# 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 _publ_contact_author ; Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_contact_letter ; This CIF contains details of the crystal structure in the paper ?Solvent-dependent modulation...' by A. B. Wragg et al., submitted to Dalton Trans. for publication. ; _publ_author_name M.Ward _publ_contact_author_name 'Mike Ward' #======================================================== data_imw1303p-1 _database_code_depnum_ccdc_archive 'CCDC 881320' #TrackingRef '- Ru2bppz_imw1303p-1_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H25 K4 N12 O7.50 Os Ru' _chemical_formula_weight 1025.21 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' K K 0.2009 0.2494 '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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7726(5) _cell_length_b 11.7903(6) _cell_length_c 13.7730(6) _cell_angle_alpha 81.743(3) _cell_angle_beta 79.366(3) _cell_angle_gamma 77.395(3) _cell_volume 1668.09(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 994 _exptl_absorpt_coefficient_mu 4.818 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.35 _exptl_absorpt_correction_T_max 0.59 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27714 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 30.53 _reflns_number_total 10092 _reflns_number_gt 7672 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. The 18 restraints are ossiated with isotropic restraints (ISOR) on three Atoms K1, O4, O5 which were needed to prevent the thermal ellipsoids from becoming unrealistically eccentric ; _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^)+(0.1038P)^2^+5.9936P] 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_extinction_coef ? _refine_ls_number_reflns 10092 _refine_ls_number_parameters 427 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1707 _refine_ls_wR_factor_gt 0.1513 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.047 _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 Os1 Os 0.41694(3) 0.66532(3) -0.26588(3) 0.01045(10) Uani 0.50 1 d P . . Ru1 Ru 0.41694(3) 0.66532(3) -0.26588(3) 0.01045(10) Uani 0.50 1 d P . . Os2 Os 0.17478(3) 0.92418(3) 0.17610(2) 0.00889(9) Uani 0.50 1 d P . . Ru2 Ru 0.17478(3) 0.92418(3) 0.17610(2) 0.00889(9) Uani 0.50 1 d P . . C2 C 0.6619(7) 0.5313(6) -0.1860(6) 0.0162(13) Uani 1 1 d . . . H2A H 0.6845 0.5035 -0.2480 0.019 Uiso 1 1 calc R . . C3 C 0.7405(7) 0.4849(6) -0.1143(6) 0.0170(14) Uani 1 1 d . . . H3A H 0.8160 0.4304 -0.1291 0.020 Uiso 1 1 calc R . . C4 C 0.7027(7) 0.5225(6) -0.0197(5) 0.0131(12) Uani 1 1 d . . . H4A H 0.7508 0.4913 0.0309 0.016 Uiso 1 1 calc R . . C5 C 0.5929(7) 0.6067(6) -0.0029(5) 0.0127(12) Uani 1 1 d . . . H5A H 0.5658 0.6323 0.0598 0.015 Uiso 1 1 calc R . . C6 C 0.5223(6) 0.6538(5) -0.0787(5) 0.0094(11) Uani 1 1 d . . . C8 C 0.3996(6) 0.7366(5) -0.0646(5) 0.0111(12) Uani 1 1 d . . . C9 C 0.3568(6) 0.8104(5) 0.0127(5) 0.0098(11) Uani 1 1 d . . . C11 C 0.1482(6) 0.8368(6) -0.0210(5) 0.0121(12) Uani 1 1 d . . . H11A H 0.0598 0.8611 -0.0032 0.014 Uiso 1 1 calc R . . C12 C 0.1948(7) 0.7865(6) -0.1078(5) 0.0142(13) Uani 1 1 d . . . H12A H 0.1389 0.7889 -0.1524 0.017 Uiso 1 1 calc R . . C14 C 0.4417(7) 0.9586(6) 0.1973(5) 0.0146(13) Uani 1 1 d . . . H14A H 0.3974 0.9959 0.2523 0.017 Uiso 1 1 calc R . . C15 C 0.5745(7) 0.9546(6) 0.1708(5) 0.0146(13) Uani 1 1 d . . . H15A H 0.6187 0.9862 0.2088 0.017 Uiso 1 1 calc R . . C16 C 0.6384(7) 0.9024(6) 0.0866(5) 0.0125(12) Uani 1 1 d . . . H16A H 0.7260 0.9003 0.0664 0.015 Uiso 1 1 calc R . . C17 C 0.5705(6) 0.8533(5) 0.0326(5) 0.0121(12) Uani 1 1 d . . . H17A H 0.6119 0.8193 -0.0247 0.015 Uiso 1 1 calc R . . C18 C 0.4403(6) 0.8555(5) 0.0652(5) 0.0080(11) Uani 1 1 d . . . C21 C 0.3775(7) 0.5004(6) -0.2375(5) 0.0155(13) Uani 1 1 d . . . C22 C 0.2704(7) 0.7129(6) -0.3412(5) 0.0149(13) Uani 1 1 d . . . C23 C 0.5315(6) 0.6088(6) -0.3872(5) 0.0116(12) Uani 1 1 d . . . C24 C 0.4757(7) 0.8184(6) -0.3169(5) 0.0152(13) Uani 1 1 d . . . C31 C 0.1539(7) 0.9899(6) 0.3042(5) 0.0157(13) Uani 1 1 d . . . C32 C -0.0134(7) 0.9260(6) 0.1954(6) 0.0172(14) Uani 1 1 d . . . C33 C 0.1451(7) 1.0943(6) 0.1162(5) 0.0148(13) Uani 1 1 d . . . C34 C 0.1938(6) 0.7640(6) 0.2556(5) 0.0129(12) Uani 1 1 d . . . N1 N 0.5558(5) 0.6136(5) -0.1701(4) 0.0115(10) Uani 1 1 d . . . N7 N 0.3194(5) 0.7335(5) -0.1304(4) 0.0098(10) Uani 1 1 d . . . N10 N 0.2278(5) 0.8518(5) 0.0387(4) 0.0093(10) Uani 1 1 d . . . N13 N 0.3763(5) 0.9098(5) 0.1454(4) 0.0107(10) Uani 1 1 d . . . N21 N 0.3670(7) 0.4041(6) -0.2341(5) 0.0249(15) Uani 1 1 d . . . N22 N 0.1833(7) 0.7388(6) -0.3841(6) 0.0259(15) Uani 1 1 d . . . N23 N 0.6006(7) 0.5788(6) -0.4581(5) 0.0205(13) Uani 1 1 d . . . N24 N 0.5170(7) 0.8987(6) -0.3596(5) 0.0219(13) Uani 1 1 d . . . N31 N 0.1457(6) 1.0308(6) 0.3783(5) 0.0193(13) Uani 1 1 d . . . N32 N -0.1232(7) 0.9204(7) 0.2145(6) 0.0283(16) Uani 1 1 d . . . N33 N 0.1252(6) 1.1943(6) 0.0899(5) 0.0228(14) Uani 1 1 d . . . N34 N 0.1987(7) 0.6790(5) 0.3085(5) 0.0217(13) Uani 1 1 d . . . K1 K 0.8181(4) 0.5399(3) 0.3907(3) 0.0758(10) Uani 1 1 d U . . K2 K -0.12936(17) 1.00692(15) 0.41504(13) 0.0216(3) Uani 1 1 d . . . K3 K 0.4205(2) 0.66968(15) 0.40145(15) 0.0278(4) Uani 1 1 d . . . K4 K 0.78400(18) 0.74767(15) -0.40559(15) 0.0263(4) Uani 1 1 d . . . O1 O 0.4572(8) 0.8739(6) 0.4431(5) 0.0427(19) Uani 1 1 d . . . O2 O -0.2670(8) 0.8200(9) 0.3982(7) 0.057(2) Uani 1 1 d . . . O3 O 0.0061(5) 0.7826(5) 0.4743(4) 0.0207(11) Uani 1 1 d . . . O4 O 0.8771(6) 0.6521(6) 0.2326(5) 0.0331(14) Uani 1 1 d U . . O5 O 0.9812(9) 0.6105(8) 0.0355(7) 0.057(2) Uani 1 1 d U . . O6 O 0.9461(8) 0.6726(7) -0.2577(6) 0.0461(19) Uani 1 1 d . . . O7 O 0.8916(11) 0.5217(10) -0.4334(9) 0.023(2) Uiso 0.50 1 d P . 1 O7A O 0.9211(12) 0.5186(11) -0.3662(10) 0.028(3) Uiso 0.50 1 d P . 2 O8 O 0.641(3) 0.748(2) -0.197(2) 0.094(8) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.01176(17) 0.00996(16) 0.00987(17) -0.00255(12) -0.00178(13) -0.00165(12) Ru1 0.01176(17) 0.00996(16) 0.00987(17) -0.00255(12) -0.00178(13) -0.00165(12) Os2 0.00791(16) 0.01001(16) 0.00838(16) -0.00249(11) -0.00037(12) -0.00079(11) Ru2 0.00791(16) 0.01001(16) 0.00838(16) -0.00249(11) -0.00037(12) -0.00079(11) C2 0.013(3) 0.017(3) 0.017(3) -0.008(3) 0.002(3) -0.001(2) C3 0.013(3) 0.014(3) 0.021(4) -0.007(3) -0.003(3) 0.007(2) C4 0.014(3) 0.012(3) 0.012(3) -0.001(2) -0.002(2) -0.001(2) C5 0.015(3) 0.013(3) 0.011(3) 0.000(2) -0.003(2) -0.004(2) C6 0.010(3) 0.003(2) 0.014(3) -0.001(2) 0.000(2) -0.001(2) C8 0.012(3) 0.011(3) 0.011(3) 0.000(2) -0.002(2) -0.004(2) C9 0.004(3) 0.011(3) 0.014(3) -0.006(2) 0.000(2) -0.001(2) C11 0.008(3) 0.017(3) 0.013(3) -0.004(2) -0.001(2) -0.002(2) C12 0.011(3) 0.020(3) 0.015(3) -0.003(3) -0.005(2) -0.007(2) C14 0.010(3) 0.020(3) 0.014(3) -0.008(3) -0.003(2) -0.001(2) C15 0.012(3) 0.020(3) 0.015(3) -0.009(3) -0.002(3) -0.003(2) C16 0.010(3) 0.013(3) 0.014(3) 0.000(2) -0.003(2) -0.002(2) C17 0.013(3) 0.009(3) 0.015(3) -0.004(2) 0.000(2) -0.002(2) C18 0.010(3) 0.006(2) 0.008(3) 0.001(2) -0.001(2) -0.003(2) C21 0.017(3) 0.020(3) 0.011(3) 0.002(2) -0.005(3) -0.007(3) C22 0.019(3) 0.013(3) 0.013(3) -0.002(2) 0.000(3) -0.004(2) C23 0.012(3) 0.011(3) 0.012(3) -0.003(2) 0.000(2) -0.002(2) C24 0.017(3) 0.015(3) 0.015(3) -0.005(2) -0.004(3) -0.005(3) C31 0.010(3) 0.019(3) 0.016(3) -0.002(3) 0.004(2) -0.004(2) C32 0.013(3) 0.017(3) 0.021(4) -0.003(3) -0.005(3) 0.000(2) C33 0.013(3) 0.016(3) 0.015(3) -0.004(2) -0.002(3) -0.001(2) C34 0.010(3) 0.016(3) 0.011(3) -0.004(2) 0.003(2) -0.001(2) N1 0.012(3) 0.013(2) 0.011(3) -0.002(2) -0.002(2) -0.003(2) N7 0.010(2) 0.009(2) 0.010(3) -0.0020(19) -0.002(2) 0.0007(19) N10 0.009(2) 0.010(2) 0.008(2) -0.0031(19) 0.0032(19) -0.0017(19) N13 0.010(2) 0.014(2) 0.008(2) -0.003(2) 0.000(2) -0.002(2) N21 0.035(4) 0.019(3) 0.025(4) 0.002(3) -0.012(3) -0.011(3) N22 0.024(4) 0.029(4) 0.025(4) -0.005(3) -0.011(3) 0.001(3) N23 0.024(3) 0.021(3) 0.013(3) 0.000(2) -0.001(2) 0.000(3) N24 0.028(4) 0.017(3) 0.022(3) -0.006(2) -0.003(3) -0.006(3) N31 0.017(3) 0.024(3) 0.016(3) -0.006(2) -0.002(2) -0.001(2) N32 0.014(3) 0.048(4) 0.027(4) -0.020(3) 0.002(3) -0.008(3) N33 0.013(3) 0.025(3) 0.027(4) -0.002(3) 0.002(3) -0.001(2) N34 0.029(4) 0.015(3) 0.016(3) -0.003(2) 0.003(3) 0.001(3) K1 0.0732(16) 0.0827(17) 0.0763(17) -0.0208(14) -0.0049(14) -0.0239(14) K2 0.0202(8) 0.0228(7) 0.0199(8) -0.0001(6) -0.0023(6) -0.0028(6) K3 0.0383(10) 0.0178(7) 0.0317(10) -0.0002(7) -0.0167(8) -0.0070(7) K4 0.0212(8) 0.0216(8) 0.0355(10) -0.0028(7) 0.0001(7) -0.0070(6) O1 0.077(6) 0.023(3) 0.037(4) 0.008(3) -0.031(4) -0.018(3) O2 0.041(5) 0.093(7) 0.046(5) 0.004(5) -0.016(4) -0.033(5) O3 0.020(3) 0.022(3) 0.016(3) -0.004(2) 0.000(2) 0.004(2) O4 0.030(2) 0.034(2) 0.041(2) -0.0121(16) -0.0004(16) -0.0162(16) O5 0.053(3) 0.056(3) 0.062(3) 0.0027(18) -0.0130(19) -0.0125(18) O6 0.053(5) 0.062(5) 0.032(4) -0.013(4) 0.001(3) -0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Os1 C22 1.983(7) . ? Os1 C23 1.990(7) . ? Os1 C24 2.030(7) . ? Os1 C21 2.048(7) . ? Os1 N1 2.109(5) . ? Os1 N7 2.138(6) . ? Os2 C31 1.983(7) . ? Os2 C32 1.991(7) . ? Os2 C34 2.031(7) . ? Os2 C33 2.037(7) . ? Os2 N13 2.107(6) . ? Os2 N10 2.118(5) . ? C2 N1 1.335(9) . ? C2 C3 1.394(10) . ? C3 C4 1.398(10) . ? C4 C5 1.375(9) . ? C5 C6 1.386(9) . ? C6 N1 1.366(8) . ? C6 C8 1.461(9) . ? C8 N7 1.371(8) . ? C8 C9 1.419(9) . ? C9 N10 1.367(8) . ? C9 C18 1.474(8) . ? C11 N10 1.346(8) . ? C11 C12 1.373(9) . ? C12 N7 1.351(9) . ? C14 N13 1.349(8) . ? C14 C15 1.402(10) . ? C15 C16 1.387(9) . ? C16 C17 1.390(9) . ? C17 C18 1.388(9) . ? C18 N13 1.354(8) . ? C21 N21 1.159(9) . ? C21 K3 3.382(8) 2_665 ? C21 K1 3.389(8) 2_665 ? C22 N22 1.162(10) . ? C22 K2 3.417(7) 2_575 ? C22 K1 3.510(8) 2_665 ? C23 N23 1.162(9) . ? C23 K3 3.239(6) 2_665 ? C23 K3 3.276(7) 1_554 ? C23 K4 3.422(7) . ? C24 N24 1.170(10) . ? C24 K4 3.287(8) . ? C31 N31 1.171(10) . ? C31 K2 3.128(7) . ? C32 N32 1.178(10) . ? C32 K2 3.246(8) . ? C33 N33 1.167(10) . ? C34 N34 1.150(9) . ? C34 K3 3.350(7) . ? N21 K3 3.011(8) 2_665 ? N21 K1 3.110(8) 2_665 ? N22 K2 2.911(7) 2_575 ? N22 K1 3.304(8) 2_665 ? N23 K1 2.835(8) 1_554 ? N23 K3 2.921(7) 1_554 ? N23 K3 2.968(7) 2_665 ? N23 K4 3.324(7) . ? N24 K4 3.043(7) . ? N31 K2 2.796(7) 2_576 ? N31 K4 2.965(7) 2_675 ? N31 K2 2.981(7) . ? N32 K2 3.064(7) . ? N34 K3 2.887(7) . ? K1 O4 2.435(8) . ? K1 O7 2.650(12) 1_556 ? K1 O7A 2.712(13) 2_765 ? K1 N23 2.835(8) 1_556 ? K1 N21 3.110(8) 2_665 ? K1 O7 3.197(12) 2_765 ? K1 O2 3.240(11) 1_655 ? K1 N22 3.304(8) 2_665 ? K1 C21 3.389(8) 2_665 ? K1 C22 3.510(8) 2_665 ? K1 K4 3.900(4) 1_556 ? K1 K3 4.204(4) . ? K2 N31 2.796(7) 2_576 ? K2 O3 2.815(5) . ? K2 N22 2.911(7) 2_575 ? K2 O2 2.968(9) . ? K2 C22 3.417(7) 2_575 ? K2 K4 3.814(3) 1_456 ? K2 K2 3.920(3) 2_576 ? K2 K3 5.039(3) 2_576 ? K3 O1 2.679(7) . ? K3 N23 2.921(7) 1_556 ? K3 N23 2.968(7) 2_665 ? K3 N21 3.011(8) 2_665 ? K3 C23 3.239(6) 2_665 ? K3 C23 3.276(7) 1_556 ? K3 C21 3.382(8) 2_665 ? K3 K1 4.351(4) 2_666 ? K3 K3 4.682(4) 2_666 ? K4 O7 2.715(11) . ? K4 O3 2.722(6) 1_654 ? K4 O7A 2.812(12) . ? K4 O2 2.831(9) 1_654 ? K4 O6 2.847(9) . ? K4 N31 2.965(7) 2_675 ? K4 O8 3.00(3) . ? K4 K2 3.814(3) 1_654 ? O2 K4 2.831(9) 1_456 ? O2 K1 3.240(11) 1_455 ? O3 K4 2.722(6) 1_456 ? O7 K1 2.650(12) 1_554 ? O7 K1 3.197(12) 2_765 ? O7A K1 2.712(13) 2_765 ? 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 C22 Os1 C23 89.9(3) . . ? C22 Os1 C24 90.6(3) . . ? C23 Os1 C24 83.9(3) . . ? C22 Os1 C21 88.8(3) . . ? C23 Os1 C21 85.7(3) . . ? C24 Os1 C21 169.6(3) . . ? C22 Os1 N1 173.0(3) . . ? C23 Os1 N1 96.5(2) . . ? C24 Os1 N1 92.8(2) . . ? C21 Os1 N1 88.8(2) . . ? C22 Os1 N7 97.4(2) . . ? C23 Os1 N7 171.2(2) . . ? C24 Os1 N7 90.9(3) . . ? C21 Os1 N7 99.4(3) . . ? N1 Os1 N7 76.5(2) . . ? C31 Os2 C32 90.6(3) . . ? C31 Os2 C34 87.0(3) . . ? C32 Os2 C34 87.1(3) . . ? C31 Os2 C33 84.8(3) . . ? C32 Os2 C33 90.7(3) . . ? C34 Os2 C33 171.5(3) . . ? C31 Os2 N13 94.9(2) . . ? C32 Os2 N13 174.2(2) . . ? C34 Os2 N13 91.2(2) . . ? C33 Os2 N13 91.8(3) . . ? C31 Os2 N10 171.2(2) . . ? C32 Os2 N10 98.2(3) . . ? C34 Os2 N10 92.6(2) . . ? C33 Os2 N10 95.9(2) . . ? N13 Os2 N10 76.3(2) . . ? N1 C2 C3 123.3(6) . . ? C2 C3 C4 118.2(6) . . ? C5 C4 C3 118.6(6) . . ? C4 C5 C6 120.4(6) . . ? N1 C6 C5 121.1(6) . . ? N1 C6 C8 114.9(6) . . ? C5 C6 C8 123.5(6) . . ? N7 C8 C9 119.9(6) . . ? N7 C8 C6 114.1(6) . . ? C9 C8 C6 125.8(6) . . ? N10 C9 C8 119.3(6) . . ? N10 C9 C18 114.8(5) . . ? C8 C9 C18 125.8(6) . . ? N10 C11 C12 121.4(6) . . ? N7 C12 C11 122.0(6) . . ? N13 C14 C15 121.9(6) . . ? C16 C15 C14 118.4(6) . . ? C15 C16 C17 119.6(6) . . ? C18 C17 C16 119.2(6) . . ? N13 C18 C17 121.6(6) . . ? N13 C18 C9 113.8(5) . . ? C17 C18 C9 124.4(6) . . ? N21 C21 Os1 170.2(7) . . ? N21 C21 K3 61.7(5) . 2_665 ? Os1 C21 K3 108.6(3) . 2_665 ? N21 C21 K1 66.3(5) . 2_665 ? Os1 C21 K1 111.2(3) . 2_665 ? K3 C21 K1 76.77(16) 2_665 2_665 ? N22 C22 Os1 178.5(7) . . ? N22 C22 K2 55.0(5) . 2_575 ? Os1 C22 K2 126.1(3) . 2_575 ? N22 C22 K1 70.2(5) . 2_665 ? Os1 C22 K1 108.6(3) . 2_665 ? K2 C22 K1 125.2(2) 2_575 2_665 ? N23 C23 Os1 177.7(6) . . ? N23 C23 K3 66.2(4) . 2_665 ? Os1 C23 K3 115.7(3) . 2_665 ? N23 C23 K3 62.2(4) . 1_554 ? Os1 C23 K3 118.3(3) . 1_554 ? K3 C23 K3 91.87(17) 2_665 1_554 ? N23 C23 K4 75.4(5) . . ? Os1 C23 K4 102.5(2) . . ? K3 C23 K4 121.2(2) 2_665 . ? K3 C23 K4 108.0(2) 1_554 . ? N24 C24 Os1 169.6(6) . . ? N24 C24 K4 67.7(5) . . ? Os1 C24 K4 106.0(3) . . ? N31 C31 Os2 177.3(7) . . ? N31 C31 K2 71.9(5) . . ? Os2 C31 K2 110.5(3) . . ? N32 C32 Os2 174.0(7) . . ? N32 C32 K2 70.7(5) . . ? Os2 C32 K2 106.0(3) . . ? N33 C33 Os2 174.4(7) . . ? N34 C34 Os2 173.3(6) . . ? N34 C34 K3 56.9(5) . . ? Os2 C34 K3 121.9(3) . . ? C2 N1 C6 118.3(6) . . ? C2 N1 Os1 124.6(5) . . ? C6 N1 Os1 116.2(4) . . ? C12 N7 C8 117.0(6) . . ? C12 N7 Os1 128.4(4) . . ? C8 N7 Os1 114.0(4) . . ? C11 N10 C9 117.9(5) . . ? C11 N10 Os2 127.0(4) . . ? C9 N10 Os2 115.0(4) . . ? C14 N13 C18 119.3(6) . . ? C14 N13 Os2 123.1(5) . . ? C18 N13 Os2 117.4(4) . . ? C21 N21 K3 98.5(6) . 2_665 ? C21 N21 K1 93.7(5) . 2_665 ? K3 N21 K1 86.7(2) 2_665 2_665 ? C22 N22 K2 105.9(5) . 2_575 ? C22 N22 K1 90.4(5) . 2_665 ? K2 N22 K1 163.6(3) 2_575 2_665 ? C23 N23 K1 162.8(6) . 1_554 ? C23 N23 K3 97.2(5) . 1_554 ? K1 N23 K3 93.8(2) 1_554 1_554 ? C23 N23 K3 92.8(5) . 2_665 ? K1 N23 K3 97.1(2) 1_554 2_665 ? K3 N23 K3 105.3(2) 1_554 2_665 ? C23 N23 K4 84.9(5) . . ? K1 N23 K4 78.12(19) 1_554 . ? K3 N23 K4 120.2(2) 1_554 . ? K3 N23 K4 134.4(2) 2_665 . ? C24 N24 K4 91.4(5) . . ? C31 N31 K2 147.1(6) . 2_576 ? C31 N31 K4 128.3(6) . 2_675 ? K2 N31 K4 82.85(17) 2_576 2_675 ? C31 N31 K2 86.1(5) . . ? K2 N31 K2 85.41(19) 2_576 . ? K4 N31 K2 120.5(2) 2_675 . ? C32 N32 K2 88.1(5) . . ? C34 N34 K3 103.6(5) . . ? O4 K1 O7 132.6(3) . 1_556 ? O4 K1 O7A 78.6(3) . 2_765 ? O7 K1 O7A 71.5(4) 1_556 2_765 ? O4 K1 N23 131.7(3) . 1_556 ? O7 K1 N23 69.5(3) 1_556 1_556 ? O7A K1 N23 141.0(3) 2_765 1_556 ? O4 K1 N21 60.3(2) . 2_665 ? O7 K1 N21 158.2(3) 1_556 2_665 ? O7A K1 N21 130.1(3) 2_765 2_665 ? N23 K1 N21 88.9(2) 1_556 2_665 ? O4 K1 O7 92.2(3) . 2_765 ? O7 K1 O7 53.8(4) 1_556 2_765 ? O7A K1 O7 17.7(3) 2_765 2_765 ? N23 K1 O7 123.4(3) 1_556 2_765 ? N21 K1 O7 147.6(3) 2_665 2_765 ? O4 K1 O2 66.7(2) . 1_655 ? O7 K1 O2 88.8(3) 1_556 1_655 ? O7A K1 O2 108.5(3) 2_765 1_655 ? N23 K1 O2 73.0(2) 1_556 1_655 ? N21 K1 O2 81.3(2) 2_665 1_655 ? O7 K1 O2 104.4(3) 2_765 1_655 ? O4 K1 N22 116.7(2) . 2_665 ? O7 K1 N22 98.2(3) 1_556 2_665 ? O7A K1 N22 87.7(3) 2_765 2_665 ? N23 K1 N22 95.8(2) 1_556 2_665 ? N21 K1 N22 87.01(19) 2_665 2_665 ? O7 K1 N22 91.5(3) 2_765 2_665 ? O2 K1 N22 163.8(2) 1_655 2_665 ? O4 K1 C21 73.8(2) . 2_665 ? O7 K1 C21 153.1(3) 1_556 2_665 ? O7A K1 C21 127.4(3) 2_765 2_665 ? N23 K1 C21 88.9(2) 1_556 2_665 ? N21 K1 C21 19.95(17) 2_665 2_665 ? O7 K1 C21 143.8(3) 2_765 2_665 ? O2 K1 C21 100.3(2) 1_655 2_665 ? N22 K1 C21 67.18(18) 2_665 2_665 ? O4 K1 C22 108.0(2) . 2_665 ? O7 K1 C22 114.0(3) 1_556 2_665 ? O7A K1 C22 103.1(3) 2_765 2_665 ? N23 K1 C22 90.8(2) 1_556 2_665 ? N21 K1 C22 68.19(18) 2_665 2_665 ? O7 K1 C22 109.7(3) 2_765 2_665 ? O2 K1 C22 145.7(2) 1_655 2_665 ? N22 K1 C22 19.33(17) 2_665 2_665 ? C21 K1 C22 48.25(17) 2_665 2_665 ? O4 K1 K4 106.04(19) . 1_556 ? O7 K1 K4 44.0(2) 1_556 1_556 ? O7A K1 K4 95.6(3) 2_765 1_556 ? N23 K1 K4 56.53(15) 1_556 1_556 ? N21 K1 K4 120.76(18) 2_665 1_556 ? O7 K1 K4 81.0(2) 2_765 1_556 ? O2 K1 K4 45.57(16) 1_655 1_556 ? N22 K1 K4 136.89(18) 2_665 1_556 ? C21 K1 K4 134.61(17) 2_665 1_556 ? C22 K1 K4 143.65(17) 2_665 1_556 ? O4 K1 K3 94.2(2) . . ? O7 K1 K3 112.5(3) 1_556 . ? O7A K1 K3 172.3(3) 2_765 . ? N23 K1 K3 43.89(14) 1_556 . ? N21 K1 K3 45.65(16) 2_665 . ? O7 K1 K3 164.7(2) 2_765 . ? O2 K1 K3 65.79(16) 1_655 . ? N22 K1 K3 97.98(15) 2_665 . ? C21 K1 K3 51.55(14) 2_665 . ? C22 K1 K3 81.47(14) 2_665 . ? K4 K1 K3 83.82(8) 1_556 . ? N31 K2 O3 69.10(18) 2_576 . ? N31 K2 N22 100.9(2) 2_576 2_575 ? O3 K2 N22 156.68(19) . 2_575 ? N31 K2 O2 95.9(2) 2_576 . ? O3 K2 O2 67.7(2) . . ? N22 K2 O2 135.5(2) 2_575 . ? N31 K2 N31 94.59(19) 2_576 . ? O3 K2 N31 75.64(18) . . ? N22 K2 N31 84.5(2) 2_575 . ? O2 K2 N31 134.9(2) . . ? N31 K2 N32 151.2(2) 2_576 . ? O3 K2 N32 87.5(2) . . ? N22 K2 N32 106.8(2) 2_575 . ? O2 K2 N32 58.5(2) . . ? N31 K2 N32 95.67(19) . . ? N31 K2 C31 113.0(2) 2_576 . ? O3 K2 C31 73.39(18) . . ? N22 K2 C31 92.7(2) 2_575 . ? O2 K2 C31 118.0(2) . . ? N31 K2 C31 21.93(18) . . ? N32 K2 C31 73.82(19) . . ? N31 K2 C32 150.94(19) 2_576 . ? O3 K2 C32 82.04(17) . . ? N22 K2 C32 104.6(2) 2_575 . ? O2 K2 C32 75.4(2) . . ? N31 K2 C32 74.41(18) . . ? N32 K2 C32 21.26(18) . . ? C31 K2 C32 52.56(19) . . ? N31 K2 C22 111.02(18) 2_576 2_575 ? O3 K2 C22 175.26(18) . 2_575 ? N22 K2 C22 19.09(18) 2_575 2_575 ? O2 K2 C22 116.8(2) . 2_575 ? N31 K2 C22 99.67(18) . 2_575 ? N32 K2 C22 93.7(2) . 2_575 ? C31 K2 C22 102.53(19) . 2_575 ? C32 K2 C22 97.46(18) . 2_575 ? N31 K2 K4 50.47(14) 2_576 1_456 ? O3 K2 K4 45.46(12) . 1_456 ? N22 K2 K4 142.78(17) 2_575 1_456 ? O2 K2 K4 47.35(17) . 1_456 ? N31 K2 K4 116.95(14) . 1_456 ? N32 K2 K4 101.09(17) . 1_456 ? C31 K2 K4 118.82(14) . 1_456 ? C32 K2 K4 110.23(14) . 1_456 ? C22 K2 K4 138.45(14) 2_575 1_456 ? N31 K2 K2 49.27(14) 2_576 2_576 ? O3 K2 K2 63.70(12) . 2_576 ? N22 K2 K2 93.60(15) 2_575 2_576 ? O2 K2 K2 127.60(19) . 2_576 ? N31 K2 K2 45.31(13) . 2_576 ? N32 K2 K2 134.42(15) . 2_576 ? C31 K2 K2 64.73(14) . 2_576 ? C32 K2 K2 114.78(14) . 2_576 ? C22 K2 K2 112.55(13) 2_575 2_576 ? K4 K2 K2 83.72(6) 1_456 2_576 ? N31 K2 K3 65.35(14) 2_576 2_576 ? O3 K2 K3 134.15(12) . 2_576 ? N22 K2 K3 44.43(16) 2_575 2_576 ? O2 K2 K3 111.78(19) . 2_576 ? N31 K2 K3 112.42(13) . 2_576 ? N32 K2 K3 133.26(15) . 2_576 ? C31 K2 K3 129.95(14) . 2_576 ? C32 K2 K3 143.69(13) . 2_576 ? C22 K2 K3 46.78(12) 2_575 2_576 ? K4 K2 K3 98.35(5) 1_456 2_576 ? K2 K2 K3 89.57(6) 2_576 2_576 ? O1 K3 N34 116.4(2) . . ? O1 K3 N23 81.6(2) . 1_556 ? N34 K3 N23 156.0(2) . 1_556 ? O1 K3 N23 151.8(2) . 2_665 ? N34 K3 N23 83.26(19) . 2_665 ? N23 K3 N23 74.7(2) 1_556 2_665 ? O1 K3 N21 105.7(2) . 2_665 ? N34 K3 N21 99.97(19) . 2_665 ? N23 K3 N21 89.25(19) 1_556 2_665 ? N23 K3 N21 89.31(19) 2_665 2_665 ? O1 K3 C23 159.4(2) . 2_665 ? N34 K3 C23 84.18(17) . 2_665 ? N23 K3 C23 78.65(18) 1_556 2_665 ? N23 K3 C23 20.99(17) 2_665 2_665 ? N21 K3 C23 68.58(18) 2_665 2_665 ? O1 K3 C23 75.04(18) . 1_556 ? N34 K3 C23 144.0(2) . 1_556 ? N23 K3 C23 20.60(17) 1_556 1_556 ? N23 K3 C23 77.41(17) 2_665 1_556 ? N21 K3 C23 109.79(19) 2_665 1_556 ? C23 K3 C23 88.13(17) 2_665 1_556 ? O1 K3 C34 100.49(19) . . ? N34 K3 C34 19.48(18) . . ? N23 K3 C34 174.8(2) 1_556 . ? N23 K3 C34 101.97(18) 2_665 . ? N21 K3 C34 94.74(18) 2_665 . ? C23 K3 C34 99.71(17) 2_665 . ? C23 K3 C34 155.42(18) 1_556 . ? O1 K3 C21 124.8(2) . 2_665 ? N34 K3 C21 93.62(18) . 2_665 ? N23 K3 C21 87.66(18) 1_556 2_665 ? N23 K3 C21 69.84(18) 2_665 2_665 ? N21 K3 C21 19.80(17) 2_665 2_665 ? C23 K3 C21 48.96(17) 2_665 2_665 ? C23 K3 C21 107.50(17) 1_556 2_665 ? C34 K3 C21 94.97(17) . 2_665 ? O1 K3 K1 88.4(2) . . ? N34 K3 K1 145.30(15) . . ? N23 K3 K1 42.28(15) 1_556 . ? N23 K3 K1 84.27(15) 2_665 . ? N21 K3 K1 47.60(14) 2_665 . ? C23 K3 K1 73.06(13) 2_665 . ? C23 K3 K1 62.47(13) 1_556 . ? C34 K3 K1 142.10(14) . . ? C21 K3 K1 51.69(13) 2_665 . ? O1 K3 K1 121.9(2) . 2_666 ? N34 K3 K1 74.87(15) . 2_666 ? N23 K3 K1 82.16(15) 1_556 2_666 ? N23 K3 K1 40.29(14) 2_665 2_666 ? N21 K3 K1 129.39(14) 2_665 2_666 ? C23 K3 K1 60.82(14) 2_665 2_666 ? C23 K3 K1 70.69(14) 1_556 2_666 ? C34 K3 K1 92.74(14) . 2_666 ? C21 K3 K1 109.67(14) 2_665 2_666 ? K1 K3 K1 113.67(7) . 2_666 ? O1 K3 K3 117.84(16) . 2_666 ? N34 K3 K3 119.72(15) . 2_666 ? N23 K3 K3 37.71(14) 1_556 2_666 ? N23 K3 K3 37.01(13) 2_665 2_666 ? N21 K3 K3 89.09(14) 2_665 2_666 ? C23 K3 K3 44.37(12) 2_665 2_666 ? C23 K3 K3 43.76(11) 1_556 2_666 ? C34 K3 K3 138.85(14) . 2_666 ? C21 K3 K3 75.88(13) 2_665 2_666 ? K1 K3 K3 58.33(7) . 2_666 ? K1 K3 K3 55.34(7) 2_666 2_666 ? O7 K4 O3 81.4(3) . 1_654 ? O7 K4 O7A 21.3(3) . . ? O3 K4 O7A 84.7(3) 1_654 . ? O7 K4 O2 96.7(3) . 1_654 ? O3 K4 O2 70.9(2) 1_654 1_654 ? O7A K4 O2 117.4(3) . 1_654 ? O7 K4 O6 75.4(3) . . ? O3 K4 O6 83.8(2) 1_654 . ? O7A K4 O6 54.6(3) . . ? O2 K4 O6 154.5(2) 1_654 . ? O7 K4 N31 141.1(3) . 2_675 ? O3 K4 N31 67.91(18) 1_654 2_675 ? O7A K4 N31 127.7(3) . 2_675 ? O2 K4 N31 95.2(2) 1_654 2_675 ? O6 K4 N31 78.0(2) . 2_675 ? O7 K4 O8 107.0(6) . . ? O3 K4 O8 144.7(5) 1_654 . ? O7A K4 O8 92.1(6) . . ? O2 K4 O8 138.7(5) 1_654 . ? O6 K4 O8 66.2(5) . . ? N31 K4 O8 87.2(5) 2_675 . ? O7 K4 N24 138.6(3) . . ? O3 K4 N24 134.00(18) 1_654 . ? O7A K4 N24 141.2(3) . . ? O2 K4 N24 80.7(2) 1_654 . ? O6 K4 N24 121.4(2) . . ? N31 K4 N24 79.86(18) 2_675 . ? O8 K4 N24 59.1(5) . . ? O7 K4 C24 119.6(3) . . ? O3 K4 C24 154.30(18) 1_654 . ? O7A K4 C24 120.4(3) . . ? O2 K4 C24 90.8(2) 1_654 . ? O6 K4 C24 114.3(2) . . ? N31 K4 C24 97.02(18) 2_675 . ? O8 K4 C24 48.2(5) . . ? N24 K4 C24 20.84(18) . . ? O7 K4 N23 61.5(3) . . ? O3 K4 N23 122.45(18) 1_654 . ? O7A K4 N23 75.6(3) . . ? O2 K4 N23 71.7(2) 1_654 . ? O6 K4 N23 121.9(2) . . ? N31 K4 N23 156.57(18) 2_675 . ? O8 K4 N23 90.3(5) . . ? N24 K4 N23 78.90(17) . . ? C24 K4 N23 64.74(16) . . ? O7 K4 C23 74.3(3) . . ? O3 K4 C23 142.15(18) 1_654 . ? O7A K4 C23 82.9(3) . . ? O2 K4 C23 83.5(2) 1_654 . ? O6 K4 C23 116.4(2) . . ? N31 K4 C23 144.01(18) 2_675 . ? O8 K4 C23 71.5(5) . . ? N24 K4 C23 64.39(17) . . ? C24 K4 C23 47.19(16) . . ? N23 K4 C23 19.76(16) . . ? O7 K4 K2 123.4(3) . 1_654 ? O3 K4 K2 47.50(12) 1_654 1_654 ? O7A K4 K2 131.9(3) . 1_654 ? O2 K4 K2 50.45(18) 1_654 1_654 ? O6 K4 K2 113.68(17) . 1_654 ? N31 K4 K2 46.68(13) 2_675 1_654 ? O8 K4 K2 128.3(5) . 1_654 ? N24 K4 K2 86.52(14) . 1_654 ? C24 K4 K2 106.93(14) . 1_654 ? N23 K4 K2 121.91(13) . 1_654 ? C23 K4 K2 129.73(13) . 1_654 ? K4 O2 K2 82.2(2) 1_456 . ? K4 O2 K1 79.6(2) 1_456 1_455 ? K2 O2 K1 134.2(3) . 1_455 ? K4 O3 K2 87.05(16) 1_456 . ? K1 O7 K4 93.2(4) 1_554 . ? K1 O7 K1 126.2(4) 1_554 2_765 ? K4 O7 K1 110.6(4) . 2_765 ? K1 O7A K4 123.6(5) 2_765 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.603 _refine_diff_density_min -2.613 _refine_diff_density_rms 0.358