# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Ki-Whan Chi' V.Vajpayee _publ_contact_author_name 'Vaishali Vajpayee' _publ_contact_author_email vaishalivajpayee@gmail.com data_p21n _database_code_depnum_ccdc_archive 'CCDC 841900' #TrackingRef '- 5_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H72 N4 O8 Ru4, 4(F6 P), C H3 N O2' _chemical_formula_sum 'C36.50 H37.50 F12 N2.50 O5 P2 Ru2' _chemical_formula_weight 1083.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0028 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N -0.0031 0.0056 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0042 0.0102 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1274 0.1530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -0.9454 1.2848 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F -0.0055 0.0172 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 8.6300(17) _cell_length_b 35.969(7) _cell_length_c 13.430(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.55(3) _cell_angle_gamma 90.00 _cell_volume 4132.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17417 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 30.36 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6300 _exptl_absorpt_correction_T_max 0.9200 _exptl_absorpt_process_details HKL2000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.90000 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron-PAL _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17417 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.36 _reflns_number_total 5158 _reflns_number_gt 4202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ADSC Quantum software' _computing_cell_refinement 'DENZO (Z. Otwinowski and W. Minor, 1997)' _computing_data_reduction 'HKL2000 (Z. Otwinowski and W. Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Materials Studio 4.1' _computing_publication_material 'Materials Studio 4.1' _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. A nitromethane molecle were restrained by SIMU and SADI commands. The molecule has symmetry-related disorder by an inversion center. So I fixed its occupancy (0.5) and used FREE commands to remove bonds with a symmetry-related molecules. SADI N1N O1N, N1N O2N SADI O1N C1N, O2N C1N SIMU 0.02 O1N > C1N EQIV $1 -x, -y, -z+1 FREE C1N C1N_$1 ; _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^)+(0.1180P)^2^+8.0115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5158 _refine_ls_number_parameters 561 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1656 _refine_ls_wR_factor_gt 0.1557 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru1 Ru 0.56203(7) 0.147503(15) 0.02158(4) 0.0477(2) Uani 1 1 d . . . Ru2 Ru 0.28678(7) 0.161439(15) 0.36621(4) 0.0451(2) Uani 1 1 d . . . P1 P 0.3329(3) 0.06285(6) 0.67826(14) 0.0661(7) Uani 1 1 d . . . P2 P 0.0382(3) 0.22830(6) -0.27824(15) 0.0614(6) Uani 1 1 d . . . F1 F 0.4418(7) 0.05057(13) 0.7781(3) 0.0879(17) Uani 1 1 d . . . F2 F 0.2839(7) 0.09931(14) 0.7334(4) 0.0907(16) Uani 1 1 d . . . F3 F 0.4747(6) 0.08448(16) 0.6427(4) 0.0889(16) Uani 1 1 d . . . F4 F 0.1851(8) 0.04169(15) 0.7132(4) 0.1006(19) Uani 1 1 d . . . F5 F 0.3758(7) 0.02598(14) 0.6240(4) 0.101(2) Uani 1 1 d . . . F6 F 0.2203(6) 0.07556(12) 0.5783(3) 0.0709(13) Uani 1 1 d . . . F7 F 0.1378(6) 0.19223(13) -0.2424(4) 0.0807(15) Uani 1 1 d . . . F8 F 0.0950(6) 0.24873(14) -0.1744(4) 0.0811(15) Uani 1 1 d . . . F9 F 0.1881(6) 0.24466(15) -0.3236(4) 0.0896(16) Uani 1 1 d . . . F10 F -0.0617(6) 0.26463(12) -0.3148(3) 0.0737(13) Uani 1 1 d . . . F11 F -0.1093(6) 0.21243(13) -0.2312(3) 0.0728(13) Uani 1 1 d . . . F12 F -0.0199(6) 0.20855(13) -0.3824(3) 0.0782(14) Uani 1 1 d . . . O1 O 0.2270(6) 0.15934(12) 0.2087(4) 0.0496(13) Uani 1 1 d . . . O2 O 0.5101(6) 0.15899(12) 0.3187(3) 0.0500(13) Uani 1 1 d . . . O3 O 0.3399(6) 0.15478(12) 0.0673(3) 0.0483(12) Uani 1 1 d . . . O4 O 0.6206(7) 0.15305(13) 0.1780(4) 0.0513(13) Uani 1 1 d . . . N1 N 0.3016(7) 0.10307(16) 0.3553(4) 0.0466(15) Uani 1 1 d . . . N2 N -0.5167(7) -0.09110(16) -0.0556(4) 0.0486(15) Uani 1 1 d . . . C1 C 0.3444(10) 0.15746(18) 0.1620(6) 0.0469(19) Uani 1 1 d . . . C2 C 0.5042(10) 0.15697(18) 0.2243(5) 0.0436(18) Uani 1 1 d . . . C3 C 0.1516(9) 0.2119(2) 0.3725(5) 0.054(2) Uani 1 1 d . . . H3 H 0.1153 0.2251 0.3081 0.065 Uiso 1 1 calc R . . C4 C 0.3029(9) 0.21920(19) 0.4198(5) 0.0527(19) Uani 1 1 d . . . H4 H 0.3704 0.2373 0.3887 0.063 Uiso 1 1 calc R . . C5 C 0.1288(10) 0.1585(2) 0.4791(6) 0.056(2) Uani 1 1 d . . . H5 H 0.0777 0.1342 0.4902 0.067 Uiso 1 1 calc R . . C6 C 0.0617(9) 0.1812(2) 0.4002(5) 0.054(2) Uani 1 1 d . . . C7 C 0.3734(9) 0.1944(2) 0.4994(5) 0.0509(19) Uani 1 1 d . . . C8 C 0.2831(10) 0.16502(19) 0.5288(5) 0.0510(19) Uani 1 1 d . . . H8 H 0.3357 0.1451 0.5729 0.061 Uiso 1 1 calc R . . C9 C 0.5402(9) 0.2018(2) 0.5425(6) 0.059(2) Uani 1 1 d . . . H9 H 0.5968 0.2102 0.4862 0.070 Uiso 1 1 calc R . . C10 C 0.6244(11) 0.1674(3) 0.5888(7) 0.083(3) Uani 1 1 d . . . H10A H 0.7325 0.1738 0.6149 0.124 Uiso 1 1 calc R . . H10B H 0.6242 0.1480 0.5375 0.124 Uiso 1 1 calc R . . H10C H 0.5706 0.1582 0.6438 0.124 Uiso 1 1 calc R . . C11 C 0.5406(11) 0.2336(3) 0.6152(8) 0.094(3) Uani 1 1 d . . . H11A H 0.6483 0.2390 0.6445 0.141 Uiso 1 1 calc R . . H11B H 0.4787 0.2268 0.6687 0.141 Uiso 1 1 calc R . . H11C H 0.4951 0.2556 0.5797 0.141 Uiso 1 1 calc R . . C12 C -0.0962(10) 0.1730(2) 0.3452(7) 0.070(2) Uani 1 1 d . . . H12A H -0.1206 0.1466 0.3531 0.106 Uiso 1 1 calc R . . H12B H -0.0973 0.1787 0.2738 0.106 Uiso 1 1 calc R . . H12C H -0.1745 0.1883 0.3727 0.106 Uiso 1 1 calc R . . C13 C 0.1946(9) 0.08365(19) 0.2964(5) 0.0513(19) Uani 1 1 d . . . H13 H 0.1102 0.0967 0.2596 0.062 Uiso 1 1 calc R . . C14 C 0.4213(10) 0.0842(2) 0.4051(5) 0.054(2) Uani 1 1 d . . . H14 H 0.5002 0.0978 0.4457 0.064 Uiso 1 1 calc R . . C15 C 0.4361(10) 0.0461(2) 0.4006(5) 0.056(2) Uani 1 1 d . . . H15 H 0.5219 0.0339 0.4385 0.067 Uiso 1 1 calc R . . C16 C 0.2001(9) 0.04484(19) 0.2860(5) 0.0522(19) Uani 1 1 d . . . C17 C 0.3243(10) 0.0260(2) 0.3402(5) 0.062(2) Uani 1 1 d . . . H17 H 0.3322 -0.0003 0.3358 0.074 Uiso 1 1 calc R . . C18 C 0.0868(10) 0.0264(2) 0.2185(6) 0.057(2) Uani 1 1 d . . . C19 C -0.0102(10) 0.0112(2) 0.1597(6) 0.060(2) Uani 1 1 d . . . C20 C -0.1229(10) -0.0061(2) 0.0920(5) 0.056(2) Uani 1 1 d . . . C21 C -0.2233(10) -0.02064(19) 0.0371(5) 0.055(2) Uani 1 1 d . . . C22 C -0.3517(9) -0.03795(19) -0.0239(5) 0.053(2) Uani 1 1 d . . . C23 C -0.3975(9) -0.07424(19) -0.0016(5) 0.0496(18) Uani 1 1 d . . . H23 H -0.3415 -0.0870 0.0538 0.060 Uiso 1 1 calc R . . C24 C -0.4372(10) -0.0196(2) -0.1050(6) 0.060(2) Uani 1 1 d . . . H24 H -0.4095 0.0050 -0.1219 0.072 Uiso 1 1 calc R . . C25 C -0.5614(9) -0.03716(19) -0.1600(5) 0.053(2) Uani 1 1 d . . . H25 H -0.6214 -0.0249 -0.2149 0.064 Uiso 1 1 calc R . . C26 C -0.5975(9) -0.0732(2) -0.1338(5) 0.0529(19) Uani 1 1 d . . . H26 H -0.6822 -0.0856 -0.1724 0.064 Uiso 1 1 calc R . . C27 C 0.4903(11) 0.1639(2) -0.1334(6) 0.059(2) Uani 1 1 d . . . H27 H 0.3803 0.1592 -0.1647 0.071 Uiso 1 1 calc R . . C28 C 0.5259(10) 0.1967(2) -0.0740(5) 0.056(2) Uani 1 1 d . . . C29 C 0.6729(10) 0.1990(2) -0.0140(6) 0.057(2) Uani 1 1 d . . . H29 H 0.6899 0.2189 0.0386 0.068 Uiso 1 1 calc R . . C30 C 0.7829(10) 0.1693(2) -0.0114(6) 0.060(2) Uani 1 1 d . . . H30 H 0.8740 0.1691 0.0429 0.072 Uiso 1 1 calc R . . C31 C 0.7518(10) 0.1372(2) -0.0702(6) 0.059(2) Uani 1 1 d . . . C32 C 0.4019(10) 0.2251(2) -0.0693(6) 0.064(2) Uani 1 1 d . . . H32A H 0.4350 0.2427 -0.0149 0.097 Uiso 1 1 calc R . . H32B H 0.3049 0.2129 -0.0568 0.097 Uiso 1 1 calc R . . H32C H 0.3840 0.2386 -0.1333 0.097 Uiso 1 1 calc R . . C33 C 0.8626(11) 0.1054(2) -0.0684(6) 0.071(2) Uani 1 1 d . . . H33 H 0.7985 0.0822 -0.0750 0.085 Uiso 1 1 calc R . . C34 C 0.9442(17) 0.1083(4) -0.1623(10) 0.160(7) Uani 1 1 d . . . H34A H 1.0175 0.0875 -0.1637 0.240 Uiso 1 1 calc R . . H34B H 1.0014 0.1318 -0.1613 0.240 Uiso 1 1 calc R . . H34C H 0.8661 0.1073 -0.2222 0.240 Uiso 1 1 calc R . . C35 C 0.6024(10) 0.1352(2) -0.1326(6) 0.060(2) Uani 1 1 d . . . H35 H 0.5674 0.1106 -0.1618 0.071 Uiso 1 1 calc R . . C36 C 0.9737(11) 0.1021(2) 0.0264(7) 0.080(3) Uani 1 1 d . . . H36A H 1.0416 0.0805 0.0221 0.119 Uiso 1 1 calc R . . H36B H 0.9147 0.0991 0.0834 0.119 Uiso 1 1 calc R . . H36C H 1.0377 0.1247 0.0360 0.119 Uiso 1 1 calc R . . O1N O -0.1974(16) 0.0624(6) 0.5445(12) 0.124(6) Uani 0.50 1 d PDU . . O2N O -0.1433(16) 0.0706(4) 0.3889(12) 0.093(4) Uani 0.50 1 d PDU . . N1N N -0.155(2) 0.0660(10) 0.4712(12) 0.139(9) Uani 0.50 1 d PDU . . C1N C -0.079(4) 0.0339(11) 0.4774(14) 0.194(15) Uani 0.50 1 d PDU . . H1N1 H -0.0294 0.0302 0.4165 0.291 Uiso 0.50 1 calc PR . . H1N2 H -0.1528 0.0136 0.4838 0.291 Uiso 0.50 1 calc PR . . H1N3 H 0.0012 0.0342 0.5362 0.291 Uiso 0.50 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 0.0708(5) 0.0341(4) 0.0382(4) -0.0006(2) 0.0074(3) -0.0041(3) Ru2 0.0666(5) 0.0333(4) 0.0344(3) -0.0033(2) 0.0031(3) -0.0018(3) P1 0.117(2) 0.0418(11) 0.0390(11) 0.0018(9) 0.0071(12) 0.0069(12) P2 0.0816(17) 0.0474(12) 0.0549(12) -0.0012(9) 0.0081(11) 0.0071(11) F1 0.154(5) 0.056(3) 0.046(3) 0.005(2) -0.014(3) 0.009(3) F2 0.136(5) 0.059(3) 0.080(3) -0.021(3) 0.023(3) 0.004(3) F3 0.097(4) 0.110(4) 0.058(3) 0.021(3) 0.005(3) -0.009(3) F4 0.154(5) 0.089(4) 0.060(3) 0.011(3) 0.016(3) -0.044(4) F5 0.156(5) 0.065(3) 0.073(3) -0.025(3) -0.018(3) 0.042(3) F6 0.098(4) 0.060(3) 0.053(3) 0.015(2) 0.005(2) 0.013(3) F7 0.106(4) 0.050(3) 0.083(3) 0.000(2) 0.001(3) 0.016(3) F8 0.092(4) 0.072(3) 0.077(3) -0.023(3) -0.002(3) 0.003(3) F9 0.096(4) 0.077(4) 0.102(4) 0.008(3) 0.033(3) 0.000(3) F10 0.097(4) 0.048(3) 0.073(3) 0.001(2) 0.001(3) 0.012(2) F11 0.085(3) 0.073(3) 0.061(3) -0.001(2) 0.015(2) -0.015(3) F12 0.108(4) 0.073(3) 0.052(3) -0.011(2) 0.004(3) 0.017(3) O1 0.063(4) 0.038(3) 0.047(3) -0.001(2) 0.003(3) -0.006(2) O2 0.068(3) 0.039(3) 0.041(3) -0.003(2) -0.001(2) -0.004(2) O3 0.069(4) 0.041(3) 0.034(3) 0.000(2) 0.001(2) -0.006(2) O4 0.067(4) 0.036(3) 0.049(3) -0.005(2) 0.001(3) -0.002(2) N1 0.066(4) 0.044(3) 0.029(3) -0.003(3) 0.003(3) -0.009(3) N2 0.067(4) 0.044(3) 0.035(3) -0.005(3) 0.006(3) -0.002(3) C1 0.068(6) 0.026(4) 0.047(5) -0.002(3) 0.007(4) -0.004(3) C2 0.058(5) 0.035(4) 0.038(4) -0.005(3) 0.006(4) -0.002(3) C3 0.075(6) 0.042(4) 0.045(4) -0.008(3) 0.007(4) 0.005(4) C4 0.075(6) 0.038(4) 0.045(4) -0.005(3) 0.007(4) 0.003(4) C5 0.078(6) 0.036(4) 0.053(5) -0.013(3) 0.008(4) -0.002(4) C6 0.066(5) 0.045(4) 0.049(4) -0.009(3) 0.002(4) 0.003(4) C7 0.065(5) 0.047(4) 0.040(4) -0.012(3) 0.003(4) 0.000(4) C8 0.072(6) 0.036(4) 0.045(4) -0.001(3) 0.007(4) 0.004(4) C9 0.070(6) 0.049(5) 0.056(5) -0.014(4) 0.002(4) -0.004(4) C10 0.083(7) 0.077(7) 0.081(6) -0.015(5) -0.017(5) -0.003(5) C11 0.078(7) 0.094(7) 0.104(8) -0.063(6) -0.010(6) 0.002(5) C12 0.073(6) 0.059(5) 0.077(6) -0.017(4) 0.001(5) 0.004(4) C13 0.070(5) 0.044(4) 0.040(4) 0.003(3) 0.008(4) 0.001(4) C14 0.078(6) 0.046(5) 0.035(4) -0.002(3) 0.003(4) -0.002(4) C15 0.081(6) 0.041(4) 0.044(4) -0.005(3) 0.001(4) 0.005(4) C16 0.080(6) 0.037(4) 0.041(4) -0.007(3) 0.013(4) -0.006(4) C17 0.100(7) 0.032(4) 0.052(5) 0.001(3) 0.008(5) 0.004(4) C18 0.085(6) 0.034(4) 0.052(5) -0.005(4) 0.005(4) -0.003(4) C19 0.086(6) 0.038(4) 0.057(5) -0.001(4) 0.014(5) 0.000(4) C20 0.081(6) 0.039(4) 0.046(4) -0.005(4) 0.004(4) -0.005(4) C21 0.086(6) 0.031(4) 0.047(4) -0.002(3) 0.009(4) -0.007(4) C22 0.079(6) 0.038(4) 0.043(4) -0.004(3) 0.011(4) -0.002(4) C23 0.070(5) 0.039(4) 0.039(4) -0.004(3) 0.005(4) 0.001(4) C24 0.092(6) 0.034(4) 0.054(5) 0.002(3) 0.015(4) 0.001(4) C25 0.083(6) 0.034(4) 0.041(4) 0.003(3) 0.002(4) -0.002(4) C26 0.069(5) 0.049(5) 0.041(4) -0.004(3) 0.008(4) -0.001(4) C27 0.084(6) 0.045(5) 0.048(4) 0.006(3) 0.016(4) 0.001(4) C28 0.085(6) 0.040(4) 0.046(4) 0.004(3) 0.015(4) -0.002(4) C29 0.073(6) 0.040(4) 0.057(5) 0.010(3) 0.007(4) -0.004(4) C30 0.071(6) 0.043(5) 0.067(5) 0.010(4) 0.011(4) -0.007(4) C31 0.083(6) 0.044(5) 0.052(5) 0.009(4) 0.020(4) 0.005(4) C32 0.085(6) 0.054(5) 0.055(5) 0.002(4) 0.009(4) 0.006(4) C33 0.088(7) 0.061(5) 0.070(6) 0.011(4) 0.034(5) 0.004(5) C34 0.199(15) 0.141(12) 0.167(13) 0.086(10) 0.127(12) 0.099(11) C35 0.081(6) 0.051(5) 0.048(4) 0.008(4) 0.015(4) -0.004(4) C36 0.072(6) 0.053(5) 0.111(8) -0.002(5) 0.004(6) 0.009(4) O1N 0.053(9) 0.225(18) 0.101(11) 0.041(12) 0.038(8) 0.055(10) O2N 0.069(9) 0.099(10) 0.117(11) 0.023(9) 0.036(9) -0.012(7) N1N 0.030(11) 0.26(2) 0.115(15) -0.015(19) -0.016(12) -0.026(13) C1N 0.17(3) 0.34(4) 0.077(15) -0.07(2) 0.036(17) -0.19(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 O4 2.105(5) . ? Ru1 O3 2.104(5) . ? Ru1 N2 2.127(6) 3 ? Ru1 C30 2.160(8) . ? Ru1 C29 2.168(7) . ? Ru1 C27 2.174(8) . ? Ru1 C28 2.184(7) . ? Ru1 C35 2.190(8) . ? Ru1 C31 2.206(8) . ? Ru2 O1 2.112(5) . ? Ru2 N1 2.109(6) . ? Ru2 O2 2.110(6) . ? Ru2 C3 2.166(7) . ? Ru2 C5 2.171(8) . ? Ru2 C6 2.172(8) . ? Ru2 C7 2.194(7) . ? Ru2 C4 2.197(7) . ? Ru2 C8 2.192(7) . ? P1 F3 1.576(6) . ? P1 F5 1.580(5) . ? P1 F2 1.591(5) . ? P1 F6 1.617(5) . ? P1 F4 1.607(6) . ? P1 F1 1.596(5) . ? P2 F8 1.595(5) . ? P2 F7 1.595(5) . ? P2 F12 1.590(5) . ? P2 F11 1.599(5) . ? P2 F9 1.611(6) . ? P2 F10 1.607(5) . ? O1 C1 1.261(9) . ? O2 C2 1.264(8) . ? O3 C1 1.271(9) . ? O4 C2 1.257(9) . ? N1 C14 1.340(9) . ? N1 C13 1.331(9) . ? N2 C23 1.326(9) . ? N2 C26 1.345(9) . ? N2 Ru1 2.127(6) 3 ? C1 C2 1.516(11) . ? C3 C4 1.399(10) . ? C3 C6 1.427(11) . ? C4 C7 1.462(10) . ? C5 C6 1.401(10) . ? C5 C8 1.428(11) . ? C6 C12 1.492(11) . ? C7 C8 1.401(10) . ? C7 C9 1.503(11) . ? C9 C11 1.503(10) . ? C9 C10 1.526(12) . ? C13 C16 1.405(10) . ? C14 C15 1.378(10) . ? C15 C17 1.380(11) . ? C16 C17 1.390(11) . ? C16 C18 1.409(11) . ? C18 C19 1.204(10) . ? C19 C20 1.388(11) . ? C20 C21 1.184(10) . ? C21 C22 1.431(11) . ? C22 C24 1.398(10) . ? C22 C23 1.408(10) . ? C24 C25 1.374(10) . ? C25 C26 1.390(10) . ? C27 C28 1.436(10) . ? C27 C35 1.413(11) . ? C28 C29 1.414(11) . ? C28 C32 1.488(11) . ? C29 C30 1.428(11) . ? C30 C31 1.404(11) . ? C31 C35 1.444(11) . ? C31 C33 1.488(11) . ? C33 C36 1.496(12) . ? C33 C34 1.526(13) . ? O1N N1N 1.103(14) . ? O2N N1N 1.136(14) . ? N1N C1N 1.32(5) . ? 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 O4 Ru1 O3 78.8(2) . . ? O4 Ru1 N2 84.40(19) . 3 ? O3 Ru1 N2 81.7(2) . 3 ? O4 Ru1 C30 93.9(3) . . ? O3 Ru1 C30 151.3(2) . . ? N2 Ru1 C30 125.6(3) 3 . ? O4 Ru1 C29 94.8(2) . . ? O3 Ru1 C29 113.8(2) . . ? N2 Ru1 C29 164.1(3) 3 . ? C30 Ru1 C29 38.5(3) . . ? O4 Ru1 C27 158.6(2) . . ? O3 Ru1 C27 95.2(3) . . ? N2 Ru1 C27 115.3(2) 3 . ? C30 Ru1 C27 81.6(3) . . ? C29 Ru1 C27 68.7(3) . . ? O4 Ru1 C28 120.4(2) . . ? O3 Ru1 C28 90.3(3) . . ? N2 Ru1 C28 152.0(3) 3 . ? C30 Ru1 C28 69.3(3) . . ? C29 Ru1 C28 37.9(3) . . ? C27 Ru1 C28 38.5(3) . . ? O4 Ru1 C35 156.3(3) . . ? O3 Ru1 C35 124.4(3) . . ? N2 Ru1 C35 93.9(3) 3 . ? C30 Ru1 C35 68.0(3) . . ? C29 Ru1 C35 80.5(3) . . ? C27 Ru1 C35 37.8(3) . . ? C28 Ru1 C35 68.7(3) . . ? O4 Ru1 C31 118.4(3) . . ? O3 Ru1 C31 162.8(3) . . ? N2 Ru1 C31 97.5(3) 3 . ? C30 Ru1 C31 37.5(3) . . ? C29 Ru1 C31 68.9(3) . . ? C27 Ru1 C31 69.5(3) . . ? C28 Ru1 C31 82.4(3) . . ? C35 Ru1 C31 38.4(3) . . ? O1 Ru2 N1 84.48(18) . . ? O1 Ru2 O2 78.9(2) . . ? N1 Ru2 O2 82.6(2) . . ? O1 Ru2 C3 90.4(2) . . ? N1 Ru2 C3 151.0(3) . . ? O2 Ru2 C3 124.4(2) . . ? O1 Ru2 C5 127.2(3) . . ? N1 Ru2 C5 92.9(2) . . ? O2 Ru2 C5 153.1(3) . . ? C3 Ru2 C5 67.8(3) . . ? O1 Ru2 C6 96.6(2) . . ? N1 Ru2 C6 113.9(3) . . ? O2 Ru2 C6 162.6(2) . . ? C3 Ru2 C6 38.4(3) . . ? C5 Ru2 C6 37.7(3) . . ? O1 Ru2 C7 148.0(2) . . ? N1 Ru2 C7 125.3(2) . . ? O2 Ru2 C7 92.4(2) . . ? C3 Ru2 C7 69.0(3) . . ? C5 Ru2 C7 68.6(3) . . ? C6 Ru2 C7 82.5(3) . . ? O1 Ru2 C4 111.0(2) . . ? N1 Ru2 C4 164.2(2) . . ? O2 Ru2 C4 96.8(2) . . ? C3 Ru2 C4 37.4(3) . . ? C5 Ru2 C4 80.5(3) . . ? C6 Ru2 C4 69.0(3) . . ? C7 Ru2 C4 38.9(3) . . ? O1 Ru2 C8 165.1(3) . . ? N1 Ru2 C8 97.9(2) . . ? O2 Ru2 C8 115.9(3) . . ? C3 Ru2 C8 80.4(3) . . ? C5 Ru2 C8 38.2(3) . . ? C6 Ru2 C8 69.0(3) . . ? C7 Ru2 C8 37.2(3) . . ? C4 Ru2 C8 68.1(3) . . ? F3 P1 F5 92.1(4) . . ? F3 P1 F2 89.9(3) . . ? F5 P1 F2 178.0(4) . . ? F3 P1 F6 90.9(3) . . ? F5 P1 F6 90.4(3) . . ? F2 P1 F6 89.2(3) . . ? F3 P1 F4 178.4(3) . . ? F5 P1 F4 88.9(4) . . ? F2 P1 F4 89.1(3) . . ? F6 P1 F4 87.9(3) . . ? F3 P1 F1 89.8(3) . . ? F5 P1 F1 90.4(3) . . ? F2 P1 F1 90.0(3) . . ? F6 P1 F1 179.0(3) . . ? F4 P1 F1 91.5(3) . . ? F8 P2 F7 91.1(3) . . ? F8 P2 F12 179.0(3) . . ? F7 P2 F12 89.9(3) . . ? F8 P2 F11 89.3(3) . . ? F7 P2 F11 90.9(3) . . ? F12 P2 F11 90.7(3) . . ? F8 P2 F9 89.6(3) . . ? F7 P2 F9 89.1(3) . . ? F12 P2 F9 90.4(3) . . ? F11 P2 F9 178.9(3) . . ? F8 P2 F10 89.0(3) . . ? F7 P2 F10 179.7(3) . . ? F12 P2 F10 90.0(3) . . ? F11 P2 F10 89.3(3) . . ? F9 P2 F10 90.7(3) . . ? C1 O1 Ru2 113.2(4) . . ? C2 O2 Ru2 112.8(5) . . ? C1 O3 Ru1 113.1(5) . . ? C2 O4 Ru1 113.7(4) . . ? C14 N1 C13 117.4(6) . . ? C14 N1 Ru2 121.3(5) . . ? C13 N1 Ru2 121.3(5) . . ? C23 N2 C26 119.6(6) . . ? C23 N2 Ru1 118.0(5) . 3 ? C26 N2 Ru1 122.2(5) . 3 ? O1 C1 O3 125.5(7) . . ? O1 C1 C2 117.3(7) . . ? O3 C1 C2 117.2(8) . . ? O4 C2 O2 125.0(7) . . ? O4 C2 C1 117.1(7) . . ? O2 C2 C1 117.8(8) . . ? C4 C3 C6 122.3(7) . . ? C4 C3 Ru2 72.5(4) . . ? C6 C3 Ru2 71.1(4) . . ? C3 C4 C7 119.4(7) . . ? C3 C4 Ru2 70.1(4) . . ? C7 C4 Ru2 70.4(4) . . ? C6 C5 C8 121.7(7) . . ? C6 C5 Ru2 71.2(5) . . ? C8 C5 Ru2 71.7(5) . . ? C5 C6 C3 117.6(7) . . ? C5 C6 C12 121.3(8) . . ? C3 C6 C12 121.2(7) . . ? C5 C6 Ru2 71.1(5) . . ? C3 C6 Ru2 70.5(4) . . ? C12 C6 Ru2 128.0(5) . . ? C8 C7 C4 118.3(7) . . ? C8 C7 C9 124.3(7) . . ? C4 C7 C9 117.4(7) . . ? C8 C7 Ru2 71.3(4) . . ? C4 C7 Ru2 70.7(4) . . ? C9 C7 Ru2 128.0(5) . . ? C7 C8 C5 120.7(7) . . ? C7 C8 Ru2 71.4(4) . . ? C5 C8 Ru2 70.1(4) . . ? C11 C9 C7 107.7(7) . . ? C11 C9 C10 113.1(7) . . ? C7 C9 C10 113.3(7) . . ? N1 C13 C16 123.4(7) . . ? N1 C14 C15 123.5(7) . . ? C17 C15 C14 119.0(7) . . ? C17 C16 C13 117.7(7) . . ? C17 C16 C18 122.0(7) . . ? C13 C16 C18 120.2(7) . . ? C15 C17 C16 118.9(7) . . ? C19 C18 C16 178.8(8) . . ? C18 C19 C20 179.5(9) . . ? C21 C20 C19 177.2(9) . . ? C20 C21 C22 176.0(9) . . ? C24 C22 C23 118.0(7) . . ? C24 C22 C21 122.0(7) . . ? C23 C22 C21 120.0(7) . . ? N2 C23 C22 121.8(7) . . ? C25 C24 C22 119.8(7) . . ? C24 C25 C26 118.5(7) . . ? N2 C26 C25 122.3(7) . . ? C28 C27 C35 120.0(8) . . ? C28 C27 Ru1 71.2(4) . . ? C35 C27 Ru1 71.7(4) . . ? C29 C28 C27 118.4(7) . . ? C29 C28 C32 122.2(7) . . ? C27 C28 C32 119.1(8) . . ? C29 C28 Ru1 70.4(4) . . ? C27 C28 Ru1 70.3(4) . . ? C32 C28 Ru1 125.5(5) . . ? C28 C29 C30 120.9(7) . . ? C28 C29 Ru1 71.7(4) . . ? C30 C29 Ru1 70.4(4) . . ? C31 C30 C29 121.7(8) . . ? C31 C30 Ru1 73.1(5) . . ? C29 C30 Ru1 71.0(4) . . ? C30 C31 C35 117.2(7) . . ? C30 C31 C33 123.2(8) . . ? C35 C31 C33 119.6(8) . . ? C30 C31 Ru1 69.4(5) . . ? C35 C31 Ru1 70.2(5) . . ? C33 C31 Ru1 130.0(5) . . ? C31 C33 C36 114.4(7) . . ? C31 C33 C34 107.5(7) . . ? C36 C33 C34 113.3(9) . . ? C31 C35 C27 121.8(8) . . ? C31 C35 Ru1 71.4(4) . . ? C27 C35 Ru1 70.5(4) . . ? O1N N1N O2N 165(2) . . ? O1N N1N C1N 94(2) . . ? O2N N1N C1N 95(2) . . ? _diffrn_measured_fraction_theta_max 0.841 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.040 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.127