# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2122 data_global #======================================================== # SUBMISSION DETAILS _publ_contact_author ; Dr. Mike Ward School of Chemistry Cantock's Close University of Bristol Bristol BS8 1TS ; _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the crystal structure in the paper Polynuclear osmium-dioxolene complexes: comparison of...' by A. M. Barthram et al, submitted to Dalton Transactions for publication. ; #======================================================== data_sad _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 F6 N4 O2 Os P' _chemical_formula_weight 755.63 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' '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' 'F' 'F' 0.0171 0.0103 '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' 'Os' 'Os' -1.2165 7.6030 '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' _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 11.8056(14) _cell_length_b 14.869(3) _cell_length_c 14.909(3) _cell_angle_alpha 90.000(11) _cell_angle_beta 104.011(10) _cell_angle_gamma 90.000(14) _cell_volume 2539.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green ' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.977 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 5.163 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.08 _exptl_absorpt_correction_T_max 0.60 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8036 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2910 _reflns_number_gt 2647 _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^)+(0.0311P)^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 2910 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0549 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Os1 Os 0.5000 0.528215(13) 0.7500 0.02330(7) Uani 1 2 d S . . O31 O 0.56508(19) 0.63105(16) 0.68970(14) 0.0286(5) Uani 1 1 d . . . N11 N 0.3587(2) 0.51871(19) 0.63788(18) 0.0273(6) Uani 1 1 d . . . N21 N 0.5586(2) 0.43573(19) 0.66887(17) 0.0240(5) Uani 1 1 d . . . C22 C 0.4834(3) 0.4155(2) 0.5865(2) 0.0263(6) Uani 1 1 d . . . C12 C 0.3701(3) 0.4607(2) 0.5700(2) 0.0289(7) Uani 1 1 d . . . C26 C 0.6660(3) 0.3980(2) 0.6874(2) 0.0310(7) Uani 1 1 d . . . H26 H 0.7194 0.4118 0.7444 0.037 Uiso 1 1 calc R . . C32 C 0.5343(3) 0.7119(2) 0.7167(2) 0.0291(7) Uani 1 1 d . . . C23 C 0.5149(3) 0.3572(2) 0.5241(2) 0.0315(7) Uani 1 1 d . . . H23A H 0.4608 0.3436 0.4674 0.038 Uiso 1 1 calc R . . C13 C 0.2795(3) 0.4478(3) 0.4916(3) 0.0372(8) Uani 1 1 d . . . H13A H 0.2880 0.4066 0.4450 0.045 Uiso 1 1 calc R . . C16 C 0.2578(3) 0.5651(3) 0.6282(2) 0.0336(8) Uani 1 1 d . . . H16A H 0.2499 0.6058 0.6754 0.040 Uiso 1 1 calc R . . C25 C 0.7012(3) 0.3401(3) 0.6270(2) 0.0340(8) Uani 1 1 d . . . H25A H 0.7775 0.3150 0.6422 0.041 Uiso 1 1 calc R . . C14 C 0.1770(4) 0.4959(3) 0.4826(3) 0.0446(10) Uani 1 1 d . . . H14A H 0.1145 0.4884 0.4294 0.053 Uiso 1 1 calc R . . C33 C 0.5650(3) 0.7930(3) 0.6829(2) 0.0363(8) Uani 1 1 d . . . H33 H 0.6087 0.7933 0.6371 0.044 Uiso 1 1 calc R . . C15 C 0.1660(3) 0.5548(3) 0.5515(3) 0.0418(9) Uani 1 1 d . . . H15A H 0.0959 0.5880 0.5462 0.050 Uiso 1 1 calc R . . C34 C 0.5320(3) 0.8734(3) 0.7157(3) 0.0406(9) Uani 1 1 d . . . H34 H 0.5525 0.9288 0.6920 0.049 Uiso 1 1 calc R . . C24 C 0.6242(3) 0.3192(3) 0.5443(2) 0.0348(8) Uani 1 1 d . . . H24A H 0.6464 0.2792 0.5019 0.042 Uiso 1 1 calc R . . P1 P 0.5000 0.16809(12) 0.7500 0.0878(9) Uani 1 2 d S . . F1 F 0.5069(4) 0.1671(2) 0.6454(3) 0.1144(15) Uani 1 1 d . . . F3 F 0.4051(4) 0.0914(4) 0.7269(3) 0.1318(16) Uani 1 1 d . . . F2 F 0.4078(8) 0.2395(4) 0.7269(4) 0.324(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Os1 0.02483(10) 0.02980(11) 0.01608(9) 0.000 0.00652(6) 0.000 O31 0.0341(12) 0.0313(13) 0.0217(11) -0.0008(10) 0.0093(9) -0.0038(11) N11 0.0274(13) 0.0348(16) 0.0199(13) 0.0035(12) 0.0065(10) -0.0011(12) N21 0.0270(13) 0.0272(14) 0.0187(12) 0.0014(11) 0.0075(10) -0.0013(12) C22 0.0309(15) 0.0291(17) 0.0193(14) 0.0025(13) 0.0070(12) -0.0026(15) C12 0.0329(17) 0.0319(19) 0.0221(15) 0.0027(14) 0.0069(13) -0.0033(15) C26 0.0302(16) 0.038(2) 0.0255(16) 0.0006(15) 0.0076(13) -0.0002(15) C32 0.0293(17) 0.0343(19) 0.0206(15) 0.0003(14) 0.0001(12) -0.0009(15) C23 0.0396(18) 0.0336(18) 0.0211(15) -0.0034(15) 0.0069(13) -0.0054(16) C13 0.0388(19) 0.041(2) 0.0275(17) -0.0012(15) 0.0003(15) -0.0027(17) C16 0.0311(17) 0.041(2) 0.0305(17) 0.0039(16) 0.0107(14) 0.0042(16) C25 0.0323(17) 0.038(2) 0.0337(18) 0.0004(16) 0.0117(14) 0.0043(16) C14 0.036(2) 0.057(3) 0.035(2) 0.0037(19) -0.0027(16) -0.0028(19) C33 0.0332(18) 0.042(2) 0.0301(18) 0.0018(16) 0.0019(14) -0.0057(17) C15 0.0294(18) 0.055(3) 0.039(2) 0.0083(18) 0.0046(15) 0.0064(17) C34 0.0308(18) 0.038(2) 0.048(2) 0.0065(18) -0.0011(15) -0.0054(17) C24 0.046(2) 0.0336(19) 0.0293(17) -0.0047(15) 0.0179(15) 0.0011(17) P1 0.179(3) 0.0315(9) 0.0899(15) 0.000 0.1037(18) 0.000 F1 0.225(4) 0.063(2) 0.096(3) 0.0001(19) 0.117(3) -0.005(3) F3 0.134(3) 0.173(5) 0.107(3) 0.019(3) 0.067(3) -0.045(4) F2 0.695(19) 0.192(5) 0.135(6) 0.065(5) 0.197(10) 0.307(9) _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 O31 2.018(2) 2_656 ? Os1 O31 2.018(2) . ? Os1 N21 2.058(3) . ? Os1 N21 2.058(3) 2_656 ? Os1 N11 2.061(3) . ? Os1 N11 2.061(3) 2_656 ? O31 C32 1.345(4) . ? N11 C16 1.354(4) . ? N11 C12 1.361(4) . ? N21 C26 1.353(4) . ? N21 C22 1.363(4) . ? C22 C23 1.387(5) . ? C22 C12 1.463(5) . ? C12 C13 1.393(5) . ? C26 C25 1.380(5) . ? C32 C33 1.389(5) . ? C32 C32 1.425(7) 2_656 ? C23 C24 1.374(5) . ? C13 C14 1.385(6) . ? C16 C15 1.380(5) . ? C25 C24 1.379(5) . ? C14 C15 1.379(6) . ? C33 C34 1.383(6) . ? C34 C34 1.410(8) 2_656 ? P1 F2 1.499(6) 2_656 ? P1 F2 1.499(5) . ? P1 F3 1.577(5) 2_656 ? P1 F3 1.577(5) . ? P1 F1 1.582(3) 2_656 ? P1 F1 1.582(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Os1 O31 81.46(13) 2_656 . ? O31 Os1 N21 170.54(9) 2_656 . ? O31 Os1 N21 91.50(10) . . ? O31 Os1 N21 91.50(10) 2_656 2_656 ? O31 Os1 N21 170.55(9) . 2_656 ? N21 Os1 N21 96.16(15) . 2_656 ? O31 Os1 N11 95.32(10) 2_656 . ? O31 Os1 N11 90.65(10) . . ? N21 Os1 N11 78.38(11) . . ? N21 Os1 N11 96.31(10) 2_656 . ? O31 Os1 N11 90.65(10) 2_656 2_656 ? O31 Os1 N11 95.32(10) . 2_656 ? N21 Os1 N11 96.30(10) . 2_656 ? N21 Os1 N11 78.38(11) 2_656 2_656 ? N11 Os1 N11 172.13(16) . 2_656 ? C32 O31 Os1 112.6(2) . . ? C16 N11 C12 119.1(3) . . ? C16 N11 Os1 124.8(2) . . ? C12 N11 Os1 116.1(2) . . ? C26 N21 C22 117.8(3) . . ? C26 N21 Os1 126.1(2) . . ? C22 N21 Os1 116.0(2) . . ? N21 C22 C23 121.3(3) . . ? N21 C22 C12 114.8(3) . . ? C23 C22 C12 123.8(3) . . ? N11 C12 C13 121.1(3) . . ? N11 C12 C22 114.6(3) . . ? C13 C12 C22 124.2(3) . . ? N21 C26 C25 122.8(3) . . ? O31 C32 C33 123.7(3) . . ? O31 C32 C32 116.67(18) . 2_656 ? C33 C32 C32 119.7(2) . 2_656 ? C24 C23 C22 120.1(3) . . ? C14 C13 C12 119.0(4) . . ? N11 C16 C15 121.7(3) . . ? C24 C25 C26 119.1(3) . . ? C15 C14 C13 119.6(4) . . ? C34 C33 C32 120.1(4) . . ? C14 C15 C16 119.4(4) . . ? C33 C34 C34 120.2(2) . 2_656 ? C23 C24 C25 118.9(3) . . ? F2 P1 F2 89.9(7) 2_656 . ? F2 P1 F3 91.4(4) 2_656 2_656 ? F2 P1 F3 178.7(4) . 2_656 ? F2 P1 F3 178.7(4) 2_656 . ? F2 P1 F3 91.4(4) . . ? F3 P1 F3 87.4(4) 2_656 . ? F2 P1 F1 89.3(3) 2_656 2_656 ? F2 P1 F1 91.4(3) . 2_656 ? F3 P1 F1 88.9(2) 2_656 2_656 ? F3 P1 F1 90.3(2) . 2_656 ? F2 P1 F1 91.4(3) 2_656 . ? F2 P1 F1 89.3(3) . . ? F3 P1 F1 90.3(2) 2_656 . ? F3 P1 F1 88.9(2) . . ? F1 P1 F1 178.9(3) 2_656 . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.890 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.104