# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. Bruce' _publ_contact_author_email MICHAEL.BRUCE@ADELAIDE.EDU.AU _publ_section_title ; Some reactions of an ?3-tetracyanobutadienyl-ruthenium complex ; loop_ _publ_author_name 'M. Bruce' 'Mark Alexander Fox' 'Paul Low' 'Brian W. Skelton' 'Natasha N. Zaitseva' # Attachment '1.br1377c.cif' data_br1377c _database_code_depnum_ccdc_archive 'CCDC 730741' _audit_creation_date 2008-10-14T21:02:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C37 H25 N4 P Ru' _chemical_formula_moiety 'C37 H25 N4 P Ru' _chemical_formula_weight 657.65 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc 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 8.71670(10) _cell_length_b 17.6764(2) _cell_length_c 19.8463(2) _cell_angle_alpha 90 _cell_angle_beta 99.2310(10) _cell_angle_gamma 90 _cell_volume 3018.31(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12176 _cell_measurement_theta_min 3.3603 _cell_measurement_theta_max 67.0339 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.958 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.827 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0762737853 _diffrn_orient_matrix_ub_12 -0.0673407339 _diffrn_orient_matrix_ub_13 0.0316901226 _diffrn_orient_matrix_ub_21 -0.0843957767 _diffrn_orient_matrix_ub_22 -0.0228414097 _diffrn_orient_matrix_ub_23 -0.0713370519 _diffrn_orient_matrix_ub_31 0.1384130947 _diffrn_orient_matrix_ub_32 -0.0509208588 _diffrn_orient_matrix_ub_33 -0.0097576206 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0412 _diffrn_reflns_number 30233 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 67.12 _diffrn_reflns_theta_full 67.12 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 5340 _reflns_number_gt 4429 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.0760P] 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_number_reflns 5340 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.06 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.16147(3) 0.272678(12) 0.673871(11) 0.01333(10) Uani 1 1 d . . . P1 P 0.39848(9) 0.33221(4) 0.72111(4) 0.01401(17) Uani 1 1 d . . . C111 C 0.5303(4) 0.26675(17) 0.77334(16) 0.0158(6) Uani 1 1 d . . . C112 C 0.4772(4) 0.19594(19) 0.79085(18) 0.0231(7) Uani 1 1 d . . . H112 H 0.3743 0.1805 0.773 0.028 Uiso 1 1 calc R . . C113 C 0.5736(5) 0.1478(2) 0.83412(19) 0.0283(8) Uani 1 1 d . . . H113 H 0.5357 0.0999 0.8457 0.034 Uiso 1 1 calc R . . C114 C 0.7230(4) 0.1689(2) 0.86019(18) 0.0261(8) Uani 1 1 d . . . H114 H 0.7888 0.1357 0.8894 0.031 Uiso 1 1 calc R . . C115 C 0.7768(4) 0.2390(2) 0.84347(17) 0.0226(7) Uani 1 1 d . . . H115 H 0.8797 0.254 0.8618 0.027 Uiso 1 1 calc R . . C116 C 0.6825(4) 0.2874(2) 0.80046(17) 0.0205(7) Uani 1 1 d . . . H116 H 0.7215 0.3351 0.7892 0.025 Uiso 1 1 calc R . . C121 C 0.3647(4) 0.40541(18) 0.78202(17) 0.0170(6) Uani 1 1 d . . . C122 C 0.4006(4) 0.39512(19) 0.85264(17) 0.0213(7) Uani 1 1 d . . . H122 H 0.4459 0.3489 0.8704 0.026 Uiso 1 1 calc R . . C123 C 0.3703(4) 0.4521(2) 0.89689(18) 0.0273(8) Uani 1 1 d . . . H123 H 0.3948 0.4446 0.9448 0.033 Uiso 1 1 calc R . . C124 C 0.3048(5) 0.5196(2) 0.8716(2) 0.0302(8) Uani 1 1 d . . . H124 H 0.2837 0.5582 0.9021 0.036 Uiso 1 1 calc R . . C125 C 0.2702(5) 0.5308(2) 0.8018(2) 0.0301(8) Uani 1 1 d . . . H125 H 0.2266 0.5775 0.7844 0.036 Uiso 1 1 calc R . . C126 C 0.2987(4) 0.47432(19) 0.75700(18) 0.0221(7) Uani 1 1 d . . . H126 H 0.2735 0.4823 0.7092 0.027 Uiso 1 1 calc R . . C131 C 0.5203(4) 0.38518(17) 0.66973(16) 0.0161(6) Uani 1 1 d . . . C132 C 0.6184(4) 0.44249(19) 0.70064(18) 0.0213(7) Uani 1 1 d . . . H132 H 0.6187 0.4546 0.7473 0.026 Uiso 1 1 calc R . . C133 C 0.7153(4) 0.4818(2) 0.6637(2) 0.0267(8) Uani 1 1 d . . . H133 H 0.7829 0.5197 0.6855 0.032 Uiso 1 1 calc R . . C134 C 0.7140(5) 0.4662(2) 0.5954(2) 0.0305(9) Uani 1 1 d . . . H134 H 0.7793 0.4937 0.5701 0.037 Uiso 1 1 calc R . . C135 C 0.6169(4) 0.4100(2) 0.56383(19) 0.0265(8) Uani 1 1 d . . . H135 H 0.6151 0.3992 0.5168 0.032 Uiso 1 1 calc R . . C136 C 0.5217(4) 0.36932(19) 0.60122(17) 0.0212(7) Uani 1 1 d . . . H136 H 0.457 0.3303 0.5795 0.025 Uiso 1 1 calc R . . C1 C 0.2750(4) 0.18418(18) 0.62311(16) 0.0178(7) Uani 1 1 d . . . C2 C 0.1569(4) 0.22448(18) 0.57523(15) 0.0160(6) Uani 1 1 d . . . C3 C 0.1687(4) 0.30490(18) 0.57892(16) 0.0162(6) Uani 1 1 d . . . C4 C 0.1527(4) 0.36164(19) 0.53246(16) 0.0180(7) Uani 1 1 d . . . N11 N 0.5689(4) 0.19381(18) 0.61504(16) 0.0275(7) Uani 1 1 d . . . C11 C 0.4385(4) 0.19036(18) 0.61896(17) 0.0209(7) Uani 1 1 d . . . N12 N 0.2070(4) 0.05061(17) 0.66474(16) 0.0293(7) Uani 1 1 d . . . C12 C 0.2359(4) 0.10916(19) 0.64489(17) 0.0211(7) Uani 1 1 d . . . C21 C 0.0304(4) 0.18282(18) 0.53113(16) 0.0176(7) Uani 1 1 d . . . C22 C -0.1247(4) 0.2056(2) 0.52247(17) 0.0221(7) Uani 1 1 d . . . H22 H -0.1536 0.2494 0.5451 0.026 Uiso 1 1 calc R . . C23 C -0.2369(4) 0.1637(2) 0.48063(17) 0.0261(8) Uani 1 1 d . . . H23 H -0.3431 0.1782 0.4762 0.031 Uiso 1 1 calc R . . C24 C -0.1957(5) 0.1012(2) 0.44532(18) 0.0278(8) Uani 1 1 d . . . H24 H -0.2734 0.0729 0.417 0.033 Uiso 1 1 calc R . . C25 C -0.0419(5) 0.0801(2) 0.45139(19) 0.0306(9) Uani 1 1 d . . . H25 H -0.0129 0.0382 0.4262 0.037 Uiso 1 1 calc R . . C26 C 0.0711(4) 0.1206(2) 0.49462(19) 0.0274(8) Uani 1 1 d . . . H26 H 0.1769 0.1056 0.4992 0.033 Uiso 1 1 calc R . . C41 C 0.1411(4) 0.4387(2) 0.55453(16) 0.0215(7) Uani 1 1 d . . . N41 N 0.1327(4) 0.49975(18) 0.57271(16) 0.0332(8) Uani 1 1 d . . . C42 C 0.1614(4) 0.34877(19) 0.46187(18) 0.0222(7) Uani 1 1 d . . . N42 N 0.1715(4) 0.33704(19) 0.40591(16) 0.0344(8) Uani 1 1 d . . . C101 C -0.0639(4) 0.22412(18) 0.69113(17) 0.0184(7) Uani 1 1 d . . . H101 H -0.1179 0.1874 0.6613 0.022 Uiso 1 1 calc R . . C102 C 0.0447(4) 0.20864(19) 0.75047(17) 0.0193(7) Uani 1 1 d . . . H102 H 0.0747 0.1599 0.7681 0.023 Uiso 1 1 calc R . . C103 C 0.1005(4) 0.27831(19) 0.77872(17) 0.0207(7) Uani 1 1 d . . . H103 H 0.1761 0.2848 0.8184 0.025 Uiso 1 1 calc R . . C104 C 0.0232(4) 0.33837(19) 0.73701(17) 0.0200(7) Uani 1 1 d . . . H104 H 0.0382 0.3912 0.7443 0.024 Uiso 1 1 calc R . . C105 C -0.0786(4) 0.3039(2) 0.68362(17) 0.0200(7) Uani 1 1 d . . . H105 H -0.1457 0.3296 0.6485 0.024 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 0.01205(14) 0.01325(14) 0.01411(14) 0.00074(8) 0.00037(9) -0.00041(9) P1 0.0134(4) 0.0128(4) 0.0158(4) -0.0010(3) 0.0021(3) -0.0007(3) C111 0.0183(17) 0.0152(15) 0.0138(14) -0.0023(11) 0.0020(12) 0.0031(13) C112 0.0206(18) 0.0193(17) 0.0266(17) 0.0017(13) -0.0048(14) -0.0010(14) C113 0.035(2) 0.0178(16) 0.0297(19) 0.0056(14) -0.0005(16) 0.0023(15) C114 0.029(2) 0.0254(18) 0.0222(17) 0.0006(14) -0.0022(14) 0.0104(15) C115 0.0157(17) 0.034(2) 0.0176(16) 0.0010(14) -0.0002(13) 0.0050(14) C116 0.0172(17) 0.0236(17) 0.0215(16) 0.0003(13) 0.0053(13) 0.0013(14) C121 0.0110(16) 0.0160(15) 0.0238(16) -0.0038(13) 0.0023(12) -0.0025(12) C122 0.0184(17) 0.0219(17) 0.0233(17) -0.0010(13) 0.0030(13) -0.0036(14) C123 0.027(2) 0.034(2) 0.0215(17) -0.0076(15) 0.0062(14) -0.0078(16) C124 0.035(2) 0.0244(19) 0.035(2) -0.0123(15) 0.0158(17) -0.0060(16) C125 0.032(2) 0.0202(18) 0.040(2) -0.0052(15) 0.0104(17) 0.0009(15) C126 0.0213(18) 0.0202(17) 0.0251(17) -0.0029(14) 0.0044(14) 0.0024(14) C131 0.0129(16) 0.0139(15) 0.0216(16) 0.0035(12) 0.0035(12) 0.0016(12) C132 0.0184(18) 0.0188(16) 0.0271(18) -0.0019(13) 0.0051(14) 0.0006(13) C133 0.0244(19) 0.0172(17) 0.040(2) 0.0010(15) 0.0094(16) -0.0049(14) C134 0.027(2) 0.0224(18) 0.045(2) 0.0126(16) 0.0144(17) 0.0038(15) C135 0.0223(19) 0.033(2) 0.0254(18) 0.0054(15) 0.0079(15) 0.0025(15) C136 0.0151(17) 0.0223(17) 0.0252(17) 0.0025(13) 0.0004(13) 0.0019(13) C1 0.0162(17) 0.0168(15) 0.0190(16) -0.0038(12) -0.0017(12) -0.0001(13) C2 0.0136(16) 0.0214(17) 0.0124(14) -0.0014(12) 0.0003(12) 0.0018(13) C3 0.0097(15) 0.0175(16) 0.0203(16) -0.0007(12) -0.0014(12) -0.0010(12) C4 0.0180(17) 0.0193(16) 0.0158(15) 0.0006(12) -0.0003(12) -0.0026(13) N11 0.0186(18) 0.0282(16) 0.0356(17) -0.0053(13) 0.0041(13) 0.0035(13) C11 0.026(2) 0.0161(16) 0.0201(16) -0.0032(12) 0.0023(14) 0.0044(14) N12 0.0339(18) 0.0215(16) 0.0293(16) 0.0007(13) -0.0047(13) -0.0014(13) C12 0.0208(18) 0.0190(18) 0.0212(16) -0.0031(13) -0.0033(13) 0.0032(14) C21 0.0191(17) 0.0158(15) 0.0164(15) 0.0006(12) -0.0019(13) -0.0034(13) C22 0.0230(18) 0.0254(17) 0.0171(16) 0.0012(13) 0.0013(13) 0.0009(14) C23 0.0184(18) 0.039(2) 0.0198(17) 0.0017(15) -0.0016(13) -0.0037(15) C24 0.032(2) 0.0226(18) 0.0246(18) 0.0021(14) -0.0068(15) -0.0076(16) C25 0.037(2) 0.0206(18) 0.0304(19) -0.0087(15) -0.0063(16) 0.0017(16) C26 0.0223(19) 0.0222(17) 0.035(2) -0.0045(15) -0.0043(15) 0.0033(15) C41 0.0242(18) 0.0248(19) 0.0137(15) 0.0031(13) -0.0022(13) -0.0026(14) N41 0.047(2) 0.0193(16) 0.0294(17) -0.0023(13) -0.0046(15) 0.0013(14) C42 0.0215(18) 0.0201(16) 0.0243(19) 0.0006(14) 0.0012(14) -0.0064(14) N42 0.048(2) 0.0365(18) 0.0186(16) -0.0033(13) 0.0056(14) -0.0088(16) C101 0.0140(16) 0.0228(17) 0.0195(16) -0.0007(13) 0.0055(13) -0.0051(13) C102 0.0160(17) 0.0229(16) 0.0194(16) 0.0029(13) 0.0038(13) -0.0037(13) C103 0.0182(17) 0.0263(18) 0.0182(16) 0.0005(13) 0.0050(13) -0.0037(14) C104 0.0158(17) 0.0226(17) 0.0228(17) -0.0009(13) 0.0069(13) 0.0000(13) C105 0.0143(16) 0.0268(18) 0.0192(16) 0.0017(13) 0.0042(13) 0.0029(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 1.979(3) . ? Ru1 C2 2.130(3) . ? Ru1 C1 2.182(3) . ? Ru1 C105 2.203(3) . ? Ru1 C104 2.204(3) . ? Ru1 C101 2.220(3) . ? Ru1 C103 2.231(3) . ? Ru1 C102 2.264(3) . ? Ru1 P1 2.3734(8) . ? P1 C121 1.827(3) . ? P1 C111 1.831(3) . ? P1 C131 1.842(3) . ? C111 C112 1.397(5) . ? C111 C116 1.398(5) . ? C112 C113 1.392(5) . ? C112 H112 0.95 . ? C113 C114 1.374(6) . ? C113 H113 0.95 . ? C114 C115 1.384(5) . ? C114 H114 0.95 . ? C115 C116 1.383(5) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.398(5) . ? C121 C126 1.403(5) . ? C122 C123 1.389(5) . ? C122 H122 0.95 . ? C123 C124 1.382(6) . ? C123 H123 0.95 . ? C124 C125 1.386(6) . ? C124 H124 0.95 . ? C125 C126 1.385(5) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.390(5) . ? C131 C132 1.402(5) . ? C132 C133 1.390(5) . ? C132 H132 0.95 . ? C133 C134 1.382(6) . ? C133 H133 0.95 . ? C134 C135 1.387(6) . ? C134 H134 0.95 . ? C135 C136 1.398(5) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C1 C11 1.445(5) . ? C1 C12 1.452(5) . ? C1 C2 1.469(4) . ? C2 C3 1.426(5) . ? C2 C21 1.488(4) . ? C3 C4 1.354(5) . ? C4 C42 1.433(5) . ? C4 C41 1.439(5) . ? N11 C11 1.153(5) . ? N12 C12 1.150(5) . ? C21 C26 1.394(5) . ? C21 C22 1.394(5) . ? C22 C23 1.390(5) . ? C22 H22 0.95 . ? C23 C24 1.387(5) . ? C23 H23 0.95 . ? C24 C25 1.378(6) . ? C24 H24 0.95 . ? C25 C26 1.395(5) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C41 N41 1.144(5) . ? C42 N42 1.147(5) . ? C101 C102 1.414(5) . ? C101 C105 1.422(5) . ? C101 H101 0.95 . ? C102 C103 1.407(5) . ? C102 H102 0.95 . ? C103 C104 1.445(5) . ? C103 H103 0.95 . ? C104 C105 1.407(5) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? 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 C3 Ru1 C2 40.41(13) . . ? C3 Ru1 C1 71.38(12) . . ? C2 Ru1 C1 39.81(12) . . ? C3 Ru1 C105 100.79(12) . . ? C2 Ru1 C105 107.65(12) . . ? C1 Ru1 C105 136.72(13) . . ? C3 Ru1 C104 119.57(13) . . ? C2 Ru1 C104 143.35(12) . . ? C1 Ru1 C104 166.00(13) . . ? C105 Ru1 C104 37.24(12) . . ? C3 Ru1 C101 114.97(12) . . ? C2 Ru1 C101 95.78(12) . . ? C1 Ru1 C101 105.80(12) . . ? C105 Ru1 C101 37.50(13) . . ? C104 Ru1 C101 62.46(12) . . ? C3 Ru1 C103 157.50(13) . . ? C2 Ru1 C103 154.58(13) . . ? C1 Ru1 C103 131.01(12) . . ? C105 Ru1 C103 62.29(12) . . ? C104 Ru1 C103 38.02(12) . . ? C101 Ru1 C103 61.59(12) . . ? C3 Ru1 C102 150.41(12) . . ? C2 Ru1 C102 118.24(12) . . ? C1 Ru1 C102 103.75(13) . . ? C105 Ru1 C102 62.00(12) . . ? C104 Ru1 C102 62.34(13) . . ? C101 Ru1 C102 36.76(12) . . ? C103 Ru1 C102 36.48(12) . . ? C3 Ru1 P1 95.16(9) . . ? C2 Ru1 P1 115.29(9) . . ? C1 Ru1 P1 93.99(9) . . ? C105 Ru1 P1 129.29(9) . . ? C104 Ru1 P1 93.59(9) . . ? C101 Ru1 P1 147.79(9) . . ? C103 Ru1 P1 86.23(9) . . ? C102 Ru1 P1 114.40(9) . . ? C121 P1 C111 103.08(15) . . ? C121 P1 C131 100.07(15) . . ? C111 P1 C131 105.64(15) . . ? C121 P1 Ru1 110.66(11) . . ? C111 P1 Ru1 111.77(11) . . ? C131 P1 Ru1 123.33(11) . . ? C112 C111 C116 118.0(3) . . ? C112 C111 P1 120.3(3) . . ? C116 C111 P1 121.6(2) . . ? C113 C112 C111 120.7(3) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 120.6(3) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C113 C114 C115 119.3(3) . . ? C113 C114 H114 120.3 . . ? C115 C114 H114 120.3 . . ? C116 C115 C114 120.8(3) . . ? C116 C115 H115 119.6 . . ? C114 C115 H115 119.6 . . ? C115 C116 C111 120.7(3) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C122 C121 C126 118.7(3) . . ? C122 C121 P1 122.5(3) . . ? C126 C121 P1 118.8(3) . . ? C123 C122 C121 120.3(3) . . ? C123 C122 H122 119.8 . . ? C121 C122 H122 119.8 . . ? C124 C123 C122 120.4(3) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C123 C124 C125 119.8(3) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C126 C125 C124 120.4(4) . . ? C126 C125 H125 119.8 . . ? C124 C125 H125 119.8 . . ? C125 C126 C121 120.3(3) . . ? C125 C126 H126 119.9 . . ? C121 C126 H126 119.9 . . ? C136 C131 C132 118.3(3) . . ? C136 C131 P1 122.4(3) . . ? C132 C131 P1 119.4(3) . . ? C133 C132 C131 120.6(3) . . ? C133 C132 H132 119.7 . . ? C131 C132 H132 119.7 . . ? C134 C133 C132 120.5(3) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.6(3) . . ? C133 C134 H134 120.2 . . ? C135 C134 H134 120.2 . . ? C134 C135 C136 120.0(3) . . ? C134 C135 H135 120 . . ? C136 C135 H135 120 . . ? C131 C136 C135 121.0(3) . . ? C131 C136 H136 119.5 . . ? C135 C136 H136 119.5 . . ? C11 C1 C12 111.5(3) . . ? C11 C1 C2 121.5(3) . . ? C12 C1 C2 117.5(3) . . ? C11 C1 Ru1 119.8(2) . . ? C12 C1 Ru1 111.8(2) . . ? C2 C1 Ru1 68.17(17) . . ? C3 C2 C1 114.4(3) . . ? C3 C2 C21 124.3(3) . . ? C1 C2 C21 121.1(3) . . ? C3 C2 Ru1 64.12(17) . . ? C1 C2 Ru1 72.03(17) . . ? C21 C2 Ru1 129.9(2) . . ? C4 C3 C2 134.8(3) . . ? C4 C3 Ru1 147.7(3) . . ? C2 C3 Ru1 75.47(18) . . ? C3 C4 C42 122.1(3) . . ? C3 C4 C41 119.9(3) . . ? C42 C4 C41 117.7(3) . . ? N11 C11 C1 178.6(4) . . ? N12 C12 C1 177.3(4) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 C2 118.0(3) . . ? C22 C21 C2 122.8(3) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.7(3) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 119.9(3) . . ? C25 C24 H24 120 . . ? C23 C24 H24 120 . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.7(3) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? N41 C41 C4 179.3(4) . . ? N42 C42 C4 178.1(4) . . ? C102 C101 C105 108.4(3) . . ? C102 C101 Ru1 73.29(19) . . ? C105 C101 Ru1 70.57(18) . . ? C102 C101 H101 125.8 . . ? C105 C101 H101 125.8 . . ? Ru1 C101 H101 122 . . ? C103 C102 C101 107.7(3) . . ? C103 C102 Ru1 70.49(19) . . ? C101 C102 Ru1 69.95(18) . . ? C103 C102 H102 126.1 . . ? C101 C102 H102 126.1 . . ? Ru1 C102 H102 125 . . ? C102 C103 C104 108.4(3) . . ? C102 C103 Ru1 73.03(19) . . ? C104 C103 Ru1 69.97(18) . . ? C102 C103 H103 125.8 . . ? C104 C103 H103 125.8 . . ? Ru1 C103 H103 122.8 . . ? C105 C104 C103 107.0(3) . . ? C105 C104 Ru1 71.33(19) . . ? C103 C104 Ru1 72.00(19) . . ? C105 C104 H104 126.5 . . ? C103 C104 H104 126.5 . . ? Ru1 C104 H104 121.9 . . ? C104 C105 C101 108.4(3) . . ? C104 C105 Ru1 71.43(19) . . ? C101 C105 Ru1 71.93(19) . . ? C104 C105 H105 125.8 . . ? C101 C105 H105 125.8 . . ? Ru1 C105 H105 122.5 . . ? #===END # Attachment '2.br1381.cif' data_br1381 _database_code_depnum_ccdc_archive 'CCDC 730742' _audit_creation_date 2009-04-29T13:31:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C38 H29 N4 O P Ru' _chemical_formula_moiety 'C38 H29 N4 O P Ru' _chemical_formula_weight 689.69 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc 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 10.1827(1) _cell_length_b 19.0790(2) _cell_length_c 16.4900(1) _cell_angle_alpha 90 _cell_angle_beta 104.380(1) _cell_angle_gamma 90 _cell_volume 3103.24(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27994 _cell_measurement_theta_min 4.4074 _cell_measurement_theta_max 40.9843 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.92 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0363918656 _diffrn_orient_matrix_ub_12 0.0287197115 _diffrn_orient_matrix_ub_13 0.0219863089 _diffrn_orient_matrix_ub_21 0.0117660463 _diffrn_orient_matrix_ub_22 -0.0193372862 _diffrn_orient_matrix_ub_23 0.0377877166 _diffrn_orient_matrix_ub_31 0.0607965115 _diffrn_orient_matrix_ub_32 -0.0134520788 _diffrn_orient_matrix_ub_33 -0.0074440514 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_unetI/netI 0.0676 _diffrn_reflns_number 85683 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 41.09 _diffrn_reflns_theta_full 40.5 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 20107 _reflns_number_gt 11897 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_publication_material 'WinGX Farrugia, L. J. (1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 20107 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.423 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.123 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 0.285618(9) 0.531524(5) 0.189658(5) 0.01558(3) Uani 1 1 d . . . P1 P 0.20494(3) 0.557492(16) 0.305662(17) 0.01522(5) Uani 1 1 d . . . C111 C 0.02526(12) 0.58229(6) 0.27613(7) 0.0194(2) Uani 1 1 d . . . C112 C -0.06587(13) 0.53541(7) 0.22622(8) 0.0234(2) Uani 1 1 d . . . H112 H -0.0346 0.4909 0.2133 0.028 Uiso 1 1 calc R . . C113 C -0.20168(13) 0.55310(9) 0.19523(9) 0.0292(3) Uani 1 1 d . . . H113 H -0.2622 0.521 0.1609 0.035 Uiso 1 1 calc R . . C114 C -0.24862(14) 0.61772(9) 0.21452(11) 0.0344(3) Uani 1 1 d . . . H114 H -0.341 0.6302 0.1928 0.041 Uiso 1 1 calc R . . C115 C -0.16023(15) 0.66393(8) 0.26552(12) 0.0366(3) Uani 1 1 d . . . H115 H -0.193 0.7076 0.28 0.044 Uiso 1 1 calc R . . C116 C -0.02320(14) 0.64692(7) 0.29588(10) 0.0292(3) Uani 1 1 d . . . H116 H 0.0369 0.6794 0.3299 0.035 Uiso 1 1 calc R . . C121 C 0.28805(12) 0.63052(6) 0.37089(7) 0.01783(19) Uani 1 1 d . . . C122 C 0.25576(14) 0.64521(7) 0.44701(8) 0.0241(2) Uani 1 1 d . . . H122 H 0.1891 0.6179 0.4637 0.029 Uiso 1 1 calc R . . C123 C 0.32013(15) 0.69928(8) 0.49831(9) 0.0278(3) Uani 1 1 d . . . H123 H 0.2966 0.7091 0.5494 0.033 Uiso 1 1 calc R . . C124 C 0.41853(15) 0.73876(7) 0.47482(9) 0.0270(3) Uani 1 1 d . . . H124 H 0.4642 0.775 0.5104 0.032 Uiso 1 1 calc R . . C125 C 0.45034(13) 0.72530(7) 0.39932(8) 0.0235(2) Uani 1 1 d . . . H125 H 0.5169 0.7529 0.3828 0.028 Uiso 1 1 calc R . . C126 C 0.38542(12) 0.67157(6) 0.34752(7) 0.0198(2) Uani 1 1 d . . . H126 H 0.4078 0.6629 0.2958 0.024 Uiso 1 1 calc R . . C131 C 0.21512(12) 0.49130(6) 0.38741(7) 0.01708(19) Uani 1 1 d . . . C132 C 0.10336(13) 0.46636(7) 0.41354(8) 0.0219(2) Uani 1 1 d . . . H132 H 0.016 0.4855 0.3903 0.026 Uiso 1 1 calc R . . C133 C 0.11944(14) 0.41350(8) 0.47349(8) 0.0271(3) Uani 1 1 d . . . H133 H 0.043 0.3973 0.4914 0.033 Uiso 1 1 calc R . . C134 C 0.24576(15) 0.38445(7) 0.50721(8) 0.0280(3) Uani 1 1 d . . . H134 H 0.2556 0.3473 0.5466 0.034 Uiso 1 1 calc R . . C135 C 0.35815(14) 0.40997(7) 0.48302(8) 0.0260(3) Uani 1 1 d . . . H135 H 0.4454 0.3908 0.5066 0.031 Uiso 1 1 calc R . . C136 C 0.34265(12) 0.46348(7) 0.42445(8) 0.0207(2) Uani 1 1 d . . . H136 H 0.4202 0.4815 0.4093 0.025 Uiso 1 1 calc R . . C1 C 0.19229(13) 0.35093(7) 0.07858(7) 0.0212(2) Uani 1 1 d . . . C11 C 0.10018(14) 0.29977(7) 0.03163(8) 0.0259(3) Uani 1 1 d . . . N11 N 0.02993(15) 0.25739(7) -0.00519(9) 0.0379(3) Uani 1 1 d . . . C12 C 0.30374(15) 0.36954(7) 0.04435(8) 0.0270(3) Uani 1 1 d . . . N12 N 0.39049(15) 0.38524(8) 0.01502(9) 0.0403(3) Uani 1 1 d . . . C2 C 0.17889(12) 0.37907(6) 0.15252(7) 0.01749(19) Uani 1 1 d . . . C21 C 0.05824(12) 0.36222(6) 0.18431(7) 0.0180(2) Uani 1 1 d . . . C22 C -0.07207(13) 0.36547(7) 0.13084(8) 0.0233(2) Uani 1 1 d . . . H22 H -0.0836 0.3792 0.0741 0.028 Uiso 1 1 calc R . . C23 C -0.18411(14) 0.34873(8) 0.16041(9) 0.0290(3) Uani 1 1 d . . . H23 H -0.2726 0.3526 0.1246 0.035 Uiso 1 1 calc R . . C24 C -0.16680(15) 0.32635(8) 0.24254(10) 0.0311(3) Uani 1 1 d . . . H24 H -0.2435 0.3134 0.2622 0.037 Uiso 1 1 calc R . . C25 C -0.03884(15) 0.32285(8) 0.29567(9) 0.0284(3) Uani 1 1 d . . . H25 H -0.0279 0.3073 0.3517 0.034 Uiso 1 1 calc R . . C26 C 0.07430(13) 0.34197(7) 0.26772(8) 0.0223(2) Uani 1 1 d . . . H26 H 0.1619 0.3413 0.3051 0.027 Uiso 1 1 calc R . . C3 C 0.28532(11) 0.42480(7) 0.19963(6) 0.01668(19) Uani 1 1 d . . . C4 C 0.40172(12) 0.39502(6) 0.24818(7) 0.0183(2) Uani 1 1 d . . . C41 C 0.42506(12) 0.32176(7) 0.26453(8) 0.0215(2) Uani 1 1 d . . . N41 N 0.44385(13) 0.26293(6) 0.27820(8) 0.0302(2) Uani 1 1 d . . . C51 C 0.50757(11) 0.44419(6) 0.28423(7) 0.01774(19) Uani 1 1 d . . . N52 N 0.47980(10) 0.50940(6) 0.26598(6) 0.01864(17) Uani 1 1 d . . . H52 H 0.5431(19) 0.5410(10) 0.2854(11) 0.031(5) Uiso 1 1 d . . . O5 O 0.62112(9) 0.41659(5) 0.33219(6) 0.02417(18) Uani 1 1 d . . . C5 C 0.72835(13) 0.46303(8) 0.37202(9) 0.0277(3) Uani 1 1 d . . . H5A H 0.7512 0.4938 0.3299 0.042 Uiso 1 1 calc R . . H5B H 0.8083 0.4356 0.3996 0.042 Uiso 1 1 calc R . . H5C H 0.6989 0.4915 0.4138 0.042 Uiso 1 1 calc R . . C101 C 0.33198(16) 0.56510(9) 0.07144(9) 0.0317(3) Uani 1 1 d . . . H101 H 0.408 0.5479 0.0538 0.038 Uiso 1 1 calc R . . C102 C 0.20062(16) 0.53428(7) 0.05406(8) 0.0283(3) Uani 1 1 d . . . H102 H 0.1733 0.4931 0.0219 0.034 Uiso 1 1 calc R . . C103 C 0.11743(14) 0.57543(8) 0.09288(8) 0.0271(3) Uani 1 1 d . . . H103 H 0.0255 0.5665 0.0924 0.033 Uiso 1 1 calc R . . C104 C 0.19813(16) 0.63282(7) 0.13273(8) 0.0285(3) Uani 1 1 d . . . H104 H 0.1681 0.6694 0.1629 0.034 Uiso 1 1 calc R . . C105 C 0.32847(15) 0.62657(8) 0.12024(9) 0.0313(3) Uani 1 1 d . . . H105 H 0.4019 0.6578 0.1407 0.038 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 0.01537(4) 0.01555(4) 0.01520(4) 0.00249(3) 0.00262(3) -0.00001(3) P1 0.01437(12) 0.01429(12) 0.01649(12) 0.00179(9) 0.00290(9) 0.00038(10) C111 0.0162(5) 0.0195(5) 0.0221(5) 0.0047(4) 0.0037(4) 0.0024(4) C112 0.0182(5) 0.0248(6) 0.0254(6) -0.0001(4) 0.0021(4) 0.0014(4) C113 0.0184(6) 0.0335(7) 0.0322(7) 0.0027(5) -0.0001(5) -0.0014(5) C114 0.0174(6) 0.0342(8) 0.0491(9) 0.0129(7) 0.0035(6) 0.0062(5) C115 0.0235(7) 0.0252(7) 0.0599(10) 0.0052(6) 0.0080(6) 0.0082(5) C116 0.0206(6) 0.0197(6) 0.0455(8) 0.0006(5) 0.0052(5) 0.0022(5) C121 0.0184(5) 0.0154(5) 0.0185(5) 0.0009(4) 0.0022(4) 0.0006(4) C122 0.0268(6) 0.0235(6) 0.0236(6) -0.0024(4) 0.0090(5) -0.0037(5) C123 0.0350(7) 0.0256(6) 0.0239(6) -0.0043(5) 0.0094(5) -0.0026(5) C124 0.0319(7) 0.0193(5) 0.0271(6) -0.0023(4) 0.0023(5) -0.0017(5) C125 0.0243(6) 0.0188(5) 0.0260(6) 0.0008(4) 0.0033(5) -0.0038(4) C126 0.0199(5) 0.0189(5) 0.0201(5) 0.0013(4) 0.0038(4) -0.0004(4) C131 0.0174(5) 0.0162(4) 0.0170(5) 0.0008(4) 0.0030(4) -0.0010(4) C132 0.0178(5) 0.0252(6) 0.0216(5) 0.0036(4) 0.0030(4) -0.0029(4) C133 0.0268(6) 0.0289(6) 0.0255(6) 0.0054(5) 0.0063(5) -0.0089(5) C134 0.0357(7) 0.0228(6) 0.0238(6) 0.0074(5) 0.0043(5) -0.0032(5) C135 0.0278(6) 0.0249(6) 0.0243(6) 0.0059(5) 0.0046(5) 0.0067(5) C136 0.0184(5) 0.0239(6) 0.0203(5) 0.0038(4) 0.0056(4) 0.0035(4) C1 0.0232(5) 0.0202(5) 0.0192(5) -0.0002(4) 0.0034(4) 0.0031(4) C11 0.0299(6) 0.0239(6) 0.0215(6) -0.0040(4) 0.0019(5) 0.0061(5) N11 0.0395(7) 0.0310(7) 0.0381(7) -0.0143(5) -0.0001(5) 0.0030(5) C12 0.0324(7) 0.0249(6) 0.0247(6) -0.0006(5) 0.0089(5) 0.0064(5) N12 0.0447(8) 0.0388(8) 0.0456(8) 0.0039(6) 0.0263(7) 0.0079(6) C2 0.0177(5) 0.0157(5) 0.0177(5) 0.0011(4) 0.0018(4) 0.0019(4) C21 0.0190(5) 0.0148(5) 0.0190(5) -0.0011(4) 0.0026(4) -0.0016(4) C22 0.0217(5) 0.0232(6) 0.0227(5) -0.0003(4) 0.0011(4) -0.0011(4) C23 0.0193(6) 0.0302(7) 0.0359(7) -0.0072(5) 0.0038(5) -0.0048(5) C24 0.0280(7) 0.0295(7) 0.0399(8) -0.0080(6) 0.0160(6) -0.0099(5) C25 0.0365(7) 0.0267(6) 0.0251(6) -0.0024(5) 0.0133(5) -0.0079(5) C26 0.0248(6) 0.0219(5) 0.0193(5) 0.0001(4) 0.0035(4) -0.0015(4) C3 0.0123(4) 0.0229(5) 0.0148(5) 0.0039(4) 0.0034(4) 0.0002(4) C4 0.0180(5) 0.0159(5) 0.0201(5) 0.0015(4) 0.0031(4) 0.0011(4) C41 0.0178(5) 0.0216(5) 0.0231(5) -0.0002(4) 0.0014(4) 0.0005(4) N41 0.0274(6) 0.0218(5) 0.0396(7) 0.0034(5) 0.0052(5) 0.0034(4) C51 0.0139(4) 0.0207(5) 0.0184(5) 0.0014(4) 0.0036(4) 0.0016(4) N52 0.0156(4) 0.0191(4) 0.0207(4) 0.0007(3) 0.0035(3) -0.0027(4) O5 0.0156(4) 0.0244(4) 0.0283(4) 0.0006(3) -0.0024(3) 0.0024(3) C5 0.0161(5) 0.0354(7) 0.0283(6) 0.0015(5) -0.0010(4) -0.0043(5) C101 0.0377(8) 0.0371(8) 0.0235(6) 0.0127(5) 0.0139(6) 0.0068(6) C102 0.0416(8) 0.0242(6) 0.0153(5) 0.0042(4) -0.0002(5) 0.0016(5) C103 0.0213(6) 0.0326(7) 0.0240(6) 0.0116(5) -0.0005(4) 0.0022(5) C104 0.0408(8) 0.0212(6) 0.0217(6) 0.0066(4) 0.0046(5) 0.0093(5) C105 0.0336(7) 0.0288(7) 0.0280(6) 0.0129(5) 0.0009(5) -0.0097(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C3 2.0429(13) . ? Ru1 N52 2.1062(10) . ? Ru1 C102 2.1887(13) . ? Ru1 C103 2.1964(12) . ? Ru1 C101 2.2115(13) . ? Ru1 C104 2.2348(13) . ? Ru1 C105 2.2445(13) . ? Ru1 P1 2.3152(3) . ? P1 C131 1.8312(12) . ? P1 C121 1.8337(12) . ? P1 C111 1.8346(12) . ? C111 C116 1.3964(18) . ? C111 C112 1.3998(18) . ? C112 C113 1.3917(18) . ? C112 H112 0.95 . ? C113 C114 1.387(2) . ? C113 H113 0.95 . ? C114 C115 1.385(2) . ? C114 H114 0.95 . ? C115 C116 1.398(2) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.3910(16) . ? C121 C122 1.4025(17) . ? C122 C123 1.3908(19) . ? C122 H122 0.95 . ? C123 C124 1.383(2) . ? C123 H123 0.95 . ? C124 C125 1.3861(19) . ? C124 H124 0.95 . ? C125 C126 1.3919(17) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.3954(17) . ? C131 C132 1.3967(17) . ? C132 C133 1.3931(18) . ? C132 H132 0.95 . ? C133 C134 1.384(2) . ? C133 H133 0.95 . ? C134 C135 1.390(2) . ? C134 H134 0.95 . ? C135 C136 1.3872(17) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C1 C2 1.3696(16) . ? C1 C12 1.4321(19) . ? C1 C11 1.4391(19) . ? C11 N11 1.1482(19) . ? C12 N12 1.1473(19) . ? C2 C3 1.4565(16) . ? C2 C21 1.4857(16) . ? C21 C26 1.3985(17) . ? C21 C22 1.4003(17) . ? C22 C23 1.3847(19) . ? C22 H22 0.95 . ? C23 C24 1.389(2) . ? C23 H23 0.95 . ? C24 C25 1.379(2) . ? C24 H24 0.95 . ? C25 C26 1.3916(18) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.3774(16) . ? C4 C41 1.4321(17) . ? C4 C51 1.4412(17) . ? C41 N41 1.1515(17) . ? C51 N52 1.2946(16) . ? C51 O5 1.3362(14) . ? N52 H52 0.883(19) . ? O5 C5 1.4326(16) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C101 C102 1.424(2) . ? C101 C105 1.428(2) . ? C101 H101 0.95 . ? C102 C103 1.419(2) . ? C102 H102 0.95 . ? C103 C104 1.427(2) . ? C103 H103 0.95 . ? C104 C105 1.398(2) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? 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 C3 Ru1 N52 76.82(4) . . ? C3 Ru1 C102 95.63(5) . . ? N52 Ru1 C102 133.60(5) . . ? C3 Ru1 C103 114.97(5) . . ? N52 Ru1 C103 163.25(5) . . ? C102 Ru1 C103 37.76(6) . . ? C3 Ru1 C101 111.38(5) . . ? N52 Ru1 C101 102.15(5) . . ? C102 Ru1 C101 37.75(6) . . ? C103 Ru1 C101 63.11(5) . . ? C3 Ru1 C104 152.54(5) . . ? N52 Ru1 C104 129.90(5) . . ? C102 Ru1 C104 62.28(5) . . ? C103 Ru1 C104 37.57(5) . . ? C101 Ru1 C104 61.92(5) . . ? C3 Ru1 C105 148.29(5) . . ? N52 Ru1 C105 101.19(5) . . ? C102 Ru1 C105 62.43(5) . . ? C103 Ru1 C105 62.39(5) . . ? C101 Ru1 C105 37.37(6) . . ? C104 Ru1 C105 36.37(6) . . ? C3 Ru1 P1 97.98(3) . . ? N52 Ru1 P1 91.28(3) . . ? C102 Ru1 P1 135.04(4) . . ? C103 Ru1 P1 98.40(4) . . ? C101 Ru1 P1 149.72(4) . . ? C104 Ru1 P1 88.61(4) . . ? C105 Ru1 P1 113.72(4) . . ? C131 P1 C121 99.13(5) . . ? C131 P1 C111 104.11(5) . . ? C121 P1 C111 104.14(6) . . ? C131 P1 Ru1 119.59(4) . . ? C121 P1 Ru1 116.13(4) . . ? C111 P1 Ru1 111.78(4) . . ? C116 C111 C112 118.71(11) . . ? C116 C111 P1 123.56(10) . . ? C112 C111 P1 117.58(9) . . ? C113 C112 C111 120.94(13) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.5 . . ? C114 C113 C112 119.92(14) . . ? C114 C113 H113 120 . . ? C112 C113 H113 120 . . ? C115 C114 C113 119.73(13) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.65(14) . . ? C114 C115 H115 119.7 . . ? C116 C115 H115 119.7 . . ? C111 C116 C115 120.03(14) . . ? C111 C116 H116 120 . . ? C115 C116 H116 120 . . ? C126 C121 C122 118.50(11) . . ? C126 C121 P1 121.48(9) . . ? C122 C121 P1 120.01(9) . . ? C123 C122 C121 120.85(12) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C124 C123 C122 119.88(12) . . ? C124 C123 H123 120.1 . . ? C122 C123 H123 120.1 . . ? C123 C124 C125 119.85(12) . . ? C123 C124 H124 120.1 . . ? C125 C124 H124 120.1 . . ? C124 C125 C126 120.43(12) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C121 C126 C125 120.47(11) . . ? C121 C126 H126 119.8 . . ? C125 C126 H126 119.8 . . ? C136 C131 C132 118.45(11) . . ? C136 C131 P1 117.45(9) . . ? C132 C131 P1 124.09(9) . . ? C133 C132 C131 120.29(12) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 120.58(12) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.58(12) . . ? C133 C134 H134 120.2 . . ? C135 C134 H134 120.2 . . ? C136 C135 C134 119.87(12) . . ? C136 C135 H135 120.1 . . ? C134 C135 H135 120.1 . . ? C135 C136 C131 121.15(12) . . ? C135 C136 H136 119.4 . . ? C131 C136 H136 119.4 . . ? C2 C1 C12 121.16(12) . . ? C2 C1 C11 123.30(12) . . ? C12 C1 C11 115.50(11) . . ? N11 C11 C1 177.81(15) . . ? N12 C12 C1 178.08(16) . . ? C1 C2 C3 118.96(11) . . ? C1 C2 C21 120.22(11) . . ? C3 C2 C21 120.82(10) . . ? C26 C21 C22 119.50(11) . . ? C26 C21 C2 120.12(10) . . ? C22 C21 C2 120.37(10) . . ? C23 C22 C21 120.19(12) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.87(13) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.35(12) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.40(13) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.60(12) . . ? C25 C26 H26 120.2 . . ? C21 C26 H26 120.2 . . ? C4 C3 C2 118.81(11) . . ? C4 C3 Ru1 116.08(8) . . ? C2 C3 Ru1 124.75(8) . . ? C3 C4 C41 126.20(11) . . ? C3 C4 C51 114.76(11) . . ? C41 C4 C51 119.04(11) . . ? N41 C41 C4 179.57(14) . . ? N52 C51 O5 128.55(11) . . ? N52 C51 C4 115.58(10) . . ? O5 C51 C4 115.87(11) . . ? C51 N52 Ru1 116.74(8) . . ? C51 N52 H52 118.3(12) . . ? Ru1 N52 H52 124.9(12) . . ? C51 O5 C5 118.46(10) . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C102 C101 C105 107.40(13) . . ? C102 C101 Ru1 70.26(7) . . ? C105 C101 Ru1 72.57(7) . . ? C102 C101 H101 126.3 . . ? C105 C101 H101 126.3 . . ? Ru1 C101 H101 122.6 . . ? C103 C102 C101 108.48(13) . . ? C103 C102 Ru1 71.41(7) . . ? C101 C102 Ru1 71.99(8) . . ? C103 C102 H102 125.8 . . ? C101 C102 H102 125.8 . . ? Ru1 C102 H102 122.5 . . ? C102 C103 C104 106.99(12) . . ? C102 C103 Ru1 70.83(7) . . ? C104 C103 Ru1 72.67(7) . . ? C102 C103 H103 126.5 . . ? C104 C103 H103 126.5 . . ? Ru1 C103 H103 121.8 . . ? C105 C104 C103 109.02(13) . . ? C105 C104 Ru1 72.19(8) . . ? C103 C104 Ru1 69.75(7) . . ? C105 C104 H104 125.5 . . ? C103 C104 H104 125.5 . . ? Ru1 C104 H104 124.2 . . ? C104 C105 C101 108.10(13) . . ? C104 C105 Ru1 71.44(7) . . ? C101 C105 Ru1 70.06(8) . . ? C104 C105 H105 126 . . ? C101 C105 H105 126 . . ? Ru1 C105 H105 124.2 . . ? #===END # Attachment '3.br1386.cif' data_br1386 _database_code_depnum_ccdc_archive 'CCDC 730743' _audit_creation_date 2007-12-04T11:09:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41 H35 N7 Na O P Ru' _chemical_formula_moiety 'C41 H35 N7 Na O P Ru' _chemical_formula_weight 796.79 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -P_2ybc 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 19.5078(8) _cell_length_b 9.6382(2) _cell_length_c 22.4454(9) _cell_angle_alpha 90 _cell_angle_beta 115.464(5) _cell_angle_gamma 90 _cell_volume 3810.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13941 _cell_measurement_theta_min 2.7881 _cell_measurement_theta_max 31.8758 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.72183 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0116822916 _diffrn_orient_matrix_ub_12 -0.0575268672 _diffrn_orient_matrix_ub_13 0.0250138198 _diffrn_orient_matrix_ub_21 0.0084798982 _diffrn_orient_matrix_ub_22 0.04520452 _diffrn_orient_matrix_ub_23 0.031555256 _diffrn_orient_matrix_ub_31 -0.0319293596 _diffrn_orient_matrix_ub_32 -0.0090690112 _diffrn_orient_matrix_ub_33 -0.0013983625 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_unetI/netI 0.0874 _diffrn_reflns_number 47404 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.8 _diffrn_reflns_theta_max 29 _diffrn_reflns_theta_full 29 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 10103 _reflns_number_gt 6251 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.0000P] 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_number_reflns 10103 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.122 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.207 _refine_diff_density_min -0.6 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.294592(15) 0.59237(3) 0.379376(13) 0.01819(8) Uani 1 1 d . . . P1 P 0.31070(5) 0.58972(9) 0.28387(4) 0.01898(18) Uani 1 1 d . . . C111 C 0.41053(19) 0.5739(3) 0.29981(16) 0.0215(7) Uani 1 1 d . . . C112 C 0.4501(2) 0.4515(4) 0.32759(17) 0.0250(8) Uani 1 1 d . . . H112 H 0.4239 0.3761 0.3358 0.03 Uiso 1 1 calc R . . C113 C 0.5266(2) 0.4384(4) 0.34334(17) 0.0281(8) Uani 1 1 d . . . H113 H 0.5523 0.3536 0.3608 0.034 Uiso 1 1 calc R . . C114 C 0.5654(2) 0.5489(4) 0.33358(19) 0.0350(9) Uani 1 1 d . . . H114 H 0.618 0.5406 0.3445 0.042 Uiso 1 1 calc R . . C115 C 0.5278(2) 0.6723(4) 0.3078(2) 0.0427(11) Uani 1 1 d . . . H115 H 0.5549 0.7489 0.302 0.051 Uiso 1 1 calc R . . C116 C 0.4508(2) 0.6843(4) 0.29055(19) 0.0316(9) Uani 1 1 d . . . H116 H 0.4253 0.7687 0.2722 0.038 Uiso 1 1 calc R . . C121 C 0.2602(2) 0.4631(3) 0.21892(16) 0.0206(7) Uani 1 1 d . . . C122 C 0.2950(2) 0.3665(4) 0.19510(17) 0.0258(8) Uani 1 1 d . . . H122 H 0.3487 0.3572 0.2155 0.031 Uiso 1 1 calc R . . C123 C 0.2516(2) 0.2834(4) 0.14157(17) 0.0307(9) Uani 1 1 d . . . H123 H 0.2758 0.2179 0.1253 0.037 Uiso 1 1 calc R . . C124 C 0.1735(2) 0.2953(4) 0.11177(18) 0.0308(9) Uani 1 1 d . . . H124 H 0.1442 0.2382 0.0751 0.037 Uiso 1 1 calc R . . C125 C 0.1379(2) 0.3897(4) 0.13493(17) 0.0287(8) Uani 1 1 d . . . H125 H 0.0841 0.3973 0.1148 0.034 Uiso 1 1 calc R . . C126 C 0.1811(2) 0.4732(4) 0.18769(17) 0.0259(8) Uani 1 1 d . . . H126 H 0.1564 0.5394 0.2032 0.031 Uiso 1 1 calc R . . C131 C 0.2768(2) 0.7420(3) 0.23003(16) 0.0233(8) Uani 1 1 d . . . C132 C 0.2809(2) 0.7425(4) 0.16948(18) 0.0317(9) Uani 1 1 d . . . H132 H 0.3093 0.6731 0.1599 0.038 Uiso 1 1 calc R . . C133 C 0.2433(2) 0.8444(4) 0.12321(19) 0.0372(10) Uani 1 1 d . . . H133 H 0.2466 0.8457 0.0822 0.045 Uiso 1 1 calc R . . C134 C 0.2008(2) 0.9446(4) 0.13675(19) 0.0361(10) Uani 1 1 d . . . H134 H 0.1733 1.0119 0.1043 0.043 Uiso 1 1 calc R . . C135 C 0.1987(2) 0.9464(4) 0.19661(19) 0.0333(9) Uani 1 1 d . . . H135 H 0.1708 1.0168 0.2061 0.04 Uiso 1 1 calc R . . C136 C 0.2368(2) 0.8465(4) 0.24381(18) 0.0257(8) Uani 1 1 d . . . H136 H 0.2355 0.8496 0.2856 0.031 Uiso 1 1 calc R . . C1 C 0.29562(19) 0.2531(3) 0.47032(16) 0.0201(7) Uani 1 1 d . . . C11 C 0.3344(2) 0.1452(4) 0.51717(18) 0.0261(8) Uani 1 1 d . . . N11 N 0.3621(2) 0.0612(3) 0.55598(16) 0.0345(8) Uani 1 1 d . . . C12 C 0.2448(2) 0.3356(4) 0.48635(16) 0.0243(8) Uani 1 1 d . . . N12 N 0.20530(19) 0.4008(3) 0.50080(15) 0.0316(7) Uani 1 1 d . . . C2 C 0.30337(18) 0.2801(3) 0.41319(16) 0.0192(7) Uani 1 1 d . . . C21 C 0.35770(19) 0.2030(3) 0.39548(16) 0.0193(7) Uani 1 1 d . . . C22 C 0.43188(19) 0.1789(3) 0.44114(16) 0.0214(7) Uani 1 1 d . . . H22 H 0.4482 0.2089 0.4855 0.026 Uiso 1 1 calc R . . C23 C 0.4824(2) 0.1116(3) 0.42267(17) 0.0248(8) Uani 1 1 d . . . H23 H 0.5333 0.0964 0.4541 0.03 Uiso 1 1 calc R . . C24 C 0.4584(2) 0.0662(3) 0.35769(18) 0.0255(8) Uani 1 1 d . . . H24 H 0.4931 0.021 0.3447 0.031 Uiso 1 1 calc R . . C25 C 0.3839(2) 0.0873(3) 0.31235(17) 0.0241(7) Uani 1 1 d . . . H25 H 0.367 0.0537 0.2685 0.029 Uiso 1 1 calc R . . C26 C 0.3336(2) 0.1571(3) 0.33061(16) 0.0217(7) Uani 1 1 d . . . H26 H 0.283 0.1737 0.299 0.026 Uiso 1 1 calc R . . C3 C 0.25667(18) 0.3921(3) 0.37126(15) 0.0181(7) Uani 1 1 d . . . C4 C 0.1815(2) 0.3669(3) 0.33195(16) 0.0201(7) Uani 1 1 d . . . C41 C 0.14873(19) 0.2306(4) 0.32084(17) 0.0228(7) Uani 1 1 d . . . N41 N 0.12616(17) 0.1190(3) 0.31239(16) 0.0307(7) Uani 1 1 d . . . C51 C 0.1370(2) 0.4908(3) 0.30625(17) 0.0220(7) Uani 1 1 d . . . N52 N 0.17778(16) 0.6087(3) 0.32561(13) 0.0206(6) Uani 1 1 d . . . N53 N 0.12768(17) 0.7131(3) 0.30061(15) 0.0264(7) Uani 1 1 d . . . N54 N 0.06020(17) 0.6591(3) 0.26762(16) 0.0316(7) Uani 1 1 d . . . N55 N 0.06379(17) 0.5176(3) 0.26985(15) 0.0273(7) Uani 1 1 d . . . C101 C 0.3755(2) 0.5850(4) 0.48369(17) 0.0363(10) Uani 1 1 d . . . H101 H 0.3863 0.5018 0.5088 0.044 Uiso 1 1 calc R . . C102 C 0.4137(2) 0.6323(4) 0.44699(18) 0.0326(9) Uani 1 1 d . . . H102 H 0.4543 0.5871 0.4422 0.039 Uiso 1 1 calc R . . C103 C 0.3797(2) 0.7619(4) 0.41827(17) 0.0358(10) Uani 1 1 d . . . H103 H 0.3948 0.8193 0.3915 0.043 Uiso 1 1 calc R . . C104 C 0.3211(2) 0.7899(4) 0.4360(2) 0.0409(11) Uani 1 1 d . . . H104 H 0.2885 0.8684 0.4228 0.049 Uiso 1 1 calc R . . C105 C 0.3185(2) 0.6810(4) 0.47703(19) 0.0384(10) Uani 1 1 d . . . H105 H 0.2842 0.674 0.4967 0.046 Uiso 1 1 calc R . . Na1 Na -0.05242(8) 0.41286(14) 0.19850(7) 0.0290(3) Uani 1 1 d . . . C01 C -0.0353(4) 0.6493(7) 0.0831(4) 0.096(2) Uani 1 1 d . . . H01A H -0.0194 0.6487 0.1309 0.144 Uiso 1 1 calc R . . H01B H -0.0591 0.7386 0.0649 0.144 Uiso 1 1 calc R . . H01C H 0.0091 0.6354 0.0741 0.144 Uiso 1 1 calc R . . C02 C -0.0920(4) 0.5331(8) 0.0514(3) 0.098(2) Uani 1 1 d . . . H02A H -0.1408 0.5554 0.0529 0.118 Uiso 1 1 calc R . . H02B H -0.1015 0.5224 0.0046 0.118 Uiso 1 1 calc R . . O03 O -0.0616(2) 0.4061(4) 0.08670(17) 0.0701(11) Uani 1 1 d . . . C04 C -0.0996(4) 0.2862(10) 0.0513(3) 0.105(3) Uani 1 1 d . . . H04A H -0.113 0.2991 0.0038 0.126 Uiso 1 1 calc R . . H04B H -0.1472 0.2727 0.0562 0.126 Uiso 1 1 calc R . . C05 C -0.0507(5) 0.1605(8) 0.0760(4) 0.116(3) Uani 1 1 d . . . H05A H -0.0067 0.1684 0.0659 0.175 Uiso 1 1 calc R . . H05B H -0.08 0.0777 0.0545 0.175 Uiso 1 1 calc R . . H05C H -0.0332 0.1528 0.1239 0.175 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 0.02005(14) 0.01447(12) 0.01987(13) -0.00130(12) 0.00841(10) -0.00243(12) P1 0.0210(4) 0.0164(4) 0.0201(4) -0.0007(4) 0.0093(4) -0.0026(4) C111 0.0211(17) 0.0264(19) 0.0186(16) -0.0019(14) 0.0102(14) -0.0038(14) C112 0.0236(19) 0.0263(18) 0.0259(19) -0.0007(14) 0.0113(16) -0.0043(15) C113 0.026(2) 0.032(2) 0.0259(19) -0.0011(15) 0.0116(16) -0.0015(15) C114 0.022(2) 0.047(2) 0.039(2) 0.0025(19) 0.0157(18) -0.0017(18) C115 0.030(2) 0.039(2) 0.064(3) 0.006(2) 0.026(2) -0.0086(19) C116 0.027(2) 0.028(2) 0.043(2) 0.0040(17) 0.0180(19) -0.0018(16) C121 0.0239(19) 0.0191(16) 0.0208(17) 0.0022(14) 0.0115(15) -0.0003(14) C122 0.0237(19) 0.0269(18) 0.0248(18) 0.0008(15) 0.0086(16) 0.0031(15) C123 0.039(2) 0.0242(19) 0.0265(19) -0.0053(15) 0.0117(18) 0.0081(17) C124 0.035(2) 0.0238(19) 0.0242(19) -0.0028(15) 0.0037(17) -0.0004(16) C125 0.0255(19) 0.031(2) 0.0268(19) -0.0032(16) 0.0081(16) 0.0020(16) C126 0.027(2) 0.0285(19) 0.0264(19) -0.0033(15) 0.0150(16) 0.0020(16) C131 0.028(2) 0.0190(17) 0.0212(17) 0.0029(14) 0.0090(15) -0.0021(14) C132 0.042(2) 0.026(2) 0.031(2) 0.0010(16) 0.0186(18) -0.0017(17) C133 0.053(3) 0.033(2) 0.024(2) 0.0028(17) 0.015(2) -0.008(2) C134 0.046(3) 0.0196(19) 0.033(2) 0.0052(15) 0.008(2) -0.0016(17) C135 0.034(2) 0.025(2) 0.036(2) 0.0000(16) 0.0101(19) -0.0012(16) C136 0.025(2) 0.0205(17) 0.030(2) -0.0020(15) 0.0105(16) -0.0049(15) C1 0.0211(18) 0.0170(16) 0.0216(17) 0.0011(13) 0.0085(14) 0.0014(14) C11 0.028(2) 0.0253(18) 0.0271(19) 0.0007(16) 0.0138(17) 0.0026(16) N11 0.041(2) 0.0321(19) 0.0362(18) 0.0102(14) 0.0221(16) 0.0141(15) C12 0.031(2) 0.0213(18) 0.0211(18) 0.0054(14) 0.0112(16) 0.0017(16) N12 0.0416(19) 0.0285(17) 0.0301(16) 0.0076(14) 0.0206(15) 0.0086(16) C2 0.0165(17) 0.0131(15) 0.0267(18) -0.0010(13) 0.0080(14) -0.0039(13) C21 0.0222(18) 0.0129(15) 0.0245(17) 0.0030(13) 0.0118(15) 0.0022(13) C22 0.0238(19) 0.0212(17) 0.0183(17) -0.0014(13) 0.0083(15) -0.0005(14) C23 0.0197(18) 0.0201(18) 0.0325(19) 0.0029(15) 0.0093(15) -0.0004(14) C24 0.028(2) 0.0185(18) 0.034(2) -0.0013(14) 0.0178(17) 0.0010(14) C25 0.0295(19) 0.0197(16) 0.0248(17) -0.0037(15) 0.0135(15) -0.0043(16) C26 0.0224(18) 0.0207(17) 0.0198(17) 0.0021(14) 0.0071(15) 0.0008(14) C3 0.0194(17) 0.0181(17) 0.0200(16) -0.0040(13) 0.0114(13) -0.0016(14) C4 0.0258(19) 0.0129(15) 0.0237(18) 0.0010(13) 0.0127(15) 0.0008(13) C41 0.0172(18) 0.0228(18) 0.0265(18) 0.0002(15) 0.0076(15) 0.0005(14) N41 0.0238(17) 0.0218(17) 0.0404(19) -0.0026(13) 0.0080(15) -0.0037(13) C51 0.0237(19) 0.0165(17) 0.0263(18) -0.0016(14) 0.0113(16) -0.0010(14) N52 0.0232(15) 0.0162(14) 0.0248(15) 0.0020(11) 0.0125(12) 0.0033(12) N53 0.0222(17) 0.0190(15) 0.0367(18) 0.0035(13) 0.0113(14) 0.0016(13) N54 0.0233(17) 0.0184(16) 0.048(2) 0.0075(14) 0.0106(16) 0.0042(13) N55 0.0242(17) 0.0164(15) 0.0376(18) 0.0053(13) 0.0099(14) 0.0025(13) C101 0.046(2) 0.0228(18) 0.0213(18) 0.0000(16) -0.0030(17) -0.0096(19) C102 0.026(2) 0.039(2) 0.029(2) -0.0148(17) 0.0080(17) -0.0059(17) C103 0.045(3) 0.038(2) 0.0202(18) -0.0069(17) 0.0097(18) -0.024(2) C104 0.043(3) 0.024(2) 0.041(2) -0.0144(18) 0.005(2) 0.0010(18) C105 0.037(2) 0.049(3) 0.033(2) -0.0193(19) 0.020(2) -0.016(2) Na1 0.0257(7) 0.0189(7) 0.0379(8) 0.0016(6) 0.0094(6) 0.0012(6) C01 0.102(6) 0.083(5) 0.107(5) 0.039(4) 0.049(5) 0.038(4) C02 0.100(6) 0.135(7) 0.052(4) 0.037(4) 0.025(4) 0.051(5) O03 0.052(2) 0.107(3) 0.050(2) -0.006(2) 0.0208(18) 0.006(2) C04 0.084(5) 0.154(8) 0.074(4) -0.058(5) 0.032(4) -0.052(5) C05 0.155(8) 0.089(5) 0.135(7) -0.058(5) 0.091(6) -0.074(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.047(3) . ? Ru1 N52 2.076(3) . ? Ru1 C101 2.191(4) . ? Ru1 C102 2.195(4) . ? Ru1 C105 2.207(4) . ? Ru1 C104 2.223(4) . ? Ru1 C103 2.224(4) . ? Ru1 P1 2.2965(8) . ? P1 C111 1.829(3) . ? P1 C121 1.830(3) . ? P1 C131 1.834(3) . ? C111 C116 1.391(5) . ? C111 C112 1.401(5) . ? C112 C113 1.384(5) . ? C112 H112 0.95 . ? C113 C114 1.377(5) . ? C113 H113 0.95 . ? C114 C115 1.386(6) . ? C114 H114 0.95 . ? C115 C116 1.385(5) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.387(5) . ? C121 C126 1.397(5) . ? C122 C123 1.388(5) . ? C122 H122 0.95 . ? C123 C124 1.380(5) . ? C123 H123 0.95 . ? C124 C125 1.375(5) . ? C124 H124 0.95 . ? C125 C126 1.380(5) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.388(5) . ? C131 C132 1.395(5) . ? C132 C133 1.389(5) . ? C132 H132 0.95 . ? C133 C134 1.388(6) . ? C133 H133 0.95 . ? C134 C135 1.362(5) . ? C134 H134 0.95 . ? C135 C136 1.387(5) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C1 C2 1.379(5) . ? C1 C12 1.431(5) . ? C1 C11 1.441(5) . ? C11 N11 1.141(4) . ? C12 N12 1.145(4) . ? C2 C3 1.464(4) . ? C2 C21 1.482(5) . ? C21 C22 1.387(5) . ? C21 C26 1.396(4) . ? C22 C23 1.383(5) . ? C22 H22 0.95 . ? C23 C24 1.397(5) . ? C23 H23 0.95 . ? C24 C25 1.385(5) . ? C24 H24 0.95 . ? C25 C26 1.388(5) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.369(5) . ? C4 C41 1.435(5) . ? C4 C51 1.442(4) . ? C41 N41 1.147(4) . ? N41 Na1 2.403(3) 2_545 ? C51 N55 1.331(4) . ? C51 N52 1.348(4) . ? N52 N53 1.346(4) . ? N53 N54 1.309(4) . ? N53 Na1 2.427(3) 2 ? N54 N55 1.365(4) . ? N54 Na1 2.585(3) 2 ? N55 Na1 2.367(3) . ? C101 C102 1.404(6) . ? C101 C105 1.404(6) . ? C101 H101 0.95 . ? C102 C103 1.431(6) . ? C102 H102 0.95 . ? C103 C104 1.389(6) . ? C103 H103 0.95 . ? C104 C105 1.411(6) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? Na1 N41 2.403(3) 2 ? Na1 N53 2.427(3) 2_545 ? Na1 O03 2.438(4) . ? Na1 N54 2.585(3) 2_545 ? C01 C02 1.519(10) . ? C01 H01A 0.98 . ? C01 H01B 0.98 . ? C01 H01C 0.98 . ? C02 O03 1.440(7) . ? C02 H02A 0.99 . ? C02 H02B 0.99 . ? O03 C04 1.418(7) . ? C04 C05 1.493(11) . ? C04 H04A 0.99 . ? C04 H04B 0.99 . ? C05 H05A 0.98 . ? C05 H05B 0.98 . ? C05 H05C 0.98 . ? 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 C3 Ru1 N52 75.84(12) . . ? C3 Ru1 C101 97.53(13) . . ? N52 Ru1 C101 136.88(14) . . ? C3 Ru1 C102 117.49(14) . . ? N52 Ru1 C102 163.70(13) . . ? C101 Ru1 C102 37.35(15) . . ? C3 Ru1 C105 111.56(14) . . ? N52 Ru1 C105 104.98(13) . . ? C101 Ru1 C105 37.23(16) . . ? C102 Ru1 C105 62.39(15) . . ? C3 Ru1 C104 147.65(15) . . ? N52 Ru1 C104 101.25(13) . . ? C101 Ru1 C104 62.17(15) . . ? C102 Ru1 C104 62.45(15) . . ? C105 Ru1 C104 37.15(15) . . ? C3 Ru1 C103 155.27(15) . . ? N52 Ru1 C103 128.36(14) . . ? C101 Ru1 C103 62.04(14) . . ? C102 Ru1 C103 37.78(15) . . ? C105 Ru1 C103 61.47(14) . . ? C104 Ru1 C103 36.41(15) . . ? C3 Ru1 P1 95.49(9) . . ? N52 Ru1 P1 90.84(8) . . ? C101 Ru1 P1 132.26(12) . . ? C102 Ru1 P1 96.79(10) . . ? C105 Ru1 P1 151.14(11) . . ? C104 Ru1 P1 116.84(12) . . ? C103 Ru1 P1 89.76(10) . . ? C111 P1 C121 105.28(15) . . ? C111 P1 C131 104.32(16) . . ? C121 P1 C131 95.21(15) . . ? C111 P1 Ru1 112.33(11) . . ? C121 P1 Ru1 120.53(11) . . ? C131 P1 Ru1 116.80(12) . . ? C116 C111 C112 118.2(3) . . ? C116 C111 P1 122.0(3) . . ? C112 C111 P1 119.6(3) . . ? C113 C112 C111 121.2(3) . . ? C113 C112 H112 119.4 . . ? C111 C112 H112 119.4 . . ? C114 C113 C112 119.6(4) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C113 C114 C115 120.2(4) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C116 C115 C114 120.3(4) . . ? C116 C115 H115 119.9 . . ? C114 C115 H115 119.9 . . ? C115 C116 C111 120.6(4) . . ? C115 C116 H116 119.7 . . ? C111 C116 H116 119.7 . . ? C122 C121 C126 118.1(3) . . ? C122 C121 P1 124.7(3) . . ? C126 C121 P1 117.0(3) . . ? C121 C122 C123 120.2(3) . . ? C121 C122 H122 119.9 . . ? C123 C122 H122 119.9 . . ? C124 C123 C122 120.5(3) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C125 C124 C123 120.2(3) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C124 C125 C126 119.3(3) . . ? C124 C125 H125 120.4 . . ? C126 C125 H125 120.4 . . ? C125 C126 C121 121.7(3) . . ? C125 C126 H126 119.1 . . ? C121 C126 H126 119.1 . . ? C136 C131 C132 119.2(3) . . ? C136 C131 P1 120.8(3) . . ? C132 C131 P1 119.3(3) . . ? C133 C132 C131 119.9(4) . . ? C133 C132 H132 120.1 . . ? C131 C132 H132 120.1 . . ? C134 C133 C132 120.1(4) . . ? C134 C133 H133 119.9 . . ? C132 C133 H133 119.9 . . ? C135 C134 C133 119.9(4) . . ? C135 C134 H134 120 . . ? C133 C134 H134 120 . . ? C134 C135 C136 120.7(4) . . ? C134 C135 H135 119.6 . . ? C136 C135 H135 119.6 . . ? C135 C136 C131 120.1(3) . . ? C135 C136 H136 120 . . ? C131 C136 H136 120 . . ? C2 C1 C12 119.6(3) . . ? C2 C1 C11 125.6(3) . . ? C12 C1 C11 114.8(3) . . ? N11 C11 C1 175.8(4) . . ? N12 C12 C1 178.3(4) . . ? C1 C2 C3 116.7(3) . . ? C1 C2 C21 122.1(3) . . ? C3 C2 C21 121.1(3) . . ? C22 C21 C26 119.6(3) . . ? C22 C21 C2 121.7(3) . . ? C26 C21 C2 118.7(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 119.7(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.4(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 119.9(3) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C4 C3 C2 118.8(3) . . ? C4 C3 Ru1 118.1(2) . . ? C2 C3 Ru1 122.5(2) . . ? C3 C4 C41 123.2(3) . . ? C3 C4 C51 113.8(3) . . ? C41 C4 C51 122.8(3) . . ? N41 C41 C4 176.4(4) . . ? C41 N41 Na1 164.3(3) . 2_545 ? N55 C51 N52 111.3(3) . . ? N55 C51 C4 135.1(3) . . ? N52 C51 C4 113.5(3) . . ? N53 N52 C51 105.9(3) . . ? N53 N52 Ru1 135.9(2) . . ? C51 N52 Ru1 118.1(2) . . ? N54 N53 N52 108.2(3) . . ? N54 N53 Na1 81.68(19) . 2 ? N52 N53 Na1 157.4(2) . 2 ? N53 N54 N55 110.7(3) . . ? N53 N54 Na1 68.25(18) . 2 ? N55 N54 Na1 160.5(3) . 2 ? C51 N55 N54 104.0(3) . . ? C51 N55 Na1 142.7(2) . . ? N54 N55 Na1 112.5(2) . . ? C102 C101 C105 108.6(4) . . ? C102 C101 Ru1 71.5(2) . . ? C105 C101 Ru1 72.0(2) . . ? C102 C101 H101 125.7 . . ? C105 C101 H101 125.7 . . ? Ru1 C101 H101 122.4 . . ? C101 C102 C103 106.7(4) . . ? C101 C102 Ru1 71.2(2) . . ? C103 C102 Ru1 72.2(2) . . ? C101 C102 H102 126.6 . . ? C103 C102 H102 126.6 . . ? Ru1 C102 H102 121.8 . . ? C104 C103 C102 108.6(3) . . ? C104 C103 Ru1 71.8(2) . . ? C102 C103 Ru1 70.0(2) . . ? C104 C103 H103 125.7 . . ? C102 C103 H103 125.7 . . ? Ru1 C103 H103 124.1 . . ? C103 C104 C105 107.9(4) . . ? C103 C104 Ru1 71.8(2) . . ? C105 C104 Ru1 70.8(2) . . ? C103 C104 H104 126 . . ? C105 C104 H104 126 . . ? Ru1 C104 H104 123 . . ? C101 C105 C104 108.1(4) . . ? C101 C105 Ru1 70.7(2) . . ? C104 C105 Ru1 72.0(2) . . ? C101 C105 H105 125.9 . . ? C104 C105 H105 125.9 . . ? Ru1 C105 H105 122.9 . . ? N55 Na1 N41 94.22(11) . 2 ? N55 Na1 N53 137.70(12) . 2_545 ? N41 Na1 N53 108.60(11) 2 2_545 ? N55 Na1 O03 109.47(13) . . ? N41 Na1 O03 98.13(13) 2 . ? N53 Na1 O03 102.13(13) 2_545 . ? N55 Na1 N54 111.39(11) . 2_545 ? N41 Na1 N54 134.73(12) 2 2_545 ? N53 Na1 N54 30.07(9) 2_545 2_545 ? O03 Na1 N54 106.85(13) . 2_545 ? C02 C01 H01A 109.5 . . ? C02 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? C02 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? O03 C02 C01 108.9(5) . . ? O03 C02 H02A 109.9 . . ? C01 C02 H02A 109.9 . . ? O03 C02 H02B 109.9 . . ? C01 C02 H02B 109.9 . . ? H02A C02 H02B 108.3 . . ? C04 O03 C02 113.1(6) . . ? C04 O03 Na1 112.8(4) . . ? C02 O03 Na1 112.0(3) . . ? O03 C04 C05 110.9(6) . . ? O03 C04 H04A 109.5 . . ? C05 C04 H04A 109.5 . . ? O03 C04 H04B 109.5 . . ? C05 C04 H04B 109.4 . . ? H04A C04 H04B 108 . . ? C04 C05 H05A 109.5 . . ? C04 C05 H05B 109.5 . . ? H05A C05 H05B 109.5 . . ? C04 C05 H05C 109.5 . . ? H05A C05 H05C 109.5 . . ? H05B C05 H05C 109.5 . . ? #===END # Attachment '4.br1391.cif' data_br1391 _database_code_depnum_ccdc_archive 'CCDC 730744' _audit_creation_date 2007-12-12T20:26:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C78 H60 N7 P3 Ru2' _chemical_formula_moiety 'C78 H60 N7 P3 Ru2' _chemical_formula_weight 1390.38 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6767(4) _cell_length_b 15.6939(5) _cell_length_c 18.7018(7) _cell_angle_alpha 102.871(3) _cell_angle_beta 104.493(3) _cell_angle_gamma 90.705(3) _cell_volume 3502.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20384 _cell_measurement_theta_min 2.644 _cell_measurement_theta_max 34.1438 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.97724 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.006687949 _diffrn_orient_matrix_ub_12 0.0050614775 _diffrn_orient_matrix_ub_13 -0.0354019458 _diffrn_orient_matrix_ub_21 -0.0113222149 _diffrn_orient_matrix_ub_22 0.044628513 _diffrn_orient_matrix_ub_23 0.0092514327 _diffrn_orient_matrix_ub_31 0.0564099088 _diffrn_orient_matrix_ub_32 0.0118486772 _diffrn_orient_matrix_ub_33 0.0168164838 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_unetI/netI 0.1594 _diffrn_reflns_number 74235 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 34.2 _diffrn_reflns_theta_full 33.25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 27609 _reflns_number_gt 14417 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+0.0000P] 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_number_reflns 27609 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.475 _refine_diff_density_min -0.7 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 0.573919(13) 0.761432(11) 0.227027(10) 0.01660(4) Uani 1 1 d . . . Ru2 Ru 0.354738(13) 0.441179(11) 0.288820(9) 0.01522(4) Uani 1 1 d . . . C1 C 0.37391(17) 0.95411(13) 0.21685(12) 0.0221(5) Uani 1 1 d . . . C11 C 0.35748(18) 1.04475(16) 0.21554(13) 0.0279(5) Uani 1 1 d . . . N11 N 0.34151(17) 1.11577(14) 0.21408(13) 0.0416(6) Uani 1 1 d . . . C12 C 0.29324(19) 0.89187(15) 0.16030(14) 0.0286(6) Uani 1 1 d . . . N12 N 0.22926(18) 0.84543(14) 0.11358(13) 0.0448(6) Uani 1 1 d . . . C2 C 0.45608(16) 0.92859(13) 0.26862(12) 0.0173(4) Uani 1 1 d . . . C21 C 0.54022(17) 0.99382(13) 0.32359(13) 0.0215(5) Uani 1 1 d . . . C22 C 0.59133(18) 1.05835(14) 0.30080(14) 0.0278(5) Uani 1 1 d . . . H22 H 0.573 1.061 0.2489 0.033 Uiso 1 1 calc R . . C23 C 0.66896(19) 1.11872(16) 0.35401(16) 0.0395(7) Uani 1 1 d . . . H23 H 0.704 1.1625 0.3384 0.047 Uiso 1 1 calc R . . C24 C 0.6956(2) 1.11555(16) 0.42961(16) 0.0420(7) Uani 1 1 d . . . H24 H 0.7486 1.1573 0.4658 0.05 Uiso 1 1 calc R . . C25 C 0.6454(2) 1.05197(15) 0.45261(14) 0.0346(6) Uani 1 1 d . . . H25 H 0.6635 1.0501 0.5047 0.042 Uiso 1 1 calc R . . C26 C 0.56846(17) 0.99058(14) 0.39974(13) 0.0240(5) Uani 1 1 d . . . H26 H 0.5349 0.9462 0.4156 0.029 Uiso 1 1 calc R . . C3 C 0.46318(15) 0.83620(13) 0.27075(11) 0.0165(4) Uani 1 1 d . . . C4 C 0.38518(16) 0.79534(13) 0.29282(11) 0.0171(4) Uani 1 1 d . . . C41 C 0.30294(17) 0.83864(14) 0.32463(12) 0.0202(5) Uani 1 1 d . . . N41 N 0.24088(16) 0.87717(13) 0.35101(12) 0.0336(5) Uani 1 1 d . . . C51 C 0.39433(15) 0.70166(13) 0.28281(11) 0.0164(4) Uani 1 1 d . . . N52 N 0.47538(13) 0.67009(11) 0.25223(9) 0.0166(4) Uani 1 1 d . . . N53 N 0.47395(13) 0.58405(11) 0.24998(9) 0.0170(4) Uani 1 1 d . . . N54 N 0.39309(13) 0.56719(11) 0.27954(9) 0.0168(4) Uani 1 1 d . . . N55 N 0.34171(13) 0.63946(11) 0.30133(9) 0.0156(4) Uani 1 1 d . . . P1 P 0.69792(4) 0.76029(4) 0.34090(3) 0.01708(12) Uani 1 1 d . . . C111 C 0.82743(16) 0.82484(14) 0.36021(12) 0.0189(4) Uani 1 1 d . . . C112 C 0.82368(18) 0.91058(15) 0.35217(14) 0.0273(5) Uani 1 1 d . . . H112 H 0.7554 0.9324 0.3328 0.033 Uiso 1 1 calc R . . C113 C 0.91904(19) 0.96478(16) 0.37220(15) 0.0354(6) Uani 1 1 d . . . H113 H 0.9159 1.0237 0.3674 0.042 Uiso 1 1 calc R . . C114 C 1.01793(19) 0.93269(17) 0.39907(15) 0.0365(6) Uani 1 1 d . . . H114 H 1.0833 0.9695 0.4123 0.044 Uiso 1 1 calc R . . C115 C 1.02278(19) 0.84775(17) 0.40695(14) 0.0343(6) Uani 1 1 d . . . H115 H 1.0914 0.8261 0.4255 0.041 Uiso 1 1 calc R . . C116 C 0.92814(17) 0.79368(15) 0.38795(13) 0.0251(5) Uani 1 1 d . . . H116 H 0.9319 0.7351 0.3938 0.03 Uiso 1 1 calc R . . C121 C 0.66383(16) 0.79458(14) 0.43242(12) 0.0191(4) Uani 1 1 d . . . C122 C 0.72548(18) 0.85964(14) 0.49233(13) 0.0243(5) Uani 1 1 d . . . H122 H 0.7884 0.8881 0.4866 0.029 Uiso 1 1 calc R . . C123 C 0.6959(2) 0.88335(15) 0.56032(13) 0.0287(5) Uani 1 1 d . . . H123 H 0.7389 0.9277 0.6007 0.034 Uiso 1 1 calc R . . C124 C 0.6043(2) 0.84289(15) 0.56965(13) 0.0303(6) Uani 1 1 d . . . H124 H 0.5835 0.8598 0.6159 0.036 Uiso 1 1 calc R . . C125 C 0.54382(18) 0.77789(16) 0.51115(13) 0.0272(5) Uani 1 1 d . . . H125 H 0.4814 0.7492 0.5174 0.033 Uiso 1 1 calc R . . C126 C 0.57285(17) 0.75379(14) 0.44320(13) 0.0229(5) Uani 1 1 d . . . H126 H 0.5301 0.7088 0.4034 0.028 Uiso 1 1 calc R . . C131 C 0.74250(16) 0.64970(13) 0.34527(12) 0.0180(4) Uani 1 1 d . . . C132 C 0.74958(17) 0.61431(14) 0.40800(13) 0.0245(5) Uani 1 1 d . . . H132 H 0.7326 0.6482 0.452 0.029 Uiso 1 1 calc R . . C133 C 0.78130(18) 0.52962(15) 0.40672(14) 0.0280(5) Uani 1 1 d . . . H133 H 0.7849 0.5057 0.4496 0.034 Uiso 1 1 calc R . . C134 C 0.80747(17) 0.48026(14) 0.34403(13) 0.0250(5) Uani 1 1 d . . . H134 H 0.8281 0.4221 0.3433 0.03 Uiso 1 1 calc R . . C135 C 0.80382(18) 0.51522(15) 0.28221(13) 0.0293(5) Uani 1 1 d . . . H135 H 0.8244 0.482 0.2394 0.035 Uiso 1 1 calc R . . C136 C 0.76994(19) 0.59925(16) 0.28264(13) 0.0308(6) Uani 1 1 d . . . H136 H 0.7655 0.6224 0.2393 0.037 Uiso 1 1 calc R . . P2 P 0.18245(4) 0.47706(4) 0.30531(3) 0.01754(12) Uani 1 1 d . . . C211 C 0.18348(16) 0.54852(13) 0.39847(11) 0.0175(4) Uani 1 1 d . . . C212 C 0.08538(17) 0.55882(14) 0.41976(12) 0.0229(5) Uani 1 1 d . . . H212 H 0.0208 0.5258 0.3878 0.027 Uiso 1 1 calc R . . C213 C 0.08089(18) 0.61624(14) 0.48661(12) 0.0229(5) Uani 1 1 d . . . H213 H 0.0134 0.6232 0.5 0.027 Uiso 1 1 calc R . . C214 C 0.17496(18) 0.66342(13) 0.53391(12) 0.0218(5) Uani 1 1 d . . . H214 H 0.172 0.7032 0.5797 0.026 Uiso 1 1 calc R . . C215 C 0.27312(18) 0.65303(13) 0.51493(12) 0.0214(5) Uani 1 1 d . . . H215 H 0.3378 0.6847 0.5481 0.026 Uiso 1 1 calc R . . C216 C 0.27755(17) 0.59621(13) 0.44715(11) 0.0183(4) Uani 1 1 d . . . H216 H 0.3452 0.5899 0.434 0.022 Uiso 1 1 calc R . . C221 C 0.09618(17) 0.38316(14) 0.30972(13) 0.0228(5) Uani 1 1 d . . . C222 C 0.00165(18) 0.34510(14) 0.25538(14) 0.0274(5) Uani 1 1 d . . . H222 H -0.025 0.3692 0.2125 0.033 Uiso 1 1 calc R . . C223 C -0.0548(2) 0.27207(17) 0.26282(16) 0.0390(7) Uani 1 1 d . . . H223 H -0.1192 0.2471 0.2248 0.047 Uiso 1 1 calc R . . C224 C -0.0189(2) 0.23577(16) 0.32396(16) 0.0371(6) Uani 1 1 d . . . H224 H -0.0573 0.1855 0.3281 0.044 Uiso 1 1 calc R . . C225 C 0.0746(2) 0.27349(16) 0.37990(15) 0.0343(6) Uani 1 1 d . . . H225 H 0.1003 0.2495 0.4229 0.041 Uiso 1 1 calc R . . C226 C 0.13003(18) 0.34645(15) 0.37241(13) 0.0279(5) Uani 1 1 d . . . H226 H 0.1931 0.3723 0.4113 0.034 Uiso 1 1 calc R . . C231 C 0.08968(16) 0.53591(14) 0.24368(12) 0.0206(5) Uani 1 1 d . . . C232 C 0.07908(17) 0.62522(15) 0.26845(12) 0.0221(5) Uani 1 1 d . . . H232 H 0.118 0.6552 0.3183 0.027 Uiso 1 1 calc R . . C233 C 0.01277(18) 0.67092(16) 0.22156(13) 0.0275(5) Uani 1 1 d . . . H233 H 0.0071 0.7319 0.2392 0.033 Uiso 1 1 calc R . . C234 C -0.04518(18) 0.62827(17) 0.14923(13) 0.0310(6) Uani 1 1 d . . . H234 H -0.0929 0.6593 0.1179 0.037 Uiso 1 1 calc R . . C235 C -0.03372(18) 0.54022(17) 0.12233(13) 0.0294(6) Uani 1 1 d . . . H235 H -0.0726 0.511 0.0722 0.035 Uiso 1 1 calc R . . C236 C 0.03429(17) 0.49476(15) 0.16838(12) 0.0246(5) Uani 1 1 d . . . H236 H 0.0438 0.4349 0.1489 0.029 Uiso 1 1 calc R . . P3 P 0.31131(4) 0.39700(4) 0.15719(3) 0.01709(12) Uani 1 1 d . . . C311 C 0.42125(17) 0.33447(14) 0.12715(11) 0.0200(5) Uani 1 1 d . . . C312 C 0.40705(19) 0.24648(15) 0.09073(13) 0.0269(5) Uani 1 1 d . . . H312 H 0.3366 0.2167 0.0769 0.032 Uiso 1 1 calc R . . C313 C 0.4948(2) 0.20128(17) 0.07420(14) 0.0349(6) Uani 1 1 d . . . H313 H 0.4841 0.1411 0.0486 0.042 Uiso 1 1 calc R . . C314 C 0.5976(2) 0.24385(17) 0.09493(14) 0.0354(6) Uani 1 1 d . . . H314 H 0.6577 0.2127 0.0842 0.042 Uiso 1 1 calc R . . C315 C 0.6130(2) 0.33176(17) 0.13125(14) 0.0315(6) Uani 1 1 d . . . H315 H 0.6836 0.3611 0.1449 0.038 Uiso 1 1 calc R . . C316 C 0.52564(18) 0.37724(15) 0.14786(12) 0.0247(5) Uani 1 1 d . . . H316 H 0.5367 0.4375 0.1733 0.03 Uiso 1 1 calc R . . C321 C 0.19023(16) 0.32073(13) 0.11009(12) 0.0199(5) Uani 1 1 d . . . C322 C 0.16822(17) 0.25671(14) 0.14595(13) 0.0236(5) Uani 1 1 d . . . H322 H 0.214 0.2544 0.1941 0.028 Uiso 1 1 calc R . . C323 C 0.07932(19) 0.19588(15) 0.11156(14) 0.0302(6) Uani 1 1 d . . . H323 H 0.0662 0.1507 0.1353 0.036 Uiso 1 1 calc R . . C324 C 0.01038(19) 0.20094(16) 0.04323(14) 0.0341(6) Uani 1 1 d . . . H324 H -0.0515 0.1602 0.0207 0.041 Uiso 1 1 calc R . . C325 C 0.03057(19) 0.26491(16) 0.00723(14) 0.0338(6) Uani 1 1 d . . . H325 H -0.0171 0.2681 -0.0401 0.041 Uiso 1 1 calc R . . C326 C 0.12057(19) 0.32442(15) 0.04030(13) 0.0287(5) Uani 1 1 d . . . H326 H 0.1349 0.368 0.0153 0.034 Uiso 1 1 calc R . . C331 C 0.29773(17) 0.47862(13) 0.09954(12) 0.0193(4) Uani 1 1 d . . . C332 C 0.33353(19) 0.46491(15) 0.03320(12) 0.0264(5) Uani 1 1 d . . . H332 H 0.3668 0.4125 0.0177 0.032 Uiso 1 1 calc R . . C333 C 0.3211(2) 0.52694(15) -0.01034(13) 0.0297(5) Uani 1 1 d . . . H333 H 0.346 0.5168 -0.0552 0.036 Uiso 1 1 calc R . . C334 C 0.27244(18) 0.60351(15) 0.01159(13) 0.0272(5) Uani 1 1 d . . . H334 H 0.2638 0.646 -0.0182 0.033 Uiso 1 1 calc R . . C335 C 0.23672(17) 0.61775(14) 0.07664(13) 0.0237(5) Uani 1 1 d . . . H335 H 0.2032 0.6702 0.0917 0.028 Uiso 1 1 calc R . . C336 C 0.24938(16) 0.55627(14) 0.12016(12) 0.0205(5) Uani 1 1 d . . . H336 H 0.2246 0.5672 0.1651 0.025 Uiso 1 1 calc R . . C101 C 0.5323(3) 0.8025(3) 0.11939(18) 0.0620(11) Uani 1 1 d . . . H101 H 0.4689 0.8326 0.1045 0.074 Uiso 1 1 calc R . . C102 C 0.6364(4) 0.84109(19) 0.16310(18) 0.0595(10) Uani 1 1 d . . . H102 H 0.6558 0.902 0.1832 0.071 Uiso 1 1 calc R . . C103 C 0.7036(2) 0.7758(2) 0.17118(15) 0.0465(8) Uani 1 1 d . . . H103 H 0.7784 0.7836 0.1985 0.056 Uiso 1 1 calc R . . C104 C 0.6477(2) 0.69646(18) 0.13418(13) 0.0369(6) Uani 1 1 d . . . H104 H 0.6768 0.6407 0.1308 0.044 Uiso 1 1 calc R . . C105 C 0.5399(2) 0.7127(2) 0.10242(13) 0.0419(7) Uani 1 1 d . . . H105 H 0.4823 0.6698 0.0742 0.05 Uiso 1 1 calc R . . C201 C 0.49450(17) 0.45130(14) 0.38988(12) 0.0222(5) Uani 1 1 d . . . H201 H 0.5306 0.5058 0.4199 0.027 Uiso 1 1 calc R . . C202 C 0.40518(17) 0.40859(14) 0.40217(11) 0.0210(5) Uani 1 1 d . . . H202 H 0.3709 0.4287 0.4419 0.025 Uiso 1 1 calc R . . C203 C 0.37477(18) 0.32920(14) 0.34418(12) 0.0219(5) Uani 1 1 d . . . H203 H 0.3159 0.2878 0.3379 0.026 Uiso 1 1 calc R . . C204 C 0.44834(18) 0.32400(14) 0.29824(12) 0.0230(5) Uani 1 1 d . . . H204 H 0.4484 0.2773 0.2561 0.028 Uiso 1 1 calc R . . C205 C 0.52238(16) 0.39968(14) 0.32501(12) 0.0204(5) Uani 1 1 d . . . H205 H 0.5794 0.4133 0.3038 0.024 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 0.01692(9) 0.01666(9) 0.01587(9) 0.00321(7) 0.00417(7) 0.00008(7) Ru2 0.01585(8) 0.01459(9) 0.01332(9) 0.00261(6) 0.00097(7) -0.00028(6) C1 0.0222(11) 0.0153(11) 0.0252(12) 0.0036(9) 0.0010(9) 0.0016(9) C11 0.0262(12) 0.0277(14) 0.0220(12) 0.0050(10) -0.0071(10) -0.0004(10) N11 0.0438(13) 0.0226(12) 0.0463(14) 0.0087(10) -0.0111(11) 0.0031(10) C12 0.0298(13) 0.0199(12) 0.0323(14) 0.0100(10) -0.0026(11) 0.0071(10) N12 0.0433(13) 0.0281(12) 0.0457(14) 0.0079(10) -0.0194(11) 0.0003(10) C2 0.0175(10) 0.0163(11) 0.0176(11) 0.0009(8) 0.0062(8) 0.0014(8) C21 0.0189(10) 0.0133(11) 0.0271(12) 0.0009(9) 0.0001(9) 0.0026(8) C22 0.0244(12) 0.0209(12) 0.0343(14) 0.0062(10) 0.0011(10) 0.0018(10) C23 0.0287(13) 0.0241(14) 0.0567(19) 0.0066(12) -0.0024(13) -0.0048(11) C24 0.0315(14) 0.0222(13) 0.0499(18) -0.0052(12) -0.0183(13) 0.0007(11) C25 0.0401(14) 0.0226(13) 0.0267(14) -0.0013(10) -0.0118(11) 0.0075(11) C26 0.0250(12) 0.0158(11) 0.0282(13) 0.0037(9) 0.0025(10) 0.0084(9) C3 0.0139(10) 0.0160(11) 0.0149(10) 0.0009(8) -0.0025(8) -0.0003(8) C4 0.0150(10) 0.0164(11) 0.0162(10) 0.0014(8) -0.0006(8) 0.0032(8) C41 0.0210(11) 0.0181(11) 0.0197(11) 0.0046(9) 0.0020(9) -0.0033(9) N41 0.0258(11) 0.0274(12) 0.0466(14) 0.0012(10) 0.0144(10) 0.0031(9) C51 0.0113(9) 0.0187(11) 0.0159(10) 0.0026(8) -0.0009(8) -0.0008(8) N52 0.0163(8) 0.0136(9) 0.0193(9) 0.0030(7) 0.0045(7) -0.0001(7) N53 0.0167(9) 0.0182(10) 0.0150(9) 0.0025(7) 0.0033(7) -0.0011(7) N54 0.0147(8) 0.0158(9) 0.0170(9) 0.0010(7) 0.0015(7) 0.0006(7) N55 0.0154(8) 0.0157(9) 0.0154(9) 0.0038(7) 0.0033(7) 0.0001(7) P1 0.0147(3) 0.0179(3) 0.0183(3) 0.0039(2) 0.0040(2) 0.0012(2) C111 0.0173(10) 0.0216(11) 0.0175(11) 0.0032(9) 0.0056(9) -0.0030(8) C112 0.0202(11) 0.0228(13) 0.0388(15) 0.0056(10) 0.0086(10) 0.0015(9) C113 0.0296(13) 0.0218(13) 0.0544(18) 0.0021(12) 0.0167(13) -0.0055(10) C114 0.0186(12) 0.0347(15) 0.0509(17) -0.0025(12) 0.0109(12) -0.0081(10) C115 0.0180(12) 0.0400(16) 0.0395(16) 0.0039(12) 0.0023(11) 0.0013(11) C116 0.0195(11) 0.0278(13) 0.0267(13) 0.0045(10) 0.0052(10) -0.0001(9) C121 0.0186(10) 0.0224(11) 0.0190(11) 0.0093(9) 0.0055(9) 0.0048(9) C122 0.0219(11) 0.0225(12) 0.0269(13) 0.0041(10) 0.0050(10) 0.0022(9) C123 0.0397(14) 0.0224(12) 0.0218(13) 0.0018(10) 0.0068(11) 0.0050(11) C124 0.0421(15) 0.0322(14) 0.0214(13) 0.0087(10) 0.0142(11) 0.0143(11) C125 0.0213(12) 0.0408(15) 0.0268(13) 0.0177(11) 0.0106(10) 0.0095(10) C126 0.0176(11) 0.0275(13) 0.0226(12) 0.0064(9) 0.0027(9) 0.0038(9) C131 0.0141(10) 0.0184(11) 0.0195(11) 0.0027(8) 0.0024(8) -0.0002(8) C132 0.0249(12) 0.0227(12) 0.0260(13) 0.0040(10) 0.0085(10) 0.0032(9) C133 0.0303(13) 0.0279(13) 0.0297(13) 0.0133(10) 0.0093(11) 0.0038(10) C134 0.0189(11) 0.0188(12) 0.0332(14) 0.0032(10) 0.0023(10) 0.0011(9) C135 0.0315(13) 0.0296(14) 0.0240(13) 0.0011(10) 0.0063(10) 0.0094(10) C136 0.0370(14) 0.0339(14) 0.0238(13) 0.0083(10) 0.0100(11) 0.0134(11) P2 0.0163(3) 0.0190(3) 0.0150(3) 0.0021(2) 0.0016(2) -0.0014(2) C211 0.0191(10) 0.0168(11) 0.0165(11) 0.0048(8) 0.0036(8) 0.0029(8) C212 0.0193(11) 0.0270(13) 0.0193(12) 0.0028(9) 0.0015(9) -0.0004(9) C213 0.0236(11) 0.0239(12) 0.0248(12) 0.0077(9) 0.0109(10) 0.0077(9) C214 0.0310(12) 0.0151(11) 0.0191(11) 0.0003(8) 0.0090(10) 0.0019(9) C215 0.0258(12) 0.0152(11) 0.0206(12) 0.0021(9) 0.0035(9) -0.0026(9) C216 0.0213(11) 0.0176(11) 0.0162(11) 0.0047(8) 0.0047(9) -0.0001(8) C221 0.0193(11) 0.0201(12) 0.0272(13) -0.0007(9) 0.0085(10) 0.0010(9) C222 0.0261(12) 0.0237(13) 0.0304(14) 0.0033(10) 0.0066(10) -0.0033(10) C223 0.0294(14) 0.0331(15) 0.0471(18) -0.0024(13) 0.0076(13) -0.0118(11) C224 0.0392(15) 0.0212(13) 0.0553(18) 0.0030(12) 0.0261(14) -0.0055(11) C225 0.0389(15) 0.0307(14) 0.0420(16) 0.0137(12) 0.0214(13) 0.0054(12) C226 0.0256(12) 0.0310(14) 0.0278(13) 0.0079(10) 0.0076(10) -0.0056(10) C231 0.0130(10) 0.0272(12) 0.0215(12) 0.0060(9) 0.0040(9) 0.0014(9) C232 0.0212(11) 0.0286(13) 0.0176(11) 0.0072(9) 0.0054(9) 0.0005(9) C233 0.0293(13) 0.0295(13) 0.0240(13) 0.0056(10) 0.0081(10) 0.0070(10) C234 0.0267(12) 0.0443(16) 0.0252(13) 0.0160(11) 0.0050(10) 0.0128(11) C235 0.0232(12) 0.0454(16) 0.0149(11) 0.0042(10) -0.0008(9) -0.0001(11) C236 0.0210(11) 0.0290(13) 0.0198(12) 0.0017(10) 0.0018(9) -0.0019(9) P3 0.0204(3) 0.0161(3) 0.0133(3) 0.0028(2) 0.0021(2) 0.0007(2) C311 0.0248(11) 0.0231(12) 0.0114(10) 0.0045(8) 0.0027(9) 0.0030(9) C312 0.0319(13) 0.0242(13) 0.0251(13) 0.0042(10) 0.0095(10) 0.0023(10) C313 0.0470(16) 0.0298(14) 0.0312(15) 0.0036(11) 0.0186(13) 0.0122(12) C314 0.0373(15) 0.0438(16) 0.0332(15) 0.0132(12) 0.0193(12) 0.0186(12) C315 0.0285(13) 0.0400(16) 0.0300(14) 0.0107(11) 0.0126(11) 0.0030(11) C316 0.0288(12) 0.0270(13) 0.0200(12) 0.0066(9) 0.0085(10) 0.0032(10) C321 0.0214(11) 0.0190(11) 0.0164(11) 0.0000(8) 0.0030(9) 0.0022(9) C322 0.0262(12) 0.0205(12) 0.0199(12) 0.0024(9) 0.0005(9) 0.0002(9) C323 0.0362(14) 0.0220(13) 0.0313(14) 0.0077(10) 0.0058(11) -0.0052(10) C324 0.0257(13) 0.0330(14) 0.0341(15) 0.0000(11) -0.0018(11) -0.0095(10) C325 0.0311(13) 0.0370(15) 0.0246(13) 0.0067(11) -0.0078(11) -0.0034(11) C326 0.0329(13) 0.0276(13) 0.0213(12) 0.0065(10) -0.0009(10) -0.0033(10) C331 0.0219(11) 0.0188(11) 0.0147(11) 0.0034(8) 0.0005(9) -0.0010(9) C332 0.0348(13) 0.0255(13) 0.0167(11) 0.0017(9) 0.0054(10) 0.0035(10) C333 0.0434(15) 0.0313(14) 0.0172(12) 0.0092(10) 0.0097(11) 0.0023(11) C334 0.0349(13) 0.0264(13) 0.0187(12) 0.0099(10) 0.0003(10) -0.0028(10) C335 0.0216(11) 0.0197(12) 0.0257(12) 0.0036(9) 0.0000(10) -0.0004(9) C336 0.0188(10) 0.0215(12) 0.0199(11) 0.0057(9) 0.0021(9) -0.0015(9) C101 0.079(2) 0.102(3) 0.0396(18) 0.0517(19) 0.0427(18) 0.069(2) C102 0.126(3) 0.0295(16) 0.0414(18) 0.0071(13) 0.056(2) -0.0087(19) C103 0.0345(15) 0.078(2) 0.0229(14) -0.0014(14) 0.0128(12) -0.0175(15) C104 0.0569(18) 0.0412(16) 0.0182(12) 0.0083(11) 0.0181(12) 0.0217(13) C105 0.0396(15) 0.070(2) 0.0092(11) -0.0013(12) 0.0051(11) -0.0250(14) C201 0.0241(11) 0.0232(12) 0.0125(11) 0.0040(9) -0.0072(9) 0.0014(9) C202 0.0258(12) 0.0267(12) 0.0092(10) 0.0058(9) 0.0006(9) 0.0055(9) C203 0.0274(12) 0.0203(11) 0.0185(11) 0.0094(9) 0.0027(9) -0.0003(9) C204 0.0304(12) 0.0187(11) 0.0187(11) 0.0058(9) 0.0024(10) 0.0082(9) C205 0.0142(10) 0.0293(13) 0.0186(11) 0.0096(9) 0.0021(9) 0.0064(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.050(2) . ? Ru1 N52 2.0950(17) . ? Ru1 C102 2.176(3) . ? Ru1 C103 2.190(2) . ? Ru1 C101 2.191(3) . ? Ru1 C105 2.213(2) . ? Ru1 C104 2.231(2) . ? Ru1 P1 2.3127(6) . ? Ru2 N54 2.0854(17) . ? Ru2 C205 2.216(2) . ? Ru2 C204 2.217(2) . ? Ru2 C203 2.217(2) . ? Ru2 C201 2.218(2) . ? Ru2 C202 2.231(2) . ? Ru2 P3 2.3228(6) . ? Ru2 P2 2.3393(6) . ? C1 C2 1.364(3) . ? C1 C11 1.445(3) . ? C1 C12 1.447(3) . ? C11 N11 1.140(3) . ? C12 N12 1.140(3) . ? C2 C3 1.462(3) . ? C2 C21 1.483(3) . ? C21 C26 1.392(3) . ? C21 C22 1.393(3) . ? C22 C23 1.387(3) . ? C22 H22 0.95 . ? C23 C24 1.382(4) . ? C23 H23 0.95 . ? C24 C25 1.377(4) . ? C24 H24 0.95 . ? C25 C26 1.388(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.366(3) . ? C4 C41 1.432(3) . ? C4 C51 1.450(3) . ? C41 N41 1.141(3) . ? C51 N55 1.330(3) . ? C51 N52 1.345(2) . ? N52 N53 1.341(2) . ? N53 N54 1.330(2) . ? N54 N55 1.350(2) . ? P1 C111 1.831(2) . ? P1 C121 1.836(2) . ? P1 C131 1.845(2) . ? C111 C112 1.387(3) . ? C111 C116 1.391(3) . ? C112 C113 1.390(3) . ? C112 H112 0.95 . ? C113 C114 1.375(3) . ? C113 H113 0.95 . ? C114 C115 1.374(3) . ? C114 H114 0.95 . ? C115 C116 1.383(3) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.392(3) . ? C121 C122 1.393(3) . ? C122 C123 1.388(3) . ? C122 H122 0.95 . ? C123 C124 1.383(3) . ? C123 H123 0.95 . ? C124 C125 1.375(3) . ? C124 H124 0.95 . ? C125 C126 1.384(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.385(3) . ? C131 C132 1.390(3) . ? C132 C133 1.390(3) . ? C132 H132 0.95 . ? C133 C134 1.371(3) . ? C133 H133 0.95 . ? C134 C135 1.377(3) . ? C134 H134 0.95 . ? C135 C136 1.391(3) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C231 1.840(2) . ? P2 C211 1.847(2) . ? P2 C221 1.853(2) . ? C211 C216 1.394(3) . ? C211 C212 1.398(3) . ? C212 C213 1.383(3) . ? C212 H212 0.95 . ? C213 C214 1.383(3) . ? C213 H213 0.95 . ? C214 C215 1.379(3) . ? C214 H214 0.95 . ? C215 C216 1.392(3) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.389(3) . ? C221 C226 1.395(3) . ? C222 C223 1.395(3) . ? C222 H222 0.95 . ? C223 C224 1.369(4) . ? C223 H223 0.95 . ? C224 C225 1.391(4) . ? C224 H224 0.95 . ? C225 C226 1.388(3) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C231 C232 1.394(3) . ? C231 C236 1.408(3) . ? C232 C233 1.384(3) . ? C232 H232 0.95 . ? C233 C234 1.380(3) . ? C233 H233 0.95 . ? C234 C235 1.384(3) . ? C234 H234 0.95 . ? C235 C236 1.382(3) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? P3 C331 1.833(2) . ? P3 C321 1.837(2) . ? P3 C311 1.844(2) . ? C311 C312 1.384(3) . ? C311 C316 1.399(3) . ? C312 C313 1.389(3) . ? C312 H312 0.95 . ? C313 C314 1.380(3) . ? C313 H313 0.95 . ? C314 C315 1.383(3) . ? C314 H314 0.95 . ? C315 C316 1.387(3) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 C322 1.387(3) . ? C321 C326 1.395(3) . ? C322 C323 1.390(3) . ? C322 H322 0.95 . ? C323 C324 1.375(3) . ? C323 H323 0.95 . ? C324 C325 1.381(3) . ? C324 H324 0.95 . ? C325 C326 1.386(3) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C331 C336 1.392(3) . ? C331 C332 1.399(3) . ? C332 C333 1.388(3) . ? C332 H332 0.95 . ? C333 C334 1.385(3) . ? C333 H333 0.95 . ? C334 C335 1.376(3) . ? C334 H334 0.95 . ? C335 C336 1.381(3) . ? C335 H335 0.95 . ? C336 H336 0.95 . ? C101 C105 1.385(4) . ? C101 C102 1.413(5) . ? C101 H101 0.95 . ? C102 C103 1.351(4) . ? C102 H102 0.95 . ? C103 C104 1.371(4) . ? C103 H103 0.95 . ? C104 C105 1.398(4) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C201 C202 1.402(3) . ? C201 C205 1.427(3) . ? C201 H201 0.95 . ? C202 C203 1.433(3) . ? C202 H202 0.95 . ? C203 C204 1.409(3) . ? C203 H203 0.95 . ? C204 C205 1.419(3) . ? C204 H204 0.95 . ? C205 H205 0.95 . ? 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 C3 Ru1 N52 76.41(7) . . ? C3 Ru1 C102 104.41(11) . . ? N52 Ru1 C102 160.31(11) . . ? C3 Ru1 C103 138.98(11) . . ? N52 Ru1 C103 144.01(10) . . ? C102 Ru1 C103 36.03(12) . . ? C3 Ru1 C101 94.07(9) . . ? N52 Ru1 C101 122.86(12) . . ? C102 Ru1 C101 37.76(12) . . ? C103 Ru1 C101 61.24(12) . . ? C3 Ru1 C105 118.81(10) . . ? N52 Ru1 C105 100.25(8) . . ? C102 Ru1 C105 61.72(11) . . ? C103 Ru1 C105 60.93(9) . . ? C101 Ru1 C105 36.64(11) . . ? C3 Ru1 C104 154.31(9) . . ? N52 Ru1 C104 110.34(9) . . ? C102 Ru1 C104 60.73(11) . . ? C103 Ru1 C104 36.11(10) . . ? C101 Ru1 C104 61.09(10) . . ? C105 Ru1 C104 36.67(10) . . ? C3 Ru1 P1 97.71(6) . . ? N52 Ru1 P1 86.98(5) . . ? C102 Ru1 P1 112.14(11) . . ? C103 Ru1 P1 92.55(8) . . ? C101 Ru1 P1 149.84(11) . . ? C105 Ru1 P1 143.47(8) . . ? C104 Ru1 P1 107.23(7) . . ? N54 Ru2 C205 99.13(7) . . ? N54 Ru2 C204 134.27(7) . . ? C205 Ru2 C204 37.35(8) . . ? N54 Ru2 C203 154.31(7) . . ? C205 Ru2 C203 62.68(8) . . ? C204 Ru2 C203 37.07(8) . . ? N54 Ru2 C201 92.18(7) . . ? C205 Ru2 C201 37.56(8) . . ? C204 Ru2 C201 61.99(8) . . ? C203 Ru2 C201 62.25(8) . . ? N54 Ru2 C202 119.13(7) . . ? C205 Ru2 C202 62.34(8) . . ? C204 Ru2 C202 61.95(8) . . ? C203 Ru2 C202 37.59(7) . . ? C201 Ru2 C202 36.72(8) . . ? N54 Ru2 P3 88.35(5) . . ? C205 Ru2 P3 103.72(6) . . ? C204 Ru2 P3 90.45(6) . . ? C203 Ru2 P3 112.67(6) . . ? C201 Ru2 P3 140.77(6) . . ? C202 Ru2 P3 149.85(6) . . ? N54 Ru2 P2 92.33(5) . . ? C205 Ru2 P2 154.19(6) . . ? C204 Ru2 P2 132.77(6) . . ? C203 Ru2 P2 98.17(6) . . ? C201 Ru2 P2 119.53(6) . . ? C202 Ru2 P2 91.87(6) . . ? P3 Ru2 P2 99.63(2) . . ? C2 C1 C11 123.30(19) . . ? C2 C1 C12 122.16(19) . . ? C11 C1 C12 114.50(19) . . ? N11 C11 C1 178.1(2) . . ? N12 C12 C1 176.8(3) . . ? C1 C2 C3 120.62(18) . . ? C1 C2 C21 120.71(19) . . ? C3 C2 C21 118.67(18) . . ? C26 C21 C22 119.3(2) . . ? C26 C21 C2 119.1(2) . . ? C22 C21 C2 121.5(2) . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C25 C26 C21 120.3(2) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? C4 C3 C2 119.38(18) . . ? C4 C3 Ru1 118.40(15) . . ? C2 C3 Ru1 121.62(15) . . ? C3 C4 C41 124.86(19) . . ? C3 C4 C51 113.33(18) . . ? C41 C4 C51 121.80(19) . . ? N41 C41 C4 176.3(2) . . ? N55 C51 N52 111.73(18) . . ? N55 C51 C4 132.96(19) . . ? N52 C51 C4 115.21(18) . . ? N53 N52 C51 106.85(16) . . ? N53 N52 Ru1 136.40(13) . . ? C51 N52 Ru1 116.63(13) . . ? N54 N53 N52 105.99(15) . . ? N53 N54 N55 112.40(16) . . ? N53 N54 Ru2 121.69(12) . . ? N55 N54 Ru2 125.92(13) . . ? C51 N55 N54 103.03(16) . . ? C111 P1 C121 101.07(9) . . ? C111 P1 C131 102.59(9) . . ? C121 P1 C131 100.76(10) . . ? C111 P1 Ru1 115.40(7) . . ? C121 P1 Ru1 122.06(7) . . ? C131 P1 Ru1 112.28(7) . . ? C112 C111 C116 119.01(19) . . ? C112 C111 P1 118.10(16) . . ? C116 C111 P1 122.70(17) . . ? C111 C112 C113 120.5(2) . . ? C111 C112 H112 119.8 . . ? C113 C112 H112 119.8 . . ? C114 C113 C112 119.7(2) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C115 C114 C113 120.4(2) . . ? C115 C114 H114 119.8 . . ? C113 C114 H114 119.8 . . ? C114 C115 C116 120.3(2) . . ? C114 C115 H115 119.9 . . ? C116 C115 H115 119.9 . . ? C115 C116 C111 120.2(2) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C126 C121 C122 118.0(2) . . ? C126 C121 P1 119.01(16) . . ? C122 C121 P1 122.98(17) . . ? C123 C122 C121 120.7(2) . . ? C123 C122 H122 119.7 . . ? C121 C122 H122 119.7 . . ? C124 C123 C122 120.5(2) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C125 C124 C123 119.2(2) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C124 C125 C126 120.7(2) . . ? C124 C125 H125 119.7 . . ? C126 C125 H125 119.7 . . ? C125 C126 C121 120.9(2) . . ? C125 C126 H126 119.5 . . ? C121 C126 H126 119.5 . . ? C136 C131 C132 118.3(2) . . ? C136 C131 P1 118.23(17) . . ? C132 C131 P1 123.42(16) . . ? C133 C132 C131 120.4(2) . . ? C133 C132 H132 119.8 . . ? C131 C132 H132 119.8 . . ? C134 C133 C132 120.6(2) . . ? C134 C133 H133 119.7 . . ? C132 C133 H133 119.7 . . ? C133 C134 C135 119.8(2) . . ? C133 C134 H134 120.1 . . ? C135 C134 H134 120.1 . . ? C134 C135 C136 119.8(2) . . ? C134 C135 H135 120.1 . . ? C136 C135 H135 120.1 . . ? C131 C136 C135 121.1(2) . . ? C131 C136 H136 119.5 . . ? C135 C136 H136 119.5 . . ? C231 P2 C211 98.89(9) . . ? C231 P2 C221 104.70(10) . . ? C211 P2 C221 98.06(10) . . ? C231 P2 Ru2 122.42(7) . . ? C211 P2 Ru2 115.00(7) . . ? C221 P2 Ru2 114.14(7) . . ? C216 C211 C212 118.34(18) . . ? C216 C211 P2 122.52(16) . . ? C212 C211 P2 119.07(15) . . ? C213 C212 C211 121.06(19) . . ? C213 C212 H212 119.5 . . ? C211 C212 H212 119.5 . . ? C214 C213 C212 119.7(2) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C215 C214 C213 120.28(19) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C214 C215 C216 120.08(19) . . ? C214 C215 H215 120 . . ? C216 C215 H215 120 . . ? C215 C216 C211 120.48(19) . . ? C215 C216 H216 119.8 . . ? C211 C216 H216 119.8 . . ? C222 C221 C226 117.0(2) . . ? C222 C221 P2 125.69(19) . . ? C226 C221 P2 117.26(16) . . ? C221 C222 C223 121.0(2) . . ? C221 C222 H222 119.5 . . ? C223 C222 H222 119.5 . . ? C224 C223 C222 121.1(2) . . ? C224 C223 H223 119.5 . . ? C222 C223 H223 119.5 . . ? C223 C224 C225 119.1(2) . . ? C223 C224 H224 120.4 . . ? C225 C224 H224 120.4 . . ? C226 C225 C224 119.5(2) . . ? C226 C225 H225 120.2 . . ? C224 C225 H225 120.2 . . ? C225 C226 C221 122.2(2) . . ? C225 C226 H226 118.9 . . ? C221 C226 H226 118.9 . . ? C232 C231 C236 117.7(2) . . ? C232 C231 P2 120.51(16) . . ? C236 C231 P2 121.61(17) . . ? C233 C232 C231 121.1(2) . . ? C233 C232 H232 119.5 . . ? C231 C232 H232 119.5 . . ? C234 C233 C232 120.3(2) . . ? C234 C233 H233 119.9 . . ? C232 C233 H233 119.9 . . ? C233 C234 C235 119.9(2) . . ? C233 C234 H234 120 . . ? C235 C234 H234 120 . . ? C236 C235 C234 120.0(2) . . ? C236 C235 H235 120 . . ? C234 C235 H235 120 . . ? C235 C236 C231 121.0(2) . . ? C235 C236 H236 119.5 . . ? C231 C236 H236 119.5 . . ? C331 P3 C321 103.50(10) . . ? C331 P3 C311 100.89(10) . . ? C321 P3 C311 102.25(9) . . ? C331 P3 Ru2 120.31(7) . . ? C321 P3 Ru2 117.39(7) . . ? C311 P3 Ru2 109.89(7) . . ? C312 C311 C316 119.1(2) . . ? C312 C311 P3 123.23(17) . . ? C316 C311 P3 117.51(16) . . ? C311 C312 C313 120.6(2) . . ? C311 C312 H312 119.7 . . ? C313 C312 H312 119.7 . . ? C314 C313 C312 120.0(2) . . ? C314 C313 H313 120 . . ? C312 C313 H313 120 . . ? C313 C314 C315 120.0(2) . . ? C313 C314 H314 120 . . ? C315 C314 H314 120 . . ? C314 C315 C316 120.2(2) . . ? C314 C315 H315 119.9 . . ? C316 C315 H315 119.9 . . ? C315 C316 C311 120.0(2) . . ? C315 C316 H316 120 . . ? C311 C316 H316 120 . . ? C322 C321 C326 119.13(19) . . ? C322 C321 P3 117.97(16) . . ? C326 C321 P3 122.90(17) . . ? C321 C322 C323 120.1(2) . . ? C321 C322 H322 119.9 . . ? C323 C322 H322 119.9 . . ? C324 C323 C322 120.2(2) . . ? C324 C323 H323 119.9 . . ? C322 C323 H323 119.9 . . ? C323 C324 C325 120.3(2) . . ? C323 C324 H324 119.8 . . ? C325 C324 H324 119.8 . . ? C324 C325 C326 119.8(2) . . ? C324 C325 H325 120.1 . . ? C326 C325 H325 120.1 . . ? C325 C326 C321 120.4(2) . . ? C325 C326 H326 119.8 . . ? C321 C326 H326 119.8 . . ? C336 C331 C332 117.7(2) . . ? C336 C331 P3 120.55(16) . . ? C332 C331 P3 121.71(17) . . ? C333 C332 C331 120.9(2) . . ? C333 C332 H332 119.6 . . ? C331 C332 H332 119.6 . . ? C334 C333 C332 120.0(2) . . ? C334 C333 H333 120 . . ? C332 C333 H333 120 . . ? C335 C334 C333 119.7(2) . . ? C335 C334 H334 120.2 . . ? C333 C334 H334 120.2 . . ? C334 C335 C336 120.4(2) . . ? C334 C335 H335 119.8 . . ? C336 C335 H335 119.8 . . ? C335 C336 C331 121.3(2) . . ? C335 C336 H336 119.3 . . ? C331 C336 H336 119.3 . . ? C105 C101 C102 107.2(3) . . ? C105 C101 Ru1 72.52(15) . . ? C102 C101 Ru1 70.54(16) . . ? C105 C101 H101 126.4 . . ? C102 C101 H101 126.4 . . ? Ru1 C101 H101 122.2 . . ? C103 C102 C101 107.7(3) . . ? C103 C102 Ru1 72.55(16) . . ? C101 C102 Ru1 71.70(16) . . ? C103 C102 H102 126.2 . . ? C101 C102 H102 126.2 . . ? Ru1 C102 H102 121.3 . . ? C102 C103 C104 109.9(3) . . ? C102 C103 Ru1 71.42(16) . . ? C104 C103 Ru1 73.56(15) . . ? C102 C103 H103 125 . . ? C104 C103 H103 125 . . ? Ru1 C103 H103 121.6 . . ? C103 C104 C105 107.5(2) . . ? C103 C104 Ru1 70.33(14) . . ? C105 C104 Ru1 70.97(14) . . ? C103 C104 H104 126.3 . . ? C105 C104 H104 126.3 . . ? Ru1 C104 H104 124.1 . . ? C101 C105 C104 107.8(2) . . ? C101 C105 Ru1 70.84(15) . . ? C104 C105 Ru1 72.36(14) . . ? C101 C105 H105 126.1 . . ? C104 C105 H105 126.1 . . ? Ru1 C105 H105 122.4 . . ? C202 C201 C205 108.90(19) . . ? C202 C201 Ru2 72.13(11) . . ? C205 C201 Ru2 71.13(11) . . ? C202 C201 H201 125.5 . . ? C205 C201 H201 125.5 . . ? Ru2 C201 H201 122.8 . . ? C201 C202 C203 107.94(19) . . ? C201 C202 Ru2 71.14(12) . . ? C203 C202 Ru2 70.67(12) . . ? C201 C202 H202 126 . . ? C203 C202 H202 126 . . ? Ru2 C202 H202 123.8 . . ? C204 C203 C202 107.28(19) . . ? C204 C203 Ru2 71.47(12) . . ? C202 C203 Ru2 71.73(12) . . ? C204 C203 H203 126.4 . . ? C202 C203 H203 126.4 . . ? Ru2 C203 H203 122.2 . . ? C203 C204 C205 109.17(19) . . ? C203 C204 Ru2 71.47(12) . . ? C205 C204 Ru2 71.28(12) . . ? C203 C204 H204 125.4 . . ? C205 C204 H204 125.4 . . ? Ru2 C204 H204 123.5 . . ? C204 C205 C201 106.69(19) . . ? C204 C205 Ru2 71.37(11) . . ? C201 C205 Ru2 71.31(11) . . ? C204 C205 H205 126.7 . . ? C201 C205 H205 126.7 . . ? Ru2 C205 H205 122.4 . . ? #===END # Attachment '5.br1396.cif' data_br1396 _database_code_depnum_ccdc_archive 'CCDC 730745' _audit_creation_date 2008-01-15T14:57:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C68 H54 Fe N7 P3 Ru' _chemical_formula_moiety 'C68 H54 Fe N7 P3 Ru' _chemical_formula_weight 1219.01 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall -p_2ybc 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 11.8912(3) _cell_length_b 32.4015(10) _cell_length_c 15.3484(4) _cell_angle_alpha 90 _cell_angle_beta 99.774(3) _cell_angle_gamma 90 _cell_volume 5827.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6582 _cell_measurement_theta_min 2.7205 _cell_measurement_theta_max 67.1747 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.35373 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0069105767 _diffrn_orient_matrix_ub_12 -0.0033589842 _diffrn_orient_matrix_ub_13 -0.1012154837 _diffrn_orient_matrix_ub_21 0.1314317496 _diffrn_orient_matrix_ub_22 -0.0025317794 _diffrn_orient_matrix_ub_23 0.0125294585 _diffrn_orient_matrix_ub_31 -0.0063776288 _diffrn_orient_matrix_ub_32 -0.0475385443 _diffrn_orient_matrix_ub_33 0.0064995508 _diffrn_reflns_av_R_equivalents 0.1240 _diffrn_reflns_av_unetI/netI 0.0737 _diffrn_reflns_number 73154 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 67.6 _diffrn_reflns_theta_full 67.6 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 10360 _reflns_number_gt 5010 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1572P)^2^+0.0000P] 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_number_reflns 10360 _refine_ls_number_parameters 721 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.0851 _refine_ls_wR_factor_ref 0.2783 _refine_ls_wR_factor_gt 0.2329 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.949 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.81517(6) 0.31701(2) 0.07467(5) 0.0715(3) Uani 1 1 d . . . Fe2 Fe 1.07222(17) 0.38002(6) 0.42429(11) 0.1050(7) Uani 1 1 d . . . C1 C 0.4957(9) 0.2989(3) 0.1008(8) 0.096(3) Uani 1 1 d . . . C11 C 0.3855(9) 0.2846(3) 0.0595(9) 0.104(4) Uani 1 1 d . . . N11 N 0.2961(8) 0.2736(3) 0.0359(9) 0.136(4) Uani 1 1 d . . . C12 C 0.5371(11) 0.2803(4) 0.1835(11) 0.110(4) Uani 1 1 d . . . N12 N 0.5698(10) 0.2641(4) 0.2510(9) 0.132(4) Uani 1 1 d . . . C2 C 0.5585(9) 0.3279(3) 0.0629(7) 0.087(3) Uani 1 1 d . . . C21 C 0.5093(9) 0.3436(3) -0.0267(8) 0.093(3) Uani 1 1 d . . . C22 C 0.4798(10) 0.3180(5) -0.0988(10) 0.124(5) Uani 1 1 d . . . H22 H 0.4928 0.2892 -0.0912 0.149 Uiso 1 1 calc R . . C23 C 0.4321(11) 0.3325(7) -0.1819(12) 0.157(9) Uani 1 1 d . . . H23 H 0.4122 0.3146 -0.2312 0.188 Uiso 1 1 calc R . . C24 C 0.4157(14) 0.3739(7) -0.1878(10) 0.156(8) Uani 1 1 d . . . H24 H 0.383 0.3849 -0.2438 0.187 Uiso 1 1 calc R . . C25 C 0.4424(11) 0.4005(5) -0.1202(10) 0.125(4) Uani 1 1 d . . . H25 H 0.4283 0.4292 -0.1282 0.149 Uiso 1 1 calc R . . C26 C 0.4908(9) 0.3849(3) -0.0392(7) 0.092(3) Uani 1 1 d . . . H26 H 0.5117 0.4032 0.0091 0.111 Uiso 1 1 calc R . . C3 C 0.6697(8) 0.3409(3) 0.1107(7) 0.079(2) Uani 1 1 d . . . C4 C 0.6803(9) 0.3649(3) 0.1841(7) 0.092(3) Uani 1 1 d . . . C41 C 0.5868(10) 0.3860(4) 0.2095(9) 0.116(4) Uani 1 1 d . . . N41 N 0.5107(9) 0.4051(4) 0.2309(9) 0.142(4) Uani 1 1 d . . . C51 C 0.7949(8) 0.3683(3) 0.2295(7) 0.084(3) Uani 1 1 d . . . N52 N 0.8731(6) 0.3496(2) 0.1886(5) 0.077(2) Uani 1 1 d . . . N53 N 0.9722(7) 0.3536(2) 0.2429(5) 0.080(2) Uani 1 1 d . . . N54 N 0.9550(7) 0.3742(2) 0.3143(5) 0.088(2) Uani 1 1 d . . . N55 N 0.8418(8) 0.3835(3) 0.3077(6) 0.100(3) Uani 1 1 d . . . P1 P 0.85480(19) 0.37245(7) -0.00880(16) 0.0722(6) Uani 1 1 d . . . C111 C 0.8502(8) 0.3614(3) -0.1249(6) 0.078(2) Uani 1 1 d . . . C112 C 0.7568(9) 0.3400(3) -0.1719(7) 0.089(3) Uani 1 1 d . . . H112 H 0.6989 0.3305 -0.1411 0.107 Uiso 1 1 calc R . . C113 C 0.7460(12) 0.3322(4) -0.2619(7) 0.114(4) Uani 1 1 d . . . H113 H 0.6808 0.3181 -0.292 0.136 Uiso 1 1 calc R . . C114 C 0.8282(11) 0.3446(4) -0.3065(7) 0.109(4) Uani 1 1 d . . . H114 H 0.8211 0.3389 -0.3679 0.13 Uiso 1 1 calc R . . C115 C 0.9227(10) 0.3656(4) -0.2639(7) 0.102(3) Uani 1 1 d . . . H115 H 0.9792 0.3751 -0.296 0.123 Uiso 1 1 calc R . . C116 C 0.9344(9) 0.3728(3) -0.1728(6) 0.089(3) Uani 1 1 d . . . H116 H 1.0017 0.3858 -0.143 0.107 Uiso 1 1 calc R . . C121 C 0.7690(8) 0.4197(3) -0.0163(9) 0.095(3) Uani 1 1 d . . . C122 C 0.7187(9) 0.4370(4) -0.0968(11) 0.120(4) Uani 1 1 d . . . H122 H 0.7305 0.4246 -0.1507 0.144 Uiso 1 1 calc R . . C123 C 0.6499(11) 0.4730(4) -0.0987(14) 0.151(7) Uani 1 1 d . . . H123 H 0.6165 0.4853 -0.1532 0.182 Uiso 1 1 calc R . . C124 C 0.6332(12) 0.4894(5) -0.0193(18) 0.167(10) Uani 1 1 d . . . H124 H 0.5845 0.5127 -0.0198 0.201 Uiso 1 1 calc R . . C125 C 0.6827(12) 0.4739(4) 0.0589(15) 0.149(7) Uani 1 1 d . . . H125 H 0.67 0.4865 0.1122 0.178 Uiso 1 1 calc R . . C126 C 0.7534(9) 0.4390(3) 0.0618(9) 0.105(4) Uani 1 1 d . . . H126 H 0.7906 0.4286 0.1171 0.126 Uiso 1 1 calc R . . C131 C 0.9992(7) 0.3927(3) 0.0214(5) 0.068(2) Uani 1 1 d . . . C132 C 1.0245(10) 0.4339(4) 0.0333(11) 0.133(5) Uani 1 1 d . . . H132 H 0.9645 0.4534 0.0323 0.159 Uiso 1 1 calc R . . C133 C 1.1396(10) 0.4477(4) 0.0470(12) 0.157(7) Uani 1 1 d . . . H133 H 1.1555 0.4764 0.0525 0.188 Uiso 1 1 calc R . . C134 C 1.2279(9) 0.4202(3) 0.0524(8) 0.099(3) Uani 1 1 d . . . H134 H 1.3049 0.4295 0.0617 0.118 Uiso 1 1 calc R . . C135 C 1.2024(8) 0.3790(3) 0.0438(7) 0.086(3) Uani 1 1 d . . . H135 H 1.2625 0.3594 0.0484 0.103 Uiso 1 1 calc R . . C136 C 1.0913(8) 0.3656(3) 0.0288(6) 0.080(2) Uani 1 1 d . . . H136 H 1.0767 0.3368 0.0232 0.096 Uiso 1 1 calc R . . P2 P 1.2027(2) 0.34648(10) 0.36403(16) 0.0941(8) Uani 1 1 d . . . C211 C 1.1770(8) 0.2940(3) 0.3209(6) 0.089(3) Uani 1 1 d D . . C212 C 1.2348(9) 0.2789(4) 0.2562(8) 0.147(6) Uani 1 1 d D . . H212 H 1.2864 0.2963 0.2326 0.176 Uiso 1 1 calc R . . C213 C 1.2183(11) 0.2388(4) 0.2256(9) 0.163(7) Uani 1 1 d D . . H213 H 1.2552 0.2294 0.179 0.195 Uiso 1 1 calc R . . C214 C 1.1500(10) 0.2128(3) 0.2617(8) 0.120(4) Uani 1 1 d D . . H214 H 1.1464 0.1844 0.2461 0.144 Uiso 1 1 calc R . . C215 C 1.0852(15) 0.2279(4) 0.3216(10) 0.184(9) Uani 1 1 d D . . H215 H 1.0307 0.2107 0.3425 0.221 Uiso 1 1 calc R . . C216 C 1.1009(13) 0.2685(4) 0.3509(8) 0.168(7) Uani 1 1 d D . . H216 H 1.0575 0.2787 0.3928 0.202 Uiso 1 1 calc R . . C221 C 1.3487(9) 0.3405(4) 0.4266(7) 0.122(5) Uani 1 1 d D . . C222 C 1.4457(11) 0.3438(6) 0.3871(9) 0.260(15) Uani 1 1 d D . . H222 H 1.4378 0.3499 0.3258 0.312 Uiso 1 1 calc R . . C223 C 1.5530(12) 0.3381(7) 0.4362(12) 0.277(15) Uani 1 1 d D . . H223 H 1.6185 0.3403 0.4087 0.332 Uiso 1 1 calc R . . C224 C 1.5654(15) 0.3294(5) 0.5253(11) 0.223(14) Uani 1 1 d D . . H224 H 1.6392 0.3249 0.5588 0.267 Uiso 1 1 calc R . . C225 C 1.4694(17) 0.3272(9) 0.5661(10) 0.36(3) Uani 1 1 d D . . H225 H 1.4772 0.3246 0.6284 0.432 Uiso 1 1 calc R . . C226 C 1.3612(12) 0.3289(5) 0.5132(7) 0.153(6) Uani 1 1 d D . . H226 H 1.2957 0.3219 0.5379 0.184 Uiso 1 1 calc R . . C20 C 1.2315(8) 0.3786(3) 0.2707(6) 0.079(2) Uani 1 1 d . . . H20A H 1.2971 0.3674 0.2462 0.095 Uiso 1 1 calc R . . H20B H 1.164 0.3792 0.223 0.095 Uiso 1 1 calc R . . C30 C 1.2566(11) 0.4192(4) 0.3058(9) 0.116(4) Uani 1 1 d . . . H30A H 1.2528 0.4392 0.2566 0.14 Uiso 1 1 calc R . . H30B H 1.3351 0.4198 0.34 0.14 Uiso 1 1 calc R . . P3 P 1.1533(3) 0.43474(11) 0.3791(2) 0.1148(11) Uani 1 1 d . . . C311 C 1.0606(9) 0.4684(4) 0.3201(7) 0.131(6) Uani 1 1 d D . . C312 C 1.0880(14) 0.4962(4) 0.2537(10) 0.286(17) Uani 1 1 d D . . H312 H 1.1621 0.4947 0.2385 0.343 Uiso 1 1 calc R . . C313 C 1.0137(16) 0.5245(5) 0.2116(10) 0.259(15) Uani 1 1 d D . . H313 H 1.0402 0.5423 0.1702 0.311 Uiso 1 1 calc R . . C314 C 0.9015(14) 0.5292(4) 0.2247(12) 0.198(9) Uani 1 1 d D . . H314 H 0.8485 0.5473 0.1906 0.238 Uiso 1 1 calc R . . C315 C 0.8738(10) 0.5040(4) 0.2947(9) 0.130(5) Uani 1 1 d D . . H315 H 0.8022 0.5072 0.3136 0.156 Uiso 1 1 calc R . . C316 C 0.9490(11) 0.4757(4) 0.3342(8) 0.130(5) Uani 1 1 d D . . H316 H 0.9229 0.4586 0.3769 0.156 Uiso 1 1 calc R . . C321 C 1.2464(11) 0.4666(4) 0.4643(8) 0.120(4) Uani 1 1 d D . . C322 C 1.3409(14) 0.4474(5) 0.5152(9) 0.197(10) Uani 1 1 d D . . H322 H 1.3564 0.419 0.5077 0.237 Uiso 1 1 calc R . . C323 C 1.4123(14) 0.4716(6) 0.5779(10) 0.227(11) Uani 1 1 d D . . H323 H 1.479 0.4598 0.6114 0.272 Uiso 1 1 calc R . . C324 C 1.3854(15) 0.5130(5) 0.5911(11) 0.189(10) Uani 1 1 d D . . H324 H 1.4271 0.5281 0.639 0.227 Uiso 1 1 calc R . . C325 C 1.2999(16) 0.5314(5) 0.5350(15) 0.249(14) Uani 1 1 d D . . H325 H 1.2913 0.5606 0.5358 0.298 Uiso 1 1 calc R . . C326 C 1.2244(12) 0.5075(5) 0.4763(12) 0.197(9) Uani 1 1 d D . . H326 H 1.1571 0.5197 0.4443 0.236 Uiso 1 1 calc R . . C101 C 0.7572(13) 0.2532(3) 0.0723(16) 0.148(7) Uani 1 1 d . . . H101 H 0.6872 0.2451 0.0891 0.178 Uiso 1 1 calc R . . C102 C 0.7753(13) 0.2642(4) -0.0116(12) 0.126(5) Uani 1 1 d . . . H102 H 0.7188 0.266 -0.0633 0.151 Uiso 1 1 calc R . . C103 C 0.8812(14) 0.2714(3) -0.0068(8) 0.109(4) Uani 1 1 d . . . H103 H 0.9149 0.2784 -0.0566 0.131 Uiso 1 1 calc R . . C104 C 0.9419(10) 0.2680(4) 0.0765(10) 0.112(4) Uani 1 1 d . . . H104 H 1.0213 0.2727 0.0952 0.134 Uiso 1 1 calc R . . C105 C 0.8633(16) 0.2566(3) 0.1268(9) 0.124(5) Uani 1 1 d . . . H105 H 0.8782 0.2518 0.1888 0.148 Uiso 1 1 calc R . . C201 C 0.9681(18) 0.3493(7) 0.4977(9) 0.159(8) Uani 1 1 d . . . H201 H 0.9136 0.3289 0.475 0.191 Uiso 1 1 calc R . . C202 C 1.0815(17) 0.3399(5) 0.5324(8) 0.135(5) Uani 1 1 d . . . H202 H 1.117 0.3135 0.5372 0.162 Uiso 1 1 calc R . . C203 C 1.1326(17) 0.3793(5) 0.5592(9) 0.141(6) Uani 1 1 d . . . H203 H 1.2097 0.3845 0.5851 0.169 Uiso 1 1 calc R . . C204 C 1.0448(13) 0.4083(5) 0.5390(7) 0.112(4) Uani 1 1 d . . . H204 H 1.0545 0.437 0.5513 0.134 Uiso 1 1 calc R . . C205 C 0.9419(13) 0.3910(6) 0.4993(8) 0.130(5) Uani 1 1 d . . . H205 H 0.8714 0.4044 0.4784 0.156 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 0.0745(4) 0.0734(4) 0.0726(4) -0.0041(3) 0.0295(3) -0.0024(3) Fe2 0.1331(15) 0.1227(14) 0.0712(10) -0.0258(9) 0.0517(10) -0.0527(11) C1 0.084(7) 0.086(7) 0.128(9) 0.003(7) 0.048(6) 0.001(5) C11 0.064(6) 0.090(7) 0.165(11) -0.015(7) 0.037(6) -0.008(5) N11 0.080(7) 0.117(8) 0.214(12) -0.003(8) 0.037(7) -0.031(6) C12 0.095(8) 0.079(7) 0.173(14) -0.006(8) 0.065(9) -0.023(6) N12 0.117(8) 0.118(9) 0.174(12) 0.037(8) 0.057(8) -0.009(6) C2 0.098(7) 0.067(6) 0.105(8) -0.017(5) 0.041(6) -0.006(5) C21 0.079(6) 0.094(7) 0.112(8) -0.028(6) 0.033(6) -0.017(5) C22 0.085(8) 0.145(11) 0.150(12) -0.075(10) 0.037(8) -0.038(7) C23 0.069(7) 0.26(2) 0.138(13) -0.126(15) 0.013(8) -0.032(10) C24 0.119(12) 0.26(2) 0.091(10) -0.049(13) 0.036(8) -0.069(14) C25 0.103(9) 0.160(13) 0.115(10) -0.007(9) 0.029(8) -0.034(8) C26 0.094(7) 0.100(8) 0.087(7) -0.007(6) 0.027(6) -0.020(6) C3 0.075(6) 0.073(6) 0.098(7) 0.001(5) 0.036(5) -0.006(4) C4 0.085(7) 0.094(7) 0.107(8) -0.007(6) 0.046(6) -0.015(5) C41 0.091(8) 0.121(9) 0.152(11) -0.036(8) 0.064(8) -0.019(7) N41 0.108(8) 0.138(9) 0.199(12) -0.056(8) 0.078(8) 0.002(6) C51 0.076(6) 0.088(6) 0.097(7) -0.017(5) 0.038(5) -0.007(5) N52 0.075(5) 0.092(5) 0.073(5) 0.000(4) 0.041(4) -0.006(4) N53 0.092(6) 0.084(5) 0.071(5) 0.000(4) 0.036(4) -0.013(4) N54 0.097(6) 0.092(5) 0.085(5) -0.021(4) 0.048(5) -0.024(4) N55 0.104(6) 0.098(6) 0.114(7) -0.036(5) 0.066(5) -0.032(5) P1 0.0681(13) 0.0740(13) 0.0804(15) 0.0004(11) 0.0294(11) 0.0005(10) C111 0.077(6) 0.084(6) 0.069(5) 0.018(4) 0.000(5) 0.000(4) C112 0.081(6) 0.102(7) 0.086(7) -0.004(5) 0.022(5) -0.015(5) C113 0.123(10) 0.144(11) 0.068(7) 0.003(6) 0.002(6) -0.030(8) C114 0.116(9) 0.139(10) 0.069(6) 0.005(6) 0.012(6) -0.025(8) C115 0.106(8) 0.129(9) 0.077(7) 0.013(6) 0.025(6) -0.012(7) C116 0.082(6) 0.120(8) 0.066(6) 0.024(5) 0.015(5) -0.013(5) C121 0.057(5) 0.079(6) 0.161(11) 0.025(7) 0.051(6) 0.012(4) C122 0.072(6) 0.096(8) 0.198(14) 0.037(9) 0.036(8) 0.005(5) C123 0.083(8) 0.102(10) 0.27(2) 0.079(12) 0.037(11) 0.017(7) C124 0.066(9) 0.100(11) 0.35(3) -0.012(15) 0.079(14) -0.002(7) C125 0.083(9) 0.082(9) 0.29(2) -0.034(11) 0.068(12) -0.012(6) C126 0.087(7) 0.077(6) 0.170(11) -0.009(7) 0.073(7) -0.003(5) C131 0.072(5) 0.073(5) 0.068(5) -0.001(4) 0.036(4) -0.003(4) C132 0.086(7) 0.088(7) 0.242(17) -0.028(9) 0.080(9) -0.018(6) C133 0.098(9) 0.087(8) 0.31(2) -0.036(11) 0.094(11) -0.008(6) C134 0.085(7) 0.088(7) 0.130(9) -0.002(6) 0.037(6) -0.011(5) C135 0.078(6) 0.090(7) 0.091(7) 0.011(5) 0.021(5) 0.009(5) C136 0.085(7) 0.074(6) 0.081(6) 0.000(4) 0.011(5) -0.001(4) P2 0.0933(18) 0.129(2) 0.0595(14) 0.0109(14) 0.0101(13) -0.0281(16) C211 0.093(7) 0.105(7) 0.068(6) 0.028(5) 0.010(5) -0.014(6) C212 0.151(12) 0.125(11) 0.193(15) -0.006(10) 0.109(12) 0.002(9) C213 0.161(13) 0.096(10) 0.26(2) -0.010(11) 0.124(14) 0.021(9) C214 0.114(10) 0.093(8) 0.143(12) 0.027(8) -0.007(8) -0.006(7) C215 0.30(2) 0.142(14) 0.138(13) -0.051(11) 0.119(15) -0.089(15) C216 0.229(19) 0.193(17) 0.099(10) -0.017(10) 0.073(11) -0.096(14) C221 0.108(9) 0.166(12) 0.079(7) 0.037(7) -0.022(6) -0.043(8) C222 0.067(9) 0.58(5) 0.129(14) 0.09(2) -0.005(9) -0.015(16) C223 0.115(15) 0.47(5) 0.23(3) 0.14(3) -0.017(16) -0.02(2) C224 0.30(3) 0.133(13) 0.166(18) -0.021(12) -0.14(2) 0.045(15) C225 0.25(3) 0.70(7) 0.119(17) 0.15(3) -0.002(19) 0.15(4) C226 0.154(14) 0.216(18) 0.081(8) 0.039(9) -0.001(9) 0.024(12) C20 0.078(6) 0.102(7) 0.063(5) 0.009(5) 0.028(4) -0.007(5) C30 0.113(9) 0.122(10) 0.128(10) -0.002(8) 0.062(8) -0.020(7) P3 0.146(3) 0.102(2) 0.114(2) -0.0242(18) 0.073(2) -0.033(2) C311 0.099(9) 0.214(16) 0.096(8) -0.059(9) 0.058(7) -0.067(9) C312 0.43(4) 0.126(14) 0.39(3) 0.110(18) 0.33(3) 0.110(19) C313 0.39(4) 0.19(2) 0.25(2) 0.112(18) 0.23(3) 0.15(2) C314 0.24(2) 0.071(9) 0.31(3) -0.007(13) 0.11(2) 0.007(11) C315 0.127(11) 0.112(10) 0.164(13) -0.038(9) 0.065(10) -0.027(8) C316 0.153(13) 0.107(10) 0.131(11) -0.031(8) 0.022(10) -0.024(9) C321 0.126(11) 0.138(12) 0.103(9) -0.012(8) 0.041(8) -0.038(8) C322 0.23(2) 0.25(2) 0.107(12) 0.003(14) 0.006(13) -0.122(19) C323 0.33(3) 0.18(2) 0.148(16) -0.024(15) -0.013(19) -0.04(2) C324 0.23(2) 0.166(18) 0.193(19) -0.090(15) 0.097(18) -0.089(17) C325 0.153(19) 0.21(2) 0.35(4) -0.10(2) -0.06(2) -0.028(16) C326 0.126(13) 0.154(16) 0.32(3) -0.107(17) 0.055(15) -0.015(11) C101 0.119(11) 0.065(7) 0.29(2) -0.025(10) 0.119(14) -0.032(6) C102 0.091(9) 0.104(9) 0.171(14) -0.040(10) -0.011(9) 0.026(7) C103 0.173(13) 0.081(7) 0.090(8) 0.015(6) 0.072(9) 0.053(8) C104 0.088(8) 0.087(7) 0.156(12) 0.005(8) 0.004(8) 0.001(6) C105 0.205(16) 0.079(7) 0.099(9) 0.001(6) 0.059(10) -0.015(9) C201 0.189(17) 0.23(2) 0.073(8) -0.038(11) 0.075(10) -0.111(17) C202 0.194(17) 0.150(13) 0.074(8) -0.002(8) 0.064(10) -0.048(12) C203 0.199(17) 0.158(14) 0.082(8) -0.015(9) 0.069(10) -0.052(13) C204 0.149(12) 0.127(11) 0.067(7) -0.023(7) 0.040(7) -0.041(9) C205 0.144(12) 0.178(15) 0.082(8) -0.033(9) 0.060(8) -0.066(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.055(9) . ? Ru1 N52 2.057(8) . ? Ru1 C105 2.155(12) . ? Ru1 C102 2.167(12) . ? Ru1 C103 2.168(9) . ? Ru1 C101 2.177(10) . ? Ru1 C104 2.185(12) . ? Ru1 P1 2.301(2) . ? Fe2 N54 2.008(9) . ? Fe2 C204 2.060(11) . ? Fe2 C201 2.066(13) . ? Fe2 C203 2.073(15) . ? Fe2 C202 2.096(14) . ? Fe2 C205 2.111(13) . ? Fe2 P3 2.187(3) . ? Fe2 P2 2.220(4) . ? C1 C2 1.388(14) . ? C1 C12 1.415(18) . ? C1 C11 1.433(16) . ? C11 N11 1.120(13) . ? C12 N12 1.169(17) . ? C2 C3 1.461(14) . ? C2 C21 1.490(16) . ? C21 C26 1.362(15) . ? C21 C22 1.382(15) . ? C22 C23 1.39(2) . ? C22 H22 0.95 . ? C23 C24 1.36(2) . ? C23 H23 0.95 . ? C24 C25 1.344(19) . ? C24 H24 0.95 . ? C25 C26 1.374(16) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.357(14) . ? C4 C41 1.415(15) . ? C4 C51 1.425(14) . ? C41 N41 1.187(14) . ? C51 N55 1.329(13) . ? C51 N52 1.352(11) . ? N52 N53 1.330(11) . ? N53 N54 1.328(10) . ? N54 N55 1.366(12) . ? P1 C111 1.809(10) . ? P1 C131 1.823(9) . ? P1 C121 1.832(9) . ? C111 C116 1.390(13) . ? C111 C112 1.400(13) . ? C112 C113 1.390(14) . ? C112 H112 0.95 . ? C113 C114 1.346(16) . ? C113 H113 0.95 . ? C114 C115 1.379(15) . ? C114 H114 0.95 . ? C115 C116 1.400(13) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.393(16) . ? C121 C122 1.396(17) . ? C122 C123 1.422(17) . ? C122 H122 0.95 . ? C123 C124 1.38(3) . ? C123 H123 0.95 . ? C124 C125 1.34(2) . ? C124 H124 0.95 . ? C125 C126 1.406(16) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.373(13) . ? C131 C136 1.394(12) . ? C132 C133 1.421(16) . ? C132 H132 0.95 . ? C133 C134 1.368(15) . ? C133 H133 0.95 . ? C134 C135 1.372(13) . ? C134 H134 0.95 . ? C135 C136 1.372(13) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C211 1.831(10) . ? P2 C221 1.846(10) . ? P2 C20 1.849(8) . ? C211 C216 1.361(12) . ? C211 C212 1.390(12) . ? C212 C213 1.384(13) . ? C212 H212 0.95 . ? C213 C214 1.352(12) . ? C213 H213 0.95 . ? C214 C215 1.385(13) . ? C214 H214 0.95 . ? C215 C216 1.393(13) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C226 1.365(12) . ? C221 C222 1.395(13) . ? C222 C223 1.380(14) . ? C222 H222 0.95 . ? C223 C224 1.379(14) . ? C223 H223 0.95 . ? C224 C225 1.393(16) . ? C224 H224 0.95 . ? C225 C226 1.401(15) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C20 C30 1.434(14) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C30 P3 1.870(11) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? P3 C311 1.699(13) . ? P3 C321 1.874(12) . ? C311 C316 1.400(12) . ? C311 C312 1.438(13) . ? C312 C313 1.358(14) . ? C312 H312 0.95 . ? C313 C314 1.392(15) . ? C313 H313 0.95 . ? C314 C315 1.431(14) . ? C314 H314 0.95 . ? C315 C316 1.350(13) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 C326 1.370(13) . ? C321 C322 1.40(2) . ? C322 C323 1.41(2) . ? C322 H322 0.95 . ? C323 C324 1.40(3) . ? C323 H323 0.95 . ? C324 C325 1.35(3) . ? C324 H324 0.95 . ? C325 C326 1.39(2) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C101 C102 1.39(2) . ? C101 C105 1.40(2) . ? C101 H101 0.95 . ? C102 C103 1.270(18) . ? C102 H102 0.95 . ? C103 C104 1.361(16) . ? C103 H103 0.95 . ? C104 C105 1.361(17) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C201 C205 1.39(2) . ? C201 C202 1.40(2) . ? C201 H201 0.95 . ? C202 C203 1.446(19) . ? C202 H202 0.95 . ? C203 C204 1.40(2) . ? C203 H203 0.95 . ? C204 C205 1.388(17) . ? C204 H204 0.95 . ? C205 H205 0.95 . ? 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 C3 Ru1 N52 75.7(3) . . ? C3 Ru1 C105 115.2(5) . . ? N52 Ru1 C105 96.9(4) . . ? C3 Ru1 C102 110.8(5) . . ? N52 Ru1 C102 158.6(5) . . ? C105 Ru1 C102 61.8(5) . . ? C3 Ru1 C103 144.7(5) . . ? N52 Ru1 C103 137.6(5) . . ? C105 Ru1 C103 59.7(4) . . ? C102 Ru1 C103 34.1(5) . . ? C3 Ru1 C101 94.8(4) . . ? N52 Ru1 C101 124.1(7) . . ? C105 Ru1 C101 37.6(6) . . ? C102 Ru1 C101 37.3(6) . . ? C103 Ru1 C101 59.1(5) . . ? C3 Ru1 C104 151.7(5) . . ? N52 Ru1 C104 103.3(4) . . ? C105 Ru1 C104 36.6(5) . . ? C102 Ru1 C104 60.9(4) . . ? C103 Ru1 C104 36.4(4) . . ? C101 Ru1 C104 61.8(5) . . ? C3 Ru1 P1 96.7(3) . . ? N52 Ru1 P1 90.1(2) . . ? C105 Ru1 P1 148.1(4) . . ? C102 Ru1 P1 108.7(5) . . ? C103 Ru1 P1 94.8(3) . . ? C101 Ru1 P1 145.7(6) . . ? C104 Ru1 P1 111.6(4) . . ? N54 Fe2 C204 124.9(5) . . ? N54 Fe2 C201 91.1(6) . . ? C204 Fe2 C201 63.4(6) . . ? N54 Fe2 C203 155.8(5) . . ? C204 Fe2 C203 39.6(5) . . ? C201 Fe2 C203 65.7(6) . . ? N54 Fe2 C202 122.9(6) . . ? C204 Fe2 C202 66.1(6) . . ? C201 Fe2 C202 39.2(6) . . ? C203 Fe2 C202 40.6(5) . . ? N54 Fe2 C205 90.3(5) . . ? C204 Fe2 C205 38.9(5) . . ? C201 Fe2 C205 38.9(6) . . ? C203 Fe2 C205 67.6(7) . . ? C202 Fe2 C205 67.6(7) . . ? N54 Fe2 P3 95.1(3) . . ? C204 Fe2 P3 93.0(4) . . ? C201 Fe2 P3 154.3(6) . . ? C203 Fe2 P3 103.2(4) . . ? C202 Fe2 P3 142.0(5) . . ? C205 Fe2 P3 116.1(5) . . ? N54 Fe2 P2 92.2(2) . . ? C204 Fe2 P2 142.9(5) . . ? C201 Fe2 P2 121.1(7) . . ? C203 Fe2 P2 105.2(6) . . ? C202 Fe2 P2 94.5(5) . . ? C205 Fe2 P2 159.9(5) . . ? P3 Fe2 P2 83.57(13) . . ? C2 C1 C12 122.2(11) . . ? C2 C1 C11 123.5(12) . . ? C12 C1 C11 114.3(10) . . ? N11 C11 C1 172.5(15) . . ? N12 C12 C1 178.3(14) . . ? C1 C2 C3 119.4(11) . . ? C1 C2 C21 117.6(10) . . ? C3 C2 C21 123.0(9) . . ? C26 C21 C22 117.6(13) . . ? C26 C21 C2 119.7(9) . . ? C22 C21 C2 122.7(12) . . ? C21 C22 C23 122.8(15) . . ? C21 C22 H22 118.6 . . ? C23 C22 H22 118.6 . . ? C24 C23 C22 115.4(13) . . ? C24 C23 H23 122.3 . . ? C22 C23 H23 122.3 . . ? C25 C24 C23 124.7(18) . . ? C25 C24 H24 117.7 . . ? C23 C24 H24 117.7 . . ? C24 C25 C26 118.1(16) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C21 C26 C25 121.4(12) . . ? C21 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C4 C3 C2 122.1(9) . . ? C4 C3 Ru1 118.4(7) . . ? C2 C3 Ru1 119.2(7) . . ? C3 C4 C41 122.6(11) . . ? C3 C4 C51 113.4(9) . . ? C41 C4 C51 124.0(10) . . ? N41 C41 C4 177.6(13) . . ? N55 C51 N52 111.7(9) . . ? N55 C51 C4 133.6(9) . . ? N52 C51 C4 114.5(9) . . ? N53 N52 C51 105.7(8) . . ? N53 N52 Ru1 135.8(6) . . ? C51 N52 Ru1 117.9(7) . . ? N54 N53 N52 108.8(8) . . ? N53 N54 N55 109.7(8) . . ? N53 N54 Fe2 124.0(7) . . ? N55 N54 Fe2 125.2(6) . . ? C51 N55 N54 104.1(7) . . ? C111 P1 C131 101.1(4) . . ? C111 P1 C121 100.4(5) . . ? C131 P1 C121 101.8(4) . . ? C111 P1 Ru1 114.7(3) . . ? C131 P1 Ru1 114.4(3) . . ? C121 P1 Ru1 121.5(3) . . ? C116 C111 C112 116.0(9) . . ? C116 C111 P1 124.4(7) . . ? C112 C111 P1 119.6(7) . . ? C113 C112 C111 122.3(10) . . ? C113 C112 H112 118.9 . . ? C111 C112 H112 118.9 . . ? C114 C113 C112 119.9(11) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C113 C114 C115 120.7(11) . . ? C113 C114 H114 119.7 . . ? C115 C114 H114 119.7 . . ? C114 C115 C116 119.4(10) . . ? C114 C115 H115 120.3 . . ? C116 C115 H115 120.3 . . ? C111 C116 C115 121.7(10) . . ? C111 C116 H116 119.1 . . ? C115 C116 H116 119.1 . . ? C126 C121 C122 118.8(10) . . ? C126 C121 P1 118.4(9) . . ? C122 C121 P1 122.8(10) . . ? C121 C122 C123 120.4(15) . . ? C121 C122 H122 119.8 . . ? C123 C122 H122 119.8 . . ? C124 C123 C122 118.0(17) . . ? C124 C123 H123 121 . . ? C122 C123 H123 121 . . ? C125 C124 C123 122.7(16) . . ? C125 C124 H124 118.7 . . ? C123 C124 H124 118.7 . . ? C124 C125 C126 120.0(18) . . ? C124 C125 H125 120 . . ? C126 C125 H125 120 . . ? C121 C126 C125 120.1(15) . . ? C121 C126 H126 120 . . ? C125 C126 H126 120 . . ? C132 C131 C136 116.8(9) . . ? C132 C131 P1 124.0(7) . . ? C136 C131 P1 119.1(7) . . ? C131 C132 C133 120.5(11) . . ? C131 C132 H132 119.7 . . ? C133 C132 H132 119.7 . . ? C134 C133 C132 121.0(11) . . ? C134 C133 H133 119.5 . . ? C132 C133 H133 119.5 . . ? C133 C134 C135 118.1(10) . . ? C133 C134 H134 120.9 . . ? C135 C134 H134 120.9 . . ? C134 C135 C136 121.1(9) . . ? C134 C135 H135 119.5 . . ? C136 C135 H135 119.5 . . ? C135 C136 C131 122.3(9) . . ? C135 C136 H136 118.9 . . ? C131 C136 H136 118.9 . . ? C211 P2 C221 100.1(5) . . ? C211 P2 C20 106.5(4) . . ? C221 P2 C20 100.4(5) . . ? C211 P2 Fe2 121.3(3) . . ? C221 P2 Fe2 119.8(4) . . ? C20 P2 Fe2 106.4(3) . . ? C216 C211 C212 117.7(9) . . ? C216 C211 P2 121.4(8) . . ? C212 C211 P2 120.9(7) . . ? C213 C212 C211 121.0(10) . . ? C213 C212 H212 119.5 . . ? C211 C212 H212 119.5 . . ? C214 C213 C212 120.4(10) . . ? C214 C213 H213 119.8 . . ? C212 C213 H213 119.8 . . ? C213 C214 C215 119.5(10) . . ? C213 C214 H214 120.3 . . ? C215 C214 H214 120.3 . . ? C214 C215 C216 119.3(10) . . ? C214 C215 H215 120.4 . . ? C216 C215 H215 120.4 . . ? C211 C216 C215 121.7(10) . . ? C211 C216 H216 119.2 . . ? C215 C216 H216 119.2 . . ? C226 C221 C222 118.9(10) . . ? C226 C221 P2 118.2(9) . . ? C222 C221 P2 122.7(8) . . ? C223 C222 C221 120.5(11) . . ? C223 C222 H222 119.7 . . ? C221 C222 H222 119.7 . . ? C224 C223 C222 120.1(12) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 119.9(12) . . ? C223 C224 H224 120.1 . . ? C225 C224 H224 120.1 . . ? C224 C225 C226 118.7(12) . . ? C224 C225 H225 120.7 . . ? C226 C225 H225 120.7 . . ? C221 C226 C225 120.8(11) . . ? C221 C226 H226 119.6 . . ? C225 C226 H226 119.6 . . ? C30 C20 P2 106.2(7) . . ? C30 C20 H20A 110.5 . . ? P2 C20 H20A 110.5 . . ? C30 C20 H20B 110.5 . . ? P2 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? C20 C30 P3 110.9(7) . . ? C20 C30 H30A 109.5 . . ? P3 C30 H30A 109.5 . . ? C20 C30 H30B 109.5 . . ? P3 C30 H30B 109.5 . . ? H30A C30 H30B 108 . . ? C311 P3 C30 106.6(6) . . ? C311 P3 C321 105.7(6) . . ? C30 P3 C321 101.4(6) . . ? C311 P3 Fe2 114.2(4) . . ? C30 P3 Fe2 110.0(4) . . ? C321 P3 Fe2 117.7(4) . . ? C316 C311 C312 109.8(10) . . ? C316 C311 P3 124.9(9) . . ? C312 C311 P3 125.1(9) . . ? C313 C312 C311 123.5(11) . . ? C313 C312 H312 118.2 . . ? C311 C312 H312 118.2 . . ? C312 C313 C314 124.5(12) . . ? C312 C313 H313 117.7 . . ? C314 C313 H313 117.7 . . ? C313 C314 C315 113.3(11) . . ? C313 C314 H314 123.4 . . ? C315 C314 H314 123.4 . . ? C316 C315 C314 120.3(11) . . ? C316 C315 H315 119.9 . . ? C314 C315 H315 119.9 . . ? C315 C316 C311 128.2(11) . . ? C315 C316 H316 115.9 . . ? C311 C316 H316 115.9 . . ? C326 C321 C322 120.6(10) . . ? C326 C321 P3 121.5(11) . . ? C322 C321 P3 117.9(10) . . ? C321 C322 C323 117.8(12) . . ? C321 C322 H322 121.1 . . ? C323 C322 H322 121.1 . . ? C324 C323 C322 120.4(12) . . ? C324 C323 H323 119.8 . . ? C322 C323 H323 119.8 . . ? C325 C324 C323 119.6(12) . . ? C325 C324 H324 120.2 . . ? C323 C324 H324 120.2 . . ? C324 C325 C326 119.9(13) . . ? C324 C325 H325 120.1 . . ? C326 C325 H325 120.1 . . ? C321 C326 C325 120.5(12) . . ? C321 C326 H326 119.8 . . ? C325 C326 H326 119.8 . . ? C102 C101 C105 105.7(11) . . ? C102 C101 Ru1 71.0(7) . . ? C105 C101 Ru1 70.3(7) . . ? C102 C101 H101 127.2 . . ? C105 C101 H101 127.2 . . ? Ru1 C101 H101 123.3 . . ? C103 C102 C101 107.5(13) . . ? C103 C102 Ru1 73.0(7) . . ? C101 C102 Ru1 71.8(8) . . ? C103 C102 H102 126.3 . . ? C101 C102 H102 126.3 . . ? Ru1 C102 H102 120.7 . . ? C102 C103 C104 113.8(13) . . ? C102 C103 Ru1 72.9(7) . . ? C104 C103 Ru1 72.5(7) . . ? C102 C103 H103 123.1 . . ? C104 C103 H103 123.1 . . ? Ru1 C103 H103 123 . . ? C103 C104 C105 104.3(12) . . ? C103 C104 Ru1 71.1(6) . . ? C105 C104 Ru1 70.5(8) . . ? C103 C104 H104 127.8 . . ? C105 C104 H104 127.8 . . ? Ru1 C104 H104 122.5 . . ? C104 C105 C101 108.6(13) . . ? C104 C105 Ru1 73.0(7) . . ? C101 C105 Ru1 72.1(8) . . ? C104 C105 H105 125.7 . . ? C101 C105 H105 125.7 . . ? Ru1 C105 H105 121 . . ? C205 C201 C202 114.3(15) . . ? C205 C201 Fe2 72.3(8) . . ? C202 C201 Fe2 71.6(8) . . ? C205 C201 H201 122.9 . . ? C202 C201 H201 122.9 . . ? Fe2 C201 H201 124.8 . . ? C201 C202 C203 104.3(17) . . ? C201 C202 Fe2 69.2(9) . . ? C203 C202 Fe2 68.8(8) . . ? C201 C202 H202 127.8 . . ? C203 C202 H202 127.8 . . ? Fe2 C202 H202 125.7 . . ? C204 C203 C202 105.6(17) . . ? C204 C203 Fe2 69.7(9) . . ? C202 C203 Fe2 70.6(8) . . ? C204 C203 H203 127.2 . . ? C202 C203 H203 127.2 . . ? Fe2 C203 H203 124.2 . . ? C205 C204 C203 113.3(15) . . ? C205 C204 Fe2 72.6(7) . . ? C203 C204 Fe2 70.7(8) . . ? C205 C204 H204 123.4 . . ? C203 C204 H204 123.4 . . ? Fe2 C204 H204 125 . . ? C204 C205 C201 102.5(16) . . ? C204 C205 Fe2 68.6(7) . . ? C201 C205 Fe2 68.8(8) . . ? C204 C205 H205 128.7 . . ? C201 C205 H205 128.7 . . ? Fe2 C205 H205 125.5 . . ? 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 1 0.191 0.712 0.668 16.3 0.1 2 0.191 0.788 0.168 16.3 0.1 3 0.338 0.575 0.325 33.3 1.5 4 0.338 0.925 0.825 33.3 1.4 5 0.662 0.075 0.175 33.3 1.7 6 0.662 0.425 0.675 33.3 1.5 7 0.808 0.212 0.832 16.3 0.3 8 0.808 0.288 0.332 16.3 0.1 #===END # Attachment '8.br1399.cif' data_br1399 _database_code_depnum_ccdc_archive 'CCDC 730746' _audit_creation_date 2008-02-07T10:25:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41.30 H35.20 N7 O2.30 P Ru' _chemical_formula_moiety 'C41 H34 N7 O2 P Ru, 0.3(C H4 O)' _chemical_formula_weight 798.4 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -P_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5756(4) _cell_length_b 13.0641(6) _cell_length_c 13.7818(5) _cell_angle_alpha 64.569(4) _cell_angle_beta 69.109(3) _cell_angle_gamma 66.706(4) _cell_volume 1829.90(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14176 _cell_measurement_theta_min 2.8383 _cell_measurement_theta_max 36.129 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 819 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.52 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_absorpt_correction_T_min 0.851 _exptl_absorpt_correction_T_max 0.988 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 0.0145926118 _diffrn_orient_matrix_ub_12 -0.0492216047 _diffrn_orient_matrix_ub_13 -0.0165954707 _diffrn_orient_matrix_ub_21 0.0432697025 _diffrn_orient_matrix_ub_22 0.0223520654 _diffrn_orient_matrix_ub_23 -0.0458861319 _diffrn_orient_matrix_ub_31 0.043443689 _diffrn_orient_matrix_ub_32 -0.031875102 _diffrn_orient_matrix_ub_33 0.0321718211 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.1055 _diffrn_reflns_number 40379 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 36.23 _diffrn_reflns_theta_full 35 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 16687 _reflns_number_gt 10462 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.0000P] 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_number_reflns 16687 _refine_ls_number_parameters 489 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.107 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.505 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.299303(13) 0.257268(14) 0.107466(13) 0.01694(5) Uani 1 1 d . . . P1 P 0.17120(4) 0.16220(5) 0.25702(4) 0.01719(10) Uani 1 1 d . . . C111 C 0.18850(18) 0.01428(19) 0.26290(18) 0.0232(4) Uani 1 1 d . . . C112 C 0.29920(19) -0.06894(19) 0.26530(18) 0.0246(4) Uani 1 1 d . . . H112 H 0.3636 -0.0478 0.2648 0.03 Uiso 1 1 calc R . . C113 C 0.3180(2) -0.1819(2) 0.2684(2) 0.0333(5) Uani 1 1 d . . . H113 H 0.3942 -0.2379 0.2711 0.04 Uiso 1 1 calc R . . C114 C 0.2258(3) -0.2128(3) 0.2675(3) 0.0527(8) Uani 1 1 d . . . H114 H 0.2382 -0.2901 0.2693 0.063 Uiso 1 1 calc R . . C115 C 0.1142(3) -0.1303(3) 0.2639(4) 0.0688(12) Uani 1 1 d . . . H115 H 0.0507 -0.1515 0.2626 0.083 Uiso 1 1 calc R . . C116 C 0.0952(2) -0.0179(3) 0.2622(3) 0.0447(7) Uani 1 1 d . . . H116 H 0.0186 0.0376 0.2605 0.054 Uiso 1 1 calc R . . C121 C 0.17219(16) 0.14157(18) 0.39663(16) 0.0184(4) Uani 1 1 d . . . C122 C 0.20345(17) 0.03134(19) 0.47655(17) 0.0226(4) Uani 1 1 d . . . H122 H 0.22 -0.0387 0.4616 0.027 Uiso 1 1 calc R . . C123 C 0.21058(19) 0.0234(2) 0.57843(18) 0.0272(4) Uani 1 1 d . . . H123 H 0.2318 -0.0521 0.6326 0.033 Uiso 1 1 calc R . . C124 C 0.1872(2) 0.1239(2) 0.60101(18) 0.0287(5) Uani 1 1 d . . . H124 H 0.1952 0.1179 0.6694 0.034 Uiso 1 1 calc R . . C125 C 0.1518(2) 0.2342(2) 0.52337(18) 0.0291(5) Uani 1 1 d . . . H125 H 0.133 0.3039 0.5396 0.035 Uiso 1 1 calc R . . C126 C 0.14389(19) 0.2429(2) 0.42240(17) 0.0240(4) Uani 1 1 d . . . H126 H 0.1189 0.3187 0.37 0.029 Uiso 1 1 calc R . . C131 C 0.01297(16) 0.23794(18) 0.25677(17) 0.0211(4) Uani 1 1 d . . . C132 C -0.07458(17) 0.2205(2) 0.35426(19) 0.0266(4) Uani 1 1 d . . . H132 H -0.0525 0.1718 0.4227 0.032 Uiso 1 1 calc R . . C133 C -0.19398(19) 0.2742(2) 0.3515(2) 0.0336(5) Uani 1 1 d . . . H133 H -0.2531 0.2632 0.4182 0.04 Uiso 1 1 calc R . . C134 C -0.22723(19) 0.3436(2) 0.2518(2) 0.0328(5) Uani 1 1 d . . . H134 H -0.3089 0.3791 0.2501 0.039 Uiso 1 1 calc R . . C135 C -0.14139(19) 0.3610(2) 0.1554(2) 0.0306(5) Uani 1 1 d . . . H135 H -0.1639 0.4085 0.087 0.037 Uiso 1 1 calc R . . C136 C -0.02154(18) 0.3091(2) 0.15794(18) 0.0248(4) Uani 1 1 d . . . H136 H 0.0372 0.3227 0.0912 0.03 Uiso 1 1 calc R . . C1 C 0.62283(17) 0.2045(2) 0.13801(17) 0.0235(4) Uani 1 1 d . . . C11 C 0.74022(18) 0.1220(2) 0.13720(18) 0.0302(5) Uani 1 1 d . . . N11 N 0.83509(17) 0.0602(2) 0.13531(19) 0.0436(6) Uani 1 1 d . . . C12 C 0.62264(18) 0.3248(2) 0.07156(19) 0.0288(5) Uani 1 1 d . . . N12 N 0.63165(19) 0.4169(2) 0.01762(19) 0.0417(5) Uani 1 1 d . . . C2 C 0.52234(16) 0.17032(19) 0.19712(15) 0.0190(4) Uani 1 1 d . . . C21 C 0.53422(16) 0.04269(19) 0.25973(16) 0.0200(4) Uani 1 1 d . . . C22 C 0.59702(19) -0.0423(2) 0.20856(18) 0.0263(4) Uani 1 1 d . . . H22 H 0.6324 -0.0189 0.1319 0.032 Uiso 1 1 calc R . . C23 C 0.6082(2) -0.1614(2) 0.2692(2) 0.0311(5) Uani 1 1 d . . . H23 H 0.6493 -0.2191 0.2337 0.037 Uiso 1 1 calc R . . C24 C 0.5591(2) -0.1959(2) 0.3816(2) 0.0292(5) Uani 1 1 d . . . H24 H 0.5689 -0.2775 0.4236 0.035 Uiso 1 1 calc R . . C25 C 0.49561(18) -0.1112(2) 0.43288(18) 0.0246(4) Uani 1 1 d . . . H25 H 0.4622 -0.1351 0.5099 0.03 Uiso 1 1 calc R . . C26 C 0.48086(17) 0.00730(19) 0.37240(16) 0.0208(4) Uani 1 1 d . . . H26 H 0.4344 0.065 0.4072 0.025 Uiso 1 1 calc R . . C3 C 0.40410(15) 0.25565(17) 0.19342(15) 0.0170(3) Uani 1 1 d . . . C4 C 0.36802(16) 0.34655(18) 0.23337(16) 0.0191(4) Uani 1 1 d . . . C41 C 0.42884(17) 0.3628(2) 0.29402(17) 0.0238(4) Uani 1 1 d . . . N41 N 0.47589(18) 0.3753(2) 0.34333(18) 0.0366(5) Uani 1 1 d . . . C51 C 0.25644(16) 0.43016(18) 0.21117(16) 0.0194(4) Uani 1 1 d . . . N52 N 0.20871(14) 0.40677(15) 0.15100(13) 0.0183(3) Uani 1 1 d . . . N53 N 0.10553(15) 0.48894(16) 0.13973(16) 0.0256(4) Uani 1 1 d . . . N54 N 0.09614(16) 0.55697(17) 0.19228(17) 0.0289(4) Uani 1 1 d . A . N55 N 0.18635(16) 0.52431(16) 0.23895(16) 0.0263(4) Uani 1 1 d . . . C01 C 0.0133(4) 0.7997(4) 0.0527(4) 0.0375(10) Uani 0.628(5) 1 d P A 1 H01A H 0.0058 0.8562 0.0854 0.056 Uiso 0.628(5) 1 calc PR A 1 H01B H -0.0141 0.8427 -0.0163 0.056 Uiso 0.628(5) 1 calc PR A 1 H01C H 0.0966 0.7532 0.0375 0.056 Uiso 0.628(5) 1 calc PR A 1 O02 O -0.0575(2) 0.7222(2) 0.1276(2) 0.0325(8) Uani 0.628(5) 1 d P A 1 C03 C -0.0189(2) 0.6474(2) 0.2182(3) 0.0442(7) Uani 1 1 d . . . H03 H -0.0033 0.6941 0.2505 0.053 Uiso 0.628(5) 1 calc PR A 1 H03' H -0.0492 0.671 0.1515 0.053 Uiso 0.372(5) 1 d PR A 2 C04 C -0.1103(2) 0.5851(3) 0.3060(2) 0.0431(7) Uani 1 1 d . A . H04A H -0.1868 0.644 0.3226 0.052 Uiso 1 1 calc R . . H04B H -0.124 0.5328 0.2796 0.052 Uiso 1 1 calc R . . O05 O -0.06439(19) 0.5196(2) 0.39880(19) 0.0537(5) Uani 1 1 d . . . C06 C -0.1458(3) 0.4619(3) 0.4897(3) 0.0628(9) Uani 1 1 d . A . H06A H -0.2239 0.5196 0.4998 0.094 Uiso 1 1 calc R . . H06B H -0.1161 0.4281 0.557 0.094 Uiso 1 1 calc R . . H06C H -0.1527 0.3985 0.4741 0.094 Uiso 1 1 calc R . . C01' C 0.0467(11) 0.8073(12) 0.1059(11) 0.084(4) Uiso 0.372(5) 1 d P A 2 H01D H 0.0371 0.8815 0.1143 0.126 Uiso 0.372(5) 1 calc PR A 2 H01E H 0.0132 0.8248 0.0443 0.126 Uiso 0.372(5) 1 calc PR A 2 H01F H 0.1313 0.7644 0.091 0.126 Uiso 0.372(5) 1 calc PR A 2 O02' O -0.0166(6) 0.7332(7) 0.2091(6) 0.070(2) Uiso 0.372(5) 1 d P A 2 C101 C 0.44931(19) 0.2110(2) -0.02459(17) 0.0295(5) Uani 1 1 d . . . H101 H 0.53 0.1925 -0.0232 0.035 Uiso 1 1 calc R . . C102 C 0.3833(2) 0.1293(2) 0.01946(18) 0.0285(5) Uani 1 1 d . . . H102 H 0.4106 0.0467 0.0565 0.034 Uiso 1 1 calc R . . C103 C 0.2660(2) 0.1948(2) -0.00231(18) 0.0276(4) Uani 1 1 d . . . H103 H 0.2025 0.1625 0.0173 0.033 Uiso 1 1 calc R . . C104 C 0.2626(2) 0.3143(2) -0.05745(17) 0.0270(4) Uani 1 1 d . . . H104 H 0.196 0.3769 -0.0814 0.032 Uiso 1 1 calc R . . C105 C 0.3754(2) 0.3261(2) -0.07149(17) 0.0273(4) Uani 1 1 d . . . H105 H 0.3974 0.3976 -0.1058 0.033 Uiso 1 1 calc R . . O10 O 0.5844(6) 0.5461(7) 0.3657(6) 0.052(2) Uiso 0.298(6) 1 d P . . C10 C 0.5954(10) 0.4858(10) 0.4628(10) 0.054(3) Uiso 0.298(6) 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 0.01707(7) 0.01873(8) 0.01487(7) -0.00605(6) -0.00379(5) -0.00438(5) P1 0.0166(2) 0.0184(2) 0.0177(2) -0.00692(19) -0.00386(17) -0.00526(18) C111 0.0226(9) 0.0250(11) 0.0240(10) -0.0103(8) -0.0024(7) -0.0089(8) C112 0.0302(10) 0.0221(10) 0.0239(10) -0.0093(8) -0.0080(8) -0.0063(8) C113 0.0386(12) 0.0247(12) 0.0334(13) -0.0136(10) -0.0039(10) -0.0055(9) C114 0.0494(16) 0.0384(16) 0.077(2) -0.0380(16) 0.0127(15) -0.0222(13) C115 0.0349(14) 0.060(2) 0.139(4) -0.070(2) 0.0070(18) -0.0238(14) C116 0.0236(10) 0.0438(16) 0.083(2) -0.0435(16) 0.0017(12) -0.0127(10) C121 0.0172(8) 0.0201(9) 0.0178(9) -0.0060(7) -0.0009(6) -0.0082(7) C122 0.0231(9) 0.0237(10) 0.0192(9) -0.0068(8) -0.0033(7) -0.0067(8) C123 0.0256(10) 0.0303(12) 0.0191(10) -0.0038(9) -0.0044(8) -0.0071(9) C124 0.0317(10) 0.0409(14) 0.0182(10) -0.0124(9) -0.0024(8) -0.0151(10) C125 0.0397(12) 0.0316(12) 0.0215(10) -0.0125(9) -0.0008(9) -0.0172(10) C126 0.0315(10) 0.0220(10) 0.0184(9) -0.0053(8) -0.0024(8) -0.0120(8) C131 0.0172(8) 0.0212(10) 0.0274(10) -0.0102(8) -0.0055(7) -0.0052(7) C132 0.0188(8) 0.0266(11) 0.0299(11) -0.0077(9) -0.0033(8) -0.0060(8) C133 0.0188(9) 0.0311(13) 0.0434(14) -0.0084(11) -0.0039(9) -0.0072(9) C134 0.0177(9) 0.0305(12) 0.0474(15) -0.0097(11) -0.0106(9) -0.0048(8) C135 0.0252(10) 0.0311(12) 0.0364(13) -0.0073(10) -0.0132(9) -0.0078(9) C136 0.0214(9) 0.0291(11) 0.0257(10) -0.0082(9) -0.0081(8) -0.0077(8) C1 0.0167(8) 0.0290(11) 0.0184(9) -0.0038(8) -0.0040(7) -0.0048(8) C11 0.0201(9) 0.0403(14) 0.0211(10) -0.0037(10) -0.0041(7) -0.0078(9) N11 0.0216(9) 0.0541(15) 0.0344(12) -0.0072(11) -0.0039(8) -0.0012(9) C12 0.0180(9) 0.0371(13) 0.0259(11) -0.0035(10) -0.0048(7) -0.0105(9) N12 0.0322(10) 0.0467(14) 0.0378(12) 0.0007(11) -0.0068(9) -0.0204(10) C2 0.0173(8) 0.0249(10) 0.0144(8) -0.0072(7) -0.0041(6) -0.0047(7) C21 0.0157(8) 0.0231(10) 0.0201(9) -0.0086(8) -0.0045(7) -0.0025(7) C22 0.0268(10) 0.0268(11) 0.0214(10) -0.0088(9) -0.0088(8) 0.0000(8) C23 0.0321(11) 0.0276(12) 0.0300(12) -0.0145(10) -0.0126(9) 0.0055(9) C24 0.0333(11) 0.0208(11) 0.0315(12) -0.0057(9) -0.0168(9) -0.0007(9) C25 0.0257(9) 0.0291(11) 0.0189(9) -0.0066(8) -0.0069(7) -0.0077(8) C26 0.0194(8) 0.0258(10) 0.0178(9) -0.0084(8) -0.0061(7) -0.0041(7) C3 0.0157(7) 0.0179(9) 0.0142(8) -0.0010(7) -0.0031(6) -0.0065(7) C4 0.0172(8) 0.0217(10) 0.0182(9) -0.0053(8) -0.0047(6) -0.0064(7) C41 0.0213(9) 0.0293(11) 0.0216(10) -0.0106(9) -0.0016(7) -0.0086(8) N41 0.0336(10) 0.0541(14) 0.0338(11) -0.0205(10) -0.0054(8) -0.0196(10) C51 0.0189(8) 0.0199(9) 0.0204(9) -0.0080(8) -0.0025(7) -0.0069(7) N52 0.0172(7) 0.0188(8) 0.0181(8) -0.0054(6) -0.0046(6) -0.0047(6) N53 0.0227(8) 0.0212(9) 0.0315(10) -0.0087(8) -0.0102(7) -0.0016(7) N54 0.0240(8) 0.0231(10) 0.0405(11) -0.0150(9) -0.0104(8) -0.0002(7) N55 0.0271(9) 0.0219(9) 0.0318(10) -0.0132(8) -0.0080(7) -0.0032(7) C01 0.040(2) 0.031(2) 0.038(2) -0.0088(18) -0.0046(17) -0.0149(17) O02 0.0250(12) 0.0311(15) 0.0377(16) -0.0085(12) -0.0095(11) -0.0058(10) C03 0.0356(13) 0.0195(12) 0.071(2) -0.0131(13) -0.0191(13) 0.0020(10) C04 0.0300(12) 0.0460(16) 0.0328(14) -0.0155(12) -0.0056(10) 0.0105(11) O05 0.0468(11) 0.0587(14) 0.0514(13) -0.0216(11) -0.0071(9) -0.0111(10) C06 0.068(2) 0.055(2) 0.0456(19) -0.0163(16) 0.0078(16) -0.0172(17) C101 0.0258(10) 0.0440(14) 0.0172(10) -0.0161(10) -0.0021(7) -0.0045(9) C102 0.0357(11) 0.0283(12) 0.0197(10) -0.0142(9) -0.0047(8) -0.0021(9) C103 0.0348(11) 0.0326(12) 0.0228(10) -0.0162(9) -0.0043(8) -0.0113(9) C104 0.0311(10) 0.0334(12) 0.0171(10) -0.0094(9) -0.0100(8) -0.0050(9) C105 0.0334(11) 0.0349(13) 0.0136(9) -0.0063(9) -0.0027(8) -0.0141(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.0518(18) . ? Ru1 N52 2.0571(17) . ? Ru1 C102 2.194(2) . ? Ru1 C101 2.198(2) . ? Ru1 C105 2.214(2) . ? Ru1 C103 2.217(2) . ? Ru1 C104 2.226(2) . ? Ru1 P1 2.3242(5) . ? P1 C111 1.826(2) . ? P1 C121 1.829(2) . ? P1 C131 1.8393(19) . ? C111 C112 1.388(3) . ? C111 C116 1.398(3) . ? C112 C113 1.383(3) . ? C112 H112 0.95 . ? C113 C114 1.375(4) . ? C113 H113 0.95 . ? C114 C115 1.393(4) . ? C114 H114 0.95 . ? C115 C116 1.382(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.393(3) . ? C121 C126 1.395(3) . ? C122 C123 1.395(3) . ? C122 H122 0.95 . ? C123 C124 1.374(3) . ? C123 H123 0.95 . ? C124 C125 1.389(3) . ? C124 H124 0.95 . ? C125 C126 1.384(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.387(3) . ? C131 C132 1.396(3) . ? C132 C133 1.390(3) . ? C132 H132 0.95 . ? C133 C134 1.388(4) . ? C133 H133 0.95 . ? C134 C135 1.376(3) . ? C134 H134 0.95 . ? C135 C136 1.393(3) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C1 C2 1.364(3) . ? C1 C12 1.439(3) . ? C1 C11 1.443(3) . ? C11 N11 1.145(3) . ? C12 N12 1.137(3) . ? C2 C3 1.466(3) . ? C2 C21 1.485(3) . ? C21 C22 1.391(3) . ? C21 C26 1.400(3) . ? C22 C23 1.391(3) . ? C22 H22 0.95 . ? C23 C24 1.386(3) . ? C23 H23 0.95 . ? C24 C25 1.390(3) . ? C24 H24 0.95 . ? C25 C26 1.379(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.370(3) . ? C4 C51 1.436(3) . ? C4 C41 1.437(3) . ? C41 N41 1.140(3) . ? C51 N55 1.320(3) . ? C51 N52 1.364(3) . ? N52 N53 1.326(2) . ? N53 N54 1.318(3) . ? N54 N55 1.336(3) . ? N54 C03 1.503(3) . ? C01 O02 1.429(5) . ? C01 H01A 0.98 . ? C01 H01B 0.98 . ? C01 H01C 0.98 . ? O02 C03 1.326(4) . ? C03 O02' 1.085(8) . ? C03 C04 1.532(4) . ? C03 H03 1 . ? C03 H03' 1 . ? C04 O05 1.377(3) . ? C04 H04A 0.99 . ? C04 H04B 0.99 . ? O05 C06 1.439(4) . ? C06 H06A 0.98 . ? C06 H06B 0.98 . ? C06 H06C 0.98 . ? C01' O02' 1.487(14) . ? C01' H01D 0.98 . ? C01' H01E 0.98 . ? C01' H01F 0.98 . ? C101 C102 1.408(3) . ? C101 C105 1.425(3) . ? C101 H101 0.95 . ? C102 C103 1.447(3) . ? C102 H102 0.95 . ? C103 C104 1.403(3) . ? C103 H103 0.95 . ? C104 C105 1.424(3) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? O10 C10 1.253(13) . ? 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 C3 Ru1 N52 76.52(7) . . ? C3 Ru1 C102 114.30(8) . . ? N52 Ru1 C102 164.87(8) . . ? C3 Ru1 C101 94.28(8) . . ? N52 Ru1 C101 135.61(8) . . ? C102 Ru1 C101 37.41(9) . . ? C3 Ru1 C105 109.18(8) . . ? N52 Ru1 C105 104.10(8) . . ? C102 Ru1 C105 63.06(9) . . ? C101 Ru1 C105 37.69(9) . . ? C3 Ru1 C103 152.60(8) . . ? N52 Ru1 C103 130.06(8) . . ? C102 Ru1 C103 38.31(8) . . ? C101 Ru1 C103 62.74(9) . . ? C105 Ru1 C103 62.46(9) . . ? C3 Ru1 C104 146.03(8) . . ? N52 Ru1 C104 102.16(8) . . ? C102 Ru1 C104 62.86(9) . . ? C101 Ru1 C104 62.50(8) . . ? C105 Ru1 C104 37.41(8) . . ? C103 Ru1 C104 36.81(9) . . ? C3 Ru1 P1 97.85(5) . . ? N52 Ru1 P1 87.74(5) . . ? C102 Ru1 P1 100.61(7) . . ? C101 Ru1 P1 136.64(7) . . ? C105 Ru1 P1 152.28(6) . . ? C103 Ru1 P1 90.64(6) . . ? C104 Ru1 P1 116.09(6) . . ? C111 P1 C121 104.03(10) . . ? C111 P1 C131 103.08(9) . . ? C121 P1 C131 100.77(9) . . ? C111 P1 Ru1 113.62(7) . . ? C121 P1 Ru1 119.38(6) . . ? C131 P1 Ru1 113.92(7) . . ? C112 C111 C116 118.4(2) . . ? C112 C111 P1 118.95(16) . . ? C116 C111 P1 122.61(17) . . ? C113 C112 C111 121.5(2) . . ? C113 C112 H112 119.2 . . ? C111 C112 H112 119.2 . . ? C114 C113 C112 119.6(2) . . ? C114 C113 H113 120.2 . . ? C112 C113 H113 120.2 . . ? C113 C114 C115 119.9(3) . . ? C113 C114 H114 120.1 . . ? C115 C114 H114 120.1 . . ? C116 C115 C114 120.4(3) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C115 C116 C111 120.1(2) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C122 C121 C126 118.58(18) . . ? C122 C121 P1 123.90(16) . . ? C126 C121 P1 117.47(15) . . ? C121 C122 C123 120.3(2) . . ? C121 C122 H122 119.9 . . ? C123 C122 H122 119.9 . . ? C124 C123 C122 120.5(2) . . ? C124 C123 H123 119.8 . . ? C122 C123 H123 119.8 . . ? C123 C124 C125 119.7(2) . . ? C123 C124 H124 120.2 . . ? C125 C124 H124 120.2 . . ? C126 C125 C124 120.1(2) . . ? C126 C125 H125 119.9 . . ? C124 C125 H125 119.9 . . ? C125 C126 C121 120.8(2) . . ? C125 C126 H126 119.6 . . ? C121 C126 H126 119.6 . . ? C136 C131 C132 118.82(18) . . ? C136 C131 P1 119.96(15) . . ? C132 C131 P1 121.14(16) . . ? C133 C132 C131 120.2(2) . . ? C133 C132 H132 119.9 . . ? C131 C132 H132 119.9 . . ? C134 C133 C132 120.4(2) . . ? C134 C133 H133 119.8 . . ? C132 C133 H133 119.8 . . ? C135 C134 C133 119.7(2) . . ? C135 C134 H134 120.1 . . ? C133 C134 H134 120.1 . . ? C134 C135 C136 120.1(2) . . ? C134 C135 H135 119.9 . . ? C136 C135 H135 119.9 . . ? C131 C136 C135 120.8(2) . . ? C131 C136 H136 119.6 . . ? C135 C136 H136 119.6 . . ? C2 C1 C12 123.81(19) . . ? C2 C1 C11 122.5(2) . . ? C12 C1 C11 113.71(18) . . ? N11 C11 C1 177.3(3) . . ? N12 C12 C1 174.8(2) . . ? C1 C2 C3 121.21(19) . . ? C1 C2 C21 118.64(18) . . ? C3 C2 C21 120.00(16) . . ? C22 C21 C26 119.4(2) . . ? C22 C21 C2 121.30(18) . . ? C26 C21 C2 119.33(17) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C22 119.9(2) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C23 C24 C25 120.0(2) . . ? C23 C24 H24 120 . . ? C25 C24 H24 120 . . ? C26 C25 C24 120.3(2) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C21 120.09(19) . . ? C25 C26 H26 120 . . ? C21 C26 H26 120 . . ? C4 C3 C2 120.71(17) . . ? C4 C3 Ru1 117.96(13) . . ? C2 C3 Ru1 120.67(14) . . ? C3 C4 C51 113.57(17) . . ? C3 C4 C41 126.73(18) . . ? C51 C4 C41 119.69(18) . . ? N41 C41 C4 179.1(2) . . ? N55 C51 N52 111.48(17) . . ? N55 C51 C4 134.24(19) . . ? N52 C51 C4 114.24(17) . . ? N53 N52 C51 107.26(16) . . ? N53 N52 Ru1 134.96(14) . . ? C51 N52 Ru1 117.67(13) . . ? N54 N53 N52 104.40(16) . . ? N53 N54 N55 115.21(17) . . ? N53 N54 C03 121.4(2) . . ? N55 N54 C03 122.1(2) . . ? C51 N55 N54 101.64(17) . . ? C03 O02 C01 115.1(3) . . ? O02' C03 N54 118.8(5) . . ? O02 C03 N54 111.3(3) . . ? O02' C03 C04 123.9(5) . . ? O02 C03 C04 112.9(2) . . ? N54 C03 C04 109.8(2) . . ? O02 C03 H03 107.5 . . ? N54 C03 H03 107.5 . . ? C04 C03 H03 107.5 . . ? O02' C03 H03' 98.9 . . ? N54 C03 H03' 99.1 . . ? C04 C03 H03' 99.4 . . ? O05 C04 C03 107.0(2) . . ? O05 C04 H04A 110.3 . . ? C03 C04 H04A 110.3 . . ? O05 C04 H04B 110.3 . . ? C03 C04 H04B 110.3 . . ? H04A C04 H04B 108.6 . . ? C04 O05 C06 112.1(2) . . ? O05 C06 H06A 109.5 . . ? O05 C06 H06B 109.5 . . ? H06A C06 H06B 109.5 . . ? O05 C06 H06C 109.5 . . ? H06A C06 H06C 109.5 . . ? H06B C06 H06C 109.5 . . ? O02' C01' H01D 109.5 . . ? O02' C01' H01E 109.5 . . ? H01D C01' H01E 109.5 . . ? O02' C01' H01F 109.5 . . ? H01D C01' H01F 109.5 . . ? H01E C01' H01F 109.5 . . ? C03 O02' C01' 122.4(8) . . ? C102 C101 C105 108.9(2) . . ? C102 C101 Ru1 71.14(12) . . ? C105 C101 Ru1 71.76(12) . . ? C102 C101 H101 125.6 . . ? C105 C101 H101 125.6 . . ? Ru1 C101 H101 123.2 . . ? C101 C102 C103 107.2(2) . . ? C101 C102 Ru1 71.45(13) . . ? C103 C102 Ru1 71.72(12) . . ? C101 C102 H102 126.4 . . ? C103 C102 H102 126.4 . . ? Ru1 C102 H102 122.2 . . ? C104 C103 C102 107.9(2) . . ? C104 C103 Ru1 71.95(12) . . ? C102 C103 Ru1 69.97(12) . . ? C104 C103 H103 126 . . ? C102 C103 H103 126 . . ? Ru1 C103 H103 123.7 . . ? C103 C104 C105 108.7(2) . . ? C103 C104 Ru1 71.24(12) . . ? C105 C104 Ru1 70.81(11) . . ? C103 C104 H104 125.7 . . ? C105 C104 H104 125.7 . . ? Ru1 C104 H104 123.9 . . ? C104 C105 C101 107.3(2) . . ? C104 C105 Ru1 71.77(12) . . ? C101 C105 Ru1 70.55(12) . . ? C104 C105 H105 126.3 . . ? C101 C105 H105 126.3 . . ? Ru1 C105 H105 123 . . ? #===END # Attachment '6.br1404a.cif' data_br1404a _database_code_depnum_ccdc_archive 'CCDC 730747' _audit_creation_date 2008-03-06T09:30:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C79.16 H67.32 Cl1.32 N7 P3 Pt Ru' _chemical_formula_moiety 'C79 H67 Cl1 N7 P3 Pt Ru, 0.16(C H2 Cl2)' _chemical_formula_weight 1552.5 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall -P_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.9190(3) _cell_length_b 18.4210(3) _cell_length_c 22.6747(4) _cell_angle_alpha 90 _cell_angle_beta 105.141(2) _cell_angle_gamma 90 _cell_volume 7224.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16182 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 66.9842 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_colour dark_red _exptl_crystal_F_000 3122.9 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.707 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_T_max 0.829 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 0.0556049384 _diffrn_orient_matrix_ub_12 0.0011170136 _diffrn_orient_matrix_ub_13 0.0645513862 _diffrn_orient_matrix_ub_21 0.0427839033 _diffrn_orient_matrix_ub_22 -0.0665527777 _diffrn_orient_matrix_ub_23 -0.0163434781 _diffrn_orient_matrix_ub_31 0.0547179474 _diffrn_orient_matrix_ub_32 0.0507749154 _diffrn_orient_matrix_ub_33 -0.0229257095 _diffrn_reflns_av_R_equivalents 0.0927 _diffrn_reflns_av_unetI/netI 0.0649 _diffrn_reflns_number 81172 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 67.19 _diffrn_reflns_theta_full 67.19 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 12778 _reflns_number_gt 7969 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^+16.9244P] 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_number_reflns 12778 _refine_ls_number_parameters 858 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.662 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.154 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru 0.0552 3.296 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.38014(4) 0.25602(3) 0.37342(3) 0.03345(16) Uani 1 1 d . . . Pt1 Pt 0.70233(2) 0.346135(18) 0.366510(14) 0.03220(12) Uani 1 1 d . . . Cl1 Cl 0.70743(12) 0.21949(10) 0.36431(9) 0.0373(4) Uani 1 1 d . . . C1 C 0.3475(5) 0.2568(5) 0.1943(4) 0.040(2) Uani 1 1 d . . . C11 C 0.3073(5) 0.2265(5) 0.1347(4) 0.046(2) Uani 1 1 d . . . N11 N 0.2795(5) 0.2028(6) 0.0886(4) 0.065(2) Uani 1 1 d . . . C12 C 0.3523(6) 0.3350(6) 0.1982(4) 0.052(2) Uani 1 1 d . . . N12 N 0.3546(6) 0.3971(5) 0.2033(4) 0.067(3) Uani 1 1 d . . . C2 C 0.3797(5) 0.2129(5) 0.2421(4) 0.0369(19) Uani 1 1 d . . . C21 C 0.3671(6) 0.1338(5) 0.2367(3) 0.043(2) Uani 1 1 d . . . C22 C 0.2959(5) 0.1033(5) 0.2339(4) 0.046(2) Uani 1 1 d . . . H22 H 0.2537 0.1337 0.2357 0.056 Uiso 1 1 calc R . . C23 C 0.2852(6) 0.0270(5) 0.2283(4) 0.048(2) Uani 1 1 d . . . H23 H 0.2368 0.0058 0.2283 0.058 Uiso 1 1 calc R . . C24 C 0.3455(6) -0.0151(5) 0.2230(4) 0.053(2) Uani 1 1 d . . . H24 H 0.3384 -0.066 0.2183 0.063 Uiso 1 1 calc R . . C25 C 0.4165(6) 0.0145(5) 0.2243(4) 0.046(2) Uani 1 1 d . . . H25 H 0.4576 -0.0157 0.2199 0.055 Uiso 1 1 calc R . . C26 C 0.4273(5) 0.0880(5) 0.2320(4) 0.042(2) Uani 1 1 d . . . H26 H 0.4768 0.1081 0.2343 0.05 Uiso 1 1 calc R . . C3 C 0.4262(5) 0.2431(4) 0.3009(3) 0.0353(18) Uani 1 1 d . . . C4 C 0.4971(5) 0.2724(4) 0.3040(3) 0.0349(18) Uani 1 1 d . . . C41 C 0.5343(5) 0.2752(4) 0.2541(3) 0.0330(18) Uani 1 1 d . . . N41 N 0.5609(4) 0.2797(4) 0.2141(3) 0.0469(19) Uani 1 1 d . . . C51 C 0.5328(5) 0.3031(4) 0.3628(4) 0.0333(18) Uani 1 1 d . . . N52 N 0.4874(4) 0.3038(3) 0.4020(3) 0.0314(14) Uani 1 1 d . . . N53 N 0.5275(4) 0.3386(4) 0.4529(3) 0.0366(16) Uani 1 1 d . . . N54 N 0.5962(4) 0.3560(3) 0.4458(3) 0.0337(15) Uani 1 1 d . . . N55 N 0.5990(4) 0.3356(3) 0.3894(3) 0.0282(14) Uani 1 1 d . . . P1 P 0.43178(13) 0.15117(11) 0.42324(9) 0.0350(4) Uani 1 1 d . . . C111 C 0.3577(5) 0.0932(4) 0.4407(4) 0.0375(19) Uani 1 1 d . . . C112 C 0.2983(5) 0.0665(5) 0.3927(4) 0.046(2) Uani 1 1 d . . . H112 H 0.2986 0.0774 0.3518 0.055 Uiso 1 1 calc R . . C113 C 0.2391(6) 0.0246(5) 0.4034(4) 0.053(2) Uani 1 1 d . . . H113 H 0.1996 0.0066 0.3701 0.064 Uiso 1 1 calc R . . C114 C 0.2378(6) 0.0090(5) 0.4621(4) 0.052(2) Uani 1 1 d . . . H114 H 0.1977 -0.0205 0.4695 0.063 Uiso 1 1 calc R . . C115 C 0.2949(6) 0.0362(6) 0.5110(4) 0.053(3) Uani 1 1 d . . . H115 H 0.2925 0.0277 0.5518 0.064 Uiso 1 1 calc R . . C116 C 0.3557(5) 0.0759(5) 0.4995(4) 0.045(2) Uani 1 1 d . . . H116 H 0.3967 0.0914 0.5329 0.054 Uiso 1 1 calc R . . C121 C 0.4875(5) 0.0852(5) 0.3898(4) 0.040(2) Uani 1 1 d . . . C122 C 0.4705(5) 0.0127(5) 0.3832(4) 0.042(2) Uani 1 1 d . . . H122 H 0.4283 -0.0058 0.3968 0.051 Uiso 1 1 calc R . . C123 C 0.5137(5) -0.0348(5) 0.3570(4) 0.041(2) Uani 1 1 d . . . H123 H 0.4986 -0.0841 0.3494 0.049 Uiso 1 1 calc R . . C124 C 0.5788(5) -0.0085(5) 0.3425(4) 0.041(2) Uani 1 1 d . . . H124 H 0.6109 -0.0408 0.3275 0.049 Uiso 1 1 calc R . . C125 C 0.5977(5) 0.0646(4) 0.3495(3) 0.0386(19) Uani 1 1 d . . . H125 H 0.6409 0.0828 0.3371 0.046 Uiso 1 1 calc R . . C126 C 0.5532(5) 0.1114(4) 0.3749(3) 0.0351(18) Uani 1 1 d . . . H126 H 0.5676 0.1609 0.3819 0.042 Uiso 1 1 calc R . . C131 C 0.5004(5) 0.1672(4) 0.4990(3) 0.0347(18) Uani 1 1 d . . . C132 C 0.5677(5) 0.1287(5) 0.5212(4) 0.042(2) Uani 1 1 d . . . H132 H 0.5801 0.0897 0.498 0.05 Uiso 1 1 calc R . . C133 C 0.6179(6) 0.1465(5) 0.5776(4) 0.049(2) Uani 1 1 d . . . H133 H 0.6647 0.1202 0.592 0.058 Uiso 1 1 calc R . . C134 C 0.6005(6) 0.2015(5) 0.6123(4) 0.045(2) Uani 1 1 d . . . H134 H 0.6341 0.2119 0.6513 0.054 Uiso 1 1 calc R . . C135 C 0.5346(6) 0.2416(5) 0.5909(4) 0.046(2) Uani 1 1 d . . . H135 H 0.5228 0.2801 0.6148 0.055 Uiso 1 1 calc R . . C136 C 0.4848(5) 0.2260(5) 0.5337(4) 0.042(2) Uani 1 1 d . . . H136 H 0.4402 0.2551 0.5182 0.05 Uiso 1 1 calc R . . P2 P 0.68817(12) 0.46775(11) 0.36421(8) 0.0308(4) Uani 1 1 d . . . C211 C 0.5962(5) 0.4989(4) 0.3760(3) 0.0310(17) Uani 1 1 d . . . C212 C 0.5272(5) 0.4836(4) 0.3331(4) 0.041(2) Uani 1 1 d . . . H212 H 0.5282 0.4586 0.2967 0.05 Uiso 1 1 calc R . . C213 C 0.4575(5) 0.5042(5) 0.3425(4) 0.0383(19) Uani 1 1 d . . . H213 H 0.4112 0.4929 0.3123 0.046 Uiso 1 1 calc R . . C214 C 0.4530(5) 0.5415(4) 0.3955(4) 0.0372(19) Uani 1 1 d . . . C215 C 0.5210(5) 0.5580(5) 0.4371(4) 0.040(2) Uani 1 1 d . . . H215 H 0.5198 0.5839 0.4731 0.048 Uiso 1 1 calc R . . C216 C 0.5918(5) 0.5377(4) 0.4282(4) 0.0371(19) Uani 1 1 d . . . H216 H 0.6381 0.5504 0.4578 0.045 Uiso 1 1 calc R . . C217 C 0.3757(5) 0.5639(6) 0.4072(4) 0.053(2) Uani 1 1 d . . . H21A H 0.3823 0.5702 0.4512 0.08 Uiso 1 1 calc R . . H21B H 0.3371 0.526 0.3918 0.08 Uiso 1 1 calc R . . H21C H 0.3583 0.6096 0.386 0.08 Uiso 1 1 calc R . . C221 C 0.6815(5) 0.5023(4) 0.2878(4) 0.0328(17) Uani 1 1 d . . . C222 C 0.6696(5) 0.4509(5) 0.2404(4) 0.0371(18) Uani 1 1 d . . . H222 H 0.6666 0.4007 0.2492 0.045 Uiso 1 1 calc R . . C223 C 0.6624(5) 0.4735(5) 0.1804(4) 0.040(2) Uani 1 1 d . . . H223 H 0.6541 0.4384 0.1486 0.048 Uiso 1 1 calc R . . C224 C 0.6672(5) 0.5457(4) 0.1664(4) 0.0381(19) Uani 1 1 d . . . C225 C 0.6765(5) 0.5973(5) 0.2130(4) 0.041(2) Uani 1 1 d . . . H225 H 0.6794 0.6474 0.2039 0.049 Uiso 1 1 calc R . . C226 C 0.6815(5) 0.5753(5) 0.2732(4) 0.040(2) Uani 1 1 d . . . H226 H 0.6851 0.6108 0.3042 0.047 Uiso 1 1 calc R . . C227 C 0.6594(6) 0.5675(5) 0.1007(4) 0.045(2) Uani 1 1 d . . . H22A H 0.6523 0.524 0.0749 0.068 Uiso 1 1 calc R . . H22B H 0.7062 0.5931 0.0977 0.068 Uiso 1 1 calc R . . H22C H 0.6146 0.5996 0.0868 0.068 Uiso 1 1 calc R . . C231 C 0.7584(5) 0.5115(4) 0.4252(4) 0.0368(19) Uani 1 1 d . . . C232 C 0.7713(5) 0.4770(4) 0.4822(4) 0.0366(19) Uani 1 1 d . . . H232 H 0.7509 0.4298 0.4849 0.044 Uiso 1 1 calc R . . C233 C 0.8135(5) 0.5115(5) 0.5344(4) 0.041(2) Uani 1 1 d . . . H233 H 0.8211 0.4878 0.5727 0.049 Uiso 1 1 calc R . . C234 C 0.8448(5) 0.5789(5) 0.5325(4) 0.040(2) Uani 1 1 d . . . C235 C 0.8354(5) 0.6122(5) 0.4756(4) 0.0383(19) Uani 1 1 d . . . H235 H 0.859 0.6578 0.4729 0.046 Uiso 1 1 calc R . . C236 C 0.7914(5) 0.5787(4) 0.4228(4) 0.0367(19) Uani 1 1 d . . . H236 H 0.7841 0.6025 0.3846 0.044 Uiso 1 1 calc R . . C237 C 0.8862(5) 0.6176(5) 0.5904(4) 0.046(2) Uani 1 1 d . . . H23A H 0.8489 0.6459 0.6057 0.07 Uiso 1 1 calc R . . H23B H 0.9253 0.6503 0.5818 0.07 Uiso 1 1 calc R . . H23C H 0.9114 0.5819 0.6212 0.07 Uiso 1 1 calc R . . P3 P 0.82125(12) 0.34471(11) 0.34894(9) 0.0312(4) Uani 1 1 d . . . C311 C 0.8850(5) 0.2850(4) 0.4045(4) 0.0343(18) Uani 1 1 d . . . C312 C 0.9478(5) 0.2492(5) 0.3910(4) 0.040(2) Uani 1 1 d . . . H312 H 0.9564 0.2532 0.3516 0.048 Uiso 1 1 calc R . . C313 C 0.9969(6) 0.2080(5) 0.4357(4) 0.050(2) Uani 1 1 d . . . H313 H 1.0394 0.1842 0.4264 0.059 Uiso 1 1 calc R . . C314 C 0.9862(6) 0.2002(5) 0.4936(5) 0.055(3) Uani 1 1 d . . . C315 C 0.9222(6) 0.2334(5) 0.5049(4) 0.048(2) Uani 1 1 d . . . H315 H 0.9125 0.2274 0.5439 0.057 Uiso 1 1 calc R . . C316 C 0.8723(6) 0.2747(5) 0.4620(4) 0.044(2) Uani 1 1 d . . . H316 H 0.8288 0.2964 0.4715 0.053 Uiso 1 1 calc R . . C317 C 1.0407(7) 0.1541(6) 0.5421(6) 0.076(3) Uani 1 1 d . . . H31A H 1.0174 0.1063 0.5441 0.114 Uiso 1 1 calc R . . H31B H 1.0498 0.1782 0.5819 0.114 Uiso 1 1 calc R . . H31C H 1.09 0.1481 0.5314 0.114 Uiso 1 1 calc R . . C321 C 0.8200(5) 0.3129(4) 0.2723(3) 0.0343(18) Uani 1 1 d . . . C322 C 0.7535(5) 0.2826(4) 0.2353(4) 0.0373(19) Uani 1 1 d . . . H322 H 0.7094 0.276 0.2505 0.045 Uiso 1 1 calc R . . C323 C 0.7512(5) 0.2618(4) 0.1765(4) 0.0378(19) Uani 1 1 d . . . H323 H 0.7057 0.2394 0.1523 0.045 Uiso 1 1 calc R . . C324 C 0.8136(6) 0.2727(4) 0.1512(4) 0.045(2) Uani 1 1 d . . . C325 C 0.8824(6) 0.3016(5) 0.1901(4) 0.049(2) Uani 1 1 d . . . H325 H 0.9272 0.3063 0.1755 0.059 Uiso 1 1 calc R . . C326 C 0.8850(5) 0.3235(4) 0.2501(4) 0.0384(19) Uani 1 1 d . . . H326 H 0.9303 0.3452 0.2752 0.046 Uiso 1 1 calc R . . C327 C 0.8114(7) 0.2499(6) 0.0876(5) 0.059(3) Uani 1 1 d . . . H32A H 0.8375 0.2865 0.0687 0.089 Uiso 1 1 calc R . . H32B H 0.7575 0.2452 0.0637 0.089 Uiso 1 1 calc R . . H32C H 0.8377 0.2031 0.0887 0.089 Uiso 1 1 calc R . . C331 C 0.8770(4) 0.4287(4) 0.3574(3) 0.0320(17) Uani 1 1 d . . . C332 C 0.9307(5) 0.4453(5) 0.4116(4) 0.0390(19) Uani 1 1 d . . . H332 H 0.9411 0.4112 0.4442 0.047 Uiso 1 1 calc R . . C333 C 0.9693(5) 0.5108(5) 0.4189(4) 0.0376(19) Uani 1 1 d . . . H333 H 1.0071 0.5201 0.4561 0.045 Uiso 1 1 calc R . . C334 C 0.9550(5) 0.5632(5) 0.3741(4) 0.040(2) Uani 1 1 d . . . C335 C 0.9013(5) 0.5464(5) 0.3186(4) 0.0376(19) Uani 1 1 d . . . H335 H 0.891 0.5807 0.2862 0.045 Uiso 1 1 calc R . . C336 C 0.8633(5) 0.4801(4) 0.3107(4) 0.0376(19) Uani 1 1 d . . . H336 H 0.8273 0.4695 0.2728 0.045 Uiso 1 1 calc R . . C337 C 0.9943(6) 0.6362(5) 0.3864(4) 0.051(2) Uani 1 1 d . . . H33A H 0.9854 0.657 0.4237 0.076 Uiso 1 1 calc R . . H33B H 0.9731 0.6688 0.3519 0.076 Uiso 1 1 calc R . . H33C H 1.05 0.6303 0.3914 0.076 Uiso 1 1 calc R . . C101 C 0.2683(5) 0.2975(6) 0.3210(4) 0.052(2) Uani 1 1 d . . . H101 H 0.2548 0.2997 0.2776 0.062 Uiso 1 1 calc R . . C102 C 0.2540(6) 0.2385(5) 0.3555(4) 0.050(2) Uani 1 1 d . . . H102 H 0.2298 0.1939 0.3403 0.061 Uiso 1 1 calc R . . C103 C 0.2829(5) 0.2583(5) 0.4177(5) 0.055(3) Uani 1 1 d . . . H103 H 0.2803 0.2291 0.4516 0.065 Uiso 1 1 calc R . . C104 C 0.3157(5) 0.3273(5) 0.4215(4) 0.049(2) Uani 1 1 d . . . H104 H 0.3403 0.3528 0.4578 0.059 Uiso 1 1 calc R . . C105 C 0.3053(5) 0.3523(5) 0.3601(5) 0.050(2) Uani 1 1 d . . . H105 H 0.3209 0.3982 0.3482 0.06 Uiso 1 1 calc R . . Cl11 Cl 0.0434(19) 0.084(2) 0.3109(16) 0.19(2) Uani 0.160(8) 1 d P . . Cl12 Cl 0.0688(14) 0.213(3) 0.2595(13) 0.160(18) Uani 0.160(8) 1 d P . . C01 C 0.006(5) 0.146(4) 0.263(3) 0.07(2) Uiso 0.160(8) 1 d P . . H01A H -0.0392 0.1675 0.2743 0.087 Uiso 0.160(8) 1 calc PR . . H01B H -0.0131 0.1245 0.2217 0.087 Uiso 0.160(8) 1 calc PR . . 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 0.0358(4) 0.0343(3) 0.0354(3) 0.0006(3) 0.0185(3) 0.0007(3) Pt1 0.0395(2) 0.02985(18) 0.03311(18) -0.00164(14) 0.01992(14) -0.00155(15) Cl1 0.0407(11) 0.0305(9) 0.0446(10) 0.0052(8) 0.0182(8) -0.0003(8) C1 0.044(5) 0.042(5) 0.040(5) -0.001(4) 0.020(4) 0.003(4) C11 0.049(6) 0.057(6) 0.032(5) 0.008(4) 0.010(4) 0.004(4) N11 0.059(6) 0.094(7) 0.039(5) 0.000(5) 0.006(4) -0.003(5) C12 0.062(7) 0.055(7) 0.037(5) 0.007(4) 0.011(4) 0.003(5) N12 0.084(7) 0.054(6) 0.056(5) 0.015(4) 0.006(5) 0.004(5) C2 0.035(5) 0.041(5) 0.042(4) -0.003(4) 0.022(4) -0.002(4) C21 0.059(6) 0.054(6) 0.018(4) -0.002(4) 0.013(4) -0.007(4) C22 0.036(5) 0.059(6) 0.047(5) -0.001(4) 0.015(4) -0.001(4) C23 0.052(6) 0.053(6) 0.041(5) -0.013(4) 0.015(4) -0.018(5) C24 0.059(7) 0.046(6) 0.050(5) -0.005(4) 0.009(5) -0.003(5) C25 0.054(6) 0.040(5) 0.044(5) -0.003(4) 0.012(4) 0.000(4) C26 0.043(5) 0.048(5) 0.038(4) -0.009(4) 0.017(4) -0.003(4) C3 0.049(5) 0.032(4) 0.033(4) 0.005(3) 0.024(4) 0.004(4) C4 0.037(5) 0.041(5) 0.033(4) 0.000(3) 0.020(3) 0.004(4) C41 0.039(5) 0.030(4) 0.033(4) -0.006(3) 0.014(4) -0.010(3) N41 0.049(5) 0.063(5) 0.034(4) -0.011(3) 0.021(3) -0.014(4) C51 0.038(5) 0.030(4) 0.040(4) 0.004(3) 0.024(4) 0.010(4) N52 0.038(4) 0.027(3) 0.034(3) -0.004(3) 0.019(3) -0.001(3) N53 0.046(4) 0.037(4) 0.033(3) -0.002(3) 0.021(3) -0.001(3) N54 0.044(4) 0.033(4) 0.031(3) -0.006(3) 0.021(3) -0.008(3) N55 0.032(4) 0.033(4) 0.025(3) -0.010(3) 0.016(3) -0.011(3) P1 0.0459(12) 0.0293(10) 0.0375(10) 0.0002(9) 0.0245(9) -0.0017(9) C111 0.048(5) 0.031(4) 0.037(4) 0.003(3) 0.017(4) 0.005(4) C112 0.052(6) 0.046(5) 0.048(5) -0.009(4) 0.027(4) -0.012(4) C113 0.051(6) 0.053(6) 0.054(6) -0.005(5) 0.011(5) -0.009(5) C114 0.050(6) 0.057(6) 0.053(6) 0.003(5) 0.018(5) -0.026(5) C115 0.060(6) 0.066(6) 0.042(5) 0.001(5) 0.027(4) -0.022(5) C116 0.047(5) 0.050(6) 0.043(5) 0.014(4) 0.021(4) 0.001(4) C121 0.045(5) 0.043(5) 0.037(4) 0.010(4) 0.022(4) 0.009(4) C122 0.053(6) 0.043(5) 0.038(4) -0.007(4) 0.022(4) -0.009(4) C123 0.056(6) 0.030(4) 0.041(4) 0.004(4) 0.022(4) -0.002(4) C124 0.047(5) 0.041(5) 0.041(5) -0.003(4) 0.022(4) 0.005(4) C125 0.059(6) 0.029(4) 0.035(4) -0.003(3) 0.026(4) 0.001(4) C126 0.046(5) 0.026(4) 0.039(4) 0.003(3) 0.021(4) 0.000(3) C131 0.041(5) 0.038(5) 0.030(4) -0.001(3) 0.018(3) -0.002(4) C132 0.051(6) 0.034(5) 0.042(5) -0.002(4) 0.017(4) -0.001(4) C133 0.051(6) 0.057(6) 0.040(5) 0.004(4) 0.016(4) -0.004(5) C134 0.051(6) 0.045(5) 0.042(5) 0.006(4) 0.017(4) -0.009(4) C135 0.061(6) 0.043(5) 0.043(5) 0.000(4) 0.028(4) -0.007(4) C136 0.049(5) 0.042(5) 0.039(5) 0.004(4) 0.021(4) 0.000(4) P2 0.0385(12) 0.0314(10) 0.0266(9) -0.0042(8) 0.0160(8) -0.0001(8) C211 0.045(5) 0.025(4) 0.029(4) 0.005(3) 0.021(3) -0.001(3) C212 0.059(6) 0.034(5) 0.035(4) -0.007(4) 0.019(4) -0.006(4) C213 0.033(5) 0.041(5) 0.044(5) -0.002(4) 0.016(4) 0.000(4) C214 0.045(5) 0.028(4) 0.044(5) -0.001(4) 0.021(4) 0.005(4) C215 0.047(5) 0.038(5) 0.042(5) -0.004(4) 0.022(4) 0.005(4) C216 0.043(5) 0.032(4) 0.042(4) -0.005(4) 0.021(4) -0.002(4) C217 0.049(6) 0.065(7) 0.053(5) -0.008(5) 0.025(4) -0.010(5) C221 0.032(4) 0.031(4) 0.040(4) -0.004(3) 0.017(3) -0.001(3) C222 0.041(5) 0.033(4) 0.038(4) -0.009(4) 0.012(4) 0.001(4) C223 0.038(5) 0.044(5) 0.042(5) -0.003(4) 0.016(4) 0.001(4) C224 0.047(5) 0.032(5) 0.038(4) -0.003(4) 0.017(4) -0.003(4) C225 0.043(5) 0.036(5) 0.045(5) 0.005(4) 0.013(4) 0.005(4) C226 0.050(5) 0.035(5) 0.036(4) -0.004(4) 0.016(4) 0.000(4) C227 0.058(6) 0.047(5) 0.031(4) 0.006(4) 0.012(4) 0.002(4) C231 0.041(5) 0.040(5) 0.036(4) -0.007(4) 0.023(4) 0.004(4) C232 0.042(5) 0.033(4) 0.038(4) 0.008(4) 0.015(4) 0.001(4) C233 0.041(5) 0.036(5) 0.048(5) 0.007(4) 0.017(4) 0.008(4) C234 0.039(5) 0.043(5) 0.041(5) -0.004(4) 0.016(4) 0.002(4) C235 0.045(5) 0.035(5) 0.035(4) -0.001(4) 0.011(4) 0.000(4) C236 0.046(5) 0.033(5) 0.033(4) 0.003(3) 0.014(4) 0.003(4) C237 0.042(5) 0.052(6) 0.044(5) -0.011(4) 0.009(4) -0.019(4) P3 0.0371(11) 0.0279(10) 0.0337(10) -0.0023(8) 0.0184(8) 0.0004(9) C311 0.041(5) 0.020(4) 0.047(5) 0.001(3) 0.021(4) -0.003(3) C312 0.033(5) 0.048(5) 0.043(5) 0.002(4) 0.015(4) 0.001(4) C313 0.042(6) 0.042(5) 0.068(6) 0.005(5) 0.018(5) 0.003(4) C314 0.069(7) 0.034(5) 0.060(6) 0.008(4) 0.015(5) 0.011(5) C315 0.064(6) 0.032(5) 0.047(5) 0.004(4) 0.015(5) 0.002(4) C316 0.052(6) 0.036(5) 0.048(5) 0.000(4) 0.019(4) -0.003(4) C317 0.080(9) 0.061(7) 0.079(8) 0.007(6) 0.005(6) 0.021(6) C321 0.044(5) 0.030(4) 0.036(4) 0.008(3) 0.024(4) 0.009(4) C322 0.047(5) 0.034(4) 0.038(4) -0.001(4) 0.025(4) 0.002(4) C323 0.046(5) 0.031(4) 0.043(5) -0.002(4) 0.022(4) 0.002(4) C324 0.066(6) 0.028(4) 0.055(5) -0.005(4) 0.042(5) -0.009(4) C325 0.056(6) 0.053(6) 0.049(5) -0.005(4) 0.034(5) -0.009(5) C326 0.047(5) 0.033(4) 0.042(5) -0.005(4) 0.024(4) 0.000(4) C327 0.075(7) 0.056(6) 0.059(6) -0.019(5) 0.040(5) -0.018(5) C331 0.030(4) 0.033(4) 0.039(4) -0.002(3) 0.022(3) -0.004(3) C332 0.044(5) 0.044(5) 0.033(4) 0.006(4) 0.017(4) 0.004(4) C333 0.037(5) 0.041(5) 0.039(4) -0.005(4) 0.018(4) 0.000(4) C334 0.050(5) 0.039(5) 0.038(4) -0.003(4) 0.025(4) -0.004(4) C335 0.039(5) 0.037(5) 0.047(5) 0.002(4) 0.030(4) -0.001(4) C336 0.043(5) 0.040(5) 0.035(4) -0.007(4) 0.020(4) 0.005(4) C337 0.063(6) 0.047(6) 0.048(5) -0.002(4) 0.027(5) -0.014(5) C101 0.043(6) 0.075(7) 0.038(5) 0.003(5) 0.013(4) 0.013(5) C102 0.051(6) 0.048(6) 0.060(6) -0.001(5) 0.027(5) 0.008(4) C103 0.040(5) 0.056(6) 0.080(7) 0.010(5) 0.039(5) 0.007(5) C104 0.032(5) 0.063(6) 0.058(6) -0.020(5) 0.021(4) 0.001(4) C105 0.032(5) 0.044(5) 0.082(7) 0.000(5) 0.027(5) 0.010(4) Cl11 0.11(3) 0.27(5) 0.15(3) -0.04(3) -0.02(2) 0.12(3) Cl12 0.048(14) 0.32(5) 0.105(19) 0.00(2) 0.004(12) -0.03(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.038(7) . ? Ru1 N52 2.059(7) . ? Ru1 C101 2.184(9) . ? Ru1 C105 2.197(9) . ? Ru1 C102 2.213(10) . ? Ru1 C104 2.214(8) . ? Ru1 C103 2.227(9) . ? Ru1 P1 2.306(2) . ? Pt1 N55 2.058(6) . ? Pt1 P2 2.254(2) . ? Pt1 P3 2.268(2) . ? Pt1 Cl1 2.3358(19) . ? C1 C2 1.355(12) . ? C1 C12 1.445(13) . ? C1 C11 1.465(13) . ? C11 N11 1.122(12) . ? C12 N12 1.149(13) . ? C2 C21 1.475(12) . ? C2 C3 1.483(12) . ? C21 C22 1.380(13) . ? C21 C26 1.395(13) . ? C22 C23 1.420(13) . ? C22 H22 0.95 . ? C23 C24 1.360(14) . ? C23 H23 0.95 . ? C24 C25 1.378(14) . ? C24 H24 0.95 . ? C25 C26 1.372(12) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.364(12) . ? C4 C51 1.436(11) . ? C4 C41 1.457(10) . ? C41 N41 1.131(10) . ? C51 N55 1.324(10) . ? C51 N52 1.352(9) . ? N52 N53 1.351(9) . ? N53 N54 1.323(9) . ? N54 N55 1.347(8) . ? P1 C111 1.827(9) . ? P1 C131 1.856(8) . ? P1 C121 1.856(8) . ? C111 C116 1.381(11) . ? C111 C112 1.397(12) . ? C112 C113 1.384(13) . ? C112 H112 0.95 . ? C113 C114 1.368(13) . ? C113 H113 0.95 . ? C114 C115 1.391(13) . ? C114 H114 0.95 . ? C115 C116 1.391(12) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.369(12) . ? C121 C126 1.393(11) . ? C122 C123 1.400(12) . ? C122 H122 0.95 . ? C123 C124 1.379(12) . ? C123 H123 0.95 . ? C124 C125 1.388(12) . ? C124 H124 0.95 . ? C125 C126 1.397(11) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.377(12) . ? C131 C136 1.408(12) . ? C132 C133 1.397(13) . ? C132 H132 0.95 . ? C133 C134 1.368(13) . ? C133 H133 0.95 . ? C134 C135 1.369(13) . ? C134 H134 0.95 . ? C135 C136 1.399(13) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? P2 C231 1.799(9) . ? P2 C221 1.820(8) . ? P2 C211 1.830(8) . ? C211 C212 1.388(12) . ? C211 C216 1.401(11) . ? C212 C213 1.373(12) . ? C212 H212 0.95 . ? C213 C214 1.406(11) . ? C213 H213 0.95 . ? C214 C215 1.366(12) . ? C214 C217 1.532(12) . ? C215 C216 1.388(11) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C217 H21A 0.98 . ? C217 H21B 0.98 . ? C217 H21C 0.98 . ? C221 C226 1.385(11) . ? C221 C222 1.408(11) . ? C222 C223 1.397(12) . ? C222 H222 0.95 . ? C223 C224 1.375(12) . ? C223 H223 0.95 . ? C224 C225 1.399(12) . ? C224 C227 1.514(11) . ? C225 C226 1.404(12) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? C227 H22A 0.98 . ? C227 H22B 0.98 . ? C227 H22C 0.98 . ? C231 C236 1.379(12) . ? C231 C232 1.406(11) . ? C232 C233 1.383(12) . ? C232 H232 0.95 . ? C233 C234 1.368(12) . ? C233 H233 0.95 . ? C234 C235 1.398(12) . ? C234 C237 1.507(12) . ? C235 C236 1.394(12) . ? C235 H235 0.95 . ? C236 H236 0.95 . ? C237 H23A 0.98 . ? C237 H23B 0.98 . ? C237 H23C 0.98 . ? P3 C331 1.825(8) . ? P3 C321 1.828(8) . ? P3 C311 1.831(8) . ? C311 C316 1.393(12) . ? C311 C312 1.405(11) . ? C312 C313 1.383(13) . ? C312 H312 0.95 . ? C313 C314 1.381(14) . ? C313 H313 0.95 . ? C314 C315 1.383(14) . ? C314 C317 1.524(14) . ? C315 C316 1.366(13) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C317 H31A 0.98 . ? C317 H31B 0.98 . ? C317 H31C 0.98 . ? C321 C322 1.383(12) . ? C321 C326 1.398(11) . ? C322 C323 1.378(11) . ? C322 H322 0.95 . ? C323 C324 1.399(11) . ? C323 H323 0.95 . ? C324 C325 1.419(14) . ? C324 C327 1.490(12) . ? C325 C326 1.407(12) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C327 H32A 0.98 . ? C327 H32B 0.98 . ? C327 H32C 0.98 . ? C331 C332 1.382(12) . ? C331 C336 1.394(11) . ? C332 C333 1.379(12) . ? C332 H332 0.95 . ? C333 C334 1.375(12) . ? C333 H333 0.95 . ? C334 C335 1.403(12) . ? C334 C337 1.511(12) . ? C335 C336 1.388(12) . ? C335 H335 0.95 . ? C336 H336 0.95 . ? C337 H33A 0.98 . ? C337 H33B 0.98 . ? C337 H33C 0.98 . ? C101 C105 1.393(14) . ? C101 C102 1.402(14) . ? C101 H101 0.95 . ? C102 C103 1.417(15) . ? C102 H102 0.95 . ? C103 C104 1.394(13) . ? C103 H103 0.95 . ? C104 C105 1.432(14) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? Cl11 C01 1.61(8) . ? Cl12 C01 1.69(8) . ? C01 H01A 0.99 . ? C01 H01B 0.99 . ? 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 C3 Ru1 N52 76.2(3) . . ? C3 Ru1 C101 96.3(3) . . ? N52 Ru1 C101 132.1(3) . . ? C3 Ru1 C105 110.2(3) . . ? N52 Ru1 C105 100.6(3) . . ? C101 Ru1 C105 37.1(4) . . ? C3 Ru1 C102 116.4(4) . . ? N52 Ru1 C102 160.9(3) . . ? C101 Ru1 C102 37.2(4) . . ? C105 Ru1 C102 62.3(3) . . ? C3 Ru1 C104 147.1(4) . . ? N52 Ru1 C104 99.0(3) . . ? C101 Ru1 C104 62.5(3) . . ? C105 Ru1 C104 37.9(4) . . ? C102 Ru1 C104 62.5(3) . . ? C3 Ru1 C103 153.6(4) . . ? N52 Ru1 C103 128.8(3) . . ? C101 Ru1 C103 61.6(4) . . ? C105 Ru1 C103 61.7(4) . . ? C102 Ru1 C103 37.2(4) . . ? C104 Ru1 C103 36.6(3) . . ? C3 Ru1 P1 95.9(2) . . ? N52 Ru1 P1 88.94(19) . . ? C101 Ru1 P1 138.9(3) . . ? C105 Ru1 P1 153.7(3) . . ? C102 Ru1 P1 103.1(3) . . ? C104 Ru1 P1 116.7(3) . . ? C103 Ru1 P1 93.2(3) . . ? N55 Pt1 P2 89.81(18) . . ? N55 Pt1 P3 172.50(18) . . ? P2 Pt1 P3 96.47(7) . . ? N55 Pt1 Cl1 87.34(18) . . ? P2 Pt1 Cl1 175.68(8) . . ? P3 Pt1 Cl1 86.61(7) . . ? C2 C1 C12 122.6(8) . . ? C2 C1 C11 121.0(8) . . ? C12 C1 C11 116.3(8) . . ? N11 C11 C1 177.0(10) . . ? N12 C12 C1 177.1(11) . . ? C1 C2 C21 119.9(8) . . ? C1 C2 C3 121.2(8) . . ? C21 C2 C3 119.0(7) . . ? C22 C21 C26 118.4(9) . . ? C22 C21 C2 121.7(9) . . ? C26 C21 C2 119.9(8) . . ? C21 C22 C23 120.5(9) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 118.7(9) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 121.6(9) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C26 C25 C24 119.5(9) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C21 121.3(9) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C4 C3 C2 119.5(7) . . ? C4 C3 Ru1 118.7(6) . . ? C2 C3 Ru1 121.2(6) . . ? C3 C4 C51 112.8(7) . . ? C3 C4 C41 125.6(7) . . ? C51 C4 C41 121.6(7) . . ? N41 C41 C4 176.9(10) . . ? N55 C51 N52 108.5(7) . . ? N55 C51 C4 136.9(7) . . ? N52 C51 C4 114.5(7) . . ? N53 N52 C51 106.8(6) . . ? N53 N52 Ru1 135.7(5) . . ? C51 N52 Ru1 117.5(5) . . ? N54 N53 N52 108.3(6) . . ? N53 N54 N55 108.3(6) . . ? C51 N55 N54 107.9(6) . . ? C51 N55 Pt1 133.3(5) . . ? N54 N55 Pt1 118.2(5) . . ? C111 P1 C131 103.7(4) . . ? C111 P1 C121 101.8(4) . . ? C131 P1 C121 100.6(4) . . ? C111 P1 Ru1 112.0(3) . . ? C131 P1 Ru1 113.8(3) . . ? C121 P1 Ru1 122.6(3) . . ? C116 C111 C112 117.7(8) . . ? C116 C111 P1 123.3(7) . . ? C112 C111 P1 119.0(6) . . ? C113 C112 C111 121.5(8) . . ? C113 C112 H112 119.3 . . ? C111 C112 H112 119.3 . . ? C114 C113 C112 119.8(9) . . ? C114 C113 H113 120.1 . . ? C112 C113 H113 120.1 . . ? C113 C114 C115 120.2(8) . . ? C113 C114 H114 119.9 . . ? C115 C114 H114 119.9 . . ? C114 C115 C116 119.3(8) . . ? C114 C115 H115 120.3 . . ? C116 C115 H115 120.3 . . ? C111 C116 C115 121.4(9) . . ? C111 C116 H116 119.3 . . ? C115 C116 H116 119.3 . . ? C122 C121 C126 119.4(8) . . ? C122 C121 P1 123.7(7) . . ? C126 C121 P1 116.8(6) . . ? C121 C122 C123 121.5(8) . . ? C121 C122 H122 119.2 . . ? C123 C122 H122 119.2 . . ? C124 C123 C122 118.6(8) . . ? C124 C123 H123 120.7 . . ? C122 C123 H123 120.7 . . ? C123 C124 C125 120.7(8) . . ? C123 C124 H124 119.7 . . ? C125 C124 H124 119.7 . . ? C124 C125 C126 119.8(8) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C121 C126 C125 119.7(8) . . ? C121 C126 H126 120.1 . . ? C125 C126 H126 120.1 . . ? C132 C131 C136 118.4(8) . . ? C132 C131 P1 124.2(6) . . ? C136 C131 P1 117.3(7) . . ? C131 C132 C133 120.4(8) . . ? C131 C132 H132 119.8 . . ? C133 C132 H132 119.8 . . ? C134 C133 C132 120.9(9) . . ? C134 C133 H133 119.6 . . ? C132 C133 H133 119.6 . . ? C133 C134 C135 119.9(9) . . ? C133 C134 H134 120 . . ? C135 C134 H134 120 . . ? C134 C135 C136 120.0(9) . . ? C134 C135 H135 120 . . ? C136 C135 H135 120 . . ? C135 C136 C131 120.3(9) . . ? C135 C136 H136 119.9 . . ? C131 C136 H136 119.9 . . ? C231 P2 C221 115.7(4) . . ? C231 P2 C211 102.9(4) . . ? C221 P2 C211 101.1(3) . . ? C231 P2 Pt1 112.1(3) . . ? C221 P2 Pt1 110.4(3) . . ? C211 P2 Pt1 114.1(2) . . ? C212 C211 C216 117.3(8) . . ? C212 C211 P2 120.4(6) . . ? C216 C211 P2 122.3(6) . . ? C213 C212 C211 121.1(7) . . ? C213 C212 H212 119.5 . . ? C211 C212 H212 119.5 . . ? C212 C213 C214 121.6(8) . . ? C212 C213 H213 119.2 . . ? C214 C213 H213 119.2 . . ? C215 C214 C213 117.4(8) . . ? C215 C214 C217 120.3(7) . . ? C213 C214 C217 122.3(8) . . ? C214 C215 C216 121.6(8) . . ? C214 C215 H215 119.2 . . ? C216 C215 H215 119.2 . . ? C215 C216 C211 121.0(8) . . ? C215 C216 H216 119.5 . . ? C211 C216 H216 119.5 . . ? C214 C217 H21A 109.5 . . ? C214 C217 H21B 109.5 . . ? H21A C217 H21B 109.5 . . ? C214 C217 H21C 109.5 . . ? H21A C217 H21C 109.5 . . ? H21B C217 H21C 109.5 . . ? C226 C221 C222 118.7(7) . . ? C226 C221 P2 124.3(6) . . ? C222 C221 P2 116.8(6) . . ? C223 C222 C221 120.0(8) . . ? C223 C222 H222 120 . . ? C221 C222 H222 120 . . ? C224 C223 C222 121.2(8) . . ? C224 C223 H223 119.4 . . ? C222 C223 H223 119.4 . . ? C223 C224 C225 119.1(8) . . ? C223 C224 C227 119.3(7) . . ? C225 C224 C227 121.6(8) . . ? C224 C225 C226 120.2(8) . . ? C224 C225 H225 119.9 . . ? C226 C225 H225 119.9 . . ? C221 C226 C225 120.6(8) . . ? C221 C226 H226 119.7 . . ? C225 C226 H226 119.7 . . ? C224 C227 H22A 109.5 . . ? C224 C227 H22B 109.5 . . ? H22A C227 H22B 109.5 . . ? C224 C227 H22C 109.5 . . ? H22A C227 H22C 109.5 . . ? H22B C227 H22C 109.5 . . ? C236 C231 C232 118.3(8) . . ? C236 C231 P2 126.4(6) . . ? C232 C231 P2 114.7(6) . . ? C233 C232 C231 120.0(8) . . ? C233 C232 H232 120 . . ? C231 C232 H232 120 . . ? C234 C233 C232 121.9(8) . . ? C234 C233 H233 119.1 . . ? C232 C233 H233 119.1 . . ? C233 C234 C235 118.4(8) . . ? C233 C234 C237 120.9(8) . . ? C235 C234 C237 120.6(8) . . ? C236 C235 C234 120.2(8) . . ? C236 C235 H235 119.9 . . ? C234 C235 H235 119.9 . . ? C231 C236 C235 121.1(8) . . ? C231 C236 H236 119.5 . . ? C235 C236 H236 119.5 . . ? C234 C237 H23A 109.5 . . ? C234 C237 H23B 109.5 . . ? H23A C237 H23B 109.5 . . ? C234 C237 H23C 109.5 . . ? H23A C237 H23C 109.5 . . ? H23B C237 H23C 109.5 . . ? C331 P3 C321 104.0(4) . . ? C331 P3 C311 102.2(4) . . ? C321 P3 C311 108.2(4) . . ? C331 P3 Pt1 119.0(3) . . ? C321 P3 Pt1 113.1(3) . . ? C311 P3 Pt1 109.4(3) . . ? C316 C311 C312 118.4(8) . . ? C316 C311 P3 120.1(7) . . ? C312 C311 P3 121.5(6) . . ? C313 C312 C311 119.4(8) . . ? C313 C312 H312 120.3 . . ? C311 C312 H312 120.3 . . ? C314 C313 C312 122.2(9) . . ? C314 C313 H313 118.9 . . ? C312 C313 H313 118.9 . . ? C313 C314 C315 117.3(9) . . ? C313 C314 C317 121.4(10) . . ? C315 C314 C317 121.2(10) . . ? C316 C315 C314 122.2(9) . . ? C316 C315 H315 118.9 . . ? C314 C315 H315 118.9 . . ? C315 C316 C311 120.4(9) . . ? C315 C316 H316 119.8 . . ? C311 C316 H316 119.8 . . ? C314 C317 H31A 109.5 . . ? C314 C317 H31B 109.5 . . ? H31A C317 H31B 109.5 . . ? C314 C317 H31C 109.5 . . ? H31A C317 H31C 109.5 . . ? H31B C317 H31C 109.5 . . ? C322 C321 C326 120.3(7) . . ? C322 C321 P3 120.1(6) . . ? C326 C321 P3 119.6(7) . . ? C323 C322 C321 120.2(8) . . ? C323 C322 H322 119.9 . . ? C321 C322 H322 119.9 . . ? C322 C323 C324 122.2(9) . . ? C322 C323 H323 118.9 . . ? C324 C323 H323 118.9 . . ? C323 C324 C325 117.1(8) . . ? C323 C324 C327 122.3(9) . . ? C325 C324 C327 120.5(8) . . ? C326 C325 C324 120.9(8) . . ? C326 C325 H325 119.6 . . ? C324 C325 H325 119.6 . . ? C321 C326 C325 119.2(8) . . ? C321 C326 H326 120.4 . . ? C325 C326 H326 120.4 . . ? C324 C327 H32A 109.5 . . ? C324 C327 H32B 109.5 . . ? H32A C327 H32B 109.5 . . ? C324 C327 H32C 109.5 . . ? H32A C327 H32C 109.5 . . ? H32B C327 H32C 109.5 . . ? C332 C331 C336 118.0(7) . . ? C332 C331 P3 121.1(6) . . ? C336 C331 P3 120.8(6) . . ? C333 C332 C331 120.7(8) . . ? C333 C332 H332 119.7 . . ? C331 C332 H332 119.7 . . ? C334 C333 C332 122.3(8) . . ? C334 C333 H333 118.8 . . ? C332 C333 H333 118.8 . . ? C333 C334 C335 117.3(8) . . ? C333 C334 C337 120.1(8) . . ? C335 C334 C337 122.6(8) . . ? C336 C335 C334 120.6(8) . . ? C336 C335 H335 119.7 . . ? C334 C335 H335 119.7 . . ? C335 C336 C331 121.0(8) . . ? C335 C336 H336 119.5 . . ? C331 C336 H336 119.5 . . ? C334 C337 H33A 109.5 . . ? C334 C337 H33B 109.5 . . ? H33A C337 H33B 109.5 . . ? C334 C337 H33C 109.5 . . ? H33A C337 H33C 109.5 . . ? H33B C337 H33C 109.5 . . ? C105 C101 C102 109.5(9) . . ? C105 C101 Ru1 72.0(5) . . ? C102 C101 Ru1 72.5(6) . . ? C105 C101 H101 125.3 . . ? C102 C101 H101 125.3 . . ? Ru1 C101 H101 121.9 . . ? C101 C102 C103 106.5(9) . . ? C101 C102 Ru1 70.3(6) . . ? C103 C102 Ru1 71.9(5) . . ? C101 C102 H102 126.8 . . ? C103 C102 H102 126.8 . . ? Ru1 C102 H102 122.7 . . ? C104 C103 C102 109.6(9) . . ? C104 C103 Ru1 71.2(5) . . ? C102 C103 Ru1 70.8(5) . . ? C104 C103 H103 125.2 . . ? C102 C103 H103 125.2 . . ? Ru1 C103 H103 124.3 . . ? C103 C104 C105 106.7(9) . . ? C103 C104 Ru1 72.2(5) . . ? C105 C104 Ru1 70.4(5) . . ? C103 C104 H104 126.6 . . ? C105 C104 H104 126.6 . . ? Ru1 C104 H104 122.5 . . ? C101 C105 C104 107.7(9) . . ? C101 C105 Ru1 71.0(5) . . ? C104 C105 Ru1 71.7(5) . . ? C101 C105 H105 126.1 . . ? C104 C105 H105 126.1 . . ? Ru1 C105 H105 122.9 . . ? Cl11 C01 Cl12 113(5) . . ? Cl11 C01 H01A 109.1 . . ? Cl12 C01 H01A 109.1 . . ? Cl11 C01 H01B 109 . . ? Cl12 C01 H01B 109 . . ? H01A C01 H01B 107.8 . . ? #===END # Attachment '7.br1411.cif' data_br1411 _database_code_depnum_ccdc_archive 'CCDC 730748' _audit_creation_date 2008-04-22T09:44:10-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C38 H30 N7 O P Ru' _chemical_formula_moiety 'C38 H28 N7 P Ru, H2 O' _chemical_formula_weight 732.73 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall -P_2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.5236(3) _cell_length_b 13.7074(3) _cell_length_c 17.8548(3) _cell_angle_alpha 90 _cell_angle_beta 98.452(2) _cell_angle_gamma 90 _cell_volume 3273.86(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13569 _cell_measurement_theta_min 2.5218 _cell_measurement_theta_max 34.5689 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.09 _exptl_crystal_description spear _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.961 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0009 _diffrn_orient_matrix_ub_11 -0.0498982788 _diffrn_orient_matrix_ub_12 0.0145323183 _diffrn_orient_matrix_ub_13 -0.0134329221 _diffrn_orient_matrix_ub_21 -0.0119888436 _diffrn_orient_matrix_ub_22 -0.0037102222 _diffrn_orient_matrix_ub_23 0.0373773792 _diffrn_orient_matrix_ub_31 0.0137313669 _diffrn_orient_matrix_ub_32 0.0496332116 _diffrn_orient_matrix_ub_33 0.0066845429 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_unetI/netI 0.0964 _diffrn_reflns_number 52868 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 34.59 _diffrn_reflns_theta_full 33.5 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur diffractometer ; _diffrn_measurement_method '\w scans' _reflns_number_total 13247 _reflns_number_gt 8224 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 13247 _refine_ls_number_parameters 440 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0997 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.879 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.934 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.541232(12) 0.512227(12) 0.289807(9) 0.01625(5) Uani 1 1 d . . . C1 C 0.26048(16) 0.55134(16) 0.20112(12) 0.0205(4) Uani 1 1 d . . . C11 C 0.18805(17) 0.54164(18) 0.13327(13) 0.0253(5) Uani 1 1 d . . . N11 N 0.12954(16) 0.53321(17) 0.08065(13) 0.0358(5) Uani 1 1 d . . . C12 C 0.23422(16) 0.50748(16) 0.26884(13) 0.0224(4) Uani 1 1 d . . . N12 N 0.21350(16) 0.47394(16) 0.32308(12) 0.0323(5) Uani 1 1 d . . . C2 C 0.34829(15) 0.60009(15) 0.20174(12) 0.0171(4) Uani 1 1 d . . . C21 C 0.37112(15) 0.64910(15) 0.13170(11) 0.0175(4) Uani 1 1 d . . . C22 C 0.42387(17) 0.60116(17) 0.08179(13) 0.0243(5) Uani 1 1 d . . . H22 H 0.4457 0.536 0.0919 0.029 Uiso 1 1 calc R . . C23 C 0.44476(18) 0.64798(19) 0.01726(13) 0.0281(5) Uani 1 1 d . . . H23 H 0.48 0.6143 -0.0171 0.034 Uiso 1 1 calc R . . C24 C 0.41472(17) 0.74343(18) 0.00235(13) 0.0279(5) Uani 1 1 d . . . H24 H 0.4304 0.7757 -0.0415 0.033 Uiso 1 1 calc R . . C25 C 0.3619(2) 0.79139(18) 0.05169(14) 0.0317(6) Uani 1 1 d . . . H25 H 0.3406 0.8568 0.0416 0.038 Uiso 1 1 calc R . . C26 C 0.33987(19) 0.74433(17) 0.11584(13) 0.0278(5) Uani 1 1 d . . . H26 H 0.303 0.7776 0.1494 0.033 Uiso 1 1 calc R . . C3 C 0.42224(15) 0.60443(15) 0.27081(11) 0.0166(4) Uani 1 1 d . . . C4 C 0.40568(15) 0.66769(16) 0.32748(12) 0.0193(4) Uani 1 1 d . . . C41 C 0.32642(17) 0.73808(17) 0.32420(12) 0.0239(5) Uani 1 1 d . . . N41 N 0.26375(16) 0.79500(17) 0.32086(12) 0.0373(5) Uani 1 1 d . . . C51 C 0.47810(16) 0.65688(15) 0.39431(12) 0.0185(4) Uani 1 1 d . . . N52 N 0.54486(13) 0.58554(13) 0.39229(10) 0.0193(4) Uani 1 1 d . . . N53 N 0.60490(14) 0.58553(14) 0.46065(10) 0.0243(4) Uani 1 1 d . . . N54 N 0.57739(15) 0.65447(15) 0.50314(11) 0.0270(4) Uani 1 1 d . . . N55 N 0.49819(14) 0.70041(14) 0.46210(10) 0.0233(4) Uani 1 1 d . . . C55 C 0.4493(2) 0.78281(18) 0.49399(14) 0.0305(5) Uani 1 1 d . . . H55A H 0.4333 0.8332 0.4551 0.046 Uiso 1 1 calc R . . H55B H 0.4944 0.81 0.5369 0.046 Uiso 1 1 calc R . . H55C H 0.3877 0.7604 0.5113 0.046 Uiso 1 1 calc R . . P1 P 0.65673(4) 0.62650(4) 0.26035(3) 0.01674(11) Uani 1 1 d . . . C111 C 0.66954(15) 0.65020(16) 0.16099(12) 0.0200(4) Uani 1 1 d . . . C112 C 0.66266(16) 0.74215(17) 0.12732(13) 0.0235(5) Uani 1 1 d . . . H112 H 0.6494 0.7975 0.1563 0.028 Uiso 1 1 calc R . . C113 C 0.67494(18) 0.75408(18) 0.05182(13) 0.0279(5) Uani 1 1 d . . . H113 H 0.6689 0.8171 0.0295 0.034 Uiso 1 1 calc R . . C114 C 0.69579(18) 0.67481(19) 0.00923(14) 0.0307(5) Uani 1 1 d . . . H114 H 0.703 0.6829 -0.0425 0.037 Uiso 1 1 calc R . . C115 C 0.70608(19) 0.58383(19) 0.04224(14) 0.0312(6) Uani 1 1 d . . . H115 H 0.7235 0.5296 0.0137 0.037 Uiso 1 1 calc R . . C116 C 0.69121(18) 0.57091(18) 0.11691(13) 0.0269(5) Uani 1 1 d . . . H116 H 0.6958 0.5073 0.1383 0.032 Uiso 1 1 calc R . . C121 C 0.63878(15) 0.74625(15) 0.30146(12) 0.0182(4) Uani 1 1 d . . . C122 C 0.69507(16) 0.77274(16) 0.37055(12) 0.0215(4) Uani 1 1 d . . . H122 H 0.7499 0.7332 0.3916 0.026 Uiso 1 1 calc R . . C123 C 0.67223(17) 0.85552(17) 0.40869(14) 0.0273(5) Uani 1 1 d . . . H123 H 0.7098 0.871 0.4564 0.033 Uiso 1 1 calc R . . C124 C 0.59465(18) 0.91630(17) 0.37762(15) 0.0296(5) Uani 1 1 d . . . H124 H 0.5798 0.9738 0.4036 0.035 Uiso 1 1 calc R . . C125 C 0.53903(17) 0.89243(17) 0.30843(14) 0.0247(5) Uani 1 1 d . . . H125 H 0.4866 0.9343 0.2866 0.03 Uiso 1 1 calc R . . C126 C 0.55962(16) 0.80755(16) 0.27093(13) 0.0213(4) Uani 1 1 d . . . H126 H 0.5199 0.7909 0.2243 0.026 Uiso 1 1 calc R . . C131 C 0.78713(16) 0.59770(15) 0.30039(12) 0.0196(4) Uani 1 1 d . . . C132 C 0.86770(16) 0.63774(16) 0.27036(13) 0.0234(5) Uani 1 1 d . . . H132 H 0.8555 0.6787 0.2271 0.028 Uiso 1 1 calc R . . C133 C 0.96570(17) 0.61848(18) 0.30299(14) 0.0285(5) Uani 1 1 d . . . H133 H 1.0198 0.6469 0.2823 0.034 Uiso 1 1 calc R . . C134 C 0.98425(17) 0.55797(18) 0.36551(14) 0.0289(5) Uani 1 1 d . . . H134 H 1.0512 0.5443 0.3874 0.035 Uiso 1 1 calc R . . C135 C 0.90552(17) 0.51724(17) 0.39632(13) 0.0252(5) Uani 1 1 d . . . H135 H 0.9184 0.476 0.4394 0.03 Uiso 1 1 calc R . . C136 C 0.80689(16) 0.53711(16) 0.36379(13) 0.0222(5) Uani 1 1 d . . . H136 H 0.753 0.5092 0.385 0.027 Uiso 1 1 calc R . . C101 C 0.46479(17) 0.38186(16) 0.23655(14) 0.0263(5) Uani 1 1 d . . . H101 H 0.3988 0.3838 0.2096 0.032 Uiso 1 1 calc R . . C102 C 0.55378(18) 0.39609(16) 0.20461(13) 0.0251(5) Uani 1 1 d . . . H102 H 0.558 0.4096 0.153 0.03 Uiso 1 1 calc R . . C103 C 0.63673(17) 0.38626(16) 0.26511(13) 0.0230(5) Uani 1 1 d . . . H103 H 0.7056 0.3916 0.2604 0.028 Uiso 1 1 calc R . . C104 C 0.59676(18) 0.36722(16) 0.33279(13) 0.0257(5) Uani 1 1 d . . . H104 H 0.6345 0.358 0.3815 0.031 Uiso 1 1 calc R . . C105 C 0.49037(18) 0.36421(16) 0.31555(14) 0.0269(5) Uani 1 1 d . . . H105 H 0.445 0.3526 0.3504 0.032 Uiso 1 1 calc R . . O1 O 0.71440(19) 0.42168(16) 0.53004(13) 0.0583(6) Uani 1 1 d D . . H1A H 0.678(3) 0.477(2) 0.5059(18) 0.087 Uiso 1 1 d D . . H1B H 0.742(3) 0.444(3) 0.5794(12) 0.087 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ru1 0.01551(8) 0.01735(8) 0.01592(7) 0.00230(7) 0.00240(5) 0.00133(7) C1 0.0188(10) 0.0236(11) 0.0192(10) 0.0021(8) 0.0035(8) -0.0013(9) C11 0.0211(11) 0.0298(12) 0.0256(12) 0.0043(9) 0.0051(9) -0.0059(9) N11 0.0288(12) 0.0472(14) 0.0304(12) 0.0071(10) 0.0012(9) -0.0097(10) C12 0.0152(10) 0.0254(12) 0.0263(11) -0.0002(9) 0.0021(8) -0.0045(9) N12 0.0286(11) 0.0376(12) 0.0316(11) 0.0060(9) 0.0079(9) -0.0062(9) C2 0.0147(10) 0.0165(10) 0.0202(10) 0.0018(8) 0.0030(8) 0.0037(7) C21 0.0148(10) 0.0212(10) 0.0160(10) 0.0006(8) 0.0005(7) -0.0026(8) C22 0.0263(12) 0.0253(11) 0.0214(11) 0.0029(9) 0.0037(9) 0.0055(9) C23 0.0252(12) 0.0404(14) 0.0192(11) 0.0008(10) 0.0053(9) 0.0038(10) C24 0.0246(12) 0.0388(14) 0.0188(11) 0.0085(10) -0.0016(9) -0.0080(10) C25 0.0413(15) 0.0253(12) 0.0268(13) 0.0071(10) -0.0007(11) 0.0004(11) C26 0.0360(14) 0.0253(12) 0.0230(12) 0.0023(9) 0.0073(10) 0.0041(10) C3 0.0149(10) 0.0185(10) 0.0171(10) 0.0036(8) 0.0052(7) -0.0017(8) C4 0.0144(10) 0.0271(11) 0.0167(10) 0.0036(8) 0.0036(8) -0.0010(8) C41 0.0235(12) 0.0305(12) 0.0185(11) 0.0000(9) 0.0059(9) 0.0036(9) N41 0.0352(13) 0.0477(14) 0.0298(12) 0.0008(10) 0.0071(9) 0.0161(11) C51 0.0193(10) 0.0201(10) 0.0170(10) -0.0004(8) 0.0053(8) -0.0013(8) N52 0.0184(9) 0.0242(9) 0.0151(8) 0.0032(7) 0.0019(7) 0.0015(7) N53 0.0260(10) 0.0295(10) 0.0163(9) 0.0012(7) -0.0007(7) 0.0026(8) N54 0.0287(11) 0.0336(11) 0.0180(9) 0.0013(8) 0.0015(8) 0.0038(9) N55 0.0248(10) 0.0280(10) 0.0175(9) 0.0008(7) 0.0042(7) 0.0017(8) C55 0.0365(14) 0.0321(13) 0.0242(12) -0.0044(10) 0.0091(10) 0.0056(11) P1 0.0143(3) 0.0195(3) 0.0164(3) 0.0011(2) 0.00222(19) 0.0010(2) C111 0.0159(10) 0.0268(11) 0.0177(10) 0.0013(8) 0.0036(8) -0.0020(8) C112 0.0212(11) 0.0257(12) 0.0231(11) 0.0011(9) 0.0019(8) -0.0051(9) C113 0.0295(13) 0.0317(13) 0.0225(12) 0.0063(10) 0.0035(9) -0.0060(10) C114 0.0295(13) 0.0436(15) 0.0204(11) 0.0055(10) 0.0083(9) -0.0043(11) C115 0.0340(14) 0.0378(14) 0.0233(12) -0.0041(10) 0.0088(10) 0.0010(11) C116 0.0295(13) 0.0254(12) 0.0270(12) 0.0009(9) 0.0081(10) 0.0011(10) C121 0.0154(10) 0.0191(10) 0.0207(10) 0.0027(8) 0.0045(8) -0.0015(8) C122 0.0177(11) 0.0227(11) 0.0236(11) 0.0001(9) 0.0011(8) -0.0002(8) C123 0.0243(12) 0.0299(13) 0.0266(12) -0.0084(10) 0.0003(9) -0.0022(10) C124 0.0290(13) 0.0212(12) 0.0399(15) -0.0046(10) 0.0098(11) -0.0001(9) C125 0.0188(11) 0.0207(11) 0.0349(13) 0.0050(9) 0.0049(9) 0.0019(9) C126 0.0166(10) 0.0231(11) 0.0239(11) 0.0038(8) 0.0019(8) -0.0007(8) C131 0.0169(10) 0.0195(10) 0.0221(11) -0.0020(8) 0.0012(8) 0.0020(8) C132 0.0209(11) 0.0199(11) 0.0296(12) 0.0002(9) 0.0040(9) 0.0007(9) C133 0.0179(11) 0.0290(13) 0.0394(14) -0.0067(11) 0.0065(10) -0.0014(9) C134 0.0178(11) 0.0306(13) 0.0368(14) -0.0085(11) -0.0016(10) 0.0054(9) C135 0.0224(11) 0.0247(11) 0.0265(11) 0.0008(9) -0.0024(9) 0.0038(9) C136 0.0177(11) 0.0257(12) 0.0229(11) 0.0013(9) 0.0027(8) 0.0009(8) C101 0.0230(12) 0.0162(11) 0.0378(13) -0.0035(9) -0.0016(10) -0.0017(9) C102 0.0360(13) 0.0175(11) 0.0216(11) -0.0024(8) 0.0036(9) 0.0026(9) C103 0.0226(11) 0.0209(11) 0.0255(11) -0.0006(9) 0.0034(9) 0.0074(9) C104 0.0344(13) 0.0188(11) 0.0240(12) 0.0052(9) 0.0040(10) 0.0062(9) C105 0.0318(13) 0.0188(11) 0.0324(13) 0.0038(9) 0.0121(10) -0.0042(9) O1 0.0820(18) 0.0530(14) 0.0406(13) 0.0023(10) 0.0114(12) 0.0231(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.035(2) . ? Ru1 N52 2.0819(18) . ? Ru1 C101 2.208(2) . ? Ru1 C105 2.212(2) . ? Ru1 C104 2.221(2) . ? Ru1 C102 2.225(2) . ? Ru1 C103 2.239(2) . ? Ru1 P1 2.3262(6) . ? C1 C2 1.361(3) . ? C1 C12 1.441(3) . ? C1 C11 1.448(3) . ? C11 N11 1.142(3) . ? C12 N12 1.144(3) . ? C2 C3 1.470(3) . ? C2 C21 1.491(3) . ? C21 C22 1.386(3) . ? C21 C26 1.388(3) . ? C22 C23 1.384(3) . ? C22 H22 0.95 . ? C23 C24 1.384(3) . ? C23 H23 0.95 . ? C24 C25 1.380(4) . ? C24 H24 0.95 . ? C25 C26 1.385(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.376(3) . ? C4 C51 1.436(3) . ? C4 C41 1.437(3) . ? C41 N41 1.147(3) . ? C51 N52 1.335(3) . ? C51 N55 1.341(3) . ? N52 N53 1.363(2) . ? N53 N54 1.300(3) . ? N54 N55 1.360(3) . ? N55 C55 1.465(3) . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? P1 C121 1.829(2) . ? P1 C111 1.837(2) . ? P1 C131 1.846(2) . ? C111 C112 1.394(3) . ? C111 C116 1.398(3) . ? C112 C113 1.392(3) . ? C112 H112 0.95 . ? C113 C114 1.379(3) . ? C113 H113 0.95 . ? C114 C115 1.378(4) . ? C114 H114 0.95 . ? C115 C116 1.388(3) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.399(3) . ? C121 C126 1.406(3) . ? C122 C123 1.381(3) . ? C122 H122 0.95 . ? C123 C124 1.390(3) . ? C123 H123 0.95 . ? C124 C125 1.388(3) . ? C124 H124 0.95 . ? C125 C126 1.391(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C132 1.396(3) . ? C131 C136 1.398(3) . ? C132 C133 1.392(3) . ? C132 H132 0.95 . ? C133 C134 1.384(4) . ? C133 H133 0.95 . ? C134 C135 1.386(3) . ? C134 H134 0.95 . ? C135 C136 1.401(3) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C101 C102 1.419(3) . ? C101 C105 1.423(3) . ? C101 H101 0.95 . ? C102 C103 1.445(3) . ? C102 H102 0.95 . ? C103 C104 1.419(3) . ? C103 H103 0.95 . ? C104 C105 1.427(3) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? O1 H1A 0.966(17) . ? O1 H1B 0.957(18) . ? 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 C3 Ru1 N52 76.27(8) . . ? C3 Ru1 C101 97.02(8) . . ? N52 Ru1 C101 135.90(8) . . ? C3 Ru1 C105 109.99(8) . . ? N52 Ru1 C105 103.18(8) . . ? C101 Ru1 C105 37.55(9) . . ? C3 Ru1 C104 146.32(9) . . ? N52 Ru1 C104 99.50(8) . . ? C101 Ru1 C104 62.47(9) . . ? C105 Ru1 C104 37.55(9) . . ? C3 Ru1 C102 117.92(8) . . ? N52 Ru1 C102 162.12(8) . . ? C101 Ru1 C102 37.33(9) . . ? C105 Ru1 C102 62.82(9) . . ? C104 Ru1 C102 62.63(8) . . ? C3 Ru1 C103 155.66(8) . . ? N52 Ru1 C103 127.28(7) . . ? C101 Ru1 C103 62.49(9) . . ? C105 Ru1 C103 62.58(9) . . ? C104 Ru1 C103 37.10(8) . . ? C102 Ru1 C103 37.76(8) . . ? C3 Ru1 P1 94.87(6) . . ? N52 Ru1 P1 86.78(5) . . ? C101 Ru1 P1 137.30(7) . . ? C105 Ru1 P1 154.71(7) . . ? C104 Ru1 P1 118.46(7) . . ? C102 Ru1 P1 101.89(7) . . ? C103 Ru1 P1 92.80(6) . . ? C2 C1 C12 121.35(19) . . ? C2 C1 C11 122.3(2) . . ? C12 C1 C11 116.36(19) . . ? N11 C11 C1 178.6(3) . . ? N12 C12 C1 179.0(3) . . ? C1 C2 C3 120.78(19) . . ? C1 C2 C21 120.14(18) . . ? C3 C2 C21 119.08(17) . . ? C22 C21 C26 119.0(2) . . ? C22 C21 C2 121.00(19) . . ? C26 C21 C2 120.0(2) . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 119.5(2) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120 . . ? C26 C25 H25 120 . . ? C25 C26 C21 120.7(2) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C4 C3 C2 118.58(18) . . ? C4 C3 Ru1 118.62(15) . . ? C2 C3 Ru1 122.57(15) . . ? C3 C4 C51 112.42(19) . . ? C3 C4 C41 126.46(19) . . ? C51 C4 C41 121.12(19) . . ? N41 C41 C4 179.1(3) . . ? N52 C51 N55 107.59(18) . . ? N52 C51 C4 115.76(18) . . ? N55 C51 C4 136.7(2) . . ? C51 N52 N53 106.99(17) . . ? C51 N52 Ru1 116.66(13) . . ? N53 N52 Ru1 136.14(14) . . ? N54 N53 N52 109.79(18) . . ? N53 N54 N55 107.01(18) . . ? C51 N55 N54 108.62(18) . . ? C51 N55 C55 130.59(19) . . ? N54 N55 C55 120.79(19) . . ? N55 C55 H55A 109.5 . . ? N55 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N55 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C121 P1 C111 105.42(10) . . ? C121 P1 C131 102.25(10) . . ? C111 P1 C131 101.04(10) . . ? C121 P1 Ru1 112.37(7) . . ? C111 P1 Ru1 119.95(7) . . ? C131 P1 Ru1 113.79(7) . . ? C112 C111 C116 117.8(2) . . ? C112 C111 P1 124.53(17) . . ? C116 C111 P1 117.63(17) . . ? C113 C112 C111 120.9(2) . . ? C113 C112 H112 119.5 . . ? C111 C112 H112 119.5 . . ? C114 C113 C112 120.3(2) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 119.6(2) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 120.4(2) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C115 C116 C111 120.9(2) . . ? C115 C116 H116 119.6 . . ? C111 C116 H116 119.6 . . ? C122 C121 C126 118.1(2) . . ? C122 C121 P1 119.99(16) . . ? C126 C121 P1 121.27(16) . . ? C123 C122 C121 121.0(2) . . ? C123 C122 H122 119.5 . . ? C121 C122 H122 119.5 . . ? C122 C123 C124 120.4(2) . . ? C122 C123 H123 119.8 . . ? C124 C123 H123 119.8 . . ? C125 C124 C123 119.5(2) . . ? C125 C124 H124 120.2 . . ? C123 C124 H124 120.2 . . ? C124 C125 C126 120.3(2) . . ? C124 C125 H125 119.8 . . ? C126 C125 H125 119.8 . . ? C125 C126 C121 120.5(2) . . ? C125 C126 H126 119.7 . . ? C121 C126 H126 119.7 . . ? C132 C131 C136 118.5(2) . . ? C132 C131 P1 121.50(17) . . ? C136 C131 P1 119.93(17) . . ? C133 C132 C131 120.9(2) . . ? C133 C132 H132 119.5 . . ? C131 C132 H132 119.5 . . ? C134 C133 C132 120.0(2) . . ? C134 C133 H133 120 . . ? C132 C133 H133 120 . . ? C133 C134 C135 120.2(2) . . ? C133 C134 H134 119.9 . . ? C135 C134 H134 119.9 . . ? C134 C135 C136 119.8(2) . . ? C134 C135 H135 120.1 . . ? C136 C135 H135 120.1 . . ? C131 C136 C135 120.5(2) . . ? C131 C136 H136 119.7 . . ? C135 C136 H136 119.7 . . ? C102 C101 C105 108.9(2) . . ? C102 C101 Ru1 71.99(12) . . ? C105 C101 Ru1 71.36(13) . . ? C102 C101 H101 125.5 . . ? C105 C101 H101 125.5 . . ? Ru1 C101 H101 122.8 . . ? C101 C102 C103 107.3(2) . . ? C101 C102 Ru1 70.69(13) . . ? C103 C102 Ru1 71.61(12) . . ? C101 C102 H102 126.3 . . ? C103 C102 H102 126.3 . . ? Ru1 C102 H102 123 . . ? C104 C103 C102 107.6(2) . . ? C104 C103 Ru1 70.79(13) . . ? C102 C103 Ru1 70.62(12) . . ? C104 C103 H103 126.2 . . ? C102 C103 H103 126.2 . . ? Ru1 C103 H103 124 . . ? C103 C104 C105 108.6(2) . . ? C103 C104 Ru1 72.12(12) . . ? C105 C104 Ru1 70.87(12) . . ? C103 C104 H104 125.7 . . ? C105 C104 H104 125.7 . . ? Ru1 C104 H104 123 . . ? C101 C105 C104 107.4(2) . . ? C101 C105 Ru1 71.09(13) . . ? C104 C105 Ru1 71.57(13) . . ? C101 C105 H105 126.3 . . ? C104 C105 H105 126.3 . . ? Ru1 C105 H105 122.7 . . ? H1A O1 H1B 105(2) . . ? #===END # Attachment '9.br1442.cif' data_br1442 _database_code_depnum_ccdc_archive 'CCDC 730749' _audit_creation_date 2008-11-25T08:46:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C41 H34 N7 O2 P Ru' _chemical_formula_moiety 'C41 H34 N7 O2 P Ru' _chemical_formula_weight 788.79 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.3947(2) _cell_length_b 17.7047(3) _cell_length_c 17.1249(3) _cell_angle_alpha 90 _cell_angle_beta 97.322(2) _cell_angle_gamma 90 _cell_volume 3727.32(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11274 _cell_measurement_theta_min 3.2874 _cell_measurement_theta_max 32.516 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.874 _exptl_absorpt_correction_T_max .95 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 10.4738 _diffrn_orient_matrix_ub_11 -0.0297476159 _diffrn_orient_matrix_ub_12 -0.0188938048 _diffrn_orient_matrix_ub_13 -0.0323725579 _diffrn_orient_matrix_ub_21 -0.0186111522 _diffrn_orient_matrix_ub_22 -0.0267383955 _diffrn_orient_matrix_ub_23 0.0261223475 _diffrn_orient_matrix_ub_31 -0.0458102312 _diffrn_orient_matrix_ub_32 0.0230826718 _diffrn_orient_matrix_ub_33 0.0037337304 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_unetI/netI 0.1046 _diffrn_reflns_number 42565 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 32.6 _diffrn_reflns_theta_full 31 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.931 _diffrn_measurement_device_type ; Oxford Diffraction Gemini diffractometer ; _diffrn_measurement_method '\f and \w scans' _reflns_number_total 12675 _reflns_number_gt 7571 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics xtal-Ortep _computing_publication_material WinGX #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+0.0000P] 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_number_reflns 12675 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.936 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 0.867342(13) 0.764064(9) 0.561222(9) 0.01601(4) Uani 1 1 d . . . P1 P 0.71831(4) 0.69031(3) 0.58079(3) 0.01603(10) Uani 1 1 d . . . C111 C 0.67424(15) 0.70333(11) 0.67818(11) 0.0194(4) Uani 1 1 d . . . C112 C 0.64888(16) 0.77610(11) 0.70173(11) 0.0219(4) Uani 1 1 d . . . H112 H 0.6533 0.8173 0.6668 0.026 Uiso 1 1 calc R . . C113 C 0.61744(17) 0.78887(12) 0.77533(12) 0.0250(5) Uani 1 1 d . . . H113 H 0.5992 0.8385 0.7903 0.03 Uiso 1 1 calc R . . C114 C 0.61264(17) 0.72921(13) 0.82722(12) 0.0286(5) Uani 1 1 d . . . H114 H 0.5918 0.7378 0.878 0.034 Uiso 1 1 calc R . . C115 C 0.63827(17) 0.65739(13) 0.80466(12) 0.0308(5) Uani 1 1 d . . . H115 H 0.6355 0.6166 0.8404 0.037 Uiso 1 1 calc R . . C116 C 0.66799(17) 0.64388(12) 0.73072(12) 0.0258(5) Uani 1 1 d . . . H116 H 0.6842 0.5939 0.7157 0.031 Uiso 1 1 calc R . . C121 C 0.59402(15) 0.70086(10) 0.51137(11) 0.0171(4) Uani 1 1 d . . . C122 C 0.59568(16) 0.67393(11) 0.43492(11) 0.0204(4) Uani 1 1 d . . . H122 H 0.6572 0.6466 0.4224 0.024 Uiso 1 1 calc R . . C123 C 0.50873(17) 0.68660(12) 0.37713(12) 0.0251(5) Uani 1 1 d . . . H123 H 0.5114 0.6687 0.3251 0.03 Uiso 1 1 calc R . . C124 C 0.41798(17) 0.72523(11) 0.39504(12) 0.0258(5) Uani 1 1 d . . . H124 H 0.359 0.7348 0.3551 0.031 Uiso 1 1 calc R . . C125 C 0.41323(17) 0.74986(10) 0.47098(12) 0.0245(5) Uani 1 1 d . . . H125 H 0.3499 0.7748 0.4837 0.029 Uiso 1 1 calc R . . C126 C 0.50153(15) 0.73816(11) 0.52920(11) 0.0205(4) Uani 1 1 d . . . H126 H 0.4983 0.7558 0.5812 0.025 Uiso 1 1 calc R . . C131 C 0.74029(17) 0.58821(10) 0.57403(11) 0.0206(4) Uani 1 1 d . . . C132 C 0.65244(18) 0.53781(11) 0.56396(13) 0.0290(5) Uani 1 1 d . . . H132 H 0.5803 0.5566 0.5612 0.035 Uiso 1 1 calc R . . C133 C 0.6698(2) 0.46136(12) 0.55805(15) 0.0384(6) Uani 1 1 d . . . H133 H 0.6095 0.4278 0.5512 0.046 Uiso 1 1 calc R . . C134 C 0.7742(2) 0.43313(13) 0.56206(14) 0.0393(6) Uani 1 1 d . . . H134 H 0.7856 0.3803 0.5579 0.047 Uiso 1 1 calc R . . C135 C 0.8615(2) 0.48136(12) 0.57211(14) 0.0346(6) Uani 1 1 d . . . H135 H 0.9335 0.4621 0.575 0.042 Uiso 1 1 calc R . . C136 C 0.84393(18) 0.55894(12) 0.57801(12) 0.0273(5) Uani 1 1 d . . . H136 H 0.9045 0.5922 0.5849 0.033 Uiso 1 1 calc R . . C1 C 0.81636(16) 0.97094(10) 0.47892(11) 0.0176(4) Uani 1 1 d . . . C11 C 0.79670(16) 1.04946(11) 0.49526(11) 0.0190(4) Uani 1 1 d . . . N11 N 0.78181(14) 1.11248(9) 0.50381(10) 0.0240(4) Uani 1 1 d . . . C12 C 0.90277(17) 0.95918(11) 0.43184(12) 0.0214(4) Uani 1 1 d . . . N12 N 0.97410(16) 0.95438(10) 0.39578(11) 0.0313(4) Uani 1 1 d . . . C2 C 0.75825(15) 0.91334(10) 0.50577(10) 0.0164(4) Uani 1 1 d . . . C21 C 0.67773(16) 0.93091(10) 0.56036(11) 0.0188(4) Uani 1 1 d . . . C22 C 0.71071(18) 0.96767(11) 0.63154(12) 0.0269(5) Uani 1 1 d . . . H22 H 0.7848 0.9814 0.645 0.032 Uiso 1 1 calc R . . C23 C 0.6362(2) 0.98410(12) 0.68253(14) 0.0354(6) Uani 1 1 d . . . H23 H 0.6594 1.0084 0.7313 0.042 Uiso 1 1 calc R . . C24 C 0.5281(2) 0.96530(12) 0.66276(15) 0.0360(6) Uani 1 1 d . . . H24 H 0.4769 0.9768 0.6978 0.043 Uiso 1 1 calc R . . C25 C 0.49432(18) 0.92981(12) 0.59226(14) 0.0308(5) Uani 1 1 d . . . H25 H 0.4198 0.9172 0.5787 0.037 Uiso 1 1 calc R . . C26 C 0.56874(16) 0.91242(11) 0.54091(12) 0.0228(4) Uani 1 1 d . . . H26 H 0.5451 0.8878 0.4924 0.027 Uiso 1 1 calc R . . C3 C 0.78151(15) 0.83568(10) 0.48394(11) 0.0161(4) Uani 1 1 d . . . C4 C 0.75957(15) 0.81310(10) 0.40567(11) 0.0176(4) Uani 1 1 d . . . C41 C 0.69639(17) 0.85513(11) 0.34472(11) 0.0214(4) Uani 1 1 d . . . N41 N 0.64484(15) 0.88885(10) 0.29622(10) 0.0318(4) Uani 1 1 d . . . C51 C 0.81211(15) 0.74302(10) 0.39134(10) 0.0169(4) Uani 1 1 d . . . N52 N 0.87224(13) 0.71278(8) 0.45392(9) 0.0175(3) Uani 1 1 d . . . N53 N 0.92193(13) 0.64996(9) 0.42894(10) 0.0221(4) Uani 1 1 d . . . N54 N 0.89365(14) 0.64105(9) 0.35441(10) 0.0254(4) Uani 1 1 d . . . N55 N 0.82449(13) 0.69864(9) 0.32914(9) 0.0215(4) Uani 1 1 d . . . C01 C 0.8511(2) 0.80427(16) 0.19777(14) 0.0469(7) Uani 1 1 d . . . H01A H 0.7801 0.8294 0.1903 0.07 Uiso 1 1 calc R . . H01B H 0.8937 0.8199 0.1561 0.07 Uiso 1 1 calc R . . H01C H 0.89 0.8183 0.2492 0.07 Uiso 1 1 calc R . . O02 O 0.83577(14) 0.72411(10) 0.19451(9) 0.0410(4) Uani 1 1 d . . . C03 C 0.76891(19) 0.69770(13) 0.24731(12) 0.0309(5) Uani 1 1 d . . . H03 H 0.7017 0.7294 0.2438 0.037 Uiso 1 1 calc R . . C04 C 0.7376(2) 0.61528(15) 0.22684(14) 0.0433(7) Uani 1 1 d . . . H04A H 0.6996 0.612 0.1725 0.052 Uiso 1 1 calc R . . H04B H 0.8035 0.5833 0.2306 0.052 Uiso 1 1 calc R . . O05 O 0.66789(15) 0.59055(10) 0.28180(11) 0.0534(5) Uani 1 1 d . . . C06 C 0.6665(3) 0.51135(16) 0.29341(19) 0.0720(10) Uani 1 1 d . . . H06A H 0.651 0.486 0.2424 0.108 Uiso 1 1 calc R . . H06B H 0.61 0.4985 0.3263 0.108 Uiso 1 1 calc R . . H06C H 0.7375 0.4948 0.3196 0.108 Uiso 1 1 calc R . . C101 C 0.97102(17) 0.84989(12) 0.62565(12) 0.0270(5) Uani 1 1 d . . . H101 H 0.9669 0.902 0.6124 0.032 Uiso 1 1 calc R . . C102 C 0.91024(17) 0.81319(12) 0.67935(11) 0.0248(5) Uani 1 1 d . . . H102 H 0.8571 0.8356 0.7074 0.03 Uiso 1 1 calc R . . C103 C 0.94438(16) 0.73599(12) 0.68313(11) 0.0258(5) Uani 1 1 d . . . H103 H 0.9182 0.6981 0.7151 0.031 Uiso 1 1 calc R . . C104 C 1.02261(16) 0.72540(12) 0.63201(12) 0.0272(5) Uani 1 1 d . . . H104 H 1.0586 0.6793 0.6234 0.033 Uiso 1 1 calc R . . C105 C 1.03887(17) 0.79609(13) 0.59502(12) 0.0282(5) Uani 1 1 d . . . H105 H 1.0865 0.8053 0.5568 0.034 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 0.01579(8) 0.01731(7) 0.01433(7) 0.00140(7) -0.00038(5) -0.00122(7) P1 0.0165(3) 0.0158(2) 0.0154(2) 0.00180(19) 0.0004(2) -0.00003(19) C111 0.0145(10) 0.0256(11) 0.0176(10) 0.0038(8) 0.0003(8) -0.0013(8) C112 0.0205(10) 0.0273(12) 0.0177(9) 0.0039(8) 0.0011(8) -0.0031(8) C113 0.0220(11) 0.0329(12) 0.0201(10) -0.0035(9) 0.0026(9) 0.0003(9) C114 0.0229(11) 0.0459(14) 0.0182(10) 0.0032(10) 0.0073(9) -0.0002(10) C115 0.0306(13) 0.0385(14) 0.0245(11) 0.0138(10) 0.0078(10) 0.0010(10) C116 0.0242(12) 0.0281(12) 0.0257(11) 0.0081(9) 0.0046(9) 0.0032(9) C121 0.0171(10) 0.0142(9) 0.0195(10) 0.0035(7) 0.0005(8) -0.0024(7) C122 0.0161(10) 0.0239(11) 0.0209(10) 0.0003(8) 0.0017(8) -0.0009(8) C123 0.0241(12) 0.0288(12) 0.0211(10) 0.0011(8) -0.0017(9) -0.0058(9) C124 0.0198(11) 0.0248(12) 0.0299(11) 0.0053(9) -0.0080(9) -0.0015(9) C125 0.0201(10) 0.0179(12) 0.0344(12) 0.0007(8) -0.0009(9) 0.0048(8) C126 0.0217(10) 0.0161(9) 0.0231(10) -0.0011(8) 0.0012(8) -0.0008(8) C131 0.0239(11) 0.0168(10) 0.0206(10) 0.0054(8) 0.0003(9) 0.0019(8) C132 0.0263(12) 0.0208(11) 0.0389(13) 0.0057(9) -0.0002(10) -0.0002(9) C133 0.0395(15) 0.0208(12) 0.0526(16) 0.0045(11) -0.0031(12) -0.0048(10) C134 0.0493(16) 0.0188(12) 0.0486(15) 0.0039(10) 0.0020(13) 0.0055(11) C135 0.0341(13) 0.0234(11) 0.0461(15) 0.0060(10) 0.0043(11) 0.0110(10) C136 0.0273(12) 0.0233(11) 0.0309(12) 0.0046(9) 0.0022(10) 0.0040(9) C1 0.0195(10) 0.0166(10) 0.0169(9) 0.0009(7) 0.0030(8) 0.0016(8) C11 0.0160(10) 0.0233(11) 0.0179(10) 0.0027(8) 0.0027(8) -0.0015(8) N11 0.0267(10) 0.0195(9) 0.0269(9) 0.0007(7) 0.0071(8) 0.0004(7) C12 0.0243(11) 0.0163(10) 0.0235(11) 0.0007(8) 0.0024(9) -0.0004(8) N12 0.0311(11) 0.0272(10) 0.0380(11) -0.0020(8) 0.0136(9) -0.0002(8) C2 0.0170(10) 0.0183(10) 0.0131(9) 0.0001(7) -0.0008(8) 0.0005(7) C21 0.0242(11) 0.0114(9) 0.0216(10) 0.0013(7) 0.0069(9) 0.0009(8) C22 0.0294(12) 0.0238(11) 0.0290(11) -0.0073(9) 0.0099(10) -0.0099(9) C23 0.0483(16) 0.0290(12) 0.0335(13) -0.0113(10) 0.0231(12) -0.0106(11) C24 0.0396(15) 0.0251(12) 0.0488(15) -0.0026(11) 0.0270(12) 0.0014(10) C25 0.0214(12) 0.0265(12) 0.0457(14) 0.0096(10) 0.0093(11) 0.0041(9) C26 0.0227(11) 0.0197(10) 0.0256(11) 0.0061(8) 0.0015(9) 0.0008(8) C3 0.0140(9) 0.0168(9) 0.0182(9) 0.0004(7) 0.0038(8) -0.0028(7) C4 0.0182(10) 0.0186(10) 0.0156(9) 0.0010(7) 0.0009(8) 0.0005(8) C41 0.0259(11) 0.0216(11) 0.0168(10) -0.0043(8) 0.0039(9) 0.0041(8) N41 0.0380(12) 0.0339(11) 0.0224(9) 0.0010(8) 0.0001(9) 0.0125(9) C51 0.0155(9) 0.0192(10) 0.0163(9) -0.0005(8) 0.0029(8) -0.0002(7) N52 0.0168(9) 0.0167(8) 0.0195(8) 0.0016(6) 0.0041(7) 0.0017(6) N53 0.0207(9) 0.0218(9) 0.0242(9) -0.0016(7) 0.0047(8) 0.0044(7) N54 0.0248(10) 0.0249(9) 0.0264(9) -0.0027(7) 0.0031(8) 0.0083(7) N55 0.0224(9) 0.0240(9) 0.0178(8) -0.0028(7) 0.0015(7) 0.0058(7) C01 0.0510(17) 0.0559(19) 0.0373(15) 0.0111(13) 0.0189(13) 0.0131(14) O02 0.0455(10) 0.0563(12) 0.0225(8) -0.0014(8) 0.0095(8) 0.0142(9) C03 0.0295(13) 0.0428(14) 0.0198(11) -0.0082(10) 0.0012(10) 0.0113(10) C04 0.0394(15) 0.0558(17) 0.0336(14) -0.0118(12) 0.0001(12) 0.0107(13) O05 0.0523(12) 0.0497(12) 0.0595(12) -0.0107(9) 0.0123(10) 0.0019(9) C06 0.098(3) 0.0391(17) 0.081(2) -0.0212(16) 0.017(2) -0.0083(17) C101 0.0290(12) 0.0233(11) 0.0253(11) -0.0005(9) -0.0103(10) -0.0074(9) C102 0.0235(11) 0.0327(12) 0.0163(10) -0.0032(9) -0.0041(9) -0.0019(9) C103 0.0247(11) 0.0318(11) 0.0181(10) 0.0049(9) -0.0079(9) -0.0068(10) C104 0.0178(10) 0.0294(13) 0.0315(12) -0.0004(9) -0.0071(9) 0.0011(9) C105 0.0179(11) 0.0425(13) 0.0233(11) 0.0022(10) -0.0010(9) -0.0096(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C3 2.0327(18) . ? Ru1 N52 2.0574(15) . ? Ru1 C101 2.1946(19) . ? Ru1 C102 2.2039(19) . ? Ru1 C105 2.205(2) . ? Ru1 C103 2.2381(18) . ? Ru1 C104 2.2467(19) . ? Ru1 P1 2.3211(5) . ? P1 C121 1.8317(19) . ? P1 C131 1.8339(19) . ? P1 C111 1.834(2) . ? C111 C116 1.393(3) . ? C111 C112 1.398(3) . ? C112 C113 1.384(3) . ? C112 H112 0.95 . ? C113 C114 1.387(3) . ? C113 H113 0.95 . ? C114 C115 1.378(3) . ? C114 H114 0.95 . ? C115 C116 1.384(3) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.390(3) . ? C121 C122 1.396(3) . ? C122 C123 1.385(3) . ? C122 H122 0.95 . ? C123 C124 1.384(3) . ? C123 H123 0.95 . ? C124 C125 1.380(3) . ? C124 H124 0.95 . ? C125 C126 1.399(3) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.379(3) . ? C131 C132 1.401(3) . ? C132 C133 1.376(3) . ? C132 H132 0.95 . ? C133 C134 1.381(3) . ? C133 H133 0.95 . ? C134 C135 1.372(3) . ? C134 H134 0.95 . ? C135 C136 1.396(3) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C1 C2 1.362(3) . ? C1 C12 1.435(3) . ? C1 C11 1.445(3) . ? C11 N11 1.143(2) . ? C12 N12 1.144(3) . ? C2 C3 1.463(3) . ? C2 C21 1.485(3) . ? C21 C26 1.389(3) . ? C21 C22 1.396(3) . ? C22 C23 1.380(3) . ? C22 H22 0.95 . ? C23 C24 1.381(3) . ? C23 H23 0.95 . ? C24 C25 1.378(3) . ? C24 H24 0.95 . ? C25 C26 1.388(3) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C3 C4 1.392(2) . ? C4 C41 1.431(3) . ? C4 C51 1.437(3) . ? C41 N41 1.149(2) . ? C51 N52 1.337(2) . ? C51 N55 1.348(2) . ? N52 N53 1.366(2) . ? N53 N54 1.290(2) . ? N54 N55 1.366(2) . ? N55 C03 1.481(2) . ? C01 O02 1.432(3) . ? C01 H01A 0.98 . ? C01 H01B 0.98 . ? C01 H01C 0.98 . ? O02 C03 1.383(3) . ? C03 C04 1.539(3) . ? C03 H03 1 . ? C04 O05 1.425(3) . ? C04 H04A 0.99 . ? C04 H04B 0.99 . ? O05 C06 1.417(3) . ? C06 H06A 0.98 . ? C06 H06B 0.98 . ? C06 H06C 0.98 . ? C101 C105 1.415(3) . ? C101 C102 1.418(3) . ? C101 H101 0.95 . ? C102 C103 1.430(3) . ? C102 H102 0.95 . ? C103 C104 1.399(3) . ? C103 H103 0.95 . ? C104 C105 1.429(3) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? 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 C3 Ru1 N52 76.48(7) . . ? C3 Ru1 C101 96.88(7) . . ? N52 Ru1 C101 132.26(8) . . ? C3 Ru1 C102 113.36(7) . . ? N52 Ru1 C102 164.32(7) . . ? C101 Ru1 C102 37.62(8) . . ? C3 Ru1 C105 114.68(8) . . ? N52 Ru1 C105 102.16(7) . . ? C101 Ru1 C105 37.52(8) . . ? C102 Ru1 C105 62.99(8) . . ? C3 Ru1 C103 150.64(8) . . ? N52 Ru1 C103 132.65(7) . . ? C101 Ru1 C103 62.09(8) . . ? C102 Ru1 C103 37.54(8) . . ? C105 Ru1 C103 61.95(8) . . ? C3 Ru1 C104 151.96(8) . . ? N52 Ru1 C104 103.10(7) . . ? C101 Ru1 C104 62.18(8) . . ? C102 Ru1 C104 62.30(8) . . ? C105 Ru1 C104 37.42(8) . . ? C103 Ru1 C104 36.36(8) . . ? C3 Ru1 P1 94.87(5) . . ? N52 Ru1 P1 89.73(5) . . ? C101 Ru1 P1 137.96(6) . . ? C102 Ru1 P1 101.12(6) . . ? C105 Ru1 P1 149.90(6) . . ? C103 Ru1 P1 89.61(6) . . ? C104 Ru1 P1 113.17(6) . . ? C121 P1 C131 100.31(9) . . ? C121 P1 C111 104.72(9) . . ? C131 P1 C111 104.19(9) . . ? C121 P1 Ru1 117.90(6) . . ? C131 P1 Ru1 114.71(7) . . ? C111 P1 Ru1 113.28(6) . . ? C116 C111 C112 118.49(18) . . ? C116 C111 P1 122.66(16) . . ? C112 C111 P1 118.82(14) . . ? C113 C112 C111 120.86(18) . . ? C113 C112 H112 119.6 . . ? C111 C112 H112 119.6 . . ? C112 C113 C114 119.9(2) . . ? C112 C113 H113 120 . . ? C114 C113 H113 120 . . ? C115 C114 C113 119.5(2) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C114 C115 C116 120.9(2) . . ? C114 C115 H115 119.5 . . ? C116 C115 H115 119.5 . . ? C115 C116 C111 120.2(2) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C126 C121 C122 118.65(17) . . ? C126 C121 P1 123.70(14) . . ? C122 C121 P1 117.53(15) . . ? C123 C122 C121 120.76(19) . . ? C123 C122 H122 119.6 . . ? C121 C122 H122 119.6 . . ? C124 C123 C122 120.14(19) . . ? C124 C123 H123 119.9 . . ? C122 C123 H123 119.9 . . ? C125 C124 C123 119.90(18) . . ? C125 C124 H124 120.1 . . ? C123 C124 H124 120.1 . . ? C124 C125 C126 120.10(19) . . ? C124 C125 H125 120 . . ? C126 C125 H125 120 . . ? C121 C126 C125 120.40(18) . . ? C121 C126 H126 119.8 . . ? C125 C126 H126 119.8 . . ? C136 C131 C132 118.11(18) . . ? C136 C131 P1 120.82(16) . . ? C132 C131 P1 121.07(15) . . ? C133 C132 C131 120.6(2) . . ? C133 C132 H132 119.7 . . ? C131 C132 H132 119.7 . . ? C132 C133 C134 120.4(2) . . ? C132 C133 H133 119.8 . . ? C134 C133 H133 119.8 . . ? C135 C134 C133 120.0(2) . . ? C135 C134 H134 120 . . ? C133 C134 H134 120 . . ? C134 C135 C136 119.6(2) . . ? C134 C135 H135 120.2 . . ? C136 C135 H135 120.2 . . ? C131 C136 C135 121.3(2) . . ? C131 C136 H136 119.4 . . ? C135 C136 H136 119.4 . . ? C2 C1 C12 123.06(17) . . ? C2 C1 C11 123.07(18) . . ? C12 C1 C11 113.87(17) . . ? N11 C11 C1 176.1(2) . . ? N12 C12 C1 175.5(2) . . ? C1 C2 C3 119.18(17) . . ? C1 C2 C21 118.85(17) . . ? C3 C2 C21 121.86(16) . . ? C26 C21 C22 119.14(19) . . ? C26 C21 C2 120.73(17) . . ? C22 C21 C2 120.12(18) . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.0(2) . . ? C22 C23 H23 120 . . ? C24 C23 H23 120 . . ? C25 C24 C23 120.1(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.0(2) . . ? C25 C26 H26 120 . . ? C21 C26 H26 120 . . ? C4 C3 C2 119.68(16) . . ? C4 C3 Ru1 118.01(13) . . ? C2 C3 Ru1 121.57(13) . . ? C3 C4 C41 125.07(17) . . ? C3 C4 C51 112.04(16) . . ? C41 C4 C51 122.84(16) . . ? N41 C41 C4 179.3(2) . . ? N52 C51 N55 106.98(16) . . ? N52 C51 C4 115.31(16) . . ? N55 C51 C4 137.56(17) . . ? C51 N52 N53 107.62(15) . . ? C51 N52 Ru1 117.54(12) . . ? N53 N52 Ru1 134.80(12) . . ? N54 N53 N52 109.45(15) . . ? N53 N54 N55 107.61(15) . . ? C51 N55 N54 108.34(15) . . ? C51 N55 C03 131.94(17) . . ? N54 N55 C03 119.25(16) . . ? O02 C01 H01A 109.5 . . ? O02 C01 H01B 109.5 . . ? H01A C01 H01B 109.5 . . ? O02 C01 H01C 109.5 . . ? H01A C01 H01C 109.5 . . ? H01B C01 H01C 109.5 . . ? C03 O02 C01 113.40(17) . . ? O02 C03 N55 111.68(18) . . ? O02 C03 C04 109.05(18) . . ? N55 C03 C04 107.44(18) . . ? O02 C03 H03 109.5 . . ? N55 C03 H03 109.5 . . ? C04 C03 H03 109.5 . . ? O05 C04 C03 107.30(19) . . ? O05 C04 H04A 110.3 . . ? C03 C04 H04A 110.3 . . ? O05 C04 H04B 110.3 . . ? C03 C04 H04B 110.3 . . ? H04A C04 H04B 108.5 . . ? C06 O05 C04 114.6(2) . . ? O05 C06 H06A 109.5 . . ? O05 C06 H06B 109.5 . . ? H06A C06 H06B 109.5 . . ? O05 C06 H06C 109.5 . . ? H06A C06 H06C 109.5 . . ? H06B C06 H06C 109.5 . . ? C105 C101 C102 108.77(19) . . ? C105 C101 Ru1 71.65(11) . . ? C102 C101 Ru1 71.54(11) . . ? C105 C101 H101 125.6 . . ? C102 C101 H101 125.6 . . ? Ru1 C101 H101 122.8 . . ? C101 C102 C103 106.78(19) . . ? C101 C102 Ru1 70.83(11) . . ? C103 C102 Ru1 72.52(11) . . ? C101 C102 H102 126.6 . . ? C103 C102 H102 126.6 . . ? Ru1 C102 H102 121.8 . . ? C104 C103 C102 108.94(19) . . ? C104 C103 Ru1 72.15(11) . . ? C102 C103 Ru1 69.93(10) . . ? C104 C103 H103 125.5 . . ? C102 C103 H103 125.5 . . ? Ru1 C103 H103 124 . . ? C103 C104 C105 107.94(19) . . ? C103 C104 Ru1 71.49(11) . . ? C105 C104 Ru1 69.71(11) . . ? C103 C104 H104 126 . . ? C105 C104 H104 126 . . ? Ru1 C104 H104 124.4 . . ? C101 C105 C104 107.54(19) . . ? C101 C105 Ru1 70.83(12) . . ? C104 C105 Ru1 72.87(11) . . ? C101 C105 H105 126.2 . . ? C104 C105 H105 126.2 . . ? Ru1 C105 H105 121.8 . . ? 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 C3 Ru1 P1 C121 14.37(9) . . . . ? N52 Ru1 P1 C121 -62.04(8) . . . . ? C101 Ru1 P1 C121 120.28(11) . . . . ? C102 Ru1 P1 C121 129.35(9) . . . . ? C105 Ru1 P1 C121 -176.37(14) . . . . ? C103 Ru1 P1 C121 165.31(9) . . . . ? C104 Ru1 P1 C121 -166.19(9) . . . . ? C3 Ru1 P1 C131 132.18(9) . . . . ? N52 Ru1 P1 C131 55.77(8) . . . . ? C101 Ru1 P1 C131 -121.91(11) . . . . ? C102 Ru1 P1 C131 -112.84(9) . . . . ? C105 Ru1 P1 C131 -58.56(14) . . . . ? C103 Ru1 P1 C131 -76.88(9) . . . . ? C104 Ru1 P1 C131 -48.38(9) . . . . ? C3 Ru1 P1 C111 -108.36(9) . . . . ? N52 Ru1 P1 C111 175.23(8) . . . . ? C101 Ru1 P1 C111 -2.46(11) . . . . ? C102 Ru1 P1 C111 6.62(9) . . . . ? C105 Ru1 P1 C111 60.90(14) . . . . ? C103 Ru1 P1 C111 42.58(9) . . . . ? C104 Ru1 P1 C111 71.07(9) . . . . ? C121 P1 C111 C116 107.71(17) . . . . ? C131 P1 C111 C116 2.80(19) . . . . ? Ru1 P1 C111 C116 -122.52(15) . . . . ? C121 P1 C111 C112 -74.20(17) . . . . ? C131 P1 C111 C112 -179.11(15) . . . . ? Ru1 P1 C111 C112 55.56(16) . . . . ? C116 C111 C112 C113 -0.5(3) . . . . ? P1 C111 C112 C113 -178.66(15) . . . . ? C111 C112 C113 C114 1.1(3) . . . . ? C112 C113 C114 C115 -0.6(3) . . . . ? C113 C114 C115 C116 -0.5(3) . . . . ? C114 C115 C116 C111 1.1(3) . . . . ? C112 C111 C116 C115 -0.6(3) . . . . ? P1 C111 C116 C115 177.48(16) . . . . ? C131 P1 C121 C126 129.08(17) . . . . ? C111 P1 C121 C126 21.30(18) . . . . ? Ru1 P1 C121 C126 -105.67(16) . . . . ? C131 P1 C121 C122 -55.14(16) . . . . ? C111 P1 C121 C122 -162.92(15) . . . . ? Ru1 P1 C121 C122 70.11(16) . . . . ? C126 C121 C122 C123 2.5(3) . . . . ? P1 C121 C122 C123 -173.53(15) . . . . ? C121 C122 C123 C124 -1.1(3) . . . . ? C122 C123 C124 C125 -1.3(3) . . . . ? C123 C124 C125 C126 2.2(3) . . . . ? C122 C121 C126 C125 -1.5(3) . . . . ? P1 C121 C126 C125 174.23(15) . . . . ? C124 C125 C126 C121 -0.8(3) . . . . ? C121 P1 C131 C136 143.59(17) . . . . ? C111 P1 C131 C136 -108.21(17) . . . . ? Ru1 P1 C131 C136 16.20(19) . . . . ? C121 P1 C131 C132 -35.82(18) . . . . ? C111 P1 C131 C132 72.38(18) . . . . ? Ru1 P1 C131 C132 -163.21(15) . . . . ? C136 C131 C132 C133 -0.2(3) . . . . ? P1 C131 C132 C133 179.25(18) . . . . ? C131 C132 C133 C134 0.1(4) . . . . ? C132 C133 C134 C135 0.1(4) . . . . ? C133 C134 C135 C136 -0.2(4) . . . . ? C132 C131 C136 C135 0.1(3) . . . . ? P1 C131 C136 C135 -179.33(16) . . . . ? C134 C135 C136 C131 0.1(3) . . . . ? C2 C1 C11 N11 -138(3) . . . . ? C12 C1 C11 N11 42(3) . . . . ? C2 C1 C12 N12 -159(3) . . . . ? C11 C1 C12 N12 21(3) . . . . ? C12 C1 C2 C3 -2.1(3) . . . . ? C11 C1 C2 C3 177.90(16) . . . . ? C12 C1 C2 C21 174.18(17) . . . . ? C11 C1 C2 C21 -5.8(3) . . . . ? C1 C2 C21 C26 121.1(2) . . . . ? C3 C2 C21 C26 -62.7(2) . . . . ? C1 C2 C21 C22 -57.7(3) . . . . ? C3 C2 C21 C22 118.5(2) . . . . ? C26 C21 C22 C23 1.2(3) . . . . ? C2 C21 C22 C23 -179.97(19) . . . . ? C21 C22 C23 C24 -1.0(3) . . . . ? C22 C23 C24 C25 0.3(3) . . . . ? C23 C24 C25 C26 0.3(3) . . . . ? C24 C25 C26 C21 -0.2(3) . . . . ? C22 C21 C26 C25 -0.6(3) . . . . ? C2 C21 C26 C25 -179.43(17) . . . . ? C1 C2 C3 C4 -66.3(2) . . . . ? C21 C2 C3 C4 117.5(2) . . . . ? C1 C2 C3 Ru1 103.70(18) . . . . ? C21 C2 C3 Ru1 -72.5(2) . . . . ? N52 Ru1 C3 C4 6.64(14) . . . . ? C101 Ru1 C3 C4 138.53(15) . . . . ? C102 Ru1 C3 C4 173.75(14) . . . . ? C105 Ru1 C3 C4 103.99(15) . . . . ? C103 Ru1 C3 C4 -179.81(14) . . . . ? C104 Ru1 C3 C4 99.2(2) . . . . ? P1 Ru1 C3 C4 -81.91(14) . . . . ? N52 Ru1 C3 C2 -163.54(16) . . . . ? C101 Ru1 C3 C2 -31.65(16) . . . . ? C102 Ru1 C3 C2 3.58(18) . . . . ? C105 Ru1 C3 C2 -66.18(17) . . . . ? C103 Ru1 C3 C2 10.0(3) . . . . ? C104 Ru1 C3 C2 -71.0(2) . . . . ? P1 Ru1 C3 C2 107.91(15) . . . . ? C2 C3 C4 C41 -12.5(3) . . . . ? Ru1 C3 C4 C41 177.12(15) . . . . ? C2 C3 C4 C51 164.94(17) . . . . ? Ru1 C3 C4 C51 -5.4(2) . . . . ? C3 C4 C41 N41 -6E1(2) . . . . ? C51 C4 C41 N41 13E1(2) . . . . ? C3 C4 C51 N52 -0.6(2) . . . . ? C41 C4 C51 N52 176.94(18) . . . . ? C3 C4 C51 N55 -175.3(2) . . . . ? C41 C4 C51 N55 2.2(4) . . . . ? N55 C51 N52 N53 0.5(2) . . . . ? C4 C51 N52 N53 -175.81(16) . . . . ? N55 C51 N52 Ru1 -177.46(12) . . . . ? C4 C51 N52 Ru1 6.3(2) . . . . ? C3 Ru1 N52 C51 -6.97(14) . . . . ? C101 Ru1 N52 C51 -93.99(16) . . . . ? C102 Ru1 N52 C51 -137.7(2) . . . . ? C105 Ru1 N52 C51 -119.77(14) . . . . ? C103 Ru1 N52 C51 177.32(13) . . . . ? C104 Ru1 N52 C51 -158.15(14) . . . . ? P1 Ru1 N52 C51 88.10(13) . . . . ? C3 Ru1 N52 N53 175.79(19) . . . . ? C101 Ru1 N52 N53 88.77(19) . . . . ? C102 Ru1 N52 N53 45.0(3) . . . . ? C105 Ru1 N52 N53 62.99(18) . . . . ? C103 Ru1 N52 N53 0.1(2) . . . . ? C104 Ru1 N52 N53 24.62(19) . . . . ? P1 Ru1 N52 N53 -89.14(17) . . . . ? C51 N52 N53 N54 -0.4(2) . . . . ? Ru1 N52 N53 N54 177.02(14) . . . . ? N52 N53 N54 N55 0.2(2) . . . . ? N52 C51 N55 N54 -0.4(2) . . . . ? C4 C51 N55 N54 174.6(2) . . . . ? N52 C51 N55 C03 171.5(2) . . . . ? C4 C51 N55 C03 -13.5(4) . . . . ? N53 N54 N55 C51 0.1(2) . . . . ? N53 N54 N55 C03 -172.93(18) . . . . ? C01 O02 C03 N55 -73.8(2) . . . . ? C01 O02 C03 C04 167.64(19) . . . . ? C51 N55 C03 O02 107.7(2) . . . . ? N54 N55 C03 O02 -81.1(2) . . . . ? C51 N55 C03 C04 -132.7(2) . . . . ? N54 N55 C03 C04 38.4(3) . . . . ? O02 C03 C04 O05 -179.30(18) . . . . ? N55 C03 C04 O05 59.5(2) . . . . ? C03 C04 O05 C06 -155.5(2) . . . . ? C3 Ru1 C101 C105 -122.24(13) . . . . ? N52 Ru1 C101 C105 -44.27(16) . . . . ? C102 Ru1 C101 C105 117.91(18) . . . . ? C103 Ru1 C101 C105 79.41(13) . . . . ? C104 Ru1 C101 C105 38.07(12) . . . . ? P1 Ru1 C101 C105 132.60(11) . . . . ? C3 Ru1 C101 C102 119.84(13) . . . . ? N52 Ru1 C101 C102 -162.19(11) . . . . ? C105 Ru1 C101 C102 -117.91(18) . . . . ? C103 Ru1 C101 C102 -38.51(12) . . . . ? C104 Ru1 C101 C102 -79.84(13) . . . . ? P1 Ru1 C101 C102 14.69(16) . . . . ? C105 C101 C102 C103 1.7(2) . . . . ? Ru1 C101 C102 C103 64.10(13) . . . . ? C105 C101 C102 Ru1 -62.35(14) . . . . ? C3 Ru1 C102 C101 -69.72(14) . . . . ? N52 Ru1 C102 C101 56.9(3) . . . . ? C105 Ru1 C102 C101 37.16(12) . . . . ? C103 Ru1 C102 C101 115.46(18) . . . . ? C104 Ru1 C102 C101 79.50(13) . . . . ? P1 Ru1 C102 C101 -170.04(11) . . . . ? C3 Ru1 C102 C103 174.82(12) . . . . ? N52 Ru1 C102 C103 -58.5(3) . . . . ? C101 Ru1 C102 C103 -115.46(18) . . . . ? C105 Ru1 C102 C103 -78.30(13) . . . . ? C104 Ru1 C102 C103 -35.96(12) . . . . ? P1 Ru1 C102 C103 74.51(12) . . . . ? C101 C102 C103 C104 -1.0(2) . . . . ? Ru1 C102 C103 C104 61.95(14) . . . . ? C101 C102 C103 Ru1 -62.97(12) . . . . ? C3 Ru1 C103 C104 -128.45(16) . . . . ? N52 Ru1 C103 C104 43.02(16) . . . . ? C101 Ru1 C103 C104 -80.13(14) . . . . ? C102 Ru1 C103 C104 -118.72(18) . . . . ? C105 Ru1 C103 C104 -37.42(13) . . . . ? P1 Ru1 C103 C104 132.29(12) . . . . ? C3 Ru1 C103 C102 -9.7(2) . . . . ? N52 Ru1 C103 C102 161.74(11) . . . . ? C101 Ru1 C103 C102 38.59(12) . . . . ? C105 Ru1 C103 C102 81.30(13) . . . . ? C104 Ru1 C103 C102 118.72(18) . . . . ? P1 Ru1 C103 C102 -108.99(12) . . . . ? C102 C103 C104 C105 -0.1(2) . . . . ? Ru1 C103 C104 C105 60.48(13) . . . . ? C102 C103 C104 Ru1 -60.56(13) . . . . ? C3 Ru1 C104 C103 125.22(17) . . . . ? N52 Ru1 C104 C103 -148.99(12) . . . . ? C101 Ru1 C104 C103 79.87(14) . . . . ? C102 Ru1 C104 C103 37.13(12) . . . . ? C105 Ru1 C104 C103 118.04(18) . . . . ? P1 Ru1 C104 C103 -53.57(13) . . . . ? C3 Ru1 C104 C105 7.2(2) . . . . ? N52 Ru1 C104 C105 92.97(13) . . . . ? C101 Ru1 C104 C105 -38.17(13) . . . . ? C102 Ru1 C104 C105 -80.92(14) . . . . ? C103 Ru1 C104 C105 -118.04(18) . . . . ? P1 Ru1 C104 C105 -171.62(11) . . . . ? C102 C101 C105 C104 -1.8(2) . . . . ? Ru1 C101 C105 C104 -64.09(13) . . . . ? C102 C101 C105 Ru1 62.29(14) . . . . ? C103 C104 C105 C101 1.2(2) . . . . ? Ru1 C104 C105 C101 62.76(13) . . . . ? C103 C104 C105 Ru1 -61.61(14) . . . . ? C3 Ru1 C105 C101 67.54(14) . . . . ? N52 Ru1 C105 C101 148.10(12) . . . . ? C102 Ru1 C105 C101 -37.27(12) . . . . ? C103 Ru1 C105 C101 -79.81(13) . . . . ? C104 Ru1 C105 C101 -116.17(18) . . . . ? P1 Ru1 C105 C101 -100.67(15) . . . . ? C3 Ru1 C105 C104 -176.29(12) . . . . ? N52 Ru1 C105 C104 -95.74(13) . . . . ? C101 Ru1 C105 C104 116.17(18) . . . . ? C102 Ru1 C105 C104 78.90(13) . . . . ? C103 Ru1 C105 C104 36.36(12) . . . . ? P1 Ru1 C105 C104 15.5(2) . . . . ? #===END