . P1 P 0.71043(4) 0.42939(4) 0.69998(3) 0.02042(10) Uani 1 1 d . . . N1 N 0.90826(15) 0.06207(14) 0.85969(11) 0.0247(3) Uani 1 1 d . . . N2 N 0.79190(16) -0.02063(14) 0.82324(10) 0.0242(3) Uani 1 1 d . . . C1 C 0.83238(17) 0.07618(16) 0.80991(12) 0.0206(4) Uani 1 1 d . . . C2 C 0.8510(2) -0.10954(19) 0.87954(15) 0.0325(5) Uani 1 1 d . . . H21 H 0.9110 -0.1649 0.8517 0.039 Uiso 1 1 calc R . . H22 H 0.7946 -0.1494 0.9183 0.039 Uiso 1 1 calc R . . C3 C 0.9058(2) -0.04193(19) 0.91900(14) 0.0317(5) Uani 1 1 d . . . H31 H 0.8573 -0.0258 0.9703 0.038 Uiso 1 1 calc R . . H32 H 0.9854 -0.0811 0.9273 0.038 Uiso 1 1 calc R . . C4 C 0.98221(18) 0.13718(18) 0.86282(13) 0.0258(4) Uani 1 1 d . . . C5 C 0.9468(2) 0.20595(19) 0.92307(14) 0.0297(4) Uani 1 1 d . . . C6 C 0.8366(2) 0.2133(2) 0.97383(14) 0.0348(5) Uani 1 1 d . . . H6 H 0.7828 0.1709 0.9683 0.042 Uiso 1 1 calc R . . C7 C 0.8069(3) 0.2813(3) 1.03075(16) 0.0448(6) Uani 1 1 d . . . H7 H 0.7324 0.2859 1.0640 0.054 Uiso 1 1 calc R . . C8 C 0.8858(3) 0.3443(3) 1.04048(17) 0.0516(7) Uani 1 1 d . . . H8 H 0.8643 0.3909 1.0802 0.062 Uiso 1 1 calc R . . C9 C 0.9922(3) 0.3385(2) 0.99330(17) 0.0464(7) Uani 1 1 d . . . H9 H 1.0448 0.3809 1.0007 0.056 Uiso 1 1 calc R . . C10 C 1.0266(2) 0.2704(2) 0.93295(15) 0.0366(5) Uani 1 1 d . . . C11 C 1.1348(2) 0.2646(2) 0.88183(18) 0.0432(6) Uani 1 1 d . . . H11 H 1.1885 0.3068 0.8880 0.052 Uiso 1 1 calc R . . C12 C 1.1647(2) 0.2000(2) 0.82359(17) 0.0402(6) Uani 1 1 d . . . H12 H 1.2378 0.2001 0.7891 0.048 Uiso 1 1 calc R . . C13 C 1.08964(19) 0.13207(19) 0.81267(14) 0.0307(5) Uani 1 1 d . . . C14 C 1.1287(2) 0.0563(2) 0.74988(15) 0.0336(5) Uani 1 1 d . . . H14 H 1.0580 0.0553 0.7285 0.040 Uiso 1 1 calc R . . C15 C 1.2184(3) 0.0974(3) 0.67985(19) 0.0510(7) Uani 1 1 d . . . H151 H 1.1907 0.1771 0.6602 0.076 Uiso 1 1 calc R . . H152 H 1.2286 0.0532 0.6375 0.076 Uiso 1 1 calc R . . H153 H 1.2932 0.0881 0.6970 0.076 Uiso 1 1 calc R . . C16 C 1.1770(3) -0.0655(2) 0.7851(2) 0.0513(7) Uani 1 1 d . . . H161 H 1.2442 -0.0672 0.8091 0.077 Uiso 1 1 calc R . . H162 H 1.2013 -0.1120 0.7431 0.077 Uiso 1 1 calc R . . H163 H 1.1162 -0.0951 0.8256 0.077 Uiso 1 1 calc R . . C17 C 0.72706(19) -0.05211(17) 0.77416(12) 0.0245(4) Uani 1 1 d . . . C18 C 0.7861(2) -0.07830(18) 0.69840(13) 0.0297(5) Uani 1 1 d . . . C19 C 0.9041(2) -0.0708(2) 0.66796(16) 0.0393(6) Uani 1 1 d . . . H19 H 0.9486 -0.0495 0.6992 0.047 Uiso 1 1 calc R . . C20 C 0.9547(3) -0.0943(3) 0.59337(19) 0.0538(8) Uani 1 1 d . . . H20 H 1.0338 -0.0878 0.5735 0.065 Uiso 1 1 calc R . . C21 C 0.8926(3) -0.1274(3) 0.54606(19) 0.0581(9) Uani 1 1 d . . . H211 H 0.9298 -0.1445 0.4951 0.070 Uiso 1 1 calc R . . C22 C 0.7791(3) -0.1352(2) 0.57313(17) 0.0489(7) Uani 1 1 d . . . H221 H 0.7367 -0.1563 0.5404 0.059 Uiso 1 1 calc R . . C23 C 0.7227(2) -0.1121(2) 0.65009(15) 0.0360(5) Uani 1 1 d . . . C24 C 0.6058(3) -0.1207(2) 0.67916(16) 0.0408(6) Uani 1 1 d . . . H24 H 0.5626 -0.1420 0.6471 0.049 Uiso 1 1 calc R . . C25 C 0.5533(2) -0.0988(2) 0.75330(16) 0.0378(5) Uani 1 1 d . . . H25 H 0.4746 -0.1071 0.7722 0.045 Uiso 1 1 calc R . . C26 C 0.6133(2) -0.06394(19) 0.80296(13) 0.0291(4) Uani 1 1 d . . . C27 C 0.5501(2) -0.0451(2) 0.88533(14) 0.0365(5) Uani 1 1 d . . . H27 H 0.6010 -0.0141 0.9102 0.044 Uiso 1 1 calc R . . C28 C 0.4334(2) 0.0366(3) 0.8858(2) 0.0531(8) Uani 1 1 d . . . H281 H 0.4456 0.1090 0.8536 0.080 Uiso 1 1 calc R . . H282 H 0.3984 0.0477 0.9403 0.080 Uiso 1 1 calc R . . H283 H 0.3811 0.0057 0.8639 0.080 Uiso 1 1 calc R . . C29 C 0.5299(3) -0.1591(3) 0.93555(18) 0.0578(8) Uani 1 1 d . . . H291 H 0.4792 -0.1902 0.9124 0.087 Uiso 1 1 calc R . . H292 H 0.4927 -0.1479 0.9897 0.087 Uiso 1 1 calc R . . H293 H 0.6050 -0.2116 0.9365 0.087 Uiso 1 1 calc R . . C30 C 0.65886(19) 0.18784(18) 0.70301(14) 0.0277(4) Uani 1 1 d . . . H30 H 0.5934 0.1728 0.7422 0.033 Uiso 1 1 calc R . . C31 C 0.6461(2) 0.17148(19) 0.62480(15) 0.0318(5) Uani 1 1 d . . . C32 C 0.5353(2) 0.1597(2) 0.61759(17) 0.0414(6) Uani 1 1 d . . . H321 H 0.4747 0.1615 0.6626 0.050 Uiso 1 1 calc R . . C33 C 0.5115(3) 0.1456(3) 0.5468(2) 0.0550(8) Uani 1 1 d . . . H33 H 0.4361 0.1361 0.5436 0.066 Uiso 1 1 calc R . . C34 C 0.5999(3) 0.1454(3) 0.4803(2) 0.0601(9) Uani 1 1 d . . . H34 H 0.5848 0.1367 0.4311 0.072 Uiso 1 1 calc R . . C35 C 0.7083(3) 0.1579(3) 0.48588(18) 0.0528(7) Uani 1 1 d . . . H35 H 0.7677 0.1582 0.4401 0.063 Uiso 1 1 calc R . . C36 C 0.7335(2) 0.1701(2) 0.55711(16) 0.0404(6) Uani 1 1 d . . . H36 H 0.8098 0.1775 0.5599 0.049 Uiso 1 1 calc R . . C37 C 0.79250(18) 0.51162(17) 0.73775(12) 0.0235(4) Uani 1 1 d . . . H37 H 0.7735 0.5911 0.7103 0.028 Uiso 1 1 calc R . . C38 C 0.9253(2) 0.4732(2) 0.71572(16) 0.0342(5) Uani 1 1 d . . . H381 H 0.9505 0.3985 0.7471 0.041 Uiso 1 1 calc R . . H382 H 0.9469 0.4661 0.6589 0.041 Uiso 1 1 calc R . . C39 C 0.9865(2) 0.5597(2) 0.73264(17) 0.0414(6) Uani 1 1 d . . . H391 H 1.0721 0.5345 0.7190 0.050 Uiso 1 1 calc R . . H392 H 0.9643 0.6331 0.6990 0.050 Uiso 1 1 calc R . . C40 C 0.9534(2) 0.5740(2) 0.81900(17) 0.0394(6) Uani 1 1 d . . . H401 H 0.9876 0.6356 0.8270 0.047 Uiso 1 1 calc R . . H402 H 0.9865 0.5038 0.8520 0.047 Uiso 1 1 calc R . . C41 C 0.8216(2) 0.6009(2) 0.84578(16) 0.0384(5) Uani 1 1 d . . . H411 H 0.7903 0.6774 0.8195 0.046 Uiso 1 1 calc R . . H412 H 0.8040 0.6009 0.9036 0.046 Uiso 1 1 calc R . . C42 C 0.7605(2) 0.5158(2) 0.82660(14) 0.0337(5) Uani 1 1 d . . . H421 H 0.7854 0.4403 0.8568 0.040 Uiso 1 1 calc R . . H422 H 0.6749 0.5388 0.8420 0.040 Uiso 1 1 calc R . . C43 C 0.74729(19) 0.47186(18) 0.59090(12) 0.0256(4) Uani 1 1 d . . . H43 H 0.8195 0.4170 0.5734 0.031 Uiso 1 1 calc R . . C44 C 0.7777(2) 0.5892(2) 0.55929(14) 0.0366(5) Uani 1 1 d . . . H441 H 0.7069 0.6481 0.5692 0.044 Uiso 1 1 calc R . . H442 H 0.8366 0.6002 0.5874 0.044 Uiso 1 1 calc R . . C45 C 0.8260(3) 0.5999(3) 0.47022(15) 0.0462(7) Uani 1 1 d . . . H451 H 0.8431 0.6763 0.4502 0.055 Uiso 1 1 calc R . . H452 H 0.9002 0.5448 0.4611 0.055 Uiso 1 1 calc R . . C46 C 0.7412(3) 0.5796(3) 0.42476(15) 0.0466(7) Uani 1 1 d . . . H461 H 0.7780 0.5811 0.3684 0.056 Uiso 1 1 calc R . . H462 H 0.6711 0.6407 0.4279 0.056 Uiso 1 1 calc R . . C47 C 0.7051(3) 0.4670(3) 0.45768(15) 0.0442(6) Uani 1 1 d . . . H471 H 0.7736 0.4054 0.4486 0.053 Uiso 1 1 calc R . . H472 H 0.6453 0.4583 0.4294 0.053 Uiso 1 1 calc R . . C48 C 0.6555(2) 0.4576(2) 0.54678(14) 0.0338(5) Uani 1 1 d . . . H481 H 0.5845 0.5166 0.5559 0.041 Uiso 1 1 calc R . . H482 H 0.6335 0.3832 0.5670 0.041 Uiso 1 1 calc R . . C49 C 0.55653(18) 0.49198(18) 0.73705(13) 0.0247(4) Uani 1 1 d . . . H49 H 0.5498 0.4812 0.7958 0.030 Uiso 1 1 calc R . . C50 C 0.5231(2) 0.6194(2) 0.71132(15) 0.0334(5) Uani 1 1 d . . . H501 H 0.5818 0.6565 0.7220 0.040 Uiso 1 1 calc R . . H502 H 0.5231 0.6361 0.6537 0.040 Uiso 1 1 calc R . . C51 C 0.4024(2) 0.6668(2) 0.75554(18) 0.0411(6) Uani 1 1 d . . . H511 H 0.4048 0.6568 0.8127 0.049 Uiso 1 1 calc R . . H512 H 0.3815 0.7486 0.7360 0.049 Uiso 1 1 calc R . . C52 C 0.3096(2) 0.6090(2) 0.74444(17) 0.0429(6) Uani 1 1 d . . . H521 H 0.2997 0.6273 0.6883 0.051 Uiso 1 1 calc R . . H522 H 0.2341 0.6375 0.7772 0.051 Uiso 1 1 calc R . . C53 C 0.3428(2) 0.4817(2) 0.76781(17) 0.0411(6) Uani 1 1 d . . . H531 H 0.2838 0.4460 0.7561 0.049 Uiso 1 1 calc R . . H532 H 0.3422 0.4632 0.8255 0.049 Uiso 1 1 calc R . . C54 C 0.46435(19) 0.4329(2) 0.72359(15) 0.0317(5) Uani 1 1 d . . . H541 H 0.4848 0.3510 0.7430 0.038 Uiso 1 1 calc R . . H542 H 0.4631 0.4436 0.6663 0.038 Uiso 1 1 calc R . . O1 O 0.5862(6) 0.5384(4) 1.0291(3) 0.0758(18) Uani 0.50 1 d P . . C55 C 0.502(2) 0.5356(11) 1.0008(10) 0.104(5) Uani 0.50 1 d P . . 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 0.01992(8) 0.01707(8) 0.01900(8) 0.00010(5) -0.00309(5) -0.00378(5) Cl1 0.0246(2) 0.0270(2) 0.0278(2) -0.00316(19) -0.00150(18) -0.00268(19) Cl2 0.0298(2) 0.0304(3) 0.0230(2) 0.00054(19) 0.00034(19) -0.0050(2) P1 0.0213(2) 0.0193(2) 0.0196(2) -0.00150(18) -0.00337(18) -0.00360(18) N1 0.0262(8) 0.0191(8) 0.0285(9) 0.0031(7) -0.0096(7) -0.0054(7) N2 0.0283(9) 0.0187(8) 0.0259(8) 0.0013(6) -0.0071(7) -0.0072(7) C1 0.0194(8) 0.0184(9) 0.0222(9) -0.0014(7) -0.0028(7) -0.0029(7) C2 0.0377(12) 0.0211(10) 0.0388(12) 0.0061(9) -0.0144(10) -0.0082(9) C3 0.0371(12) 0.0244(10) 0.0334(11) 0.0081(9) -0.0153(9) -0.0083(9) C4 0.0262(10) 0.0222(10) 0.0303(10) 0.0030(8) -0.0130(8) -0.0062(8) C5 0.0359(11) 0.0240(10) 0.0304(11) 0.0026(8) -0.0155(9) -0.0057(9) C6 0.0406(13) 0.0341(12) 0.0295(11) -0.0023(9) -0.0130(10) -0.0036(10) C7 0.0532(16) 0.0482(16) 0.0323(13) -0.0092(11) -0.0112(12) -0.0029(13) C8 0.079(2) 0.0453(16) 0.0374(14) -0.0110(12) -0.0234(15) -0.0091(15) C9 0.070(2) 0.0341(13) 0.0451(15) -0.0023(11) -0.0310(14) -0.0153(13) C10 0.0472(14) 0.0285(11) 0.0393(13) 0.0038(10) -0.0239(11) -0.0107(10) C11 0.0436(14) 0.0365(13) 0.0577(17) 0.0036(12) -0.0249(13) -0.0192(11) C12 0.0287(12) 0.0372(13) 0.0552(16) 0.0026(11) -0.0124(11) -0.0118(10) C13 0.0262(10) 0.0261(11) 0.0388(12) 0.0033(9) -0.0122(9) -0.0046(8) C14 0.0246(10) 0.0316(12) 0.0405(13) -0.0019(10) -0.0059(9) -0.0011(9) C15 0.0355(14) 0.0586(19) 0.0523(17) -0.0042(14) 0.0023(12) -0.0101(13) C16 0.0446(16) 0.0355(14) 0.0635(19) -0.0042(13) -0.0069(14) 0.0070(12) C17 0.0326(11) 0.0173(9) 0.0247(10) -0.0003(7) -0.0054(8) -0.0092(8) C18 0.0389(12) 0.0215(10) 0.0280(10) -0.0053(8) 0.0006(9) -0.0098(9) C19 0.0395(13) 0.0355(13) 0.0427(14) -0.0124(11) 0.0029(11) -0.0110(11) C20 0.0495(17) 0.0506(17) 0.0562(18) -0.0222(14) 0.0169(14) -0.0126(14) C21 0.080(2) 0.0456(17) 0.0448(16) -0.0214(13) 0.0124(16) -0.0132(16) C22 0.077(2) 0.0374(14) 0.0351(14) -0.0128(11) -0.0031(14) -0.0182(14) C23 0.0534(15) 0.0263(11) 0.0312(12) -0.0077(9) -0.0060(10) -0.0124(10) C24 0.0562(16) 0.0364(13) 0.0384(13) -0.0064(11) -0.0136(12) -0.0210(12) C25 0.0379(13) 0.0408(14) 0.0421(14) -0.0082(11) -0.0074(10) -0.0210(11) C26 0.0328(11) 0.0277(11) 0.0284(11) -0.0033(8) -0.0043(9) -0.0115(9) C27 0.0357(12) 0.0458(14) 0.0293(11) -0.0065(10) -0.0007(9) -0.0151(11) C28 0.0329(13) 0.074(2) 0.0576(18) -0.0274(16) 0.0010(12) -0.0140(14) C29 0.069(2) 0.064(2) 0.0395(15) 0.0011(14) 0.0071(14) -0.0352(17) C30 0.0277(10) 0.0235(10) 0.0329(11) -0.0036(8) -0.0068(8) -0.0066(8) C31 0.0348(12) 0.0258(11) 0.0378(12) -0.0059(9) -0.0125(10) -0.0055(9) C32 0.0370(13) 0.0423(14) 0.0488(15) -0.0097(12) -0.0133(11) -0.0084(11) C33 0.0473(16) 0.067(2) 0.062(2) -0.0200(16) -0.0278(15) -0.0095(15) C34 0.061(2) 0.075(2) 0.0551(19) -0.0291(17) -0.0331(16) 0.0023(17) C35 0.0515(17) 0.068(2) 0.0428(15) -0.0213(14) -0.0127(13) -0.0041(15) C36 0.0373(13) 0.0479(15) 0.0400(13) -0.0141(11) -0.0108(11) -0.0063(11) C37 0.0265(10) 0.0199(9) 0.0251(10) -0.0039(7) -0.0049(8) -0.0056(7) C38 0.0267(11) 0.0373(13) 0.0419(13) -0.0146(10) -0.0059(9) -0.0057(9) C39 0.0299(12) 0.0460(15) 0.0540(16) -0.0166(12) -0.0063(11) -0.0128(11) C40 0.0431(14) 0.0335(13) 0.0498(15) -0.0116(11) -0.0207(12) -0.0082(11) C41 0.0464(14) 0.0389(13) 0.0366(13) -0.0149(11) -0.0091(11) -0.0123(11) C42 0.0393(12) 0.0400(13) 0.0257(11) -0.0089(9) -0.0032(9) -0.0150(10) C43 0.0300(10) 0.0241(10) 0.0190(9) 0.0013(7) -0.0036(8) -0.0028(8) C44 0.0498(15) 0.0317(12) 0.0267(11) 0.0032(9) -0.0041(10) -0.0145(11) C45 0.0567(17) 0.0442(15) 0.0295(12) 0.0063(11) 0.0021(11) -0.0138(13) C46 0.0612(18) 0.0468(16) 0.0223(11) 0.0041(10) -0.0062(11) -0.0015(13) C47 0.0564(17) 0.0496(16) 0.0252(11) -0.0064(11) -0.0109(11) -0.0041(13) C48 0.0388(12) 0.0349(12) 0.0271(11) -0.0036(9) -0.0095(9) -0.0041(10) C49 0.0214(9) 0.0240(10) 0.0266(10) -0.0034(8) -0.0041(8) -0.0011(7) C50 0.0277(11) 0.0263(11) 0.0425(13) -0.0072(9) -0.0040(9) 0.0013(9) C51 0.0319(12) 0.0375(14) 0.0514(15) -0.0174(12) -0.0043(11) 0.0046(10) C52 0.0249(11) 0.0519(16) 0.0476(15) -0.0152(12) -0.0032(10) 0.0039(11) C53 0.0269(11) 0.0534(16) 0.0428(14) -0.0078(12) -0.0026(10) -0.0109(11) C54 0.0265(10) 0.0320(12) 0.0368(12) -0.0056(9) -0.0066(9) -0.0049(9) O1 0.149(6) 0.037(2) 0.028(2) -0.0069(17) -0.015(3) 0.012(3) C55 0.109(7) 0.134(15) 0.037(4) 0.004(10) 0.031(4) -0.017(14) _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 C30 1.847(2) . ? Ru1 C1 2.0735(19) . ? Ru1 Cl1 2.3804(5) . ? Ru1 Cl2 2.4039(5) . ? Ru1 P1 2.4180(5) . ? P1 C49 1.854(2) . ? P1 C37 1.859(2) . ? P1 C43 1.860(2) . ? N1 C1 1.351(3) . ? N1 C4 1.439(3) . ? N1 C3 1.481(3) . ? N2 C1 1.351(2) . ? N2 C17 1.435(3) . ? N2 C2 1.477(3) . ? C2 C3 1.514(3) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 C13 1.387(3) . ? C4 C5 1.423(3) . ? C5 C6 1.417(4) . ? C5 C10 1.434(3) . ? C6 C7 1.371(4) . ? C6 H6 0.9500 . ? C7 C8 1.412(4) . ? C7 H7 0.9500 . ? C8 C9 1.355(5) . ? C8 H8 0.9500 . ? C9 C10 1.419(4) . ? C9 H9 0.9500 . ? C10 C11 1.402(4) . ? C11 C12 1.361(4) . ? C11 H11 0.9500 . ? C12 C13 1.427(3) . ? C12 H12 0.9500 . ? C13 C14 1.518(4) . ? C14 C15 1.531(4) . ? C14 C16 1.534(4) . ? C14 H14 1.0000 . ? C15 H151 0.9800 . ? C15 H152 0.9800 . ? C15 H153 0.9800 . ? C16 H161 0.9800 . ? C16 H162 0.9800 . ? C16 H163 0.9800 . ? C17 C26 1.376(3) . ? C17 C18 1.426(3) . ? C18 C19 1.414(3) . ? C18 C23 1.427(3) . ? C19 C20 1.376(4) . ? C19 H19 0.9500 . ? C20 C21 1.399(5) . ? C20 H20 0.9500 . ? C21 C22 1.357(5) . ? C21 H211 0.9500 . ? C22 C23 1.426(4) . ? C22 H221 0.9500 . ? C23 C24 1.402(4) . ? C24 C25 1.368(4) . ? C24 H24 0.9500 . ? C25 C26 1.423(3) . ? C25 H25 0.9500 . ? C26 C27 1.515(3) . ? C27 C28 1.522(4) . ? C27 C29 1.542(4) . ? C27 H27 1.0000 . ? C28 H281 0.9800 . ? C28 H282 0.9800 . ? C28 H283 0.9800 . ? C29 H291 0.9800 . ? C29 H292 0.9800 . ? C29 H293 0.9800 . ? C30 C31 1.471(3) . ? C30 H30 0.9500 . ? C31 C32 1.401(3) . ? C31 C36 1.402(4) . ? C32 C33 1.385(4) . ? C32 H321 0.9500 . ? C33 C34 1.395(5) . ? C33 H33 0.9500 . ? C34 C35 1.367(4) . ? C34 H34 0.9500 . ? C35 C36 1.392(4) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.531(3) . ? C37 C38 1.536(3) . ? C37 H37 1.0000 . ? C38 C39 1.533(3) . ? C38 H381 0.9900 . ? C38 H382 0.9900 . ? C39 C40 1.517(4) . ? C39 H391 0.9900 . ? C39 H392 0.9900 . ? C40 C41 1.522(4) . ? C40 H401 0.9900 . ? C40 H402 0.9900 . ? C41 C42 1.536(3) . ? C41 H411 0.9900 . ? C41 H412 0.9900 . ? C42 H421 0.9900 . ? C42 H422 0.9900 . ? C43 C48 1.533(3) . ? C43 C44 1.540(3) . ? C43 H43 1.0000 . ? C44 C45 1.533(3) . ? C44 H441 0.9900 . ? C44 H442 0.9900 . ? C45 C46 1.510(4) . ? C45 H451 0.9900 . ? C45 H452 0.9900 . ? C46 C47 1.516(4) . ? C46 H461 0.9900 . ? C46 H462 0.9900 . ? C47 C48 1.538(3) . ? C47 H471 0.9900 . ? C47 H472 0.9900 . ? C48 H481 0.9900 . ? C48 H482 0.9900 . ? C49 C50 1.530(3) . ? C49 C54 1.537(3) . ? C49 H49 1.0000 . ? C50 C51 1.530(3) . ? C50 H501 0.9900 . ? C50 H502 0.9900 . ? C51 C52 1.516(4) . ? C51 H511 0.9900 . ? C51 H512 0.9900 . ? C52 C53 1.523(4) . ? C52 H521 0.9900 . ? C52 H522 0.9900 . ? C53 C54 1.542(3) . ? C53 H531 0.9900 . ? C53 H532 0.9900 . ? C54 H541 0.9900 . ? C54 H542 0.9900 . ? O1 C55 1.22(2) . ? 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 C30 Ru1 C1 99.94(9) . . ? C30 Ru1 Cl1 103.43(7) . . ? C1 Ru1 Cl1 94.16(5) . . ? C30 Ru1 Cl2 88.43(7) . . ? C1 Ru1 Cl2 83.87(5) . . ? Cl1 Ru1 Cl2 168.14(2) . . ? C30 Ru1 P1 95.23(7) . . ? C1 Ru1 P1 163.03(6) . . ? Cl1 Ru1 P1 89.638(18) . . ? Cl2 Ru1 P1 89.029(18) . . ? C49 P1 C37 102.30(10) . . ? C49 P1 C43 110.39(10) . . ? C37 P1 C43 102.49(10) . . ? C49 P1 Ru1 115.10(7) . . ? C37 P1 Ru1 110.94(7) . . ? C43 P1 Ru1 114.23(7) . . ? C1 N1 C4 127.78(17) . . ? C1 N1 C3 112.61(17) . . ? C4 N1 C3 119.53(17) . . ? C1 N2 C17 126.06(17) . . ? C1 N2 C2 112.64(17) . . ? C17 N2 C2 118.77(17) . . ? N1 C1 N2 106.76(17) . . ? N1 C1 Ru1 124.31(14) . . ? N2 C1 Ru1 127.69(14) . . ? N2 C2 C3 101.81(17) . . ? N2 C2 H21 111.4 . . ? C3 C2 H21 111.4 . . ? N2 C2 H22 111.4 . . ? C3 C2 H22 111.4 . . ? H21 C2 H22 109.3 . . ? N1 C3 C2 101.19(17) . . ? N1 C3 H31 111.5 . . ? C2 C3 H31 111.5 . . ? N1 C3 H32 111.5 . . ? C2 C3 H32 111.5 . . ? H31 C3 H32 109.3 . . ? C13 C4 C5 122.5(2) . . ? C13 C4 N1 119.2(2) . . ? C5 C4 N1 118.07(19) . . ? C6 C5 C4 123.0(2) . . ? C6 C5 C10 118.6(2) . . ? C4 C5 C10 118.4(2) . . ? C7 C6 C5 120.6(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 120.7(3) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 120.2(3) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 122.7(2) . . ? C11 C10 C5 118.6(2) . . ? C9 C10 C5 118.7(3) . . ? C12 C11 C10 121.4(2) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 122.1(2) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C4 C13 C12 117.0(2) . . ? C4 C13 C14 122.4(2) . . ? C12 C13 C14 120.6(2) . . ? C13 C14 C15 113.9(2) . . ? C13 C14 C16 111.6(2) . . ? C15 C14 C16 109.3(2) . . ? C13 C14 H14 107.2 . . ? C15 C14 H14 107.2 . . ? C16 C14 H14 107.2 . . ? C14 C15 H151 109.5 . . ? C14 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? C14 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? C14 C16 H161 109.5 . . ? C14 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? C14 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C26 C17 C18 121.7(2) . . ? C26 C17 N2 119.80(19) . . ? C18 C17 N2 118.32(19) . . ? C19 C18 C17 123.3(2) . . ? C19 C18 C23 118.1(2) . . ? C17 C18 C23 118.5(2) . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.5(3) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H211 120.1 . . ? C20 C21 H211 120.1 . . ? C21 C22 C23 120.8(3) . . ? C21 C22 H221 119.6 . . ? C23 C22 H221 119.6 . . ? C24 C23 C22 121.4(3) . . ? C24 C23 C18 119.2(2) . . ? C22 C23 C18 119.4(3) . . ? C25 C24 C23 120.6(2) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 121.9(2) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C17 C26 C25 118.0(2) . . ? C17 C26 C27 123.4(2) . . ? C25 C26 C27 118.6(2) . . ? C26 C27 C28 113.2(2) . . ? C26 C27 C29 109.2(2) . . ? C28 C27 C29 109.1(2) . . ? C26 C27 H27 108.4 . . ? C28 C27 H27 108.4 . . ? C29 C27 H27 108.4 . . ? C27 C28 H281 109.5 . . ? C27 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? C27 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? C27 C29 H291 109.5 . . ? C27 C29 H292 109.5 . . ? H291 C29 H292 109.5 . . ? C27 C29 H293 109.5 . . ? H291 C29 H293 109.5 . . ? H292 C29 H293 109.5 . . ? C31 C30 Ru1 137.18(18) . . ? C31 C30 H30 111.4 . . ? Ru1 C30 H30 111.4 . . ? C32 C31 C36 117.8(2) . . ? C32 C31 C30 116.4(2) . . ? C36 C31 C30 125.8(2) . . ? C33 C32 C31 122.1(3) . . ? C33 C32 H321 119.0 . . ? C31 C32 H321 119.0 . . ? C32 C33 C34 118.9(3) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 120.0(3) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 121.4(3) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C31 119.8(3) . . ? C35 C36 H36 120.1 . . ? C31 C36 H36 120.1 . . ? C42 C37 C38 108.87(19) . . ? C42 C37 P1 115.82(15) . . ? C38 C37 P1 112.41(15) . . ? C42 C37 H37 106.4 . . ? C38 C37 H37 106.4 . . ? P1 C37 H37 106.4 . . ? C39 C38 C37 109.34(19) . . ? C39 C38 H381 109.8 . . ? C37 C38 H381 109.8 . . ? C39 C38 H382 109.8 . . ? C37 C38 H382 109.8 . . ? H381 C38 H382 108.3 . . ? C40 C39 C38 111.1(2) . . ? C40 C39 H391 109.4 . . ? C38 C39 H391 109.4 . . ? C40 C39 H392 109.4 . . ? C38 C39 H392 109.4 . . ? H391 C39 H392 108.0 . . ? C39 C40 C41 111.9(2) . . ? C39 C40 H401 109.2 . . ? C41 C40 H401 109.2 . . ? C39 C40 H402 109.2 . . ? C41 C40 H402 109.2 . . ? H401 C40 H402 107.9 . . ? C40 C41 C42 112.3(2) . . ? C40 C41 H411 109.1 . . ? C42 C41 H411 109.1 . . ? C40 C41 H412 109.1 . . ? C42 C41 H412 109.1 . . ? H411 C41 H412 107.9 . . ? C37 C42 C41 109.19(19) . . ? C37 C42 H421 109.8 . . ? C41 C42 H421 109.8 . . ? C37 C42 H422 109.8 . . ? C41 C42 H422 109.8 . . ? H421 C42 H422 108.3 . . ? C48 C43 C44 108.47(18) . . ? C48 C43 P1 113.12(15) . . ? C44 C43 P1 117.98(16) . . ? C48 C43 H43 105.4 . . ? C44 C43 H43 105.4 . . ? P1 C43 H43 105.4 . . ? C45 C44 C43 109.9(2) . . ? C45 C44 H441 109.7 . . ? C43 C44 H441 109.7 . . ? C45 C44 H442 109.7 . . ? C43 C44 H442 109.7 . . ? H441 C44 H442 108.2 . . ? C46 C45 C44 111.9(2) . . ? C46 C45 H451 109.2 . . ? C44 C45 H451 109.2 . . ? C46 C45 H452 109.2 . . ? C44 C45 H452 109.2 . . ? H451 C45 H452 107.9 . . ? C45 C46 C47 111.1(2) . . ? C45 C46 H461 109.4 . . ? C47 C46 H461 109.4 . . ? C45 C46 H462 109.4 . . ? C47 C46 H462 109.4 . . ? H461 C46 H462 108.0 . . ? C46 C47 C48 111.2(2) . . ? C46 C47 H471 109.4 . . ? C48 C47 H471 109.4 . . ? C46 C47 H472 109.4 . . ? C48 C47 H472 109.4 . . ? H471 C47 H472 108.0 . . ? C43 C48 C47 109.7(2) . . ? C43 C48 H481 109.7 . . ? C47 C48 H481 109.7 . . ? C43 C48 H482 109.7 . . ? C47 C48 H482 109.7 . . ? H481 C48 H482 108.2 . . ? C50 C49 C54 110.38(18) . . ? C50 C49 P1 114.57(15) . . ? C54 C49 P1 115.56(15) . . ? C50 C49 H49 105.0 . . ? C54 C49 H49 105.0 . . ? P1 C49 H49 105.0 . . ? C51 C50 C49 111.0(2) . . ? C51 C50 H501 109.4 . . ? C49 C50 H501 109.4 . . ? C51 C50 H502 109.4 . . ? C49 C50 H502 109.4 . . ? H501 C50 H502 108.0 . . ? C52 C51 C50 111.8(2) . . ? C52 C51 H511 109.3 . . ? C50 C51 H511 109.3 . . ? C52 C51 H512 109.3 . . ? C50 C51 H512 109.3 . . ? H511 C51 H512 107.9 . . ? C51 C52 C53 111.1(2) . . ? C51 C52 H521 109.4 . . ? C53 C52 H521 109.4 . . ? C51 C52 H522 109.4 . . ? C53 C52 H522 109.4 . . ? H521 C52 H522 108.0 . . ? C52 C53 C54 112.2(2) . . ? C52 C53 H531 109.2 . . ? C54 C53 H531 109.2 . . ? C52 C53 H532 109.2 . . ? C54 C53 H532 109.2 . . ? H531 C53 H532 107.9 . . ? C49 C54 C53 110.1(2) . . ? C49 C54 H541 109.6 . . ? C53 C54 H541 109.6 . . ? C49 C54 H542 109.6 . . ? C53 C54 H542 109.6 . . ? H541 C54 H542 108.2 . . ? 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 C30 Ru1 P1 C49 59.66(11) . . . . ? C1 Ru1 P1 C49 -93.7(2) . . . . ? Cl1 Ru1 P1 C49 163.12(8) . . . . ? Cl2 Ru1 P1 C49 -28.67(8) . . . . ? C30 Ru1 P1 C37 175.20(10) . . . . ? C1 Ru1 P1 C37 21.8(2) . . . . ? Cl1 Ru1 P1 C37 -81.35(7) . . . . ? Cl2 Ru1 P1 C37 86.86(7) . . . . ? C30 Ru1 P1 C43 -69.58(11) . . . . ? C1 Ru1 P1 C43 137.0(2) . . . . ? Cl1 Ru1 P1 C43 33.87(8) . . . . ? Cl2 Ru1 P1 C43 -157.91(8) . . . . ? C4 N1 C1 N2 173.7(2) . . . . ? C3 N1 C1 N2 -9.7(2) . . . . ? C4 N1 C1 Ru1 -18.2(3) . . . . ? C3 N1 C1 Ru1 158.35(16) . . . . ? C17 N2 C1 N1 -167.29(19) . . . . ? C2 N2 C1 N1 -5.7(2) . . . . ? C17 N2 C1 Ru1 25.2(3) . . . . ? C2 N2 C1 Ru1 -173.25(16) . . . . ? C30 Ru1 C1 N1 -173.14(17) . . . . ? Cl1 Ru1 C1 N1 82.44(17) . . . . ? Cl2 Ru1 C1 N1 -85.82(17) . . . . ? P1 Ru1 C1 N1 -20.1(3) . . . . ? C30 Ru1 C1 N2 -7.6(2) . . . . ? Cl1 Ru1 C1 N2 -112.02(17) . . . . ? Cl2 Ru1 C1 N2 79.72(18) . . . . ? P1 Ru1 C1 N2 145.47(15) . . . . ? C1 N2 C2 C3 17.7(2) . . . . ? C17 N2 C2 C3 -179.21(19) . . . . ? C1 N1 C3 C2 20.1(2) . . . . ? C4 N1 C3 C2 -163.0(2) . . . . ? N2 C2 C3 N1 -20.9(2) . . . . ? C1 N1 C4 C13 -84.5(3) . . . . ? C3 N1 C4 C13 99.1(2) . . . . ? C1 N1 C4 C5 101.8(3) . . . . ? C3 N1 C4 C5 -74.6(3) . . . . ? C13 C4 C5 C6 178.9(2) . . . . ? N1 C4 C5 C6 -7.5(3) . . . . ? C13 C4 C5 C10 -1.3(3) . . . . ? N1 C4 C5 C10 172.25(19) . . . . ? C4 C5 C6 C7 -179.8(2) . . . . ? C10 C5 C6 C7 0.4(3) . . . . ? C5 C6 C7 C8 -0.6(4) . . . . ? C6 C7 C8 C9 0.1(4) . . . . ? C7 C8 C9 C10 0.5(4) . . . . ? C8 C9 C10 C11 178.4(3) . . . . ? C8 C9 C10 C5 -0.7(4) . . . . ? C6 C5 C10 C11 -178.9(2) . . . . ? C4 C5 C10 C11 1.3(3) . . . . ? C6 C5 C10 C9 0.2(3) . . . . ? C4 C5 C10 C9 -179.6(2) . . . . ? C9 C10 C11 C12 -178.9(3) . . . . ? C5 C10 C11 C12 0.2(4) . . . . ? C10 C11 C12 C13 -1.9(4) . . . . ? C5 C4 C13 C12 -0.3(3) . . . . ? N1 C4 C13 C12 -173.78(19) . . . . ? C5 C4 C13 C14 178.3(2) . . . . ? N1 C4 C13 C14 4.8(3) . . . . ? C11 C12 C13 C4 1.9(4) . . . . ? C11 C12 C13 C14 -176.7(2) . . . . ? C4 C13 C14 C15 154.5(2) . . . . ? C12 C13 C14 C15 -27.0(3) . . . . ? C4 C13 C14 C16 -81.1(3) . . . . ? C12 C13 C14 C16 97.5(3) . . . . ? C1 N2 C17 C26 -114.9(2) . . . . ? C2 N2 C17 C26 84.5(3) . . . . ? C1 N2 C17 C18 69.6(3) . . . . ? C2 N2 C17 C18 -91.0(2) . . . . ? C26 C17 C18 C19 -177.8(2) . . . . ? N2 C17 C18 C19 -2.4(3) . . . . ? C26 C17 C18 C23 3.2(3) . . . . ? N2 C17 C18 C23 178.64(19) . . . . ? C17 C18 C19 C20 -178.1(2) . . . . ? C23 C18 C19 C20 0.8(4) . . . . ? C18 C19 C20 C21 -0.9(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? C20 C21 C22 C23 -1.2(5) . . . . ? C21 C22 C23 C24 -179.4(3) . . . . ? C21 C22 C23 C18 1.2(4) . . . . ? C19 C18 C23 C24 179.6(2) . . . . ? C17 C18 C23 C24 -1.4(3) . . . . ? C19 C18 C23 C22 -1.0(4) . . . . ? C17 C18 C23 C22 178.1(2) . . . . ? C22 C23 C24 C25 179.6(3) . . . . ? C18 C23 C24 C25 -1.0(4) . . . . ? C23 C24 C25 C26 1.6(4) . . . . ? C18 C17 C26 C25 -2.7(3) . . . . ? N2 C17 C26 C25 -178.0(2) . . . . ? C18 C17 C26 C27 175.5(2) . . . . ? N2 C17 C26 C27 0.1(3) . . . . ? C24 C25 C26 C17 0.3(4) . . . . ? C24 C25 C26 C27 -178.0(2) . . . . ? C17 C26 C27 C28 127.6(3) . . . . ? C25 C26 C27 C28 -54.3(3) . . . . ? C17 C26 C27 C29 -110.7(3) . . . . ? C25 C26 C27 C29 67.5(3) . . . . ? C1 Ru1 C30 C31 -108.5(2) . . . . ? Cl1 Ru1 C30 C31 -11.8(3) . . . . ? Cl2 Ru1 C30 C31 168.0(2) . . . . ? P1 Ru1 C30 C31 79.1(2) . . . . ? Ru1 C30 C31 C32 -167.8(2) . . . . ? Ru1 C30 C31 C36 10.1(4) . . . . ? C36 C31 C32 C33 0.9(4) . . . . ? C30 C31 C32 C33 179.0(3) . . . . ? C31 C32 C33 C34 -1.4(5) . . . . ? C32 C33 C34 C35 0.7(5) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C34 C35 C36 C31 -0.9(5) . . . . ? C32 C31 C36 C35 0.3(4) . . . . ? C30 C31 C36 C35 -177.6(3) . . . . ? C49 P1 C37 C42 52.83(18) . . . . ? C43 P1 C37 C42 167.25(17) . . . . ? Ru1 P1 C37 C42 -70.41(17) . . . . ? C49 P1 C37 C38 178.85(16) . . . . ? C43 P1 C37 C38 -66.72(18) . . . . ? Ru1 P1 C37 C38 55.61(17) . . . . ? C42 C37 C38 C39 -62.4(3) . . . . ? P1 C37 C38 C39 167.87(18) . . . . ? C37 C38 C39 C40 58.4(3) . . . . ? C38 C39 C40 C41 -53.2(3) . . . . ? C39 C40 C41 C42 52.4(3) . . . . ? C38 C37 C42 C41 60.8(3) . . . . ? P1 C37 C42 C41 -171.39(17) . . . . ? C40 C41 C42 C37 -56.1(3) . . . . ? C49 P1 C43 C48 -47.41(19) . . . . ? C37 P1 C43 C48 -155.77(16) . . . . ? Ru1 P1 C43 C48 84.16(16) . . . . ? C49 P1 C43 C44 80.7(2) . . . . ? C37 P1 C43 C44 -27.7(2) . . . . ? Ru1 P1 C43 C44 -147.75(16) . . . . ? C48 C43 C44 C45 -59.7(3) . . . . ? P1 C43 C44 C45 170.02(19) . . . . ? C43 C44 C45 C46 57.3(3) . . . . ? C44 C45 C46 C47 -54.5(3) . . . . ? C45 C46 C47 C48 55.0(3) . . . . ? C44 C43 C48 C47 60.5(3) . . . . ? P1 C43 C48 C47 -166.59(17) . . . . ? C46 C47 C48 C43 -58.7(3) . . . . ? C37 P1 C49 C50 56.57(18) . . . . ? C43 P1 C49 C50 -51.92(19) . . . . ? Ru1 P1 C49 C50 176.97(14) . . . . ? C37 P1 C49 C54 -173.39(16) . . . . ? C43 P1 C49 C54 78.11(18) . . . . ? Ru1 P1 C49 C54 -53.00(18) . . . . ? C54 C49 C50 C51 57.2(3) . . . . ? P1 C49 C50 C51 -170.28(17) . . . . ? C49 C50 C51 C52 -56.4(3) . . . . ? C50 C51 C52 C53 54.6(3) . . . . ? C51 C52 C53 C54 -54.5(3) . . . . ? C50 C49 C54 C53 -56.4(3) . . . . ? P1 C49 C54 C53 171.54(17) . . . . ? C52 C53 C54 C49 55.6(3) . . . . ? #===END data_2b _database_code_depnum_ccdc_archive 'CCDC 707354' # DT0827 _audit_creation_method SHELXL-97 _audit_creation_date 08-08-14 # CLIENT : R. Dorta # JOURNAL COMPOUND IDENTIFIER : 2b # ABSOLUTE CONFIGURATION : # POLYMORPH : # NEUTRON STUDY : # BIOLOGICAL ACTIVITY : # COMMENTS : solvent: dichloromethane / MeOH. # Disorder in some of the i-Pr groups: see _refine_special_details. _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C60 H81 Cl2 N2 P Ru' _chemical_formula_sum 'C60 H81 Cl2 N2 P Ru' _chemical_formula_weight 1033.19 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 120 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 162 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cl Cl 4 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 2 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 2 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2159(2) _cell_length_b 12.6367(3) _cell_length_c 21.1798(5) _cell_angle_alpha 97.3871(10) _cell_angle_beta 95.1677(13) _cell_angle_gamma 102.1724(13) _cell_volume 2631.12(10) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 106359 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 0.984 _exptl_special_details ; Solvent used: dichloromethane / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.797(1) Frames collected: 667 Seconds exposure per frame: 50 Degrees rotation per frame: 1.0 Crystal-Detector distance (mm): 32.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 58851 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.46 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 12008 _reflns_number_gt 8426 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF94 (Beurskens et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. Some of the i-Pr groups show evidence for slight disorder. One of these groups was modelled as disordered over two conformations. Two sets of overlapping positions were defined for the terminal methyl atoms of this i-Pr group and the site occupation factor of the major conformation of the group refined to 0.53(2). Similarity restraints were applied to the chemically equivalent bond lengths involving all disordered C-atoms, while neighbouring atoms within and between each conformation of the disordered group were restrained to have similar atomic displacement parameters. ; _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^)+(0.0630P)^2^+5.2433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12008 _refine_ls_number_parameters 624 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.201 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.097 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.18132(3) 0.47296(3) 0.254461(15) 0.02617(11) Uani 1 1 d . . . Cl1 Cl 0.39927(10) 0.52717(8) 0.21823(5) 0.0330(2) Uani 1 1 d . . . Cl2 Cl -0.04256(11) 0.38534(10) 0.26948(6) 0.0420(3) Uani 1 1 d . . . P1 P 0.25874(11) 0.33758(9) 0.31119(5) 0.0314(2) Uani 1 1 d . . . N1 N 0.1337(3) 0.6662(3) 0.18673(15) 0.0265(7) Uani 1 1 d . . . N2 N 0.0881(3) 0.5140(3) 0.12092(15) 0.0280(7) Uani 1 1 d . . . C1 C 0.1214(4) 0.5580(3) 0.18401(18) 0.0259(8) Uani 1 1 d . . . C2 C 0.1021(5) 0.5980(3) 0.0783(2) 0.0380(10) Uani 1 1 d . . . H21 H 0.0243 0.5825 0.0444 0.046 Uiso 1 1 calc R . . H22 H 0.1864 0.6034 0.0580 0.046 Uiso 1 1 calc R . . C3 C 0.1056(5) 0.7006(4) 0.12385(19) 0.0350(9) Uani 1 1 d . . . H31 H 0.1779 0.7620 0.1167 0.042 Uiso 1 1 calc R . . H32 H 0.0180 0.7225 0.1198 0.042 Uiso 1 1 calc R . . C4 C 0.1465(4) 0.7460(3) 0.24316(18) 0.0273(8) Uani 1 1 d . . . C5 C 0.2746(4) 0.8186(3) 0.2619(2) 0.0303(9) Uani 1 1 d . . . C6 C 0.3894(4) 0.8100(3) 0.2311(2) 0.0334(9) Uani 1 1 d . . . H6 H 0.3832 0.7521 0.1968 0.040 Uiso 1 1 calc R . . C7 C 0.5097(4) 0.8842(4) 0.2500(2) 0.0403(11) Uani 1 1 d . . . H7 H 0.5856 0.8773 0.2282 0.048 Uiso 1 1 calc R . . C8 C 0.5232(4) 0.9708(4) 0.3014(2) 0.0424(11) Uani 1 1 d . . . C9 C 0.4150(4) 0.9783(3) 0.3326(2) 0.0386(10) Uani 1 1 d . . . H9 H 0.4248 1.0349 0.3680 0.046 Uiso 1 1 calc R . . C10 C 0.2873(4) 0.9047(3) 0.3146(2) 0.0330(9) Uani 1 1 d . . . C11 C 0.1732(4) 0.9117(3) 0.3462(2) 0.0375(10) Uani 1 1 d . . . H11 H 0.1810 0.9664 0.3825 0.045 Uiso 1 1 calc R . . C12 C 0.0522(4) 0.8418(3) 0.3258(2) 0.0358(10) Uani 1 1 d . . . H12 H -0.0230 0.8496 0.3478 0.043 Uiso 1 1 calc R . . C13 C 0.0345(4) 0.7575(3) 0.2727(2) 0.0299(9) Uani 1 1 d . . . C14 C 0.6592(5) 1.0522(4) 0.3218(3) 0.0588(15) Uani 1 1 d . . . H14 H 0.6425 1.1155 0.3509 0.071 Uiso 1 1 calc R . . C15 C 0.7182(7) 1.0971(5) 0.2639(4) 0.089(2) Uani 1 1 d . . . H151 H 0.7424 1.0380 0.2359 0.134 Uiso 1 1 calc R . . H152 H 0.7989 1.1555 0.2788 0.134 Uiso 1 1 calc R . . H153 H 0.6510 1.1265 0.2399 0.134 Uiso 1 1 calc R . . C16 C 0.7562(7) 1.0020(6) 0.3594(5) 0.119(4) Uani 1 1 d . . . H161 H 0.7189 0.9817 0.3983 0.179 Uiso 1 1 calc R . . H162 H 0.8426 1.0551 0.3712 0.179 Uiso 1 1 calc R . . H163 H 0.7701 0.9365 0.3330 0.179 Uiso 1 1 calc R . . C17 C -0.1061(4) 0.6873(4) 0.2492(2) 0.0386(10) Uani 1 1 d . . . H17 H -0.0961 0.6225 0.2191 0.046 Uiso 1 1 calc R . . C18 C -0.1887(5) 0.7522(5) 0.2116(3) 0.0643(16) Uani 1 1 d . . . H181 H -0.2783 0.7060 0.1957 0.097 Uiso 1 1 calc R . . H182 H -0.1425 0.7746 0.1752 0.097 Uiso 1 1 calc R . . H183 H -0.1981 0.8173 0.2398 0.097 Uiso 1 1 calc R . . C19 C -0.1824(5) 0.6450(4) 0.3022(3) 0.0546(13) Uani 1 1 d . . . H191 H -0.2010 0.7067 0.3302 0.082 Uiso 1 1 calc R . . H192 H -0.1280 0.6062 0.3272 0.082 Uiso 1 1 calc R . . H193 H -0.2677 0.5947 0.2834 0.082 Uiso 1 1 calc R . . C20 C 0.0378(4) 0.4003(3) 0.09352(19) 0.0315(9) Uani 1 1 d . . . C21 C 0.1272(4) 0.3471(3) 0.05980(19) 0.0324(9) Uani 1 1 d . . . C22 C 0.2664(5) 0.3936(4) 0.0614(2) 0.0405(10) Uani 1 1 d . . . H221 H 0.3046 0.4634 0.0862 0.049 Uiso 1 1 calc R . . C23 C 0.3456(5) 0.3397(4) 0.0280(3) 0.0498(12) Uani 1 1 d . . . H23 H 0.4389 0.3726 0.0305 0.060 Uiso 1 1 calc R . . C24 C 0.2951(6) 0.2361(4) -0.0104(3) 0.0536(13) Uani 1 1 d . A . C25 C 0.1615(5) 0.1901(4) -0.0120(2) 0.0480(12) Uani 1 1 d . . . H25 H 0.1253 0.1206 -0.0373 0.058 Uiso 1 1 calc R . . C26 C 0.0746(5) 0.2422(4) 0.0229(2) 0.0384(10) Uani 1 1 d . . . C27 C -0.0627(5) 0.1924(4) 0.0238(2) 0.0429(11) Uani 1 1 d . . . H27 H -0.0990 0.1214 0.0003 0.052 Uiso 1 1 calc R . . C28 C -0.1434(5) 0.2443(4) 0.0576(2) 0.0416(11) Uani 1 1 d . . . H28 H -0.2348 0.2078 0.0575 0.050 Uiso 1 1 calc R . . C29 C -0.0970(4) 0.3511(3) 0.09310(19) 0.0340(9) Uani 1 1 d . . . C30 C 0.3897(8) 0.1774(5) -0.0471(5) 0.104(3) Uani 1 1 d D . . H301 H 0.4518 0.1704 -0.0093 0.125 Uiso 0.534(16) 1 calc PR A 1 H302 H 0.3326 0.1504 -0.0893 0.125 Uiso 0.466(16) 1 calc PR A 2 C31A C 0.485(4) 0.2462(19) -0.078(3) 0.082(7) Uani 0.534(16) 1 d PDU A 1 H311 H 0.5615 0.2118 -0.0848 0.123 Uiso 0.534(16) 1 calc PR A 1 H312 H 0.5182 0.3174 -0.0504 0.123 Uiso 0.534(16) 1 calc PR A 1 H313 H 0.4424 0.2566 -0.1190 0.123 Uiso 0.534(16) 1 calc PR A 1 C32A C 0.3418(18) 0.0639(8) -0.0712(11) 0.096(5) Uani 0.534(16) 1 d PDU A 1 H321 H 0.4162 0.0339 -0.0865 0.145 Uiso 0.534(16) 1 calc PR A 1 H322 H 0.2699 0.0545 -0.1067 0.145 Uiso 0.534(16) 1 calc PR A 1 H323 H 0.3065 0.0252 -0.0369 0.145 Uiso 0.534(16) 1 calc PR A 1 C31B C 0.502(4) 0.248(2) -0.066(3) 0.084(7) Uani 0.466(16) 1 d PDU A 2 H314 H 0.5314 0.2099 -0.1043 0.126 Uiso 0.466(16) 1 calc PR A 2 H315 H 0.5767 0.2673 -0.0315 0.126 Uiso 0.466(16) 1 calc PR A 2 H316 H 0.4766 0.3144 -0.0771 0.126 Uiso 0.466(16) 1 calc PR A 2 C32B C 0.400(2) 0.0761(13) -0.0268(11) 0.093(5) Uani 0.466(16) 1 d PDU A 2 H324 H 0.3104 0.0336 -0.0228 0.140 Uiso 0.466(16) 1 calc PR A 2 H325 H 0.4563 0.0904 0.0149 0.140 Uiso 0.466(16) 1 calc PR A 2 H326 H 0.4423 0.0347 -0.0584 0.140 Uiso 0.466(16) 1 calc PR A 2 C33 C -0.1942(4) 0.4093(4) 0.1260(2) 0.0386(10) Uani 1 1 d . . . H33 H -0.1416 0.4589 0.1647 0.046 Uiso 1 1 calc R . . C34 C -0.2531(5) 0.4815(4) 0.0827(3) 0.0522(13) Uani 1 1 d . . . H341 H -0.1802 0.5395 0.0738 0.078 Uiso 1 1 calc R . . H342 H -0.3187 0.5144 0.1046 0.078 Uiso 1 1 calc R . . H343 H -0.2979 0.4363 0.0423 0.078 Uiso 1 1 calc R . . C35 C -0.3103(5) 0.3316(4) 0.1491(2) 0.0522(13) Uani 1 1 d . . . H351 H -0.3728 0.2903 0.1120 0.078 Uiso 1 1 calc R . . H352 H -0.3583 0.3742 0.1770 0.078 Uiso 1 1 calc R . . H353 H -0.2741 0.2806 0.1730 0.078 Uiso 1 1 calc R . . C36 C 0.1851(4) 0.5746(3) 0.3249(2) 0.0359(10) Uani 1 1 d . . . H36 H 0.0968 0.5730 0.3361 0.043 Uiso 1 1 calc R . . C37 C 0.2857(5) 0.6578(3) 0.3690(2) 0.0382(10) Uani 1 1 d . . . C38 C 0.4243(5) 0.6883(4) 0.3607(2) 0.0445(11) Uani 1 1 d . . . H38 H 0.4567 0.6557 0.3241 0.053 Uiso 1 1 calc R . . C39 C 0.5123(6) 0.7660(4) 0.4062(3) 0.0549(13) Uani 1 1 d . . . H39 H 0.6050 0.7862 0.4005 0.066 Uiso 1 1 calc R . . C40 C 0.4668(6) 0.8143(5) 0.4597(3) 0.0606(15) Uani 1 1 d . . . H40 H 0.5282 0.8668 0.4907 0.073 Uiso 1 1 calc R . . C41 C 0.3302(7) 0.7858(4) 0.4683(2) 0.0581(15) Uani 1 1 d . . . H41 H 0.2977 0.8199 0.5044 0.070 Uiso 1 1 calc R . . C42 C 0.2427(5) 0.7068(4) 0.4231(2) 0.0441(11) Uani 1 1 d . . . H42 H 0.1506 0.6859 0.4296 0.053 Uiso 1 1 calc R . . C43 C 0.2461(4) 0.2085(3) 0.2551(2) 0.0358(10) Uani 1 1 d . . . H43 H 0.2882 0.1588 0.2794 0.043 Uiso 1 1 calc R . . C44 C 0.1003(5) 0.1463(4) 0.2293(3) 0.0505(13) Uani 1 1 d . . . H441 H 0.0480 0.1320 0.2657 0.061 Uiso 1 1 calc R . . H442 H 0.0563 0.1915 0.2032 0.061 Uiso 1 1 calc R . . C45 C 0.1021(5) 0.0369(4) 0.1881(2) 0.0480(12) Uani 1 1 d . . . H451 H 0.1366 -0.0111 0.2158 0.058 Uiso 1 1 calc R . . H452 H 0.0087 -0.0002 0.1696 0.058 Uiso 1 1 calc R . . C46 C 0.1879(7) 0.0521(4) 0.1348(2) 0.0637(17) Uani 1 1 d . . . H461 H 0.1448 0.0892 0.1031 0.076 Uiso 1 1 calc R . . H462 H 0.1935 -0.0206 0.1129 0.076 Uiso 1 1 calc R . . C47 C 0.3302(6) 0.1196(4) 0.1588(3) 0.0621(15) Uani 1 1 d . . . H471 H 0.3785 0.0779 0.1857 0.074 Uiso 1 1 calc R . . H472 H 0.3805 0.1334 0.1217 0.074 Uiso 1 1 calc R . . C48 C 0.3258(6) 0.2286(4) 0.1980(2) 0.0529(13) Uani 1 1 d . . . H481 H 0.2824 0.2724 0.1706 0.064 Uiso 1 1 calc R . . H482 H 0.4188 0.2705 0.2139 0.064 Uiso 1 1 calc R . . C49 C 0.1591(4) 0.2876(3) 0.37544(19) 0.0315(9) Uani 1 1 d . . . H49 H 0.0707 0.2428 0.3530 0.038 Uiso 1 1 calc R . . C50 C 0.1249(5) 0.3784(4) 0.4229(2) 0.0392(10) Uani 1 1 d . . . H501 H 0.2085 0.4225 0.4489 0.047 Uiso 1 1 calc R . . H502 H 0.0832 0.4276 0.3989 0.047 Uiso 1 1 calc R . . C51 C 0.0275(5) 0.3264(4) 0.4667(2) 0.0417(11) Uani 1 1 d . . . H511 H 0.0081 0.3848 0.4978 0.050 Uiso 1 1 calc R . . H512 H -0.0586 0.2875 0.4406 0.050 Uiso 1 1 calc R . . C52 C 0.0832(5) 0.2467(4) 0.5027(2) 0.0452(11) Uani 1 1 d . . . H521 H 0.0139 0.2112 0.5278 0.054 Uiso 1 1 calc R . . H522 H 0.1623 0.2872 0.5333 0.054 Uiso 1 1 calc R . . C53 C 0.1253(5) 0.1582(4) 0.4574(2) 0.0419(11) Uani 1 1 d . . . H531 H 0.1703 0.1127 0.4829 0.050 Uiso 1 1 calc R . . H532 H 0.0442 0.1100 0.4314 0.050 Uiso 1 1 calc R . . C54 C 0.2217(5) 0.2107(4) 0.4130(2) 0.0394(10) Uani 1 1 d . . . H541 H 0.2435 0.1525 0.3825 0.047 Uiso 1 1 calc R . . H542 H 0.3068 0.2526 0.4388 0.047 Uiso 1 1 calc R . . C55 C 0.4414(4) 0.3803(3) 0.3422(2) 0.0336(9) Uani 1 1 d . . . H55 H 0.4841 0.4248 0.3106 0.040 Uiso 1 1 calc R . . C56 C 0.4678(4) 0.4580(4) 0.4059(2) 0.0380(10) Uani 1 1 d . . . H561 H 0.4104 0.5120 0.4044 0.046 Uiso 1 1 calc R . . H562 H 0.4441 0.4159 0.4412 0.046 Uiso 1 1 calc R . . C57 C 0.6154(4) 0.5176(4) 0.4187(2) 0.0422(11) Uani 1 1 d . . . H571 H 0.6316 0.5673 0.4602 0.051 Uiso 1 1 calc R . . H572 H 0.6378 0.5625 0.3845 0.051 Uiso 1 1 calc R . . C58 C 0.7056(5) 0.4360(4) 0.4207(2) 0.0459(12) Uani 1 1 d . . . H581 H 0.8011 0.4760 0.4243 0.055 Uiso 1 1 calc R . . H582 H 0.6936 0.4002 0.4593 0.055 Uiso 1 1 calc R . . C59 C 0.6753(4) 0.3497(4) 0.3622(3) 0.0469(12) Uani 1 1 d . . . H591 H 0.7282 0.2938 0.3684 0.056 Uiso 1 1 calc R . . H592 H 0.7036 0.3837 0.3246 0.056 Uiso 1 1 calc R . . C60 C 0.5239(5) 0.2936(4) 0.3489(3) 0.0455(11) Uani 1 1 d . . . H601 H 0.5068 0.2401 0.3090 0.055 Uiso 1 1 calc R . . H602 H 0.4966 0.2537 0.3846 0.055 Uiso 1 1 calc R . . 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 0.02586(17) 0.02654(17) 0.02565(18) 0.00515(12) 0.00087(12) 0.00508(12) Cl1 0.0291(5) 0.0346(5) 0.0355(5) 0.0088(4) 0.0042(4) 0.0056(4) Cl2 0.0333(6) 0.0474(6) 0.0448(6) 0.0151(5) 0.0019(5) 0.0041(5) P1 0.0320(6) 0.0296(6) 0.0316(6) 0.0047(4) 0.0016(4) 0.0050(4) N1 0.0286(17) 0.0256(17) 0.0254(17) 0.0055(13) 0.0022(13) 0.0054(13) N2 0.0316(18) 0.0270(17) 0.0236(17) 0.0062(14) 0.0015(13) 0.0023(14) C1 0.0171(18) 0.030(2) 0.028(2) 0.0046(16) 0.0005(15) 0.0005(15) C2 0.048(3) 0.036(2) 0.029(2) 0.0098(18) 0.0041(19) 0.003(2) C3 0.040(2) 0.036(2) 0.029(2) 0.0106(18) 0.0021(18) 0.0073(19) C4 0.032(2) 0.0240(19) 0.027(2) 0.0066(16) -0.0004(16) 0.0074(16) C5 0.030(2) 0.024(2) 0.036(2) 0.0058(17) 0.0001(17) 0.0050(16) C6 0.032(2) 0.031(2) 0.036(2) 0.0052(18) 0.0024(18) 0.0060(17) C7 0.030(2) 0.036(2) 0.055(3) 0.007(2) 0.006(2) 0.0057(19) C8 0.032(2) 0.030(2) 0.061(3) 0.004(2) -0.003(2) 0.0038(18) C9 0.038(2) 0.025(2) 0.050(3) -0.0003(19) -0.003(2) 0.0062(18) C10 0.036(2) 0.024(2) 0.038(2) 0.0051(18) -0.0008(18) 0.0073(17) C11 0.044(3) 0.032(2) 0.037(2) 0.0002(19) 0.0069(19) 0.0110(19) C12 0.036(2) 0.035(2) 0.040(2) 0.0070(19) 0.0091(19) 0.0137(19) C13 0.028(2) 0.029(2) 0.033(2) 0.0077(17) 0.0029(16) 0.0060(16) C14 0.040(3) 0.033(3) 0.094(4) -0.004(3) -0.002(3) 0.002(2) C15 0.064(4) 0.055(4) 0.133(7) -0.007(4) 0.038(4) -0.020(3) C16 0.052(4) 0.067(4) 0.206(10) -0.023(5) -0.066(5) 0.003(3) C17 0.028(2) 0.040(2) 0.045(3) 0.001(2) 0.0075(19) 0.0044(18) C18 0.036(3) 0.085(4) 0.071(4) 0.013(3) -0.009(3) 0.016(3) C19 0.036(3) 0.055(3) 0.070(4) 0.017(3) 0.010(2) -0.001(2) C20 0.036(2) 0.029(2) 0.026(2) 0.0048(17) -0.0046(17) 0.0044(17) C21 0.034(2) 0.036(2) 0.028(2) 0.0090(18) -0.0002(17) 0.0083(18) C22 0.043(3) 0.039(2) 0.038(2) 0.006(2) 0.002(2) 0.008(2) C23 0.042(3) 0.053(3) 0.059(3) 0.015(3) 0.013(2) 0.013(2) C24 0.060(3) 0.046(3) 0.061(3) 0.009(3) 0.020(3) 0.019(3) C25 0.064(3) 0.041(3) 0.039(3) 0.003(2) 0.007(2) 0.012(2) C26 0.045(3) 0.036(2) 0.031(2) 0.0014(19) -0.0015(19) 0.009(2) C27 0.048(3) 0.035(2) 0.036(2) -0.001(2) -0.002(2) -0.004(2) C28 0.034(2) 0.041(3) 0.041(3) 0.002(2) -0.0040(19) -0.0048(19) C29 0.037(2) 0.036(2) 0.026(2) 0.0067(18) -0.0015(17) 0.0020(18) C30 0.111(6) 0.067(4) 0.155(8) 0.017(5) 0.087(6) 0.040(4) C31A 0.071(8) 0.113(7) 0.062(15) -0.006(6) 0.029(10) 0.022(6) C32A 0.114(13) 0.073(6) 0.122(13) 0.004(9) 0.062(10) 0.049(8) C31B 0.071(8) 0.114(7) 0.064(16) -0.010(7) 0.031(10) 0.018(6) C32B 0.114(13) 0.072(7) 0.118(14) 0.011(9) 0.063(11) 0.055(8) C33 0.034(2) 0.045(3) 0.034(2) 0.005(2) 0.0042(18) 0.0026(19) C34 0.050(3) 0.059(3) 0.050(3) 0.009(3) 0.004(2) 0.017(2) C35 0.041(3) 0.062(3) 0.047(3) 0.009(3) 0.006(2) -0.003(2) C36 0.038(2) 0.034(2) 0.037(2) 0.0066(19) 0.0026(19) 0.0120(19) C37 0.050(3) 0.030(2) 0.034(2) 0.0051(18) -0.001(2) 0.011(2) C38 0.050(3) 0.036(2) 0.046(3) 0.004(2) 0.002(2) 0.012(2) C39 0.050(3) 0.049(3) 0.061(3) 0.006(3) -0.010(3) 0.009(2) C40 0.076(4) 0.049(3) 0.043(3) -0.001(2) -0.016(3) -0.003(3) C41 0.093(5) 0.047(3) 0.035(3) 0.000(2) 0.001(3) 0.022(3) C42 0.055(3) 0.044(3) 0.037(3) 0.013(2) 0.006(2) 0.015(2) C43 0.043(3) 0.031(2) 0.031(2) 0.0040(18) -0.0005(18) 0.0061(19) C44 0.044(3) 0.039(3) 0.061(3) -0.005(2) -0.006(2) 0.005(2) C45 0.054(3) 0.035(3) 0.047(3) 0.001(2) -0.007(2) 0.002(2) C46 0.114(5) 0.035(3) 0.033(3) -0.004(2) -0.005(3) 0.009(3) C47 0.080(4) 0.051(3) 0.051(3) -0.011(3) 0.020(3) 0.013(3) C48 0.063(3) 0.040(3) 0.049(3) -0.004(2) 0.019(3) -0.004(2) C49 0.031(2) 0.035(2) 0.028(2) 0.0072(17) 0.0030(17) 0.0060(17) C50 0.039(2) 0.041(3) 0.039(2) 0.014(2) 0.0000(19) 0.009(2) C51 0.036(2) 0.050(3) 0.044(3) 0.013(2) 0.012(2) 0.014(2) C52 0.044(3) 0.052(3) 0.040(3) 0.013(2) 0.012(2) 0.007(2) C53 0.042(3) 0.039(3) 0.044(3) 0.012(2) 0.002(2) 0.004(2) C54 0.044(3) 0.035(2) 0.041(3) 0.012(2) 0.005(2) 0.009(2) C55 0.029(2) 0.037(2) 0.036(2) 0.0120(19) 0.0015(17) 0.0055(17) C56 0.035(2) 0.035(2) 0.043(3) 0.007(2) 0.0052(19) 0.0037(18) C57 0.035(2) 0.044(3) 0.044(3) 0.005(2) -0.002(2) 0.003(2) C58 0.031(2) 0.048(3) 0.056(3) 0.013(2) -0.003(2) 0.003(2) C59 0.028(2) 0.040(3) 0.071(3) 0.004(2) 0.008(2) 0.0072(19) C60 0.036(3) 0.040(3) 0.059(3) 0.005(2) 0.002(2) 0.008(2) _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 C36 1.830(4) . ? Ru1 C1 2.069(4) . ? Ru1 Cl2 2.3899(11) . ? Ru1 Cl1 2.4115(10) . ? Ru1 P1 2.4339(11) . ? P1 C55 1.863(4) . ? P1 C43 1.865(4) . ? P1 C49 1.867(4) . ? N1 C1 1.340(5) . ? N1 C4 1.438(5) . ? N1 C3 1.475(5) . ? N2 C1 1.363(5) . ? N2 C20 1.445(5) . ? N2 C2 1.473(5) . ? C2 C3 1.506(6) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 C13 1.378(6) . ? C4 C5 1.421(5) . ? C5 C6 1.410(6) . ? C5 C10 1.430(6) . ? C6 C7 1.371(6) . ? C6 H6 0.9500 . ? C7 C8 1.416(7) . ? C7 H7 0.9500 . ? C8 C9 1.351(7) . ? C8 C14 1.533(6) . ? C9 C10 1.421(6) . ? C9 H9 0.9500 . ? C10 C11 1.410(6) . ? C11 C12 1.357(6) . ? C11 H11 0.9500 . ? C12 C13 1.416(6) . ? C12 H12 0.9500 . ? C13 C17 1.522(6) . ? C14 C16 1.507(9) . ? C14 C15 1.536(9) . ? C14 H14 1.0000 . ? C15 H151 0.9800 . ? C15 H152 0.9800 . ? C15 H153 0.9800 . ? C16 H161 0.9800 . ? C16 H162 0.9800 . ? C16 H163 0.9800 . ? C17 C19 1.512(7) . ? C17 C18 1.536(7) . ? C17 H17 1.0000 . ? C18 H181 0.9800 . ? C18 H182 0.9800 . ? C18 H183 0.9800 . ? C19 H191 0.9800 . ? C19 H192 0.9800 . ? C19 H193 0.9800 . ? C20 C29 1.385(6) . ? C20 C21 1.431(6) . ? C21 C22 1.415(6) . ? C21 C26 1.419(6) . ? C22 C23 1.353(7) . ? C22 H221 0.9500 . ? C23 C24 1.418(7) . ? C23 H23 0.9500 . ? C24 C25 1.362(7) . ? C24 C30 1.540(8) . ? C25 C26 1.417(7) . ? C25 H25 0.9500 . ? C26 C27 1.414(6) . ? C27 C28 1.356(7) . ? C27 H27 0.9500 . ? C28 C29 1.419(6) . ? C28 H28 0.9500 . ? C29 C33 1.521(6) . ? C30 C32B 1.424(7) . ? C30 C32A 1.424(7) . ? C30 C31A 1.426(7) . ? C30 C31B 1.426(7) . ? C30 H301 1.0000 . ? C30 H302 1.0000 . ? C31A H311 0.9800 . ? C31A H312 0.9800 . ? C31A H313 0.9800 . ? C32A H321 0.9800 . ? C32A H322 0.9800 . ? C32A H323 0.9800 . ? C31B H314 0.9800 . ? C31B H315 0.9800 . ? C31B H316 0.9800 . ? C32B H324 0.9800 . ? C32B H325 0.9800 . ? C32B H326 0.9800 . ? C33 C35 1.533(6) . ? C33 C34 1.543(7) . ? C33 H33 1.0000 . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 H351 0.9800 . ? C35 H352 0.9800 . ? C35 H353 0.9800 . ? C36 C37 1.468(6) . ? C36 H36 0.9500 . ? C37 C42 1.383(6) . ? C37 C38 1.419(7) . ? C38 C39 1.389(7) . ? C38 H38 0.9500 . ? C39 C40 1.381(8) . ? C39 H39 0.9500 . ? C40 C41 1.401(8) . ? C40 H40 0.9500 . ? C41 C42 1.390(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.535(6) . ? C43 C44 1.543(6) . ? C43 H43 1.0000 . ? C44 C45 1.542(7) . ? C44 H441 0.9900 . ? C44 H442 0.9900 . ? C45 C46 1.497(8) . ? C45 H451 0.9900 . ? C45 H452 0.9900 . ? C46 C47 1.527(8) . ? C46 H461 0.9900 . ? C46 H462 0.9900 . ? C47 C48 1.526(7) . ? C47 H471 0.9900 . ? C47 H472 0.9900 . ? C48 H481 0.9900 . ? C48 H482 0.9900 . ? C49 C54 1.535(6) . ? C49 C50 1.544(6) . ? C49 H49 1.0000 . ? C50 C51 1.526(6) . ? C50 H501 0.9900 . ? C50 H502 0.9900 . ? C51 C52 1.511(7) . ? C51 H511 0.9900 . ? C51 H512 0.9900 . ? C52 C53 1.535(7) . ? C52 H521 0.9900 . ? C52 H522 0.9900 . ? C53 C54 1.532(6) . ? C53 H531 0.9900 . ? C53 H532 0.9900 . ? C54 H541 0.9900 . ? C54 H542 0.9900 . ? C55 C60 1.528(6) . ? C55 C56 1.530(6) . ? C55 H55 1.0000 . ? C56 C57 1.520(6) . ? C56 H561 0.9900 . ? C56 H562 0.9900 . ? C57 C58 1.523(7) . ? C57 H571 0.9900 . ? C57 H572 0.9900 . ? C58 C59 1.503(7) . ? C58 H581 0.9900 . ? C58 H582 0.9900 . ? C59 C60 1.544(6) . ? C59 H591 0.9900 . ? C59 H592 0.9900 . ? C60 H601 0.9900 . ? C60 H602 0.9900 . ? 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 C36 Ru1 C1 98.90(17) . . ? C36 Ru1 Cl2 89.24(14) . . ? C1 Ru1 Cl2 95.04(10) . . ? C36 Ru1 Cl1 104.27(14) . . ? C1 Ru1 Cl1 83.14(10) . . ? Cl2 Ru1 Cl1 166.49(4) . . ? C36 Ru1 P1 97.15(13) . . ? C1 Ru1 P1 163.84(11) . . ? Cl2 Ru1 P1 87.11(4) . . ? Cl1 Ru1 P1 91.02(4) . . ? C55 P1 C43 103.6(2) . . ? C55 P1 C49 110.04(19) . . ? C43 P1 C49 102.06(19) . . ? C55 P1 Ru1 112.55(14) . . ? C43 P1 Ru1 110.32(14) . . ? C49 P1 Ru1 116.93(14) . . ? C1 N1 C4 127.3(3) . . ? C1 N1 C3 113.9(3) . . ? C4 N1 C3 117.8(3) . . ? C1 N2 C20 128.2(3) . . ? C1 N2 C2 112.5(3) . . ? C20 N2 C2 119.2(3) . . ? N1 C1 N2 106.3(3) . . ? N1 C1 Ru1 128.6(3) . . ? N2 C1 Ru1 123.8(3) . . ? N2 C2 C3 102.3(3) . . ? N2 C2 H21 111.3 . . ? C3 C2 H21 111.3 . . ? N2 C2 H22 111.3 . . ? C3 C2 H22 111.3 . . ? H21 C2 H22 109.2 . . ? N1 C3 C2 101.9(3) . . ? N1 C3 H31 111.4 . . ? C2 C3 H31 111.4 . . ? N1 C3 H32 111.4 . . ? C2 C3 H32 111.4 . . ? H31 C3 H32 109.2 . . ? C13 C4 C5 122.4(4) . . ? C13 C4 N1 120.2(3) . . ? C5 C4 N1 117.1(3) . . ? C6 C5 C4 123.2(4) . . ? C6 C5 C10 118.5(4) . . ? C4 C5 C10 118.3(4) . . ? C7 C6 C5 120.8(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 121.2(4) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C9 C8 C7 118.7(4) . . ? C9 C8 C14 121.2(4) . . ? C7 C8 C14 120.1(4) . . ? C8 C9 C10 122.5(4) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 123.3(4) . . ? C11 C10 C5 118.4(4) . . ? C9 C10 C5 118.2(4) . . ? C12 C11 C10 121.1(4) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 122.2(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C4 C13 C12 117.5(4) . . ? C4 C13 C17 123.1(4) . . ? C12 C13 C17 119.4(4) . . ? C16 C14 C8 111.1(5) . . ? C16 C14 C15 112.1(6) . . ? C8 C14 C15 111.4(5) . . ? C16 C14 H14 107.4 . . ? C8 C14 H14 107.4 . . ? C15 C14 H14 107.4 . . ? C14 C15 H151 109.5 . . ? C14 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? C14 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? C14 C16 H161 109.5 . . ? C14 C16 H162 109.5 . . ? H161 C16 H162 109.5 . . ? C14 C16 H163 109.5 . . ? H161 C16 H163 109.5 . . ? H162 C16 H163 109.5 . . ? C19 C17 C13 113.9(4) . . ? C19 C17 C18 109.6(4) . . ? C13 C17 C18 109.8(4) . . ? C19 C17 H17 107.8 . . ? C13 C17 H17 107.8 . . ? C18 C17 H17 107.8 . . ? C17 C18 H181 109.5 . . ? C17 C18 H182 109.5 . . ? H181 C18 H182 109.5 . . ? C17 C18 H183 109.5 . . ? H181 C18 H183 109.5 . . ? H182 C18 H183 109.5 . . ? C17 C19 H191 109.5 . . ? C17 C19 H192 109.5 . . ? H191 C19 H192 109.5 . . ? C17 C19 H193 109.5 . . ? H191 C19 H193 109.5 . . ? H192 C19 H193 109.5 . . ? C29 C20 C21 122.2(4) . . ? C29 C20 N2 120.0(4) . . ? C21 C20 N2 117.3(4) . . ? C22 C21 C26 117.9(4) . . ? C22 C21 C20 123.4(4) . . ? C26 C21 C20 118.8(4) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H221 119.7 . . ? C21 C22 H221 119.7 . . ? C22 C23 C24 122.7(5) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 117.2(5) . . ? C25 C24 C30 122.0(5) . . ? C23 C24 C30 120.8(5) . . ? C24 C25 C26 122.3(5) . . ? C24 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 122.4(4) . . ? C27 C26 C21 118.4(4) . . ? C25 C26 C21 119.2(4) . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 122.7(4) . . ? C27 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C20 C29 C28 116.9(4) . . ? C20 C29 C33 122.4(4) . . ? C28 C29 C33 120.7(4) . . ? C32A C30 C31A 121.3(15) . . ? C32B C30 C31B 121.3(15) . . ? C32B C30 C24 113.8(8) . . ? C32A C30 C24 117.8(8) . . ? C31A C30 C24 115.0(12) . . ? C31B C30 C24 115.3(13) . . ? C32B C30 H301 55.6 . . ? C32A C30 H301 98.2 . . ? C31A C30 H301 98.2 . . ? C31B C30 H301 87.1 . . ? C24 C30 H301 98.2 . . ? C32B C30 H302 100.5 . . ? C32A C30 H302 57.5 . . ? C31A C30 H302 89.7 . . ? C31B C30 H302 100.5 . . ? C24 C30 H302 100.5 . . ? H301 C30 H302 154.4 . . ? C30 C31A H311 109.5 . . ? C30 C31A H312 109.5 . . ? C30 C31A H313 109.5 . . ? C30 C32A H321 109.5 . . ? C30 C32A H322 109.5 . . ? C30 C32A H323 109.5 . . ? C30 C31B H314 109.5 . . ? C30 C31B H315 109.5 . . ? H314 C31B H315 109.5 . . ? C30 C31B H316 109.5 . . ? H314 C31B H316 109.5 . . ? H315 C31B H316 109.5 . . ? C30 C32B H324 109.5 . . ? C30 C32B H325 109.5 . . ? H324 C32B H325 109.5 . . ? C30 C32B H326 109.5 . . ? H324 C32B H326 109.5 . . ? H325 C32B H326 109.5 . . ? C29 C33 C35 113.6(4) . . ? C29 C33 C34 111.9(4) . . ? C35 C33 C34 109.0(4) . . ? C29 C33 H33 107.3 . . ? C35 C33 H33 107.3 . . ? C34 C33 H33 107.3 . . ? C33 C34 H341 109.5 . . ? C33 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C33 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? C33 C35 H351 109.5 . . ? C33 C35 H352 109.5 . . ? H351 C35 H352 109.5 . . ? C33 C35 H353 109.5 . . ? H351 C35 H353 109.5 . . ? H352 C35 H353 109.5 . . ? C37 C36 Ru1 138.1(3) . . ? C37 C36 H36 110.9 . . ? Ru1 C36 H36 110.9 . . ? C42 C37 C38 118.2(4) . . ? C42 C37 C36 117.5(4) . . ? C38 C37 C36 124.3(4) . . ? C39 C38 C37 119.9(5) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.8(5) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 120.0(5) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 119.0(5) . . ? C42 C41 H41 120.5 . . ? C40 C41 H41 120.5 . . ? C37 C42 C41 122.0(5) . . ? C37 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C48 C43 C44 108.9(4) . . ? C48 C43 P1 111.8(3) . . ? C44 C43 P1 114.4(3) . . ? C48 C43 H43 107.2 . . ? C44 C43 H43 107.2 . . ? P1 C43 H43 107.2 . . ? C45 C44 C43 109.7(4) . . ? C45 C44 H441 109.7 . . ? C43 C44 H441 109.7 . . ? C45 C44 H442 109.7 . . ? C43 C44 H442 109.7 . . ? H441 C44 H442 108.2 . . ? C46 C45 C44 112.5(4) . . ? C46 C45 H451 109.1 . . ? C44 C45 H451 109.1 . . ? C46 C45 H452 109.1 . . ? C44 C45 H452 109.1 . . ? H451 C45 H452 107.8 . . ? C45 C46 C47 112.3(4) . . ? C45 C46 H461 109.1 . . ? C47 C46 H461 109.1 . . ? C45 C46 H462 109.1 . . ? C47 C46 H462 109.1 . . ? H461 C46 H462 107.9 . . ? C48 C47 C46 110.8(5) . . ? C48 C47 H471 109.5 . . ? C46 C47 H471 109.5 . . ? C48 C47 H472 109.5 . . ? C46 C47 H472 109.5 . . ? H471 C47 H472 108.1 . . ? C47 C48 C43 110.0(4) . . ? C47 C48 H481 109.7 . . ? C43 C48 H481 109.7 . . ? C47 C48 H482 109.7 . . ? C43 C48 H482 109.7 . . ? H481 C48 H482 108.2 . . ? C54 C49 C50 109.4(3) . . ? C54 C49 P1 113.7(3) . . ? C50 C49 P1 114.9(3) . . ? C54 C49 H49 106.0 . . ? C50 C49 H49 106.0 . . ? P1 C49 H49 106.0 . . ? C51 C50 C49 109.5(4) . . ? C51 C50 H501 109.8 . . ? C49 C50 H501 109.8 . . ? C51 C50 H502 109.8 . . ? C49 C50 H502 109.8 . . ? H501 C50 H502 108.2 . . ? C52 C51 C50 112.3(4) . . ? C52 C51 H511 109.1 . . ? C50 C51 H511 109.1 . . ? C52 C51 H512 109.1 . . ? C50 C51 H512 109.1 . . ? H511 C51 H512 107.9 . . ? C51 C52 C53 112.0(4) . . ? C51 C52 H521 109.2 . . ? C53 C52 H521 109.2 . . ? C51 C52 H522 109.2 . . ? C53 C52 H522 109.2 . . ? H521 C52 H522 107.9 . . ? C54 C53 C52 110.6(4) . . ? C54 C53 H531 109.5 . . ? C52 C53 H531 109.5 . . ? C54 C53 H532 109.5 . . ? C52 C53 H532 109.5 . . ? H531 C53 H532 108.1 . . ? C53 C54 C49 111.3(4) . . ? C53 C54 H541 109.4 . . ? C49 C54 H541 109.4 . . ? C53 C54 H542 109.4 . . ? C49 C54 H542 109.4 . . ? H541 C54 H542 108.0 . . ? C60 C55 C56 107.5(4) . . ? C60 C55 P1 119.9(3) . . ? C56 C55 P1 112.3(3) . . ? C60 C55 H55 105.3 . . ? C56 C55 H55 105.3 . . ? P1 C55 H55 105.3 . . ? C57 C56 C55 110.1(4) . . ? C57 C56 H561 109.6 . . ? C55 C56 H561 109.6 . . ? C57 C56 H562 109.6 . . ? C55 C56 H562 109.6 . . ? H561 C56 H562 108.1 . . ? C56 C57 C58 110.5(4) . . ? C56 C57 H571 109.5 . . ? C58 C57 H571 109.5 . . ? C56 C57 H572 109.5 . . ? C58 C57 H572 109.5 . . ? H571 C57 H572 108.1 . . ? C59 C58 C57 112.5(4) . . ? C59 C58 H581 109.1 . . ? C57 C58 H581 109.1 . . ? C59 C58 H582 109.1 . . ? C57 C58 H582 109.1 . . ? H581 C58 H582 107.8 . . ? C58 C59 C60 111.9(4) . . ? C58 C59 H591 109.2 . . ? C60 C59 H591 109.2 . . ? C58 C59 H592 109.2 . . ? C60 C59 H592 109.2 . . ? H591 C59 H592 107.9 . . ? C55 C60 C59 109.4(4) . . ? C55 C60 H601 109.8 . . ? C59 C60 H601 109.8 . . ? C55 C60 H602 109.8 . . ? C59 C60 H602 109.8 . . ? H601 C60 H602 108.2 . . ? 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 C36 Ru1 P1 C55 -72.6(2) . . . . ? C1 Ru1 P1 C55 100.3(4) . . . . ? Cl2 Ru1 P1 C55 -161.49(16) . . . . ? Cl1 Ru1 P1 C55 31.90(16) . . . . ? C36 Ru1 P1 C43 172.2(2) . . . . ? C1 Ru1 P1 C43 -14.8(4) . . . . ? Cl2 Ru1 P1 C43 83.33(15) . . . . ? Cl1 Ru1 P1 C43 -83.28(15) . . . . ? C36 Ru1 P1 C49 56.2(2) . . . . ? C1 Ru1 P1 C49 -130.8(4) . . . . ? Cl2 Ru1 P1 C49 -32.66(15) . . . . ? Cl1 Ru1 P1 C49 160.73(15) . . . . ? C4 N1 C1 N2 169.3(3) . . . . ? C3 N1 C1 N2 1.3(4) . . . . ? C4 N1 C1 Ru1 -23.8(5) . . . . ? C3 N1 C1 Ru1 168.1(3) . . . . ? C20 N2 C1 N1 -166.6(4) . . . . ? C2 N2 C1 N1 10.6(4) . . . . ? C20 N2 C1 Ru1 25.8(5) . . . . ? C2 N2 C1 Ru1 -157.1(3) . . . . ? C36 Ru1 C1 N1 22.6(4) . . . . ? Cl2 Ru1 C1 N1 112.6(3) . . . . ? Cl1 Ru1 C1 N1 -80.8(3) . . . . ? P1 Ru1 C1 N1 -150.3(3) . . . . ? C36 Ru1 C1 N2 -172.6(3) . . . . ? Cl2 Ru1 C1 N2 -82.6(3) . . . . ? Cl1 Ru1 C1 N2 83.9(3) . . . . ? P1 Ru1 C1 N2 14.4(6) . . . . ? C1 N2 C2 C3 -17.4(4) . . . . ? C20 N2 C2 C3 160.0(4) . . . . ? C1 N1 C3 C2 -11.7(4) . . . . ? C4 N1 C3 C2 179.0(3) . . . . ? N2 C2 C3 N1 16.1(4) . . . . ? C1 N1 C4 C13 -78.3(5) . . . . ? C3 N1 C4 C13 89.3(4) . . . . ? C1 N1 C4 C5 108.5(4) . . . . ? C3 N1 C4 C5 -83.8(4) . . . . ? C13 C4 C5 C6 -178.1(4) . . . . ? N1 C4 C5 C6 -5.1(6) . . . . ? C13 C4 C5 C10 1.7(6) . . . . ? N1 C4 C5 C10 174.8(3) . . . . ? C4 C5 C6 C7 178.2(4) . . . . ? C10 C5 C6 C7 -1.7(6) . . . . ? C5 C6 C7 C8 0.7(7) . . . . ? C6 C7 C8 C9 1.1(7) . . . . ? C6 C7 C8 C14 179.7(5) . . . . ? C7 C8 C9 C10 -2.0(7) . . . . ? C14 C8 C9 C10 179.4(4) . . . . ? C8 C9 C10 C11 -179.5(4) . . . . ? C8 C9 C10 C5 1.1(7) . . . . ? C6 C5 C10 C11 -178.6(4) . . . . ? C4 C5 C10 C11 1.5(6) . . . . ? C6 C5 C10 C9 0.8(6) . . . . ? C4 C5 C10 C9 -179.1(4) . . . . ? C9 C10 C11 C12 177.7(4) . . . . ? C5 C10 C11 C12 -2.9(6) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C5 C4 C13 C12 -3.5(6) . . . . ? N1 C4 C13 C12 -176.3(3) . . . . ? C5 C4 C13 C17 174.0(4) . . . . ? N1 C4 C13 C17 1.2(6) . . . . ? C11 C12 C13 C4 2.1(6) . . . . ? C11 C12 C13 C17 -175.5(4) . . . . ? C9 C8 C14 C16 102.5(7) . . . . ? C7 C8 C14 C16 -76.0(7) . . . . ? C9 C8 C14 C15 -131.8(5) . . . . ? C7 C8 C14 C15 49.6(6) . . . . ? C4 C13 C17 C19 135.2(4) . . . . ? C12 C13 C17 C19 -47.4(6) . . . . ? C4 C13 C17 C18 -101.5(5) . . . . ? C12 C13 C17 C18 76.0(5) . . . . ? C1 N2 C20 C29 79.3(5) . . . . ? C2 N2 C20 C29 -97.7(5) . . . . ? C1 N2 C20 C21 -109.1(5) . . . . ? C2 N2 C20 C21 74.0(5) . . . . ? C29 C20 C21 C22 -177.5(4) . . . . ? N2 C20 C21 C22 11.1(6) . . . . ? C29 C20 C21 C26 2.3(6) . . . . ? N2 C20 C21 C26 -169.2(4) . . . . ? C26 C21 C22 C23 0.8(7) . . . . ? C20 C21 C22 C23 -179.4(4) . . . . ? C21 C22 C23 C24 0.8(8) . . . . ? C22 C23 C24 C25 -1.2(8) . . . . ? C22 C23 C24 C30 -179.4(6) . . . . ? C23 C24 C25 C26 0.1(8) . . . . ? C30 C24 C25 C26 178.3(6) . . . . ? C24 C25 C26 C27 -177.0(5) . . . . ? C24 C25 C26 C21 1.4(7) . . . . ? C22 C21 C26 C27 176.6(4) . . . . ? C20 C21 C26 C27 -3.1(6) . . . . ? C22 C21 C26 C25 -1.9(6) . . . . ? C20 C21 C26 C25 178.4(4) . . . . ? C25 C26 C27 C28 -180.0(5) . . . . ? C21 C26 C27 C28 1.6(7) . . . . ? C26 C27 C28 C29 0.9(7) . . . . ? C21 C20 C29 C28 0.2(6) . . . . ? N2 C20 C29 C28 171.4(4) . . . . ? C21 C20 C29 C33 -176.8(4) . . . . ? N2 C20 C29 C33 -5.6(6) . . . . ? C27 C28 C29 C20 -1.9(7) . . . . ? C27 C28 C29 C33 175.2(4) . . . . ? C25 C24 C30 C32B -61.5(16) . . . . ? C23 C24 C30 C32B 116.6(14) . . . . ? C25 C24 C30 C32A -13.7(16) . . . . ? C23 C24 C30 C32A 164.4(13) . . . . ? C25 C24 C30 C31A 140(3) . . . . ? C23 C24 C30 C31A -42(3) . . . . ? C25 C24 C30 C31B 152(3) . . . . ? C23 C24 C30 C31B -30(3) . . . . ? C20 C29 C33 C35 -151.4(4) . . . . ? C28 C29 C33 C35 31.7(6) . . . . ? C20 C29 C33 C34 84.6(5) . . . . ? C28 C29 C33 C34 -92.3(5) . . . . ? C1 Ru1 C36 C37 -100.9(5) . . . . ? Cl2 Ru1 C36 C37 164.1(5) . . . . ? Cl1 Ru1 C36 C37 -15.8(5) . . . . ? P1 Ru1 C36 C37 77.1(5) . . . . ? Ru1 C36 C37 C42 -170.5(4) . . . . ? Ru1 C36 C37 C38 7.3(7) . . . . ? C42 C37 C38 C39 -0.4(7) . . . . ? C36 C37 C38 C39 -178.2(4) . . . . ? C37 C38 C39 C40 0.0(8) . . . . ? C38 C39 C40 C41 -0.6(8) . . . . ? C39 C40 C41 C42 1.6(8) . . . . ? C38 C37 C42 C41 1.3(7) . . . . ? C36 C37 C42 C41 179.4(4) . . . . ? C40 C41 C42 C37 -1.9(8) . . . . ? C55 P1 C43 C48 -63.9(4) . . . . ? C49 P1 C43 C48 -178.2(3) . . . . ? Ru1 P1 C43 C48 56.8(4) . . . . ? C55 P1 C43 C44 171.9(3) . . . . ? C49 P1 C43 C44 57.5(4) . . . . ? Ru1 P1 C43 C44 -67.4(4) . . . . ? C48 C43 C44 C45 58.8(5) . . . . ? P1 C43 C44 C45 -175.4(3) . . . . ? C43 C44 C45 C46 -55.3(6) . . . . ? C44 C45 C46 C47 52.8(6) . . . . ? C45 C46 C47 C48 -53.9(6) . . . . ? C46 C47 C48 C43 58.2(6) . . . . ? C44 C43 C48 C47 -61.1(6) . . . . ? P1 C43 C48 C47 171.6(4) . . . . ? C55 P1 C49 C54 -44.6(4) . . . . ? C43 P1 C49 C54 64.9(3) . . . . ? Ru1 P1 C49 C54 -174.7(3) . . . . ? C55 P1 C49 C50 82.6(3) . . . . ? C43 P1 C49 C50 -167.9(3) . . . . ? Ru1 P1 C49 C50 -47.4(3) . . . . ? C54 C49 C50 C51 -58.6(5) . . . . ? P1 C49 C50 C51 172.1(3) . . . . ? C49 C50 C51 C52 57.1(5) . . . . ? C50 C51 C52 C53 -54.7(5) . . . . ? C51 C52 C53 C54 53.0(5) . . . . ? C52 C53 C54 C49 -55.8(5) . . . . ? C50 C49 C54 C53 59.0(5) . . . . ? P1 C49 C54 C53 -171.0(3) . . . . ? C43 P1 C55 C60 -31.0(4) . . . . ? C49 P1 C55 C60 77.5(4) . . . . ? Ru1 P1 C55 C60 -150.2(3) . . . . ? C43 P1 C55 C56 -158.7(3) . . . . ? C49 P1 C55 C56 -50.2(4) . . . . ? Ru1 P1 C55 C56 82.1(3) . . . . ? C60 C55 C56 C57 63.6(5) . . . . ? P1 C55 C56 C57 -162.4(3) . . . . ? C55 C56 C57 C58 -58.8(5) . . . . ? C56 C57 C58 C59 52.6(5) . . . . ? C57 C58 C59 C60 -51.8(6) . . . . ? C56 C55 C60 C59 -61.5(5) . . . . ? P1 C55 C60 C59 168.7(3) . . . . ? C58 C59 C60 C55 56.5(6) . . . . ? #===END data_2c _database_code_depnum_ccdc_archive 'CCDC 707355' # DT0831 _audit_creation_method SHELXL-97 _audit_creation_date 08-09-16 # CLIENT : R. Dorta # JOURNAL COMPOUND IDENTIFIER : 2c # ABSOLUTE CONFIGURATION : # POLYMORPH : # NEUTRON STUDY : # BIOLOGICAL ACTIVITY : # COMMENTS : solvent: dichloromethane / MeOH. # One disordered dichloromethane in # asymmetric unit. SQUEEZE used - see refinement_special_details _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C67 H90 Cl N2 P Ru, C H2 Cl2' _chemical_formula_sum 'C68 H92 Cl3 N2 P Ru' _chemical_formula_weight 1175.82 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 136 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 184 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cl Cl 6 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 2 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 2 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6367(2) _cell_length_b 12.7897(2) _cell_length_c 19.6484(2) _cell_angle_alpha 87.3964(8) _cell_angle_beta 75.4952(8) _cell_angle_gamma 79.1259(8) _cell_volume 3019.14(7) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 94065 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.853 _exptl_absorpt_correction_T_max 0.951 _exptl_special_details ; Solvent used: dichloromethane / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.588(1) Frames collected: 583 Seconds exposure per frame: 96 Degrees rotation per frame: 1.2 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 77597 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _reflns_number_total 13742 _reflns_number_gt 11087 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The asymmetric unit contains one molecule of the Rh-complex plus one disordered molecule of CH~2~Cl~2~. Attempts to model the solvent molecule were unsatisfactory. Therefore, the SQUEEZE routine of the program PLATON was employed - see below. ; # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.169 -0.072 0.824 146 39 ' ' 2 -0.169 1.072 0.176 147 39 ' ' 3 0.258 0.345 0.785 9 1 ' ' 4 0.285 0.296 0.871 6 0 ' ' 5 0.483 0.450 0.406 7 0 ' ' 6 0.517 0.550 0.594 7 0 ' ' 7 0.717 0.700 0.135 6 0 ' ' 8 0.743 0.652 0.221 8 0 ' ' _platon_squeeze_details ; The asymmetric unit contains one molecule of the Rh-complex plus one disordered molecule of CH~2~Cl~2~. Attempts to model the solvent molecule were unsatisfactory. Therefore, the SQUEEZE routine of the program PLATON was employed. This procedure, which allows the disordered solvent molecule to be omitted entirely from the subsequent refinement model, gave substantially improved refinement results and there were no significant peaks of residual electron density to be found in the voids of the structure. When the solvent molecule is omitted from the model, each unit cell contains two cavities of 147 \%A^3^. The electron count in each cavity was calculated to be approximately 40 e. As the crystals grew from a CH~2~Cl~2~ / MeOH solution and the initial electron density peak distribution looked somewhat like a CH~2~Cl~2~ molecule, it is assumed the cavities contain CH~2~Cl~2~. Allowing for one molecule of CH~2~Cl~2~ per cavity yields 42 e and this estimate was used in the subsequent calculation of the empirical formula, formula weight, density, linear absorption coefficient and F(000). Thus the ratio of Rh-complex to CH~2~Cl~2~ is approximately 1:1. ; _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^)+(0.0499P)^2^+1.2220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0043(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 13740 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.489 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.069 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.172032(14) 0.256595(13) 0.248130(9) 0.02328(6) Uani 1 1 d . . . P1 P 0.22443(5) 0.31018(5) 0.13639(3) 0.02823(13) Uani 1 1 d . . . Cl1 Cl -0.01995(5) 0.25095(5) 0.24123(3) 0.03314(13) Uani 1 1 d . . . N1 N 0.36648(14) 0.12811(13) 0.28008(9) 0.0232(4) Uani 1 1 d . . . N2 N 0.39274(14) 0.29321(13) 0.26598(9) 0.0240(4) Uani 1 1 d . . . C1 C 0.30725(17) 0.04316(16) 0.28225(11) 0.0237(4) Uani 1 1 d . . . C2 C 0.35693(18) -0.04980(16) 0.24479(11) 0.0255(4) Uani 1 1 d . . . C3 C 0.28940(18) -0.12608(17) 0.24277(12) 0.0290(5) Uani 1 1 d . . . H3 H 0.3224 -0.1909 0.2181 0.035 Uiso 1 1 calc R . . C4 C 0.17861(18) -0.10925(17) 0.27518(11) 0.0282(5) Uani 1 1 d . . . H4 H 0.1353 -0.1604 0.2704 0.034 Uiso 1 1 calc R . . C5 C 0.12736(17) -0.01572(16) 0.31606(11) 0.0245(4) Uani 1 1 d . . . C6 C 0.01452(17) 0.00154(16) 0.35338(11) 0.0254(4) Uani 1 1 d . . . H6 H -0.0291 -0.0497 0.3493 0.030 Uiso 1 1 calc R . . C7 C -0.03513(17) 0.08948(16) 0.39541(11) 0.0243(4) Uani 1 1 d . . . C8 C 0.14336(18) 0.14939(16) 0.36671(10) 0.0247(4) Uani 1 1 d . . . H8 H 0.1867 0.1996 0.3731 0.030 Uiso 1 1 calc R . . C9 C 0.03345(17) 0.16291(16) 0.40158(11) 0.0245(4) Uani 1 1 d . . . H9 H 0.0019 0.2236 0.4310 0.029 Uiso 1 1 calc R . . C10 C 0.19370(17) 0.06052(15) 0.32085(10) 0.0229(4) Uani 1 1 d . . . C11 C 0.48005(19) -0.07230(18) 0.20775(12) 0.0310(5) Uani 1 1 d . . . H11 H 0.5082 -0.0039 0.2054 0.037 Uiso 1 1 calc R . . C12 C 0.5443(2) -0.1512(2) 0.25070(15) 0.0437(6) Uani 1 1 d . . . H121 H 0.5316 -0.1226 0.2981 0.065 Uiso 1 1 calc R . . H122 H 0.6239 -0.1621 0.2277 0.065 Uiso 1 1 calc R . . H123 H 0.5185 -0.2193 0.2538 0.065 Uiso 1 1 calc R . . C13 C 0.5024(2) -0.1129(2) 0.13243(14) 0.0472(7) Uani 1 1 d . . . H131 H 0.4830 -0.1837 0.1334 0.071 Uiso 1 1 calc R . . H132 H 0.5814 -0.1173 0.1091 0.071 Uiso 1 1 calc R . . H133 H 0.4573 -0.0638 0.1065 0.071 Uiso 1 1 calc R . . C14 C -0.15689(17) 0.10931(16) 0.43485(11) 0.0249(4) Uani 1 1 d . . . C15 C -0.21899(18) 0.21371(17) 0.40902(12) 0.0288(5) Uani 1 1 d . . . H151 H -0.1834 0.2738 0.4158 0.035 Uiso 1 1 calc R . . H152 H -0.2139 0.2078 0.3582 0.035 Uiso 1 1 calc R . . C16 C -0.34155(18) 0.23565(17) 0.44962(12) 0.0297(5) Uani 1 1 d . . . H16 H -0.3802 0.3032 0.4322 0.036 Uiso 1 1 calc R . . C17 C -0.34951(19) 0.24669(17) 0.52807(12) 0.0305(5) Uani 1 1 d . . . H171 H -0.4286 0.2622 0.5544 0.037 Uiso 1 1 calc R . . H172 H -0.3141 0.3065 0.5356 0.037 Uiso 1 1 calc R . . C18 C -0.29097(18) 0.14292(17) 0.55504(11) 0.0287(5) Uani 1 1 d . . . H18 H -0.2964 0.1501 0.6063 0.034 Uiso 1 1 calc R . . C19 C -0.16813(18) 0.12018(18) 0.51480(11) 0.0289(5) Uani 1 1 d . . . H191 H -0.1302 0.0535 0.5325 0.035 Uiso 1 1 calc R . . H192 H -0.1316 0.1789 0.5230 0.035 Uiso 1 1 calc R . . C20 C -0.39596(19) 0.14361(18) 0.43746(12) 0.0314(5) Uani 1 1 d . . . H201 H -0.3898 0.1364 0.3866 0.038 Uiso 1 1 calc R . . H202 H -0.4758 0.1580 0.4621 0.038 Uiso 1 1 calc R . . C21 C -0.33809(18) 0.04039(17) 0.46525(12) 0.0290(5) Uani 1 1 d . . . H21 H -0.3742 -0.0198 0.4577 0.035 Uiso 1 1 calc R . . C22 C -0.34750(19) 0.05170(18) 0.54373(12) 0.0306(5) Uani 1 1 d . . . H221 H -0.3114 -0.0155 0.5620 0.037 Uiso 1 1 calc R . . H222 H -0.4268 0.0665 0.5696 0.037 Uiso 1 1 calc R . . C23 C -0.21538(18) 0.01818(17) 0.42514(12) 0.0282(5) Uani 1 1 d . . . H231 H -0.2099 0.0094 0.3745 0.034 Uiso 1 1 calc R . . H232 H -0.1777 -0.0491 0.4423 0.034 Uiso 1 1 calc R . . C24 C 0.31992(17) 0.22854(16) 0.26223(10) 0.0237(4) Uani 1 1 d . . . C25 C 0.45382(18) 0.13005(17) 0.31670(12) 0.0270(4) Uani 1 1 d . . . H251 H 0.5157 0.0688 0.3032 0.032 Uiso 1 1 calc R . . H252 H 0.4243 0.1309 0.3684 0.032 Uiso 1 1 calc R . . C26 C 0.48979(18) 0.23502(17) 0.28992(12) 0.0286(5) Uani 1 1 d . . . H261 H 0.5043 0.2742 0.3280 0.034 Uiso 1 1 calc R . . H262 H 0.5574 0.2230 0.2506 0.034 Uiso 1 1 calc R . . C27 C 0.36196(19) 0.40601(16) 0.27386(11) 0.0267(4) Uani 1 1 d . . . C28 C 0.44346(19) 0.46877(17) 0.26312(12) 0.0298(5) Uani 1 1 d . . . C29 C 0.4104(2) 0.57428(18) 0.28980(13) 0.0358(5) Uani 1 1 d . . . H29 H 0.4649 0.6180 0.2842 0.043 Uiso 1 1 calc R . . C30 C 0.3038(2) 0.61496(18) 0.32301(13) 0.0353(5) Uani 1 1 d . . . H30 H 0.2863 0.6839 0.3434 0.042 Uiso 1 1 calc R . . C31 C 0.2181(2) 0.55544(17) 0.32756(11) 0.0293(5) Uani 1 1 d . . . C32 C 0.1065(2) 0.59947(17) 0.35993(11) 0.0308(5) Uani 1 1 d . . . H32 H 0.0892 0.6690 0.3795 0.037 Uiso 1 1 calc R . . C33 C 0.02223(19) 0.54318(17) 0.36368(11) 0.0287(5) Uani 1 1 d . . . C34 C 0.05058(19) 0.44270(17) 0.32962(11) 0.0280(5) Uani 1 1 d . . . H34 H -0.0078 0.4056 0.3297 0.034 Uiso 1 1 calc R . . C35 C 0.15775(18) 0.39530(16) 0.29635(11) 0.0251(4) Uani 1 1 d . . . C36 C 0.24606(18) 0.45021(16) 0.29935(11) 0.0263(4) Uani 1 1 d . . . C37 C 0.5632(2) 0.43573(19) 0.22097(12) 0.0335(5) Uani 1 1 d . . . H37 H 0.5713 0.3633 0.2010 0.040 Uiso 1 1 calc R . . C38 C 0.6494(2) 0.4305(2) 0.26437(14) 0.0452(6) Uani 1 1 d . . . H381 H 0.6440 0.5011 0.2838 0.068 Uiso 1 1 calc R . . H382 H 0.7241 0.4076 0.2342 0.068 Uiso 1 1 calc R . . H383 H 0.6351 0.3795 0.3028 0.068 Uiso 1 1 calc R . . C39 C 0.5884(3) 0.5134(2) 0.15902(14) 0.0474(7) Uani 1 1 d . . . H391 H 0.5335 0.5170 0.1311 0.071 Uiso 1 1 calc R . . H392 H 0.6630 0.4882 0.1293 0.071 Uiso 1 1 calc R . . H393 H 0.5846 0.5844 0.1773 0.071 Uiso 1 1 calc R . . C40 C -0.09898(19) 0.58592(17) 0.40033(11) 0.0291(5) Uani 1 1 d . . . C41 C -0.1716(2) 0.60013(18) 0.34654(12) 0.0334(5) Uani 1 1 d . . . H411 H -0.1453 0.6516 0.3100 0.040 Uiso 1 1 calc R . . H412 H -0.1641 0.5312 0.3232 0.040 Uiso 1 1 calc R . . C42 C -0.2944(2) 0.64048(19) 0.38292(13) 0.0356(5) Uani 1 1 d . . . H42 H -0.3397 0.6492 0.3473 0.043 Uiso 1 1 calc R . . C43 C -0.3057(2) 0.74796(18) 0.41804(13) 0.0369(5) Uani 1 1 d . . . H431 H -0.2789 0.8002 0.3822 0.044 Uiso 1 1 calc R . . H432 H -0.3848 0.7753 0.4408 0.044 Uiso 1 1 calc R . . C44 C -0.2373(2) 0.73411(18) 0.47314(12) 0.0352(5) Uani 1 1 d . . . H44 H -0.2451 0.8043 0.4961 0.042 Uiso 1 1 calc R . . C45 C -0.1148(2) 0.69439(17) 0.43670(12) 0.0327(5) Uani 1 1 d . . . H451 H -0.0698 0.6870 0.4719 0.039 Uiso 1 1 calc R . . H452 H -0.0882 0.7472 0.4013 0.039 Uiso 1 1 calc R . . C46 C -0.3351(2) 0.55939(19) 0.43863(14) 0.0393(6) Uani 1 1 d . . . H461 H -0.4145 0.5843 0.4620 0.047 Uiso 1 1 calc R . . H462 H -0.3280 0.4900 0.4159 0.047 Uiso 1 1 calc R . . C47 C -0.2659(2) 0.54615(18) 0.49326(13) 0.0364(5) Uani 1 1 d . . . H47 H -0.2925 0.4932 0.5295 0.044 Uiso 1 1 calc R . . C48 C -0.2788(2) 0.65394(18) 0.52886(12) 0.0377(6) Uani 1 1 d . . . H481 H -0.3578 0.6797 0.5525 0.045 Uiso 1 1 calc R . . H482 H -0.2351 0.6458 0.5648 0.045 Uiso 1 1 calc R . . C49 C -0.1437(2) 0.50729(17) 0.45744(12) 0.0323(5) Uani 1 1 d . . . H491 H -0.1349 0.4368 0.4357 0.039 Uiso 1 1 calc R . . H492 H -0.0995 0.4988 0.4931 0.039 Uiso 1 1 calc R . . C50 C 0.37670(19) 0.30017(19) 0.09765(12) 0.0316(5) Uani 1 1 d . . . H50 H 0.4038 0.3389 0.1310 0.038 Uiso 1 1 calc R . . C51 C 0.43924(19) 0.18511(19) 0.09670(12) 0.0337(5) Uani 1 1 d . . . H511 H 0.4134 0.1516 0.1428 0.040 Uiso 1 1 calc R . . H512 H 0.4225 0.1443 0.0603 0.040 Uiso 1 1 calc R . . C52 C 0.5642(2) 0.1806(2) 0.08141(13) 0.0383(6) Uani 1 1 d . . . H521 H 0.6025 0.1056 0.0814 0.046 Uiso 1 1 calc R . . H522 H 0.5815 0.2191 0.1187 0.046 Uiso 1 1 calc R . . C53 C 0.6062(2) 0.2310(2) 0.01017(13) 0.0428(6) Uani 1 1 d . . . H531 H 0.5970 0.1873 -0.0276 0.051 Uiso 1 1 calc R . . H532 H 0.6863 0.2324 0.0025 0.051 Uiso 1 1 calc R . . C54 C 0.5422(2) 0.3443(2) 0.00657(14) 0.0440(6) Uani 1 1 d . . . H541 H 0.5661 0.3723 -0.0415 0.053 Uiso 1 1 calc R . . H542 H 0.5610 0.3901 0.0394 0.053 Uiso 1 1 calc R . . C55 C 0.4159(2) 0.3506(2) 0.02519(12) 0.0387(6) Uani 1 1 d . . . H551 H 0.3953 0.3128 -0.0110 0.046 Uiso 1 1 calc R . . H552 H 0.3784 0.4260 0.0258 0.046 Uiso 1 1 calc R . . C56 C 0.1728(2) 0.2185(2) 0.08644(12) 0.0352(5) Uani 1 1 d . . . H56 H 0.0902 0.2414 0.0993 0.042 Uiso 1 1 calc R . . C57 C 0.1931(2) 0.1026(2) 0.11252(14) 0.0419(6) Uani 1 1 d . . . H571 H 0.2736 0.0725 0.0987 0.050 Uiso 1 1 calc R . . H572 H 0.1684 0.1012 0.1645 0.050 Uiso 1 1 calc R . . C58 C 0.1294(3) 0.0351(3) 0.08108(18) 0.0604(8) Uani 1 1 d . . . H581 H 0.1460 -0.0396 0.0966 0.072 Uiso 1 1 calc R . . H582 H 0.0486 0.0614 0.0987 0.072 Uiso 1 1 calc R . . C59 C 0.1599(3) 0.0390(3) 0.0016(2) 0.0763(11) Uani 1 1 d . . . H591 H 0.1136 -0.0018 -0.0167 0.092 Uiso 1 1 calc R . . H592 H 0.2388 0.0052 -0.0164 0.092 Uiso 1 1 calc R . . C60 C 0.1423(3) 0.1529(3) -0.02465(16) 0.0685(10) Uani 1 1 d . . . H601 H 0.0620 0.1837 -0.0115 0.082 Uiso 1 1 calc R . . H602 H 0.1676 0.1531 -0.0766 0.082 Uiso 1 1 calc R . . C61 C 0.2059(2) 0.2221(3) 0.00603(13) 0.0512(7) Uani 1 1 d . . . H611 H 0.2868 0.1960 -0.0110 0.061 Uiso 1 1 calc R . . H612 H 0.1891 0.2965 -0.0100 0.061 Uiso 1 1 calc R . . C62 C 0.1650(2) 0.44501(19) 0.10934(13) 0.0372(5) Uani 1 1 d . . . H62 H 0.1892 0.4484 0.0569 0.045 Uiso 1 1 calc R . . C63 C 0.0377(2) 0.4686(2) 0.13000(17) 0.0536(7) Uani 1 1 d . . . H631 H 0.0111 0.4631 0.1817 0.064 Uiso 1 1 calc R . . H632 H 0.0092 0.4150 0.1082 0.064 Uiso 1 1 calc R . . C64 C -0.0079(3) 0.5804(3) 0.1062(2) 0.0728(10) Uani 1 1 d . . . H641 H 0.0113 0.5831 0.0542 0.087 Uiso 1 1 calc R . . H642 H -0.0900 0.5950 0.1229 0.087 Uiso 1 1 calc R . . C65 C 0.0389(3) 0.6651(3) 0.1342(2) 0.0709(10) Uani 1 1 d . . . H651 H 0.0127 0.6678 0.1861 0.085 Uiso 1 1 calc R . . H652 H 0.0110 0.7354 0.1156 0.085 Uiso 1 1 calc R . . C66 C 0.1658(3) 0.6431(2) 0.11334(16) 0.0539(7) Uani 1 1 d . . . H661 H 0.1940 0.6978 0.1343 0.065 Uiso 1 1 calc R . . H662 H 0.1924 0.6469 0.0616 0.065 Uiso 1 1 calc R . . C67 C 0.2103(2) 0.53222(19) 0.13902(14) 0.0426(6) Uani 1 1 d . . . H671 H 0.1882 0.5305 0.1910 0.051 Uiso 1 1 calc R . . H672 H 0.2926 0.5178 0.1241 0.051 Uiso 1 1 calc R . . 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 0.02796(10) 0.01951(9) 0.02390(10) -0.00101(6) -0.00861(7) -0.00491(6) P1 0.0332(3) 0.0278(3) 0.0233(3) 0.0012(2) -0.0092(2) -0.0021(2) Cl1 0.0310(3) 0.0410(3) 0.0303(3) 0.0013(2) -0.0111(2) -0.0093(2) N1 0.0264(9) 0.0189(8) 0.0266(9) 0.0018(7) -0.0091(7) -0.0072(7) N2 0.0293(9) 0.0193(8) 0.0252(9) 0.0037(7) -0.0094(7) -0.0064(7) C1 0.0300(11) 0.0194(10) 0.0259(10) 0.0037(8) -0.0125(9) -0.0076(8) C2 0.0310(11) 0.0223(10) 0.0250(10) 0.0012(8) -0.0088(9) -0.0067(9) C3 0.0337(12) 0.0214(10) 0.0316(11) -0.0036(9) -0.0077(9) -0.0038(9) C4 0.0332(12) 0.0229(10) 0.0317(11) -0.0018(9) -0.0109(9) -0.0087(9) C5 0.0301(11) 0.0195(10) 0.0258(10) 0.0019(8) -0.0100(9) -0.0059(8) C6 0.0292(11) 0.0205(10) 0.0306(11) 0.0026(8) -0.0120(9) -0.0091(8) C7 0.0289(11) 0.0220(10) 0.0245(10) 0.0036(8) -0.0104(9) -0.0062(8) C8 0.0339(11) 0.0203(10) 0.0235(10) 0.0005(8) -0.0101(9) -0.0099(8) C9 0.0304(11) 0.0207(10) 0.0230(10) -0.0014(8) -0.0075(8) -0.0044(8) C10 0.0299(11) 0.0173(9) 0.0239(10) 0.0035(8) -0.0116(8) -0.0050(8) C11 0.0314(12) 0.0247(11) 0.0356(12) -0.0033(9) -0.0045(10) -0.0061(9) C12 0.0359(13) 0.0317(13) 0.0631(17) 0.0026(12) -0.0155(12) -0.0015(10) C13 0.0454(15) 0.0459(15) 0.0445(15) -0.0137(12) 0.0036(12) -0.0105(12) C14 0.0275(11) 0.0225(10) 0.0269(10) 0.0013(8) -0.0100(9) -0.0057(8) C15 0.0327(12) 0.0236(11) 0.0302(11) 0.0035(9) -0.0088(9) -0.0046(9) C16 0.0312(12) 0.0230(10) 0.0335(12) 0.0026(9) -0.0101(9) 0.0005(9) C17 0.0338(12) 0.0224(11) 0.0352(12) -0.0044(9) -0.0080(10) -0.0045(9) C18 0.0335(12) 0.0282(11) 0.0241(10) 0.0000(9) -0.0068(9) -0.0055(9) C19 0.0326(12) 0.0287(11) 0.0276(11) 0.0015(9) -0.0110(9) -0.0064(9) C20 0.0275(11) 0.0350(12) 0.0324(12) -0.0050(10) -0.0105(9) -0.0020(9) C21 0.0280(11) 0.0246(11) 0.0353(12) -0.0035(9) -0.0064(9) -0.0081(9) C22 0.0322(12) 0.0255(11) 0.0324(12) 0.0055(9) -0.0051(9) -0.0065(9) C23 0.0294(11) 0.0223(10) 0.0336(11) -0.0032(9) -0.0075(9) -0.0058(9) C24 0.0332(11) 0.0200(10) 0.0183(9) -0.0005(8) -0.0081(8) -0.0031(8) C25 0.0302(11) 0.0239(10) 0.0316(11) 0.0044(9) -0.0151(9) -0.0079(9) C26 0.0283(11) 0.0221(10) 0.0387(12) 0.0053(9) -0.0118(9) -0.0089(9) C27 0.0410(12) 0.0207(10) 0.0225(10) 0.0039(8) -0.0130(9) -0.0098(9) C28 0.0396(13) 0.0246(11) 0.0303(11) 0.0053(9) -0.0135(10) -0.0130(9) C29 0.0468(14) 0.0267(12) 0.0405(13) 0.0049(10) -0.0157(11) -0.0173(10) C30 0.0512(15) 0.0209(11) 0.0394(13) 0.0002(9) -0.0183(11) -0.0108(10) C31 0.0436(13) 0.0204(10) 0.0276(11) 0.0031(9) -0.0133(10) -0.0096(9) C32 0.0466(14) 0.0176(10) 0.0289(11) -0.0040(8) -0.0118(10) -0.0031(9) C33 0.0386(12) 0.0199(10) 0.0284(11) -0.0002(8) -0.0119(9) -0.0021(9) C34 0.0351(12) 0.0207(10) 0.0307(11) -0.0012(9) -0.0121(9) -0.0053(9) C35 0.0355(12) 0.0188(10) 0.0226(10) 0.0022(8) -0.0106(9) -0.0050(8) C36 0.0377(12) 0.0209(10) 0.0229(10) 0.0038(8) -0.0114(9) -0.0077(9) C37 0.0400(13) 0.0292(12) 0.0358(12) 0.0044(10) -0.0108(10) -0.0165(10) C38 0.0471(15) 0.0499(16) 0.0458(15) 0.0028(12) -0.0154(12) -0.0220(13) C39 0.0615(18) 0.0415(15) 0.0406(14) 0.0099(12) -0.0072(13) -0.0226(13) C40 0.0376(12) 0.0216(10) 0.0280(11) -0.0015(9) -0.0096(9) -0.0031(9) C41 0.0425(13) 0.0273(11) 0.0292(11) -0.0068(9) -0.0121(10) 0.0023(10) C42 0.0394(13) 0.0317(12) 0.0339(12) -0.0059(10) -0.0109(10) 0.0020(10) C43 0.0427(14) 0.0245(11) 0.0377(13) -0.0010(10) -0.0051(11) 0.0016(10) C44 0.0487(14) 0.0211(11) 0.0326(12) -0.0049(9) -0.0048(11) -0.0042(10) C45 0.0441(13) 0.0213(11) 0.0319(12) -0.0038(9) -0.0075(10) -0.0053(9) C46 0.0396(14) 0.0284(12) 0.0482(14) -0.0069(11) -0.0080(11) -0.0047(10) C47 0.0480(14) 0.0239(11) 0.0339(12) 0.0016(9) -0.0041(11) -0.0068(10) C48 0.0492(15) 0.0280(12) 0.0317(12) -0.0026(10) -0.0026(11) -0.0060(11) C49 0.0435(13) 0.0210(11) 0.0326(12) 0.0001(9) -0.0100(10) -0.0055(9) C50 0.0335(12) 0.0341(12) 0.0259(11) 0.0026(9) -0.0073(9) -0.0039(10) C51 0.0375(13) 0.0343(12) 0.0279(11) 0.0001(10) -0.0073(10) -0.0042(10) C52 0.0380(13) 0.0417(14) 0.0335(12) -0.0019(11) -0.0084(10) -0.0034(11) C53 0.0379(14) 0.0537(16) 0.0348(13) -0.0010(12) -0.0054(11) -0.0079(12) C54 0.0457(15) 0.0511(16) 0.0330(13) 0.0084(12) -0.0039(11) -0.0130(12) C55 0.0397(14) 0.0430(14) 0.0307(12) 0.0082(11) -0.0059(10) -0.0061(11) C56 0.0381(13) 0.0400(13) 0.0285(11) -0.0042(10) -0.0133(10) -0.0016(10) C57 0.0431(14) 0.0377(14) 0.0465(15) -0.0066(11) -0.0146(12) -0.0054(11) C58 0.0572(18) 0.0508(18) 0.078(2) -0.0219(16) -0.0214(16) -0.0111(14) C59 0.067(2) 0.088(3) 0.079(2) -0.045(2) -0.0214(19) -0.0122(19) C60 0.061(2) 0.106(3) 0.0428(16) -0.0255(18) -0.0212(15) -0.0089(19) C61 0.0522(17) 0.071(2) 0.0307(13) -0.0103(13) -0.0142(12) -0.0039(14) C62 0.0440(14) 0.0345(13) 0.0298(12) 0.0071(10) -0.0097(10) 0.0001(11) C63 0.0444(16) 0.0448(16) 0.0685(19) 0.0173(14) -0.0189(14) 0.0018(12) C64 0.0525(19) 0.058(2) 0.098(3) 0.0282(19) -0.0217(18) 0.0103(16) C65 0.072(2) 0.0423(17) 0.082(2) 0.0167(16) -0.0090(19) 0.0135(16) C66 0.073(2) 0.0343(14) 0.0477(16) 0.0118(12) -0.0108(15) -0.0012(14) C67 0.0549(16) 0.0305(13) 0.0389(14) 0.0083(11) -0.0122(12) 0.0000(11) _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 C24 1.922(2) . ? Ru1 C35 2.006(2) . ? Ru1 P1 2.2439(6) . ? Ru1 Cl1 2.4780(6) . ? P1 C62 1.857(2) . ? P1 C56 1.864(2) . ? P1 C50 1.866(2) . ? N1 C24 1.377(3) . ? N1 C1 1.425(3) . ? N1 C25 1.465(3) . ? N2 C24 1.365(3) . ? N2 C27 1.426(3) . ? N2 C26 1.481(3) . ? C1 C2 1.384(3) . ? C1 C10 1.426(3) . ? C2 C3 1.420(3) . ? C2 C11 1.522(3) . ? C3 C4 1.365(3) . ? C3 H3 0.9500 . ? C4 C5 1.425(3) . ? C4 H4 0.9500 . ? C5 C6 1.411(3) . ? C5 C10 1.421(3) . ? C6 C7 1.378(3) . ? C6 H6 0.9500 . ? C7 C9 1.420(3) . ? C7 C14 1.518(3) . ? C8 C9 1.368(3) . ? C8 C10 1.429(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C11 C13 1.531(3) . ? C11 C12 1.532(3) . ? C11 H11 1.0000 . ? C12 H121 0.9800 . ? C12 H122 0.9800 . ? C12 H123 0.9800 . ? C13 H131 0.9800 . ? C13 H132 0.9800 . ? C13 H133 0.9800 . ? C14 C23 1.535(3) . ? C14 C15 1.549(3) . ? C14 C19 1.552(3) . ? C15 C16 1.533(3) . ? C15 H151 0.9900 . ? C15 H152 0.9900 . ? C16 C20 1.526(3) . ? C16 C17 1.531(3) . ? C16 H16 1.0000 . ? C17 C18 1.533(3) . ? C17 H171 0.9900 . ? C17 H172 0.9900 . ? C18 C22 1.529(3) . ? C18 C19 1.535(3) . ? C18 H18 1.0000 . ? C19 H191 0.9900 . ? C19 H192 0.9900 . ? C20 C21 1.532(3) . ? C20 H201 0.9900 . ? C20 H202 0.9900 . ? C21 C22 1.528(3) . ? C21 C23 1.532(3) . ? C21 H21 1.0000 . ? C22 H221 0.9900 . ? C22 H222 0.9900 . ? C23 H231 0.9900 . ? C23 H232 0.9900 . ? C25 C26 1.527(3) . ? C25 H251 0.9900 . ? C25 H252 0.9900 . ? C26 H261 0.9900 . ? C26 H262 0.9900 . ? C27 C28 1.392(3) . ? C27 C36 1.436(3) . ? C28 C29 1.419(3) . ? C28 C37 1.523(3) . ? C29 C30 1.355(3) . ? C29 H29 0.9500 . ? C30 C31 1.421(3) . ? C30 H30 0.9500 . ? C31 C32 1.411(3) . ? C31 C36 1.426(3) . ? C32 C33 1.380(3) . ? C32 H32 0.9500 . ? C33 C34 1.418(3) . ? C33 C40 1.527(3) . ? C34 C35 1.383(3) . ? C34 H34 0.9500 . ? C35 C36 1.440(3) . ? C37 C38 1.533(3) . ? C37 C39 1.545(3) . ? C37 H37 1.0000 . ? C38 H381 0.9800 . ? C38 H382 0.9800 . ? C38 H383 0.9800 . ? C39 H391 0.9800 . ? C39 H392 0.9800 . ? C39 H393 0.9800 . ? C40 C49 1.544(3) . ? C40 C45 1.546(3) . ? C40 C41 1.548(3) . ? C41 C42 1.536(3) . ? C41 H411 0.9900 . ? C41 H412 0.9900 . ? C42 C43 1.532(3) . ? C42 C46 1.535(4) . ? C42 H42 1.0000 . ? C43 C44 1.531(3) . ? C43 H431 0.9900 . ? C43 H432 0.9900 . ? C44 C48 1.529(3) . ? C44 C45 1.532(3) . ? C44 H44 1.0000 . ? C45 H451 0.9900 . ? C45 H452 0.9900 . ? C46 C47 1.531(4) . ? C46 H461 0.9900 . ? C46 H462 0.9900 . ? C47 C49 1.525(3) . ? C47 C48 1.537(3) . ? C47 H47 1.0000 . ? C48 H481 0.9900 . ? C48 H482 0.9900 . ? C49 H491 0.9900 . ? C49 H492 0.9900 . ? C50 C51 1.532(3) . ? C50 C55 1.540(3) . ? C50 H50 1.0000 . ? C51 C52 1.522(3) . ? C51 H511 0.9900 . ? C51 H512 0.9900 . ? C52 C53 1.526(4) . ? C52 H521 0.9900 . ? C52 H522 0.9900 . ? C53 C54 1.529(4) . ? C53 H531 0.9900 . ? C53 H532 0.9900 . ? C54 C55 1.532(4) . ? C54 H541 0.9900 . ? C54 H542 0.9900 . ? C55 H551 0.9900 . ? C55 H552 0.9900 . ? C56 C61 1.530(3) . ? C56 C57 1.543(4) . ? C56 H56 1.0000 . ? C57 C58 1.528(4) . ? C57 H571 0.9900 . ? C57 H572 0.9900 . ? C58 C59 1.513(5) . ? C58 H581 0.9900 . ? C58 H582 0.9900 . ? C59 C60 1.518(6) . ? C59 H591 0.9900 . ? C59 H592 0.9900 . ? C60 C61 1.533(4) . ? C60 H601 0.9900 . ? C60 H602 0.9900 . ? C61 H611 0.9900 . ? C61 H612 0.9900 . ? C62 C63 1.531(4) . ? C62 C67 1.543(4) . ? C62 H62 1.0000 . ? C63 C64 1.535(4) . ? C63 H631 0.9900 . ? C63 H632 0.9900 . ? C64 C65 1.512(5) . ? C64 H641 0.9900 . ? C64 H642 0.9900 . ? C65 C66 1.527(5) . ? C65 H651 0.9900 . ? C65 H652 0.9900 . ? C66 C67 1.536(3) . ? C66 H661 0.9900 . ? C66 H662 0.9900 . ? C67 H671 0.9900 . ? C67 H672 0.9900 . ? 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 C24 Ru1 C35 84.58(8) . . ? C24 Ru1 P1 94.75(6) . . ? C35 Ru1 P1 98.65(6) . . ? C24 Ru1 Cl1 166.77(6) . . ? C35 Ru1 Cl1 104.11(6) . . ? P1 Ru1 Cl1 93.78(2) . . ? C62 P1 C56 103.92(11) . . ? C62 P1 C50 103.13(11) . . ? C56 P1 C50 107.91(11) . . ? C62 P1 Ru1 120.36(8) . . ? C56 P1 Ru1 103.43(8) . . ? C50 P1 Ru1 116.92(7) . . ? C24 N1 C1 119.02(17) . . ? C24 N1 C25 112.34(16) . . ? C1 N1 C25 125.45(17) . . ? C24 N2 C27 123.54(17) . . ? C24 N2 C26 111.97(16) . . ? C27 N2 C26 120.20(17) . . ? C2 C1 N1 120.76(19) . . ? C2 C1 C10 121.78(18) . . ? N1 C1 C10 117.35(17) . . ? C1 C2 C3 117.75(19) . . ? C1 C2 C11 122.10(19) . . ? C3 C2 C11 120.14(18) . . ? C4 C3 C2 122.14(19) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 120.63(19) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C10 119.42(18) . . ? C6 C5 C4 122.14(19) . . ? C10 C5 C4 118.41(19) . . ? C7 C6 C5 122.85(19) . . ? C7 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? C6 C7 C9 116.94(19) . . ? C6 C7 C14 123.11(18) . . ? C9 C7 C14 119.95(18) . . ? C9 C8 C10 120.73(19) . . ? C9 C8 H8 119.6 . . ? C10 C8 H8 119.6 . . ? C8 C9 C7 122.33(18) . . ? C8 C9 H9 118.8 . . ? C7 C9 H9 118.8 . . ? C5 C10 C1 119.05(18) . . ? C5 C10 C8 117.63(19) . . ? C1 C10 C8 123.28(18) . . ? C2 C11 C13 112.91(19) . . ? C2 C11 C12 110.13(19) . . ? C13 C11 C12 110.5(2) . . ? C2 C11 H11 107.7 . . ? C13 C11 H11 107.7 . . ? C12 C11 H11 107.7 . . ? C11 C12 H121 109.5 . . ? C11 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? C11 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? C11 C13 H131 109.5 . . ? C11 C13 H132 109.5 . . ? H131 C13 H132 109.5 . . ? C11 C13 H133 109.5 . . ? H131 C13 H133 109.5 . . ? H132 C13 H133 109.5 . . ? C7 C14 C23 112.28(17) . . ? C7 C14 C15 110.20(17) . . ? C23 C14 C15 108.29(17) . . ? C7 C14 C19 110.21(17) . . ? C23 C14 C19 107.42(18) . . ? C15 C14 C19 108.31(17) . . ? C16 C15 C14 110.60(18) . . ? C16 C15 H151 109.5 . . ? C14 C15 H151 109.5 . . ? C16 C15 H152 109.5 . . ? C14 C15 H152 109.5 . . ? H151 C15 H152 108.1 . . ? C20 C16 C17 110.15(19) . . ? C20 C16 C15 108.98(18) . . ? C17 C16 C15 109.55(18) . . ? C20 C16 H16 109.4 . . ? C17 C16 H16 109.4 . . ? C15 C16 H16 109.4 . . ? C16 C17 C18 109.48(17) . . ? C16 C17 H171 109.8 . . ? C18 C17 H171 109.8 . . ? C16 C17 H172 109.8 . . ? C18 C17 H172 109.8 . . ? H171 C17 H172 108.2 . . ? C22 C18 C17 109.10(18) . . ? C22 C18 C19 109.84(18) . . ? C17 C18 C19 109.52(18) . . ? C22 C18 H18 109.5 . . ? C17 C18 H18 109.5 . . ? C19 C18 H18 109.5 . . ? C18 C19 C14 110.69(17) . . ? C18 C19 H191 109.5 . . ? C14 C19 H191 109.5 . . ? C18 C19 H192 109.5 . . ? C14 C19 H192 109.5 . . ? H191 C19 H192 108.1 . . ? C16 C20 C21 109.42(17) . . ? C16 C20 H201 109.8 . . ? C21 C20 H201 109.8 . . ? C16 C20 H202 109.8 . . ? C21 C20 H202 109.8 . . ? H201 C20 H202 108.2 . . ? C22 C21 C20 109.75(17) . . ? C22 C21 C23 109.84(18) . . ? C20 C21 C23 108.92(18) . . ? C22 C21 H21 109.4 . . ? C20 C21 H21 109.4 . . ? C23 C21 H21 109.4 . . ? C21 C22 C18 109.31(18) . . ? C21 C22 H221 109.8 . . ? C18 C22 H221 109.8 . . ? C21 C22 H222 109.8 . . ? C18 C22 H222 109.8 . . ? H221 C22 H222 108.3 . . ? C21 C23 C14 111.18(17) . . ? C21 C23 H231 109.4 . . ? C14 C23 H231 109.4 . . ? C21 C23 H232 109.4 . . ? C14 C23 H232 109.4 . . ? H231 C23 H232 108.0 . . ? N2 C24 N1 106.24(17) . . ? N2 C24 Ru1 132.72(15) . . ? N1 C24 Ru1 120.61(15) . . ? N1 C25 C26 100.76(16) . . ? N1 C25 H251 111.6 . . ? C26 C25 H251 111.6 . . ? N1 C25 H252 111.6 . . ? C26 C25 H252 111.6 . . ? H251 C25 H252 109.4 . . ? N2 C26 C25 102.88(16) . . ? N2 C26 H261 111.2 . . ? C25 C26 H261 111.2 . . ? N2 C26 H262 111.2 . . ? C25 C26 H262 111.2 . . ? H261 C26 H262 109.1 . . ? C28 C27 N2 120.2(2) . . ? C28 C27 C36 121.79(19) . . ? N2 C27 C36 117.76(18) . . ? C27 C28 C29 117.3(2) . . ? C27 C28 C37 125.2(2) . . ? C29 C28 C37 117.4(2) . . ? C30 C29 C28 122.4(2) . . ? C30 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C29 C30 C31 120.6(2) . . ? C29 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 120.5(2) . . ? C32 C31 C36 120.3(2) . . ? C30 C31 C36 119.2(2) . . ? C33 C32 C31 121.12(19) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 117.6(2) . . ? C32 C33 C40 122.99(19) . . ? C34 C33 C40 119.4(2) . . ? C35 C34 C33 124.2(2) . . ? C35 C34 H34 117.9 . . ? C33 C34 H34 117.9 . . ? C34 C35 C36 117.31(18) . . ? C34 C35 Ru1 115.49(15) . . ? C36 C35 Ru1 127.20(16) . . ? C31 C36 C27 117.47(19) . . ? C31 C36 C35 118.8(2) . . ? C27 C36 C35 123.69(18) . . ? C28 C37 C38 114.0(2) . . ? C28 C37 C39 109.5(2) . . ? C38 C37 C39 109.3(2) . . ? C28 C37 H37 108.0 . . ? C38 C37 H37 108.0 . . ? C39 C37 H37 108.0 . . ? C37 C38 H381 109.5 . . ? C37 C38 H382 109.5 . . ? H381 C38 H382 109.5 . . ? C37 C38 H383 109.5 . . ? H381 C38 H383 109.5 . . ? H382 C38 H383 109.5 . . ? C37 C39 H391 109.5 . . ? C37 C39 H392 109.5 . . ? H391 C39 H392 109.5 . . ? C37 C39 H393 109.5 . . ? H391 C39 H393 109.5 . . ? H392 C39 H393 109.5 . . ? C33 C40 C49 110.32(18) . . ? C33 C40 C45 112.70(19) . . ? C49 C40 C45 107.30(18) . . ? C33 C40 C41 110.20(18) . . ? C49 C40 C41 108.18(19) . . ? C45 C40 C41 107.97(18) . . ? C42 C41 C40 110.86(18) . . ? C42 C41 H411 109.5 . . ? C40 C41 H411 109.5 . . ? C42 C41 H412 109.5 . . ? C40 C41 H412 109.5 . . ? H411 C41 H412 108.1 . . ? C43 C42 C46 109.75(19) . . ? C43 C42 C41 109.2(2) . . ? C46 C42 C41 109.17(19) . . ? C43 C42 H42 109.6 . . ? C46 C42 H42 109.6 . . ? C41 C42 H42 109.6 . . ? C44 C43 C42 109.46(19) . . ? C44 C43 H431 109.8 . . ? C42 C43 H431 109.8 . . ? C44 C43 H432 109.8 . . ? C42 C43 H432 109.8 . . ? H431 C43 H432 108.2 . . ? C48 C44 C43 110.0(2) . . ? C48 C44 C45 109.89(19) . . ? C43 C44 C45 109.00(19) . . ? C48 C44 H44 109.3 . . ? C43 C44 H44 109.3 . . ? C45 C44 H44 109.3 . . ? C44 C45 C40 111.05(19) . . ? C44 C45 H451 109.4 . . ? C40 C45 H451 109.4 . . ? C44 C45 H452 109.4 . . ? C40 C45 H452 109.4 . . ? H451 C45 H452 108.0 . . ? C47 C46 C42 109.6(2) . . ? C47 C46 H461 109.8 . . ? C42 C46 H461 109.8 . . ? C47 C46 H462 109.8 . . ? C42 C46 H462 109.8 . . ? H461 C46 H462 108.2 . . ? C49 C47 C46 109.8(2) . . ? C49 C47 C48 109.2(2) . . ? C46 C47 C48 109.3(2) . . ? C49 C47 H47 109.5 . . ? C46 C47 H47 109.5 . . ? C48 C47 H47 109.5 . . ? C44 C48 C47 109.07(19) . . ? C44 C48 H481 109.9 . . ? C47 C48 H481 109.9 . . ? C44 C48 H482 109.9 . . ? C47 C48 H482 109.9 . . ? H481 C48 H482 108.3 . . ? C47 C49 C40 111.48(19) . . ? C47 C49 H491 109.3 . . ? C40 C49 H491 109.3 . . ? C47 C49 H492 109.3 . . ? C40 C49 H492 109.3 . . ? H491 C49 H492 108.0 . . ? C51 C50 C55 108.84(19) . . ? C51 C50 P1 111.80(16) . . ? C55 C50 P1 118.74(16) . . ? C51 C50 H50 105.5 . . ? C55 C50 H50 105.5 . . ? P1 C50 H50 105.5 . . ? C52 C51 C50 111.2(2) . . ? C52 C51 H511 109.4 . . ? C50 C51 H511 109.4 . . ? C52 C51 H512 109.4 . . ? C50 C51 H512 109.4 . . ? H511 C51 H512 108.0 . . ? C51 C52 C53 110.3(2) . . ? C51 C52 H521 109.6 . . ? C53 C52 H521 109.6 . . ? C51 C52 H522 109.6 . . ? C53 C52 H522 109.6 . . ? H521 C52 H522 108.1 . . ? C52 C53 C54 110.8(2) . . ? C52 C53 H531 109.5 . . ? C54 C53 H531 109.5 . . ? C52 C53 H532 109.5 . . ? C54 C53 H532 109.5 . . ? H531 C53 H532 108.1 . . ? C53 C54 C55 112.9(2) . . ? C53 C54 H541 109.0 . . ? C55 C54 H541 109.0 . . ? C53 C54 H542 109.0 . . ? C55 C54 H542 109.0 . . ? H541 C54 H542 107.8 . . ? C54 C55 C50 110.5(2) . . ? C54 C55 H551 109.6 . . ? C50 C55 H551 109.6 . . ? C54 C55 H552 109.6 . . ? C50 C55 H552 109.6 . . ? H551 C55 H552 108.1 . . ? C61 C56 C57 110.4(2) . . ? C61 C56 P1 118.6(2) . . ? C57 C56 P1 112.18(16) . . ? C61 C56 H56 104.7 . . ? C57 C56 H56 104.7 . . ? P1 C56 H56 104.7 . . ? C58 C57 C56 110.3(2) . . ? C58 C57 H571 109.6 . . ? C56 C57 H571 109.6 . . ? C58 C57 H572 109.6 . . ? C56 C57 H572 109.6 . . ? H571 C57 H572 108.1 . . ? C59 C58 C57 111.8(3) . . ? C59 C58 H581 109.3 . . ? C57 C58 H581 109.3 . . ? C59 C58 H582 109.3 . . ? C57 C58 H582 109.3 . . ? H581 C58 H582 107.9 . . ? C58 C59 C60 111.1(3) . . ? C58 C59 H591 109.4 . . ? C60 C59 H591 109.4 . . ? C58 C59 H592 109.4 . . ? C60 C59 H592 109.4 . . ? H591 C59 H592 108.0 . . ? C59 C60 C61 111.8(3) . . ? C59 C60 H601 109.2 . . ? C61 C60 H601 109.2 . . ? C59 C60 H602 109.2 . . ? C61 C60 H602 109.2 . . ? H601 C60 H602 107.9 . . ? C56 C61 C60 110.4(3) . . ? C56 C61 H611 109.6 . . ? C60 C61 H611 109.6 . . ? C56 C61 H612 109.6 . . ? C60 C61 H612 109.6 . . ? H611 C61 H612 108.1 . . ? C63 C62 C67 109.8(2) . . ? C63 C62 P1 112.97(18) . . ? C67 C62 P1 111.38(16) . . ? C63 C62 H62 107.5 . . ? C67 C62 H62 107.5 . . ? P1 C62 H62 107.5 . . ? C62 C63 C64 111.2(2) . . ? C62 C63 H631 109.4 . . ? C64 C63 H631 109.4 . . ? C62 C63 H632 109.4 . . ? C64 C63 H632 109.4 . . ? H631 C63 H632 108.0 . . ? C65 C64 C63 111.7(3) . . ? C65 C64 H641 109.3 . . ? C63 C64 H641 109.3 . . ? C65 C64 H642 109.3 . . ? C63 C64 H642 109.3 . . ? H641 C64 H642 107.9 . . ? C64 C65 C66 111.5(3) . . ? C64 C65 H651 109.3 . . ? C66 C65 H651 109.3 . . ? C64 C65 H652 109.3 . . ? C66 C65 H652 109.3 . . ? H651 C65 H652 108.0 . . ? C65 C66 C67 110.0(2) . . ? C65 C66 H661 109.7 . . ? C67 C66 H661 109.7 . . ? C65 C66 H662 109.7 . . ? C67 C66 H662 109.7 . . ? H661 C66 H662 108.2 . . ? C66 C67 C62 111.2(2) . . ? C66 C67 H671 109.4 . . ? C62 C67 H671 109.4 . . ? C66 C67 H672 109.4 . . ? C62 C67 H672 109.4 . . ? H671 C67 H672 108.0 . . ? 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 C24 Ru1 P1 C62 -122.12(11) . . . . ? C35 Ru1 P1 C62 -36.89(12) . . . . ? Cl1 Ru1 P1 C62 68.01(10) . . . . ? C24 Ru1 P1 C56 122.63(10) . . . . ? C35 Ru1 P1 C56 -152.14(10) . . . . ? Cl1 Ru1 P1 C56 -47.24(8) . . . . ? C24 Ru1 P1 C50 4.23(10) . . . . ? C35 Ru1 P1 C50 89.45(11) . . . . ? Cl1 Ru1 P1 C50 -165.65(9) . . . . ? C24 N1 C1 C2 126.5(2) . . . . ? C25 N1 C1 C2 -75.3(3) . . . . ? C24 N1 C1 C10 -49.8(3) . . . . ? C25 N1 C1 C10 108.4(2) . . . . ? N1 C1 C2 C3 -172.90(18) . . . . ? C10 C1 C2 C3 3.3(3) . . . . ? N1 C1 C2 C11 8.2(3) . . . . ? C10 C1 C2 C11 -175.58(19) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? C11 C2 C3 C4 -179.9(2) . . . . ? C2 C3 C4 C5 -3.5(3) . . . . ? C3 C4 C5 C6 -176.5(2) . . . . ? C3 C4 C5 C10 1.5(3) . . . . ? C10 C5 C6 C7 -0.6(3) . . . . ? C4 C5 C6 C7 177.3(2) . . . . ? C5 C6 C7 C9 -1.6(3) . . . . ? C5 C6 C7 C14 179.09(19) . . . . ? C10 C8 C9 C7 1.3(3) . . . . ? C6 C7 C9 C8 1.3(3) . . . . ? C14 C7 C9 C8 -179.39(19) . . . . ? C6 C5 C10 C1 -179.18(19) . . . . ? C4 C5 C10 C1 2.8(3) . . . . ? C6 C5 C10 C8 3.1(3) . . . . ? C4 C5 C10 C8 -174.88(19) . . . . ? C2 C1 C10 C5 -5.3(3) . . . . ? N1 C1 C10 C5 171.03(18) . . . . ? C2 C1 C10 C8 172.3(2) . . . . ? N1 C1 C10 C8 -11.4(3) . . . . ? C9 C8 C10 C5 -3.5(3) . . . . ? C9 C8 C10 C1 178.94(19) . . . . ? C1 C2 C11 C13 -133.3(2) . . . . ? C3 C2 C11 C13 47.9(3) . . . . ? C1 C2 C11 C12 102.7(2) . . . . ? C3 C2 C11 C12 -76.2(3) . . . . ? C6 C7 C14 C23 2.7(3) . . . . ? C9 C7 C14 C23 -176.57(19) . . . . ? C6 C7 C14 C15 -118.1(2) . . . . ? C9 C7 C14 C15 62.6(2) . . . . ? C6 C7 C14 C19 122.5(2) . . . . ? C9 C7 C14 C19 -56.9(2) . . . . ? C7 C14 C15 C16 -178.83(17) . . . . ? C23 C14 C15 C16 58.0(2) . . . . ? C19 C14 C15 C16 -58.2(2) . . . . ? C14 C15 C16 C20 -60.4(2) . . . . ? C14 C15 C16 C17 60.2(2) . . . . ? C20 C16 C17 C18 59.4(2) . . . . ? C15 C16 C17 C18 -60.5(2) . . . . ? C16 C17 C18 C22 -60.0(2) . . . . ? C16 C17 C18 C19 60.2(2) . . . . ? C22 C18 C19 C14 60.1(2) . . . . ? C17 C18 C19 C14 -59.7(2) . . . . ? C7 C14 C19 C18 178.64(17) . . . . ? C23 C14 C19 C18 -58.7(2) . . . . ? C15 C14 C19 C18 58.0(2) . . . . ? C17 C16 C20 C21 -58.8(2) . . . . ? C15 C16 C20 C21 61.4(2) . . . . ? C16 C20 C21 C22 59.4(2) . . . . ? C16 C20 C21 C23 -60.9(2) . . . . ? C20 C21 C22 C18 -60.6(2) . . . . ? C23 C21 C22 C18 59.1(2) . . . . ? C17 C18 C22 C21 60.7(2) . . . . ? C19 C18 C22 C21 -59.3(2) . . . . ? C22 C21 C23 C14 -60.3(2) . . . . ? C20 C21 C23 C14 59.9(2) . . . . ? C7 C14 C23 C21 -179.81(18) . . . . ? C15 C14 C23 C21 -57.9(2) . . . . ? C19 C14 C23 C21 58.9(2) . . . . ? C27 N2 C24 N1 -158.95(18) . . . . ? C26 N2 C24 N1 -2.3(2) . . . . ? C27 N2 C24 Ru1 13.4(3) . . . . ? C26 N2 C24 Ru1 170.03(16) . . . . ? C1 N1 C24 N2 178.65(17) . . . . ? C25 N1 C24 N2 17.7(2) . . . . ? C1 N1 C24 Ru1 5.2(2) . . . . ? C25 N1 C24 Ru1 -155.75(14) . . . . ? C35 Ru1 C24 N2 -30.11(19) . . . . ? P1 Ru1 C24 N2 68.15(19) . . . . ? Cl1 Ru1 C24 N2 -161.89(15) . . . . ? C35 Ru1 C24 N1 141.34(16) . . . . ? P1 Ru1 C24 N1 -120.40(15) . . . . ? Cl1 Ru1 C24 N1 9.6(4) . . . . ? C24 N1 C25 C26 -24.6(2) . . . . ? C1 N1 C25 C26 175.92(19) . . . . ? C24 N2 C26 C25 -12.5(2) . . . . ? C27 N2 C26 C25 145.00(18) . . . . ? N1 C25 C26 N2 20.8(2) . . . . ? C24 N2 C27 C28 -166.97(19) . . . . ? C26 N2 C27 C28 38.2(3) . . . . ? C24 N2 C27 C36 18.8(3) . . . . ? C26 N2 C27 C36 -136.1(2) . . . . ? N2 C27 C28 C29 -163.17(19) . . . . ? C36 C27 C28 C29 10.9(3) . . . . ? N2 C27 C28 C37 21.1(3) . . . . ? C36 C27 C28 C37 -164.9(2) . . . . ? C27 C28 C29 C30 -1.6(3) . . . . ? C37 C28 C29 C30 174.5(2) . . . . ? C28 C29 C30 C31 -5.1(4) . . . . ? C29 C30 C31 C32 -177.7(2) . . . . ? C29 C30 C31 C36 2.7(3) . . . . ? C30 C31 C32 C33 178.9(2) . . . . ? C36 C31 C32 C33 -1.4(3) . . . . ? C31 C32 C33 C34 -4.3(3) . . . . ? C31 C32 C33 C40 177.9(2) . . . . ? C32 C33 C34 C35 3.7(3) . . . . ? C40 C33 C34 C35 -178.4(2) . . . . ? C33 C34 C35 C36 2.7(3) . . . . ? C33 C34 C35 Ru1 -176.80(17) . . . . ? C24 Ru1 C35 C34 -154.78(17) . . . . ? P1 Ru1 C35 C34 111.22(15) . . . . ? Cl1 Ru1 C35 C34 15.08(17) . . . . ? C24 Ru1 C35 C36 25.79(18) . . . . ? P1 Ru1 C35 C36 -68.21(18) . . . . ? Cl1 Ru1 C35 C36 -164.35(17) . . . . ? C32 C31 C36 C27 -173.57(19) . . . . ? C30 C31 C36 C27 6.1(3) . . . . ? C32 C31 C36 C35 7.9(3) . . . . ? C30 C31 C36 C35 -172.48(19) . . . . ? C28 C27 C36 C31 -13.1(3) . . . . ? N2 C27 C36 C31 161.09(18) . . . . ? C28 C27 C36 C35 165.4(2) . . . . ? N2 C27 C36 C35 -20.4(3) . . . . ? C34 C35 C36 C31 -8.3(3) . . . . ? Ru1 C35 C36 C31 171.09(15) . . . . ? C34 C35 C36 C27 173.22(19) . . . . ? Ru1 C35 C36 C27 -7.4(3) . . . . ? C27 C28 C37 C38 -117.4(2) . . . . ? C29 C28 C37 C38 66.8(3) . . . . ? C27 C28 C37 C39 119.8(2) . . . . ? C29 C28 C37 C39 -55.9(3) . . . . ? C32 C33 C40 C49 -123.9(2) . . . . ? C34 C33 C40 C49 58.3(3) . . . . ? C32 C33 C40 C45 -4.0(3) . . . . ? C34 C33 C40 C45 178.17(19) . . . . ? C32 C33 C40 C41 116.7(2) . . . . ? C34 C33 C40 C41 -61.1(3) . . . . ? C33 C40 C41 C42 178.58(19) . . . . ? C49 C40 C41 C42 57.9(2) . . . . ? C45 C40 C41 C42 -57.9(2) . . . . ? C40 C41 C42 C43 59.9(2) . . . . ? C40 C41 C42 C46 -60.1(2) . . . . ? C46 C42 C43 C44 59.0(3) . . . . ? C41 C42 C43 C44 -60.6(3) . . . . ? C42 C43 C44 C48 -59.7(2) . . . . ? C42 C43 C44 C45 60.8(2) . . . . ? C48 C44 C45 C40 60.1(2) . . . . ? C43 C44 C45 C40 -60.5(2) . . . . ? C33 C40 C45 C44 -179.67(18) . . . . ? C49 C40 C45 C44 -58.0(2) . . . . ? C41 C40 C45 C44 58.4(2) . . . . ? C43 C42 C46 C47 -59.5(2) . . . . ? C41 C42 C46 C47 60.1(2) . . . . ? C42 C46 C47 C49 -59.7(2) . . . . ? C42 C46 C47 C48 60.1(3) . . . . ? C43 C44 C48 C47 60.3(3) . . . . ? C45 C44 C48 C47 -59.7(3) . . . . ? C49 C47 C48 C44 59.8(3) . . . . ? C46 C47 C48 C44 -60.4(3) . . . . ? C46 C47 C49 C40 59.1(2) . . . . ? C48 C47 C49 C40 -60.8(2) . . . . ? C33 C40 C49 C47 -178.04(18) . . . . ? C45 C40 C49 C47 58.8(2) . . . . ? C41 C40 C49 C47 -57.4(2) . . . . ? C62 P1 C50 C51 -164.90(16) . . . . ? C56 P1 C50 C51 -55.33(18) . . . . ? Ru1 P1 C50 C51 60.63(17) . . . . ? C62 P1 C50 C55 -36.9(2) . . . . ? C56 P1 C50 C55 72.7(2) . . . . ? Ru1 P1 C50 C55 -171.34(16) . . . . ? C55 C50 C51 C52 60.2(2) . . . . ? P1 C50 C51 C52 -166.68(16) . . . . ? C50 C51 C52 C53 -59.6(3) . . . . ? C51 C52 C53 C54 54.9(3) . . . . ? C52 C53 C54 C55 -53.4(3) . . . . ? C53 C54 C55 C50 54.6(3) . . . . ? C51 C50 C55 C54 -56.7(3) . . . . ? P1 C50 C55 C54 173.87(18) . . . . ? C62 P1 C56 C61 60.9(2) . . . . ? C50 P1 C56 C61 -48.1(2) . . . . ? Ru1 P1 C56 C61 -172.60(18) . . . . ? C62 P1 C56 C57 -168.42(18) . . . . ? C50 P1 C56 C57 82.55(19) . . . . ? Ru1 P1 C56 C57 -41.94(18) . . . . ? C61 C56 C57 C58 -56.8(3) . . . . ? P1 C56 C57 C58 168.48(19) . . . . ? C56 C57 C58 C59 56.4(3) . . . . ? C57 C58 C59 C60 -55.5(4) . . . . ? C58 C59 C60 C61 55.2(4) . . . . ? C57 C56 C61 C60 56.5(3) . . . . ? P1 C56 C61 C60 -172.0(2) . . . . ? C59 C60 C61 C56 -56.0(4) . . . . ? C56 P1 C62 C63 62.5(2) . . . . ? C50 P1 C62 C63 175.0(2) . . . . ? Ru1 P1 C62 C63 -52.5(2) . . . . ? C56 P1 C62 C67 -173.29(18) . . . . ? C50 P1 C62 C67 -60.76(19) . . . . ? Ru1 P1 C62 C67 71.72(19) . . . . ? C67 C62 C63 C64 55.4(3) . . . . ? P1 C62 C63 C64 -179.6(2) . . . . ? C62 C63 C64 C65 -55.4(4) . . . . ? C63 C64 C65 C66 55.8(4) . . . . ? C64 C65 C66 C67 -56.5(4) . . . . ? C65 C66 C67 C62 57.4(3) . . . . ? C63 C62 C67 C66 -57.1(3) . . . . ? P1 C62 C67 C66 176.98(19) . . . . ? #===END data_2d _database_code_depnum_ccdc_archive 'CCDC 707356' # DT0815 _audit_creation_method SHELXL-97 _audit_creation_date 08-07-11 # CLIENT : R. Dorta # JOURNAL COMPOUND IDENTIFIER : 2d # ABSOLUTE CONFIGURATION : # POLYMORPH : # NEUTRON STUDY : # BIOLOGICAL ACTIVITY : # COMMENTS : solvent: dichloromethane / MeOH. # The asymmetric unit contains one molecule of the Ru-complex, plus one # molecule of MeOH. _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C60 H81 Cl2 N2 P Ru, C H4 O' _chemical_formula_sum 'C61 H85 Cl2 N2 O P Ru' _chemical_formula_weight 1065.23 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 244 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 340 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cl Cl 8 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 8 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; O O 4 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 4 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 4 0.0106 0.0060 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1090(2) _cell_length_b 17.8488(3) _cell_length_c 19.6533(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.3524(10) _cell_angle_gamma 90.00 _cell_volume 5616.15(15) _cell_formula_units_Z 4 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 178038 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.900 _exptl_special_details ; Solvent used: dichloromethane / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 1.048(1) Frames collected: 377 Seconds exposure per frame: 60 Degrees rotation per frame: 1.5 Crystal-Detector distance (mm): 30.0 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 107748 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.45 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _reflns_number_total 12771 _reflns_number_gt 9939 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The top peak and deepest hole are within 0.75 A of Ru1, the next top peak is within 0.85 of Cl2. The asymmetric unit contains one molecule of the Ru-complex, plus one molecule of MeOH. The idealised hydroxy O-H vector of the MeOH molecule was oriented so that the H-atom corresponded closely with the position of a difference map peak (AFIX 147). ; _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^)+(0.0634P)^2^+36.2691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12771 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2028 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 4.269 _refine_diff_density_min -2.972 _refine_diff_density_rms 0.121 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.25876(2) 0.09814(2) 0.228613(19) 0.03229(13) Uani 1 1 d . . . Cl1 Cl 0.18323(8) 0.20371(9) 0.17886(7) 0.0458(3) Uani 1 1 d . . . Cl2 Cl 0.33922(10) -0.01378(7) 0.25411(8) 0.0475(3) Uani 1 1 d . . . P1 P 0.38722(7) 0.16990(6) 0.22964(6) 0.0252(2) Uani 1 1 d . . . N1 N 0.0935(2) 0.0107(2) 0.23578(19) 0.0298(8) Uani 1 1 d . . . N3 N 0.1483(3) -0.0142(3) 0.1416(2) 0.0399(10) Uani 1 1 d . . . C2 C 0.1587(3) 0.0268(3) 0.2006(3) 0.0394(12) Uani 1 1 d . . . C4 C 0.0673(4) -0.0540(4) 0.1330(3) 0.0514(16) Uani 1 1 d . . . H41 H 0.0750 -0.1075 0.1220 0.062 Uiso 1 1 calc R . . H42 H 0.0286 -0.0309 0.0963 0.062 Uiso 1 1 calc R . . C5 C 0.0350(4) -0.0454(4) 0.2016(3) 0.0496(15) Uani 1 1 d . . . H51 H -0.0232 -0.0266 0.1967 0.059 Uiso 1 1 calc R . . H52 H 0.0377 -0.0933 0.2271 0.059 Uiso 1 1 calc R . . C6 C 0.0842(3) 0.0279(3) 0.3058(2) 0.0273(9) Uani 1 1 d . . . C7 C 0.1212(3) -0.0228(3) 0.3566(2) 0.0291(10) Uani 1 1 d . . . C8 C 0.1724(3) -0.0834(3) 0.3413(3) 0.0321(10) Uani 1 1 d . . . H8 H 0.1834 -0.0910 0.2953 0.039 Uiso 1 1 calc R . . C9 C 0.2063(3) -0.1315(3) 0.3908(3) 0.0370(11) Uani 1 1 d . . . C10 C 0.1897(3) -0.1195(3) 0.4592(3) 0.0398(12) Uani 1 1 d . . . H10 H 0.2124 -0.1530 0.4940 0.048 Uiso 1 1 calc R . . C11 C 0.1422(3) -0.0613(3) 0.4762(3) 0.0364(11) Uani 1 1 d . . . H11 H 0.1330 -0.0542 0.5227 0.044 Uiso 1 1 calc R . . C12 C 0.1058(3) -0.0106(3) 0.4256(2) 0.0303(10) Uani 1 1 d . . . C13 C 0.0547(3) 0.0501(3) 0.4409(3) 0.0342(11) Uani 1 1 d . . . H13 H 0.0448 0.0589 0.4869 0.041 Uiso 1 1 calc R . . C14 C 0.0195(3) 0.0959(3) 0.3906(3) 0.0344(10) Uani 1 1 d . . . H14 H -0.0147 0.1361 0.4025 0.041 Uiso 1 1 calc R . . C15 C 0.0322(3) 0.0857(3) 0.3207(3) 0.0321(10) Uani 1 1 d . . . C16 C 0.1896(3) -0.0078(3) 0.0803(3) 0.0415(12) Uani 1 1 d . . . C17 C 0.1584(4) 0.0465(3) 0.0326(3) 0.0468(15) Uani 1 1 d . . . C18 C 0.0954(3) 0.1020(4) 0.0453(3) 0.0438(13) Uani 1 1 d . . . H18 H 0.0765 0.1036 0.0894 0.053 Uiso 1 1 calc R . . C19 C 0.0630(4) 0.1506(3) -0.0019(3) 0.0489(14) Uani 1 1 d . . . C20 C 0.0940(4) 0.1514(4) -0.0643(4) 0.0533(15) Uani 1 1 d . . . H20 H 0.0737 0.1879 -0.0971 0.064 Uiso 1 1 calc R . . C21 C 0.1518(3) 0.1024(3) -0.0806(3) 0.0411(12) Uani 1 1 d . . . H21 H 0.1707 0.1056 -0.1247 0.049 Uiso 1 1 calc R . . C22 C 0.1860(3) 0.0461(3) -0.0352(3) 0.0371(11) Uani 1 1 d . . . C23 C 0.2430(4) -0.0078(4) -0.0515(4) 0.0524(15) Uani 1 1 d . . . H23 H 0.2620 -0.0089 -0.0956 0.063 Uiso 1 1 calc R . . C24 C 0.2722(4) -0.0609(4) -0.0008(3) 0.0564(17) Uani 1 1 d . . . H24 H 0.3120 -0.0975 -0.0106 0.068 Uiso 1 1 calc R . . C25 C 0.2427(4) -0.0597(3) 0.0635(3) 0.0409(12) Uani 1 1 d . . . C26 C 0.2637(4) -0.1961(3) 0.3762(3) 0.0480(14) Uani 1 1 d . . . H26 H 0.2457 -0.2413 0.4009 0.058 Uiso 1 1 calc R . . C27 C 0.3537(4) -0.1784(5) 0.4046(4) 0.067(2) Uani 1 1 d . . . H271 H 0.3893 -0.2217 0.3980 0.100 Uiso 1 1 calc R . . H272 H 0.3560 -0.1670 0.4535 0.100 Uiso 1 1 calc R . . H273 H 0.3735 -0.1350 0.3804 0.100 Uiso 1 1 calc R . . C28 C 0.2606(4) -0.2162(4) 0.3006(4) 0.0564(16) Uani 1 1 d . . . H281 H 0.2831 -0.1746 0.2758 0.085 Uiso 1 1 calc R . . H282 H 0.2026 -0.2256 0.2819 0.085 Uiso 1 1 calc R . . H283 H 0.2941 -0.2613 0.2955 0.085 Uiso 1 1 calc R . . C29 C -0.0127(3) 0.1352(3) 0.2654(3) 0.0394(12) Uani 1 1 d . . . H29 H 0.0132 0.1266 0.2222 0.047 Uiso 1 1 calc R . . C30 C -0.0053(4) 0.2189(3) 0.2827(3) 0.0482(14) Uani 1 1 d . . . H301 H -0.0285 0.2484 0.2430 0.072 Uiso 1 1 calc R . . H302 H 0.0537 0.2319 0.2944 0.072 Uiso 1 1 calc R . . H303 H -0.0363 0.2299 0.3217 0.072 Uiso 1 1 calc R . . C31 C -0.1054(4) 0.1134(4) 0.2522(4) 0.0636(19) Uani 1 1 d . . . H311 H -0.1101 0.0597 0.2419 0.095 Uiso 1 1 calc R . . H312 H -0.1322 0.1421 0.2133 0.095 Uiso 1 1 calc R . . H313 H -0.1332 0.1243 0.2930 0.095 Uiso 1 1 calc R . . C32 C -0.0055(4) 0.2061(4) 0.0128(3) 0.0554(16) Uani 1 1 d . . . H32 H -0.0383 0.2196 -0.0317 0.067 Uiso 1 1 calc R . . C33 C -0.0654(4) 0.1703(5) 0.0591(4) 0.078(2) Uani 1 1 d . . . H331 H -0.0361 0.1624 0.1049 0.116 Uiso 1 1 calc R . . H332 H -0.0851 0.1220 0.0397 0.116 Uiso 1 1 calc R . . H333 H -0.1132 0.2036 0.0621 0.116 Uiso 1 1 calc R . . C34 C 0.0318(5) 0.2753(4) 0.0439(4) 0.070(2) Uani 1 1 d . . . H341 H 0.0624 0.2635 0.0886 0.105 Uiso 1 1 calc R . . H342 H -0.0125 0.3115 0.0499 0.105 Uiso 1 1 calc R . . H343 H 0.0703 0.2967 0.0139 0.105 Uiso 1 1 calc R . . C35 C 0.2737(4) -0.1258(3) 0.1128(3) 0.0484(14) Uani 1 1 d . . . H35 H 0.2593 -0.1135 0.1598 0.058 Uiso 1 1 calc R . . C36 C 0.2320(4) -0.1996(3) 0.0907(4) 0.0529(15) Uani 1 1 d . . . H361 H 0.1712 -0.1942 0.0889 0.079 Uiso 1 1 calc R . . H362 H 0.2511 -0.2388 0.1237 0.079 Uiso 1 1 calc R . . H363 H 0.2467 -0.2133 0.0453 0.079 Uiso 1 1 calc R . . C37 C 0.3698(4) -0.1369(4) 0.1167(4) 0.0618(18) Uani 1 1 d . . . H371 H 0.3872 -0.1758 0.1505 0.093 Uiso 1 1 calc R . . H372 H 0.3980 -0.0898 0.1304 0.093 Uiso 1 1 calc R . . H373 H 0.3846 -0.1522 0.0717 0.093 Uiso 1 1 calc R . . C38 C 0.2323(3) 0.1301(3) 0.3129(2) 0.0318(10) Uani 1 1 d . . . H38 H 0.1912 0.1685 0.3083 0.038 Uiso 1 1 calc R . . C39 C 0.2571(3) 0.1125(3) 0.3843(2) 0.0342(11) Uani 1 1 d . . . C40 C 0.2293(3) 0.1606(3) 0.4335(3) 0.0406(12) Uani 1 1 d . . . H40 H 0.1949 0.2021 0.4190 0.049 Uiso 1 1 calc R . . C41 C 0.2514(4) 0.1487(4) 0.5031(3) 0.0547(17) Uani 1 1 d . . . H411 H 0.2315 0.1812 0.5359 0.066 Uiso 1 1 calc R . . C42 C 0.3026(4) 0.0889(4) 0.5239(3) 0.0609(19) Uani 1 1 d . . . H421 H 0.3181 0.0806 0.5714 0.073 Uiso 1 1 calc R . . C43 C 0.3313(4) 0.0416(4) 0.4770(3) 0.0571(17) Uani 1 1 d . . . H43 H 0.3673 0.0013 0.4920 0.068 Uiso 1 1 calc R . . C44 C 0.3080(3) 0.0523(3) 0.4071(3) 0.0438(13) Uani 1 1 d . . . H44 H 0.3269 0.0184 0.3749 0.053 Uiso 1 1 calc R . . C45 C 0.4241(3) 0.1621(3) 0.1439(2) 0.0293(9) Uani 1 1 d . . . H45 H 0.4800 0.1870 0.1468 0.035 Uiso 1 1 calc R . . C46 C 0.3681(4) 0.2009(4) 0.0861(3) 0.0463(14) Uani 1 1 d . . . H461 H 0.3129 0.1761 0.0799 0.056 Uiso 1 1 calc R . . H462 H 0.3596 0.2539 0.0985 0.056 Uiso 1 1 calc R . . C47 C 0.4087(4) 0.1972(4) 0.0192(3) 0.0526(15) Uani 1 1 d . . . H471 H 0.3707 0.2201 -0.0182 0.063 Uiso 1 1 calc R . . H472 H 0.4612 0.2264 0.0243 0.063 Uiso 1 1 calc R . . C48 C 0.4274(5) 0.1173(4) 0.0004(3) 0.0579(17) Uani 1 1 d . . . H481 H 0.4582 0.1172 -0.0405 0.069 Uiso 1 1 calc R . . H482 H 0.3742 0.0900 -0.0114 0.069 Uiso 1 1 calc R . . C49 C 0.4789(6) 0.0770(4) 0.0586(3) 0.071(2) Uani 1 1 d . . . H491 H 0.5349 0.1002 0.0665 0.085 Uiso 1 1 calc R . . H492 H 0.4861 0.0239 0.0459 0.085 Uiso 1 1 calc R . . C50 C 0.4369(5) 0.0807(3) 0.1245(3) 0.0511(15) Uani 1 1 d . . . H501 H 0.3823 0.0548 0.1178 0.061 Uiso 1 1 calc R . . H502 H 0.4722 0.0551 0.1619 0.061 Uiso 1 1 calc R . . C51 C 0.4774(3) 0.1329(3) 0.2868(2) 0.0308(10) Uani 1 1 d . . . H511 H 0.4720 0.0772 0.2842 0.037 Uiso 1 1 calc R . . C52 C 0.5659(3) 0.1501(3) 0.2692(3) 0.0416(12) Uani 1 1 d . . . H521 H 0.5769 0.2045 0.2741 0.050 Uiso 1 1 calc R . . H522 H 0.5704 0.1361 0.2210 0.050 Uiso 1 1 calc R . . C53 C 0.6314(4) 0.1064(4) 0.3167(3) 0.0493(14) Uani 1 1 d . . . H531 H 0.6246 0.0522 0.3072 0.059 Uiso 1 1 calc R . . H532 H 0.6879 0.1211 0.3064 0.059 Uiso 1 1 calc R . . C54 C 0.6240(4) 0.1205(3) 0.3917(3) 0.0493(14) Uani 1 1 d . . . H541 H 0.6388 0.1732 0.4029 0.059 Uiso 1 1 calc R . . H542 H 0.6639 0.0878 0.4199 0.059 Uiso 1 1 calc R . . C55 C 0.5360(4) 0.1049(4) 0.4086(3) 0.0598(18) Uani 1 1 d . . . H551 H 0.5317 0.1169 0.4572 0.072 Uiso 1 1 calc R . . H552 H 0.5228 0.0511 0.4014 0.072 Uiso 1 1 calc R . . C56 C 0.4733(3) 0.1527(4) 0.3625(3) 0.0427(13) Uani 1 1 d . . . H561 H 0.4161 0.1436 0.3745 0.051 Uiso 1 1 calc R . . H562 H 0.4863 0.2064 0.3700 0.051 Uiso 1 1 calc R . . C57 C 0.3783(3) 0.2727(3) 0.2405(2) 0.0291(9) Uani 1 1 d . . . H57 H 0.3336 0.2891 0.2042 0.035 Uiso 1 1 calc R . . C58 C 0.4553(3) 0.3183(3) 0.2284(3) 0.0396(12) Uani 1 1 d . . . H581 H 0.4734 0.3045 0.1836 0.048 Uiso 1 1 calc R . . H582 H 0.5014 0.3062 0.2643 0.048 Uiso 1 1 calc R . . C59 C 0.4373(4) 0.4031(3) 0.2295(3) 0.0474(14) Uani 1 1 d . . . H591 H 0.4889 0.4312 0.2236 0.057 Uiso 1 1 calc R . . H592 H 0.3948 0.4160 0.1910 0.057 Uiso 1 1 calc R . . C60 C 0.4059(4) 0.4256(3) 0.2967(3) 0.0413(12) Uani 1 1 d . . . H601 H 0.4511 0.4184 0.3345 0.050 Uiso 1 1 calc R . . H602 H 0.3909 0.4794 0.2950 0.050 Uiso 1 1 calc R . . C61 C 0.3308(4) 0.3801(3) 0.3106(3) 0.0438(13) Uani 1 1 d . . . H611 H 0.2833 0.3926 0.2761 0.053 Uiso 1 1 calc R . . H612 H 0.3147 0.3936 0.3562 0.053 Uiso 1 1 calc R . . C62 C 0.3473(4) 0.2957(3) 0.3085(3) 0.0382(11) Uani 1 1 d . . . H621 H 0.2953 0.2682 0.3145 0.046 Uiso 1 1 calc R . . H622 H 0.3898 0.2819 0.3468 0.046 Uiso 1 1 calc R . . O1 O 0.1206(4) 0.3698(4) 0.2249(3) 0.0820(16) Uani 1 1 d . . . H1 H 0.1271 0.3968 0.2601 0.098 Uiso 1 1 calc R . . C71 C 0.1291(7) 0.4136(5) 0.1671(5) 0.090(3) Uani 1 1 d . . . H711 H 0.1651 0.4566 0.1802 0.135 Uiso 1 1 calc R . . H712 H 0.0740 0.4313 0.1475 0.135 Uiso 1 1 calc R . . H713 H 0.1543 0.3834 0.1331 0.135 Uiso 1 1 calc R . . 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 0.0346(2) 0.0389(2) 0.02415(19) -0.00591(16) 0.00667(14) -0.01510(17) Cl1 0.0357(6) 0.0634(9) 0.0370(7) 0.0050(6) -0.0027(5) 0.0020(6) Cl2 0.0579(8) 0.0310(6) 0.0569(8) -0.0055(6) 0.0218(7) -0.0086(6) P1 0.0285(6) 0.0234(5) 0.0240(5) -0.0018(4) 0.0044(4) -0.0033(4) N1 0.0287(19) 0.033(2) 0.0276(19) -0.0030(16) 0.0023(15) -0.0094(16) N3 0.043(2) 0.040(2) 0.036(2) 0.0002(19) 0.0026(19) -0.005(2) C2 0.043(3) 0.046(3) 0.030(2) -0.001(2) 0.006(2) -0.009(2) C4 0.047(3) 0.066(4) 0.042(3) -0.016(3) 0.009(2) -0.030(3) C5 0.048(3) 0.063(4) 0.038(3) -0.018(3) 0.008(2) -0.033(3) C6 0.026(2) 0.030(2) 0.027(2) 0.0009(18) 0.0062(17) -0.0048(18) C7 0.028(2) 0.029(2) 0.031(2) 0.0012(18) 0.0085(18) -0.0070(18) C8 0.032(2) 0.031(2) 0.035(2) 0.0007(19) 0.0102(19) -0.0049(19) C9 0.030(2) 0.034(3) 0.048(3) 0.007(2) 0.010(2) -0.005(2) C10 0.035(3) 0.040(3) 0.044(3) 0.014(2) 0.003(2) -0.003(2) C11 0.034(3) 0.043(3) 0.033(3) 0.006(2) 0.006(2) -0.007(2) C12 0.026(2) 0.033(2) 0.032(2) 0.0018(19) 0.0073(18) -0.0075(19) C13 0.035(3) 0.039(3) 0.031(2) 0.000(2) 0.0117(19) -0.008(2) C14 0.029(2) 0.037(3) 0.038(3) -0.002(2) 0.0106(19) -0.002(2) C15 0.028(2) 0.034(3) 0.034(2) 0.003(2) 0.0052(19) -0.0047(19) C16 0.042(3) 0.044(3) 0.038(3) 0.001(2) 0.000(2) -0.008(2) C17 0.044(3) 0.054(3) 0.039(3) 0.013(3) -0.013(2) -0.029(3) C18 0.030(3) 0.068(4) 0.033(3) -0.021(3) 0.004(2) -0.016(3) C19 0.043(3) 0.044(3) 0.056(4) 0.001(3) -0.008(3) -0.008(3) C20 0.042(3) 0.050(4) 0.066(4) 0.011(3) 0.001(3) -0.014(3) C21 0.036(3) 0.051(3) 0.035(3) 0.007(2) 0.001(2) -0.012(2) C22 0.032(2) 0.046(3) 0.032(3) 0.007(2) 0.0017(19) -0.011(2) C23 0.045(3) 0.051(4) 0.064(4) 0.009(3) 0.018(3) -0.006(3) C24 0.041(3) 0.073(4) 0.056(4) -0.021(3) 0.007(3) 0.006(3) C25 0.048(3) 0.037(3) 0.039(3) -0.008(2) 0.009(2) -0.013(2) C26 0.045(3) 0.038(3) 0.063(4) 0.009(3) 0.016(3) 0.006(2) C27 0.043(3) 0.086(5) 0.070(5) -0.005(4) 0.000(3) 0.023(4) C28 0.053(4) 0.040(3) 0.077(4) -0.009(3) 0.011(3) 0.012(3) C29 0.040(3) 0.036(3) 0.041(3) 0.003(2) 0.003(2) 0.000(2) C30 0.050(3) 0.038(3) 0.058(4) 0.007(3) 0.009(3) 0.007(3) C31 0.044(3) 0.064(4) 0.078(5) 0.013(4) -0.017(3) -0.003(3) C32 0.047(3) 0.060(4) 0.057(4) 0.013(3) -0.006(3) 0.009(3) C33 0.046(4) 0.114(7) 0.075(5) 0.024(5) 0.012(3) 0.014(4) C34 0.063(4) 0.064(5) 0.079(5) -0.007(4) -0.015(4) 0.021(4) C35 0.048(3) 0.043(3) 0.052(3) -0.004(3) -0.001(3) 0.005(3) C36 0.058(4) 0.035(3) 0.065(4) -0.001(3) 0.000(3) -0.002(3) C37 0.045(3) 0.047(4) 0.089(5) 0.004(3) -0.012(3) 0.007(3) C38 0.028(2) 0.039(3) 0.028(2) 0.000(2) 0.0058(18) -0.007(2) C39 0.032(2) 0.042(3) 0.030(2) -0.002(2) 0.0061(19) -0.014(2) C40 0.038(3) 0.052(3) 0.031(3) -0.006(2) 0.006(2) -0.011(2) C41 0.053(4) 0.080(5) 0.031(3) -0.012(3) 0.004(2) -0.022(3) C42 0.063(4) 0.085(5) 0.033(3) 0.013(3) 0.000(3) -0.022(4) C43 0.049(3) 0.066(4) 0.054(4) 0.020(3) -0.004(3) -0.007(3) C44 0.043(3) 0.045(3) 0.043(3) 0.005(2) 0.003(2) -0.006(2) C45 0.033(2) 0.028(2) 0.028(2) -0.0045(18) 0.0068(18) -0.0014(19) C46 0.056(3) 0.056(4) 0.028(3) 0.002(2) 0.010(2) 0.015(3) C47 0.067(4) 0.064(4) 0.029(3) 0.006(3) 0.015(3) 0.010(3) C48 0.080(5) 0.065(4) 0.031(3) -0.013(3) 0.019(3) -0.006(4) C49 0.117(6) 0.054(4) 0.047(4) -0.012(3) 0.033(4) 0.024(4) C50 0.087(5) 0.033(3) 0.035(3) -0.007(2) 0.016(3) 0.008(3) C51 0.033(2) 0.025(2) 0.034(2) 0.0002(19) -0.0011(19) -0.0020(19) C52 0.037(3) 0.048(3) 0.040(3) 0.006(2) 0.002(2) 0.002(2) C53 0.036(3) 0.050(3) 0.059(4) 0.002(3) -0.005(3) 0.007(3) C54 0.044(3) 0.044(3) 0.056(4) 0.009(3) -0.012(3) -0.003(3) C55 0.049(3) 0.085(5) 0.042(3) 0.024(3) -0.009(3) -0.011(3) C56 0.034(3) 0.061(4) 0.033(3) 0.007(2) 0.001(2) -0.006(2) C57 0.031(2) 0.028(2) 0.029(2) -0.0032(18) 0.0063(18) -0.0026(18) C58 0.046(3) 0.027(2) 0.049(3) -0.008(2) 0.019(2) -0.011(2) C59 0.071(4) 0.027(3) 0.048(3) -0.002(2) 0.017(3) -0.010(3) C60 0.051(3) 0.028(3) 0.044(3) -0.008(2) 0.002(2) 0.002(2) C61 0.045(3) 0.036(3) 0.051(3) -0.015(2) 0.007(2) 0.002(2) C62 0.047(3) 0.033(3) 0.037(3) -0.007(2) 0.015(2) -0.008(2) O1 0.086(4) 0.093(4) 0.072(4) -0.021(3) 0.030(3) 0.003(3) C71 0.128(8) 0.063(5) 0.077(6) -0.019(4) 0.000(5) 0.015(5) _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 C38 1.846(5) . ? Ru1 C2 2.080(5) . ? Ru1 Cl1 2.3924(15) . ? Ru1 Cl2 2.4038(16) . ? Ru1 P1 2.4320(12) . ? P1 C45 1.853(5) . ? P1 C57 1.855(5) . ? P1 C51 1.857(5) . ? N1 C2 1.352(6) . ? N1 C6 1.434(6) . ? N1 C5 1.483(6) . ? N3 C2 1.365(7) . ? N3 C16 1.443(7) . ? N3 C4 1.479(7) . ? C4 C5 1.505(8) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 C15 1.380(7) . ? C6 C7 1.428(7) . ? C7 C8 1.413(7) . ? C7 C12 1.423(6) . ? C8 C9 1.365(7) . ? C8 H8 0.9500 . ? C9 C10 1.416(8) . ? C9 C26 1.525(8) . ? C10 C11 1.353(8) . ? C10 H10 0.9500 . ? C11 C12 1.423(7) . ? C11 H11 0.9500 . ? C12 C13 1.412(7) . ? C13 C14 1.356(7) . ? C13 H13 0.9500 . ? C14 C15 1.423(7) . ? C14 H14 0.9500 . ? C15 C29 1.521(7) . ? C16 C25 1.327(8) . ? C16 C17 1.402(8) . ? C17 C22 1.450(8) . ? C17 C18 1.460(9) . ? C18 C19 1.333(9) . ? C18 H18 0.9500 . ? C19 C20 1.374(9) . ? C19 C32 1.535(9) . ? C20 C21 1.342(9) . ? C20 H20 0.9500 . ? C21 C22 1.414(7) . ? C21 H21 0.9500 . ? C22 C23 1.392(8) . ? C23 C24 1.417(10) . ? C23 H23 0.9500 . ? C24 C25 1.399(8) . ? C24 H24 0.9500 . ? C25 C35 1.573(8) . ? C26 C28 1.523(9) . ? C26 C27 1.528(9) . ? C26 H26 1.0000 . ? C27 H271 0.9800 . ? C27 H272 0.9800 . ? C27 H273 0.9800 . ? C28 H281 0.9800 . ? C28 H282 0.9800 . ? C28 H283 0.9800 . ? C29 C30 1.533(8) . ? C29 C31 1.537(8) . ? C29 H29 1.0000 . ? C30 H301 0.9800 . ? C30 H302 0.9800 . ? C30 H303 0.9800 . ? C31 H311 0.9800 . ? C31 H312 0.9800 . ? C31 H313 0.9800 . ? C32 C34 1.476(10) . ? C32 C33 1.536(10) . ? C32 H32 1.0000 . ? C33 H331 0.9800 . ? C33 H332 0.9800 . ? C33 H333 0.9800 . ? C34 H341 0.9800 . ? C34 H342 0.9800 . ? C34 H343 0.9800 . ? C35 C36 1.520(8) . ? C35 C37 1.554(9) . ? C35 H35 1.0000 . ? C36 H361 0.9800 . ? C36 H362 0.9800 . ? C36 H363 0.9800 . ? C37 H371 0.9800 . ? C37 H372 0.9800 . ? C37 H373 0.9800 . ? C38 C39 1.451(7) . ? C38 H38 0.9500 . ? C39 C44 1.394(8) . ? C39 C40 1.403(7) . ? C40 C41 1.390(8) . ? C40 H40 0.9500 . ? C41 C42 1.383(10) . ? C41 H411 0.9500 . ? C42 C43 1.368(10) . ? C42 H421 0.9500 . ? C43 C44 1.396(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.521(7) . ? C45 C46 1.536(7) . ? C45 H45 1.0000 . ? C46 C47 1.535(7) . ? C46 H461 0.9900 . ? C46 H462 0.9900 . ? C47 C48 1.512(9) . ? C47 H471 0.9900 . ? C47 H472 0.9900 . ? C48 C49 1.519(10) . ? C48 H481 0.9900 . ? C48 H482 0.9900 . ? C49 C50 1.527(8) . ? C49 H491 0.9900 . ? C49 H492 0.9900 . ? C50 H501 0.9900 . ? C50 H502 0.9900 . ? C51 C52 1.535(7) . ? C51 C56 1.537(7) . ? C51 H511 1.0000 . ? C52 C53 1.540(7) . ? C52 H521 0.9900 . ? C52 H522 0.9900 . ? C53 C54 1.512(9) . ? C53 H531 0.9900 . ? C53 H532 0.9900 . ? C54 C55 1.518(9) . ? C54 H541 0.9900 . ? C54 H542 0.9900 . ? C55 C56 1.538(8) . ? C55 H551 0.9900 . ? C55 H552 0.9900 . ? C56 H561 0.9900 . ? C56 H562 0.9900 . ? C57 C58 1.524(7) . ? C57 C62 1.533(6) . ? C57 H57 1.0000 . ? C58 C59 1.542(7) . ? C58 H581 0.9900 . ? C58 H582 0.9900 . ? C59 C60 1.518(8) . ? C59 H591 0.9900 . ? C59 H592 0.9900 . ? C60 C61 1.508(8) . ? C60 H601 0.9900 . ? C60 H602 0.9900 . ? C61 C62 1.530(7) . ? C61 H611 0.9900 . ? C61 H612 0.9900 . ? C62 H621 0.9900 . ? C62 H622 0.9900 . ? O1 C71 1.397(10) . ? O1 H1 0.8400 . ? C71 H711 0.9800 . ? C71 H712 0.9800 . ? C71 H713 0.9800 . ? 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 C38 Ru1 C2 100.2(2) . . ? C38 Ru1 Cl1 88.05(17) . . ? C2 Ru1 Cl1 91.73(16) . . ? C38 Ru1 Cl2 104.03(17) . . ? C2 Ru1 Cl2 85.99(17) . . ? Cl1 Ru1 Cl2 167.92(5) . . ? C38 Ru1 P1 96.37(15) . . ? C2 Ru1 P1 163.39(15) . . ? Cl1 Ru1 P1 88.99(5) . . ? Cl2 Ru1 P1 89.84(5) . . ? C45 P1 C57 102.5(2) . . ? C45 P1 C51 102.4(2) . . ? C57 P1 C51 110.3(2) . . ? C45 P1 Ru1 108.14(15) . . ? C57 P1 Ru1 116.42(15) . . ? C51 P1 Ru1 115.21(16) . . ? C2 N1 C6 128.0(4) . . ? C2 N1 C5 113.7(4) . . ? C6 N1 C5 116.8(4) . . ? C2 N3 C16 129.9(5) . . ? C2 N3 C4 112.2(4) . . ? C16 N3 C4 115.2(4) . . ? N1 C2 N3 106.9(4) . . ? N1 C2 Ru1 128.2(4) . . ? N3 C2 Ru1 124.9(4) . . ? N3 C4 C5 103.7(4) . . ? N3 C4 H41 111.0 . . ? C5 C4 H41 111.0 . . ? N3 C4 H42 111.0 . . ? C5 C4 H42 111.0 . . ? H41 C4 H42 109.0 . . ? N1 C5 C4 102.1(4) . . ? N1 C5 H51 111.3 . . ? C4 C5 H51 111.3 . . ? N1 C5 H52 111.3 . . ? C4 C5 H52 111.3 . . ? H51 C5 H52 109.2 . . ? C15 C6 C7 122.8(4) . . ? C15 C6 N1 119.6(4) . . ? C7 C6 N1 117.1(4) . . ? C8 C7 C12 119.2(4) . . ? C8 C7 C6 123.0(4) . . ? C12 C7 C6 117.8(4) . . ? C9 C8 C7 121.8(5) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 118.6(5) . . ? C8 C9 C26 123.0(5) . . ? C10 C9 C26 118.4(5) . . ? C11 C10 C9 121.4(5) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 121.1(5) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 123.0(5) . . ? C13 C12 C7 119.2(4) . . ? C11 C12 C7 117.8(5) . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 122.2(5) . . ? C13 C14 H14 118.9 . . ? C15 C14 H14 118.9 . . ? C6 C15 C14 117.1(4) . . ? C6 C15 C29 122.4(4) . . ? C14 C15 C29 120.5(5) . . ? C25 C16 C17 120.6(6) . . ? C25 C16 N3 121.5(5) . . ? C17 C16 N3 116.6(5) . . ? C16 C17 C22 119.2(6) . . ? C16 C17 C18 124.0(5) . . ? C22 C17 C18 116.7(5) . . ? C19 C18 C17 123.2(5) . . ? C19 C18 H18 118.4 . . ? C17 C18 H18 118.4 . . ? C18 C19 C20 118.4(6) . . ? C18 C19 C32 121.5(6) . . ? C20 C19 C32 120.1(6) . . ? C21 C20 C19 122.4(6) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 122.9(5) . . ? C20 C21 H21 118.5 . . ? C22 C21 H21 118.5 . . ? C23 C22 C21 124.5(5) . . ? C23 C22 C17 119.5(5) . . ? C21 C22 C17 116.1(5) . . ? C22 C23 C24 118.5(6) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 120.4(6) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C16 C25 C24 121.9(6) . . ? C16 C25 C35 122.6(5) . . ? C24 C25 C35 115.5(5) . . ? C28 C26 C9 114.0(5) . . ? C28 C26 C27 109.4(5) . . ? C9 C26 C27 110.1(5) . . ? C28 C26 H26 107.7 . . ? C9 C26 H26 107.7 . . ? C27 C26 H26 107.7 . . ? C26 C27 H271 109.5 . . ? C26 C27 H272 109.5 . . ? H271 C27 H272 109.5 . . ? C26 C27 H273 109.5 . . ? H271 C27 H273 109.5 . . ? H272 C27 H273 109.5 . . ? C26 C28 H281 109.5 . . ? C26 C28 H282 109.5 . . ? H281 C28 H282 109.5 . . ? C26 C28 H283 109.5 . . ? H281 C28 H283 109.5 . . ? H282 C28 H283 109.5 . . ? C15 C29 C30 112.9(5) . . ? C15 C29 C31 110.5(5) . . ? C30 C29 C31 109.6(5) . . ? C15 C29 H29 107.9 . . ? C30 C29 H29 107.9 . . ? C31 C29 H29 107.9 . . ? C29 C30 H301 109.5 . . ? C29 C30 H302 109.5 . . ? H301 C30 H302 109.5 . . ? C29 C30 H303 109.5 . . ? H301 C30 H303 109.5 . . ? H302 C30 H303 109.5 . . ? C29 C31 H311 109.5 . . ? C29 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C29 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? C34 C32 C19 110.4(5) . . ? C34 C32 C33 110.9(7) . . ? C19 C32 C33 110.8(6) . . ? C34 C32 H32 108.2 . . ? C19 C32 H32 108.2 . . ? C33 C32 H32 108.2 . . ? C32 C33 H331 109.5 . . ? C32 C33 H332 109.5 . . ? H331 C33 H332 109.5 . . ? C32 C33 H333 109.5 . . ? H331 C33 H333 109.5 . . ? H332 C33 H333 109.5 . . ? C32 C34 H341 109.5 . . ? C32 C34 H342 109.5 . . ? H341 C34 H342 109.5 . . ? C32 C34 H343 109.5 . . ? H341 C34 H343 109.5 . . ? H342 C34 H343 109.5 . . ? C36 C35 C37 108.0(5) . . ? C36 C35 C25 112.0(5) . . ? C37 C35 C25 111.8(5) . . ? C36 C35 H35 108.3 . . ? C37 C35 H35 108.3 . . ? C25 C35 H35 108.3 . . ? C35 C36 H361 109.5 . . ? C35 C36 H362 109.5 . . ? H361 C36 H362 109.5 . . ? C35 C36 H363 109.5 . . ? H361 C36 H363 109.5 . . ? H362 C36 H363 109.5 . . ? C35 C37 H371 109.5 . . ? C35 C37 H372 109.5 . . ? H371 C37 H372 109.5 . . ? C35 C37 H373 109.5 . . ? H371 C37 H373 109.5 . . ? H372 C37 H373 109.5 . . ? C39 C38 Ru1 137.3(4) . . ? C39 C38 H38 111.3 . . ? Ru1 C38 H38 111.3 . . ? C44 C39 C40 118.1(5) . . ? C44 C39 C38 124.5(5) . . ? C40 C39 C38 117.3(5) . . ? C41 C40 C39 121.1(6) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C42 C41 C40 119.3(6) . . ? C42 C41 H411 120.4 . . ? C40 C41 H411 120.4 . . ? C43 C42 C41 120.8(6) . . ? C43 C42 H421 119.6 . . ? C41 C42 H421 119.6 . . ? C42 C43 C44 120.3(6) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C39 C44 C43 120.4(6) . . ? C39 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C50 C45 C46 109.3(4) . . ? C50 C45 P1 111.5(3) . . ? C46 C45 P1 114.6(3) . . ? C50 C45 H45 107.0 . . ? C46 C45 H45 107.0 . . ? P1 C45 H45 107.0 . . ? C47 C46 C45 110.1(5) . . ? C47 C46 H461 109.6 . . ? C45 C46 H461 109.6 . . ? C47 C46 H462 109.6 . . ? C45 C46 H462 109.6 . . ? H461 C46 H462 108.2 . . ? C48 C47 C46 111.5(5) . . ? C48 C47 H471 109.3 . . ? C46 C47 H471 109.3 . . ? C48 C47 H472 109.3 . . ? C46 C47 H472 109.3 . . ? H471 C47 H472 108.0 . . ? C47 C48 C49 111.6(5) . . ? C47 C48 H481 109.3 . . ? C49 C48 H481 109.3 . . ? C47 C48 H482 109.3 . . ? C49 C48 H482 109.3 . . ? H481 C48 H482 108.0 . . ? C48 C49 C50 111.3(6) . . ? C48 C49 H491 109.4 . . ? C50 C49 H491 109.4 . . ? C48 C49 H492 109.4 . . ? C50 C49 H492 109.4 . . ? H491 C49 H492 108.0 . . ? C45 C50 C49 109.8(5) . . ? C45 C50 H501 109.7 . . ? C49 C50 H501 109.7 . . ? C45 C50 H502 109.7 . . ? C49 C50 H502 109.7 . . ? H501 C50 H502 108.2 . . ? C52 C51 C56 108.3(4) . . ? C52 C51 P1 118.5(3) . . ? C56 C51 P1 112.9(3) . . ? C52 C51 H511 105.4 . . ? C56 C51 H511 105.4 . . ? P1 C51 H511 105.4 . . ? C51 C52 C53 110.7(5) . . ? C51 C52 H521 109.5 . . ? C53 C52 H521 109.5 . . ? C51 C52 H522 109.5 . . ? C53 C52 H522 109.5 . . ? H521 C52 H522 108.1 . . ? C54 C53 C52 112.6(5) . . ? C54 C53 H531 109.1 . . ? C52 C53 H531 109.1 . . ? C54 C53 H532 109.1 . . ? C52 C53 H532 109.1 . . ? H531 C53 H532 107.8 . . ? C53 C54 C55 111.0(5) . . ? C53 C54 H541 109.4 . . ? C55 C54 H541 109.4 . . ? C53 C54 H542 109.4 . . ? C55 C54 H542 109.4 . . ? H541 C54 H542 108.0 . . ? C54 C55 C56 109.7(5) . . ? C54 C55 H551 109.7 . . ? C56 C55 H551 109.7 . . ? C54 C55 H552 109.7 . . ? C56 C55 H552 109.7 . . ? H551 C55 H552 108.2 . . ? C51 C56 C55 110.3(5) . . ? C51 C56 H561 109.6 . . ? C55 C56 H561 109.6 . . ? C51 C56 H562 109.6 . . ? C55 C56 H562 109.6 . . ? H561 C56 H562 108.1 . . ? C58 C57 C62 110.0(4) . . ? C58 C57 P1 115.8(3) . . ? C62 C57 P1 113.7(3) . . ? C58 C57 H57 105.4 . . ? C62 C57 H57 105.4 . . ? P1 C57 H57 105.4 . . ? C57 C58 C59 111.3(5) . . ? C57 C58 H581 109.4 . . ? C59 C58 H581 109.4 . . ? C57 C58 H582 109.4 . . ? C59 C58 H582 109.4 . . ? H581 C58 H582 108.0 . . ? C60 C59 C58 110.7(5) . . ? C60 C59 H591 109.5 . . ? C58 C59 H591 109.5 . . ? C60 C59 H592 109.5 . . ? C58 C59 H592 109.5 . . ? H591 C59 H592 108.1 . . ? C61 C60 C59 111.5(5) . . ? C61 C60 H601 109.3 . . ? C59 C60 H601 109.3 . . ? C61 C60 H602 109.3 . . ? C59 C60 H602 109.3 . . ? H601 C60 H602 108.0 . . ? C60 C61 C62 112.3(5) . . ? C60 C61 H611 109.1 . . ? C62 C61 H611 109.1 . . ? C60 C61 H612 109.1 . . ? C62 C61 H612 109.1 . . ? H611 C61 H612 107.9 . . ? C61 C62 C57 111.2(4) . . ? C61 C62 H621 109.4 . . ? C57 C62 H621 109.4 . . ? C61 C62 H622 109.4 . . ? C57 C62 H622 109.4 . . ? H621 C62 H622 108.0 . . ? C71 O1 H1 109.5 . . ? O1 C71 H711 109.5 . . ? O1 C71 H712 109.5 . . ? H711 C71 H712 109.5 . . ? O1 C71 H713 109.5 . . ? H711 C71 H713 109.5 . . ? H712 C71 H713 109.5 . . ? 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 C38 Ru1 P1 C45 -171.5(2) . . . . ? C2 Ru1 P1 C45 9.1(6) . . . . ? Cl1 Ru1 P1 C45 -83.53(16) . . . . ? Cl2 Ru1 P1 C45 84.44(16) . . . . ? C38 Ru1 P1 C57 -56.8(2) . . . . ? C2 Ru1 P1 C57 123.8(6) . . . . ? Cl1 Ru1 P1 C57 31.11(17) . . . . ? Cl2 Ru1 P1 C57 -160.92(17) . . . . ? C38 Ru1 P1 C51 74.7(2) . . . . ? C2 Ru1 P1 C51 -104.7(6) . . . . ? Cl1 Ru1 P1 C51 162.62(18) . . . . ? Cl2 Ru1 P1 C51 -29.40(18) . . . . ? C6 N1 C2 N3 166.9(5) . . . . ? C5 N1 C2 N3 1.5(7) . . . . ? C6 N1 C2 Ru1 -12.1(8) . . . . ? C5 N1 C2 Ru1 -177.6(4) . . . . ? C16 N3 C2 N1 166.5(5) . . . . ? C4 N3 C2 N1 6.3(7) . . . . ? C16 N3 C2 Ru1 -14.4(8) . . . . ? C4 N3 C2 Ru1 -174.6(4) . . . . ? C38 Ru1 C2 N1 0.6(5) . . . . ? Cl1 Ru1 C2 N1 -87.7(5) . . . . ? Cl2 Ru1 C2 N1 104.1(5) . . . . ? P1 Ru1 C2 N1 180.0(3) . . . . ? C38 Ru1 C2 N3 -178.3(5) . . . . ? Cl1 Ru1 C2 N3 93.3(5) . . . . ? Cl2 Ru1 C2 N3 -74.8(5) . . . . ? P1 Ru1 C2 N3 1.1(10) . . . . ? C2 N3 C4 C5 -11.1(7) . . . . ? C16 N3 C4 C5 -174.4(5) . . . . ? C2 N1 C5 C4 -8.1(7) . . . . ? C6 N1 C5 C4 -175.3(5) . . . . ? N3 C4 C5 N1 10.7(7) . . . . ? C2 N1 C6 C15 104.3(6) . . . . ? C5 N1 C6 C15 -90.6(6) . . . . ? C2 N1 C6 C7 -83.8(6) . . . . ? C5 N1 C6 C7 81.3(6) . . . . ? C15 C6 C7 C8 178.0(4) . . . . ? N1 C6 C7 C8 6.4(6) . . . . ? C15 C6 C7 C12 -2.4(7) . . . . ? N1 C6 C7 C12 -174.1(4) . . . . ? C12 C7 C8 C9 1.1(7) . . . . ? C6 C7 C8 C9 -179.3(4) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C7 C8 C9 C26 -178.3(5) . . . . ? C8 C9 C10 C11 -0.8(8) . . . . ? C26 C9 C10 C11 177.2(5) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C10 C11 C12 C13 178.9(5) . . . . ? C10 C11 C12 C7 -0.3(7) . . . . ? C8 C7 C12 C13 180.0(4) . . . . ? C6 C7 C12 C13 0.4(6) . . . . ? C8 C7 C12 C11 -0.8(6) . . . . ? C6 C7 C12 C11 179.6(4) . . . . ? C11 C12 C13 C14 -178.3(5) . . . . ? C7 C12 C13 C14 0.9(7) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C7 C6 C15 C14 3.0(7) . . . . ? N1 C6 C15 C14 174.5(4) . . . . ? C7 C6 C15 C29 -174.7(4) . . . . ? N1 C6 C15 C29 -3.2(7) . . . . ? C13 C14 C15 C6 -1.7(7) . . . . ? C13 C14 C15 C29 176.1(5) . . . . ? C2 N3 C16 C25 110.3(7) . . . . ? C4 N3 C16 C25 -90.0(7) . . . . ? C2 N3 C16 C17 -82.6(7) . . . . ? C4 N3 C16 C17 77.2(7) . . . . ? C25 C16 C17 C22 -1.0(8) . . . . ? N3 C16 C17 C22 -168.2(4) . . . . ? C25 C16 C17 C18 175.5(5) . . . . ? N3 C16 C17 C18 8.2(8) . . . . ? C16 C17 C18 C19 -176.1(5) . . . . ? C22 C17 C18 C19 0.4(8) . . . . ? C17 C18 C19 C20 -4.0(8) . . . . ? C17 C18 C19 C32 177.7(5) . . . . ? C18 C19 C20 C21 4.0(9) . . . . ? C32 C19 C20 C21 -177.6(6) . . . . ? C19 C20 C21 C22 -0.2(9) . . . . ? C20 C21 C22 C23 176.8(6) . . . . ? C20 C21 C22 C17 -3.3(8) . . . . ? C16 C17 C22 C23 -0.3(7) . . . . ? C18 C17 C22 C23 -177.0(5) . . . . ? C16 C17 C22 C21 179.8(5) . . . . ? C18 C17 C22 C21 3.2(7) . . . . ? C21 C22 C23 C24 180.0(5) . . . . ? C17 C22 C23 C24 0.1(8) . . . . ? C22 C23 C24 C25 1.2(9) . . . . ? C17 C16 C25 C24 2.4(8) . . . . ? N3 C16 C25 C24 169.0(5) . . . . ? C17 C16 C25 C35 -174.7(5) . . . . ? N3 C16 C25 C35 -8.1(8) . . . . ? C23 C24 C25 C16 -2.6(9) . . . . ? C23 C24 C25 C35 174.7(6) . . . . ? C8 C9 C26 C28 -16.3(8) . . . . ? C10 C9 C26 C28 165.7(5) . . . . ? C8 C9 C26 C27 107.1(6) . . . . ? C10 C9 C26 C27 -70.9(7) . . . . ? C6 C15 C29 C30 -133.2(5) . . . . ? C14 C15 C29 C30 49.2(7) . . . . ? C6 C15 C29 C31 103.7(6) . . . . ? C14 C15 C29 C31 -73.9(6) . . . . ? C18 C19 C32 C34 87.4(7) . . . . ? C20 C19 C32 C34 -91.0(7) . . . . ? C18 C19 C32 C33 -35.9(8) . . . . ? C20 C19 C32 C33 145.7(6) . . . . ? C16 C25 C35 C36 104.6(7) . . . . ? C24 C25 C35 C36 -72.7(7) . . . . ? C16 C25 C35 C37 -134.0(6) . . . . ? C24 C25 C35 C37 48.7(7) . . . . ? C2 Ru1 C38 C39 100.0(5) . . . . ? Cl1 Ru1 C38 C39 -168.6(5) . . . . ? Cl2 Ru1 C38 C39 11.6(5) . . . . ? P1 Ru1 C38 C39 -79.9(5) . . . . ? Ru1 C38 C39 C44 -8.5(8) . . . . ? Ru1 C38 C39 C40 169.8(4) . . . . ? C44 C39 C40 C41 -0.4(8) . . . . ? C38 C39 C40 C41 -178.9(5) . . . . ? C39 C40 C41 C42 1.0(9) . . . . ? C40 C41 C42 C43 -0.3(10) . . . . ? C41 C42 C43 C44 -1.1(10) . . . . ? C40 C39 C44 C43 -1.0(8) . . . . ? C38 C39 C44 C43 177.4(5) . . . . ? C42 C43 C44 C39 1.7(9) . . . . ? C57 P1 C45 C50 179.4(4) . . . . ? C51 P1 C45 C50 65.0(4) . . . . ? Ru1 P1 C45 C50 -57.1(4) . . . . ? C57 P1 C45 C46 -55.8(4) . . . . ? C51 P1 C45 C46 -170.2(4) . . . . ? Ru1 P1 C45 C46 67.7(4) . . . . ? C50 C45 C46 C47 -59.3(6) . . . . ? P1 C45 C46 C47 174.8(4) . . . . ? C45 C46 C47 C48 56.1(7) . . . . ? C46 C47 C48 C49 -53.7(8) . . . . ? C47 C48 C49 C50 54.7(8) . . . . ? C46 C45 C50 C49 60.3(7) . . . . ? P1 C45 C50 C49 -172.0(5) . . . . ? C48 C49 C50 C45 -58.1(8) . . . . ? C45 P1 C51 C52 36.3(4) . . . . ? C57 P1 C51 C52 -72.3(4) . . . . ? Ru1 P1 C51 C52 153.4(3) . . . . ? C45 P1 C51 C56 164.3(4) . . . . ? C57 P1 C51 C56 55.8(4) . . . . ? Ru1 P1 C51 C56 -78.6(4) . . . . ? C56 C51 C52 C53 57.2(6) . . . . ? P1 C51 C52 C53 -172.6(4) . . . . ? C51 C52 C53 C54 -54.9(7) . . . . ? C52 C53 C54 C55 54.0(7) . . . . ? C53 C54 C55 C56 -56.4(7) . . . . ? C52 C51 C56 C55 -61.1(6) . . . . ? P1 C51 C56 C55 165.7(4) . . . . ? C54 C55 C56 C51 61.0(7) . . . . ? C45 P1 C57 C58 -51.7(4) . . . . ? C51 P1 C57 C58 56.8(4) . . . . ? Ru1 P1 C57 C58 -169.5(3) . . . . ? C45 P1 C57 C62 179.4(4) . . . . ? C51 P1 C57 C62 -72.1(4) . . . . ? Ru1 P1 C57 C62 61.6(4) . . . . ? C62 C57 C58 C59 -56.8(6) . . . . ? P1 C57 C58 C59 172.6(4) . . . . ? C57 C58 C59 C60 56.7(7) . . . . ? C58 C59 C60 C61 -54.9(7) . . . . ? C59 C60 C61 C62 54.6(7) . . . . ? C60 C61 C62 C57 -54.9(6) . . . . ? C58 C57 C62 C61 55.5(6) . . . . ? P1 C57 C62 C61 -172.8(4) . . . . ? #===END #===END data_2e _database_code_depnum_ccdc_archive 'CCDC 707357' # DT0817 _audit_creation_method SHELXL-97 _audit_creation_date 08-07-08 # CLIENT : R. Dorta # JOURNAL COMPOUND IDENTIFIER : 2e # ABSOLUTE CONFIGURATION : # POLYMORPH : # NEUTRON STUDY : # BIOLOGICAL ACTIVITY : # COMMENTS : solvent: dichloromethane / MeOH. # The asymmetric unit contains one molecule of the Ru-complex plus # two molecules of dichloromethane. _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_moiety 'C60 H77 Cl2 N2 P Ru, 2(C H2 Cl2)' _chemical_formula_sum 'C62 H81 Cl6 N2 P Ru' _chemical_formula_weight 1199.03 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 124 0.0033 0.0016 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; H H 162 0.0000 0.0000 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Cl Cl 12 0.1484 0.1585 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; N N 4 0.0061 0.0033 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; P P 2 -1.2594 0.8363 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; Ru Ru 2 0.1023 0.0942 ; International Tables for Crystallography (1992). Vol. C, Tables 4.2.6.8 and 6.1.1.4 ; _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6690(1) _cell_length_b 13.4007(1) _cell_length_c 20.8987(2) _cell_angle_alpha 91.2229(5) _cell_angle_beta 99.1757(6) _cell_angle_gamma 113.2695(5) _cell_volume 2950.90(4) _cell_formula_units_Z 2 _cell_measurement_temperature 160(1) _cell_measurement_reflns_used 128764 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_absorpt_correction_T_min 0.943 _exptl_absorpt_correction_T_max 0.981 _exptl_special_details ; Solvent used: dichloromethane / MeOH Cooling Device: Oxford Cryosystems Cryostream 700 Crystal mount: glued on a glass fibre Mosaicity (deg.): 0.460(1) Frames collected: 1188 Seconds exposure per frame: 120 Degrees rotation per frame: 0.6 Crystal-Detector distance (mm): 30.7 ; _diffrn_ambient_temperature 160(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Nonius FR590 sealed tube generator' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_detector '65 mm CCD camera on \k goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD area-detector diffractometer' _diffrn_measurement_method '\f and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_reflns_number 70098 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.04 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 10403 _reflns_number_gt 8712 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'COLLECT (Nonius, 2000)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. The asymmetric unit contains one molecule of the Ru-complex plus two molecules of dichloromethane. ; _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^)+(0.0539P)^2^+6.7226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10403 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.742 _refine_diff_density_min -1.751 _refine_diff_density_rms 0.087 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.75458(2) 0.31419(2) 0.741552(13) 0.01717(10) Uani 1 1 d . . . Cl1 Cl 0.61527(8) 0.39362(7) 0.69330(4) 0.0255(2) Uani 1 1 d . . . Cl2 Cl 0.92574(8) 0.26787(7) 0.79061(4) 0.0274(2) Uani 1 1 d . . . P1 P 0.80532(8) 0.28359(7) 0.63707(4) 0.0194(2) Uani 1 1 d . . . N1 N 0.8195(3) 0.4876(2) 0.85463(13) 0.0214(6) Uani 1 1 d . . . N3 N 0.6771(3) 0.3344(2) 0.87408(14) 0.0221(6) Uani 1 1 d . . . C2 C 0.7493(3) 0.3827(3) 0.82999(16) 0.0189(7) Uani 1 1 d . . . C4 C 0.6909(4) 0.4102(3) 0.93000(19) 0.0327(9) Uani 1 1 d . . . H41 H 0.7074 0.3806 0.9718 0.039 Uiso 1 1 calc R . . H42 H 0.6143 0.4257 0.9282 0.039 Uiso 1 1 calc R . . C5 C 0.8041(4) 0.5107(3) 0.92119(18) 0.0330(9) Uani 1 1 d . . . H51 H 0.7870 0.5771 0.9250 0.040 Uiso 1 1 calc R . . H52 H 0.8803 0.5197 0.9534 0.040 Uiso 1 1 calc R . . C6 C 0.9193(3) 0.5705(3) 0.82937(16) 0.0234(8) Uani 1 1 d . . . C7 C 1.0446(3) 0.5745(3) 0.84667(17) 0.0283(8) Uani 1 1 d . . . C8 C 1.0716(4) 0.4951(3) 0.88181(19) 0.0335(9) Uani 1 1 d . . . H8 H 1.0045 0.4365 0.8952 0.040 Uiso 1 1 calc R . . C9 C 1.1926(4) 0.5012(4) 0.8969(2) 0.0501(12) Uani 1 1 d . . . H9 H 1.2090 0.4466 0.9201 0.060 Uiso 1 1 calc R . . C10 C 1.2935(4) 0.5887(5) 0.8778(3) 0.0603(16) Uani 1 1 d . . . H10 H 1.3775 0.5926 0.8885 0.072 Uiso 1 1 calc R . . C11 C 1.2716(4) 0.6673(5) 0.8445(2) 0.0530(13) Uani 1 1 d . . . H11 H 1.3405 0.7254 0.8320 0.064 Uiso 1 1 calc R . . C12 C 1.1472(4) 0.6637(4) 0.82829(19) 0.0363(10) Uani 1 1 d . . . C13 C 1.1210(4) 0.7444(4) 0.7956(2) 0.0401(11) Uani 1 1 d . . . H13 H 1.1888 0.8042 0.7835 0.048 Uiso 1 1 calc R . . C14 C 1.0010(4) 0.7396(3) 0.78078(19) 0.0349(9) Uani 1 1 d . . . H14 H 0.9871 0.7961 0.7587 0.042 Uiso 1 1 calc R . . C15 C 0.8959(4) 0.6518(3) 0.79756(17) 0.0259(8) Uani 1 1 d . . . C16 C 0.5794(3) 0.2260(3) 0.86892(16) 0.0233(7) Uani 1 1 d . . . C17 C 0.4518(4) 0.2126(3) 0.84568(17) 0.0285(8) Uani 1 1 d . . . C18 C 0.4196(4) 0.2970(4) 0.82089(19) 0.0364(9) Uani 1 1 d . . . H18 H 0.4846 0.3659 0.8172 0.044 Uiso 1 1 calc R . . C19 C 0.2945(5) 0.2800(5) 0.8021(2) 0.0521(13) Uani 1 1 d . . . H19 H 0.2736 0.3378 0.7864 0.063 Uiso 1 1 calc R . . C20 C 0.1970(4) 0.1779(5) 0.8060(2) 0.0553(14) Uani 1 1 d . . . H20 H 0.1108 0.1676 0.7934 0.066 Uiso 1 1 calc R . . C21 C 0.2251(4) 0.0943(4) 0.8274(2) 0.0489(12) Uani 1 1 d . . . H21 H 0.1582 0.0253 0.8288 0.059 Uiso 1 1 calc R . . C22 C 0.3527(4) 0.1078(4) 0.84796(19) 0.0347(9) Uani 1 1 d . . . C23 C 0.3846(4) 0.0231(4) 0.8716(2) 0.0387(10) Uani 1 1 d . . . H23 H 0.3191 -0.0470 0.8724 0.046 Uiso 1 1 calc R . . C24 C 0.5072(4) 0.0392(3) 0.89338(19) 0.0355(9) Uani 1 1 d . . . H24 H 0.5254 -0.0198 0.9092 0.043 Uiso 1 1 calc R . . C25 C 0.6095(3) 0.1427(3) 0.89318(17) 0.0255(8) Uani 1 1 d . . . C26 C 0.7660(4) 0.6539(3) 0.78233(18) 0.0275(8) Uani 1 1 d . . . H26 H 0.7031 0.5819 0.7915 0.033 Uiso 1 1 calc R . . C27 C 0.7276(4) 0.6698(3) 0.71085(19) 0.0327(9) Uani 1 1 d . . . H271 H 0.7865 0.7418 0.7007 0.039 Uiso 1 1 calc R . . H272 H 0.7338 0.6129 0.6823 0.039 Uiso 1 1 calc R . . C28 C 0.5932(5) 0.6631(4) 0.6976(2) 0.0444(11) Uani 1 1 d . . . H281 H 0.5339 0.5893 0.7050 0.053 Uiso 1 1 calc R . . H282 H 0.5708 0.6746 0.6514 0.053 Uiso 1 1 calc R . . C29 C 0.5780(5) 0.7480(4) 0.7413(2) 0.0528(12) Uani 1 1 d . . . H291 H 0.6288 0.8220 0.7300 0.063 Uiso 1 1 calc R . . H292 H 0.4878 0.7376 0.7339 0.063 Uiso 1 1 calc R . . C30 C 0.6211(5) 0.7386(4) 0.8129(2) 0.0491(12) Uani 1 1 d . . . H301 H 0.5622 0.6688 0.8258 0.059 Uiso 1 1 calc R . . H302 H 0.6179 0.7988 0.8399 0.059 Uiso 1 1 calc R . . C31 C 0.7556(4) 0.7432(4) 0.8259(2) 0.0390(10) Uani 1 1 d . . . H311 H 0.7789 0.7332 0.8722 0.047 Uiso 1 1 calc R . . H312 H 0.8158 0.8158 0.8172 0.047 Uiso 1 1 calc R . . C32 C 0.7439(3) 0.1590(3) 0.92167(17) 0.0264(8) Uani 1 1 d . . . H32 H 0.8022 0.2275 0.9061 0.032 Uiso 1 1 calc R . . C33 C 0.7685(4) 0.1750(4) 0.99639(19) 0.0372(10) Uani 1 1 d . . . H331 H 0.7485 0.2364 1.0103 0.045 Uiso 1 1 calc R . . H332 H 0.7120 0.1083 1.0133 0.045 Uiso 1 1 calc R . . C34 C 0.9060(4) 0.1985(4) 1.0248(2) 0.0467(11) Uani 1 1 d . . . H341 H 0.9619 0.2688 1.0112 0.056 Uiso 1 1 calc R . . H342 H 0.9180 0.2054 1.0729 0.056 Uiso 1 1 calc R . . C35 C 0.9435(4) 0.1090(4) 1.0028(2) 0.0436(11) Uani 1 1 d . . . H351 H 0.8949 0.0405 1.0210 0.052 Uiso 1 1 calc R . . H352 H 1.0349 0.1295 1.0195 0.052 Uiso 1 1 calc R . . C36 C 0.9175(5) 0.0903(4) 0.9285(2) 0.0449(11) Uani 1 1 d . . . H361 H 0.9734 0.1560 0.9106 0.054 Uiso 1 1 calc R . . H362 H 0.9374 0.0283 0.9153 0.054 Uiso 1 1 calc R . . C37 C 0.7802(4) 0.0661(4) 0.90067(19) 0.0376(10) Uani 1 1 d . . . H371 H 0.7246 -0.0029 0.9158 0.045 Uiso 1 1 calc R . . H372 H 0.7666 0.0566 0.8526 0.045 Uiso 1 1 calc R . . C38 C 0.6449(3) 0.1727(3) 0.74564(17) 0.0238(8) Uani 1 1 d . . . H38 H 0.6857 0.1355 0.7724 0.029 Uiso 1 1 calc R . . C39 C 0.5116(3) 0.1001(3) 0.71937(17) 0.0253(8) Uani 1 1 d . . . C40 C 0.4178(4) 0.1340(3) 0.69035(19) 0.0310(9) Uani 1 1 d . . . H40 H 0.4370 0.2096 0.6887 0.037 Uiso 1 1 calc R . . C41 C 0.2978(4) 0.0581(4) 0.6642(2) 0.0394(10) Uani 1 1 d . . . H411 H 0.2348 0.0820 0.6449 0.047 Uiso 1 1 calc R . . C42 C 0.2681(4) -0.0521(3) 0.6660(2) 0.0416(10) Uani 1 1 d . . . H421 H 0.1854 -0.1039 0.6476 0.050 Uiso 1 1 calc R . . C43 C 0.3600(4) -0.0865(3) 0.6947(2) 0.0387(10) Uani 1 1 d . . . H43 H 0.3407 -0.1621 0.6960 0.046 Uiso 1 1 calc R . . C44 C 0.4777(4) -0.0116(3) 0.72093(18) 0.0297(8) Uani 1 1 d . . . H44 H 0.5393 -0.0364 0.7411 0.036 Uiso 1 1 calc R . . C45 C 0.6752(3) 0.2600(3) 0.56692(16) 0.0221(7) Uani 1 1 d . . . H45 H 0.6333 0.3085 0.5783 0.026 Uiso 1 1 calc R . . C46 C 0.5712(3) 0.1440(3) 0.55951(17) 0.0255(8) Uani 1 1 d . . . H461 H 0.6027 0.0921 0.5424 0.031 Uiso 1 1 calc R . . H462 H 0.5497 0.1231 0.6026 0.031 Uiso 1 1 calc R . . C47 C 0.4527(3) 0.1374(3) 0.51325(18) 0.0298(8) Uani 1 1 d . . . H471 H 0.4182 0.1860 0.5317 0.036 Uiso 1 1 calc R . . H472 H 0.3871 0.0619 0.5083 0.036 Uiso 1 1 calc R . . C48 C 0.4840(4) 0.1715(3) 0.44658(18) 0.0327(9) Uani 1 1 d . . . H481 H 0.5079 0.1172 0.4258 0.039 Uiso 1 1 calc R . . H482 H 0.4078 0.1724 0.4184 0.039 Uiso 1 1 calc R . . C49 C 0.5920(4) 0.2834(3) 0.45244(18) 0.0316(9) Uani 1 1 d . . . H491 H 0.5637 0.3390 0.4675 0.038 Uiso 1 1 calc R . . H492 H 0.6145 0.3002 0.4090 0.038 Uiso 1 1 calc R . . C50 C 0.7095(3) 0.2901(3) 0.49995(17) 0.0293(8) Uani 1 1 d . . . H501 H 0.7764 0.3650 0.5041 0.035 Uiso 1 1 calc R . . H502 H 0.7429 0.2394 0.4831 0.035 Uiso 1 1 calc R . . C51 C 0.8741(3) 0.1808(3) 0.63065(17) 0.0252(8) Uani 1 1 d . . . H511 H 0.9561 0.2104 0.6623 0.030 Uiso 1 1 calc R . . C52 C 0.7965(4) 0.0697(3) 0.65312(19) 0.0300(8) Uani 1 1 d . . . H521 H 0.7771 0.0805 0.6965 0.036 Uiso 1 1 calc R . . H522 H 0.7151 0.0336 0.6223 0.036 Uiso 1 1 calc R . . C53 C 0.8705(4) -0.0033(4) 0.6567(2) 0.0401(10) Uani 1 1 d . . . H531 H 0.9474 0.0295 0.6909 0.048 Uiso 1 1 calc R . . H532 H 0.8172 -0.0757 0.6691 0.048 Uiso 1 1 calc R . . C54 C 0.9091(5) -0.0176(4) 0.5924(2) 0.0449(11) Uani 1 1 d . . . H541 H 0.8324 -0.0586 0.5592 0.054 Uiso 1 1 calc R . . H542 H 0.9621 -0.0602 0.5975 0.054 Uiso 1 1 calc R . . C55 C 0.9836(4) 0.0933(4) 0.5695(2) 0.0456(11) Uani 1 1 d . . . H551 H 1.0648 0.1305 0.6004 0.055 Uiso 1 1 calc R . . H552 H 1.0037 0.0822 0.5264 0.055 Uiso 1 1 calc R . . C56 C 0.9099(4) 0.1657(3) 0.56476(19) 0.0328(9) Uani 1 1 d . . . H561 H 0.8321 0.1319 0.5312 0.039 Uiso 1 1 calc R . . H562 H 0.9626 0.2377 0.5516 0.039 Uiso 1 1 calc R . . C57 C 0.9329(3) 0.4107(3) 0.62018(17) 0.0233(7) Uani 1 1 d . . . H57 H 0.9477 0.3975 0.5755 0.028 Uiso 1 1 calc R . . C58 C 1.0604(4) 0.4431(4) 0.6668(2) 0.0386(10) Uani 1 1 d . . . H581 H 1.0860 0.3809 0.6683 0.046 Uiso 1 1 calc R . . H582 H 1.0520 0.4626 0.7112 0.046 Uiso 1 1 calc R . . C59 C 1.1616(4) 0.5410(4) 0.6428(2) 0.0431(11) Uani 1 1 d . . . H591 H 1.2430 0.5641 0.6738 0.052 Uiso 1 1 calc R . . H592 H 1.1749 0.5190 0.6000 0.052 Uiso 1 1 calc R . . C60 C 1.1222(4) 0.6369(3) 0.6363(2) 0.0443(11) Uani 1 1 d . . . H601 H 1.1216 0.6660 0.6802 0.053 Uiso 1 1 calc R . . H602 H 1.1855 0.6958 0.6169 0.053 Uiso 1 1 calc R . . C61 C 0.9922(4) 0.6045(3) 0.5944(2) 0.0430(11) Uani 1 1 d . . . H611 H 0.9957 0.5860 0.5488 0.052 Uiso 1 1 calc R . . H612 H 0.9669 0.6668 0.5951 0.052 Uiso 1 1 calc R . . C62 C 0.8935(4) 0.5065(3) 0.6189(2) 0.0368(10) Uani 1 1 d . . . H621 H 0.8852 0.5266 0.6633 0.044 Uiso 1 1 calc R . . H622 H 0.8100 0.4852 0.5901 0.044 Uiso 1 1 calc R . . Cl3 Cl 0.33112(19) 0.39200(19) 0.48363(9) 0.1024(7) Uani 1 1 d . . . Cl4 Cl 0.28042(16) 0.32969(18) 0.61265(13) 0.1124(8) Uani 1 1 d . . . Cl5 Cl 0.44832(19) 0.19124(14) 1.01727(8) 0.0813(5) Uani 1 1 d . . . Cl6 Cl 0.3864(2) 0.3794(2) 1.00515(10) 0.1113(8) Uani 1 1 d . . . C63 C 0.3876(5) 0.4112(5) 0.5680(3) 0.0606(14) Uani 1 1 d . . . H631 H 0.4652 0.3967 0.5767 0.073 Uiso 1 1 calc R . . H632 H 0.4115 0.4886 0.5831 0.073 Uiso 1 1 calc R . . C64 C 0.3281(6) 0.2325(7) 0.9935(4) 0.114(3) Uani 1 1 d . . . H641 H 0.2604 0.1992 1.0192 0.137 Uiso 1 1 calc R . . H642 H 0.2913 0.2075 0.9470 0.137 Uiso 1 1 calc R . . 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 0.01783(15) 0.01486(15) 0.01788(15) 0.00149(10) 0.00348(10) 0.00552(11) Cl1 0.0289(5) 0.0234(4) 0.0275(4) 0.0036(3) 0.0031(3) 0.0147(4) Cl2 0.0263(4) 0.0311(5) 0.0256(4) 0.0023(4) 0.0022(3) 0.0136(4) P1 0.0201(4) 0.0163(4) 0.0201(4) 0.0003(3) 0.0033(3) 0.0055(4) N1 0.0267(16) 0.0178(15) 0.0183(14) -0.0003(11) 0.0054(12) 0.0072(12) N3 0.0271(16) 0.0191(15) 0.0209(15) 0.0019(12) 0.0076(12) 0.0091(13) C2 0.0183(16) 0.0187(17) 0.0220(17) 0.0041(14) 0.0022(13) 0.0103(14) C4 0.046(2) 0.024(2) 0.028(2) -0.0001(16) 0.0172(17) 0.0096(18) C5 0.044(2) 0.026(2) 0.0243(19) -0.0013(16) 0.0126(17) 0.0068(18) C6 0.0230(18) 0.0200(18) 0.0212(17) -0.0040(14) 0.0043(14) 0.0025(15) C7 0.0270(19) 0.030(2) 0.0228(18) -0.0094(15) 0.0016(15) 0.0084(16) C8 0.028(2) 0.039(2) 0.029(2) -0.0104(17) -0.0028(16) 0.0129(18) C9 0.044(3) 0.067(3) 0.042(3) -0.015(2) -0.010(2) 0.033(3) C10 0.026(2) 0.093(4) 0.056(3) -0.025(3) -0.005(2) 0.024(3) C11 0.027(2) 0.068(4) 0.049(3) -0.017(3) 0.008(2) 0.004(2) C12 0.024(2) 0.045(3) 0.030(2) -0.0136(18) 0.0058(16) 0.0029(18) C13 0.035(2) 0.032(2) 0.036(2) -0.0054(18) 0.0142(18) -0.0070(18) C14 0.039(2) 0.024(2) 0.031(2) 0.0000(16) 0.0103(17) 0.0019(17) C15 0.032(2) 0.0191(18) 0.0218(18) -0.0023(14) 0.0066(15) 0.0046(15) C16 0.0240(18) 0.0233(19) 0.0209(17) 0.0019(14) 0.0082(14) 0.0062(15) C17 0.0277(19) 0.037(2) 0.0206(18) 0.0013(16) 0.0076(15) 0.0117(17) C18 0.034(2) 0.047(3) 0.034(2) 0.0032(19) 0.0062(17) 0.023(2) C19 0.054(3) 0.073(4) 0.043(3) 0.002(2) 0.001(2) 0.042(3) C20 0.028(2) 0.087(4) 0.048(3) -0.009(3) 0.000(2) 0.024(3) C21 0.029(2) 0.064(3) 0.042(3) -0.004(2) 0.0065(19) 0.007(2) C22 0.024(2) 0.045(3) 0.027(2) 0.0002(18) 0.0066(16) 0.0049(18) C23 0.033(2) 0.035(2) 0.034(2) 0.0048(18) 0.0086(18) -0.0018(18) C24 0.040(2) 0.025(2) 0.034(2) 0.0091(17) 0.0078(18) 0.0045(18) C25 0.0297(19) 0.0232(19) 0.0210(17) 0.0047(14) 0.0077(15) 0.0069(16) C26 0.034(2) 0.0193(18) 0.0291(19) 0.0051(15) 0.0076(16) 0.0102(16) C27 0.047(2) 0.026(2) 0.029(2) 0.0072(16) 0.0077(17) 0.0186(18) C28 0.058(3) 0.042(3) 0.040(2) 0.007(2) -0.002(2) 0.031(2) C29 0.061(3) 0.053(3) 0.062(3) 0.012(2) 0.012(3) 0.040(3) C30 0.056(3) 0.045(3) 0.056(3) -0.003(2) 0.015(2) 0.028(2) C31 0.050(3) 0.034(2) 0.035(2) -0.0026(18) 0.0099(19) 0.018(2) C32 0.0280(19) 0.0234(19) 0.0263(19) 0.0061(15) 0.0056(15) 0.0085(16) C33 0.041(2) 0.045(3) 0.028(2) -0.0027(18) -0.0001(17) 0.022(2) C34 0.045(3) 0.055(3) 0.038(2) -0.008(2) -0.009(2) 0.026(2) C35 0.045(3) 0.052(3) 0.037(2) 0.005(2) -0.0022(19) 0.027(2) C36 0.056(3) 0.055(3) 0.040(2) 0.009(2) 0.007(2) 0.040(2) C37 0.056(3) 0.037(2) 0.028(2) 0.0031(17) 0.0033(19) 0.029(2) C38 0.0264(19) 0.0233(19) 0.0223(17) 0.0031(14) 0.0050(14) 0.0103(15) C39 0.0266(19) 0.0233(19) 0.0232(18) 0.0015(14) 0.0078(15) 0.0062(15) C40 0.027(2) 0.023(2) 0.041(2) 0.0052(17) 0.0057(17) 0.0076(16) C41 0.028(2) 0.036(2) 0.049(3) 0.0053(19) 0.0002(18) 0.0107(18) C42 0.025(2) 0.029(2) 0.057(3) -0.001(2) 0.0003(19) -0.0008(17) C43 0.042(2) 0.022(2) 0.047(2) 0.0031(18) 0.0085(19) 0.0071(18) C44 0.037(2) 0.0211(19) 0.032(2) 0.0046(16) 0.0110(17) 0.0105(17) C45 0.0239(18) 0.0181(18) 0.0220(17) 0.0021(14) 0.0029(14) 0.0066(15) C46 0.0258(19) 0.0224(19) 0.0232(18) 0.0009(14) 0.0009(14) 0.0059(15) C47 0.0245(19) 0.027(2) 0.031(2) 0.0019(16) -0.0006(15) 0.0053(16) C48 0.034(2) 0.032(2) 0.0260(19) 0.0006(16) -0.0034(16) 0.0108(18) C49 0.032(2) 0.032(2) 0.0259(19) 0.0062(16) -0.0006(16) 0.0103(17) C50 0.0259(19) 0.033(2) 0.0241(19) 0.0061(16) 0.0026(15) 0.0067(16) C51 0.0262(19) 0.0237(19) 0.0257(18) -0.0044(15) 0.0006(15) 0.0121(16) C52 0.037(2) 0.0224(19) 0.034(2) 0.0026(16) 0.0078(17) 0.0151(17) C53 0.045(2) 0.030(2) 0.049(3) 0.0030(19) 0.002(2) 0.021(2) C54 0.050(3) 0.035(2) 0.059(3) -0.004(2) 0.008(2) 0.027(2) C55 0.046(3) 0.045(3) 0.058(3) -0.002(2) 0.018(2) 0.027(2) C56 0.038(2) 0.032(2) 0.034(2) 0.0010(17) 0.0125(17) 0.0173(18) C57 0.0232(18) 0.0191(18) 0.0237(18) 0.0018(14) 0.0065(14) 0.0036(15) C58 0.025(2) 0.040(2) 0.035(2) 0.0066(18) 0.0012(17) -0.0016(18) C59 0.029(2) 0.044(3) 0.038(2) 0.010(2) 0.0024(18) -0.0041(19) C60 0.044(3) 0.030(2) 0.036(2) -0.0062(18) 0.0167(19) -0.0112(19) C61 0.045(3) 0.021(2) 0.062(3) 0.010(2) 0.022(2) 0.0075(19) C62 0.033(2) 0.022(2) 0.053(3) 0.0031(18) 0.0150(19) 0.0058(17) Cl3 0.0995(13) 0.1289(17) 0.0813(12) -0.0101(11) -0.0304(10) 0.0674(13) Cl4 0.0584(10) 0.1029(15) 0.191(2) 0.0801(15) 0.0449(12) 0.0366(10) Cl5 0.1191(14) 0.0650(10) 0.0685(9) 0.0166(8) 0.0295(9) 0.0413(10) Cl6 0.169(2) 0.1423(19) 0.0847(12) 0.0079(12) 0.0210(13) 0.1285(18) C63 0.055(3) 0.052(3) 0.071(4) 0.007(3) -0.003(3) 0.023(3) C64 0.051(4) 0.174(8) 0.089(5) -0.079(5) 0.020(3) 0.017(4) _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 C38 1.834(4) . ? Ru1 C2 2.067(3) . ? Ru1 Cl1 2.3839(9) . ? Ru1 Cl2 2.4040(9) . ? Ru1 P1 2.4191(9) . ? P1 C57 1.852(3) . ? P1 C45 1.857(3) . ? P1 C51 1.859(4) . ? N1 C2 1.355(4) . ? N1 C6 1.438(4) . ? N1 C5 1.473(4) . ? N3 C2 1.349(4) . ? N3 C16 1.438(4) . ? N3 C4 1.478(5) . ? C4 C5 1.508(5) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? C5 H51 0.9900 . ? C5 H52 0.9900 . ? C6 C15 1.383(5) . ? C6 C7 1.428(5) . ? C7 C8 1.412(6) . ? C7 C12 1.431(6) . ? C8 C9 1.367(6) . ? C8 H8 0.9500 . ? C9 C10 1.413(8) . ? C9 H9 0.9500 . ? C10 C11 1.359(8) . ? C10 H10 0.9500 . ? C11 C12 1.418(6) . ? C11 H11 0.9500 . ? C12 C13 1.399(7) . ? C13 C14 1.360(6) . ? C13 H13 0.9500 . ? C14 C15 1.423(5) . ? C14 H14 0.9500 . ? C15 C26 1.509(5) . ? C16 C25 1.380(5) . ? C16 C17 1.428(5) . ? C17 C18 1.410(6) . ? C17 C22 1.432(6) . ? C18 C19 1.374(6) . ? C18 H18 0.9500 . ? C19 C20 1.406(8) . ? C19 H19 0.9500 . ? C20 C21 1.352(8) . ? C20 H20 0.9500 . ? C21 C22 1.419(6) . ? C21 H21 0.9500 . ? C22 C23 1.404(6) . ? C23 C24 1.358(6) . ? C23 H23 0.9500 . ? C24 C25 1.429(5) . ? C24 H24 0.9500 . ? C25 C32 1.512(5) . ? C26 C27 1.534(5) . ? C26 C31 1.543(5) . ? C26 H26 1.0000 . ? C27 C28 1.515(6) . ? C27 H271 0.9900 . ? C27 H272 0.9900 . ? C28 C29 1.527(6) . ? C28 H281 0.9900 . ? C28 H282 0.9900 . ? C29 C30 1.525(7) . ? C29 H291 0.9900 . ? C29 H292 0.9900 . ? C30 C31 1.525(6) . ? C30 H301 0.9900 . ? C30 H302 0.9900 . ? C31 H311 0.9900 . ? C31 H312 0.9900 . ? C32 C33 1.536(5) . ? C32 C37 1.540(5) . ? C32 H32 1.0000 . ? C33 C34 1.521(6) . ? C33 H331 0.9900 . ? C33 H332 0.9900 . ? C34 C35 1.516(6) . ? C34 H341 0.9900 . ? C34 H342 0.9900 . ? C35 C36 1.530(6) . ? C35 H351 0.9900 . ? C35 H352 0.9900 . ? C36 C37 1.515(6) . ? C36 H361 0.9900 . ? C36 H362 0.9900 . ? C37 H371 0.9900 . ? C37 H372 0.9900 . ? C38 C39 1.475(5) . ? C38 H38 0.9500 . ? C39 C44 1.392(5) . ? C39 C40 1.403(5) . ? C40 C41 1.379(6) . ? C40 H40 0.9500 . ? C41 C42 1.380(6) . ? C41 H411 0.9500 . ? C42 C43 1.385(6) . ? C42 H421 0.9500 . ? C43 C44 1.357(6) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.535(5) . ? C45 C50 1.535(5) . ? C45 H45 1.0000 . ? C46 C47 1.526(5) . ? C46 H461 0.9900 . ? C46 H462 0.9900 . ? C47 C48 1.530(5) . ? C47 H471 0.9900 . ? C47 H472 0.9900 . ? C48 C49 1.518(5) . ? C48 H481 0.9900 . ? C48 H482 0.9900 . ? C49 C50 1.529(5) . ? C49 H491 0.9900 . ? C49 H492 0.9900 . ? C50 H501 0.9900 . ? C50 H502 0.9900 . ? C51 C56 1.533(5) . ? C51 C52 1.536(5) . ? C51 H511 1.0000 . ? C52 C53 1.535(5) . ? C52 H521 0.9900 . ? C52 H522 0.9900 . ? C53 C54 1.517(6) . ? C53 H531 0.9900 . ? C53 H532 0.9900 . ? C54 C55 1.527(7) . ? C54 H541 0.9900 . ? C54 H542 0.9900 . ? C55 C56 1.526(6) . ? C55 H551 0.9900 . ? C55 H552 0.9900 . ? C56 H561 0.9900 . ? C56 H562 0.9900 . ? C57 C62 1.525(5) . ? C57 C58 1.536(5) . ? C57 H57 1.0000 . ? C58 C59 1.536(5) . ? C58 H581 0.9900 . ? C58 H582 0.9900 . ? C59 C60 1.528(7) . ? C59 H591 0.9900 . ? C59 H592 0.9900 . ? C60 C61 1.516(6) . ? C60 H601 0.9900 . ? C60 H602 0.9900 . ? C61 C62 1.528(5) . ? C61 H611 0.9900 . ? C61 H612 0.9900 . ? C62 H621 0.9900 . ? C62 H622 0.9900 . ? Cl3 C63 1.756(6) . ? Cl4 C63 1.722(6) . ? Cl5 C64 1.709(8) . ? Cl6 C64 1.807(9) . ? C63 H631 0.9900 . ? C63 H632 0.9900 . ? C64 H641 0.9900 . ? C64 H642 0.9900 . ? 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 C38 Ru1 C2 99.64(14) . . ? C38 Ru1 Cl1 102.28(12) . . ? C2 Ru1 Cl1 86.80(9) . . ? C38 Ru1 Cl2 88.49(12) . . ? C2 Ru1 Cl2 91.28(9) . . ? Cl1 Ru1 Cl2 169.22(3) . . ? C38 Ru1 P1 96.10(11) . . ? C2 Ru1 P1 164.18(10) . . ? Cl1 Ru1 P1 91.39(3) . . ? Cl2 Ru1 P1 87.58(3) . . ? C57 P1 C45 102.77(16) . . ? C57 P1 C51 102.78(17) . . ? C45 P1 C51 110.37(16) . . ? C57 P1 Ru1 108.54(11) . . ? C45 P1 Ru1 114.20(11) . . ? C51 P1 Ru1 116.57(12) . . ? C2 N1 C6 128.5(3) . . ? C2 N1 C5 113.4(3) . . ? C6 N1 C5 117.1(3) . . ? C2 N3 C16 128.5(3) . . ? C2 N3 C4 113.4(3) . . ? C16 N3 C4 117.5(3) . . ? N3 C2 N1 106.5(3) . . ? N3 C2 Ru1 128.0(2) . . ? N1 C2 Ru1 125.5(2) . . ? N3 C4 C5 102.4(3) . . ? N3 C4 H41 111.3 . . ? C5 C4 H41 111.3 . . ? N3 C4 H42 111.3 . . ? C5 C4 H42 111.3 . . ? H41 C4 H42 109.2 . . ? N1 C5 C4 102.5(3) . . ? N1 C5 H51 111.3 . . ? C4 C5 H51 111.3 . . ? N1 C5 H52 111.3 . . ? C4 C5 H52 111.3 . . ? H51 C5 H52 109.2 . . ? C15 C6 C7 121.9(3) . . ? C15 C6 N1 119.8(3) . . ? C7 C6 N1 117.6(3) . . ? C8 C7 C6 122.9(4) . . ? C8 C7 C12 118.7(4) . . ? C6 C7 C12 118.4(4) . . ? C9 C8 C7 121.1(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 119.9(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.8(5) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C13 C12 C11 122.7(4) . . ? C13 C12 C7 118.7(4) . . ? C11 C12 C7 118.7(4) . . ? C14 C13 C12 121.7(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 121.6(4) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C6 C15 C14 117.7(4) . . ? C6 C15 C26 123.3(3) . . ? C14 C15 C26 118.9(3) . . ? C25 C16 C17 122.7(3) . . ? C25 C16 N3 119.5(3) . . ? C17 C16 N3 117.4(3) . . ? C18 C17 C16 123.3(4) . . ? C18 C17 C22 119.0(4) . . ? C16 C17 C22 117.7(4) . . ? C19 C18 C17 120.2(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 121.2(5) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 122.4(4) . . ? C23 C22 C17 119.2(4) . . ? C21 C22 C17 118.4(4) . . ? C24 C23 C22 121.3(4) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C25 121.8(4) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C16 C25 C24 117.4(4) . . ? C16 C25 C32 122.6(3) . . ? C24 C25 C32 120.0(3) . . ? C15 C26 C27 113.2(3) . . ? C15 C26 C31 111.9(3) . . ? C27 C26 C31 108.7(3) . . ? C15 C26 H26 107.6 . . ? C27 C26 H26 107.6 . . ? C31 C26 H26 107.6 . . ? C28 C27 C26 110.6(3) . . ? C28 C27 H271 109.5 . . ? C26 C27 H271 109.5 . . ? C28 C27 H272 109.5 . . ? C26 C27 H272 109.5 . . ? H271 C27 H272 108.1 . . ? C27 C28 C29 111.6(4) . . ? C27 C28 H281 109.3 . . ? C29 C28 H281 109.3 . . ? C27 C28 H282 109.3 . . ? C29 C28 H282 109.3 . . ? H281 C28 H282 108.0 . . ? C30 C29 C28 111.0(4) . . ? C30 C29 H291 109.4 . . ? C28 C29 H291 109.4 . . ? C30 C29 H292 109.4 . . ? C28 C29 H292 109.4 . . ? H291 C29 H292 108.0 . . ? C29 C30 C31 111.6(4) . . ? C29 C30 H301 109.3 . . ? C31 C30 H301 109.3 . . ? C29 C30 H302 109.3 . . ? C31 C30 H302 109.3 . . ? H301 C30 H302 108.0 . . ? C30 C31 C26 110.9(4) . . ? C30 C31 H311 109.5 . . ? C26 C31 H311 109.5 . . ? C30 C31 H312 109.5 . . ? C26 C31 H312 109.5 . . ? H311 C31 H312 108.0 . . ? C25 C32 C33 111.2(3) . . ? C25 C32 C37 114.1(3) . . ? C33 C32 C37 108.9(3) . . ? C25 C32 H32 107.4 . . ? C33 C32 H32 107.4 . . ? C37 C32 H32 107.4 . . ? C34 C33 C32 111.2(3) . . ? C34 C33 H331 109.4 . . ? C32 C33 H331 109.4 . . ? C34 C33 H332 109.4 . . ? C32 C33 H332 109.4 . . ? H331 C33 H332 108.0 . . ? C35 C34 C33 111.7(4) . . ? C35 C34 H341 109.3 . . ? C33 C34 H341 109.3 . . ? C35 C34 H342 109.3 . . ? C33 C34 H342 109.3 . . ? H341 C34 H342 108.0 . . ? C34 C35 C36 110.9(4) . . ? C34 C35 H351 109.5 . . ? C36 C35 H351 109.5 . . ? C34 C35 H352 109.5 . . ? C36 C35 H352 109.5 . . ? H351 C35 H352 108.1 . . ? C37 C36 C35 111.1(4) . . ? C37 C36 H361 109.4 . . ? C35 C36 H361 109.4 . . ? C37 C36 H362 109.4 . . ? C35 C36 H362 109.4 . . ? H361 C36 H362 108.0 . . ? C36 C37 C32 111.2(4) . . ? C36 C37 H371 109.4 . . ? C32 C37 H371 109.4 . . ? C36 C37 H372 109.4 . . ? C32 C37 H372 109.4 . . ? H371 C37 H372 108.0 . . ? C39 C38 Ru1 138.3(3) . . ? C39 C38 H38 110.9 . . ? Ru1 C38 H38 110.9 . . ? C44 C39 C40 117.3(3) . . ? C44 C39 C38 117.2(3) . . ? C40 C39 C38 125.4(3) . . ? C41 C40 C39 120.3(4) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.7(4) . . ? C40 C41 H411 119.6 . . ? C42 C41 H411 119.6 . . ? C41 C42 C43 119.4(4) . . ? C41 C42 H421 120.3 . . ? C43 C42 H421 120.3 . . ? C44 C43 C42 119.7(4) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C39 122.5(4) . . ? C43 C44 H44 118.8 . . ? C39 C44 H44 118.8 . . ? C46 C45 C50 108.9(3) . . ? C46 C45 P1 112.8(2) . . ? C50 C45 P1 118.6(2) . . ? C46 C45 H45 105.1 . . ? C50 C45 H45 105.1 . . ? P1 C45 H45 105.1 . . ? C47 C46 C45 110.5(3) . . ? C47 C46 H461 109.6 . . ? C45 C46 H461 109.6 . . ? C47 C46 H462 109.6 . . ? C45 C46 H462 109.6 . . ? H461 C46 H462 108.1 . . ? C46 C47 C48 110.5(3) . . ? C46 C47 H471 109.5 . . ? C48 C47 H471 109.5 . . ? C46 C47 H472 109.5 . . ? C48 C47 H472 109.5 . . ? H471 C47 H472 108.1 . . ? C49 C48 C47 111.4(3) . . ? C49 C48 H481 109.3 . . ? C47 C48 H481 109.3 . . ? C49 C48 H482 109.3 . . ? C47 C48 H482 109.3 . . ? H481 C48 H482 108.0 . . ? C48 C49 C50 111.9(3) . . ? C48 C49 H491 109.2 . . ? C50 C49 H491 109.2 . . ? C48 C49 H492 109.2 . . ? C50 C49 H492 109.2 . . ? H491 C49 H492 107.9 . . ? C49 C50 C45 109.9(3) . . ? C49 C50 H501 109.7 . . ? C45 C50 H501 109.7 . . ? C49 C50 H502 109.7 . . ? C45 C50 H502 109.7 . . ? H501 C50 H502 108.2 . . ? C56 C51 C52 110.4(3) . . ? C56 C51 P1 115.7(3) . . ? C52 C51 P1 114.2(3) . . ? C56 C51 H511 105.1 . . ? C52 C51 H511 105.1 . . ? P1 C51 H511 105.1 . . ? C53 C52 C51 110.5(3) . . ? C53 C52 H521 109.5 . . ? C51 C52 H521 109.5 . . ? C53 C52 H522 109.5 . . ? C51 C52 H522 109.5 . . ? H521 C52 H522 108.1 . . ? C54 C53 C52 111.9(4) . . ? C54 C53 H531 109.2 . . ? C52 C53 H531 109.2 . . ? C54 C53 H532 109.2 . . ? C52 C53 H532 109.2 . . ? H531 C53 H532 107.9 . . ? C53 C54 C55 110.5(4) . . ? C53 C54 H541 109.5 . . ? C55 C54 H541 109.5 . . ? C53 C54 H542 109.5 . . ? C55 C54 H542 109.5 . . ? H541 C54 H542 108.1 . . ? C56 C55 C54 112.1(4) . . ? C56 C55 H551 109.2 . . ? C54 C55 H551 109.2 . . ? C56 C55 H552 109.2 . . ? C54 C55 H552 109.2 . . ? H551 C55 H552 107.9 . . ? C55 C56 C51 110.1(3) . . ? C55 C56 H561 109.6 . . ? C51 C56 H561 109.6 . . ? C55 C56 H562 109.6 . . ? C51 C56 H562 109.6 . . ? H561 C56 H562 108.2 . . ? C62 C57 C58 109.3(3) . . ? C62 C57 P1 112.0(2) . . ? C58 C57 P1 114.4(3) . . ? C62 C57 H57 106.9 . . ? C58 C57 H57 106.9 . . ? P1 C57 H57 106.9 . . ? C57 C58 C59 109.3(3) . . ? C57 C58 H581 109.8 . . ? C59 C58 H581 109.8 . . ? C57 C58 H582 109.8 . . ? C59 C58 H582 109.8 . . ? H581 C58 H582 108.3 . . ? C60 C59 C58 111.4(4) . . ? C60 C59 H591 109.4 . . ? C58 C59 H591 109.4 . . ? C60 C59 H592 109.4 . . ? C58 C59 H592 109.4 . . ? H591 C59 H592 108.0 . . ? C61 C60 C59 112.2(3) . . ? C61 C60 H601 109.2 . . ? C59 C60 H601 109.2 . . ? C61 C60 H602 109.2 . . ? C59 C60 H602 109.2 . . ? H601 C60 H602 107.9 . . ? C60 C61 C62 110.9(4) . . ? C60 C61 H611 109.5 . . ? C62 C61 H611 109.5 . . ? C60 C61 H612 109.5 . . ? C62 C61 H612 109.5 . . ? H611 C61 H612 108.0 . . ? C57 C62 C61 110.2(3) . . ? C57 C62 H621 109.6 . . ? C61 C62 H621 109.6 . . ? C57 C62 H622 109.6 . . ? C61 C62 H622 109.6 . . ? H621 C62 H622 108.1 . . ? Cl4 C63 Cl3 114.2(3) . . ? Cl4 C63 H631 108.7 . . ? Cl3 C63 H631 108.7 . . ? Cl4 C63 H632 108.7 . . ? Cl3 C63 H632 108.7 . . ? H631 C63 H632 107.6 . . ? Cl5 C64 Cl6 110.5(4) . . ? Cl5 C64 H641 109.6 . . ? Cl6 C64 H641 109.6 . . ? Cl5 C64 H642 109.6 . . ? Cl6 C64 H642 109.6 . . ? H641 C64 H642 108.1 . . ? 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 C38 Ru1 P1 C57 -173.56(17) . . . . ? C2 Ru1 P1 C57 0.8(4) . . . . ? Cl1 Ru1 P1 C57 83.93(12) . . . . ? Cl2 Ru1 P1 C57 -85.34(12) . . . . ? C38 Ru1 P1 C45 72.47(17) . . . . ? C2 Ru1 P1 C45 -113.2(3) . . . . ? Cl1 Ru1 P1 C45 -30.04(12) . . . . ? Cl2 Ru1 P1 C45 160.69(12) . . . . ? C38 Ru1 P1 C51 -58.19(17) . . . . ? C2 Ru1 P1 C51 116.2(4) . . . . ? Cl1 Ru1 P1 C51 -160.70(13) . . . . ? Cl2 Ru1 P1 C51 30.04(13) . . . . ? C16 N3 C2 N1 174.7(3) . . . . ? C4 N3 C2 N1 3.9(4) . . . . ? C16 N3 C2 Ru1 -4.9(5) . . . . ? C4 N3 C2 Ru1 -175.8(3) . . . . ? C6 N1 C2 N3 173.9(3) . . . . ? C5 N1 C2 N3 5.5(4) . . . . ? C6 N1 C2 Ru1 -6.5(5) . . . . ? C5 N1 C2 Ru1 -174.9(3) . . . . ? C38 Ru1 C2 N3 -4.0(3) . . . . ? Cl1 Ru1 C2 N3 98.0(3) . . . . ? Cl2 Ru1 C2 N3 -92.6(3) . . . . ? P1 Ru1 C2 N3 -178.26(19) . . . . ? C38 Ru1 C2 N1 176.5(3) . . . . ? Cl1 Ru1 C2 N1 -81.6(3) . . . . ? Cl2 Ru1 C2 N1 87.8(3) . . . . ? P1 Ru1 C2 N1 2.2(6) . . . . ? C2 N3 C4 C5 -11.0(4) . . . . ? C16 N3 C4 C5 177.1(3) . . . . ? C2 N1 C5 C4 -12.0(4) . . . . ? C6 N1 C5 C4 178.2(3) . . . . ? N3 C4 C5 N1 12.6(4) . . . . ? C2 N1 C6 C15 103.7(4) . . . . ? C5 N1 C6 C15 -88.2(4) . . . . ? C2 N1 C6 C7 -85.3(4) . . . . ? C5 N1 C6 C7 82.8(4) . . . . ? C15 C6 C7 C8 177.0(3) . . . . ? N1 C6 C7 C8 6.2(5) . . . . ? C15 C6 C7 C12 -2.2(5) . . . . ? N1 C6 C7 C12 -173.0(3) . . . . ? C6 C7 C8 C9 179.3(4) . . . . ? C12 C7 C8 C9 -1.6(6) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? C8 C9 C10 C11 -0.1(7) . . . . ? C9 C10 C11 C12 0.3(7) . . . . ? C10 C11 C12 C13 178.2(4) . . . . ? C10 C11 C12 C7 -1.1(6) . . . . ? C8 C7 C12 C13 -177.6(4) . . . . ? C6 C7 C12 C13 1.5(5) . . . . ? C8 C7 C12 C11 1.7(5) . . . . ? C6 C7 C12 C11 -179.2(3) . . . . ? C11 C12 C13 C14 -179.7(4) . . . . ? C7 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 -0.2(6) . . . . ? C7 C6 C15 C14 1.6(5) . . . . ? N1 C6 C15 C14 172.2(3) . . . . ? C7 C6 C15 C26 -176.0(3) . . . . ? N1 C6 C15 C26 -5.4(5) . . . . ? C13 C14 C15 C6 -0.4(5) . . . . ? C13 C14 C15 C26 177.3(4) . . . . ? C2 N3 C16 C25 93.9(4) . . . . ? C4 N3 C16 C25 -95.6(4) . . . . ? C2 N3 C16 C17 -93.5(4) . . . . ? C4 N3 C16 C17 77.0(4) . . . . ? C25 C16 C17 C18 179.9(3) . . . . ? N3 C16 C17 C18 7.5(5) . . . . ? C25 C16 C17 C22 -0.1(5) . . . . ? N3 C16 C17 C22 -172.5(3) . . . . ? C16 C17 C18 C19 -177.0(4) . . . . ? C22 C17 C18 C19 3.0(6) . . . . ? C17 C18 C19 C20 -1.4(7) . . . . ? C18 C19 C20 C21 -0.9(7) . . . . ? C19 C20 C21 C22 1.4(7) . . . . ? C20 C21 C22 C23 178.8(4) . . . . ? C20 C21 C22 C17 0.2(6) . . . . ? C18 C17 C22 C23 179.0(4) . . . . ? C16 C17 C22 C23 -1.0(5) . . . . ? C18 C17 C22 C21 -2.4(6) . . . . ? C16 C17 C22 C21 177.6(3) . . . . ? C21 C22 C23 C24 -177.4(4) . . . . ? C17 C22 C23 C24 1.2(6) . . . . ? C22 C23 C24 C25 -0.2(6) . . . . ? C17 C16 C25 C24 1.1(5) . . . . ? N3 C16 C25 C24 173.3(3) . . . . ? C17 C16 C25 C32 -176.0(3) . . . . ? N3 C16 C25 C32 -3.8(5) . . . . ? C23 C24 C25 C16 -1.0(6) . . . . ? C23 C24 C25 C32 176.3(4) . . . . ? C6 C15 C26 C27 -129.2(4) . . . . ? C14 C15 C26 C27 53.3(4) . . . . ? C6 C15 C26 C31 107.6(4) . . . . ? C14 C15 C26 C31 -69.9(4) . . . . ? C15 C26 C27 C28 175.9(3) . . . . ? C31 C26 C27 C28 -59.1(4) . . . . ? C26 C27 C28 C29 58.1(5) . . . . ? C27 C28 C29 C30 -54.7(6) . . . . ? C28 C29 C30 C31 53.7(6) . . . . ? C29 C30 C31 C26 -56.3(5) . . . . ? C15 C26 C31 C30 -176.0(3) . . . . ? C27 C26 C31 C30 58.2(4) . . . . ? C16 C25 C32 C33 99.0(4) . . . . ? C24 C25 C32 C33 -78.1(4) . . . . ? C16 C25 C32 C37 -137.3(4) . . . . ? C24 C25 C32 C37 45.6(5) . . . . ? C25 C32 C33 C34 -176.4(4) . . . . ? C37 C32 C33 C34 57.0(5) . . . . ? C32 C33 C34 C35 -56.7(5) . . . . ? C33 C34 C35 C36 55.0(5) . . . . ? C34 C35 C36 C37 -55.3(5) . . . . ? C35 C36 C37 C32 57.4(5) . . . . ? C25 C32 C37 C36 177.4(3) . . . . ? C33 C32 C37 C36 -57.6(4) . . . . ? C2 Ru1 C38 C39 101.2(4) . . . . ? Cl1 Ru1 C38 C39 12.4(4) . . . . ? Cl2 Ru1 C38 C39 -167.8(4) . . . . ? P1 Ru1 C38 C39 -80.4(4) . . . . ? Ru1 C38 C39 C44 162.3(3) . . . . ? Ru1 C38 C39 C40 -14.7(6) . . . . ? C44 C39 C40 C41 -0.5(6) . . . . ? C38 C39 C40 C41 176.4(4) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C40 C41 C42 C43 0.5(7) . . . . ? C41 C42 C43 C44 0.2(7) . . . . ? C42 C43 C44 C39 -1.1(6) . . . . ? C40 C39 C44 C43 1.2(6) . . . . ? C38 C39 C44 C43 -176.0(4) . . . . ? C57 P1 C45 C46 164.6(3) . . . . ? C51 P1 C45 C46 55.6(3) . . . . ? Ru1 P1 C45 C46 -78.0(3) . . . . ? C57 P1 C45 C50 35.6(3) . . . . ? C51 P1 C45 C50 -73.5(3) . . . . ? Ru1 P1 C45 C50 152.9(2) . . . . ? C50 C45 C46 C47 -60.5(4) . . . . ? P1 C45 C46 C47 165.6(2) . . . . ? C45 C46 C47 C48 58.1(4) . . . . ? C46 C47 C48 C49 -54.5(4) . . . . ? C47 C48 C49 C50 54.2(5) . . . . ? C48 C49 C50 C45 -56.7(4) . . . . ? C46 C45 C50 C49 59.1(4) . . . . ? P1 C45 C50 C49 -170.0(3) . . . . ? C57 P1 C51 C56 -59.3(3) . . . . ? C45 P1 C51 C56 49.7(3) . . . . ? Ru1 P1 C51 C56 -177.9(2) . . . . ? C57 P1 C51 C52 170.8(3) . . . . ? C45 P1 C51 C52 -80.2(3) . . . . ? Ru1 P1 C51 C52 52.2(3) . . . . ? C56 C51 C52 C53 56.8(4) . . . . ? P1 C51 C52 C53 -170.8(3) . . . . ? C51 C52 C53 C54 -56.0(5) . . . . ? C52 C53 C54 C55 54.9(5) . . . . ? C53 C54 C55 C56 -55.7(5) . . . . ? C54 C55 C56 C51 57.0(5) . . . . ? C52 C51 C56 C55 -57.2(4) . . . . ? P1 C51 C56 C55 171.1(3) . . . . ? C45 P1 C57 C62 61.9(3) . . . . ? C51 P1 C57 C62 176.6(3) . . . . ? Ru1 P1 C57 C62 -59.3(3) . . . . ? C45 P1 C57 C58 -172.9(3) . . . . ? C51 P1 C57 C58 -58.3(3) . . . . ? Ru1 P1 C57 C58 65.8(3) . . . . ? C62 C57 C58 C59 -60.3(4) . . . . ? P1 C57 C58 C59 173.2(3) . . . . ? C57 C58 C59 C60 56.5(5) . . . . ? C58 C59 C60 C61 -53.6(5) . . . . ? C59 C60 C61 C62 53.5(5) . . . . ? C58 C57 C62 C61 61.1(4) . . . . ? P1 C57 C62 C61 -171.0(3) . . . . ? C60 C61 C62 C57 -57.4(5) . . . . ? #===END