# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global #=============================================================================== _audit_creation_date 04-09-02 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Le Floch,Pascal' F.Mathey N.Mezailles 'Audrey Moores' 'Louis Ricard' _publ_contact_author_name 'Dr Pascal Le Floch' _publ_contact_author_address ; Department of Chemistry Heteroelements et Coordination, UMR CNRS 7653 Ecole Polytechnique Palaiseau Cedex 91128 FRANCE ; _publ_contact_author_email LEFLOCH@POLY.POLYTECHNIQUE.FR _publ_requested_journal 'Chemical Communications' _publ_section_title ; Neutral and dianionic Iron and Ruthenium 1,4-Diphosphabutadiene Complexes. ; _publ_section_exptl_prep ; All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #=============================================================================== data_compound_2 _database_code_CSD 208890 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C212 H296 Fe2 N8 Na4 O33 P8' _chemical_formula_weight 3935.99 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' Na Na 0.0362 0.0249 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 52.679(1) _cell_length_b 13.722(1) _cell_length_c 30.639(1) _cell_angle_alpha 90.00 _cell_angle_beta 113.190(1) _cell_angle_gamma 90.00 _cell_volume 20358.3(1.7) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8416 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type 'multiple scans' _exptl_absorpt_correction_T_min 0.9397 _exptl_absorpt_correction_T_max 0.9664 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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_% ? _diffrn_reflns_number 17520 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _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 3.00 _diffrn_reflns_theta_max 20.81 _reflns_number_total 10501 _reflns_number_gt 6551 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0909P)^2^+85.0889P] 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 10501 _refine_ls_number_parameters 1203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0737 _refine_ls_wR_factor_ref 0.2125 _refine_ls_wR_factor_gt 0.1785 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe 0.126974(2) 0.074875(7) 0.741253(3) 0.05320(4) Uani 1 1 d . . . P1 P 0.157496(4) 0.062796(14) 0.816116(6) 0.05581(7) Uani 1 1 d . . . P2 P 0.106553(4) -0.041649(14) 0.765922(6) 0.05355(7) Uani 1 1 d . . . P3 P 0.129946(4) 0.231466(14) 0.721931(6) 0.05398(7) Uani 1 1 d . . . P4 P 0.111976(4) 0.052276(14) 0.662437(6) 0.05385(7) Uani 1 1 d . . . Na1 Na 0.239858(6) -0.28179(2) 0.791545(9) 0.06714(11) Uani 1 1 d . . . Na2 Na -0.030085(5) 0.16269(2) 0.608447(9) 0.06027(10) Uani 1 1 d . . . O1 O 0.265088(10) -0.43883(4) 0.813200(16) 0.0724(2) Uani 1 1 d . . . O2 O 0.238262(11) -0.35381(4) 0.864966(16) 0.0789(2) Uani 1 1 d . . . O3 O 0.218055(9) -0.12365(4) 0.781791(17) 0.0688(2) Uani 1 1 d . . . O4 O 0.268470(10) -0.15838(4) 0.853587(17) 0.0732(2) Uani 1 1 d . . . O5 O 0.238933(10) -0.22848(4) 0.713424(17) 0.0748(2) Uani 1 1 d . . . O6 O 0.210633(10) -0.39056(4) 0.722522(16) 0.0704(2) Uani 1 1 d . . . O7 O 0.011690(10) 0.20413(4) 0.677072(16) 0.0731(2) Uani 1 1 d . . . O8 O -0.032398(10) 0.33006(4) 0.637154(17) 0.0769(2) Uani 1 1 d . . . O9 O -0.033972(12) 0.04795(4) 0.669792(17) 0.1022(2) Uani 1 1 d . . . O10 O -0.022366(10) -0.01076(4) 0.596280(17) 0.0835(2) Uani 1 1 d . . . O11 O -0.029679(10) 0.25732(4) 0.537066(16) 0.0773(2) Uani 1 1 d . . . O12 O -0.070336(10) 0.13486(4) 0.536064(16) 0.0734(2) Uani 1 1 d . . . N1 N 0.291550(12) -0.26419(5) 0.79576(2) 0.0689(2) Uani 1 1 d . . . N2 N 0.187169(12) -0.29861(5) 0.78546(2) 0.0748(2) Uani 1 1 d . . . N3 N 0.016902(11) 0.13130(4) 0.590616(19) 0.0604(2) Uani 1 1 d . . . N4 N -0.076446(12) 0.19216(5) 0.62514(2) 0.0717(3) Uani 1 1 d . . . C1 C 0.146770(13) -0.02102(5) 0.85119(2) 0.0534(3) Uani 1 1 d . . . C2 C 0.125647(13) -0.08163(5) 0.82572(2) 0.0517(2) Uani 1 1 d . . . C3 C 0.114446(12) 0.24903(5) 0.65857(2) 0.0475(2) Uani 1 1 d . . . C4 C 0.112151(13) 0.16489(5) 0.63194(2) 0.0493(2) Uani 1 1 d . . . C5 C 0.170674(14) 0.16841(5) 0.85380(2) 0.0540(3) Uani 1 1 d . . . C6 C 0.158859(16) 0.20914(6) 0.88191(2) 0.0722(3) Uani 1 1 d . . . H6 H 0.1435 0.1763 0.8840 0.087 Uiso 1 1 calc R . . C7 C 0.167376(18) 0.29385(6) 0.90742(3) 0.0854(3) Uani 1 1 d . . . H7 H 0.1581 0.3177 0.9263 0.103 Uiso 1 1 calc R . . C8 C 0.189424(18) 0.34344(6) 0.90535(3) 0.0852(4) Uani 1 1 d . . . H8 H 0.1956 0.4028 0.9222 0.102 Uiso 1 1 calc R . . C9 C 0.202481(18) 0.30478(7) 0.87815(3) 0.0968(4) Uani 1 1 d . . . H9 H 0.2180 0.3372 0.8767 0.116 Uiso 1 1 calc R . . C10 C 0.193092(16) 0.21856(6) 0.85281(3) 0.0756(3) Uani 1 1 d . . . H10 H 0.2024 0.1936 0.8343 0.091 Uiso 1 1 calc R . . C11 C 0.161396(14) -0.02326(5) 0.90408(2) 0.0541(3) Uani 1 1 d . . . C12 C 0.147125(14) -0.03378(5) 0.93333(2) 0.0548(3) Uani 1 1 d . . . H12 H 0.1277 -0.0420 0.9193 0.066 Uiso 1 1 calc R . . C13 C 0.160249(16) -0.03264(5) 0.98195(2) 0.0643(3) Uani 1 1 d . . . H13 H 0.1498 -0.0406 1.0009 0.077 Uiso 1 1 calc R . . C14 C 0.188570(17) -0.02002(6) 1.00341(3) 0.0764(3) Uani 1 1 d . . . H14 H 0.1977 -0.0186 1.0370 0.092 Uiso 1 1 calc R . . C15 C 0.203461(16) -0.00948(6) 0.97524(2) 0.0694(3) Uani 1 1 d . . . H15 H 0.2229 -0.0012 0.9896 0.083 Uiso 1 1 calc R . . C16 C 0.190136(15) -0.01091(5) 0.92647(2) 0.0590(3) Uani 1 1 d . . . H16 H 0.2006 -0.0034 0.9076 0.071 Uiso 1 1 calc R . . C17 C 0.117649(13) -0.16873(5) 0.84568(2) 0.0526(2) Uani 1 1 d . . . C18 C 0.090100(14) -0.18896(5) 0.83572(2) 0.0607(3) Uani 1 1 d . . . H18 H 0.0763 -0.1453 0.8161 0.073 Uiso 1 1 calc R . . C19 C 0.081962(15) -0.27185(6) 0.85371(2) 0.0683(3) Uani 1 1 d . . . H19 H 0.0629 -0.2841 0.8461 0.082 Uiso 1 1 calc R . . C20 C 0.101295(16) -0.33411(6) 0.88196(2) 0.0700(3) Uani 1 1 d . . . H20 H 0.0958 -0.3895 0.8947 0.084 Uiso 1 1 calc R . . C21 C 0.128912(16) -0.31810(5) 0.89256(2) 0.0683(3) Uani 1 1 d . . . H21 H 0.1425 -0.3627 0.9119 0.082 Uiso 1 1 calc R . . C22 C 0.136667(15) -0.23417(5) 0.87416(2) 0.0584(3) Uani 1 1 d . . . H22 H 0.1557 -0.2226 0.8818 0.070 Uiso 1 1 calc R . . C23 C 0.090208(13) -0.14835(5) 0.73103(2) 0.0516(2) Uani 1 1 d . . . C24 C 0.099622(14) -0.24488(5) 0.73984(2) 0.0607(3) Uani 1 1 d . . . H24 H 0.1155 -0.2598 0.7676 0.073 Uiso 1 1 calc R . . C25 C 0.086088(15) -0.31850(6) 0.70857(2) 0.0693(3) Uani 1 1 d . . . H25 H 0.0927 -0.3835 0.7155 0.083 Uiso 1 1 calc R . . C26 C 0.063539(16) -0.30012(6) 0.66813(3) 0.0804(3) Uani 1 1 d . . . H26 H 0.0548 -0.3515 0.6466 0.096 Uiso 1 1 calc R . . C27 C 0.053398(15) -0.20612(6) 0.65857(3) 0.0754(3) Uani 1 1 d . . . H27 H 0.0374 -0.1923 0.6309 0.091 Uiso 1 1 calc R . . C28 C 0.066888(14) -0.13276(6) 0.68990(2) 0.0637(3) Uani 1 1 d . . . H28 H 0.0599 -0.0683 0.6829 0.076 Uiso 1 1 calc R . . C29 C 0.115082(14) 0.32711(5) 0.74628(2) 0.0553(3) Uani 1 1 d . . . C30 C 0.131656(16) 0.37079(5) 0.78875(2) 0.0677(3) Uani 1 1 d . . . H30 H 0.1502 0.3491 0.8045 0.081 Uiso 1 1 calc R . . C31 C 0.122154(18) 0.44518(6) 0.80912(3) 0.0790(3) Uani 1 1 d . . . H31 H 0.1340 0.4738 0.8382 0.095 Uiso 1 1 calc R . . C32 C 0.095583(17) 0.47668(6) 0.78690(3) 0.0768(3) Uani 1 1 d . . . H32 H 0.0889 0.5273 0.8008 0.092 Uiso 1 1 calc R . . C33 C 0.078402(15) 0.43598(6) 0.74472(2) 0.0685(3) Uani 1 1 d . . . H33 H 0.0600 0.4589 0.7291 0.082 Uiso 1 1 calc R . . C34 C 0.088190(14) 0.36032(5) 0.72475(2) 0.0612(3) Uani 1 1 d . . . H34 H 0.0761 0.3313 0.6959 0.073 Uiso 1 1 calc R . . C35 C 0.105977(13) 0.34562(5) 0.63762(2) 0.0494(2) Uani 1 1 d . . . C36 C 0.120303(15) 0.42852(5) 0.65915(2) 0.0606(3) Uani 1 1 d . . . H36 H 0.1371 0.4215 0.6863 0.073 Uiso 1 1 calc R . . C37 C 0.111234(17) 0.52137(6) 0.64276(2) 0.0732(3) Uani 1 1 d . . . H37 H 0.1217 0.5766 0.6587 0.088 Uiso 1 1 calc R . . C38 C 0.086986(18) 0.53376(6) 0.60330(3) 0.0823(4) Uani 1 1 d . . . H38 H 0.0804 0.5972 0.5921 0.099 Uiso 1 1 calc R . . C39 C 0.072617(16) 0.45244(6) 0.58051(3) 0.0779(3) Uani 1 1 d . . . H39 H 0.0563 0.4605 0.5527 0.093 Uiso 1 1 calc R . . C40 C 0.081324(14) 0.35848(6) 0.59699(2) 0.0604(3) Uani 1 1 d . . . H40 H 0.0708 0.3036 0.5810 0.072 Uiso 1 1 calc R . . C41 C 0.106683(13) 0.16574(5) 0.58061(2) 0.0493(2) Uani 1 1 d . . . C42 C 0.121585(14) 0.22607(5) 0.56240(2) 0.0604(3) Uani 1 1 d . . . H42 H 0.1353 0.2682 0.5834 0.073 Uiso 1 1 calc R . . C43 C 0.116951(15) 0.22616(6) 0.51478(2) 0.0704(3) Uani 1 1 d . . . H43 H 0.1276 0.2675 0.5036 0.084 Uiso 1 1 calc R . . C44 C 0.097018(16) 0.16676(6) 0.48326(3) 0.0731(3) Uani 1 1 d . . . H44 H 0.0937 0.1673 0.4505 0.088 Uiso 1 1 calc R . . C45 C 0.081889(15) 0.10621(6) 0.50025(2) 0.0673(3) Uani 1 1 d . . . H45 H 0.0678 0.0658 0.4789 0.081 Uiso 1 1 calc R . . C46 C 0.087320(14) 0.10463(5) 0.54874(2) 0.0552(3) Uani 1 1 d . . . H46 H 0.0774 0.0604 0.5601 0.066 Uiso 1 1 calc R . . C47 C 0.127321(13) -0.04045(5) 0.63715(2) 0.0467(2) Uani 1 1 d . . . C48 C 0.122077(15) -0.13920(5) 0.64342(2) 0.0585(3) Uani 1 1 d . . . H48 H 0.1114 -0.1556 0.6611 0.070 Uiso 1 1 calc R . . C49 C 0.132254(15) -0.21115(5) 0.62427(2) 0.0662(3) Uani 1 1 d . . . H49 H 0.1284 -0.2770 0.6291 0.079 Uiso 1 1 calc R . . C50 C 0.147969(15) -0.19282(5) 0.59803(2) 0.0643(3) Uani 1 1 d . . . H50 H 0.1547 -0.2441 0.5847 0.077 Uiso 1 1 calc R . . C51 C 0.153277(14) -0.09746(5) 0.59231(2) 0.0574(3) Uani 1 1 d . . . H51 H 0.1640 -0.0822 0.5745 0.069 Uiso 1 1 calc R . . C52 C 0.143554(13) -0.02213(5) 0.61152(2) 0.0555(3) Uani 1 1 d . . . H52 H 0.1480 0.0432 0.6071 0.067 Uiso 1 1 calc R . . C53 C 0.271057(16) -0.46619(6) 0.86069(2) 0.0793(3) Uani 1 1 d . . . H53A H 0.2859 -0.4243 0.8826 0.095 Uiso 1 1 calc R . . H53B H 0.2775 -0.5347 0.8658 0.095 Uiso 1 1 calc R . . C54 C 0.245771(17) -0.45544(6) 0.87038(3) 0.0825(4) Uani 1 1 d . . . H54A H 0.2306 -0.4953 0.8478 0.099 Uiso 1 1 calc R . . H54B H 0.2493 -0.4774 0.9030 0.099 Uiso 1 1 calc R . . C55 C 0.213020(17) -0.33292(7) 0.87095(3) 0.0938(4) Uani 1 1 d . . . H55A H 0.2129 -0.2635 0.8797 0.113 Uiso 1 1 calc R . . H55B H 0.2123 -0.3730 0.8973 0.113 Uiso 1 1 calc R . . C56 C 0.187643(16) -0.35364(7) 0.82613(3) 0.0894(3) Uani 1 1 d . . . H56A H 0.1871 -0.4241 0.8188 0.107 Uiso 1 1 calc R . . H56B H 0.1709 -0.3378 0.8319 0.107 Uiso 1 1 calc R . . C57 C 0.176974(16) -0.19642(6) 0.78457(3) 0.0856(3) Uani 1 1 d . . . H57A H 0.1566 -0.1955 0.7681 0.103 Uiso 1 1 calc R . . H57B H 0.1818 -0.1736 0.8175 0.103 Uiso 1 1 calc R . . C58 C 0.189062(15) -0.12930(6) 0.76002(3) 0.0758(3) Uani 1 1 d . . . H58A H 0.1836 -0.1514 0.7268 0.091 Uiso 1 1 calc R . . H58B H 0.1813 -0.0634 0.7592 0.091 Uiso 1 1 calc R . . C59 C 0.227831(16) -0.06317(6) 0.82245(3) 0.0776(3) Uani 1 1 d . . . H59A H 0.2223 -0.0897 0.8475 0.093 Uiso 1 1 calc R . . H59B H 0.2202 0.0035 0.8144 0.093 Uiso 1 1 calc R . . C60 C 0.258727(17) -0.06160(6) 0.83916(3) 0.0810(3) Uani 1 1 d . . . H60A H 0.2641 -0.0400 0.8132 0.097 Uiso 1 1 calc R . . H60B H 0.2668 -0.0160 0.8662 0.097 Uiso 1 1 calc R . . C61 C 0.297388(16) -0.16844(6) 0.86660(3) 0.0793(3) Uani 1 1 d . . . H61A H 0.3040 -0.2254 0.8879 0.095 Uiso 1 1 calc R . . H61B H 0.3068 -0.1098 0.8846 0.095 Uiso 1 1 calc R . . C62 C 0.305133(16) -0.18112(6) 0.82592(3) 0.0788(3) Uani 1 1 d . . . H62A H 0.3004 -0.1210 0.8065 0.095 Uiso 1 1 calc R . . H62B H 0.3254 -0.1900 0.8378 0.095 Uiso 1 1 calc R . . C63 C 0.288226(15) -0.44334(6) 0.79961(2) 0.0727(3) Uani 1 1 d . . . H63A H 0.2814 -0.4496 0.7647 0.087 Uiso 1 1 calc R . . H63B H 0.2993 -0.5021 0.8139 0.087 Uiso 1 1 calc R . . C64 C 0.306609(16) -0.35337(6) 0.81541(3) 0.0733(3) Uani 1 1 d . . . H64A H 0.3144 -0.3494 0.8505 0.088 Uiso 1 1 calc R . . H64B H 0.3222 -0.3598 0.8052 0.088 Uiso 1 1 calc R . . C65 C 0.289042(16) -0.24823(7) 0.74658(3) 0.0798(3) Uani 1 1 d . . . H65A H 0.2871 -0.3120 0.7304 0.096 Uiso 1 1 calc R . . H65B H 0.3061 -0.2168 0.7472 0.096 Uiso 1 1 calc R . . C66 C 0.264515(15) -0.18495(7) 0.71880(3) 0.0801(3) Uani 1 1 d . . . H66A H 0.2664 -0.1216 0.7353 0.096 Uiso 1 1 calc R . . H66B H 0.2645 -0.1721 0.6870 0.096 Uiso 1 1 calc R . . C67 C 0.229588(16) -0.29990(7) 0.67698(3) 0.0844(4) Uani 1 1 d . . . H67A H 0.2439 -0.3507 0.6825 0.101 Uiso 1 1 calc R . . H67B H 0.2257 -0.2695 0.6457 0.101 Uiso 1 1 calc R . . C68 C 0.204190(16) -0.34337(7) 0.67793(3) 0.0802(3) Uani 1 1 d . . . H68A H 0.1902 -0.2919 0.6735 0.096 Uiso 1 1 calc R . . H68B H 0.1965 -0.3912 0.6518 0.096 Uiso 1 1 calc R . . C69 C 0.187492(15) -0.42817(6) 0.72885(3) 0.0726(3) Uani 1 1 d . . . H69A H 0.1937 -0.4767 0.7548 0.087 Uiso 1 1 calc R . . H69B H 0.1755 -0.4621 0.6995 0.087 Uiso 1 1 calc R . . C70 C 0.170957(16) -0.35005(6) 0.74053(3) 0.0814(3) Uani 1 1 d . . . H70A H 0.1644 -0.3021 0.7143 0.098 Uiso 1 1 calc R . . H70B H 0.1545 -0.3801 0.7431 0.098 Uiso 1 1 calc R . . C71 C 0.039909(15) 0.17454(6) 0.63096(2) 0.0696(3) Uani 1 1 d . . . H71A H 0.0410 0.2451 0.6252 0.084 Uiso 1 1 calc R . . H71B H 0.0575 0.1441 0.6335 0.084 Uiso 1 1 calc R . . C72 C 0.036162(14) 0.16003(6) 0.67721(2) 0.0669(3) Uani 1 1 d . . . H72A H 0.0356 0.0893 0.6832 0.080 Uiso 1 1 calc R . . H72B H 0.0523 0.1878 0.7036 0.080 Uiso 1 1 calc R . . C73 C 0.014167(15) 0.30495(6) 0.68677(3) 0.0795(3) Uani 1 1 d . . . H73A H 0.0190 0.3396 0.6627 0.095 Uiso 1 1 calc R . . H73B H 0.0289 0.3172 0.7185 0.095 Uiso 1 1 calc R . . C74 C -0.012368(16) 0.33956(6) 0.68541(3) 0.0840(3) Uani 1 1 d . . . H74A H -0.0181 0.3003 0.7071 0.101 Uiso 1 1 calc R . . H74B H -0.0109 0.4085 0.6956 0.101 Uiso 1 1 calc R . . C75 C -0.059935(16) 0.35944(6) 0.62889(3) 0.0914(4) Uani 1 1 d . . . H75A H -0.0702 0.3697 0.5944 0.110 Uiso 1 1 calc R . . H75B H -0.0592 0.4227 0.6449 0.110 Uiso 1 1 calc R . . C76 C -0.075193(16) 0.28947(7) 0.64560(3) 0.0959(4) Uani 1 1 d . . . H76A H -0.0662 0.2848 0.6806 0.115 Uiso 1 1 calc R . . H76B H -0.0942 0.3138 0.6372 0.115 Uiso 1 1 calc R . . C77 C -0.079274(16) 0.11424(6) 0.65554(3) 0.0841(3) Uani 1 1 d . . . H77A H -0.0886 0.0575 0.6358 0.101 Uiso 1 1 calc R . . H77B H -0.0908 0.1372 0.6723 0.101 Uiso 1 1 calc R . . C78 C -0.051618(16) 0.08431(6) 0.69095(3) 0.0797(3) Uani 1 1 d . . . H78A H -0.0427 0.1411 0.7110 0.096 Uiso 1 1 calc R . . H78B H -0.0541 0.0334 0.7118 0.096 Uiso 1 1 calc R . . C79 C -0.033296(18) -0.04651(6) 0.66175(3) 0.1066(4) Uani 1 1 d . . . H79A H -0.0523 -0.0693 0.6431 0.128 Uiso 1 1 calc R . . H79B H -0.0265 -0.0814 0.6925 0.128 Uiso 1 1 calc R . . C80 C -0.016010(16) -0.07183(6) 0.63658(2) 0.0764(3) Uani 1 1 d . . . H80A H 0.0037 -0.0640 0.6579 0.092 Uiso 1 1 calc R . . H80B H -0.0191 -0.1408 0.6264 0.092 Uiso 1 1 calc R . . C81 C -0.006369(14) -0.02649(6) 0.56895(2) 0.0723(3) Uani 1 1 d . . . H81A H -0.0171 -0.0052 0.5359 0.087 Uiso 1 1 calc R . . H81B H -0.0028 -0.0972 0.5683 0.087 Uiso 1 1 calc R . . C82 C 0.020558(15) 0.02648(6) 0.58774(3) 0.0711(3) Uani 1 1 d . . . H82A H 0.0320 0.0012 0.6197 0.085 Uiso 1 1 calc R . . H82B H 0.0305 0.0138 0.5668 0.085 Uiso 1 1 calc R . . C83 C 0.013612(15) 0.17774(6) 0.54608(2) 0.0699(3) Uani 1 1 d . . . H83A H 0.0038 0.1329 0.5195 0.084 Uiso 1 1 calc R . . H83B H 0.0320 0.1912 0.5459 0.084 Uiso 1 1 calc R . . C84 C -0.002311(15) 0.27160(7) 0.53892(3) 0.0840(3) Uani 1 1 d . . . H84A H 0.0078 0.3168 0.5653 0.101 Uiso 1 1 calc R . . H84B H -0.0035 0.3023 0.5090 0.101 Uiso 1 1 calc R . . C85 C -0.048493(16) 0.21612(7) 0.49337(3) 0.0917(4) Uani 1 1 d . . . H85A H -0.0413 0.1534 0.4871 0.110 Uiso 1 1 calc R . . H85B H -0.0511 0.2609 0.4666 0.110 Uiso 1 1 calc R . . C86 C -0.075309(17) 0.20063(8) 0.49840(3) 0.1014(4) Uani 1 1 d . . . H86A H -0.0823 0.2632 0.5053 0.122 Uiso 1 1 calc R . . H86B H -0.0892 0.1736 0.4686 0.122 Uiso 1 1 calc R . . C87 C -0.093997(15) 0.11432(7) 0.54564(3) 0.0814(3) Uani 1 1 d . . . H87A H -0.0918 0.0496 0.5609 0.098 Uiso 1 1 calc R . . H87B H -0.1104 0.1116 0.5153 0.098 Uiso 1 1 calc R . . C88 C -0.098704(16) 0.18922(7) 0.57729(3) 0.0911(4) Uani 1 1 d . . . H88A H -0.1003 0.2542 0.5624 0.109 Uiso 1 1 calc R . . H88B H -0.1164 0.1751 0.5802 0.109 Uiso 1 1 calc R . . C89 C 0.26510(3) -0.13903(8) 0.96205(4) 0.1445(6) Uani 1 1 d . . . H89A H 0.2672 -0.1076 0.9346 0.173 Uiso 1 1 calc R . . H89B H 0.2452 -0.1440 0.9555 0.173 Uiso 1 1 calc R . . C90 C 0.27935(2) -0.08587(7) 1.00441(3) 0.1274(6) Uani 1 1 d . . . H90A H 0.2826 -0.0185 0.9962 0.153 Uiso 1 1 calc R . . H90B H 0.2678 -0.0823 1.0231 0.153 Uiso 1 1 calc R . . O91 O 0.304401(16) -0.12860(6) 1.03172(3) 0.1402(4) Uani 1 1 d . . . C92 C 0.30534(2) -0.22167(8) 1.00976(4) 0.1507(6) Uani 1 1 d . . . H92A H 0.3199 -0.2205 0.9969 0.181 Uiso 1 1 calc R . . H92B H 0.3097 -0.2745 1.0336 0.181 Uiso 1 1 calc R . . C93 C 0.27868(2) -0.23891(8) 0.97179(3) 0.1139(5) Uani 1 1 d . . . H93A H 0.2677 -0.2856 0.9818 0.137 Uiso 1 1 calc R . . H93B H 0.2808 -0.2648 0.9432 0.137 Uiso 1 1 calc R . . C94 C 0.25963(3) 0.13171(15) 0.93246(7) 0.2900(11) Uani 1 1 d . . . H94A H 0.2454 0.1493 0.9010 0.348 Uiso 1 1 calc R . . H94B H 0.2553 0.0671 0.9422 0.348 Uiso 1 1 calc R . . C95 C 0.26240(5) 0.19891(13) 0.96443(5) 0.3712(14) Uani 1 1 d . . . H95A H 0.2432 0.2104 0.9615 0.445 Uiso 1 1 calc R . . H95B H 0.2716 0.1641 0.9949 0.445 Uiso 1 1 calc R . . O96 O 0.27280(5) 0.27958(10) 0.97238(9) 0.5580(17) Uani 1 1 d . . . C97 C 0.30150(3) 0.2333(2) 0.95838(6) 0.3302(13) Uani 1 1 d . . . H97A H 0.3059 0.2764 0.9364 0.396 Uiso 1 1 calc R . . H97B H 0.3183 0.2201 0.9871 0.396 Uiso 1 1 calc R . . C98 C 0.28570(3) 0.13524(12) 0.93311(5) 0.1906(8) Uani 1 1 d . . . H98A H 0.2846 0.1326 0.9002 0.229 Uiso 1 1 calc R . . H98B H 0.2963 0.0778 0.9504 0.229 Uiso 1 1 calc R . . C99 C -0.01845(3) -0.47161(10) 0.57863(6) 0.2908(8) Uani 1 1 d . . . H99A H -0.0072 -0.4935 0.6114 0.349 Uiso 1 1 calc R . . H99B H -0.0273 -0.5299 0.5597 0.349 Uiso 1 1 calc R . . C100 C -0.00405(3) -0.43620(10) 0.56261(5) 0.2175(7) Uani 1 1 d . . . H10A H -0.0084 -0.4609 0.5301 0.261 Uiso 1 1 calc R . . H10B H 0.0155 -0.4511 0.5824 0.261 Uiso 1 1 calc R . . O101 O -0.00891(2) -0.33294(8) 0.56176(4) 0.2327(6) Uani 1 1 d . . . C102 C -0.03527(3) -0.32451(9) 0.55633(5) 0.1812(7) Uani 1 1 d . . . H10A' H -0.0477 -0.3252 0.5223 0.217 Uiso 1 1 calc R . . H10B' H -0.0382 -0.2632 0.5707 0.217 Uiso 1 1 calc R . . C104 C 0.37788(4) 0.05533(10) 1.02949(3) 0.2753(11) Uani 1 1 d . . . H10C H 0.3811 0.0016 1.0526 0.330 Uiso 1 1 calc R . . H10D H 0.3853 0.1176 1.0459 0.330 Uiso 1 1 calc R . . C105 C 0.35663(5) 0.0603(2) 1.00394(5) 0.5106(19) Uani 1 1 d . . . H10E H 0.3543 0.1305 0.9958 0.613 Uiso 1 1 calc R . . H10F H 0.3458 0.0491 1.0235 0.613 Uiso 1 1 calc R . . C106 C 0.38724(4) 0.03142(14) 0.98827(6) 0.2988(12) Uani 1 1 d . . . H10C' H 0.3969 0.0879 0.9818 0.359 Uiso 1 1 calc R . . H10D' H 0.3999 -0.0252 0.9967 0.359 Uiso 1 1 calc R . . O103 O 0.36200(3) 0.00890(11) 0.94630(4) 0.2859(7) Uani 1 1 d . . . C108 C 0.00955(2) -0.27377(8) 0.73647(3) 0.1372(6) Uani 1 1 d . . . H10E' H -0.0005 -0.2555 0.7027 0.165 Uiso 1 1 calc R . . H10F' H 0.0255 -0.2297 0.7514 0.165 Uiso 1 1 calc R . . C109 C 0.01808(2) -0.37741(9) 0.74168(4) 0.1512(6) Uani 1 1 d . . . H10G H 0.0197 -0.4002 0.7122 0.181 Uiso 1 1 calc R . . H10H H 0.0364 -0.3844 0.7682 0.181 Uiso 1 1 calc R . . O110 O 0.0000 0.57011(12) 0.7500 0.2977(10) Uani 1 2 d S . . C107 C -0.04004(3) -0.40521(12) 0.57972(5) 0.2828(8) Uani 1 1 d . . . H10G' H -0.0587 -0.4326 0.5625 0.339 Uiso 1 1 calc R . . H10H' H -0.0376 -0.3892 0.6127 0.339 Uiso 1 1 calc R . . C103 C 0.34084(3) 0.01430(15) 0.96075(5) 0.4145(8) Uani 1 1 d . . . H10I H 0.3339 -0.0505 0.9651 0.497 Uiso 1 1 calc R . . H10J H 0.3254 0.0552 0.9397 0.497 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 Fe1 0.06223(5) 0.04150(6) 0.05582(5) -0.00106(5) 0.02318(4) -0.00037(5) P1 0.06193(11) 0.04616(11) 0.05788(9) -0.00121(9) 0.02201(7) -0.00116(10) P2 0.06088(10) 0.04308(11) 0.05607(9) -0.00044(9) 0.02236(7) 0.00031(9) P3 0.06266(10) 0.04228(11) 0.05586(9) -0.00241(9) 0.02210(7) -0.00038(9) P4 0.06674(11) 0.03897(10) 0.05687(9) -0.00054(8) 0.02544(7) -0.00185(9) Na1 0.06496(15) 0.05912(17) 0.07697(15) -0.00528(14) 0.02754(11) -0.00360(15) Na2 0.06204(15) 0.05358(16) 0.06541(14) -0.00252(13) 0.02532(10) 0.00064(14) O1 0.0785(3) 0.0664(3) 0.0672(3) 0.0044(3) 0.0231(2) -0.0023(3) O2 0.0964(3) 0.0687(3) 0.0702(3) -0.0053(3) 0.0311(2) -0.0146(3) O3 0.0575(3) 0.0570(3) 0.0885(3) -0.0091(3) 0.0249(2) -0.0038(3) O4 0.0746(3) 0.0517(3) 0.0875(3) -0.0061(3) 0.0256(2) -0.0045(3) O5 0.0644(3) 0.0744(3) 0.0823(3) 0.0039(3) 0.0254(2) 0.0082(3) O6 0.0635(3) 0.0671(3) 0.0783(3) -0.0084(3) 0.0256(2) 0.0025(3) O7 0.0746(3) 0.0740(3) 0.0718(3) -0.0161(3) 0.0301(2) -0.0123(3) O8 0.0779(3) 0.0628(3) 0.1010(3) -0.0111(3) 0.0470(2) -0.0061(3) O9 0.1638(4) 0.0742(4) 0.1101(3) 0.0131(3) 0.0984(2) 0.0143(3) O10 0.0969(3) 0.0688(3) 0.1027(3) 0.0121(3) 0.0586(2) 0.0060(3) O11 0.0764(3) 0.0808(4) 0.0763(3) 0.0168(3) 0.0319(2) 0.0121(3) O12 0.0666(3) 0.0762(4) 0.0704(3) 0.0060(3) 0.0193(2) 0.0055(3) N1 0.0683(4) 0.0631(4) 0.0669(3) 0.0052(3) 0.0175(3) 0.0037(3) N2 0.0813(4) 0.0578(4) 0.0956(4) -0.0174(3) 0.0461(2) -0.0111(3) N3 0.0576(3) 0.0541(4) 0.0656(3) 0.0068(3) 0.0203(2) 0.0047(3) N4 0.0643(4) 0.0680(4) 0.0810(3) -0.0015(3) 0.0266(3) -0.0056(3) C1 0.0558(4) 0.0545(4) 0.0505(3) 0.0023(3) 0.0215(3) 0.0114(4) C2 0.0527(4) 0.0445(4) 0.0567(3) -0.0025(3) 0.0205(3) -0.0014(3) C3 0.0449(3) 0.0296(4) 0.0694(4) 0.0019(3) 0.0240(3) -0.0039(3) C4 0.0507(4) 0.0413(4) 0.0512(3) 0.0078(3) 0.0151(3) 0.0013(3) C5 0.0542(4) 0.0571(4) 0.0478(3) 0.0031(3) 0.0170(3) -0.0002(4) C6 0.0822(4) 0.0589(5) 0.0834(4) -0.0073(4) 0.0411(3) -0.0117(4) C7 0.1156(6) 0.0602(5) 0.0908(4) -0.0201(4) 0.0517(4) -0.0126(5) C8 0.0962(6) 0.0622(5) 0.0747(5) -0.0124(4) 0.0093(4) -0.0166(5) C9 0.0955(5) 0.0811(6) 0.1247(6) -0.0291(5) 0.0551(4) -0.0368(5) C10 0.0787(4) 0.0754(5) 0.0812(4) -0.0187(4) 0.0408(3) -0.0167(4) C11 0.0689(4) 0.0387(4) 0.0581(3) -0.0003(3) 0.0285(3) 0.0028(3) C12 0.0626(4) 0.0427(4) 0.0553(3) -0.0002(3) 0.0191(3) 0.0078(4) C13 0.0874(5) 0.0501(4) 0.0590(4) -0.0069(3) 0.0326(3) -0.0021(4) C14 0.0926(5) 0.0765(6) 0.0537(4) -0.0066(4) 0.0218(3) -0.0015(5) C15 0.0729(5) 0.0643(5) 0.0629(4) 0.0004(4) 0.0182(3) 0.0076(4) C16 0.0707(4) 0.0381(4) 0.0672(4) 0.0016(3) 0.0260(3) 0.0002(4) C17 0.0625(4) 0.0495(4) 0.0523(3) -0.0025(3) 0.0296(2) 0.0030(3) C18 0.0623(4) 0.0621(5) 0.0636(4) -0.0061(4) 0.0311(3) -0.0010(4) C19 0.0697(4) 0.0695(5) 0.0709(4) 0.0014(4) 0.0332(3) -0.0039(4) C20 0.0963(5) 0.0596(5) 0.0605(4) -0.0052(4) 0.0376(3) -0.0220(4) C21 0.0919(5) 0.0483(4) 0.0639(4) -0.0043(4) 0.0299(3) -0.0015(4) C22 0.0575(4) 0.0558(4) 0.0603(4) -0.0022(4) 0.0214(3) -0.0034(4) C23 0.0570(4) 0.0477(4) 0.0519(3) 0.0014(3) 0.0235(3) -0.0015(3) C24 0.0666(4) 0.0457(4) 0.0714(4) 0.0002(4) 0.0289(3) 0.0007(4) C25 0.0891(5) 0.0486(5) 0.0742(4) -0.0013(4) 0.0364(3) 0.0008(4) C26 0.0913(5) 0.0588(5) 0.0911(5) -0.0226(4) 0.0359(4) -0.0179(4) C27 0.0627(5) 0.0774(5) 0.0748(4) -0.0187(4) 0.0148(3) 0.0101(4) C28 0.0640(4) 0.0511(4) 0.0716(4) -0.0018(4) 0.0221(3) 0.0043(4) C29 0.0734(4) 0.0336(4) 0.0594(3) -0.0013(3) 0.0266(3) -0.0055(3) C30 0.0818(5) 0.0519(5) 0.0591(4) -0.0028(4) 0.0167(3) 0.0052(4) C31 0.1045(6) 0.0588(5) 0.0600(4) -0.0030(4) 0.0178(4) 0.0099(5) C32 0.1212(5) 0.0416(4) 0.0786(4) -0.0103(4) 0.0513(3) -0.0018(4) C33 0.0720(4) 0.0587(5) 0.0785(4) -0.0055(4) 0.0338(3) 0.0028(4) C34 0.0732(4) 0.0423(4) 0.0752(4) -0.0101(3) 0.0369(3) -0.0049(4) C35 0.0593(4) 0.0401(4) 0.0511(3) -0.0004(3) 0.0244(3) -0.0016(3) C36 0.0704(4) 0.0420(4) 0.0638(4) 0.0029(3) 0.0206(3) -0.0024(4) C37 0.0962(5) 0.0442(4) 0.0689(4) -0.0078(4) 0.0215(4) -0.0090(4) C38 0.1058(6) 0.0398(4) 0.0940(5) 0.0017(4) 0.0317(4) 0.0065(4) C39 0.0824(5) 0.0742(5) 0.0716(4) 0.0101(4) 0.0245(4) 0.0114(5) C40 0.0589(4) 0.0576(5) 0.0640(4) 0.0016(4) 0.0234(3) 0.0032(4) C41 0.0426(3) 0.0471(4) 0.0548(3) -0.0006(3) 0.0156(3) 0.0087(3) C42 0.0716(4) 0.0461(4) 0.0640(4) 0.0008(3) 0.0272(3) -0.0075(4) C43 0.0813(4) 0.0658(5) 0.0731(4) 0.0082(4) 0.0400(3) 0.0033(4) C44 0.0885(5) 0.0709(5) 0.0635(4) -0.0019(4) 0.0338(3) 0.0073(4) C45 0.0606(4) 0.0656(5) 0.0670(4) -0.0121(4) 0.0158(3) -0.0018(4) C46 0.0612(4) 0.0497(4) 0.0559(3) 0.0011(3) 0.0244(3) 0.0043(4) C47 0.0484(4) 0.0458(4) 0.0418(3) 0.0012(3) 0.0134(2) 0.0042(3) C48 0.0739(4) 0.0529(4) 0.0536(3) 0.0027(3) 0.0302(3) 0.0073(4) C49 0.0824(5) 0.0424(4) 0.0675(4) 0.0079(4) 0.0228(3) -0.0051(4) C50 0.0821(4) 0.0500(4) 0.0650(4) 0.0034(4) 0.0333(3) 0.0182(4) C51 0.0598(4) 0.0509(4) 0.0604(4) 0.0067(3) 0.0226(3) 0.0097(4) C52 0.0546(4) 0.0497(4) 0.0595(4) 0.0002(3) 0.0195(3) -0.0072(4) C53 0.0851(5) 0.0758(6) 0.0651(4) 0.0164(4) 0.0168(4) -0.0084(5) C54 0.0967(6) 0.0702(5) 0.0737(4) 0.0159(4) 0.0261(4) -0.0097(5) C55 0.1202(5) 0.0838(6) 0.1007(4) -0.0176(5) 0.0686(3) -0.0171(5) C56 0.0877(5) 0.0860(6) 0.1142(5) -0.0177(5) 0.0609(3) -0.0230(5) C57 0.0642(4) 0.0697(5) 0.1278(5) -0.0264(5) 0.0432(4) -0.0040(4) C58 0.0688(5) 0.0576(5) 0.1015(5) -0.0108(4) 0.0340(3) 0.0007(4) C59 0.0769(5) 0.0613(5) 0.0906(5) -0.0089(4) 0.0288(4) -0.0042(4) C60 0.0844(5) 0.0574(5) 0.0974(5) -0.0109(4) 0.0316(4) -0.0119(4) C61 0.0734(5) 0.0680(5) 0.0818(5) -0.0036(4) 0.0146(4) -0.0020(5) C62 0.0608(5) 0.0819(6) 0.0867(5) 0.0061(5) 0.0216(4) -0.0006(5) C63 0.0772(5) 0.0790(5) 0.0597(4) 0.0101(4) 0.0248(3) 0.0192(4) C64 0.0647(5) 0.0751(5) 0.0728(4) 0.0143(4) 0.0193(3) 0.0073(4) C65 0.0650(5) 0.0877(6) 0.0814(5) 0.0173(5) 0.0229(3) -0.0005(5) C66 0.0648(5) 0.0899(6) 0.0854(5) 0.0153(5) 0.0294(3) -0.0049(5) C67 0.0774(5) 0.1026(7) 0.0714(4) -0.0040(5) 0.0275(3) 0.0041(5) C68 0.0728(5) 0.0815(6) 0.0747(5) -0.0080(5) 0.0166(4) 0.0100(5) C69 0.0704(5) 0.0558(5) 0.0897(5) -0.0157(4) 0.0295(3) -0.0043(4) C70 0.0582(5) 0.0748(6) 0.1048(5) -0.0202(5) 0.0251(4) -0.0091(4) C71 0.0601(4) 0.0776(5) 0.0663(4) -0.0013(4) 0.0197(3) -0.0073(4) C72 0.0588(4) 0.0667(5) 0.0673(4) -0.0055(4) 0.0164(3) -0.0080(4) C73 0.0593(4) 0.0988(6) 0.0839(4) -0.0296(4) 0.0320(3) -0.0147(5) C74 0.0922(5) 0.0736(5) 0.0998(5) -0.0270(4) 0.0522(3) -0.0191(5) C75 0.0853(5) 0.0640(5) 0.1360(6) -0.0160(5) 0.0555(4) 0.0085(4) C76 0.0787(4) 0.0915(6) 0.1391(5) -0.0258(5) 0.0660(3) -0.0104(5) C77 0.0862(5) 0.0849(6) 0.0885(5) -0.0015(5) 0.0421(3) -0.0182(5) C78 0.1019(5) 0.0720(5) 0.0793(4) -0.0055(4) 0.0508(3) -0.0138(5) C79 0.1424(6) 0.0737(6) 0.1412(5) 0.0336(5) 0.0959(4) 0.0107(5) C80 0.0909(5) 0.0556(5) 0.0914(4) 0.0118(4) 0.0452(3) 0.0009(4) C81 0.0840(4) 0.0727(5) 0.0705(4) -0.0116(4) 0.0415(3) 0.0001(4) C82 0.0634(4) 0.0684(5) 0.0794(4) -0.0071(4) 0.0256(3) -0.0040(4) C83 0.0612(4) 0.0722(5) 0.0782(4) 0.0039(4) 0.0295(3) 0.0029(4) C84 0.0876(5) 0.0896(6) 0.0893(4) 0.0156(4) 0.0505(3) -0.0001(5) C85 0.0849(5) 0.1175(7) 0.0721(4) 0.0337(5) 0.0303(3) 0.0233(5) C86 0.0808(5) 0.1355(8) 0.0823(5) 0.0309(5) 0.0261(4) 0.0179(6) C87 0.0698(5) 0.0871(6) 0.0840(5) -0.0105(5) 0.0267(4) -0.0145(5) C88 0.0705(4) 0.0862(6) 0.1310(5) 0.0078(5) 0.0550(3) 0.0111(5) C89 0.1999(11) 0.1172(8) 0.0919(6) 0.0029(6) 0.0311(6) 0.0582(8) C90 0.1586(10) 0.0823(7) 0.0959(7) 0.0029(6) 0.0013(7) 0.0310(7) O91 0.1188(5) 0.1430(6) 0.1376(5) -0.0391(5) 0.0275(4) -0.0011(5) C92 0.1091(8) 0.1159(8) 0.1823(9) -0.0760(7) 0.0092(7) 0.0134(7) C93 0.1339(8) 0.0984(7) 0.0974(6) -0.0020(6) 0.0328(5) -0.0043(7) C94 0.2703(14) 0.2646(19) 0.4144(17) 0.1414(16) 0.2197(10) 0.1136(14) C95 0.667(3) 0.2697(15) 0.1200(10) -0.0161(10) 0.0940(12) 0.2574(15) O96 0.491(2) 0.1530(10) 0.621(3) 0.0744(15) -0.221(2) -0.1206(12) C97 0.1665(13) 0.623(3) 0.1502(11) 0.0985(16) 0.0077(9) -0.1512(16) C98 0.1706(10) 0.2463(16) 0.1478(9) 0.0292(11) 0.0552(7) 0.0844(11) C99 0.3514(12) 0.1325(9) 0.5399(14) 0.1718(9) 0.3379(8) 0.1163(9) C100 0.2679(8) 0.1408(12) 0.3588(10) -0.0181(9) 0.2468(5) 0.0249(8) O101 0.2375(8) 0.1787(9) 0.3351(9) 0.0904(7) 0.1698(5) 0.0164(7) C102 0.1904(10) 0.1120(10) 0.2755(12) 0.0276(9) 0.1284(7) 0.0431(8) C104 0.614(2) 0.1351(10) 0.0793(5) -0.0587(6) 0.1388(8) -0.0262(14) C105 0.869(3) 0.599(4) 0.1593(7) -0.0839(14) 0.3056(9) 0.065(3) C106 0.3193(19) 0.2984(17) 0.2939(16) -0.1793(13) 0.1371(13) -0.1668(15) O103 0.3556(11) 0.2676(13) 0.3004(9) -0.1088(9) 0.1997(7) -0.1009(11) C108 0.1745(10) 0.1092(7) 0.1151(7) 0.0326(5) 0.0435(6) -0.0380(7) C109 0.1397(8) 0.1339(10) 0.1867(9) -0.0053(8) 0.0715(6) 0.0071(8) O110 0.4413(17) 0.1260(12) 0.4499(16) 0.000 0.3088(10) 0.000 C107 0.3451(9) 0.1661(14) 0.5219(11) 0.0345(12) 0.3687(6) 0.0320(10) C103 0.4132(8) 0.4734(18) 0.5991(9) -0.4038(11) 0.4589(5) -0.3269(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 Fe1 P2 2.2194(3) . ? Fe1 P1 2.22921(19) . ? Fe1 P4 2.2471(2) . ? Fe1 P3 2.2506(3) . ? P1 C1 1.8097(8) . ? P1 C5 1.8122(7) . ? P2 C2 1.7938(6) . ? P2 C23 1.8174(7) . ? P3 C3 1.8014(6) . ? P3 C29 1.8309(8) . ? P4 C4 1.8078(7) . ? P4 C47 1.8347(8) . ? Na1 O3 2.4180(6) . ? Na1 O1 2.4811(6) . ? Na1 O5 2.4849(6) . ? Na1 O2 2.4886(6) . ? Na1 O4 2.5488(5) . ? Na1 O6 2.5507(5) . ? Na1 N1 2.6857(8) . ? Na1 N2 2.7174(8) . ? Na2 O12 2.4201(5) . ? Na2 O7 2.4378(5) . ? Na2 O10 2.4676(6) . ? Na2 O8 2.4793(6) . ? Na2 O9 2.5212(7) . ? Na2 O11 2.5508(6) . ? Na2 N4 2.7154(8) . ? Na2 N3 2.7705(7) . ? O1 C53 1.4129(9) . ? O1 C63 1.4361(11) . ? O2 C55 1.4409(12) . ? O2 C54 1.4413(10) . ? O3 C58 1.4076(9) . ? O3 C59 1.4145(9) . ? O4 C61 1.4214(10) . ? O4 C60 1.4296(9) . ? O5 C67 1.4201(10) . ? O5 C66 1.4231(10) . ? O6 C69 1.4057(10) . ? O6 C68 1.4268(10) . ? O7 C73 1.4101(10) . ? O7 C72 1.4226(10) . ? O8 C75 1.4289(10) . ? O8 C74 1.4449(8) . ? O9 C79 1.3225(11) . ? O9 C78 1.4169(11) . ? O10 C80 1.4189(9) . ? O10 C81 1.4189(11) . ? O11 C85 1.4314(8) . ? O11 C84 1.4337(10) . ? O12 C86 1.4060(11) . ? O12 C87 1.4167(11) . ? N1 C64 1.4536(10) . ? N1 C62 1.4644(10) . ? N1 C65 1.4761(10) . ? N2 C56 1.4487(11) . ? N2 C70 1.4822(9) . ? N2 C57 1.4980(10) . ? N3 C83 1.4532(10) . ? N3 C82 1.4584(10) . ? N3 C71 1.4728(8) . ? N4 C77 1.4635(11) . ? N4 C76 1.4656(11) . ? N4 C88 1.4738(9) . ? C1 C2 1.3620(9) . ? C1 C11 1.4958(8) . ? C2 C17 1.4776(10) . ? C3 C4 1.3913(9) . ? C3 C35 1.4636(9) . ? C4 C41 1.4829(9) . ? C5 C6 1.3653(12) . ? C5 C10 1.3775(12) . ? C6 C7 1.3736(11) . ? C7 C8 1.3690(14) . ? C8 C9 1.3785(15) . ? C9 C10 1.3947(12) . ? C11 C12 1.3855(12) . ? C11 C16 1.4048(10) . ? C12 C13 1.3735(9) . ? C13 C14 1.3840(11) . ? C14 C15 1.3835(13) . ? C15 C16 1.3784(9) . ? C17 C22 1.3721(9) . ? C17 C18 1.3883(10) . ? C18 C19 1.4028(11) . ? C19 C20 1.3499(10) . ? C20 C21 1.3777(12) . ? C21 C22 1.4117(11) . ? C23 C28 1.3870(8) . ? C23 C24 1.4029(10) . ? C24 C25 1.3816(10) . ? C25 C26 1.3604(9) . ? C26 C27 1.3826(11) . ? C27 C28 1.3793(10) . ? C29 C34 1.3834(9) . ? C29 C30 1.3856(9) . ? C30 C31 1.3886(12) . ? C31 C32 1.3635(11) . ? C32 C33 1.3710(9) . ? C33 C34 1.4024(11) . ? C35 C36 1.3809(9) . ? C35 C40 1.4121(8) . ? C36 C37 1.3838(10) . ? C37 C38 1.3806(10) . ? C38 C39 1.3746(11) . ? C39 C40 1.3948(11) . ? C41 C46 1.3831(9) . ? C41 C42 1.3992(11) . ? C42 C43 1.3815(10) . ? C43 C44 1.3787(10) . ? C44 C45 1.3868(13) . ? C45 C46 1.3981(10) . ? C47 C52 1.3929(11) . ? C47 C48 1.4111(10) . ? C48 C49 1.3616(11) . ? C49 C50 1.3854(13) . ? C50 C51 1.3638(10) . ? C51 C52 1.3836(11) . ? C53 C54 1.4818(14) . ? C55 C56 1.5193(10) . ? C57 C58 1.4821(13) . ? C59 C60 1.5018(12) . ? C61 C62 1.4667(13) . ? C63 C64 1.5255(11) . ? C65 C66 1.5105(11) . ? C67 C68 1.4757(13) . ? C69 C70 1.5105(13) . ? C71 C72 1.5189(12) . ? C73 C74 1.4613(12) . ? C75 C76 1.4676(14) . ? C77 C78 1.4911(10) . ? C79 C80 1.4484(14) . ? C81 C82 1.4929(10) . ? C83 C84 1.5052(12) . ? C85 C86 1.4952(14) . ? C87 C88 1.4993(13) . ? C89 C90 1.4188(14) . ? C89 C93 1.5202(16) . ? C90 O91 1.3839(13) . ? O91 C92 1.4534(15) . ? C92 C93 1.4477(14) . ? C94 C95 1.311(3) . ? C94 C98 1.366(2) . ? C95 O96 1.217(2) . ? C95 C98 2.029(3) . ? O96 C97 1.839(3) . ? C97 C98 1.611(3) . ? C99 C100 1.160(2) . ? C99 C107 1.468(2) . ? C100 O101 1.4382(18) . ? O101 C102 1.3367(18) . ? C102 C107 1.395(2) . ? C104 C105 1.087(3) . ? C104 C106 1.561(3) . ? C105 C103 1.405(2) . ? C105 C106 1.897(4) . ? C106 O103 1.4733(19) . ? O103 C103 1.354(2) . ? C108 C109 1.4812(16) . ? C108 C108 1.536(3) 2_556 ? C109 O110 1.2971(17) 1_545 ? O110 C109 1.2968(17) 1_565 ? O110 C109 1.2970(17) 2_566 ? 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 P2 Fe1 P1 81.139(8) . . ? P2 Fe1 P4 104.721(8) . . ? P1 Fe1 P4 154.346(10) . . ? P2 Fe1 P3 150.540(10) . . ? P1 Fe1 P3 104.179(8) . . ? P4 Fe1 P3 83.137(8) . . ? C1 P1 C5 105.11(3) . . ? C1 P1 Fe1 113.01(2) . . ? C5 P1 Fe1 122.43(2) . . ? C2 P2 C23 107.44(3) . . ? C2 P2 Fe1 114.59(2) . . ? C23 P2 Fe1 124.12(3) . . ? C3 P3 C29 104.96(3) . . ? C3 P3 Fe1 111.24(2) . . ? C29 P3 Fe1 119.47(3) . . ? C4 P4 C47 106.36(3) . . ? C4 P4 Fe1 111.49(2) . . ? C47 P4 Fe1 121.507(19) . . ? O3 Na1 O1 172.24(2) . . ? O3 Na1 O5 77.80(2) . . ? O1 Na1 O5 108.57(2) . . ? O3 Na1 O2 106.54(2) . . ? O1 Na1 O2 67.58(2) . . ? O5 Na1 O2 173.11(2) . . ? O3 Na1 O4 66.957(17) . . ? O1 Na1 O4 106.285(17) . . ? O5 Na1 O4 107.72(2) . . ? O2 Na1 O4 79.060(19) . . ? O3 Na1 O6 108.688(18) . . ? O1 Na1 O6 78.366(17) . . ? O5 Na1 O6 66.243(19) . . ? O2 Na1 O6 107.03(2) . . ? O4 Na1 O6 173.58(2) . . ? O3 Na1 N1 110.40(2) . . ? O1 Na1 N1 68.84(2) . . ? O5 Na1 N1 69.805(19) . . ? O2 Na1 N1 112.753(19) . . ? O4 Na1 N1 67.28(2) . . ? O6 Na1 N1 111.22(2) . . ? O3 Na1 N2 69.21(2) . . ? O1 Na1 N2 111.70(2) . . ? O5 Na1 N2 109.078(19) . . ? O2 Na1 N2 68.35(2) . . ? O4 Na1 N2 113.31(2) . . ? O6 Na1 N2 68.08(2) . . ? N1 Na1 N2 178.88(2) . . ? O12 Na2 O7 174.15(2) . . ? O12 Na2 O10 81.163(18) . . ? O7 Na2 O10 102.052(18) . . ? O12 Na2 O8 108.878(19) . . ? O7 Na2 O8 68.392(17) . . ? O10 Na2 O8 168.847(18) . . ? O12 Na2 O9 106.59(2) . . ? O7 Na2 O9 79.247(19) . . ? O10 Na2 O9 64.97(2) . . ? O8 Na2 O9 106.51(2) . . ? O12 Na2 O11 66.093(18) . . ? O7 Na2 O11 108.14(2) . . ? O10 Na2 O11 107.70(2) . . ? O8 Na2 O11 81.42(2) . . ? O9 Na2 O11 170.98(2) . . ? O12 Na2 N4 70.59(2) . . ? O7 Na2 N4 112.10(2) . . ? O10 Na2 N4 112.71(2) . . ? O8 Na2 N4 67.78(2) . . ? O9 Na2 N4 67.01(2) . . ? O11 Na2 N4 113.43(2) . . ? O12 Na2 N3 108.85(2) . . ? O7 Na2 N3 68.481(19) . . ? O10 Na2 N3 66.86(2) . . ? O8 Na2 N3 112.74(2) . . ? O9 Na2 N3 113.02(2) . . ? O11 Na2 N3 66.440(18) . . ? N4 Na2 N3 179.38(2) . . ? C53 O1 C63 114.64(5) . . ? C53 O1 Na1 112.63(5) . . ? C63 O1 Na1 112.73(4) . . ? C55 O2 C54 113.77(7) . . ? C55 O2 Na1 113.42(4) . . ? C54 O2 Na1 112.51(5) . . ? C58 O3 C59 113.60(6) . . ? C58 O3 Na1 112.53(4) . . ? C59 O3 Na1 115.29(4) . . ? C61 O4 C60 113.05(6) . . ? C61 O4 Na1 113.48(5) . . ? C60 O4 Na1 110.59(4) . . ? C67 O5 C66 113.57(7) . . ? C67 O5 Na1 115.06(5) . . ? C66 O5 Na1 110.70(4) . . ? C69 O6 C68 113.98(5) . . ? C69 O6 Na1 111.94(4) . . ? C68 O6 Na1 111.51(4) . . ? C73 O7 C72 114.09(6) . . ? C73 O7 Na2 112.82(4) . . ? C72 O7 Na2 114.36(4) . . ? C75 O8 C74 115.92(7) . . ? C75 O8 Na2 112.76(4) . . ? C74 O8 Na2 109.18(4) . . ? C79 O9 C78 120.07(8) . . ? C79 O9 Na2 117.20(6) . . ? C78 O9 Na2 112.43(5) . . ? C80 O10 C81 115.60(6) . . ? C80 O10 Na2 115.77(5) . . ? C81 O10 Na2 114.04(5) . . ? C85 O11 C84 113.97(6) . . ? C85 O11 Na2 111.37(5) . . ? C84 O11 Na2 112.54(4) . . ? C86 O12 C87 113.76(6) . . ? C86 O12 Na2 117.63(5) . . ? C87 O12 Na2 111.50(4) . . ? C64 N1 C62 110.04(5) . . ? C64 N1 C65 111.26(7) . . ? C62 N1 C65 110.71(7) . . ? C64 N1 Na1 108.78(5) . . ? C62 N1 Na1 109.54(5) . . ? C65 N1 Na1 106.42(4) . . ? C56 N2 C70 111.05(6) . . ? C56 N2 C57 112.84(7) . . ? C70 N2 C57 110.95(5) . . ? C56 N2 Na1 108.30(4) . . ? C70 N2 Na1 107.67(5) . . ? C57 N2 Na1 105.72(5) . . ? C83 N3 C82 110.21(6) . . ? C83 N3 C71 111.46(6) . . ? C82 N3 C71 111.31(5) . . ? C83 N3 Na2 109.36(4) . . ? C82 N3 Na2 108.35(5) . . ? C71 N3 Na2 106.00(5) . . ? C77 N4 C76 113.09(7) . . ? C77 N4 C88 111.88(6) . . ? C76 N4 C88 109.55(6) . . ? C77 N4 Na2 109.61(5) . . ? C76 N4 Na2 108.90(5) . . ? C88 N4 Na2 103.34(5) . . ? C2 C1 C11 124.36(7) . . ? C2 C1 P1 115.05(5) . . ? C11 C1 P1 120.55(5) . . ? C1 C2 C17 123.95(5) . . ? C1 C2 P2 113.67(5) . . ? C17 C2 P2 122.25(4) . . ? C4 C3 C35 123.58(6) . . ? C4 C3 P3 114.76(5) . . ? C35 C3 P3 121.62(5) . . ? C3 C4 C41 123.44(6) . . ? C3 C4 P4 115.03(5) . . ? C41 C4 P4 121.10(5) . . ? C6 C5 C10 114.66(7) . . ? C6 C5 P1 125.03(6) . . ? C10 C5 P1 120.13(6) . . ? C5 C6 C7 125.27(8) . . ? C8 C7 C6 119.16(9) . . ? C7 C8 C9 118.11(8) . . ? C8 C9 C10 120.74(9) . . ? C5 C10 C9 122.04(9) . . ? C12 C11 C16 116.85(6) . . ? C12 C11 C1 121.58(6) . . ? C16 C11 C1 121.52(7) . . ? C13 C12 C11 122.06(7) . . ? C12 C13 C14 120.31(8) . . ? C15 C14 C13 119.13(7) . . ? C16 C15 C14 120.19(7) . . ? C15 C16 C11 121.46(8) . . ? C22 C17 C18 116.57(7) . . ? C22 C17 C2 122.46(6) . . ? C18 C17 C2 120.96(6) . . ? C17 C18 C19 122.03(6) . . ? C20 C19 C18 119.67(7) . . ? C19 C20 C21 120.68(8) . . ? C20 C21 C22 118.73(6) . . ? C17 C22 C21 122.29(7) . . ? C28 C23 C24 116.10(6) . . ? C28 C23 P2 117.08(5) . . ? C24 C23 P2 126.71(4) . . ? C25 C24 C23 120.67(6) . . ? C26 C25 C24 121.55(7) . . ? C25 C26 C27 119.45(7) . . ? C28 C27 C26 118.90(6) . . ? C27 C28 C23 123.30(7) . . ? C34 C29 C30 116.97(7) . . ? C34 C29 P3 124.32(5) . . ? C30 C29 P3 118.71(6) . . ? C29 C30 C31 122.33(7) . . ? C32 C31 C30 119.30(7) . . ? C31 C32 C33 120.56(8) . . ? C32 C33 C34 119.54(7) . . ? C29 C34 C33 121.28(6) . . ? C36 C35 C40 117.26(6) . . ? C36 C35 C3 121.44(5) . . ? C40 C35 C3 121.03(6) . . ? C35 C36 C37 122.65(6) . . ? C38 C37 C36 119.96(7) . . ? C39 C38 C37 118.65(7) . . ? C38 C39 C40 121.98(6) . . ? C39 C40 C35 119.47(6) . . ? C46 C41 C42 116.79(6) . . ? C46 C41 C4 121.69(7) . . ? C42 C41 C4 121.49(5) . . ? C43 C42 C41 121.89(6) . . ? C44 C43 C42 120.55(8) . . ? C43 C44 C45 118.89(7) . . ? C44 C45 C46 120.05(6) . . ? C41 C46 C45 121.76(7) . . ? C52 C47 C48 116.53(7) . . ? C52 C47 P4 125.69(5) . . ? C48 C47 P4 117.78(6) . . ? C49 C48 C47 120.41(8) . . ? C48 C49 C50 123.03(7) . . ? C51 C50 C49 116.64(7) . . ? C50 C51 C52 122.22(8) . . ? C51 C52 C47 121.15(7) . . ? O1 C53 C54 109.07(6) . . ? O2 C54 C53 107.52(7) . . ? O2 C55 C56 112.04(7) . . ? N2 C56 C55 113.01(7) . . ? C58 C57 N2 111.61(8) . . ? O3 C58 C57 113.37(6) . . ? O3 C59 C60 106.17(7) . . ? O4 C60 C59 107.52(7) . . ? O4 C61 C62 113.53(6) . . ? N1 C62 C61 113.47(7) . . ? O1 C63 C64 112.23(7) . . ? N1 C64 C63 112.04(6) . . ? N1 C65 C66 111.92(7) . . ? O5 C66 C65 112.64(7) . . ? O5 C67 C68 107.43(7) . . ? O6 C68 C67 109.07(6) . . ? O6 C69 C70 112.61(7) . . ? N2 C70 C69 112.51(6) . . ? N3 C71 C72 111.34(7) . . ? O7 C72 C71 113.08(5) . . ? O7 C73 C74 107.74(7) . . ? O8 C74 C73 107.75(7) . . ? O8 C75 C76 114.26(7) . . ? N4 C76 C75 112.68(8) . . ? N4 C77 C78 110.43(7) . . ? O9 C78 C77 113.16(6) . . ? O9 C79 C80 113.77(8) . . ? O10 C80 C79 109.83(7) . . ? O10 C81 C82 113.16(6) . . ? N3 C82 C81 112.05(6) . . ? N3 C83 C84 111.44(7) . . ? O11 C84 C83 112.51(7) . . ? O11 C85 C86 107.11(7) . . ? O12 C86 C85 107.31(7) . . ? O12 C87 C88 112.38(7) . . ? N4 C88 C87 113.13(7) . . ? C90 C89 C93 104.20(8) . . ? O91 C90 C89 111.74(10) . . ? C90 O91 C92 106.90(7) . . ? C93 C92 O91 108.44(9) . . ? C92 C93 C89 104.07(9) . . ? C95 C94 C98 98.55(17) . . ? O96 C95 C94 134.3(3) . . ? O96 C95 C98 100.2(2) . . ? C94 C95 C98 41.74(12) . . ? C95 O96 C97 89.20(19) . . ? C98 C97 O96 94.82(12) . . ? C94 C98 C97 111.27(16) . . ? C94 C98 C95 39.71(11) . . ? C97 C98 C95 72.99(11) . . ? C100 C99 C107 113.02(14) . . ? C99 C100 O101 106.20(14) . . ? C102 O101 C100 104.85(11) . . ? O101 C102 C107 104.83(11) . . ? C105 C104 C106 89.68(15) . . ? C104 C105 C103 135.2(3) . . ? C104 C105 C106 55.37(16) . . ? C103 C105 C106 85.11(15) . . ? O103 C106 C104 106.63(16) . . ? O103 C106 C105 72.52(12) . . ? C104 C106 C105 34.96(9) . . ? C103 O103 C106 106.23(14) . . ? C109 C108 C108 100.21(8) . 2_556 ? O110 C109 C108 109.82(12) 1_545 . ? C109 O110 C109 112.54(17) 1_565 2_566 ? C102 C107 C99 100.55(14) . . ? O103 C103 C105 94.26(15) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.444 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.058 #=============================================================================== data_compound_5 _database_code_CSD 208891 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H71 Cl3 P4 Ru Sn2' _chemical_formula_weight 1709.18 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' 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' 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 13.3669(1) _cell_length_b 52.3062(3) _cell_length_c 12.5912(1) _cell_angle_alpha 90.00 _cell_angle_beta 115.8570(1) _cell_angle_gamma 90.00 _cell_volume 7922.06(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description cube _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type 'multiple scans' _exptl_absorpt_correction_T_min 0.8512 _exptl_absorpt_correction_T_max 0.8512 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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_% ? _diffrn_reflns_number 32603 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -69 _diffrn_reflns_limit_k_max 70 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.70 _reflns_number_total 18771 _reflns_number_gt 13381 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0701P)^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_extinction_coef ? _refine_ls_number_reflns 18771 _refine_ls_number_parameters 963 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 Cl1 Cl 0.46059(13) -0.22733(3) 0.35033(16) 0.0938(5) Uani 1 1 d . . . Cl2 Cl 0.33521(17) -0.22333(4) 0.48379(18) 0.1140(7) Uani 1 1 d . . . Cl3 Cl 0.22767(14) -0.22084(4) 0.22893(18) 0.1184(7) Uani 1 1 d . . . C89 C 0.3460(4) -0.21278(13) 0.3561(5) 0.0736(16) Uani 1 1 d . . . H89 H 0.3561 -0.1938 0.3597 0.17(4) Uiso 1 1 d R . . Sn1 Sn 0.965378(18) -0.112944(5) 0.292673(19) 0.02331(7) Uani 1 1 d . . . Sn2 Sn 0.681206(18) -0.132514(5) 0.478042(19) 0.02500(7) Uani 1 1 d . . . Ru1 Ru 0.83729(2) -0.124914(5) 0.40158(2) 0.02004(7) Uani 1 1 d . . . P1 P 0.97500(7) -0.139589(18) 0.57209(7) 0.02321(19) Uani 1 1 d . . . P2 P 0.85244(7) -0.166845(18) 0.35534(7) 0.02440(19) Uani 1 1 d . . . P3 P 0.69754(7) -0.107564(18) 0.23611(7) 0.02348(19) Uani 1 1 d . . . P4 P 0.84677(7) -0.083380(17) 0.45315(7) 0.02276(19) Uani 1 1 d . . . C1 C 1.0181(3) -0.17044(7) 0.5732(3) 0.0241(7) Uani 1 1 d . . . C2 C 0.9559(3) -0.18424(7) 0.4651(3) 0.0247(7) Uani 1 1 d . . . C3 C 0.6778(3) -0.07529(7) 0.2446(3) 0.0259(8) Uani 1 1 d . . . C4 C 0.7505(3) -0.06294(7) 0.3531(3) 0.0245(7) Uani 1 1 d . . . C5 C 1.0594(3) -0.12480(7) 0.7121(3) 0.0249(7) Uani 1 1 d . . . C6 C 1.0087(3) -0.11478(7) 0.7783(3) 0.0313(8) Uani 1 1 d . . . H6 H 0.9300 -0.1152 0.7481 0.053(13) Uiso 1 1 d R . . C7 C 1.0720(4) -0.10405(8) 0.8885(3) 0.0438(10) Uani 1 1 d . . . H7 H 1.0373 -0.0973 0.9341 0.050(12) Uiso 1 1 d R . . C8 C 1.1841(4) -0.10345(9) 0.9295(3) 0.0441(11) Uani 1 1 d . . . H8 H 1.2276 -0.0961 1.0047 0.072(15) Uiso 1 1 d R . . C9 C 1.2363(3) -0.11301(8) 0.8670(3) 0.0416(10) Uani 1 1 d . . . H9 H 1.3151 -0.1124 0.8987 0.058(14) Uiso 1 1 d R . . C10 C 1.1750(3) -0.12365(7) 0.7576(3) 0.0315(8) Uani 1 1 d . . . H10 H 1.2113 -0.1302 0.7132 0.035(11) Uiso 1 1 d R . . C11 C 1.1110(3) -0.18284(7) 0.6750(3) 0.0268(8) Uani 1 1 d . . . C12 C 1.1995(3) -0.19408(7) 0.6603(3) 0.0326(9) Uani 1 1 d . . . H12 H 1.1993 -0.1940 0.5848 0.014(8) Uiso 1 1 d R . . C13 C 1.2867(3) -0.20527(8) 0.7548(4) 0.0420(10) Uani 1 1 d . . . H13 H 1.3467 -0.2125 0.7441 0.040(11) Uiso 1 1 d R . . C14 C 1.2874(3) -0.20598(8) 0.8637(3) 0.0425(10) Uani 1 1 d . . . H14 H 1.3477 -0.2138 0.9279 0.050(12) Uiso 1 1 d R . . C15 C 1.2004(3) -0.19525(8) 0.8807(3) 0.0404(10) Uani 1 1 d . . . H15 H 1.2010 -0.1956 0.9565 0.040(11) Uiso 1 1 d R . . C16 C 1.1123(3) -0.18401(7) 0.7855(3) 0.0319(8) Uani 1 1 d . . . H16 H 1.0519 -0.1770 0.7965 0.031(10) Uiso 1 1 d R . . C17 C 0.9732(3) -0.21150(7) 0.4518(3) 0.0255(7) Uani 1 1 d . . . C18 C 1.0098(3) -0.22016(8) 0.3698(3) 0.0327(8) Uani 1 1 d . . . H18 H 1.0235 -0.2081 0.3212 0.026(9) Uiso 1 1 d R . . C19 C 1.0265(3) -0.24581(8) 0.3576(3) 0.0386(9) Uani 1 1 d . . . H19 H 1.0531 -0.2512 0.3025 0.036(10) Uiso 1 1 d R . . C20 C 1.0042(3) -0.26386(8) 0.4264(4) 0.0392(10) Uani 1 1 d . . . H20 H 1.0133 -0.2816 0.4164 0.053(13) Uiso 1 1 d R . . C21 C 0.9690(3) -0.25575(8) 0.5092(4) 0.0407(10) Uani 1 1 d . . . H21 H 0.9545 -0.2679 0.5566 0.037(11) Uiso 1 1 d R . . C22 C 0.9547(3) -0.22975(8) 0.5230(3) 0.0370(9) Uani 1 1 d . . . H22 H 0.9322 -0.2243 0.5814 0.058(13) Uiso 1 1 d R . . C23 C 0.7706(3) -0.18987(7) 0.2421(3) 0.0282(8) Uani 1 1 d . . . C24 C 0.7846(3) -0.19305(8) 0.1414(3) 0.0403(10) Uani 1 1 d . . . H24 H 0.8383 -0.1830 0.1297 0.052(13) Uiso 1 1 d R . . C25 C 0.7215(4) -0.21065(10) 0.0564(4) 0.0558(13) Uani 1 1 d . . . H25 H 0.7325 -0.2129 -0.0126 0.075(16) Uiso 1 1 d R . . C26 C 0.6432(4) -0.22482(10) 0.0727(5) 0.0650(15) Uani 1 1 d . . . H26 H 0.5993 -0.2368 0.0144 0.10(2) Uiso 1 1 d R . . C27 C 0.6276(4) -0.22176(9) 0.1732(5) 0.0573(13) Uani 1 1 d . . . H27 H 0.5719 -0.2314 0.1830 0.063(14) Uiso 1 1 d R . . C28 C 0.6928(3) -0.20469(8) 0.2597(4) 0.0412(10) Uani 1 1 d . . . H28 H 0.6846 -0.2031 0.3306 0.020(9) Uiso 1 1 d R . . C29 C 0.6114(3) -0.12038(7) 0.0904(3) 0.0265(8) Uani 1 1 d . . . C30 C 0.5785(3) -0.14545(8) 0.0846(3) 0.0356(9) Uani 1 1 d . . . H30 H 0.5986 -0.1549 0.1554 0.034(10) Uiso 1 1 d R . . C31 C 0.5165(3) -0.15706(9) -0.0233(4) 0.0465(11) Uani 1 1 d . . . H31 H 0.4932 -0.1743 -0.0265 0.055(13) Uiso 1 1 d R . . C32 C 0.4887(3) -0.14346(9) -0.1257(3) 0.0445(11) Uani 1 1 d . . . H32 H 0.4457 -0.1514 -0.1997 0.050(12) Uiso 1 1 d R . . C33 C 0.5227(3) -0.11848(8) -0.1221(3) 0.0383(10) Uani 1 1 d . . . H33 H 0.5035 -0.1093 -0.1934 0.019(9) Uiso 1 1 d R . . C34 C 0.5851(3) -0.10679(8) -0.0142(3) 0.0336(9) Uani 1 1 d . . . H34 H 0.6097 -0.0897 -0.0114 0.041(12) Uiso 1 1 d R . . C35 C 0.5971(3) -0.06029(7) 0.1419(3) 0.0273(8) Uani 1 1 d . . . C36 C 0.4840(3) -0.06539(8) 0.0952(3) 0.0355(9) Uani 1 1 d . . . H36 H 0.4563 -0.0776 0.1315 0.041(11) Uiso 1 1 d R . . C37 C 0.4112(3) -0.05235(8) -0.0065(4) 0.0437(10) Uani 1 1 d . . . H37 H 0.3336 -0.0557 -0.0386 0.057(13) Uiso 1 1 d R . . C38 C 0.4507(4) -0.03476(9) -0.0606(4) 0.0525(12) Uani 1 1 d . . . H38 H 0.4007 -0.0264 -0.1307 0.067(14) Uiso 1 1 d R . . C39 C 0.5634(3) -0.02928(8) -0.0123(3) 0.0445(10) Uani 1 1 d . . . H39 H 0.5904 -0.0168 -0.0482 0.043(11) Uiso 1 1 d R . . C40 C 0.6376(3) -0.04214(7) 0.0894(3) 0.0342(9) Uani 1 1 d . . . H40 H 0.7149 -0.0385 0.1223 0.022(9) Uiso 1 1 d R . . C41 C 0.7372(3) -0.03545(7) 0.3746(3) 0.0274(8) Uani 1 1 d . . . C42 C 0.6326(3) -0.02585(8) 0.3524(3) 0.0377(9) Uani 1 1 d . . . H42 H 0.5701 -0.0370 0.3225 0.027(10) Uiso 1 1 d R . . C43 C 0.6181(4) -0.00066(9) 0.3729(4) 0.0521(12) Uani 1 1 d . . . H43 H 0.5465 0.0055 0.3589 0.038(11) Uiso 1 1 d R . . C44 C 0.7090(5) 0.01589(9) 0.4146(4) 0.0581(13) Uani 1 1 d . . . H44 H 0.6993 0.0334 0.4276 0.070(15) Uiso 1 1 d R . . C45 C 0.8127(4) 0.00679(8) 0.4369(4) 0.0440(10) Uani 1 1 d . . . H45 H 0.8749 0.0180 0.4659 0.033(10) Uiso 1 1 d R . . C46 C 0.8269(3) -0.01862(7) 0.4172(3) 0.0331(9) Uani 1 1 d . . . H46 H 0.8989 -0.0247 0.4330 0.016(8) Uiso 1 1 d R . . C47 C 0.9385(3) -0.06663(7) 0.5857(3) 0.0254(7) Uani 1 1 d . . . C48 C 0.9009(3) -0.05270(7) 0.6550(3) 0.0307(8) Uani 1 1 d . . . H48 H 0.8237 -0.0521 0.6351 0.026(9) Uiso 1 1 d R . . C49 C 0.9758(3) -0.03977(7) 0.7531(3) 0.0348(9) Uani 1 1 d . . . H49 H 0.9502 -0.0301 0.8004 0.047(12) Uiso 1 1 d R . . C50 C 1.0870(4) -0.04078(8) 0.7821(3) 0.0410(10) Uani 1 1 d . . . H50 H 1.1378 -0.0314 0.8484 0.073(15) Uiso 1 1 d R . . C51 C 1.1267(3) -0.05514(8) 0.7168(3) 0.0350(9) Uani 1 1 d . . . H51 H 1.2043 -0.0561 0.7393 0.050(12) Uiso 1 1 d R . . C52 C 1.0527(3) -0.06813(7) 0.6188(3) 0.0284(8) Uani 1 1 d . . . H52 H 1.0793 -0.0781 0.5736 0.026(9) Uiso 1 1 d R . . C53 C 0.9484(3) -0.07503(7) 0.2156(3) 0.0264(8) Uani 1 1 d . . . C54 C 0.9743(3) -0.05284(7) 0.2831(3) 0.0297(8) Uani 1 1 d . . . H54 H 0.9986 -0.0540 0.3660 0.052(12) Uiso 1 1 d R . . C55 C 0.9651(3) -0.02887(8) 0.2309(3) 0.0361(9) Uani 1 1 d . . . H55 H 0.9834 -0.0139 0.2786 0.061(14) Uiso 1 1 d R . . C56 C 0.9296(3) -0.02673(8) 0.1104(4) 0.0419(10) Uani 1 1 d . . . H56 H 0.9228 -0.0104 0.0745 0.036(10) Uiso 1 1 d R . . C57 C 0.9043(4) -0.04874(8) 0.0438(3) 0.0440(10) Uani 1 1 d . . . H57 H 0.8802 -0.0476 -0.0391 0.041(11) Uiso 1 1 d R . . C58 C 0.9131(3) -0.07206(8) 0.0944(3) 0.0366(9) Uani 1 1 d . . . H58 H 0.8946 -0.0868 0.0457 0.033(10) Uiso 1 1 d R . . C59 C 1.1406(3) -0.11550(7) 0.4110(3) 0.0276(8) Uani 1 1 d . . . C60 C 1.2082(3) -0.09405(8) 0.4431(3) 0.0336(9) Uani 1 1 d . . . H60 H 1.1777 -0.0777 0.4137 0.027(10) Uiso 1 1 d R . . C61 C 1.3218(3) -0.09650(9) 0.5192(3) 0.0416(10) Uani 1 1 d . . . H61 H 1.3672 -0.0816 0.5425 0.036(10) Uiso 1 1 d R . . C62 C 1.3680(3) -0.11970(9) 0.5599(3) 0.0384(10) Uani 1 1 d . . . H62 H 1.4454 -0.1211 0.6098 0.029(10) Uiso 1 1 d R . . C63 C 1.3018(3) -0.14140(9) 0.5284(3) 0.0402(10) Uani 1 1 d . . . H63 H 1.3338 -0.1577 0.5567 0.082(17) Uiso 1 1 d R . . C64 C 1.1893(3) -0.13935(8) 0.4558(3) 0.0337(9) Uani 1 1 d . . . H64 H 1.1443 -0.1543 0.4358 0.045(12) Uiso 1 1 d R . . C65 C 0.9442(3) -0.13707(7) 0.1442(3) 0.0275(8) Uani 1 1 d . . . C66 C 1.0273(3) -0.15338(8) 0.1470(3) 0.0342(9) Uani 1 1 d . . . H66 H 1.0967 -0.1537 0.2150 0.038(11) Uiso 1 1 d R . . C67 C 1.0108(3) -0.16923(9) 0.0526(4) 0.0442(10) Uani 1 1 d . . . H67 H 1.0685 -0.1805 0.0572 0.051(13) Uiso 1 1 d R . . C68 C 0.9111(3) -0.16886(8) -0.0487(3) 0.0428(10) Uani 1 1 d . . . H68 H 0.9003 -0.1796 -0.1136 0.056(13) Uiso 1 1 d R . . C69 C 0.8274(3) -0.15260(8) -0.0540(3) 0.0408(10) Uani 1 1 d . . . H69 H 0.7585 -0.1522 -0.1227 0.046(12) Uiso 1 1 d R . . C70 C 0.8444(3) -0.13678(7) 0.0418(3) 0.0321(8) Uani 1 1 d . . . H70 H 0.7867 -0.1256 0.0369 0.050(13) Uiso 1 1 d R . . C71 C 0.6906(3) -0.16597(7) 0.5842(3) 0.0280(8) Uani 1 1 d . . . C72 C 0.7656(3) -0.18587(8) 0.6071(3) 0.0375(9) Uani 1 1 d . . . H72 H 0.8209 -0.1848 0.5790 0.028(10) Uiso 1 1 d R . . C73 C 0.7618(4) -0.20731(9) 0.6702(4) 0.0458(11) Uani 1 1 d . . . H73 H 0.8137 -0.2208 0.6843 0.050(13) Uiso 1 1 d R . . C74 C 0.6824(3) -0.20904(8) 0.7125(3) 0.0407(10) Uani 1 1 d . . . H74 H 0.6800 -0.2236 0.7562 0.026(9) Uiso 1 1 d R . . C75 C 0.6073(4) -0.18964(8) 0.6910(4) 0.0451(10) Uani 1 1 d . . . H75 H 0.5528 -0.1908 0.7202 0.041(11) Uiso 1 1 d R . . C76 C 0.6102(3) -0.16835(8) 0.6267(4) 0.0415(10) Uani 1 1 d . . . H76 H 0.5568 -0.1552 0.6114 0.067(15) Uiso 1 1 d R . . C77 C 0.5121(3) -0.13777(7) 0.3430(3) 0.0287(8) Uani 1 1 d . . . C78 C 0.4856(3) -0.16010(9) 0.2805(4) 0.0455(11) Uani 1 1 d . . . H78 H 0.5410 -0.1729 0.2993 0.080(17) Uiso 1 1 d R . . C79 C 0.3801(4) -0.16470(10) 0.1902(4) 0.0547(12) Uani 1 1 d . . . H79 H 0.3646 -0.1803 0.1475 0.11(2) Uiso 1 1 d R . . C80 C 0.2984(3) -0.14639(9) 0.1634(3) 0.0466(11) Uani 1 1 d . . . H80 H 0.2263 -0.1491 0.1012 0.042(11) Uiso 1 1 d R . . C81 C 0.3225(4) -0.12452(10) 0.2273(4) 0.0520(12) Uani 1 1 d . . . H81 H 0.2655 -0.1122 0.2119 0.057(14) Uiso 1 1 d R . . C82 C 0.4289(3) -0.11956(9) 0.3149(3) 0.0390(10) Uani 1 1 d . . . H82 H 0.4446 -0.1037 0.3556 0.044(12) Uiso 1 1 d R . . C83 C 0.6644(3) -0.10130(7) 0.5825(3) 0.0293(8) Uani 1 1 d . . . C84 C 0.7013(3) -0.10368(8) 0.7043(3) 0.0354(9) Uani 1 1 d . . . H84 H 0.7362 -0.1191 0.7421 0.034(11) Uiso 1 1 d R . . C85 C 0.6886(3) -0.08430(9) 0.7708(3) 0.0446(11) Uani 1 1 d . . . H85 H 0.7157 -0.0864 0.8537 0.040(11) Uiso 1 1 d R . . C86 C 0.6366(3) -0.06164(9) 0.7185(4) 0.0477(11) Uani 1 1 d . . . H86 H 0.6264 -0.0484 0.7647 0.043(11) Uiso 1 1 d R . . C87 C 0.6002(3) -0.05855(8) 0.5997(4) 0.0408(10) Uani 1 1 d . . . H87 H 0.5654 -0.0430 0.5632 0.044(12) Uiso 1 1 d R . . C88 C 0.6136(3) -0.07801(8) 0.5316(3) 0.0348(9) Uani 1 1 d . . . H88 H 0.5879 -0.0755 0.4491 0.013(8) Uiso 1 1 d 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 Cl1 0.0809(10) 0.0873(13) 0.1266(14) 0.0455(10) 0.0576(10) 0.0353(9) Cl2 0.1316(16) 0.1195(17) 0.1171(14) -0.0411(12) 0.0786(13) -0.0412(13) Cl3 0.0776(11) 0.1235(18) 0.1129(14) 0.0480(12) 0.0032(10) -0.0114(11) C89 0.060(3) 0.062(4) 0.091(4) 0.006(3) 0.025(3) 0.005(3) Sn1 0.02297(12) 0.02146(15) 0.02424(12) -0.00054(9) 0.00911(10) 0.00038(9) Sn2 0.02352(13) 0.02400(15) 0.02624(13) 0.00170(10) 0.00971(10) 0.00023(10) Ru1 0.02009(13) 0.01724(17) 0.01954(13) -0.00003(10) 0.00562(10) 0.00043(10) P1 0.0222(4) 0.0210(5) 0.0210(4) -0.0002(3) 0.0044(3) 0.0015(4) P2 0.0280(5) 0.0191(5) 0.0212(4) -0.0005(3) 0.0062(3) 0.0013(4) P3 0.0219(4) 0.0210(5) 0.0219(4) 0.0011(3) 0.0043(3) 0.0000(4) P4 0.0241(4) 0.0189(5) 0.0218(4) -0.0007(3) 0.0068(3) 0.0006(4) C1 0.0234(17) 0.019(2) 0.0261(17) 0.0029(14) 0.0074(14) 0.0033(14) C2 0.0228(17) 0.019(2) 0.0284(17) 0.0024(14) 0.0077(14) -0.0018(14) C3 0.0230(17) 0.028(2) 0.0258(17) 0.0058(15) 0.0101(14) 0.0033(15) C4 0.0235(17) 0.020(2) 0.0297(17) -0.0003(14) 0.0117(14) 0.0004(14) C5 0.0275(18) 0.019(2) 0.0228(16) 0.0018(13) 0.0063(14) 0.0015(14) C6 0.037(2) 0.027(2) 0.0279(18) 0.0019(15) 0.0119(16) 0.0011(16) C7 0.061(3) 0.040(3) 0.031(2) -0.0100(18) 0.021(2) -0.003(2) C8 0.053(3) 0.042(3) 0.0242(19) -0.0033(18) 0.0043(18) 0.001(2) C9 0.035(2) 0.035(3) 0.036(2) -0.0057(18) -0.0020(17) -0.0050(18) C10 0.0284(19) 0.027(2) 0.0335(19) -0.0026(16) 0.0088(16) 0.0013(16) C11 0.0268(18) 0.020(2) 0.0243(17) 0.0015(14) 0.0030(14) 0.0023(15) C12 0.033(2) 0.027(2) 0.034(2) 0.0012(16) 0.0108(16) 0.0051(16) C13 0.027(2) 0.038(3) 0.047(2) 0.0010(19) 0.0033(17) 0.0081(18) C14 0.032(2) 0.033(3) 0.039(2) 0.0087(18) -0.0056(18) 0.0047(17) C15 0.041(2) 0.039(3) 0.027(2) 0.0046(17) 0.0021(17) -0.0071(19) C16 0.036(2) 0.026(2) 0.0309(19) 0.0056(16) 0.0120(16) -0.0010(16) C17 0.0218(16) 0.022(2) 0.0240(16) -0.0010(14) 0.0022(13) 0.0014(14) C18 0.040(2) 0.027(2) 0.0308(19) -0.0024(16) 0.0155(16) 0.0000(17) C19 0.046(2) 0.031(3) 0.040(2) -0.0063(18) 0.0202(19) 0.0047(18) C20 0.046(2) 0.014(2) 0.050(2) -0.0029(17) 0.0132(19) 0.0065(17) C21 0.046(2) 0.025(2) 0.051(2) 0.0053(19) 0.022(2) -0.0008(18) C22 0.041(2) 0.029(2) 0.044(2) 0.0064(18) 0.0218(18) 0.0074(18) C23 0.0284(18) 0.016(2) 0.0278(18) 0.0012(14) 0.0010(14) 0.0026(14) C24 0.049(2) 0.031(3) 0.033(2) -0.0049(17) 0.0107(18) -0.0063(19) C25 0.074(3) 0.046(3) 0.034(2) -0.018(2) 0.011(2) -0.009(3) C26 0.055(3) 0.049(4) 0.060(3) -0.023(3) -0.004(3) -0.008(2) C27 0.045(3) 0.032(3) 0.081(4) -0.009(2) 0.014(2) -0.013(2) C28 0.038(2) 0.031(3) 0.049(2) -0.0024(19) 0.0139(19) -0.0014(18) C29 0.0206(17) 0.024(2) 0.0266(17) 0.0017(14) 0.0027(14) 0.0036(14) C30 0.032(2) 0.030(2) 0.0307(19) -0.0009(16) 0.0000(16) -0.0019(17) C31 0.044(2) 0.032(3) 0.046(2) -0.0049(19) 0.0037(19) -0.005(2) C32 0.034(2) 0.054(3) 0.030(2) -0.0120(19) 0.0001(17) 0.002(2) C33 0.036(2) 0.042(3) 0.029(2) -0.0010(18) 0.0073(16) 0.0091(19) C34 0.037(2) 0.033(3) 0.0249(18) 0.0007(16) 0.0078(16) 0.0033(17) C35 0.0261(18) 0.022(2) 0.0270(17) 0.0022(14) 0.0054(14) 0.0044(15) C36 0.0294(19) 0.034(3) 0.035(2) 0.0016(17) 0.0072(16) 0.0063(17) C37 0.028(2) 0.040(3) 0.046(2) 0.004(2) 0.0001(18) 0.0112(18) C38 0.056(3) 0.039(3) 0.035(2) 0.005(2) -0.006(2) 0.016(2) C39 0.056(3) 0.033(3) 0.037(2) 0.0111(18) 0.013(2) 0.002(2) C40 0.037(2) 0.026(2) 0.033(2) 0.0047(16) 0.0099(16) 0.0016(16) C41 0.0315(18) 0.022(2) 0.0285(18) 0.0034(15) 0.0128(15) 0.0044(15) C42 0.038(2) 0.029(2) 0.044(2) 0.0022(18) 0.0158(18) 0.0063(18) C43 0.058(3) 0.033(3) 0.070(3) 0.005(2) 0.032(2) 0.016(2) C44 0.089(4) 0.019(3) 0.074(3) -0.001(2) 0.043(3) 0.008(3) C45 0.052(3) 0.027(3) 0.051(2) -0.0022(19) 0.021(2) -0.005(2) C46 0.039(2) 0.022(2) 0.038(2) 0.0028(16) 0.0167(17) 0.0011(16) C47 0.0312(18) 0.018(2) 0.0236(16) 0.0012(14) 0.0085(14) -0.0026(14) C48 0.037(2) 0.022(2) 0.0305(19) -0.0016(15) 0.0131(16) -0.0007(16) C49 0.046(2) 0.027(2) 0.0264(18) -0.0038(16) 0.0114(17) 0.0036(18) C50 0.054(3) 0.025(2) 0.0272(19) -0.0026(16) 0.0027(18) -0.0060(19) C51 0.030(2) 0.029(2) 0.034(2) 0.0019(16) 0.0029(16) -0.0016(16) C52 0.0305(19) 0.027(2) 0.0243(17) 0.0004(15) 0.0085(15) -0.0006(15) C53 0.0278(18) 0.021(2) 0.0309(18) 0.0024(15) 0.0130(15) 0.0019(14) C54 0.034(2) 0.026(2) 0.0314(19) 0.0010(15) 0.0164(16) -0.0006(16) C55 0.042(2) 0.025(2) 0.043(2) -0.0045(18) 0.0209(18) -0.0027(17) C56 0.054(3) 0.026(3) 0.048(2) 0.0115(19) 0.025(2) 0.0039(19) C57 0.066(3) 0.037(3) 0.031(2) 0.0064(18) 0.022(2) 0.003(2) C58 0.053(2) 0.025(2) 0.032(2) -0.0018(17) 0.0195(18) -0.0029(18) C59 0.0235(17) 0.034(2) 0.0238(17) 0.0014(15) 0.0089(14) -0.0001(15) C60 0.0255(18) 0.031(2) 0.042(2) -0.0042(17) 0.0116(16) -0.0001(16) C61 0.028(2) 0.050(3) 0.046(2) -0.015(2) 0.0151(18) -0.0125(19) C62 0.0247(19) 0.055(3) 0.0276(19) -0.0034(18) 0.0041(16) 0.0060(19) C63 0.035(2) 0.042(3) 0.037(2) 0.0084(19) 0.0100(18) 0.0092(19) C64 0.0256(19) 0.035(3) 0.036(2) 0.0028(17) 0.0088(16) 0.0004(17) C65 0.0298(18) 0.025(2) 0.0275(17) -0.0036(15) 0.0121(15) -0.0034(15) C66 0.0278(19) 0.033(2) 0.038(2) -0.0066(17) 0.0110(16) -0.0004(16) C67 0.042(2) 0.040(3) 0.053(3) -0.017(2) 0.024(2) 0.001(2) C68 0.051(3) 0.043(3) 0.035(2) -0.0102(19) 0.0196(19) -0.006(2) C69 0.042(2) 0.044(3) 0.0263(19) 0.0019(18) 0.0055(17) -0.0044(19) C70 0.036(2) 0.028(2) 0.0315(19) 0.0023(16) 0.0131(16) 0.0052(17) C71 0.0298(18) 0.022(2) 0.0317(18) 0.0025(15) 0.0131(15) 0.0012(15) C72 0.033(2) 0.043(3) 0.037(2) 0.0041(18) 0.0161(17) 0.0028(18) C73 0.056(3) 0.034(3) 0.045(2) 0.0123(19) 0.020(2) 0.011(2) C74 0.056(3) 0.028(3) 0.035(2) 0.0037(17) 0.0164(19) -0.009(2) C75 0.055(3) 0.038(3) 0.057(3) 0.002(2) 0.038(2) -0.005(2) C76 0.044(2) 0.027(2) 0.066(3) 0.011(2) 0.035(2) 0.0036(19) C77 0.0250(18) 0.031(2) 0.0292(18) 0.0036(16) 0.0111(15) -0.0007(15) C78 0.032(2) 0.034(3) 0.055(3) -0.004(2) 0.0050(19) -0.0018(19) C79 0.050(3) 0.041(3) 0.052(3) -0.006(2) 0.002(2) -0.005(2) C80 0.036(2) 0.058(3) 0.032(2) 0.007(2) 0.0021(18) -0.009(2) C81 0.038(2) 0.063(4) 0.045(3) 0.007(2) 0.008(2) 0.016(2) C82 0.032(2) 0.041(3) 0.035(2) 0.0019(18) 0.0066(17) 0.0034(18) C83 0.0273(18) 0.028(2) 0.0324(19) -0.0018(15) 0.0130(15) -0.0012(15) C84 0.035(2) 0.035(3) 0.034(2) 0.0002(18) 0.0131(17) -0.0009(18) C85 0.047(2) 0.058(3) 0.031(2) -0.012(2) 0.0183(18) -0.010(2) C86 0.047(3) 0.046(3) 0.059(3) -0.021(2) 0.032(2) -0.005(2) C87 0.038(2) 0.027(3) 0.059(3) -0.003(2) 0.023(2) 0.0018(18) C88 0.036(2) 0.032(2) 0.036(2) -0.0001(17) 0.0159(17) -0.0013(17) _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 Cl1 C89 1.740(6) . ? Cl2 C89 1.764(6) . ? Cl3 C89 1.742(6) . ? Sn1 C59 2.163(3) . ? Sn1 C65 2.169(3) . ? Sn1 C53 2.176(3) . ? Sn1 Ru1 2.6929(3) . ? Sn2 C83 2.169(4) . ? Sn2 C71 2.172(4) . ? Sn2 C77 2.174(3) . ? Sn2 Ru1 2.6814(3) . ? Ru1 P4 2.2551(9) . ? Ru1 P1 2.2671(9) . ? Ru1 P3 2.2933(9) . ? Ru1 P2 2.3007(10) . ? P1 C1 1.711(4) . ? P1 C5 1.801(3) . ? P2 C2 1.728(3) . ? P2 C23 1.822(4) . ? P3 C3 1.719(4) . ? P3 C29 1.817(3) . ? P4 C4 1.724(3) . ? P4 C47 1.809(3) . ? C1 C2 1.441(5) . ? C1 C11 1.488(4) . ? C2 C17 1.466(5) . ? C3 C4 1.439(5) . ? C3 C35 1.494(4) . ? C4 C41 1.488(5) . ? C5 C6 1.386(5) . ? C5 C10 1.395(5) . ? C6 C7 1.389(5) . ? C7 C8 1.356(6) . ? C8 C9 1.355(6) . ? C9 C10 1.376(5) . ? C11 C16 1.385(5) . ? C11 C12 1.403(5) . ? C12 C13 1.381(5) . ? C13 C14 1.367(6) . ? C14 C15 1.390(6) . ? C15 C16 1.392(5) . ? C17 C18 1.397(5) . ? C17 C22 1.404(5) . ? C18 C19 1.380(5) . ? C19 C20 1.398(6) . ? C20 C21 1.384(6) . ? C21 C22 1.395(6) . ? C23 C24 1.371(5) . ? C23 C28 1.390(5) . ? C24 C25 1.384(5) . ? C25 C26 1.370(7) . ? C26 C27 1.378(7) . ? C27 C28 1.384(6) . ? C29 C30 1.375(5) . ? C29 C34 1.400(5) . ? C30 C31 1.385(5) . ? C31 C32 1.375(6) . ? C32 C33 1.378(6) . ? C33 C34 1.388(5) . ? C35 C36 1.388(5) . ? C35 C40 1.394(5) . ? C36 C37 1.402(5) . ? C37 C38 1.379(6) . ? C38 C39 1.386(6) . ? C39 C40 1.403(5) . ? C41 C46 1.392(5) . ? C41 C42 1.395(5) . ? C42 C43 1.372(6) . ? C43 C44 1.395(7) . ? C44 C45 1.374(6) . ? C45 C46 1.380(6) . ? C47 C48 1.390(5) . ? C47 C52 1.397(5) . ? C48 C49 1.381(5) . ? C49 C50 1.368(6) . ? C50 C51 1.379(6) . ? C51 C52 1.378(5) . ? C53 C54 1.391(5) . ? C53 C58 1.396(5) . ? C54 C55 1.396(5) . ? C55 C56 1.382(5) . ? C56 C57 1.377(6) . ? C57 C58 1.357(5) . ? C59 C60 1.386(5) . ? C59 C64 1.406(5) . ? C60 C61 1.404(5) . ? C61 C62 1.357(6) . ? C62 C63 1.386(6) . ? C63 C64 1.382(5) . ? C65 C66 1.388(5) . ? C65 C70 1.394(5) . ? C66 C67 1.386(5) . ? C67 C68 1.386(6) . ? C68 C69 1.383(6) . ? C69 C70 1.397(5) . ? C71 C72 1.386(5) . ? C71 C76 1.400(5) . ? C72 C73 1.388(6) . ? C73 C74 1.382(6) . ? C74 C75 1.370(6) . ? C75 C76 1.387(6) . ? C77 C78 1.366(6) . ? C77 C82 1.388(5) . ? C78 C79 1.393(6) . ? C79 C80 1.380(6) . ? C80 C81 1.354(6) . ? C81 C82 1.392(6) . ? C83 C84 1.397(5) . ? C83 C88 1.406(5) . ? C84 C85 1.372(6) . ? C85 C86 1.386(6) . ? C86 C87 1.366(6) . ? C87 C88 1.392(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 Cl1 C89 Cl3 108.6(4) . . ? Cl1 C89 Cl2 109.0(3) . . ? Cl3 C89 Cl2 111.1(3) . . ? C59 Sn1 C65 104.63(13) . . ? C59 Sn1 C53 103.58(13) . . ? C65 Sn1 C53 101.35(13) . . ? C59 Sn1 Ru1 111.89(9) . . ? C65 Sn1 Ru1 115.50(9) . . ? C53 Sn1 Ru1 118.24(9) . . ? C83 Sn2 C71 103.10(13) . . ? C83 Sn2 C77 102.83(13) . . ? C71 Sn2 C77 98.08(13) . . ? C83 Sn2 Ru1 114.14(9) . . ? C71 Sn2 Ru1 119.68(9) . . ? C77 Sn2 Ru1 116.40(9) . . ? P4 Ru1 P1 97.65(3) . . ? P4 Ru1 P3 78.55(3) . . ? P1 Ru1 P3 176.01(3) . . ? P4 Ru1 P2 172.36(3) . . ? P1 Ru1 P2 78.00(3) . . ? P3 Ru1 P2 105.91(3) . . ? P4 Ru1 Sn2 89.67(2) . . ? P1 Ru1 Sn2 92.71(2) . . ? P3 Ru1 Sn2 86.09(2) . . ? P2 Ru1 Sn2 96.76(2) . . ? P4 Ru1 Sn1 87.38(2) . . ? P1 Ru1 Sn1 97.30(2) . . ? P3 Ru1 Sn1 83.81(2) . . ? P2 Ru1 Sn1 86.97(2) . . ? Sn2 Ru1 Sn1 169.856(13) . . ? C1 P1 C5 109.39(16) . . ? C1 P1 Ru1 117.29(11) . . ? C5 P1 Ru1 133.20(12) . . ? C2 P2 C23 106.02(17) . . ? C2 P2 Ru1 115.32(12) . . ? C23 P2 Ru1 137.66(12) . . ? C3 P3 C29 112.22(16) . . ? C3 P3 Ru1 114.75(11) . . ? C29 P3 Ru1 132.68(12) . . ? C4 P4 C47 111.32(17) . . ? C4 P4 Ru1 117.18(12) . . ? C47 P4 Ru1 131.50(12) . . ? C2 C1 C11 121.0(3) . . ? C2 C1 P1 114.3(2) . . ? C11 C1 P1 124.7(3) . . ? C1 C2 C17 122.7(3) . . ? C1 C2 P2 115.0(3) . . ? C17 C2 P2 122.1(2) . . ? C4 C3 C35 121.3(3) . . ? C4 C3 P3 116.2(2) . . ? C35 C3 P3 122.3(3) . . ? C3 C4 C41 121.5(3) . . ? C3 C4 P4 113.3(3) . . ? C41 C4 P4 125.2(2) . . ? C6 C5 C10 118.7(3) . . ? C6 C5 P1 119.3(3) . . ? C10 C5 P1 122.0(3) . . ? C5 C6 C7 120.6(4) . . ? C8 C7 C6 118.7(4) . . ? C9 C8 C7 122.3(4) . . ? C8 C9 C10 119.8(4) . . ? C9 C10 C5 119.9(4) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 C1 121.6(3) . . ? C12 C11 C1 120.3(3) . . ? C13 C12 C11 120.5(4) . . ? C14 C13 C12 120.6(4) . . ? C13 C14 C15 120.2(3) . . ? C14 C15 C16 119.2(4) . . ? C11 C16 C15 121.3(4) . . ? C18 C17 C22 117.9(3) . . ? C18 C17 C2 121.6(3) . . ? C22 C17 C2 120.5(3) . . ? C19 C18 C17 121.5(4) . . ? C18 C19 C20 120.0(4) . . ? C21 C20 C19 119.6(4) . . ? C20 C21 C22 120.2(4) . . ? C21 C22 C17 120.7(4) . . ? C24 C23 C28 119.5(4) . . ? C24 C23 P2 121.8(3) . . ? C28 C23 P2 118.7(3) . . ? C23 C24 C25 120.9(4) . . ? C26 C25 C24 119.5(4) . . ? C25 C26 C27 120.4(4) . . ? C26 C27 C28 120.1(5) . . ? C27 C28 C23 119.5(4) . . ? C30 C29 C34 119.4(3) . . ? C30 C29 P3 116.9(3) . . ? C34 C29 P3 123.5(3) . . ? C29 C30 C31 120.7(4) . . ? C32 C31 C30 119.6(4) . . ? C31 C32 C33 120.6(4) . . ? C32 C33 C34 119.9(4) . . ? C33 C34 C29 119.6(4) . . ? C36 C35 C40 120.4(3) . . ? C36 C35 C3 120.5(3) . . ? C40 C35 C3 119.0(3) . . ? C35 C36 C37 119.2(4) . . ? C38 C37 C36 120.8(4) . . ? C37 C38 C39 119.9(4) . . ? C38 C39 C40 120.1(4) . . ? C35 C40 C39 119.6(4) . . ? C46 C41 C42 118.0(4) . . ? C46 C41 C4 122.0(3) . . ? C42 C41 C4 120.0(3) . . ? C43 C42 C41 121.3(4) . . ? C42 C43 C44 119.7(4) . . ? C45 C44 C43 119.9(4) . . ? C44 C45 C46 120.1(4) . . ? C45 C46 C41 121.1(4) . . ? C48 C47 C52 119.3(3) . . ? C48 C47 P4 123.2(3) . . ? C52 C47 P4 117.5(3) . . ? C49 C48 C47 119.9(3) . . ? C50 C49 C48 120.0(4) . . ? C49 C50 C51 121.2(4) . . ? C52 C51 C50 119.3(4) . . ? C51 C52 C47 120.3(3) . . ? C54 C53 C58 116.8(3) . . ? C54 C53 Sn1 122.6(2) . . ? C58 C53 Sn1 120.6(3) . . ? C53 C54 C55 121.0(3) . . ? C56 C55 C54 120.4(4) . . ? C57 C56 C55 118.5(4) . . ? C58 C57 C56 121.1(4) . . ? C57 C58 C53 122.2(4) . . ? C60 C59 C64 118.2(3) . . ? C60 C59 Sn1 121.6(3) . . ? C64 C59 Sn1 120.3(3) . . ? C59 C60 C61 119.9(4) . . ? C62 C61 C60 121.2(4) . . ? C61 C62 C63 119.7(4) . . ? C64 C63 C62 120.0(4) . . ? C63 C64 C59 120.9(4) . . ? C66 C65 C70 117.5(3) . . ? C66 C65 Sn1 122.2(3) . . ? C70 C65 Sn1 120.3(3) . . ? C67 C66 C65 121.3(3) . . ? C68 C67 C66 120.6(4) . . ? C69 C68 C67 119.1(4) . . ? C68 C69 C70 119.9(4) . . ? C65 C70 C69 121.5(4) . . ? C72 C71 C76 117.4(3) . . ? C72 C71 Sn2 125.2(3) . . ? C76 C71 Sn2 117.3(3) . . ? C71 C72 C73 121.5(4) . . ? C74 C73 C72 119.9(4) . . ? C75 C74 C73 119.7(4) . . ? C74 C75 C76 120.3(4) . . ? C75 C76 C71 121.1(4) . . ? C78 C77 C82 117.6(3) . . ? C78 C77 Sn2 118.6(3) . . ? C82 C77 Sn2 123.8(3) . . ? C77 C78 C79 122.2(4) . . ? C80 C79 C78 119.4(5) . . ? C81 C80 C79 118.9(4) . . ? C80 C81 C82 121.7(4) . . ? C77 C82 C81 120.1(4) . . ? C84 C83 C88 116.6(3) . . ? C84 C83 Sn2 121.2(3) . . ? C88 C83 Sn2 122.2(3) . . ? C85 C84 C83 121.7(4) . . ? C84 C85 C86 120.8(4) . . ? C87 C86 C85 119.2(4) . . ? C86 C87 C88 120.5(4) . . ? C87 C88 C83 121.3(4) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.70 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.721 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.113 #===============================================================================