# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 data_cop20m5 _audit_creation_date 2013-05-06 _audit_creation_method ; Olex2 1.2 (compiled Apr 9 2013 14:10:59, GUI svn.r4458) ; _chemical_name_common ? _chemical_name_systematic Osmium(0)(eta4-1,5-cyclooctadiene)(eta6-1,3,5,7-cyclooctatetraene) _chemical_formula_moiety 'C16 H20 Os' _chemical_formula_sum 'C16 H20 Os' _chemical_formula_weight 402.52 _chemical_melting_point ? 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' Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.293(2) _cell_length_b 8.9556(16) _cell_length_c 13.020(2) _cell_angle_alpha 90 _cell_angle_beta 115.750(4) _cell_angle_gamma 90 _cell_volume 1291.1(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7529 _cell_measurement_temperature 233(2) _cell_measurement_theta_max 32.03 _cell_measurement_theta_min 2.93 _exptl_absorpt_coefficient_mu 9.851 _exptl_absorpt_correction_T_max 0.2156 _exptl_absorpt_correction_T_min 0.0950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1543 before and 0.0368 after correction. The Ratio of minimum to maximum transmission is 0.4406. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.071 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 768 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method 'crystallized from pentane' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.14 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_unetI/netI 0.0298 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.932 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 19522 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.969 _diffrn_reflns_theta_min 1.839 _diffrn_ambient_temperature 233.15 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'Bruker SMART CCD 1K area detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.932 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 1K area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_source 'sealed X-ray tube' _diffrn_source_target Mo _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3771 _reflns_number_total 4897 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection 'SMART V5.629, Bruker AXS, Inc., USA' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. and MERCURY 3.1, Cambridge Crystallographic Data Centre (CCDC), 2012 ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 1.030 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.170 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 4897 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0195 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0188P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0424 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Os1 Os 0.26757(2) 0.08392(2) 0.24916(2) 0.02253(3) Uani 1 1 d . . . . . C1 C 0.2430(3) -0.1432(3) 0.1792(2) 0.0338(6) Uani 1 1 d . . . . . H1 H 0.305(3) -0.156(3) 0.148(3) 0.041 Uiso 1 1 d . U . . . C2 C 0.2998(3) -0.1513(3) 0.3007(2) 0.0317(5) Uani 1 1 d . . . . . H2 H 0.385(3) -0.174(3) 0.327(3) 0.038 Uiso 1 1 d . U . . . C3 C 0.2365(3) -0.2056(3) 0.3717(3) 0.0370(6) Uani 1 1 d . . . . . H3A H 0.294(3) -0.262(3) 0.441(3) 0.044 Uiso 1 1 d . U . . . H3B H 0.172(3) -0.279(3) 0.327(3) 0.044 Uiso 1 1 d . U . . . C4 C 0.1857(3) -0.0758(3) 0.4138(2) 0.0366(6) Uani 1 1 d . . . . . H4A H 0.116(3) -0.108(3) 0.420(3) 0.044 Uiso 1 1 d . U . . . H4B H 0.249(3) -0.044(3) 0.493(3) 0.044 Uiso 1 1 d . U . . . C5 C 0.1554(2) 0.0578(3) 0.3349(2) 0.0280(5) Uani 1 1 d . . . . . H5 H 0.144(3) 0.145(3) 0.372(3) 0.034 Uiso 1 1 d . U . . . C6 C 0.0832(2) 0.0465(3) 0.2131(2) 0.0288(5) Uani 1 1 d . . . . . H6 H 0.031(3) 0.134(3) 0.173(3) 0.035 Uiso 1 1 d . U . . . C7 C 0.0288(3) -0.1000(3) 0.1541(2) 0.0373(6) Uani 1 1 d . . . . . H7A H -0.0500 -0.0802 0.0902 0.045 Uiso 1 1 calc R U . . . H7B H 0.0158 -0.1656 0.2080 0.045 Uiso 1 1 calc R U . . . C8 C 0.1097(3) -0.1792(3) 0.1096(3) 0.0413(7) Uani 1 1 d . . . . . H8A H 0.087(3) -0.148(4) 0.034(3) 0.050 Uiso 1 1 d . U . . . H8B H 0.095(3) -0.279(4) 0.105(3) 0.050 Uiso 1 1 d . U . . . C9 C 0.3369(3) 0.4122(3) 0.3233(3) 0.0372(6) Uani 1 1 d . . . . . H9 H 0.336(3) 0.517(4) 0.317(3) 0.045 Uiso 1 1 d . U . . . C10 C 0.4286(3) 0.3385(3) 0.3998(3) 0.0383(6) Uani 1 1 d . . . . . H10 H 0.498(3) 0.397(3) 0.457(3) 0.046 Uiso 1 1 d . U . . . C11 C 0.4306(3) 0.1731(3) 0.3933(2) 0.0345(6) Uani 1 1 d . . . . . H11 H 0.460(3) 0.128(3) 0.460(3) 0.041 Uiso 1 1 d . U . . . C12 C 0.4660(3) 0.1066(3) 0.3127(3) 0.0391(7) Uani 1 1 d . . . . . H12 H 0.525(3) 0.029(4) 0.339(3) 0.047 Uiso 1 1 d . U . . . C13 C 0.4146(3) 0.1328(4) 0.1933(3) 0.0420(7) Uani 1 1 d . . . . . H13 H 0.450(3) 0.077(3) 0.157(3) 0.050 Uiso 1 1 d . U . . . C14 C 0.3078(3) 0.2026(3) 0.1139(3) 0.0402(7) Uani 1 1 d . . . . . H14 H 0.286(3) 0.175(4) 0.036(3) 0.048 Uiso 1 1 d . U . . . C15 C 0.2184(3) 0.2798(3) 0.1319(2) 0.0358(6) Uani 1 1 d . . . . . H15 H 0.146(3) 0.286(3) 0.065(3) 0.043 Uiso 1 1 d . U . . . C16 C 0.2316(3) 0.3253(3) 0.2417(2) 0.0324(5) Uani 1 1 d . . . . . H16 H 0.153(3) 0.346(3) 0.242(2) 0.039 Uiso 1 1 d . U . . . 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 0.02209(5) 0.02232(4) 0.02329(5) -0.00155(4) 0.00998(3) -0.00087(4) C1 0.0421(16) 0.0271(12) 0.0340(14) -0.0091(10) 0.0182(12) -0.0034(11) C2 0.0310(14) 0.0233(12) 0.0401(15) -0.0037(10) 0.0148(12) 0.0015(10) C3 0.0425(16) 0.0275(13) 0.0400(15) 0.0066(11) 0.0171(13) 0.0016(11) C4 0.0458(17) 0.0345(13) 0.0356(14) 0.0028(11) 0.0233(13) -0.0022(12) C5 0.0280(13) 0.0284(12) 0.0310(12) -0.0006(9) 0.0161(10) 0.0003(9) C6 0.0228(12) 0.0296(12) 0.0316(12) -0.0008(9) 0.0098(10) -0.0020(9) C7 0.0294(14) 0.0363(14) 0.0381(14) -0.0019(11) 0.0070(11) -0.0087(11) C8 0.0476(18) 0.0362(15) 0.0341(15) -0.0091(12) 0.0123(13) -0.0099(13) C9 0.0449(16) 0.0244(11) 0.0480(16) -0.0078(12) 0.0254(14) -0.0099(12) C10 0.0412(17) 0.0332(14) 0.0380(15) -0.0070(11) 0.0150(13) -0.0111(12) C11 0.0293(14) 0.0323(13) 0.0327(14) 0.0013(11) 0.0050(11) -0.0051(10) C12 0.0223(13) 0.0318(14) 0.0602(19) -0.0020(12) 0.0151(13) -0.0009(10) C13 0.0401(17) 0.0439(16) 0.057(2) -0.0094(14) 0.0349(16) -0.0087(13) C14 0.0474(18) 0.0457(16) 0.0352(15) -0.0001(12) 0.0251(14) -0.0093(13) C15 0.0337(14) 0.0353(14) 0.0357(14) 0.0103(11) 0.0128(11) -0.0019(11) C16 0.0319(13) 0.0270(12) 0.0403(15) 0.0071(10) 0.0174(12) 0.0034(10) _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 C1 2.195(2) . ? Os1 C2 2.194(3) . ? Os1 C5 2.131(3) . ? Os1 C6 2.132(3) . ? Os1 C11 2.215(3) . ? Os1 C12 2.219(3) . ? Os1 C13 2.265(3) . ? Os1 C14 2.287(3) . ? Os1 C15 2.230(3) . ? Os1 C16 2.200(3) . ? C1 H1 1.02(3) . ? C1 C2 1.427(4) . ? C1 C8 1.523(4) . ? C2 H2 0.97(3) . ? C2 C3 1.523(4) . ? C3 H3A 1.01(3) . ? C3 H3B 1.00(3) . ? C3 C4 1.530(4) . ? C4 H4A 0.94(4) . ? C4 H4B 1.02(3) . ? C4 C5 1.515(3) . ? C5 H5 0.97(3) . ? C5 C6 1.446(4) . ? C6 H6 1.00(3) . ? C6 C7 1.520(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 C8 1.526(4) . ? C8 H8A 0.94(3) . ? C8 H8B 0.90(3) . ? C9 H9 0.94(3) . ? C9 C10 1.313(4) . ? C9 C16 1.489(4) . ? C10 H10 1.00(3) . ? C10 C11 1.484(4) . ? C11 H11 0.88(3) . ? C11 C12 1.429(4) . ? C12 H12 0.95(3) . ? C12 C13 1.420(5) . ? C13 H13 0.92(3) . ? C13 C14 1.416(5) . ? C14 H14 0.96(3) . ? C14 C15 1.401(4) . ? C15 H15 0.94(3) . ? C15 C16 1.426(4) . ? C16 H16 0.98(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 C1 Os1 C11 126.62(11) . . ? C1 Os1 C12 99.81(11) . . ? C1 Os1 C13 91.80(11) . . ? C1 Os1 C14 98.51(11) . . ? C1 Os1 C15 119.82(11) . . ? C1 Os1 C16 154.58(11) . . ? C2 Os1 C1 37.94(11) . . ? C2 Os1 C11 96.34(11) . . ? C2 Os1 C12 87.16(11) . . ? C2 Os1 C13 102.74(11) . . ? C2 Os1 C14 127.65(11) . . ? C2 Os1 C15 157.51(11) . . ? C2 Os1 C16 164.36(10) . . ? C5 Os1 C1 96.42(10) . . ? C5 Os1 C2 78.85(10) . . ? C5 Os1 C6 39.65(10) . . ? C5 Os1 C11 98.59(11) . . ? C5 Os1 C12 132.21(12) . . ? C5 Os1 C13 167.92(11) . . ? C5 Os1 C14 149.29(11) . . ? C5 Os1 C15 113.60(10) . . ? C5 Os1 C16 88.13(10) . . ? C6 Os1 C1 79.70(11) . . ? C6 Os1 C2 87.14(10) . . ? C6 Os1 C11 136.67(11) . . ? C6 Os1 C12 171.11(11) . . ? C6 Os1 C13 151.63(11) . . ? C6 Os1 C14 117.90(11) . . ? C6 Os1 C15 91.53(10) . . ? C6 Os1 C16 88.31(10) . . ? C11 Os1 C12 37.60(11) . . ? C11 Os1 C13 69.37(12) . . ? C11 Os1 C14 93.78(11) . . ? C11 Os1 C15 99.94(10) . . ? C12 Os1 C13 36.92(12) . . ? C12 Os1 C14 70.99(12) . . ? C12 Os1 C15 96.34(11) . . ? C13 Os1 C14 36.24(12) . . ? C15 Os1 C13 69.19(12) . . ? C15 Os1 C14 36.11(11) . . ? C16 Os1 C11 76.92(10) . . ? C16 Os1 C12 95.40(11) . . ? C16 Os1 C13 88.22(11) . . ? C16 Os1 C14 67.42(10) . . ? C16 Os1 C15 37.56(9) . . ? Os1 C1 H1 106.0(17) . . ? C2 C1 Os1 70.98(13) . . ? C2 C1 H1 110.3(18) . . ? C2 C1 C8 122.1(3) . . ? C8 C1 Os1 111.20(19) . . ? C8 C1 H1 122.7(17) . . ? Os1 C2 H2 109.6(18) . . ? C1 C2 Os1 71.08(14) . . ? C1 C2 H2 109.9(18) . . ? C1 C2 C3 123.7(3) . . ? C3 C2 Os1 114.84(18) . . ? C3 C2 H2 118.1(18) . . ? C2 C3 H3A 111.0(17) . . ? C2 C3 H3B 110.2(17) . . ? C2 C3 C4 111.8(2) . . ? H3A C3 H3B 105(2) . . ? C4 C3 H3A 107.3(17) . . ? C4 C3 H3B 111.4(18) . . ? C3 C4 H4A 108.9(18) . . ? C3 C4 H4B 108.6(18) . . ? H4A C4 H4B 109(2) . . ? C5 C4 C3 112.0(2) . . ? C5 C4 H4A 109.5(19) . . ? C5 C4 H4B 108.6(17) . . ? Os1 C5 H5 116.5(18) . . ? C4 C5 Os1 114.67(18) . . ? C4 C5 H5 110.3(18) . . ? C6 C5 Os1 70.22(14) . . ? C6 C5 C4 122.8(2) . . ? C6 C5 H5 117.0(18) . . ? Os1 C6 H6 111.8(18) . . ? C5 C6 Os1 70.12(14) . . ? C5 C6 H6 117.9(18) . . ? C5 C6 C7 122.7(2) . . ? C7 C6 Os1 116.06(18) . . ? C7 C6 H6 111.5(18) . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C6 C7 C8 112.1(2) . . ? H7A C7 H7B 107.9 . . ? C8 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C1 C8 C7 112.7(2) . . ? C1 C8 H8A 108(2) . . ? C1 C8 H8B 112(2) . . ? C7 C8 H8A 108(2) . . ? C7 C8 H8B 110(2) . . ? H8A C8 H8B 105(3) . . ? C10 C9 H9 123(2) . . ? C10 C9 C16 118.2(3) . . ? C16 C9 H9 119(2) . . ? C9 C10 H10 118.3(17) . . ? C9 C10 C11 119.2(3) . . ? C11 C10 H10 122.3(17) . . ? Os1 C11 H11 120(2) . . ? C10 C11 Os1 112.2(2) . . ? C10 C11 H11 114.2(19) . . ? C12 C11 Os1 71.33(16) . . ? C12 C11 C10 118.4(3) . . ? C12 C11 H11 114(2) . . ? Os1 C12 H12 127(2) . . ? C11 C12 Os1 71.07(16) . . ? C11 C12 H12 117.8(19) . . ? C13 C12 Os1 73.31(17) . . ? C13 C12 C11 127.0(3) . . ? C13 C12 H12 114.9(19) . . ? Os1 C13 H13 133(2) . . ? C12 C13 Os1 69.78(16) . . ? C12 C13 H13 113(2) . . ? C14 C13 Os1 72.74(17) . . ? C14 C13 C12 134.7(3) . . ? C14 C13 H13 111(2) . . ? Os1 C14 H14 130(2) . . ? C13 C14 Os1 71.02(16) . . ? C13 C14 H14 114(2) . . ? C15 C14 Os1 69.70(15) . . ? C15 C14 C13 129.9(3) . . ? C15 C14 H14 115(2) . . ? Os1 C15 H15 123.6(18) . . ? C14 C15 Os1 74.19(16) . . ? C14 C15 H15 111.4(19) . . ? C14 C15 C16 123.5(3) . . ? C16 C15 Os1 70.09(15) . . ? C16 C15 H15 124.6(19) . . ? Os1 C16 H16 111.6(17) . . ? C9 C16 Os1 112.7(2) . . ? C9 C16 H16 116.6(17) . . ? C15 C16 Os1 72.35(15) . . ? C15 C16 C9 123.4(3) . . ? C15 C16 H16 111.7(17) . . ? _database_code_depnum_ccdc_archive ? _shelx_estimated_absorpt_T_max 0.339 _shelx_estimated_absorpt_T_min 0.130 _shelx_hkl_checksum 35947 _shelx_hkl_file ; 1 0 0 23.10 0.71 1 0 0 22.56 0.70 -1 0 0 22.87 0.80 -1 0 0 23.08 0.70 1 0 0 24.61 0.81 2 0 0 802.51 22.38 2 0 0 819.21 22.08 -2 0 0 812.86 22.09 -2 0 0 679.87 22.37 -2 0 0 883.10 23.29 3 0 0 35.46 1.13 3 0 0 34.92 1.08 -3 0 0 34.59 1.52 -3 0 0 35.76 1.11 4 0 0 569.39 16.14 4 0 0 580.14 15.91 -4 0 0 574.81 16.90 5 0 0 139.64 3.90 5 0 0 136.22 3.99 -5 0 0 135.88 4.46 -6 0 0 339.10 10.52 6 0 0 364.22 9.91 6 0 0 343.45 9.73 7 0 0 197.41 5.78 -7 0 0 209.54 6.44 7 0 0 208.11 5.91 -8 0 0 85.44 3.23 8 0 0 82.83 2.54 8 0 0 84.71 2.63 9 0 0 115.31 3.40 -9 0 0 114.40 4.10 9 0 0 113.83 3.49 10 0 0 37.95 1.43 -10 0 0 38.32 2.27 10 0 0 38.12 1.52 11 0 0 104.43 3.28 -11 0 0 106.34 3.85 11 0 0 100.49 3.17 -12 0 0 11.78 1.41 12 0 0 9.48 0.94 13 0 0 63.70 2.29 -13 0 0 65.42 2.89 14 0 0 0.12 0.91 -14 0 0 0.49 1.29 15 0 0 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7.56 0.56 -3 4 4 6.74 0.59 2 -4 -4 167.64 4.84 -2 -4 4 172.26 4.89 -2 4 4 174.71 5.01 -2 4 4 168.48 4.86 2 4 -4 169.01 4.83 2 4 -4 166.74 4.96 -1 -4 4 6.14 0.46 -1 4 4 5.73 0.52 1 4 -4 6.11 0.45 -1 4 4 6.45 0.38 -1 4 4 5.99 0.46 1 4 -4 5.78 0.44 0 -4 4 112.56 3.18 0 4 4 107.83 3.15 0 4 4 103.79 3.21 0 4 -4 109.12 3.09 0 4 4 106.86 3.17 0 4 -4 103.01 3.23 1 -4 4 0.37 0.38 -1 -4 -4 0.53 0.31 -1 4 -4 0.36 0.33 -1 4 -4 0.49 0.46 1 4 4 0.39 0.44 1 4 4 0.57 0.42 -2 -4 -4 112.49 3.55 2 -4 4 119.75 3.50 2 4 4 117.18 3.42 -2 4 -4 119.17 3.71 2 4 4 119.13 3.53 -2 4 -4 119.40 3.38 3 -4 4 5.45 0.53 -3 -4 -4 5.25 0.47 -3 4 -4 4.64 0.79 3 4 4 4.67 0.59 -3 4 -4 4.91 0.42 3 4 4 4.71 0.52 -4 -4 -4 55.31 1.88 4 -4 4 54.53 1.83 -4 4 -4 53.83 1.67 4 4 4 49.96 1.74 4 4 4 56.83 1.95 -4 4 -4 54.17 2.29 -5 -4 -4 10.03 0.78 5 -4 4 11.63 0.81 5 4 4 10.14 0.71 -5 4 -4 12.96 1.16 -5 4 -4 10.25 0.62 5 4 4 11.09 0.90 6 -4 4 22.32 1.17 -6 -4 -4 22.04 1.39 6 4 4 22.05 1.12 -6 4 -4 24.58 1.54 -6 4 -4 23.93 1.03 6 4 4 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18 5.91 0.92 7 2 -18 4.08 1.08 -6 2 18 2.95 0.87 6 2 -18 4.63 1.09 5 -2 -18 2.93 1.08 5 2 -18 1.27 1.07 4 -2 -18 5.79 1.18 4 2 -18 7.48 1.13 3 -2 -18 0.80 1.07 3 2 -18 1.33 1.01 -2 -2 18 3.84 2.03 2 -2 -18 7.17 1.17 2 2 -18 4.88 1.12 -1 -2 18 -1.51 1.98 1 2 -18 0.52 1.16 0 -2 18 4.30 2.09 -14 -3 18 22.66 1.66 -13 -3 18 -0.97 1.17 13 -3 -18 -0.51 1.64 12 -3 -18 26.77 2.06 -12 -3 18 23.13 1.49 -12 3 18 25.61 1.82 12 3 -18 25.89 1.77 11 -3 -18 1.32 1.59 -11 -3 18 -0.58 0.99 -11 3 18 1.91 1.05 11 3 -18 1.63 1.26 -10 -3 18 26.02 1.63 10 -3 -18 26.27 2.04 -10 3 18 25.58 1.65 10 3 -18 23.93 1.67 9 -3 -18 8.83 1.68 -9 -3 18 5.46 0.95 -9 3 18 5.05 1.01 9 3 -18 6.77 1.22 -8 -3 18 22.29 1.50 8 3 -18 23.98 1.50 -8 3 18 23.24 1.48 7 3 -18 14.75 1.36 -7 3 18 11.78 1.07 6 3 -18 15.96 1.33 -6 3 18 11.82 1.08 5 3 -18 21.97 1.43 4 -3 -18 6.27 1.25 4 3 -18 9.71 1.17 3 -3 -18 25.05 1.83 3 3 -18 23.52 1.48 -2 -3 18 2.03 2.15 2 3 -18 2.48 1.16 -1 -3 18 19.73 2.33 1 3 -18 18.62 1.60 12 -4 -18 -0.10 1.59 12 4 -18 -0.05 1.38 11 -4 -18 8.65 1.79 11 4 -18 7.08 1.49 10 -4 -18 0.52 1.51 -10 4 18 0.16 1.00 10 4 -18 -0.08 1.23 9 -4 -18 8.16 1.73 -9 -4 18 5.85 1.02 -9 4 18 6.24 1.09 9 4 -18 6.95 1.35 8 4 -18 3.34 1.23 -8 4 18 0.76 0.93 -7 4 18 7.21 1.01 6 -4 -18 0.02 1.13 -6 4 18 2.14 0.93 5 -4 -18 4.13 1.21 4 -4 -18 6.40 1.29 -3 -4 18 0.80 2.13 -2 -4 18 6.90 2.39 11 -5 -18 -2.11 1.68 10 -5 -18 3.74 1.88 10 5 -18 6.61 1.49 9 -5 -18 -1.21 1.80 9 5 -18 2.46 1.32 8 5 -18 4.89 1.30 -8 5 18 4.24 1.05 -7 5 18 1.30 0.97 -6 5 18 1.95 0.97 -3 -5 18 4.52 2.25 9 6 -18 17.54 1.54 12 0 -19 -1.02 1.54 -11 0 19 -0.07 1.04 11 0 -19 0.29 1.48 10 0 -19 -0.71 1.50 -10 0 19 -0.18 1.00 -9 0 19 -0.74 0.92 -8 0 19 -0.06 0.90 7 0 -19 0.02 1.14 -7 0 19 0.47 0.90 6 0 -19 -0.26 1.14 5 0 -19 0.42 1.19 4 0 -19 -1.26 1.14 12 -1 -19 23.49 2.16 12 1 -19 21.56 1.93 -11 -1 19 0.09 1.05 11 -1 -19 0.49 1.72 11 1 -19 1.48 1.49 -10 -1 19 19.71 1.35 10 -1 -19 24.40 1.86 10 1 -19 21.60 1.70 -10 1 19 17.78 1.37 -9 -1 19 2.02 0.92 -9 1 19 2.86 1.00 -8 -1 19 14.88 1.17 -8 1 19 14.28 1.18 7 1 -19 6.05 1.26 -7 1 19 4.25 0.98 6 1 -19 11.12 1.35 5 -1 -19 15.44 1.42 5 1 -19 13.96 1.39 4 1 -19 4.88 1.20 12 -2 -19 2.56 1.91 -12 -2 19 -0.27 1.15 12 2 -19 -1.27 1.45 -11 -2 19 17.21 1.35 11 -2 -19 18.53 1.96 11 2 -19 17.95 1.65 -10 -2 19 3.36 1.05 10 -2 -19 3.38 1.78 10 2 -19 3.07 1.33 -9 -2 19 14.75 1.20 -9 2 19 17.30 1.30 -8 -2 19 5.89 1.02 8 2 -19 2.68 1.18 -8 2 19 5.42 1.01 -7 2 19 8.28 1.06 7 2 -19 10.26 1.35 6 2 -19 13.08 1.40 5 2 -19 6.70 1.27 4 2 -19 12.10 1.33 3 2 -19 0.45 1.16 -12 -3 19 -0.35 1.17 -11 -3 19 0.05 1.12 11 -3 -19 1.19 1.87 11 3 -19 -1.59 1.37 10 -3 -19 1.90 1.84 -10 -3 19 -0.47 1.02 10 3 -19 -0.02 1.41 -9 -3 19 -0.50 0.97 8 3 -19 -2.39 1.26 7 3 -19 -0.02 1.24 6 3 -19 0.77 1.20 5 3 -19 -0.33 1.22 4 3 -19 0.53 1.18 10 4 -19 4.37 1.54 11 0 -20 22.34 2.08 8 3 -20 13.40 1.62 0 0 0 0.00 0.00 ; _shelx_res_checksum 10650 _shelx_res_file ; TITL p21c in P2(1)/c CELL 0.71073 12.2934 8.9556 13.0199 90 115.75 90 ZERR 4 0.0021 0.0016 0.0023 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Os UNIT 64 80 4 L.S. 8 PLAN 20 SIZE 0.14 0.25 0.35 TEMP -40 BOND $H rem WGHT 0.025400 rem WGHT 0.022700 rem WGHT 0.022500 rem AFIX 13 rem AFIX 0 rem AFIX 23 rem AFIX 43 fmap 2 acta MERG 2 OMIT 0 0 2 OMIT -1 1 1 REM D:/coperet/cop20m5/work/deposition/cop20m5.hkl WGHT 0.018800 FVAR 0.10190 OS1 3 0.267572 0.083915 0.249165 11.00000 0.02209 0.02232 = 0.02329 -0.00155 0.00998 -0.00087 C1 1 0.242971 -0.143220 0.179225 11.00000 0.04207 0.02709 = 0.03396 -0.00907 0.01820 -0.00341 H1 2 0.305379 -0.155758 0.147785 11.00000 -1.20000 C2 1 0.299828 -0.151292 0.300725 11.00000 0.03096 0.02332 = 0.04014 -0.00365 0.01480 0.00146 H2 2 0.384975 -0.174192 0.327442 11.00000 -1.20000 C3 1 0.236547 -0.205598 0.371671 11.00000 0.04251 0.02748 = 0.04002 0.00655 0.01709 0.00161 H3A 2 0.294066 -0.262132 0.440987 11.00000 -1.20000 H3B 2 0.172268 -0.279069 0.327329 11.00000 -1.20000 C4 1 0.185686 -0.075820 0.413817 11.00000 0.04581 0.03454 = 0.03557 0.00276 0.02333 -0.00224 H4A 2 0.115613 -0.108323 0.419631 11.00000 -1.20000 H4B 2 0.249121 -0.044170 0.492847 11.00000 -1.20000 C5 1 0.155356 0.057834 0.334875 11.00000 0.02798 0.02842 = 0.03101 -0.00057 0.01610 0.00026 H5 2 0.143540 0.145355 0.372105 11.00000 -1.20000 C6 1 0.083171 0.046493 0.213053 11.00000 0.02282 0.02964 = 0.03165 -0.00084 0.00976 -0.00196 H6 2 0.030780 0.133931 0.172705 11.00000 -1.20000 C7 1 0.028776 -0.099973 0.154091 11.00000 0.02939 0.03630 = 0.03806 -0.00191 0.00697 -0.00870 AFIX 23 H7A 2 -0.049982 -0.080247 0.090236 11.00000 -1.20000 H7B 2 0.015782 -0.165585 0.207977 11.00000 -1.20000 AFIX 0 C8 1 0.109688 -0.179221 0.109628 11.00000 0.04763 0.03621 = 0.03414 -0.00906 0.01228 -0.00987 H8A 2 0.086707 -0.147902 0.034067 11.00000 -1.20000 H8B 2 0.094941 -0.278528 0.104869 11.00000 -1.20000 C9 1 0.336945 0.412217 0.323347 11.00000 0.04494 0.02437 = 0.04799 -0.00781 0.02542 -0.00992 H9 2 0.335581 0.516508 0.316760 11.00000 -1.20000 C10 1 0.428641 0.338476 0.399836 11.00000 0.04124 0.03325 = 0.03804 -0.00704 0.01505 -0.01112 H10 2 0.498086 0.396911 0.456911 11.00000 -1.20000 C11 1 0.430595 0.173145 0.393261 11.00000 0.02933 0.03228 = 0.03275 0.00128 0.00501 -0.00507 H11 2 0.460202 0.128331 0.459720 11.00000 -1.20000 C12 1 0.466015 0.106576 0.312708 11.00000 0.02230 0.03180 = 0.06020 -0.00204 0.01513 -0.00088 H12 2 0.524720 0.028792 0.338952 11.00000 -1.20000 C13 1 0.414608 0.132838 0.193314 11.00000 0.04006 0.04393 = 0.05692 -0.00945 0.03486 -0.00865 H13 2 0.450074 0.076806 0.156926 11.00000 -1.20000 C14 1 0.307766 0.202582 0.113888 11.00000 0.04744 0.04572 = 0.03516 -0.00006 0.02507 -0.00926 H14 2 0.286211 0.175345 0.036358 11.00000 -1.20000 C15 1 0.218404 0.279755 0.131889 11.00000 0.03372 0.03532 = 0.03574 0.01031 0.01276 -0.00187 H15 2 0.146229 0.286307 0.064505 11.00000 -1.20000 C16 1 0.231582 0.325260 0.241683 11.00000 0.03188 0.02700 = 0.04031 0.00705 0.01743 0.00341 H16 2 0.153023 0.346457 0.241640 11.00000 -1.20000 HKLF 4 REM p21c in P2(1)/c REM R1 = 0.0195 for 3771 Fo > 4sig(Fo) and 0.0354 for all 4897 data REM 208 parameters refined using 0 restraints END WGHT 0.0188 0.0000 REM Highest difference peak 1.030, deepest hole -1.376, 1-sigma level 0.170 Q1 1 0.3177 0.0355 0.2578 11.00000 0.05 1.03 Q2 1 0.4237 -0.0779 0.2212 11.00000 0.05 0.58 Q3 1 0.5650 -0.1025 0.3225 11.00000 0.05 0.58 Q4 1 0.0109 -0.0849 0.1003 11.00000 0.05 0.57 Q5 1 0.5111 0.1197 0.3001 11.00000 0.05 0.56 Q6 1 0.5029 -0.0966 0.2474 11.00000 0.05 0.55 Q7 1 0.4572 0.1739 0.2520 11.00000 0.05 0.55 Q8 1 0.0754 0.0806 0.2831 11.00000 0.05 0.54 Q9 1 0.4434 0.1120 0.5114 11.00000 0.05 0.53 Q10 1 0.0478 -0.0196 0.1938 11.00000 0.05 0.53 Q11 1 0.4842 0.0990 0.4136 11.00000 0.05 0.53 Q12 1 -0.0718 0.0617 0.1931 11.00000 0.05 0.52 Q13 1 -0.0667 -0.0225 0.0374 11.00000 0.05 0.51 Q14 1 0.0349 0.0113 0.0190 11.00000 0.05 0.51 Q15 1 0.0515 -0.1050 0.0476 11.00000 0.05 0.51 Q16 1 0.5266 0.2135 0.2733 11.00000 0.05 0.51 Q17 1 0.1214 -0.0021 0.3269 11.00000 0.05 0.49 Q18 1 0.5315 -0.1680 0.3173 11.00000 0.05 0.49 Q19 1 0.4679 -0.0056 0.1431 11.00000 0.05 0.49 Q20 1 0.5683 0.0855 0.5478 11.00000 0.05 0.48 ; _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2012-9