# 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 ? _publ_contact_author_email chanchal_bhaumik@yahoo.co.in _publ_contact_author_name 'Chanchal Bhaumik' loop_ _publ_author_name S.Baitalik C.Bhaumik S.Das D.Maity data_sbtru _database_code_depnum_ccdc_archive 'CCDC 842087' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl2 N10 O8 Ru' _chemical_formula_weight 1355.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fddd ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 23.6887(17) _cell_length_b 36.416(4) _cell_length_c 38.285(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 33027(5) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9864 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 19.23 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.090 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11104 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8721 _exptl_absorpt_correction_T_max 0.9139 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 94008 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7302 _reflns_number_gt 4531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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_extinction_coef ? _refine_ls_number_reflns 7302 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.2186 _refine_ls_wR_factor_gt 0.1818 _refine_ls_goodness_of_fit_ref 0.757 _refine_ls_restrained_S_all 0.757 _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 -0.1250 0.3750 0.013503(11) 0.05824(17) Uani 1 2 d S . . C1 C -0.18351(19) 0.42072(13) -0.04316(11) 0.0733(11) Uani 1 1 d . . . H1 H -0.2155 0.4067 -0.0386 0.088 Uiso 1 1 calc R . . C2 C -0.1861(2) 0.44659(14) -0.06907(14) 0.0898(15) Uani 1 1 d . . . H2 H -0.2191 0.4496 -0.0819 0.108 Uiso 1 1 calc R . . C3 C -0.1399(2) 0.46799(15) -0.07596(13) 0.0866(14) Uani 1 1 d . . . H3 H -0.1409 0.4856 -0.0935 0.104 Uiso 1 1 calc R . . C4 C -0.0913(2) 0.46267(12) -0.05598(12) 0.0763(12) Uani 1 1 d . . . H4 H -0.0596 0.4772 -0.0597 0.092 Uiso 1 1 calc R . . C5 C -0.09053(18) 0.43585(11) -0.03092(10) 0.0624(10) Uani 1 1 d . . . C6 C -0.1052(2) 0.31967(12) 0.07261(12) 0.0753(12) Uani 1 1 d . . . H6 H -0.1418 0.3115 0.0686 0.090 Uiso 1 1 calc R . . C7 C -0.0750(2) 0.30473(15) 0.09961(13) 0.0928(16) Uani 1 1 d . . . H7 H -0.0910 0.2864 0.1134 0.111 Uiso 1 1 calc R . . C8 C -0.0217(2) 0.31667(16) 0.10632(14) 0.1000(17) Uani 1 1 d . . . H8 H -0.0013 0.3070 0.1249 0.120 Uiso 1 1 calc R . . C9 C 0.0015(2) 0.34329(14) 0.08515(12) 0.0851(14) Uani 1 1 d . . . H9 H 0.0382 0.3514 0.0891 0.102 Uiso 1 1 calc R . . C10 C -0.02951(16) 0.35773(11) 0.05829(10) 0.0609(10) Uani 1 1 d . . . C11 C -0.00999(17) 0.38755(11) 0.03478(10) 0.0595(10) Uani 1 1 d . . . C12 C 0.04298(18) 0.40276(11) 0.03419(10) 0.0660(11) Uani 1 1 d . . . H12 H 0.0713 0.3934 0.0485 0.079 Uiso 1 1 calc R . . C13 C 0.05426(17) 0.43224(11) 0.01207(10) 0.0623(10) Uani 1 1 d . . . C14 C 0.01084(19) 0.44446(11) -0.00927(10) 0.0665(11) Uani 1 1 d . . . H14 H 0.0168 0.4644 -0.0240 0.080 Uiso 1 1 calc R . . C15 C -0.04104(17) 0.42739(10) -0.00891(9) 0.0550(9) Uani 1 1 d . . . C16 C 0.11096(18) 0.44986(12) 0.01219(11) 0.0675(11) Uani 1 1 d . . . C17 C 0.12921(19) 0.47307(16) -0.01508(12) 0.0822(14) Uani 1 1 d . . . H17 H 0.1055 0.4776 -0.0340 0.099 Uiso 1 1 calc R . . C18 C 0.1818(2) 0.48912(16) -0.01398(13) 0.0895(15) Uani 1 1 d . . . H18 H 0.1927 0.5044 -0.0322 0.107 Uiso 1 1 calc R . . C19 C 0.2189(2) 0.48333(13) 0.01318(13) 0.0785(13) Uani 1 1 d . . . C20 C 0.2006(2) 0.46019(14) 0.04025(14) 0.0904(15) Uani 1 1 d . . . H20 H 0.2242 0.4559 0.0592 0.108 Uiso 1 1 calc R . . C21 C 0.1484(2) 0.44387(13) 0.03906(12) 0.0831(13) Uani 1 1 d . . . H21 H 0.1379 0.4282 0.0571 0.100 Uiso 1 1 calc R . . C22 C 0.2730(2) 0.50193(14) 0.01441(14) 0.0832(14) Uani 1 1 d . . . C23 C 0.3453(2) 0.53339(17) 0.00129(17) 0.0974(16) Uani 1 1 d . . . C24 C 0.3560(2) 0.52054(15) 0.03414(17) 0.0944(16) Uani 1 1 d . . . C25 C 0.3820(2) 0.55843(17) -0.0200(2) 0.0969(17) Uani 1 1 d . . . C26 C 0.3777(2) 0.5579(2) -0.0552(2) 0.123(2) Uani 1 1 d . . . H26 H 0.3521 0.5420 -0.0656 0.147 Uiso 1 1 calc R . . C27 C 0.4106(3) 0.5807(2) -0.0764(2) 0.143(3) Uani 1 1 d . . . H27 H 0.4071 0.5800 -0.1006 0.171 Uiso 1 1 calc R . . C28 C 0.4201(3) 0.5822(2) -0.0059(2) 0.141(3) Uani 1 1 d . . . H28 H 0.4231 0.5836 0.0183 0.169 Uiso 1 1 calc R . . C29 C 0.4043(3) 0.52176(16) 0.0579(2) 0.1057(19) Uani 1 1 d . . . C30 C 0.4482(4) 0.6042(2) -0.0607(3) 0.153(4) Uani 1 1 d . . . H30 H 0.4695 0.6202 -0.0743 0.183 Uiso 1 1 calc R . . C31 C 0.4544(4) 0.6043(3) -0.0261(3) 0.164(4) Uani 1 1 d . . . H31 H 0.4816 0.6191 -0.0157 0.197 Uiso 1 1 calc R . . C32 C 0.4567(3) 0.5099(2) 0.0468(3) 0.168(3) Uani 1 1 d . . . H32 H 0.4605 0.5002 0.0244 0.201 Uiso 1 1 calc R . . C33 C 0.3987(4) 0.5326(2) 0.0922(3) 0.147(3) Uani 1 1 d . . . H33 H 0.3635 0.5391 0.1010 0.177 Uiso 1 1 calc R . . C36 C 0.4472(5) 0.5338(3) 0.1140(3) 0.181(4) Uani 1 1 d . . . H36 H 0.4429 0.5411 0.1371 0.217 Uiso 1 1 calc R . . C37 C 0.5048(4) 0.5122(4) 0.0686(4) 0.201(6) Uani 1 1 d . . . H37 H 0.5401 0.5053 0.0601 0.241 Uiso 1 1 calc R . . C38 C 0.4991(6) 0.5247(4) 0.1026(4) 0.196(6) Uani 1 1 d . . . H38 H 0.5303 0.5267 0.1172 0.235 Uiso 1 1 calc R . . Cl2 Cl 0.74272(7) 0.52836(5) 0.85946(4) 0.1052(5) Uani 1 1 d . . . N1 N -0.13753(14) 0.41465(9) -0.02418(8) 0.0631(8) Uani 1 1 d . . . N2 N -0.08347(14) 0.34590(8) 0.05169(8) 0.0596(8) Uani 1 1 d . . . N3 N -0.05063(13) 0.39944(8) 0.01347(7) 0.0542(7) Uani 1 1 d . . . N4 N 0.29462(19) 0.52267(12) -0.01046(12) 0.0940(13) Uani 1 1 d . . . N5 N 0.30849(18) 0.50039(12) 0.04217(13) 0.0941(12) Uani 1 1 d . . . H5 H 0.3024 0.4889 0.0614 0.113 Uiso 1 1 calc R . . O1 O 0.72338(19) 0.52021(15) 0.82570(11) 0.1346(16) Uani 1 1 d . . . O2 O 0.7081(3) 0.5261(3) 0.88527(16) 0.255(5) Uani 1 1 d . . . O3 O 0.7368(4) 0.5687(2) 0.8634(2) 0.183(4) Uani 0.70 1 d P . . O4 O 0.8009(3) 0.5275(3) 0.8607(2) 0.143(3) Uani 0.70 1 d P . . O3A O 0.7652(11) 0.4980(7) 0.8717(3) 0.386(18) Uani 0.60 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 0.0585(3) 0.0603(3) 0.0559(3) 0.000 0.000 -0.0052(2) C1 0.066(3) 0.079(3) 0.075(3) 0.002(2) -0.001(2) 0.000(2) C2 0.087(4) 0.091(3) 0.092(3) 0.020(3) -0.015(3) 0.010(3) C3 0.095(4) 0.087(3) 0.079(3) 0.015(3) -0.002(3) 0.002(3) C4 0.081(3) 0.074(3) 0.074(3) 0.015(2) -0.003(2) -0.002(2) C5 0.072(3) 0.057(2) 0.058(2) 0.0015(18) 0.009(2) -0.002(2) C6 0.075(3) 0.070(3) 0.081(3) 0.014(2) -0.007(2) -0.015(2) C7 0.091(4) 0.100(4) 0.087(3) 0.037(3) -0.008(3) -0.025(3) C8 0.090(4) 0.112(4) 0.097(4) 0.048(3) -0.019(3) -0.018(3) C9 0.070(3) 0.097(3) 0.088(3) 0.031(3) -0.010(3) -0.014(3) C10 0.055(2) 0.069(2) 0.058(2) 0.010(2) 0.0010(18) -0.002(2) C11 0.057(2) 0.060(2) 0.061(2) 0.0021(18) -0.0022(19) -0.0048(19) C12 0.065(3) 0.071(3) 0.062(2) 0.006(2) -0.005(2) -0.005(2) C13 0.056(2) 0.062(2) 0.068(3) 0.004(2) 0.007(2) -0.0037(19) C14 0.074(3) 0.061(2) 0.065(3) 0.015(2) 0.008(2) -0.002(2) C15 0.062(3) 0.053(2) 0.049(2) -0.0037(17) 0.0012(17) -0.0018(19) C16 0.067(3) 0.068(3) 0.067(3) 0.004(2) 0.006(2) -0.005(2) C17 0.075(3) 0.100(4) 0.072(3) 0.024(3) -0.001(2) -0.015(3) C18 0.071(3) 0.111(4) 0.086(3) 0.026(3) 0.008(3) -0.019(3) C19 0.064(3) 0.084(3) 0.087(3) 0.011(3) 0.006(2) -0.004(2) C20 0.076(3) 0.101(4) 0.094(4) 0.020(3) -0.011(3) -0.025(3) C21 0.087(3) 0.082(3) 0.081(3) 0.020(3) -0.005(3) -0.022(3) C22 0.067(3) 0.089(3) 0.093(4) 0.008(3) 0.009(3) -0.014(3) C23 0.063(3) 0.102(4) 0.127(5) 0.026(4) 0.007(3) -0.012(3) C24 0.073(3) 0.083(3) 0.127(5) 0.010(3) 0.000(3) -0.017(3) C25 0.076(4) 0.090(4) 0.126(5) 0.025(4) 0.015(3) 0.000(3) C26 0.075(4) 0.139(6) 0.154(7) 0.036(5) 0.022(4) -0.014(3) C27 0.088(5) 0.178(7) 0.162(7) 0.065(6) 0.040(5) 0.009(5) C28 0.139(6) 0.110(5) 0.173(7) 0.021(5) 0.029(5) -0.037(5) C29 0.076(4) 0.087(4) 0.154(6) 0.031(4) -0.002(4) -0.019(3) C30 0.100(6) 0.142(7) 0.217(10) 0.080(7) 0.044(6) -0.003(5) C31 0.142(7) 0.142(7) 0.209(9) 0.052(7) 0.007(7) -0.056(6) C32 0.084(5) 0.181(8) 0.239(10) 0.010(7) -0.004(6) 0.010(5) C33 0.131(6) 0.147(7) 0.164(8) 0.027(6) -0.043(6) -0.044(5) C36 0.169(9) 0.160(8) 0.214(10) 0.037(7) -0.091(9) -0.049(8) C37 0.072(6) 0.215(12) 0.317(16) 0.072(13) -0.033(9) 0.014(6) C38 0.129(9) 0.171(10) 0.288(17) 0.081(12) -0.069(12) -0.032(8) Cl2 0.0945(11) 0.1489(14) 0.0723(8) 0.0185(9) 0.0027(8) 0.0438(9) N1 0.071(2) 0.065(2) 0.0537(18) -0.0012(16) -0.0037(16) 0.0025(17) N2 0.059(2) 0.0592(18) 0.0608(19) 0.0051(15) 0.0006(15) -0.0010(15) N3 0.0583(19) 0.0533(17) 0.0511(17) -0.0003(14) 0.0002(14) 0.0031(15) N4 0.074(3) 0.096(3) 0.112(3) 0.018(3) 0.011(2) -0.018(2) N5 0.076(3) 0.097(3) 0.110(3) 0.021(3) 0.000(3) -0.018(2) O1 0.128(3) 0.184(4) 0.092(3) -0.018(3) -0.027(2) 0.057(3) O2 0.203(7) 0.461(15) 0.103(4) -0.005(6) 0.025(4) -0.110(8) O3 0.251(10) 0.124(6) 0.174(7) -0.024(5) -0.029(7) 0.072(6) O4 0.065(4) 0.250(10) 0.113(5) -0.031(6) -0.013(3) 0.021(4) O3A 0.54(3) 0.50(3) 0.121(8) 0.080(13) 0.064(14) 0.43(3) _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 N3 1.974(3) . ? Ru1 N3 1.974(3) 2_455 ? Ru1 N2 2.056(3) 2_455 ? Ru1 N2 2.056(3) . ? Ru1 N1 2.063(3) . ? Ru1 N1 2.063(3) 2_455 ? C1 N1 1.328(4) . ? C1 C2 1.370(6) . ? C2 C3 1.369(7) . ? C3 C4 1.397(7) . ? C4 C5 1.369(6) . ? C5 N1 1.379(4) . ? C5 C15 1.476(5) . ? C6 N2 1.349(4) . ? C6 C7 1.369(6) . ? C7 C8 1.360(7) . ? C8 C9 1.379(6) . ? C9 C10 1.369(6) . ? C10 N2 1.372(4) . ? C10 C11 1.484(5) . ? C11 N3 1.334(4) . ? C11 C12 1.372(5) . ? C12 C13 1.393(5) . ? C13 C14 1.387(6) . ? C13 C16 1.489(6) . ? C14 C15 1.377(5) . ? C15 N3 1.350(4) . ? C16 C21 1.375(5) . ? C16 C17 1.411(6) . ? C17 C18 1.377(6) . ? C18 C19 1.377(6) . ? C19 C20 1.404(6) . ? C19 C22 1.451(5) . ? C20 C21 1.373(5) . ? C22 N4 1.319(6) . ? C22 N5 1.356(6) . ? C23 N4 1.341(7) . ? C23 C24 1.365(8) . ? C23 C25 1.499(8) . ? C24 N5 1.377(6) . ? C24 C29 1.462(9) . ? C25 C26 1.353(9) . ? C25 C28 1.361(9) . ? C26 C27 1.399(9) . ? C27 C30 1.373(12) . ? C28 C31 1.381(10) . ? C29 C33 1.379(10) . ? C29 C32 1.381(10) . ? C30 C31 1.332(13) . ? C32 C37 1.415(14) . ? C33 C36 1.421(11) . ? C36 C38 1.345(16) . ? C37 C38 1.388(17) . ? Cl2 O2 1.286(6) . ? Cl2 O3A 1.312(14) . ? Cl2 O4 1.379(6) . ? Cl2 O1 1.403(4) . ? Cl2 O3 1.484(8) . ? O2 O3A 1.772(15) . ? O4 O3A 1.43(3) . ? 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 N3 Ru1 N3 179.9(2) . 2_455 ? N3 Ru1 N2 101.25(12) . 2_455 ? N3 Ru1 N2 78.80(12) 2_455 2_455 ? N3 Ru1 N2 78.80(12) . . ? N3 Ru1 N2 101.25(12) 2_455 . ? N2 Ru1 N2 89.37(18) 2_455 . ? N3 Ru1 N1 79.18(13) . . ? N3 Ru1 N1 100.76(13) 2_455 . ? N2 Ru1 N1 93.88(13) 2_455 . ? N2 Ru1 N1 157.96(13) . . ? N3 Ru1 N1 100.76(13) . 2_455 ? N3 Ru1 N1 79.18(13) 2_455 2_455 ? N2 Ru1 N1 157.96(13) 2_455 2_455 ? N2 Ru1 N1 93.88(13) . 2_455 ? N1 Ru1 N1 91.24(18) . 2_455 ? N1 C1 C2 123.2(4) . . ? C3 C2 C1 119.7(5) . . ? C2 C3 C4 118.4(5) . . ? C5 C4 C3 119.5(5) . . ? C4 C5 N1 121.4(4) . . ? C4 C5 C15 124.0(4) . . ? N1 C5 C15 114.7(3) . . ? N2 C6 C7 122.1(4) . . ? C8 C7 C6 120.0(4) . . ? C7 C8 C9 119.0(5) . . ? C10 C9 C8 119.8(4) . . ? C9 C10 N2 121.2(3) . . ? C9 C10 C11 124.7(4) . . ? N2 C10 C11 114.1(3) . . ? N3 C11 C12 121.3(3) . . ? N3 C11 C10 112.5(3) . . ? C12 C11 C10 126.2(4) . . ? C11 C12 C13 119.8(4) . . ? C14 C13 C12 117.6(4) . . ? C14 C13 C16 122.2(4) . . ? C12 C13 C16 120.2(4) . . ? C15 C14 C13 120.7(4) . . ? N3 C15 C14 119.8(3) . . ? N3 C15 C5 112.7(3) . . ? C14 C15 C5 127.5(3) . . ? C21 C16 C17 116.8(4) . . ? C21 C16 C13 121.0(3) . . ? C17 C16 C13 122.2(4) . . ? C18 C17 C16 120.6(4) . . ? C19 C18 C17 122.3(4) . . ? C18 C19 C20 117.0(4) . . ? C18 C19 C22 121.1(4) . . ? C20 C19 C22 121.9(4) . . ? C21 C20 C19 120.8(4) . . ? C20 C21 C16 122.5(3) . . ? N4 C22 N5 110.4(4) . . ? N4 C22 C19 126.0(5) . . ? N5 C22 C19 123.6(4) . . ? N4 C23 C24 112.0(5) . . ? N4 C23 C25 120.9(6) . . ? C24 C23 C25 127.0(5) . . ? C23 C24 N5 103.8(5) . . ? C23 C24 C29 134.9(5) . . ? N5 C24 C29 121.2(6) . . ? C26 C25 C28 116.9(6) . . ? C26 C25 C23 119.3(6) . . ? C28 C25 C23 123.8(7) . . ? C25 C26 C27 121.9(8) . . ? C30 C27 C26 118.4(8) . . ? C25 C28 C31 122.7(9) . . ? C33 C29 C32 118.0(8) . . ? C33 C29 C24 121.6(7) . . ? C32 C29 C24 120.2(8) . . ? C31 C30 C27 120.6(8) . . ? C30 C31 C28 119.3(9) . . ? C29 C32 C37 121.6(11) . . ? C29 C33 C36 119.4(10) . . ? C38 C36 C33 122.7(13) . . ? C38 C37 C32 119.6(12) . . ? C36 C38 C37 118.4(13) . . ? O2 Cl2 O3A 86.0(9) . . ? O2 Cl2 O4 127.5(5) . . ? O3A Cl2 O4 64.1(13) . . ? O2 Cl2 O1 119.1(4) . . ? O3A Cl2 O1 106.4(10) . . ? O4 Cl2 O1 110.7(4) . . ? O2 Cl2 O3 85.8(6) . . ? O3A Cl2 O3 146.7(13) . . ? O4 Cl2 O3 96.4(6) . . ? O1 Cl2 O3 105.8(4) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Ru1 128.1(2) . . ? C5 N1 Ru1 113.99(19) . . ? C6 N2 C10 117.9(3) . . ? C6 N2 Ru1 127.2(2) . . ? C10 N2 Ru1 114.51(18) . . ? C11 N3 C15 120.8(2) . . ? C11 N3 Ru1 119.83(18) . . ? C15 N3 Ru1 119.39(19) . . ? C22 N4 C23 105.8(5) . . ? C22 N5 C24 108.0(5) . . ? Cl2 O2 O3A 47.6(7) . . ? Cl2 O4 O3A 55.6(6) . . ? Cl2 O3A O4 60.2(11) . . ? Cl2 O3A O2 46.4(5) . . ? O4 O3A O2 96.0(13) . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.129 0.125 0.125 1322 264 ' ' 2 0.379 -0.125 0.375 1322 265 ' ' 3 0.629 0.125 0.625 1322 264 ' ' 4 0.879 -0.125 0.875 1322 265 ' ' 5 0.875 0.098 0.375 24 6 ' ' 6 0.375 0.098 0.875 24 6 ' ' 7 0.375 0.152 0.375 24 6 ' ' 8 0.875 0.152 0.875 24 6 ' ' 9 0.871 0.375 0.375 1322 265 ' ' 10 0.371 0.375 0.875 1322 265 ' ' 11 0.625 0.348 0.125 23 6 ' ' 12 0.125 0.348 0.625 23 6 ' ' 13 0.125 0.402 0.125 24 6 ' ' 14 0.625 0.402 0.625 24 6 ' ' 15 0.629 0.625 0.125 1322 264 ' ' 16 0.129 0.625 0.625 1322 264 ' ' 17 0.375 0.598 0.375 24 6 ' ' 18 0.875 0.598 0.875 24 6 ' ' 19 0.875 0.652 0.375 24 6 ' ' 20 0.375 0.652 0.875 24 6 ' ' 21 0.125 0.848 0.125 23 6 ' ' 22 0.625 0.848 0.625 23 6 ' ' 23 0.625 0.902 0.125 24 6 ' ' 24 0.125 0.902 0.625 24 6 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.697 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.059 # Attachment '2.cif' data_q _database_code_depnum_ccdc_archive 'CCDC 842088' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl2 N10 O8 Os' _chemical_formula_weight 1444.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 36.393(7) _cell_length_b 37.524(12) _cell_length_c 23.564(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32179(14) _cell_formula_units_Z 16 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9913 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 19.28 _exptl_crystal_description rectangular _exptl_crystal_colour black _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11616 _exptl_absorpt_coefficient_mu 1.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5637 _exptl_absorpt_correction_T_max 0.6657 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 90724 _diffrn_reflns_av_R_equivalents 0.1229 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7105 _reflns_number_gt 4253 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2002)' _computing_publication_material 'SHELXTL (Bruker, 2002)' _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^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_extinction_coef ? _refine_ls_number_reflns 7105 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.3750 0.014399(9) 0.3750 0.05973(14) Uani 1 2 d S . . C1 C 0.42942(16) 0.07445(18) 0.3535(3) 0.0771(19) Uani 1 1 d . . . H1 H 0.4369 0.0710 0.3908 0.093 Uiso 1 1 calc R . . C2 C 0.44544(18) 0.10116(19) 0.3227(3) 0.088(2) Uani 1 1 d . . . H2 H 0.4647 0.1142 0.3382 0.105 Uiso 1 1 calc R . . C3 C 0.4331(2) 0.1088(2) 0.2688(3) 0.099(2) Uani 1 1 d . . . H3 H 0.4422 0.1281 0.2484 0.119 Uiso 1 1 calc R . . C4 C 0.40666(17) 0.08636(17) 0.2465(3) 0.0790(19) Uani 1 1 d . . . H4 H 0.3987 0.0897 0.2094 0.095 Uiso 1 1 calc R . . C5 C 0.39216(15) 0.05939(16) 0.2783(2) 0.0618(15) Uani 1 1 d . . . C6 C 0.36224(14) 0.03555(15) 0.2577(3) 0.0600(15) Uani 1 1 d . . . C7 C 0.34662(14) 0.03433(15) 0.2050(2) 0.0622(15) Uani 1 1 d . . . H7 H 0.3555 0.0490 0.1763 0.075 Uiso 1 1 calc R . . C8 C 0.31765(14) 0.01145(15) 0.1940(2) 0.0570(14) Uani 1 1 d . . . C9 C 0.30543(14) -0.01027(15) 0.2383(3) 0.0604(15) Uani 1 1 d . . . H9 H 0.2860 -0.0258 0.2321 0.072 Uiso 1 1 calc R . . C10 C 0.32159(14) -0.00902(14) 0.2906(2) 0.0535(14) Uani 1 1 d . . . C11 C 0.31327(15) -0.03131(17) 0.3410(3) 0.0653(16) Uani 1 1 d . . . C12 C 0.28594(16) -0.05582(17) 0.3432(3) 0.0729(17) Uani 1 1 d . . . H12 H 0.2709 -0.0596 0.3119 0.087 Uiso 1 1 calc R . . C13 C 0.28057(19) -0.07541(19) 0.3930(3) 0.088(2) Uani 1 1 d . . . H13 H 0.2624 -0.0928 0.3948 0.105 Uiso 1 1 calc R . . C14 C 0.30232(19) -0.06860(19) 0.4391(3) 0.088(2) Uani 1 1 d . . . H14 H 0.2989 -0.0813 0.4726 0.106 Uiso 1 1 calc R . . C15 C 0.32971(17) -0.04253(16) 0.4358(3) 0.0743(17) Uani 1 1 d . . . H15 H 0.3443 -0.0378 0.4673 0.089 Uiso 1 1 calc R . . C16 C 0.29963(15) 0.01120(16) 0.1366(3) 0.0656(17) Uani 1 1 d . . . C17 C 0.30685(16) 0.03813(19) 0.0971(3) 0.0786(19) Uani 1 1 d . . . H17 H 0.3230 0.0563 0.1071 0.094 Uiso 1 1 calc R . . C18 C 0.29121(17) 0.0389(2) 0.0445(3) 0.088(2) Uani 1 1 d . . . H18 H 0.2974 0.0570 0.0193 0.106 Uiso 1 1 calc R . . C19 C 0.26649(18) 0.0131(2) 0.0285(3) 0.0786(19) Uani 1 1 d . . . C20 C 0.25976(18) -0.01478(18) 0.0659(3) 0.083(2) Uani 1 1 d . . . H20 H 0.2444 -0.0333 0.0545 0.099 Uiso 1 1 calc R . . C21 C 0.2754(2) -0.01599(17) 0.1204(3) 0.0810(19) Uani 1 1 d . . . H21 H 0.2697 -0.0345 0.1452 0.097 Uiso 1 1 calc R . . C22 C 0.24782(19) 0.0149(2) -0.0262(3) 0.094(2) Uani 1 1 d . . . C23 C 0.2293(2) 0.0364(2) -0.1106(3) 0.097(2) Uani 1 1 d . . . C24 C 0.2147(2) 0.0029(3) -0.1016(3) 0.098(2) Uani 1 1 d . . . C25 C 0.1909(2) -0.0188(3) -0.1359(4) 0.109(3) Uani 1 1 d . . . C26 C 0.1679(3) -0.0031(3) -0.1773(4) 0.157(4) Uani 1 1 d . . . H26 H 0.1672 0.0216 -0.1806 0.189 Uiso 1 1 calc R . . C27 C 0.1469(4) -0.0231(4) -0.2121(6) 0.174(6) Uani 1 1 d . . . H27 H 0.1338 -0.0123 -0.2412 0.208 Uiso 1 1 calc R . . C28 C 0.1449(3) -0.0587(5) -0.2050(5) 0.155(5) Uani 1 1 d . . . H28 H 0.1289 -0.0721 -0.2273 0.186 Uiso 1 1 calc R . . C29 C 0.1670(3) -0.0759(3) -0.1637(4) 0.140(4) Uani 1 1 d . . . H29 H 0.1659 -0.1005 -0.1592 0.168 Uiso 1 1 calc R . . C30 C 0.1907(3) -0.0551(3) -0.1295(3) 0.115(3) Uani 1 1 d . . . H30 H 0.2059 -0.0660 -0.1030 0.138 Uiso 1 1 calc R . . C31 C 0.2271(2) 0.0625(3) -0.1574(3) 0.110(3) Uani 1 1 d . . . C32 C 0.2148(3) 0.0962(3) -0.1499(5) 0.151(4) Uiso 1 1 d . . . H32 H 0.2076 0.1035 -0.1140 0.181 Uiso 1 1 calc R . . C33 C 0.2129(3) 0.1215(3) -0.1977(6) 0.167(4) Uiso 1 1 d . . . H33 H 0.2048 0.1449 -0.1945 0.201 Uiso 1 1 calc R . . C34 C 0.2246(3) 0.1057(3) -0.2488(5) 0.158(4) Uiso 1 1 d . . . H34 H 0.2242 0.1206 -0.2804 0.190 Uiso 1 1 calc R . . C35 C 0.2355(3) 0.0750(3) -0.2582(5) 0.163(4) Uiso 1 1 d . . . H35 H 0.2402 0.0677 -0.2952 0.196 Uiso 1 1 calc R . . C36 C 0.2409(3) 0.0506(3) -0.2118(5) 0.156(4) Uiso 1 1 d . . . H36 H 0.2525 0.0287 -0.2165 0.187 Uiso 1 1 calc R . . Cl1 Cl 0.27868(7) 0.10874(6) 0.25708(9) 0.0988(6) Uani 1 1 d . . . N1 N 0.40334(11) 0.05307(11) 0.3320(2) 0.0607(12) Uani 1 1 d . . . N2 N 0.35019(11) 0.01418(11) 0.30080(19) 0.0543(11) Uani 1 1 d . . . N3 N 0.33530(13) -0.02409(12) 0.3873(2) 0.0636(13) Uani 1 1 d . . . N4 N 0.22705(16) -0.01049(17) -0.0482(3) 0.098(2) Uani 1 1 d . . . N5 N 0.24954(16) 0.0439(2) -0.0623(3) 0.0995(19) Uani 1 1 d . . . H5 H 0.2612 0.0634 -0.0557 0.119 Uiso 1 1 calc R . . O1 O 0.27177(14) 0.07391(14) 0.2769(2) 0.1072(16) Uani 1 1 d . . . O2 O 0.2773(2) 0.11279(16) 0.1993(3) 0.148(3) Uani 1 1 d . . . O3 O 0.3126(4) 0.1187(3) 0.2739(5) 0.293(8) Uani 1 1 d . . . O4 O 0.2641(5) 0.1333(2) 0.2825(6) 0.312(9) Uani 1 1 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 Os1 0.05422(19) 0.0625(2) 0.0625(2) 0.000 -0.00458(17) 0.000 C1 0.069(4) 0.088(5) 0.075(4) 0.002(4) -0.022(3) -0.019(4) C2 0.073(4) 0.091(5) 0.099(6) 0.012(5) -0.016(4) -0.032(4) C3 0.095(5) 0.111(6) 0.093(6) 0.029(5) -0.023(4) -0.041(5) C4 0.081(4) 0.092(5) 0.065(4) 0.014(4) -0.013(3) -0.031(4) C5 0.054(3) 0.078(4) 0.054(4) 0.011(3) -0.009(3) -0.015(3) C6 0.050(3) 0.059(4) 0.071(4) 0.003(3) -0.003(3) -0.004(3) C7 0.054(3) 0.074(4) 0.058(4) 0.011(3) -0.005(3) -0.006(3) C8 0.050(3) 0.062(4) 0.059(4) -0.001(3) 0.002(3) -0.001(3) C9 0.049(3) 0.064(4) 0.068(4) -0.010(3) -0.004(3) -0.008(3) C10 0.048(3) 0.052(4) 0.060(4) -0.001(3) 0.000(3) -0.003(2) C11 0.059(4) 0.072(4) 0.064(4) -0.006(3) -0.009(3) -0.005(3) C12 0.061(4) 0.085(5) 0.072(5) -0.003(4) -0.002(3) -0.012(3) C13 0.079(5) 0.088(5) 0.097(6) 0.006(4) 0.019(4) -0.024(4) C14 0.082(5) 0.098(5) 0.085(5) 0.019(4) 0.012(4) -0.026(4) C15 0.078(4) 0.075(4) 0.071(4) 0.000(4) 0.000(3) 0.009(4) C16 0.053(3) 0.074(4) 0.071(4) -0.008(3) -0.009(3) -0.008(3) C17 0.062(4) 0.093(5) 0.080(5) 0.010(4) -0.013(4) -0.020(3) C18 0.063(4) 0.126(6) 0.076(5) 0.007(4) -0.018(4) -0.020(4) C19 0.075(4) 0.109(6) 0.051(4) -0.007(4) -0.006(3) -0.009(4) C20 0.080(4) 0.096(5) 0.072(5) -0.012(4) -0.011(4) -0.022(4) C21 0.089(5) 0.083(5) 0.071(5) -0.002(4) -0.009(4) -0.017(4) C22 0.073(5) 0.129(7) 0.079(5) -0.003(5) -0.010(4) -0.008(5) C23 0.094(5) 0.117(7) 0.079(6) -0.005(5) -0.015(4) -0.022(5) C24 0.087(5) 0.140(7) 0.067(5) -0.019(5) -0.007(4) -0.019(5) C25 0.082(5) 0.142(8) 0.103(7) -0.015(6) 0.005(5) -0.034(5) C26 0.114(7) 0.218(11) 0.139(9) -0.020(8) -0.057(7) -0.034(8) C27 0.148(10) 0.210(14) 0.163(12) -0.003(11) -0.050(9) -0.053(10) C28 0.087(6) 0.281(17) 0.098(8) -0.058(10) -0.021(6) -0.040(10) C29 0.141(8) 0.166(9) 0.114(8) -0.061(7) 0.017(7) -0.062(8) C30 0.133(7) 0.129(8) 0.082(6) -0.033(6) -0.001(5) -0.017(6) C31 0.093(6) 0.171(9) 0.066(5) -0.012(6) -0.009(4) -0.034(6) Cl1 0.1325(17) 0.0747(13) 0.0892(15) 0.0031(12) -0.0457(13) 0.0212(13) N1 0.056(3) 0.061(3) 0.066(3) 0.000(2) -0.007(2) -0.005(2) N2 0.048(2) 0.050(3) 0.065(3) 0.002(2) 0.004(2) -0.002(2) N3 0.065(3) 0.052(3) 0.074(4) 0.000(2) 0.005(2) 0.006(2) N4 0.081(4) 0.136(6) 0.077(4) -0.037(4) -0.009(3) -0.026(4) N5 0.089(4) 0.134(6) 0.076(4) -0.002(4) -0.017(3) -0.012(4) O1 0.124(4) 0.097(4) 0.101(4) 0.024(3) -0.035(3) -0.021(3) O2 0.223(7) 0.132(5) 0.091(4) 0.036(4) -0.064(4) -0.055(5) O3 0.372(15) 0.183(9) 0.322(13) 0.130(9) -0.257(13) -0.151(10) O4 0.50(2) 0.134(7) 0.303(14) 0.080(7) 0.209(15) 0.140(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 N2 1.968(4) 12 ? Os1 N2 1.968(4) . ? Os1 N1 2.048(4) . ? Os1 N1 2.048(4) 12 ? Os1 N3 2.063(5) 12 ? Os1 N3 2.063(5) . ? C1 N1 1.341(6) . ? C1 C2 1.367(8) . ? C1 H1 0.9300 . ? C2 C3 1.377(9) . ? C2 H2 0.9300 . ? C3 C4 1.384(8) . ? C3 H3 0.9300 . ? C4 C5 1.365(7) . ? C4 H4 0.9300 . ? C5 N1 1.352(6) . ? C5 C6 1.490(7) . ? C6 N2 1.366(6) . ? C6 C7 1.368(7) . ? C7 C8 1.384(7) . ? C7 H7 0.9300 . ? C8 C9 1.398(7) . ? C8 C16 1.503(8) . ? C9 C10 1.366(7) . ? C9 H9 0.9300 . ? C10 N2 1.378(5) . ? C10 C11 1.484(8) . ? C11 C12 1.356(8) . ? C11 N3 1.382(6) . ? C12 C13 1.399(9) . ? C12 H12 0.9300 . ? C13 C14 1.368(9) . ? C13 H13 0.9300 . ? C14 C15 1.399(8) . ? C14 H14 0.9300 . ? C15 N3 1.350(6) . ? C15 H15 0.9300 . ? C16 C17 1.398(8) . ? C16 C21 1.402(6) . ? C17 C18 1.364(8) . ? C17 H17 0.9300 . ? C18 C19 1.373(8) . ? C18 H18 0.9300 . ? C19 C20 1.391(8) . ? C19 C22 1.459(7) . ? C20 C21 1.404(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 N4 1.321(8) . ? C22 N5 1.382(9) . ? C23 C24 1.380(11) . ? C23 N5 1.385(8) . ? C23 C31 1.478(11) . ? C24 N4 1.428(10) . ? C24 C25 1.436(11) . ? C25 C30 1.372(11) . ? C25 C26 1.414(12) . ? C26 C27 1.348(14) . ? C26 H26 0.9300 . ? C27 C28 1.348(15) . ? C27 H27 0.9300 . ? C28 C29 1.417(15) . ? C28 H28 0.9300 . ? C29 C30 1.415(11) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.352(12) . ? C31 C36 1.447(12) . ? C32 C33 1.475(13) . ? C32 H32 0.9300 . ? C33 C34 1.410(14) . ? C33 H33 0.9300 . ? C34 C35 1.237(13) . ? C34 H34 0.9300 . ? C35 C36 1.440(13) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? Cl1 O4 1.221(9) . ? Cl1 O3 1.348(9) . ? Cl1 O2 1.371(6) . ? Cl1 O1 1.410(5) . ? N5 H5 0.8600 . ? 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 N2 Os1 N2 179.5(2) 12 . ? N2 Os1 N1 102.18(17) 12 . ? N2 Os1 N1 78.16(17) . . ? N2 Os1 N1 78.16(17) 12 12 ? N2 Os1 N1 102.18(17) . 12 ? N1 Os1 N1 89.8(2) . 12 ? N2 Os1 N3 78.53(18) 12 12 ? N2 Os1 N3 101.13(18) . 12 ? N1 Os1 N3 94.22(17) . 12 ? N1 Os1 N3 156.68(18) 12 12 ? N2 Os1 N3 101.13(18) 12 . ? N2 Os1 N3 78.53(18) . . ? N1 Os1 N3 156.68(18) . . ? N1 Os1 N3 94.22(17) 12 . ? N3 Os1 N3 91.2(2) 12 . ? N1 C1 C2 122.7(6) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 120.2(6) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 116.8(7) . . ? C2 C3 H3 121.6 . . ? C4 C3 H3 121.6 . . ? C5 C4 C3 120.8(6) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C6 114.8(4) . . ? C4 C5 C6 123.3(5) . . ? N2 C6 C7 121.5(5) . . ? N2 C6 C5 110.2(5) . . ? C7 C6 C5 128.2(5) . . ? C6 C7 C8 120.5(5) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C7 C8 C9 117.6(5) . . ? C7 C8 C16 120.3(5) . . ? C9 C8 C16 122.0(5) . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 N2 120.3(5) . . ? C9 C10 C11 127.9(5) . . ? N2 C10 C11 111.7(4) . . ? C12 C11 N3 121.9(6) . . ? C12 C11 C10 124.2(5) . . ? N3 C11 C10 113.8(4) . . ? C11 C12 C13 119.4(6) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.2(6) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? N3 C15 C14 120.9(6) . . ? N3 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C17 C16 C21 117.6(5) . . ? C17 C16 C8 120.8(5) . . ? C21 C16 C8 121.6(5) . . ? C18 C17 C16 122.7(6) . . ? C18 C17 H17 118.6 . . ? C16 C17 H17 118.6 . . ? C17 C18 C19 120.6(7) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C20 118.1(6) . . ? C18 C19 C22 121.1(6) . . ? C20 C19 C22 120.8(5) . . ? C19 C20 C21 122.2(5) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 118.7(5) . . ? C16 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? N4 C22 N5 110.7(7) . . ? N4 C22 C19 125.5(8) . . ? N5 C22 C19 123.8(7) . . ? C24 C23 N5 105.3(7) . . ? C24 C23 C31 134.1(7) . . ? N5 C23 C31 120.6(8) . . ? C23 C24 N4 109.5(7) . . ? C23 C24 C25 131.4(9) . . ? N4 C24 C25 119.1(8) . . ? C30 C25 C26 118.9(9) . . ? C30 C25 C24 120.3(9) . . ? C26 C25 C24 120.7(10) . . ? C27 C26 C25 121.6(12) . . ? C27 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C26 C27 C28 120.5(14) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C29 120.3(11) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 119.0(11) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C25 C30 C29 119.4(10) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C31 C36 121.2(11) . . ? C32 C31 C23 122.7(9) . . ? C36 C31 C23 116.0(10) . . ? C31 C32 C33 121.3(12) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 111.5(12) . . ? C34 C33 H33 124.3 . . ? C32 C33 H33 124.3 . . ? C35 C34 C33 129.8(14) . . ? C35 C34 H34 115.1 . . ? C33 C34 H34 115.1 . . ? C34 C35 C36 120.1(13) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 115.3(11) . . ? C35 C36 H36 122.3 . . ? C31 C36 H36 122.3 . . ? O4 Cl1 O3 92.5(9) . . ? O4 Cl1 O2 112.8(7) . . ? O3 Cl1 O2 107.1(6) . . ? O4 Cl1 O1 117.5(6) . . ? O3 Cl1 O1 108.9(4) . . ? O2 Cl1 O1 115.1(3) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Os1 126.5(3) . . ? C5 N1 Os1 115.8(2) . . ? C6 N2 C10 118.9(3) . . ? C6 N2 Os1 120.7(3) . . ? C10 N2 Os1 120.3(3) . . ? C15 N3 C11 118.7(4) . . ? C15 N3 Os1 125.7(3) . . ? C11 N3 Os1 115.6(3) . . ? C22 N4 C24 105.8(7) . . ? C22 N5 C23 108.7(7) . . ? C22 N5 H5 125.7 . . ? C23 N5 H5 125.7 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.010 0.125 0.625 14 0 ' ' 2 0.010 0.375 0.875 15 3 ' ' 3 -0.010 0.625 0.125 14 0 ' ' 4 0.010 0.875 0.375 15 3 ' ' 5 0.125 0.125 0.637 1206 273 ' ' 6 0.125 0.625 0.137 1206 273 ' ' 7 0.098 0.375 0.375 24 9 ' ' 8 0.098 0.875 0.875 24 9 ' ' 9 0.152 0.375 0.875 24 8 ' ' 10 0.152 0.875 0.375 24 8 ' ' 11 0.240 0.375 0.375 14 1 ' ' 12 0.240 0.875 0.875 14 1 ' ' 13 0.266 0.125 0.625 12 1 ' ' 14 0.266 0.625 0.125 12 1 ' ' 15 0.375 0.375 0.362 1207 275 ' ' 16 0.375 0.875 0.862 1207 275 ' ' 17 0.348 0.125 0.125 24 9 ' ' 18 0.348 0.625 0.625 24 9 ' ' 19 0.402 0.125 0.625 24 8 ' ' 20 0.402 0.625 0.125 24 8 ' ' 21 0.490 0.125 0.125 14 0 ' ' 22 0.490 0.625 0.625 14 0 ' ' 23 0.516 0.375 0.375 12 2 ' ' 24 0.516 0.875 0.875 12 2 ' ' 25 0.625 0.125 0.137 1206 273 ' ' 26 0.625 0.625 0.637 1206 273 ' ' 27 0.598 0.375 0.875 24 9 ' ' 28 0.598 0.875 0.375 24 9 ' ' 29 0.652 0.375 0.375 24 8 ' ' 30 0.652 0.875 0.875 24 8 ' ' 31 0.740 0.375 0.875 14 1 ' ' 32 0.740 0.875 0.375 14 1 ' ' 33 0.766 0.125 0.125 12 1 ' ' 34 0.766 0.625 0.625 12 1 ' ' 35 0.875 0.375 0.862 1203 275 ' ' 36 0.875 0.875 0.362 1203 275 ' ' 37 0.848 0.125 0.625 24 9 ' ' 38 0.848 0.625 0.125 24 9 ' ' 39 0.902 0.125 0.125 24 8 ' ' 40 0.902 0.625 0.625 24 8 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.780 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.080