# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Seisenbaeva, Gulaim' 'Mallah, Talal' 'Kessler, Vadim' _publ_contact_author_name 'Kessler, Vadim' _publ_contact_author_email vadim.kessler@kemi.slu.se _publ_section_title ; Highly symmetric organic ligand capped heteroelement Lindqvist structures derived from 3d-elements ; # Attachment '- Comp1.CIF' data_nitiet1m _database_code_depnum_ccdc_archive 'CCDC 679201' #TrackingRef '- Comp1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Ni2 O16 Ti2' _chemical_formula_weight 970.12 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.995(8) _cell_length_b 14.664(10) _cell_length_c 14.907(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.246(12) _cell_angle_gamma 90.00 _cell_volume 2444(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 618 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 21.00 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.132 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.8485 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; 'the data for refinement cut-off at 1 \%A resolution, 2 theta = 42.00 deg, because of poor reflectivity'? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5787 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0835 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 22.00 _reflns_number_total 2769 _reflns_number_gt 1479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL 6.31' _computing_publication_material 'Bruker SHELXTL 6.31' _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^)+(0.0847P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 2769 _refine_ls_number_parameters 263 _refine_ls_number_restraints 242 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1478 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.41707(9) 0.58370(7) 0.00939(7) 0.0586(4) Uani 1 1 d U . . Ti2 Ti 0.50844(14) 0.43383(9) 0.17050(11) 0.0638(5) Uani 1 1 d U . . O1 O 0.4232(4) 0.4385(3) 0.0234(3) 0.0520(13) Uani 1 1 d U . . O2 O 0.3548(4) 0.5860(3) -0.1394(3) 0.0619(14) Uani 1 1 d U . . O3 O 0.4359(5) 0.7197(3) 0.0154(4) 0.0728(16) Uani 1 1 d U . . O4 O 0.5012(5) 0.5620(3) 0.1546(4) 0.0668(15) Uani 1 1 d U . . O5 O 0.3482(5) 0.4342(4) 0.1883(4) 0.0767(16) Uani 1 1 d U . . O6 O 0.4832(5) 0.2961(3) 0.1690(4) 0.0751(16) Uani 1 1 d U . . O7 O 0.2567(5) 0.5947(4) 0.0196(4) 0.0751(16) Uani 1 1 d U . . O8 O 0.5864(6) 0.4314(4) 0.2994(4) 0.0874(18) Uani 1 1 d U . . C10 C 0.2191(12) 0.3805(11) -0.0317(11) 0.215(8) Uani 1 1 d U . . H10A H 0.1673 0.3417 -0.0811 0.322 Uiso 1 1 calc R . . H10B H 0.1851 0.4405 -0.0381 0.322 Uiso 1 1 calc R . . H10C H 0.2282 0.3562 0.0304 0.322 Uiso 1 1 calc R . . C11 C 0.3573(10) 0.7768(6) 0.0162(6) 0.080(3) Uani 1 1 d U . . C12 C 0.4660(16) 0.6548(9) 0.2673(10) 0.204(8) Uani 1 1 d U . . H12A H 0.4992 0.7001 0.3162 0.306 Uiso 1 1 calc R . . H12B H 0.4455 0.6015 0.2954 0.306 Uiso 1 1 calc R . . H12C H 0.3956 0.6787 0.2184 0.306 Uiso 1 1 calc R . . C13 C 0.2488(9) 0.7548(7) 0.0231(7) 0.089(3) Uani 1 1 d U . . H13A H 0.2007 0.8032 0.0271 0.107 Uiso 1 1 calc R . . C14 C 0.2040(9) 0.6673(8) 0.0248(6) 0.081(3) Uani 1 1 d U . . C15 C 0.3199(9) 0.2809(7) 0.2149(7) 0.098(3) Uani 1 1 d U . . H15A H 0.2731 0.2398 0.2331 0.118 Uiso 1 1 calc R . . C16 C 0.2495(9) 0.6377(6) -0.1959(6) 0.088(3) Uani 1 1 d U . . H16A H 0.2653 0.6713 -0.2461 0.105 Uiso 1 1 calc R . . H16B H 0.2294 0.6811 -0.1550 0.105 Uiso 1 1 calc R . . C17 C 0.4132(10) 0.2458(6) 0.1919(7) 0.084(3) Uani 1 1 d U . . C18 C 0.2907(9) 0.3725(7) 0.2129(7) 0.085(3) Uani 1 1 d U . . C21 C 0.1468(10) 0.5732(9) -0.2402(8) 0.161(5) Uani 1 1 d U . . H21A H 0.0771 0.6070 -0.2781 0.242 Uiso 1 1 calc R . . H21B H 0.1306 0.5409 -0.1903 0.242 Uiso 1 1 calc R . . H21C H 0.1671 0.5304 -0.2806 0.242 Uiso 1 1 calc R . . C22 C 0.0816(9) 0.6575(8) 0.0303(8) 0.132(4) Uani 1 1 d U . . H22A H 0.0625 0.5940 0.0308 0.198 Uiso 1 1 calc R . . H22B H 0.0234 0.6864 -0.0246 0.198 Uiso 1 1 calc R . . H22C H 0.0809 0.6859 0.0881 0.198 Uiso 1 1 calc R . . C23 C 0.3218(10) 0.3849(7) -0.0399(8) 0.112(4) Uani 1 1 d U . . H23A H 0.3072 0.4058 -0.1049 0.135 Uiso 1 1 calc R . . H23B H 0.3501 0.3225 -0.0366 0.135 Uiso 1 1 calc R . . C24 C 0.3905(10) 0.8758(6) 0.0068(7) 0.122(4) Uani 1 1 d U . . H24A H 0.4679 0.8781 0.0015 0.183 Uiso 1 1 calc R . . H24B H 0.3924 0.9094 0.0626 0.183 Uiso 1 1 calc R . . H24C H 0.3322 0.9023 -0.0497 0.183 Uiso 1 1 calc R . . C26 C 0.4357(11) 0.1466(6) 0.1926(8) 0.124(4) Uani 1 1 d U . . H26A H 0.5044 0.1357 0.1755 0.186 Uiso 1 1 calc R . . H26B H 0.3672 0.1170 0.1470 0.186 Uiso 1 1 calc R . . H26C H 0.4500 0.1227 0.2558 0.186 Uiso 1 1 calc R . . C27 C 0.570(2) 0.4243(13) 0.4385(13) 0.223(8) Uani 1 1 d DU . . C29 C 0.690(3) 0.385(2) 0.450(2) 0.164(9) Uani 0.40(2) 1 d PDU . . C29A C 0.622(3) 0.3811(16) 0.3830(15) 0.161(8) Uani 0.60(2) 1 d PDU . . C31 C 0.5463(13) 0.6328(7) 0.2282(8) 0.136(5) Uani 1 1 d U . . H31A H 0.6187 0.6112 0.2782 0.164 Uiso 1 1 calc R . . H31B H 0.5665 0.6867 0.1995 0.164 Uiso 1 1 calc R . . C33 C 0.1841(9) 0.4029(8) 0.2341(7) 0.124(4) Uani 1 1 d U . . H33A H 0.1781 0.4682 0.2300 0.185 Uiso 1 1 calc R . . H33B H 0.1924 0.3838 0.2978 0.185 Uiso 1 1 calc R . . H33C H 0.1132 0.3763 0.1883 0.185 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 Ni1 0.0638(8) 0.0574(6) 0.0554(8) 0.0014(5) 0.0226(6) 0.0095(6) Ti2 0.0735(12) 0.0617(10) 0.0594(11) 0.0058(7) 0.0276(9) 0.0052(8) O1 0.052(3) 0.054(3) 0.051(3) 0.001(2) 0.020(3) 0.000(2) O2 0.061(3) 0.068(3) 0.054(3) 0.009(2) 0.017(3) 0.011(3) O3 0.080(4) 0.059(3) 0.074(4) 0.000(3) 0.022(3) 0.017(3) O4 0.086(4) 0.059(3) 0.055(3) -0.005(2) 0.026(3) 0.004(3) O5 0.086(4) 0.082(4) 0.076(4) 0.008(3) 0.047(3) 0.000(3) O6 0.089(5) 0.064(3) 0.078(4) 0.012(3) 0.037(3) 0.004(3) O7 0.073(4) 0.081(4) 0.075(4) 0.001(3) 0.032(3) 0.014(3) O8 0.107(5) 0.081(4) 0.068(4) 0.009(3) 0.023(3) 0.011(3) C10 0.105(10) 0.30(2) 0.232(17) 0.010(14) 0.050(11) -0.077(12) C11 0.099(7) 0.072(5) 0.063(6) 0.000(5) 0.022(6) 0.026(5) C12 0.32(2) 0.167(13) 0.141(13) -0.003(9) 0.106(13) 0.102(14) C13 0.092(7) 0.091(5) 0.083(7) -0.013(6) 0.029(6) 0.040(5) C14 0.076(6) 0.107(6) 0.060(6) 0.001(6) 0.024(5) 0.022(5) C15 0.099(8) 0.095(6) 0.109(8) 0.027(6) 0.048(6) -0.013(5) C16 0.091(7) 0.111(8) 0.055(6) 0.005(5) 0.019(5) 0.031(5) C17 0.099(8) 0.071(5) 0.085(8) 0.010(5) 0.036(6) -0.010(5) C18 0.092(7) 0.097(6) 0.077(7) 0.019(6) 0.043(6) 0.003(5) C21 0.079(8) 0.218(15) 0.144(12) -0.014(10) -0.012(8) -0.002(8) C22 0.083(8) 0.183(11) 0.137(10) -0.017(8) 0.049(8) 0.019(7) C23 0.092(8) 0.111(7) 0.119(8) -0.002(6) 0.021(6) -0.045(6) C24 0.164(11) 0.063(5) 0.127(9) -0.010(6) 0.038(8) 0.026(6) C26 0.166(11) 0.066(5) 0.141(10) 0.017(6) 0.056(8) -0.009(6) C27 0.31(2) 0.259(19) 0.131(11) 0.017(12) 0.118(12) 0.016(15) C29 0.26(2) 0.17(2) 0.041(10) -0.005(13) 0.027(14) -0.011(18) C29A 0.28(2) 0.183(17) 0.018(8) 0.007(9) 0.044(10) -0.013(15) C31 0.246(16) 0.078(6) 0.083(7) -0.004(5) 0.057(8) 0.036(8) C33 0.111(9) 0.164(10) 0.126(10) 0.016(8) 0.077(8) -0.001(7) _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 Ni1 O7 1.991(6) . ? Ni1 O3 2.006(5) . ? Ni1 O4 2.055(5) . ? Ni1 O2 2.068(5) . ? Ni1 O1 2.138(5) . ? Ni1 O1 2.167(5) 3_665 ? Ni1 Ti2 3.129(2) 3_665 ? Ni1 Ti2 3.145(2) . ? Ti2 O8 1.807(6) . ? Ti2 O4 1.892(5) . ? Ti2 O2 1.882(5) 3_665 ? Ti2 O6 2.041(6) . ? Ti2 O5 2.034(6) . ? Ti2 O1 2.058(5) . ? Ti2 Ni1 3.129(2) 3_665 ? O1 C23 1.468(10) . ? O1 Ni1 2.167(5) 3_665 ? O2 C16 1.453(9) . ? O2 Ti2 1.882(5) 3_665 ? O3 C11 1.263(9) . ? O4 C31 1.465(11) . ? O5 C18 1.269(10) . ? O6 C17 1.254(10) . ? O7 C14 1.255(10) . ? O8 C29A 1.38(2) . ? O8 C29 2.25(3) . ? C10 C23 1.283(15) . ? C11 C13 1.381(12) . ? C11 C24 1.525(12) . ? C12 C31 1.333(17) . ? C13 C14 1.395(13) . ? C14 C22 1.507(13) . ? C15 C18 1.386(12) . ? C15 C17 1.383(12) . ? C16 C21 1.503(13) . ? C17 C26 1.478(12) . ? C18 C33 1.493(13) . ? C27 C29A 1.365(17) . ? C27 C29 1.506(19) . ? C29 C29A 1.04(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 O7 Ni1 O3 90.7(2) . . ? O7 Ni1 O4 92.9(2) . . ? O3 Ni1 O4 95.9(2) . . ? O7 Ni1 O2 95.6(2) . . ? O3 Ni1 O2 91.3(2) . . ? O4 Ni1 O2 168.76(19) . . ? O7 Ni1 O1 94.2(2) . . ? O3 Ni1 O1 170.63(19) . . ? O4 Ni1 O1 75.89(18) . . ? O2 Ni1 O1 96.16(19) . . ? O7 Ni1 O1 171.0(2) . 3_665 ? O3 Ni1 O1 93.8(2) . 3_665 ? O4 Ni1 O1 94.4(2) . 3_665 ? O2 Ni1 O1 76.47(19) . 3_665 ? O1 Ni1 O1 82.55(18) . 3_665 ? O7 Ni1 Ti2 131.03(16) . 3_665 ? O3 Ni1 Ti2 93.32(16) . 3_665 ? O4 Ni1 Ti2 134.91(16) . 3_665 ? O2 Ni1 Ti2 35.59(14) . 3_665 ? O1 Ni1 Ti2 89.52(13) . 3_665 ? O1 Ni1 Ti2 40.88(13) 3_665 3_665 ? O7 Ni1 Ti2 94.41(17) . . ? O3 Ni1 Ti2 131.17(16) . . ? O4 Ni1 Ti2 35.41(14) . . ? O2 Ni1 Ti2 136.12(15) . . ? O1 Ni1 Ti2 40.49(13) . . ? O1 Ni1 Ti2 88.57(12) 3_665 . ? Ti2 Ni1 Ti2 117.92(5) 3_665 . ? O8 Ti2 O4 97.8(2) . . ? O8 Ti2 O2 95.6(3) . 3_665 ? O4 Ti2 O2 97.3(2) . 3_665 ? O8 Ti2 O6 90.5(2) . . ? O4 Ti2 O6 168.9(2) . . ? O2 Ti2 O6 89.1(2) 3_665 . ? O8 Ti2 O5 90.6(3) . . ? O4 Ti2 O5 90.7(2) . . ? O2 Ti2 O5 169.2(2) 3_665 . ? O6 Ti2 O5 82.0(2) . . ? O8 Ti2 O1 178.6(3) . . ? O4 Ti2 O1 81.4(2) . . ? O2 Ti2 O1 83.3(2) 3_665 . ? O6 Ti2 O1 90.4(2) . . ? O5 Ti2 O1 90.6(2) . . ? O8 Ti2 Ni1 135.3(2) . 3_665 ? O4 Ti2 Ni1 89.32(16) . 3_665 ? O2 Ti2 Ni1 39.75(15) 3_665 3_665 ? O6 Ti2 Ni1 89.81(16) . 3_665 ? O5 Ti2 Ni1 133.56(17) . 3_665 ? O1 Ti2 Ni1 43.57(13) . 3_665 ? O8 Ti2 Ni1 136.78(18) . . ? O4 Ti2 Ni1 38.99(16) . . ? O2 Ti2 Ni1 90.78(16) 3_665 . ? O6 Ti2 Ni1 132.36(16) . . ? O5 Ti2 Ni1 90.78(16) . . ? O1 Ti2 Ni1 42.41(12) . . ? Ni1 Ti2 Ni1 62.08(5) 3_665 . ? C23 O1 Ti2 130.0(5) . . ? C23 O1 Ni1 118.7(5) . . ? Ti2 O1 Ni1 97.10(18) . . ? C23 O1 Ni1 111.6(5) . 3_665 ? Ti2 O1 Ni1 95.54(19) . 3_665 ? Ni1 O1 Ni1 97.45(18) . 3_665 ? C16 O2 Ti2 126.2(5) . 3_665 ? C16 O2 Ni1 122.1(5) . . ? Ti2 O2 Ni1 104.7(2) 3_665 . ? C11 O3 Ni1 126.0(6) . . ? C31 O4 Ti2 128.5(6) . . ? C31 O4 Ni1 125.9(5) . . ? Ti2 O4 Ni1 105.6(2) . . ? C18 O5 Ti2 132.4(6) . . ? C17 O6 Ti2 133.7(6) . . ? C14 O7 Ni1 126.5(6) . . ? C29A O8 C29 18.5(15) . . ? C29A O8 Ti2 147.7(11) . . ? C29 O8 Ti2 163.0(9) . . ? O3 C11 C13 124.9(9) . . ? O3 C11 C24 114.2(10) . . ? C13 C11 C24 120.9(9) . . ? C11 C13 C14 126.6(9) . . ? O7 C14 C13 125.0(9) . . ? O7 C14 C22 116.4(10) . . ? C13 C14 C22 118.6(9) . . ? C18 C15 C17 125.2(9) . . ? O2 C16 C21 109.2(8) . . ? O6 C17 C15 121.9(9) . . ? O6 C17 C26 116.3(10) . . ? C15 C17 C26 121.8(10) . . ? O5 C18 C15 122.5(10) . . ? O5 C18 C33 116.4(9) . . ? C15 C18 C33 121.0(9) . . ? C10 C23 O1 124.4(12) . . ? C29A C27 C29 42.1(12) . . ? C29A C29 C27 61.7(15) . . ? C29A C29 O8 25(2) . . ? C27 C29 O8 66.7(14) . . ? C29 C29A C27 76.3(14) . . ? C29 C29A O8 137(3) . . ? C27 C29A O8 104(2) . . ? C12 C31 O4 111.7(14) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 0.485 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.069 # Attachment '- Comp2.CIF' data_cotiet3m _database_code_depnum_ccdc_archive 'CCDC 771907' #TrackingRef '- Comp2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H68 Co2 O16 Ti2' _chemical_formula_weight 970.56 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.158(13) _cell_length_b 14.852(18) _cell_length_c 15.153(15) _cell_angle_alpha 90.00 _cell_angle_beta 111.74(3) _cell_angle_gamma 90.00 _cell_volume 2542(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 978 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 21.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 1.001 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6672 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; 'the data for refinement cut-off at 1 \%A resolution, 2 theta = 42.00 deg, because of poor reflectivity' ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8477 _diffrn_reflns_av_R_equivalents 0.1049 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 21.00 _reflns_number_total 2715 _reflns_number_gt 1276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL 6.31' _computing_publication_material 'Bruker SHELXTL 6.31' _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^)+(0.1348P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 2715 _refine_ls_number_parameters 263 _refine_ls_number_restraints 206 _refine_ls_R_factor_all 0.1620 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2281 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.923 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.91637(13) 0.91568(8) 0.01081(9) 0.0756(7) Uani 1 1 d U . . Ti2 Ti 0.98732(17) 0.93366(11) -0.17269(12) 0.0747(7) Uani 1 1 d U . . O1 O 0.9264(5) 1.0622(4) 0.0262(4) 0.0658(17) Uani 1 1 d U . . O2 O 0.8522(5) 0.9126(4) -0.1382(4) 0.0739(16) Uani 1 1 d U . . O3 O 0.9090(6) 0.9310(4) -0.3000(4) 0.092(2) Uani 1 1 d U . . O4 O 0.9341(6) 0.7781(4) 0.0187(4) 0.092(2) Uani 1 1 d U . . O5 O 1.0060(6) 0.9378(4) 0.1572(4) 0.0789(19) Uani 1 1 d U . . O6 O 1.0152(6) 0.7960(4) -0.1698(4) 0.086(2) Uani 1 1 d U . . O7 O 1.1483(6) 0.9341(4) -0.1914(5) 0.088(2) Uani 1 1 d U . . O8 O 0.7519(6) 0.9018(5) 0.0214(5) 0.095(2) Uani 1 1 d U . . C1 C 1.0873(12) 0.7460(7) -0.1931(7) 0.091(3) Uani 1 1 d U . . C2 C 0.7444(12) 0.7408(9) 0.0229(8) 0.111(4) Uani 1 1 d U . . H2A H 0.6961 0.6927 0.0242 0.133 Uiso 1 1 calc R . . C3 C 1.1778(11) 0.7810(9) -0.2152(8) 0.108(3) Uani 1 1 d U . . H3A H 1.2235 0.7403 -0.2335 0.129 Uiso 1 1 calc R . . C4 C 0.8537(13) 0.7206(8) 0.0185(8) 0.105(4) Uani 1 1 d U . . C5 C 1.0636(12) 0.6477(7) -0.1945(9) 0.135(5) Uani 1 1 d U . . H5A H 1.1230 0.6156 -0.2093 0.202 Uiso 1 1 calc R . . H5B H 0.9870 0.6350 -0.2417 0.202 Uiso 1 1 calc R . . H5C H 1.0655 0.6292 -0.1333 0.202 Uiso 1 1 calc R . . C6 C 0.7465(10) 0.8589(8) -0.1944(8) 0.108(4) Uani 1 1 d U . . H6A H 0.7281 0.8163 -0.1533 0.129 Uiso 1 1 calc R . . H6B H 0.7624 0.8254 -0.2433 0.129 Uiso 1 1 calc R . . C7 C 0.7004(11) 0.8283(10) 0.0257(7) 0.102(3) Uani 1 1 d U . . C8 C 0.5751(10) 0.8395(10) 0.0330(9) 0.161(5) Uani 1 1 d U . . H8A H 0.5554 0.9023 0.0306 0.241 Uiso 1 1 calc R . . H8B H 0.5769 0.8143 0.0918 0.241 Uiso 1 1 calc R . . H8C H 0.5166 0.8087 -0.0191 0.241 Uiso 1 1 calc R . . C9 C 0.8870(12) 0.6219(7) 0.0106(9) 0.144(5) Uani 1 1 d U . . H9A H 0.9654 0.6192 0.0094 0.216 Uiso 1 1 calc R . . H9B H 0.8317 0.5962 -0.0468 0.216 Uiso 1 1 calc R . . H9C H 0.8848 0.5886 0.0643 0.216 Uiso 1 1 calc R . . C17 C 0.8270(12) 1.1178(9) -0.0310(10) 0.134(5) Uani 1 1 d DU . . H17A H 0.8528 1.1794 -0.0143 0.161 Uiso 1 1 calc R . . H17B H 0.8218 1.1097 -0.0960 0.161 Uiso 1 1 calc R . . C16 C 0.6436(11) 0.9207(9) -0.2392(10) 0.170(6) Uani 1 1 d U . . H16A H 0.5765 0.8866 -0.2789 0.254 Uiso 1 1 calc R . . H16B H 0.6638 0.9649 -0.2769 0.254 Uiso 1 1 calc R . . H16C H 0.6244 0.9504 -0.1904 0.254 Uiso 1 1 calc R . . C15 C 1.0511(13) 0.8674(8) 0.2321(8) 0.129(5) Uani 1 1 d U . . H15A H 1.0723 0.8139 0.2053 0.155 Uiso 1 1 calc R . . H15B H 1.1217 0.8892 0.2827 0.155 Uiso 1 1 calc R . . C14 C 1.3150(11) 0.9029(9) -0.2331(8) 0.136(5) Uani 1 1 d U . . H14A H 1.3237 0.9669 -0.2243 0.203 Uiso 1 1 calc R . . H14B H 1.3046 0.8882 -0.2974 0.203 Uiso 1 1 calc R . . H14C H 1.3847 0.8735 -0.1904 0.203 Uiso 1 1 calc R . . C13 C 0.9610(16) 0.8450(11) 0.2706(9) 0.197(8) Uani 1 1 d U . . H13A H 0.9919 0.8009 0.3200 0.295 Uiso 1 1 calc R . . H13B H 0.8926 0.8211 0.2209 0.295 Uiso 1 1 calc R . . H13C H 0.9394 0.8983 0.2962 0.295 Uiso 1 1 calc R . . C12 C 0.891(2) 0.8907(13) -0.3889(11) 0.205(8) Uani 1 1 d U . . C11 C 1.2087(11) 0.8719(9) -0.2132(8) 0.096(3) Uani 1 1 d U . . C10 C 0.7137(14) 1.1154(13) -0.0357(15) 0.258(11) Uani 1 1 d DU . . H10A H 0.6665 1.1562 -0.0840 0.386 Uiso 1 1 calc R . . H10B H 0.7113 1.1329 0.0245 0.386 Uiso 1 1 calc R . . H10C H 0.6831 1.0555 -0.0509 0.386 Uiso 1 1 calc R . . C18A C 0.795(6) 0.877(3) -0.448(2) 0.211(14) Uani 0.40(3) 1 d PU . . C18B C 0.934(4) 0.927(2) -0.4474(16) 0.211(12) Uani 0.60(3) 1 d PU . . 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 Co1 0.0812(12) 0.0719(10) 0.0670(10) -0.0027(7) 0.0198(8) -0.0161(8) Ti2 0.0843(15) 0.0706(13) 0.0643(12) -0.0044(8) 0.0217(11) -0.0042(10) O1 0.069(4) 0.068(4) 0.058(4) 0.004(3) 0.021(4) 0.002(3) O2 0.072(4) 0.078(4) 0.069(4) 0.001(3) 0.023(3) -0.010(3) O3 0.119(5) 0.093(5) 0.060(4) -0.005(3) 0.030(4) -0.010(4) O4 0.103(6) 0.070(4) 0.084(4) -0.001(3) 0.013(4) -0.018(4) O5 0.101(5) 0.068(4) 0.063(4) 0.005(3) 0.024(4) -0.008(4) O6 0.096(6) 0.071(4) 0.087(5) -0.013(3) 0.030(4) -0.005(3) O7 0.092(5) 0.094(5) 0.084(5) -0.005(4) 0.040(4) -0.006(4) O8 0.095(5) 0.106(5) 0.084(5) 0.002(4) 0.033(4) -0.022(4) C1 0.118(10) 0.073(6) 0.080(7) -0.009(6) 0.034(7) 0.008(6) C2 0.107(9) 0.108(7) 0.091(8) 0.011(7) 0.005(8) -0.047(7) C3 0.108(10) 0.104(7) 0.113(9) -0.011(8) 0.043(8) 0.020(7) C4 0.123(10) 0.082(6) 0.090(8) 0.001(6) 0.016(9) -0.030(6) C5 0.164(13) 0.070(6) 0.160(11) -0.028(7) 0.048(10) 0.005(7) C6 0.089(8) 0.123(9) 0.088(7) -0.008(6) 0.006(6) -0.032(6) C7 0.095(8) 0.131(8) 0.075(7) 0.008(8) 0.026(7) -0.030(7) C8 0.089(10) 0.225(15) 0.161(13) 0.031(10) 0.037(10) -0.028(8) C9 0.184(13) 0.077(6) 0.142(11) 0.002(7) 0.027(10) -0.032(7) C17 0.092(9) 0.127(8) 0.146(11) -0.008(8) 0.001(9) 0.029(8) C16 0.095(9) 0.186(15) 0.169(14) 0.014(10) -0.021(9) -0.005(9) C15 0.209(15) 0.082(8) 0.085(7) -0.008(5) 0.041(8) -0.030(9) C14 0.119(11) 0.178(12) 0.130(11) -0.022(9) 0.070(9) -0.016(8) C13 0.29(2) 0.193(16) 0.116(11) 0.003(9) 0.079(12) -0.124(15) C12 0.29(2) 0.245(16) 0.061(8) -0.035(10) 0.049(11) 0.001(15) C11 0.088(8) 0.116(8) 0.084(8) -0.008(7) 0.033(7) 0.000(6) C10 0.097(10) 0.28(2) 0.35(3) 0.014(18) 0.028(16) 0.044(14) C18A 0.33(3) 0.20(3) 0.040(18) -0.011(18) -0.002(17) 0.01(3) C18B 0.32(3) 0.26(3) 0.057(14) 0.016(15) 0.076(16) 0.09(2) _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 Co1 O4 2.053(7) . ? Co1 O8 2.075(8) . ? Co1 O2 2.099(6) . ? Co1 O5 2.103(6) . ? Co1 O1 2.188(6) . ? Co1 O1 2.207(6) 3_775 ? Ti2 O3 1.809(6) . ? Ti2 O5 1.921(6) 3_775 ? Ti2 O2 1.925(7) . ? Ti2 O1 2.075(6) 3_775 ? Ti2 O6 2.071(7) . ? Ti2 O7 2.080(8) . ? O1 C17 1.455(13) . ? O1 Ti2 2.075(6) 3_775 ? O1 Co1 2.207(6) 3_775 ? O2 C6 1.483(11) . ? O3 C12 1.413(15) . ? O4 C4 1.298(13) . ? O5 C15 1.491(12) . ? O5 Ti2 1.921(6) 3_775 ? O6 C1 1.293(12) . ? O7 C11 1.297(12) . ? O8 C7 1.272(12) . ? C1 C3 1.366(15) . ? C1 C5 1.487(14) . ? C2 C4 1.388(16) . ? C2 C7 1.412(16) . ? C3 C11 1.398(15) . ? C4 C9 1.537(16) . ? C6 C16 1.497(15) . ? C7 C8 1.576(16) . ? C17 C10 1.353(14) . ? C15 C13 1.457(18) . ? C14 C11 1.505(15) . ? C12 C18A 1.19(5) . ? C12 C18B 1.30(3) . ? C18A C18B 1.84(6) . ? 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 O4 Co1 O8 88.9(3) . . ? O4 Co1 O2 91.7(2) . . ? O8 Co1 O2 95.5(3) . . ? O4 Co1 O5 95.3(2) . . ? O8 Co1 O5 94.1(3) . . ? O2 Co1 O5 168.2(2) . . ? O4 Co1 O1 169.5(2) . . ? O8 Co1 O1 96.2(3) . . ? O2 Co1 O1 96.9(2) . . ? O5 Co1 O1 75.2(2) . . ? O4 Co1 O1 94.6(3) . 3_775 ? O8 Co1 O1 170.0(2) . 3_775 ? O2 Co1 O1 75.0(2) . 3_775 ? O5 Co1 O1 94.9(2) . 3_775 ? O1 Co1 O1 82.0(2) . 3_775 ? O3 Ti2 O5 97.7(3) . 3_775 ? O3 Ti2 O2 96.9(3) . . ? O5 Ti2 O2 97.4(3) 3_775 . ? O3 Ti2 O1 178.7(3) . 3_775 ? O5 Ti2 O1 81.9(2) 3_775 3_775 ? O2 Ti2 O1 81.9(3) . 3_775 ? O3 Ti2 O6 91.0(3) . . ? O5 Ti2 O6 168.4(3) 3_775 . ? O2 Ti2 O6 89.0(3) . . ? O1 Ti2 O6 89.5(2) 3_775 . ? O3 Ti2 O7 90.3(3) . . ? O5 Ti2 O7 90.8(3) 3_775 . ? O2 Ti2 O7 168.2(3) . . ? O1 Ti2 O7 91.0(3) 3_775 . ? O6 Ti2 O7 81.5(3) . . ? C17 O1 Ti2 126.9(7) . 3_775 ? C17 O1 Co1 119.9(6) . . ? Ti2 O1 Co1 97.4(2) 3_775 . ? C17 O1 Co1 111.7(7) . 3_775 ? Ti2 O1 Co1 97.2(2) 3_775 3_775 ? Co1 O1 Co1 98.0(2) . 3_775 ? C6 O2 Ti2 125.2(6) . . ? C6 O2 Co1 121.8(6) . . ? Ti2 O2 Co1 105.9(3) . . ? C12 O3 Ti2 149.4(10) . . ? C4 O4 Co1 126.3(8) . . ? C15 O5 Ti2 128.1(6) . 3_775 ? C15 O5 Co1 126.5(6) . . ? Ti2 O5 Co1 105.4(3) 3_775 . ? C1 O6 Ti2 133.0(7) . . ? C11 O7 Ti2 133.0(7) . . ? C7 O8 Co1 126.6(8) . . ? O6 C1 C3 122.6(11) . . ? O6 C1 C5 114.8(12) . . ? C3 C1 C5 122.6(12) . . ? C4 C2 C7 125.5(12) . . ? C1 C3 C11 126.6(12) . . ? O4 C4 C2 126.3(12) . . ? O4 C4 C9 114.0(12) . . ? C2 C4 C9 119.7(12) . . ? O2 C6 C16 109.3(9) . . ? O8 C7 C2 126.1(13) . . ? O8 C7 C8 114.9(13) . . ? C2 C7 C8 119.1(12) . . ? C10 C17 O1 128.4(15) . . ? C13 C15 O5 110.2(13) . . ? C18A C12 C18B 95(3) . . ? C18A C12 O3 124(3) . . ? C18B C12 O3 121(2) . . ? O7 C11 C3 121.4(12) . . ? O7 C11 C14 116.2(11) . . ? C3 C11 C14 122.4(12) . . ? C12 C18A C18B 45(2) . . ? C12 C18B C18A 40.2(16) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.446 _refine_diff_density_min -0.336 _refine_diff_density_rms 0.079 # Attachment '- Comp3.cif' data_nitipr10 _database_code_depnum_ccdc_archive 'CCDC 679203' #TrackingRef '- Comp3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Ni5 O19 Ti' _chemical_formula_weight 1222.45 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.26(2) _cell_length_b 20.26(2) _cell_length_c 11.623(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4133(8) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 667 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 20.79 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1914 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6029 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; 'Data cut-off at 1\%A resolution, 2theta=42.0 deg, because of poor reflectivity' ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2284 _diffrn_reflns_av_R_equivalents 0.0870 _diffrn_reflns_av_sigmaI/netI 0.0730 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 3 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 21.00 _reflns_number_total 827 _reflns_number_gt 547 _reflns_threshold_expression >2sigma(I) #_computing_data_collection ? _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0958P)^2^+88.9431P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 827 _refine_ls_number_parameters 140 _refine_ls_number_restraints 238 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2255 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.07933(11) 0.09673(11) 0.1099(2) 0.0671(11) Uani 0.17 1 d PDU . . Ni1 Ni 0.07933(11) 0.09673(11) 0.1099(2) 0.0671(11) Uani 0.83 1 d PU . . O1 O 0.0000 0.0000 0.0000 0.048(3) Uani 1 6 d SU . . O2 O 0.0553(6) 0.1585(5) 0.0006(9) 0.078(3) Uani 1 1 d U . . O3 O 0.0879(5) 0.0164(6) 0.2000(10) 0.081(3) Uani 1 1 d DU . . O4 O 0.1488(7) 0.1814(6) 0.2004(11) 0.106(4) Uani 1 1 d DU . . C1 C 0.1504(12) 0.0061(11) 0.363(2) 0.138(7) Uani 1 1 d DU . . C2 C 0.1080(17) 0.2916(11) 0.017(3) 0.190(10) Uani 1 1 d U . . C3 C 0.187(2) 0.1987(15) 0.283(3) 0.142(10) Uani 0.58(3) 1 d PDU . . C4 C 0.2412(14) 0.2784(14) 0.311(2) 0.169(9) Uani 1 1 d DU . . C5 C 0.129(3) 0.0451(16) 0.291(3) 0.121(7) Uani 0.50 1 d PDU . . C6A C 0.056(4) 0.224(2) 0.034(6) 0.137(10) Uani 0.41(4) 1 d PU . . C6B C 0.100(3) 0.2374(19) -0.040(5) 0.152(10) Uani 0.59(4) 1 d PU . . C7 C 0.2316(13) 0.233(3) 0.198(3) 0.140(12) Uani 0.42(3) 1 d PDU . . C8A C 0.072(5) 0.004(5) 0.335(7) 0.107(8) Uani 0.25 1 d PU . . C9 C 0.175(3) 0.1268(13) 0.356(3) 0.153(11) Uani 0.50 1 d PDU . . C8B C 0.165(4) 0.023(5) 0.245(8) 0.115(7) Uani 0.25 1 d PU . . 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 Ti1 0.0601(14) 0.0530(14) 0.082(2) -0.0139(11) -0.0115(11) 0.0237(10) Ni1 0.0601(14) 0.0530(14) 0.082(2) -0.0139(11) -0.0115(11) 0.0237(10) O1 0.046(5) 0.046(5) 0.052(11) 0.000 0.000 0.023(3) O2 0.086(7) 0.048(4) 0.101(9) -0.009(5) -0.007(5) 0.034(5) O3 0.076(7) 0.098(6) 0.076(8) -0.004(5) -0.023(5) 0.049(6) O4 0.098(8) 0.095(6) 0.108(10) -0.039(6) -0.033(6) 0.035(6) C1 0.127(13) 0.180(14) 0.102(14) 0.007(12) -0.048(11) 0.074(13) C2 0.22(2) 0.047(7) 0.26(3) -0.004(13) 0.02(2) 0.039(13) C3 0.137(19) 0.122(11) 0.116(17) -0.045(11) -0.052(11) 0.026(14) C4 0.155(18) 0.133(12) 0.16(2) -0.069(12) -0.062(14) 0.026(12) C5 0.124(16) 0.136(12) 0.091(16) -0.009(9) -0.048(11) 0.056(11) C6A 0.18(2) 0.040(10) 0.19(3) 0.003(12) 0.005(18) 0.055(11) C6B 0.20(2) 0.051(9) 0.18(2) 0.019(10) 0.016(17) 0.042(13) C7 0.113(12) 0.126(19) 0.11(2) -0.037(12) -0.072(15) 0.008(13) C8A 0.121(14) 0.131(18) 0.065(11) -0.018(13) -0.050(15) 0.060(14) C9 0.15(2) 0.152(12) 0.11(2) -0.025(10) -0.059(17) 0.038(15) C8B 0.090(13) 0.147(19) 0.100(16) 0.002(15) -0.057(14) 0.053(15) _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 Ti1 O4 1.902(11) . ? Ti1 O2 2.007(10) . ? Ti1 O2 2.007(10) 11 ? Ti1 O3 2.014(10) . ? Ti1 O3 2.032(10) 2 ? Ti1 O1 2.215(3) . ? Ti1 Ni1 3.131(5) 12 ? Ti1 Ti1 3.131(5) 12 ? Ti1 Ti1 3.131(5) 11 ? Ti1 Ni1 3.131(5) 11 ? Ti1 Ti1 3.135(5) 3 ? Ti1 Ni1 3.135(5) 3 ? O1 Ni1 2.215(3) 10 ? O1 Ti1 2.215(3) 10 ? O1 Ni1 2.215(3) 11 ? O1 Ti1 2.215(3) 11 ? O1 Ni1 2.215(3) 12 ? O1 Ti1 2.215(3) 12 ? O1 Ni1 2.215(3) 3 ? O1 Ti1 2.215(3) 3 ? O1 Ti1 2.215(3) 2 ? O1 Ni1 2.215(3) 2 ? O2 C6A 1.37(5) . ? O2 C6B 1.47(4) . ? O2 Ni1 2.007(10) 12 ? O2 Ti1 2.007(10) 12 ? O3 C5 1.291(16) . ? O3 C8B 1.58(7) . ? O3 C8A 1.59(9) . ? O3 Ni1 2.032(10) 3 ? O3 Ti1 2.032(10) 3 ? O4 C3 1.170(17) . ? O4 C7 1.467(19) . ? C1 C5 1.36(3) . ? C1 C8B 1.41(9) . ? C1 C8A 1.59(8) . ? C2 C6B 1.23(5) . ? C2 C6A 1.26(6) . ? C3 C7 1.28(5) . ? C3 C4 1.47(3) . ? C3 C9 1.596(19) . ? C4 C7 1.555(19) . ? C5 C8A 1.15(9) . ? C5 C8B 1.16(9) . ? C5 C9 1.623(18) . ? C6A C6B 1.17(6) . ? C8A C8B 2.01(12) . ? 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 O4 Ti1 O2 95.1(5) . . ? O4 Ti1 O2 95.0(5) . 11 ? O2 Ti1 O2 89.40(13) . 11 ? O4 Ti1 O3 96.8(5) . . ? O2 Ti1 O3 168.2(4) . . ? O2 Ti1 O3 89.8(4) 11 . ? O4 Ti1 O3 97.2(5) . 2 ? O2 Ti1 O3 89.1(4) . 2 ? O2 Ti1 O3 167.7(4) 11 2 ? O3 Ti1 O3 89.2(6) . 2 ? O4 Ti1 O1 178.4(4) . . ? O2 Ti1 O1 83.8(3) . . ? O2 Ti1 O1 83.8(3) 11 . ? O3 Ti1 O1 84.4(3) . . ? O3 Ti1 O1 84.0(3) 2 . ? O4 Ti1 Ni1 133.8(4) . 12 ? O2 Ti1 Ni1 38.8(3) . 12 ? O2 Ti1 Ni1 85.4(3) 11 12 ? O3 Ti1 Ni1 129.4(3) . 12 ? O3 Ti1 Ni1 85.8(3) 2 12 ? O1 Ti1 Ni1 45.04(5) . 12 ? O4 Ti1 Ti1 133.8(4) . 12 ? O2 Ti1 Ti1 38.8(3) . 12 ? O2 Ti1 Ti1 85.4(3) 11 12 ? O3 Ti1 Ti1 129.4(3) . 12 ? O3 Ti1 Ti1 85.8(3) 2 12 ? O1 Ti1 Ti1 45.04(5) . 12 ? Ni1 Ti1 Ti1 0.00(8) 12 12 ? O4 Ti1 Ti1 133.8(4) . 11 ? O2 Ti1 Ti1 85.9(3) . 11 ? O2 Ti1 Ti1 38.7(3) 11 11 ? O3 Ti1 Ti1 86.1(3) . 11 ? O3 Ti1 Ti1 129.0(3) 2 11 ? O1 Ti1 Ti1 45.04(5) . 11 ? Ni1 Ti1 Ti1 60.08(12) 12 11 ? Ti1 Ti1 Ti1 60.08(12) 12 11 ? O4 Ti1 Ni1 133.8(4) . 11 ? O2 Ti1 Ni1 85.9(3) . 11 ? O2 Ti1 Ni1 38.7(3) 11 11 ? O3 Ti1 Ni1 86.1(3) . 11 ? O3 Ti1 Ni1 129.0(3) 2 11 ? O1 Ti1 Ni1 45.04(5) . 11 ? Ni1 Ti1 Ni1 60.08(12) 12 11 ? Ti1 Ti1 Ni1 60.08(12) 12 11 ? Ti1 Ti1 Ni1 0.00(8) 11 11 ? O4 Ti1 Ti1 136.2(4) . 3 ? O2 Ti1 Ti1 128.8(3) . 3 ? O2 Ti1 Ti1 85.8(3) 11 3 ? O3 Ti1 Ti1 39.4(3) . 3 ? O3 Ti1 Ti1 85.7(3) 2 3 ? O1 Ti1 Ti1 44.96(5) . 3 ? Ni1 Ti1 Ti1 90.0 12 3 ? Ti1 Ti1 Ti1 90.0 12 3 ? Ti1 Ti1 Ti1 59.96(6) 11 3 ? Ni1 Ti1 Ti1 59.96(6) 11 3 ? O4 Ti1 Ni1 136.2(4) . 3 ? O2 Ti1 Ni1 128.8(3) . 3 ? O2 Ti1 Ni1 85.8(3) 11 3 ? O3 Ti1 Ni1 39.4(3) . 3 ? O3 Ti1 Ni1 85.7(3) 2 3 ? O1 Ti1 Ni1 44.96(5) . 3 ? Ni1 Ti1 Ni1 90.0 12 3 ? Ti1 Ti1 Ni1 90.0 12 3 ? Ti1 Ti1 Ni1 59.96(6) 11 3 ? Ni1 Ti1 Ni1 59.96(6) 11 3 ? Ti1 Ti1 Ni1 0.00(11) 3 3 ? Ni1 O1 Ti1 180.00(13) 10 . ? Ni1 O1 Ti1 0.00(19) 10 10 ? Ti1 O1 Ti1 180.00(19) . 10 ? Ni1 O1 Ni1 90.07(10) 10 11 ? Ti1 O1 Ni1 89.93(10) . 11 ? Ti1 O1 Ni1 90.07(10) 10 11 ? Ni1 O1 Ti1 90.07(10) 10 11 ? Ti1 O1 Ti1 89.93(10) . 11 ? Ti1 O1 Ti1 90.07(10) 10 11 ? Ni1 O1 Ti1 0.00(13) 11 11 ? Ni1 O1 Ni1 90.07(10) 10 12 ? Ti1 O1 Ni1 89.93(10) . 12 ? Ti1 O1 Ni1 90.07(10) 10 12 ? Ni1 O1 Ni1 90.07(10) 11 12 ? Ti1 O1 Ni1 90.07(10) 11 12 ? Ni1 O1 Ti1 90.07(10) 10 12 ? Ti1 O1 Ti1 89.93(10) . 12 ? Ti1 O1 Ti1 90.07(10) 10 12 ? Ni1 O1 Ti1 90.07(10) 11 12 ? Ti1 O1 Ti1 90.07(10) 11 12 ? Ni1 O1 Ti1 0.00(13) 12 12 ? Ni1 O1 Ni1 89.93(10) 10 3 ? Ti1 O1 Ni1 90.07(10) . 3 ? Ti1 O1 Ni1 89.93(10) 10 3 ? Ni1 O1 Ni1 89.93(10) 11 3 ? Ti1 O1 Ni1 89.93(10) 11 3 ? Ni1 O1 Ni1 180.00(8) 12 3 ? Ti1 O1 Ni1 180.00(8) 12 3 ? Ni1 O1 Ti1 89.93(10) 10 3 ? Ti1 O1 Ti1 90.07(10) . 3 ? Ti1 O1 Ti1 89.93(10) 10 3 ? Ni1 O1 Ti1 89.93(10) 11 3 ? Ti1 O1 Ti1 89.93(10) 11 3 ? Ni1 O1 Ti1 180.00(8) 12 3 ? Ti1 O1 Ti1 180.00(8) 12 3 ? Ni1 O1 Ti1 0.00(13) 3 3 ? Ni1 O1 Ti1 89.93(10) 10 2 ? Ti1 O1 Ti1 90.07(10) . 2 ? Ti1 O1 Ti1 89.93(10) 10 2 ? Ni1 O1 Ti1 180.00(13) 11 2 ? Ti1 O1 Ti1 180.00(13) 11 2 ? Ni1 O1 Ti1 89.93(10) 12 2 ? Ti1 O1 Ti1 89.93(10) 12 2 ? Ni1 O1 Ti1 90.07(10) 3 2 ? Ti1 O1 Ti1 90.07(10) 3 2 ? Ni1 O1 Ni1 89.93(10) 10 2 ? Ti1 O1 Ni1 90.07(10) . 2 ? Ti1 O1 Ni1 89.93(10) 10 2 ? Ni1 O1 Ni1 180.00(13) 11 2 ? Ti1 O1 Ni1 180.00(13) 11 2 ? Ni1 O1 Ni1 89.93(10) 12 2 ? Ti1 O1 Ni1 89.93(10) 12 2 ? Ni1 O1 Ni1 90.07(10) 3 2 ? Ti1 O1 Ni1 90.07(10) 3 2 ? Ti1 O1 Ni1 0.00(13) 2 2 ? C6A O2 C6B 48(3) . . ? C6A O2 Ti1 122(3) . . ? C6B O2 Ti1 132(2) . . ? C6A O2 Ni1 127(3) . 12 ? C6B O2 Ni1 118(2) . 12 ? Ti1 O2 Ni1 102.5(4) . 12 ? C6A O2 Ti1 127(3) . 12 ? C6B O2 Ti1 118(2) . 12 ? Ti1 O2 Ti1 102.5(4) . 12 ? Ni1 O2 Ti1 0.0(2) 12 12 ? C5 O3 C8B 46(4) . . ? C5 O3 C8A 45(3) . . ? C8B O3 C8A 78(4) . . ? C5 O3 Ti1 111.1(13) . . ? C8B O3 Ti1 126(3) . . ? C8A O3 Ti1 123(3) . . ? C5 O3 Ni1 147.0(14) . 3 ? C8B O3 Ni1 116(4) . 3 ? C8A O3 Ni1 111(3) . 3 ? Ti1 O3 Ni1 101.6(5) . 3 ? C5 O3 Ti1 147.0(14) . 3 ? C8B O3 Ti1 116(4) . 3 ? C8A O3 Ti1 111(3) . 3 ? Ti1 O3 Ti1 101.6(5) . 3 ? Ni1 O3 Ti1 0.0(2) 3 3 ? C3 O4 C7 57(2) . . ? C3 O4 Ti1 143.4(15) . . ? C7 O4 Ti1 134.5(14) . . ? C5 C1 C8B 50(4) . . ? C5 C1 C8A 45(3) . . ? C8B C1 C8A 84(4) . . ? C6B C2 C6A 56(3) . . ? O4 C3 C7 73(2) . . ? O4 C3 C4 122(2) . . ? C7 C3 C4 68.5(18) . . ? O4 C3 C9 112.8(19) . . ? C7 C3 C9 130(5) . . ? C4 C3 C9 125(2) . . ? C3 C4 C7 50(2) . . ? C8A C5 C8B 121(7) . . ? C8A C5 O3 81(4) . . ? C8B C5 O3 80(4) . . ? C8A C5 C1 78(4) . . ? C8B C5 C1 67(4) . . ? O3 C5 C1 124(2) . . ? C8A C5 C9 113(6) . . ? C8B C5 C9 117(6) . . ? O3 C5 C9 139(2) . . ? C1 C5 C9 96.9(13) . . ? C6B C6A C2 61(4) . . ? C6B C6A O2 70(4) . . ? C2 C6A O2 128(7) . . ? C6A C6B C2 63(4) . . ? C6A C6B O2 62(3) . . ? C2 C6B O2 122(5) . . ? C3 C7 O4 49.8(12) . . ? C3 C7 C4 61.3(18) . . ? O4 C7 C4 99.7(17) . . ? C5 C8A C1 57(4) . . ? C5 C8A O3 53(4) . . ? C1 C8A O3 95(5) . . ? C5 C8A C8B 30(4) . . ? C1 C8A C8B 44(3) . . ? O3 C8A C8B 51(3) . . ? C3 C9 C5 115.6(19) . . ? C5 C8B C1 63(5) . . ? C5 C8B O3 54(3) . . ? C1 C8B O3 103(6) . . ? C5 C8B C8A 29(4) . . ? C1 C8B C8A 52(4) . . ? O3 C8B C8A 51(3) . . ? _diffrn_measured_fraction_theta_max 0.834 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.834 _refine_diff_density_max 0.507 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.100 # Attachment '- Comp4.CIF' data_cotiet7m _database_code_depnum_ccdc_archive 'CCDC 771908' #TrackingRef '- Comp4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Co5 O19 Ti' _chemical_formula_weight 1223.55 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.305(5) _cell_length_b 20.305(5) _cell_length_c 11.585(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4137(2) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 864 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 20.98 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1899 _exptl_absorpt_coefficient_mu 1.672 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4336 _exptl_absorpt_correction_T_max 0.5922 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5970 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1789 _reflns_number_gt 1100 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0996P)^2^+25.3198P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 1789 _refine_ls_number_parameters 142 _refine_ls_number_restraints 201 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2040 _refine_ls_wR_factor_gt 0.1856 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.07977(5) 0.09803(5) 0.11144(8) 0.0598(4) Uani 0.83 1 d PU . . Ti1 Ti 0.07977(5) 0.09803(5) 0.11144(8) 0.0598(4) Uani 0.17 1 d PU . . O1 O 0.0000 0.0000 0.0000 0.0385(16) Uani 1 6 d SU . . O2 O 0.0508(3) 0.1579(3) 0.0035(5) 0.0904(16) Uani 1 1 d U . . O3 O 0.0878(3) 0.0179(3) 0.1993(5) 0.1051(18) Uani 1 1 d U . . O4 O 0.1477(3) 0.1815(4) 0.2055(7) 0.127(2) Uani 1 1 d U . . C1 C 0.2429(7) 0.2806(7) 0.3203(13) 0.182(6) Uani 1 1 d U . . C2 C 0.1955(7) 0.2154(6) 0.2573(11) 0.137(3) Uani 1 1 d U . . C3A C 0.1912(13) 0.1461(15) 0.332(2) 0.134(6) Uani 0.489(17) 1 d PU . . C3B C 0.2571(12) 0.2249(15) 0.156(2) 0.159(9) Uani 0.511(17) 1 d PU . . C4A C 0.0732(10) 0.0057(11) 0.3317(16) 0.107(4) Uani 0.537(13) 1 d PU . . C4B C 0.1681(11) 0.0266(13) 0.2253(17) 0.101(4) Uani 0.463(13) 1 d PU . . C5 C 0.1526(5) 0.0158(6) 0.3685(8) 0.115(3) Uani 1 1 d U . . C6A C 0.0337(8) 0.2132(7) 0.0594(13) 0.088(4) Uani 0.601(13) 1 d PU . . C6B C 0.0723(17) 0.2377(14) -0.052(2) 0.118(6) Uani 0.399(13) 1 d PU . . C7 C 0.1093(7) 0.2932(5) 0.0168(11) 0.135(4) Uani 1 1 d U . . C4C C 0.1461(14) 0.0619(17) 0.303(2) 0.093(4) Uani 0.336(18) 1 d PU . . 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 Co1 0.0501(6) 0.0526(6) 0.0703(7) -0.0132(4) -0.0119(4) 0.0209(4) Ti1 0.0501(6) 0.0526(6) 0.0703(7) -0.0132(4) -0.0119(4) 0.0209(4) O1 0.035(2) 0.035(2) 0.045(4) 0.000 0.000 0.0176(12) O2 0.095(4) 0.050(2) 0.131(4) -0.031(2) -0.030(3) 0.040(2) O3 0.120(4) 0.121(4) 0.087(4) 0.006(3) -0.044(3) 0.070(4) O4 0.089(4) 0.112(4) 0.160(6) -0.055(4) -0.057(4) 0.035(4) C1 0.137(10) 0.136(7) 0.205(13) -0.078(9) -0.067(9) 0.018(8) C2 0.117(7) 0.105(6) 0.149(9) -0.056(6) -0.049(6) 0.026(6) C3A 0.110(13) 0.142(7) 0.141(13) -0.037(7) -0.025(9) 0.056(8) C3B 0.101(9) 0.174(19) 0.139(13) -0.034(10) -0.048(8) 0.021(12) C4A 0.094(7) 0.135(10) 0.090(7) 0.012(7) -0.012(7) 0.054(7) C4B 0.103(8) 0.129(12) 0.088(7) -0.001(8) -0.018(7) 0.071(9) C5 0.095(6) 0.152(7) 0.080(5) 0.018(5) -0.035(4) 0.048(6) C6A 0.116(9) 0.053(6) 0.101(8) -0.008(5) -0.004(7) 0.046(5) C6B 0.155(16) 0.088(8) 0.087(10) 0.019(7) -0.012(9) 0.043(11) C7 0.148(9) 0.044(4) 0.188(11) -0.005(5) 0.005(7) 0.030(5) C4C 0.074(8) 0.130(8) 0.089(10) -0.005(6) -0.019(6) 0.060(6) _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 Co1 O4 1.904(6) . ? Co1 O3 1.994(5) . ? Co1 O2 2.008(5) 11 ? Co1 O2 2.026(5) . ? Co1 O3 2.041(6) 2 ? Co1 O1 2.2424(9) . ? Co1 Ti1 3.1669(17) 11 ? Co1 Ti1 3.1669(17) 12 ? Co1 Ti1 3.1756(17) 2 ? Co1 Ti1 3.1756(17) 3 ? O1 Ti1 2.2424(9) 10 ? O1 Co1 2.2424(9) 10 ? O1 Ti1 2.2424(9) 2 ? O1 Co1 2.2424(9) 2 ? O1 Ti1 2.2424(9) 11 ? O1 Co1 2.2424(9) 11 ? O1 Ti1 2.2424(9) 12 ? O1 Co1 2.2424(9) 3 ? O1 Co1 2.2424(9) 12 ? O1 Ti1 2.2424(9) 3 ? O2 C6A 1.481(13) . ? O2 C6B 1.59(2) . ? O2 Ti1 2.008(5) 12 ? O2 Co1 2.008(5) 12 ? O3 C4A 1.558(19) . ? O3 C4B 1.579(19) . ? O3 C4C 1.61(3) . ? O3 Ti1 2.041(6) 3 ? O3 Co1 2.041(6) 3 ? O4 C2 1.053(10) . ? C1 C2 1.393(13) . ? C2 C3A 1.62(3) . ? C2 C3B 1.65(3) . ? C3A C4C 1.52(3) . ? C3B C6B 1.61(3) 11 ? C4A C4C 1.38(3) . ? C4A C5 1.579(19) . ? C4B C4C 1.36(3) . ? C4B C5 1.68(2) . ? C5 C4C 1.26(3) . ? C6A C6B 1.46(3) . ? C6A C7 1.657(16) . ? C6B C7 1.27(3) . ? C6B C3B 1.61(3) 12 ? 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 O4 Co1 O3 96.6(3) . . ? O4 Co1 O2 96.3(3) . 11 ? O3 Co1 O2 91.7(3) . 11 ? O4 Co1 O2 96.8(3) . . ? O3 Co1 O2 166.4(2) . . ? O2 Co1 O2 89.35(5) 11 . ? O4 Co1 O3 97.7(3) . 2 ? O3 Co1 O3 89.0(4) . 2 ? O2 Co1 O3 165.8(2) 11 2 ? O2 Co1 O3 86.7(3) . 2 ? O4 Co1 O1 179.8(3) . . ? O3 Co1 O1 83.54(17) . . ? O2 Co1 O1 83.50(15) 11 . ? O2 Co1 O1 83.08(13) . . ? O3 Co1 O1 82.49(14) 2 . ? O4 Co1 Ti1 134.7(2) . 11 ? O3 Co1 Ti1 85.46(19) . 11 ? O2 Co1 Ti1 38.48(14) 11 11 ? O2 Co1 Ti1 86.96(15) . 11 ? O3 Co1 Ti1 127.57(14) 2 11 ? O1 Co1 Ti1 45.079(19) . 11 ? O4 Co1 Ti1 134.8(2) . 12 ? O3 Co1 Ti1 128.62(17) . 12 ? O2 Co1 Ti1 83.78(18) 11 12 ? O2 Co1 Ti1 38.06(13) . 12 ? O3 Co1 Ti1 84.72(18) 2 12 ? O1 Co1 Ti1 45.079(19) . 12 ? Ti1 Co1 Ti1 60.18(4) 11 12 ? O4 Co1 Ti1 135.3(2) . 2 ? O3 Co1 Ti1 85.41(17) . 2 ? O2 Co1 Ti1 128.37(15) 11 2 ? O2 Co1 Ti1 83.27(16) . 2 ? O3 Co1 Ti1 37.57(14) 2 2 ? O1 Co1 Ti1 44.921(19) . 2 ? Ti1 Co1 Ti1 90.0 11 2 ? Ti1 Co1 Ti1 59.91(2) 12 2 ? O4 Co1 Ti1 135.2(2) . 3 ? O3 Co1 Ti1 38.62(17) . 3 ? O2 Co1 Ti1 87.02(15) 11 3 ? O2 Co1 Ti1 127.96(13) . 3 ? O3 Co1 Ti1 84.68(16) 2 3 ? O1 Co1 Ti1 44.921(19) . 3 ? Ti1 Co1 Ti1 59.91(2) 11 3 ? Ti1 Co1 Ti1 90.0 12 3 ? Ti1 Co1 Ti1 60.0 2 3 ? Ti1 O1 Co1 0.00(8) 10 10 ? Ti1 O1 Co1 180.00(8) 10 . ? Co1 O1 Co1 180.00(8) 10 . ? Ti1 O1 Ti1 89.84(4) 10 2 ? Co1 O1 Ti1 89.84(4) 10 2 ? Co1 O1 Ti1 90.16(4) . 2 ? Ti1 O1 Co1 89.84(4) 10 2 ? Co1 O1 Co1 89.84(4) 10 2 ? Co1 O1 Co1 90.16(4) . 2 ? Ti1 O1 Co1 0.00(5) 2 2 ? Ti1 O1 Ti1 90.16(4) 10 11 ? Co1 O1 Ti1 90.16(4) 10 11 ? Co1 O1 Ti1 89.84(4) . 11 ? Ti1 O1 Ti1 180.00(4) 2 11 ? Co1 O1 Ti1 180.00(4) 2 11 ? Ti1 O1 Co1 90.16(4) 10 11 ? Co1 O1 Co1 90.16(4) 10 11 ? Co1 O1 Co1 89.84(4) . 11 ? Ti1 O1 Co1 180.00(4) 2 11 ? Co1 O1 Co1 180.00(4) 2 11 ? Ti1 O1 Co1 0.00(5) 11 11 ? Ti1 O1 Ti1 90.16(4) 10 12 ? Co1 O1 Ti1 90.16(4) 10 12 ? Co1 O1 Ti1 89.84(4) . 12 ? Ti1 O1 Ti1 89.84(4) 2 12 ? Co1 O1 Ti1 89.84(4) 2 12 ? Ti1 O1 Ti1 90.16(4) 11 12 ? Co1 O1 Ti1 90.16(4) 11 12 ? Ti1 O1 Co1 89.84(4) 10 3 ? Co1 O1 Co1 89.84(4) 10 3 ? Co1 O1 Co1 90.16(4) . 3 ? Ti1 O1 Co1 90.16(4) 2 3 ? Co1 O1 Co1 90.16(4) 2 3 ? Ti1 O1 Co1 89.84(4) 11 3 ? Co1 O1 Co1 89.84(4) 11 3 ? Ti1 O1 Co1 180.00(4) 12 3 ? Ti1 O1 Co1 90.16(4) 10 12 ? Co1 O1 Co1 90.16(4) 10 12 ? Co1 O1 Co1 89.84(4) . 12 ? Ti1 O1 Co1 89.84(4) 2 12 ? Co1 O1 Co1 89.84(4) 2 12 ? Ti1 O1 Co1 90.16(4) 11 12 ? Co1 O1 Co1 90.16(4) 11 12 ? Ti1 O1 Co1 0.00(5) 12 12 ? Co1 O1 Co1 180.00(4) 3 12 ? Ti1 O1 Ti1 89.84(4) 10 3 ? Co1 O1 Ti1 89.84(4) 10 3 ? Co1 O1 Ti1 90.16(4) . 3 ? Ti1 O1 Ti1 90.16(4) 2 3 ? Co1 O1 Ti1 90.16(4) 2 3 ? Ti1 O1 Ti1 89.84(4) 11 3 ? Co1 O1 Ti1 89.84(4) 11 3 ? Ti1 O1 Ti1 180.00(4) 12 3 ? Co1 O1 Ti1 0.00(5) 3 3 ? Co1 O1 Ti1 180.00(4) 12 3 ? C6A O2 C6B 56.7(12) . . ? C6A O2 Ti1 123.6(6) . 12 ? C6B O2 Ti1 105.4(10) . 12 ? C6A O2 Co1 123.6(6) . 12 ? C6B O2 Co1 105.4(10) . 12 ? Ti1 O2 Co1 0.00(10) 12 12 ? C6A O2 Co1 115.7(6) . . ? C6B O2 Co1 148.0(10) . . ? Ti1 O2 Co1 103.5(2) 12 . ? Co1 O2 Co1 103.5(2) 12 . ? C4A O3 C4B 86.3(10) . . ? C4A O3 C4C 51.8(11) . . ? C4B O3 C4C 50.5(11) . . ? C4A O3 Co1 123.1(8) . . ? C4B O3 Co1 120.5(9) . . ? C4C O3 Co1 105.4(11) . . ? C4A O3 Ti1 110.6(8) . 3 ? C4B O3 Ti1 112.2(8) . 3 ? C4C O3 Ti1 150.7(11) . 3 ? Co1 O3 Ti1 103.8(2) . 3 ? C4A O3 Co1 110.6(8) . 3 ? C4B O3 Co1 112.2(8) . 3 ? C4C O3 Co1 150.7(11) . 3 ? Co1 O3 Co1 103.8(2) . 3 ? Ti1 O3 Co1 0.00(10) 3 3 ? C2 O4 Co1 158.3(9) . . ? O4 C2 C1 153.4(15) . . ? O4 C2 C3A 96.1(12) . . ? C1 C2 C3A 104.8(13) . . ? O4 C2 C3B 93.9(12) . . ? C1 C2 C3B 97.9(12) . . ? C3A C2 C3B 101.1(16) . . ? C2 C3A C4C 126.7(18) . . ? C6B C3B C2 123.8(17) 11 . ? C4C C4A O3 65.9(13) . . ? C4C C4A C5 49.9(12) . . ? O3 C4A C5 98.3(11) . . ? C4C C4B O3 65.9(13) . . ? C4C C4B C5 47.6(13) . . ? O3 C4B C5 93.3(11) . . ? C4C C5 C4A 57.0(13) . . ? C4C C5 C4B 52.7(14) . . ? C4A C5 C4B 82.2(10) . . ? C6B C6A O2 65.3(12) . . ? C6B C6A C7 47.7(11) . . ? O2 C6A C7 99.1(10) . . ? C7 C6B C6A 74.2(16) . . ? C7 C6B C3B 114(2) . 12 ? C6A C6B C3B 120(2) . 12 ? C7 C6B O2 113.0(17) . . ? C6A C6B O2 58.0(9) . . ? C3B C6B O2 129.6(19) 12 . ? C6B C7 C6A 58.1(13) . . ? C5 C4C C4B 79.8(19) . . ? C5 C4C C4A 73.1(17) . . ? C4B C4C C4A 103(2) . . ? C5 C4C C3A 118(2) . . ? C4B C4C C3A 125(2) . . ? C4A C4C C3A 132(2) . . ? C5 C4C O3 111(2) . . ? C4B C4C O3 63.6(14) . . ? C4A C4C O3 62.2(13) . . ? C3A C4C O3 131(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.596 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.087 # Attachment '- Comp5.cif' data_mg5ti0 _database_code_depnum_ccdc_archive 'CCDC 771909' #TrackingRef '- Comp5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H72 Mg5 O19 Ti' _chemical_formula_weight 1050.45 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.426(19) _cell_length_b 20.426(19) _cell_length_c 11.738(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4241(7) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 468 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 19.90 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_absorpt_coefficient_mu 0.271 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8764 _exptl_absorpt_correction_T_max 0.9354 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; 'Data cut-off at 1\%A resolution, 2theta=42.0 deg, because of poor reflectivity' ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2289 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 21.00 _reflns_number_total 958 _reflns_number_gt 631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0860P)^2^+45.4247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 958 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2632 _refine_ls_wR_factor_gt 0.2450 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mg1 Mg 0.07918(13) 0.09772(12) 0.1098(2) 0.0645(12) Uani 0.83 1 d P . . Ti1 Ti 0.07918(13) 0.09772(12) 0.1098(2) 0.0645(12) Uani 0.17 1 d P . . O1 O 0.0000 0.0000 0.0000 0.046(3) Uani 1 6 d S . . O2 O 0.0496(3) 0.1576(3) 0.0037(6) 0.095(2) Uani 1 1 d . . . O3 O 0.0890(4) 0.0193(4) 0.1972(6) 0.112(3) Uani 1 1 d . . . O4 O 0.1465(5) 0.1799(4) 0.2013(7) 0.120(3) Uani 1 1 d . . . C1 C 0.2411(9) 0.2784(9) 0.3207(16) 0.205(8) Uani 1 1 d . . . C2 C 0.1958(11) 0.2112(11) 0.2548(19) 0.191(8) Uani 1 1 d . . . C3A C 0.187(2) 0.135(2) 0.335(3) 0.19(2) Uiso 0.48(3) 1 d P . . C3B C 0.262(2) 0.219(2) 0.127(4) 0.21(2) Uiso 0.52(3) 1 d P . . C4A C 0.081(3) 0.009(2) 0.336(3) 0.22(2) Uiso 0.57(5) 1 d P . . C4B C 0.157(2) 0.020(2) 0.248(4) 0.17(2) Uiso 0.43(5) 1 d P . . C5 C 0.1518(9) 0.0111(10) 0.3675(15) 0.171(6) Uani 1 1 d . . . C6A C 0.035(2) 0.218(2) 0.068(3) 0.093(19) Uiso 0.29(3) 1 d P . . C6B C 0.0887(14) 0.2366(16) -0.026(2) 0.163(12) Uiso 0.71(3) 1 d P . . C7 C 0.1061(13) 0.2925(8) 0.0303(18) 0.228(10) Uani 1 1 d . . . C4C C 0.1424(17) 0.0593(17) 0.292(3) 0.064(16) Uiso 0.31(4) 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mg1 0.0575(17) 0.0544(17) 0.075(2) -0.0194(13) -0.0156(13) 0.0226(12) Ti1 0.0575(17) 0.0544(17) 0.075(2) -0.0194(13) -0.0156(13) 0.0226(12) O1 0.040(4) 0.040(4) 0.057(8) 0.000 0.000 0.020(2) O2 0.073(4) 0.047(4) 0.157(7) -0.017(4) 0.002(4) 0.025(3) O3 0.130(6) 0.149(7) 0.088(6) 0.006(5) -0.031(5) 0.093(5) O4 0.096(6) 0.105(6) 0.141(7) -0.046(5) -0.045(5) 0.036(5) C1 0.176(15) 0.142(13) 0.224(18) -0.092(13) -0.056(13) 0.025(11) C2 0.153(15) 0.155(16) 0.24(2) -0.077(15) -0.075(15) 0.059(13) C5 0.123(12) 0.209(16) 0.142(15) 0.042(12) -0.023(10) 0.054(11) C7 0.34(3) 0.080(10) 0.23(2) -0.036(12) -0.012(18) 0.083(14) _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 Mg1 O4 1.885(8) . ? Mg1 O3 1.996(7) . ? Mg1 O2 2.012(7) 11 ? Mg1 O2 2.037(7) . ? Mg1 O3 2.067(8) 2 ? Mg1 O1 2.243(3) . ? Mg1 Mg1 3.180(5) 2 ? Mg1 Ti1 3.180(5) 2 ? Mg1 Mg1 3.180(5) 3 ? Mg1 Ti1 3.180(5) 3 ? Mg1 Mg1 3.164(5) 12 ? Mg1 Ti1 3.164(5) 12 ? O1 Ti1 2.243(3) 10 ? O1 Mg1 2.243(3) 10 ? O1 Ti1 2.243(3) 12 ? O1 Mg1 2.243(3) 12 ? O1 Mg1 2.243(3) 11 ? O1 Ti1 2.243(3) 11 ? O1 Mg1 2.243(3) 3 ? O1 Ti1 2.243(3) 3 ? O1 Ti1 2.243(3) 2 ? O1 Mg1 2.243(3) 2 ? O2 C6A 1.60(4) . ? O2 C6B 1.44(3) . ? O2 Ti1 2.012(7) 12 ? O2 Mg1 2.012(7) 12 ? O3 C4B 1.51(4) . ? O3 C4C 1.49(3) . ? O3 C4A 1.64(4) . ? O3 Ti1 2.067(8) 3 ? O3 Mg1 2.067(8) 3 ? O4 C2 1.083(16) . ? C1 C2 1.44(2) . ? C2 C3A 1.76(4) . ? C2 C3B 1.97(4) . ? C3A C4C 1.43(5) . ? C3B C6B 1.74(4) 11 ? C4A C4C 1.27(4) . ? C4A C5 1.48(4) . ? C4B C4C 1.12(4) . ? C4B C5 1.41(5) . ? C5 C4C 1.40(3) . ? C6A C6B 1.46(4) . ? C6A C7 1.55(4) . ? C6B C7 1.21(3) . ? C6B C3B 1.74(4) 12 ? 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 O4 Mg1 O3 95.7(4) . . ? O4 Mg1 O2 95.5(3) . 11 ? O3 Mg1 O2 91.7(3) . 11 ? O4 Mg1 O2 96.8(3) . . ? O3 Mg1 O2 167.3(3) . . ? O2 Mg1 O2 89.56(12) 11 . ? O4 Mg1 O3 98.0(3) . 2 ? O3 Mg1 O3 89.9(5) . 2 ? O2 Mg1 O3 166.2(3) 11 2 ? O2 Mg1 O3 86.0(3) . 2 ? O4 Mg1 O1 179.4(3) . . ? O3 Mg1 O1 84.2(2) . . ? O2 Mg1 O1 83.9(2) 11 . ? O2 Mg1 O1 83.37(19) . . ? O3 Mg1 O1 82.6(2) 2 . ? O4 Mg1 Mg1 135.7(3) . 2 ? O3 Mg1 Mg1 86.2(2) . 2 ? O2 Mg1 Mg1 128.7(2) 11 2 ? O2 Mg1 Mg1 83.18(19) . 2 ? O3 Mg1 Mg1 37.71(19) 2 2 ? O1 Mg1 Mg1 44.86(5) . 2 ? O4 Mg1 Ti1 135.7(3) . 2 ? O3 Mg1 Ti1 86.2(2) . 2 ? O2 Mg1 Ti1 128.7(2) 11 2 ? O2 Mg1 Ti1 83.18(19) . 2 ? O3 Mg1 Ti1 37.71(19) 2 2 ? O1 Mg1 Ti1 44.86(5) . 2 ? Mg1 Mg1 Ti1 0.00(16) 2 2 ? O4 Mg1 Mg1 135.0(3) . 3 ? O3 Mg1 Mg1 39.3(2) . 3 ? O2 Mg1 Mg1 87.45(19) 11 3 ? O2 Mg1 Mg1 128.17(18) . 3 ? O3 Mg1 Mg1 85.1(2) 2 3 ? O1 Mg1 Mg1 44.86(5) . 3 ? Mg1 Mg1 Mg1 60.0 2 3 ? Ti1 Mg1 Mg1 60.0 2 3 ? O4 Mg1 Ti1 135.0(3) . 3 ? O3 Mg1 Ti1 39.3(2) . 3 ? O2 Mg1 Ti1 87.45(19) 11 3 ? O2 Mg1 Ti1 128.17(18) . 3 ? O3 Mg1 Ti1 85.1(2) 2 3 ? O1 Mg1 Ti1 44.86(5) . 3 ? Mg1 Mg1 Ti1 60.0 2 3 ? Ti1 Mg1 Ti1 60.0 2 3 ? Mg1 Mg1 Ti1 0.00(12) 3 3 ? O4 Mg1 Mg1 135.0(3) . 12 ? O3 Mg1 Mg1 129.3(2) . 12 ? O2 Mg1 Mg1 84.0(2) 11 12 ? O2 Mg1 Mg1 38.30(18) . 12 ? O3 Mg1 Mg1 84.4(2) 2 12 ? O1 Mg1 Mg1 45.14(5) . 12 ? Mg1 Mg1 Mg1 59.83(6) 2 12 ? Ti1 Mg1 Mg1 59.83(6) 2 12 ? Mg1 Mg1 Mg1 90.0 3 12 ? Ti1 Mg1 Mg1 90.0 3 12 ? O4 Mg1 Ti1 135.0(3) . 12 ? O3 Mg1 Ti1 129.3(2) . 12 ? O2 Mg1 Ti1 84.0(2) 11 12 ? O2 Mg1 Ti1 38.30(18) . 12 ? O3 Mg1 Ti1 84.4(2) 2 12 ? O1 Mg1 Ti1 45.14(5) . 12 ? Mg1 Mg1 Ti1 59.83(6) 2 12 ? Ti1 Mg1 Ti1 59.83(6) 2 12 ? Mg1 Mg1 Ti1 90.0 3 12 ? Ti1 Mg1 Ti1 90.0 3 12 ? Mg1 Mg1 Ti1 0.00(9) 12 12 ? Ti1 O1 Mg1 0.0(2) 10 10 ? Ti1 O1 Mg1 180.00(14) 10 . ? Mg1 O1 Mg1 180.00(14) 10 . ? Ti1 O1 Ti1 90.29(10) 10 12 ? Mg1 O1 Ti1 90.29(10) 10 12 ? Mg1 O1 Ti1 89.71(10) . 12 ? Ti1 O1 Mg1 90.29(10) 10 12 ? Mg1 O1 Mg1 90.29(10) 10 12 ? Mg1 O1 Mg1 89.71(10) . 12 ? Ti1 O1 Mg1 0.00(14) 12 12 ? Ti1 O1 Mg1 90.29(10) 10 11 ? Mg1 O1 Mg1 90.29(10) 10 11 ? Mg1 O1 Mg1 89.71(10) . 11 ? Ti1 O1 Mg1 90.29(10) 12 11 ? Mg1 O1 Mg1 90.29(10) 12 11 ? Ti1 O1 Ti1 90.29(10) 10 11 ? Mg1 O1 Ti1 90.29(10) 10 11 ? Mg1 O1 Ti1 89.71(10) . 11 ? Ti1 O1 Ti1 90.29(10) 12 11 ? Mg1 O1 Ti1 90.29(10) 12 11 ? Mg1 O1 Ti1 0.00(15) 11 11 ? Ti1 O1 Mg1 89.71(10) 10 3 ? Mg1 O1 Mg1 89.71(10) 10 3 ? Mg1 O1 Mg1 90.29(10) . 3 ? Ti1 O1 Mg1 180.00(14) 12 3 ? Mg1 O1 Mg1 180.00(14) 12 3 ? Mg1 O1 Mg1 89.71(10) 11 3 ? Ti1 O1 Mg1 89.71(10) 11 3 ? Ti1 O1 Ti1 89.71(10) 10 3 ? Mg1 O1 Ti1 89.71(10) 10 3 ? Mg1 O1 Ti1 90.29(10) . 3 ? Ti1 O1 Ti1 180.00(14) 12 3 ? Mg1 O1 Ti1 180.00(14) 12 3 ? Mg1 O1 Ti1 89.71(10) 11 3 ? Ti1 O1 Ti1 89.71(10) 11 3 ? Mg1 O1 Ti1 0.00(14) 3 3 ? Ti1 O1 Ti1 89.71(10) 10 2 ? Mg1 O1 Ti1 89.71(10) 10 2 ? Mg1 O1 Ti1 90.29(10) . 2 ? Ti1 O1 Ti1 89.71(10) 12 2 ? Mg1 O1 Ti1 89.71(10) 12 2 ? Mg1 O1 Ti1 180.00(15) 11 2 ? Ti1 O1 Ti1 180.00(15) 11 2 ? Mg1 O1 Ti1 90.29(10) 3 2 ? Ti1 O1 Ti1 90.29(10) 3 2 ? Ti1 O1 Mg1 89.71(10) 10 2 ? Mg1 O1 Mg1 89.71(10) 10 2 ? Mg1 O1 Mg1 90.29(10) . 2 ? Ti1 O1 Mg1 89.71(10) 12 2 ? Mg1 O1 Mg1 89.71(10) 12 2 ? Mg1 O1 Mg1 180.00(15) 11 2 ? Ti1 O1 Mg1 180.00(15) 11 2 ? Mg1 O1 Mg1 90.29(10) 3 2 ? Ti1 O1 Mg1 90.29(10) 3 2 ? Ti1 O1 Mg1 0.00(15) 2 2 ? C6A O2 C6B 57.2(15) . . ? C6A O2 Ti1 127.4(13) . 12 ? C6B O2 Ti1 120.5(11) . 12 ? C6A O2 Mg1 127.4(13) . 12 ? C6B O2 Mg1 120.5(11) . 12 ? Ti1 O2 Mg1 0.0(3) 12 12 ? C6A O2 Mg1 113.6(14) . . ? C6B O2 Mg1 131.0(10) . . ? Ti1 O2 Mg1 102.8(3) 12 . ? Mg1 O2 Mg1 102.8(3) 12 . ? C4B O3 C4C 43.8(17) . . ? C4B O3 C4A 69(2) . . ? C4C O3 C4A 47.4(16) . . ? C4B O3 Mg1 131.0(16) . . ? C4C O3 Mg1 106.6(13) . . ? C4A O3 Mg1 124.5(14) . . ? C4B O3 Ti1 113.4(18) . 3 ? C4C O3 Ti1 150.4(12) . 3 ? C4A O3 Ti1 113.2(15) . 3 ? Mg1 O3 Ti1 103.0(3) . 3 ? C4B O3 Mg1 113.4(18) . 3 ? C4C O3 Mg1 150.4(12) . 3 ? C4A O3 Mg1 113.2(15) . 3 ? Mg1 O3 Mg1 103.0(3) . 3 ? Ti1 O3 Mg1 0.0(3) 3 3 ? C2 O4 Mg1 154.9(13) . . ? O4 C2 C1 147(2) . . ? O4 C2 C3A 97.7(19) . . ? C1 C2 C3A 107(2) . . ? O4 C2 C3B 90.0(18) . . ? C1 C2 C3B 104.3(18) . . ? C3A C2 C3B 103.9(19) . . ? C4C C3A C2 120(3) . . ? C6B C3B C2 123(2) 11 . ? C4C C4A C5 61(2) . . ? C4C C4A O3 60(2) . . ? C5 C4A O3 102(3) . . ? C4C C4B O3 67(3) . . ? C4C C4B C5 66(3) . . ? O3 C4B C5 112(3) . . ? C4C C5 C4A 52.1(18) . . ? C4C C5 C4B 46.8(18) . . ? C4A C5 C4B 77(2) . . ? C6B C6A O2 56.0(17) . . ? C6B C6A C7 47.2(16) . . ? O2 C6A C7 100(2) . . ? C7 C6B C6A 70(2) . . ? C7 C6B O2 132(2) . . ? C6A C6B O2 66.8(19) . . ? C7 C6B C3B 92(2) . 12 ? C6A C6B C3B 99(2) . 12 ? O2 C6B C3B 115(2) . 12 ? C6B C7 C6A 62.7(17) . . ? C5 C4C C4B 67(3) . . ? C5 C4C C4A 67(2) . . ? C4B C4C C4A 97(3) . . ? C5 C4C O3 114(2) . . ? C4B C4C O3 69(3) . . ? C4A C4C O3 73(2) . . ? C5 C4C C3A 107(3) . . ? C4B C4C C3A 133(4) . . ? C4A C4C C3A 125(3) . . ? O3 C4C C3A 139(3) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.303 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.059 # Attachment '- Comp6.cif' data_cotipn1m _database_code_depnum_ccdc_archive 'CCDC 773140' #TrackingRef '- Comp6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H98 Co4 O19 Ti2' _chemical_formula_weight 1334.80 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.0908(8) _cell_length_b 14.0908(8) _cell_length_c 16.6137(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3298.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 668(I>4sigma(I)) _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 24.00 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 1.274 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6640 _exptl_absorpt_correction_T_max 0.8319 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8816 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1673 _reflns_number_gt 1129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0596P)^2^+2.0765P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1673 _refine_ls_number_parameters 115 _refine_ls_number_restraints 131 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.07236(4) 0.14538(4) 0.0000 0.0474(2) Uani 1 2 d SU . . Ti2 Ti 0.0000 0.0000 0.12905(6) 0.0468(3) Uani 1 4 d SU . . O1 O 0.0000 0.0000 0.0000 0.0391(11) Uani 1 8 d SU . . O2 O 0.20400(19) 0.08126(19) 0.0000 0.0522(7) Uani 1 2 d SU . . O3 O 0.1324(2) 0.2736(2) 0.0000 0.0735(10) Uani 1 2 d SU . . O4 O 0.05055(14) 0.12849(13) 0.11781(13) 0.0510(5) Uani 1 1 d U . . O5 O 0.0000 0.0000 0.2360(3) 0.0727(13) Uani 1 4 d SDU . . C6 C 0.0317(2) 0.2070(2) 0.1688(2) 0.0650(9) Uani 1 1 d U . . H6A H -0.0165 0.1893 0.2077 0.078 Uiso 1 1 calc R . . H6B H 0.0070 0.2590 0.1368 0.078 Uiso 1 1 calc R . . C2 C 0.2826(3) 0.1258(3) 0.0000 0.0596(12) Uani 1 2 d SU . . C1 C 0.3726(3) 0.0682(4) 0.0000 0.0831(17) Uani 1 2 d SU . . H1A H 0.3571 0.0018 0.0000 0.125 Uiso 1 2 calc SR . . H1B H 0.4091 0.0830 0.0472 0.125 Uiso 0.25 1 calc PR . . H1C H 0.4091 0.0830 -0.0472 0.125 Uiso 0.25 1 calc PR . . C7 C 0.1186(3) 0.2393(3) 0.2124(3) 0.0948(14) Uani 1 1 d U . . H7A H 0.1668 0.2572 0.1736 0.114 Uiso 1 1 calc R . . H7B H 0.1434 0.1874 0.2444 0.114 Uiso 1 1 calc R . . C3 C 0.2923(4) 0.2222(4) 0.0000 0.0886(18) Uani 1 2 d SU . . H3A H 0.3541 0.2453 0.0000 0.106 Uiso 1 2 calc SR . . C4 C 0.2205(4) 0.2897(4) 0.0000 0.100(2) Uani 1 2 d SU . . C8 C 0.0976(4) 0.3234(4) 0.2671(3) 0.139(2) Uani 1 1 d U . . H8A H 0.1549 0.3430 0.2936 0.209 Uiso 1 1 calc R . . H8B H 0.0514 0.3053 0.3067 0.209 Uiso 1 1 calc R . . H8C H 0.0733 0.3751 0.2355 0.209 Uiso 1 1 calc R . . C5 C 0.2452(6) 0.3941(5) 0.0000 0.203(6) Uani 1 2 d SU . . H5A H 0.1880 0.4310 0.0000 0.305 Uiso 1 2 calc SR . . H5B H 0.2817 0.4088 -0.0472 0.305 Uiso 0.25 1 calc PR . . H5C H 0.2817 0.4088 0.0472 0.305 Uiso 0.25 1 calc PR . . C11 C 0.092(2) 0.047(4) 0.369(2) 0.264(14) Uani 0.25 1 d PDU . . C10 C 0.0000 0.0000 0.3837(8) 0.271(11) Uani 1 4 d SDU . . C9 C -0.0548(15) -0.012(5) 0.3108(8) 0.173(10) Uani 0.25 1 d PDU . . 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 Co1 0.0448(4) 0.0405(3) 0.0569(4) 0.000 0.000 -0.0018(2) Ti2 0.0475(4) 0.0475(4) 0.0455(6) 0.000 0.000 0.000 O1 0.0381(16) 0.0381(16) 0.041(3) 0.000 0.000 0.000 O2 0.0433(15) 0.0462(16) 0.067(2) 0.000 0.000 -0.0006(12) O3 0.0590(19) 0.0443(17) 0.117(3) 0.000 0.000 -0.0028(14) O4 0.0500(11) 0.0466(11) 0.0565(13) -0.0122(9) -0.0016(9) -0.0023(8) O5 0.086(2) 0.086(2) 0.046(2) 0.000 0.000 0.000 C6 0.064(2) 0.061(2) 0.070(2) -0.0205(17) 0.0008(16) 0.0007(16) C2 0.041(2) 0.055(2) 0.083(3) 0.000 0.000 -0.0066(19) C1 0.042(3) 0.072(3) 0.135(5) 0.000 0.000 -0.002(2) C7 0.083(3) 0.090(3) 0.111(3) -0.047(3) -0.022(2) -0.001(2) C3 0.049(3) 0.057(3) 0.160(6) 0.000 0.000 -0.014(2) C4 0.068(3) 0.051(3) 0.182(7) 0.000 0.000 -0.017(2) C8 0.123(4) 0.124(4) 0.171(5) -0.090(4) -0.037(4) 0.001(3) C5 0.095(6) 0.050(4) 0.465(18) 0.000 0.000 -0.025(4) C11 0.34(3) 0.35(3) 0.10(2) -0.01(3) -0.031(19) -0.01(3) C10 0.369(16) 0.369(16) 0.074(7) 0.000 0.000 0.000 C9 0.231(19) 0.24(2) 0.047(7) 0.035(19) 0.035(7) 0.05(2) _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 Co1 O3 1.996(3) . ? Co1 O4 1.995(2) 10 ? Co1 O4 1.995(2) . ? Co1 O2 2.063(3) . ? Co1 O1 2.2883(5) . ? Co1 O2 2.317(3) 3 ? Co1 Ti2 3.1358(8) 9 ? Co1 Ti2 3.1358(8) . ? Ti2 O5 1.777(5) . ? Ti2 O4 1.9546(19) 3 ? Ti2 O4 1.9546(19) 4 ? Ti2 O4 1.9546(19) . ? Ti2 O4 1.9546(19) 2 ? Ti2 O1 2.1441(11) . ? Ti2 Co1 3.1358(8) 9 ? Ti2 Co1 3.1358(8) 11 ? Ti2 Co1 3.1358(8) 3 ? O1 Ti2 2.1441(11) 9 ? O1 Co1 2.2883(5) 11 ? O1 Co1 2.2883(5) 9 ? O1 Co1 2.2883(5) 3 ? O2 C2 1.273(5) . ? O2 Co1 2.317(3) 11 ? O3 C4 1.262(6) . ? O4 C6 1.419(3) . ? O5 C9 1.473(13) 4 ? O5 C9 1.473(13) . ? O5 C9 1.473(13) 2 ? O5 C9 1.473(13) 3 ? C6 C7 1.495(5) . ? C2 C3 1.364(7) . ? C2 C1 1.507(6) . ? C7 C8 1.522(5) . ? C3 C4 1.389(7) . ? C4 C5 1.511(8) . ? C11 C10 1.468(18) . ? C11 C11 2.05(2) 3 ? C11 C11 2.05(2) 4 ? C11 C9 1.75(6) 4 ? C10 C11 1.468(18) 3 ? C10 C11 1.468(18) 4 ? C10 C11 1.468(18) 2 ? C10 C9 1.445(15) 3 ? C10 C9 1.445(15) 2 ? C10 C9 1.445(15) 4 ? C10 C9 1.445(15) . ? C9 C9 1.12(2) 4 ? C9 C9 1.12(2) 3 ? C9 C11 1.75(6) 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 O3 Co1 O4 99.98(6) . 10 ? O3 Co1 O4 99.98(6) . . ? O4 Co1 O4 157.54(11) 10 . ? O3 Co1 O2 90.87(12) . . ? O4 Co1 O2 94.95(6) 10 . ? O4 Co1 O2 94.95(6) . . ? O3 Co1 O1 178.64(10) . . ? O4 Co1 O1 79.90(5) 10 . ? O4 Co1 O1 79.90(5) . . ? O2 Co1 O1 90.49(8) . . ? O3 Co1 O2 94.21(12) . 3 ? O4 Co1 O2 84.18(6) 10 3 ? O4 Co1 O2 84.18(6) . 3 ? O2 Co1 O2 174.92(11) . 3 ? O1 Co1 O2 84.42(7) . 3 ? O3 Co1 Ti2 136.846(16) . 9 ? O4 Co1 Ti2 37.00(5) 10 9 ? O4 Co1 Ti2 122.86(6) . 9 ? O2 Co1 Ti2 90.36(6) . 9 ? O1 Co1 Ti2 43.137(16) . 9 ? O2 Co1 Ti2 85.93(5) 3 9 ? O3 Co1 Ti2 136.846(16) . . ? O4 Co1 Ti2 122.86(6) 10 . ? O4 Co1 Ti2 37.00(5) . . ? O2 Co1 Ti2 90.36(6) . . ? O1 Co1 Ti2 43.137(16) . . ? O2 Co1 Ti2 85.93(5) 3 . ? Ti2 Co1 Ti2 86.27(3) 9 . ? O5 Ti2 O4 95.49(7) . 3 ? O5 Ti2 O4 95.49(7) . 4 ? O4 Ti2 O4 169.03(14) 3 4 ? O5 Ti2 O4 95.49(7) . . ? O4 Ti2 O4 89.476(13) 3 . ? O4 Ti2 O4 89.476(13) 4 . ? O5 Ti2 O4 95.49(7) . 2 ? O4 Ti2 O4 89.476(13) 3 2 ? O4 Ti2 O4 89.476(13) 4 2 ? O4 Ti2 O4 169.03(14) . 2 ? O5 Ti2 O1 180.0 . . ? O4 Ti2 O1 84.51(7) 3 . ? O4 Ti2 O1 84.51(7) 4 . ? O4 Ti2 O1 84.51(7) . . ? O4 Ti2 O1 84.51(7) 2 . ? O5 Ti2 Co1 133.137(16) . 9 ? O4 Ti2 Co1 82.62(6) 3 9 ? O4 Ti2 Co1 89.87(6) 4 9 ? O4 Ti2 Co1 131.17(8) . 9 ? O4 Ti2 Co1 37.91(6) 2 9 ? O1 Ti2 Co1 46.863(16) . 9 ? O5 Ti2 Co1 133.137(16) . 11 ? O4 Ti2 Co1 131.17(8) 3 11 ? O4 Ti2 Co1 37.91(6) 4 11 ? O4 Ti2 Co1 89.87(6) . 11 ? O4 Ti2 Co1 82.62(6) 2 11 ? O1 Ti2 Co1 46.863(16) . 11 ? Co1 Ti2 Co1 62.128(18) 9 11 ? O5 Ti2 Co1 133.137(16) . 3 ? O4 Ti2 Co1 37.91(6) 3 3 ? O4 Ti2 Co1 131.17(8) 4 3 ? O4 Ti2 Co1 82.62(6) . 3 ? O4 Ti2 Co1 89.87(6) 2 3 ? O1 Ti2 Co1 46.863(16) . 3 ? Co1 Ti2 Co1 62.128(18) 9 3 ? Co1 Ti2 Co1 93.73(3) 11 3 ? O5 Ti2 Co1 133.137(16) . . ? O4 Ti2 Co1 89.87(6) 3 . ? O4 Ti2 Co1 82.62(6) 4 . ? O4 Ti2 Co1 37.91(6) . . ? O4 Ti2 Co1 131.17(8) 2 . ? O1 Ti2 Co1 46.863(16) . . ? Co1 Ti2 Co1 93.73(3) 9 . ? Co1 Ti2 Co1 62.128(18) 11 . ? Co1 Ti2 Co1 62.128(18) 3 . ? Ti2 O1 Ti2 180.0 9 . ? Ti2 O1 Co1 90.0 9 . ? Ti2 O1 Co1 90.0 . . ? Ti2 O1 Co1 90.0 9 11 ? Ti2 O1 Co1 90.0 . 11 ? Co1 O1 Co1 90.0 . 11 ? Ti2 O1 Co1 90.0 9 9 ? Ti2 O1 Co1 90.0 . 9 ? Co1 O1 Co1 180.00(3) . 9 ? Co1 O1 Co1 90.0 11 9 ? Ti2 O1 Co1 90.0 9 3 ? Ti2 O1 Co1 90.0 . 3 ? Co1 O1 Co1 90.0 . 3 ? Co1 O1 Co1 180.00(3) 11 3 ? Co1 O1 Co1 90.0 9 3 ? C2 O2 Co1 124.5(3) . . ? C2 O2 Co1 140.5(3) . 11 ? Co1 O2 Co1 95.08(11) . 11 ? C4 O3 Co1 125.4(3) . . ? C6 O4 Ti2 126.6(2) . . ? C6 O4 Co1 121.5(2) . . ? Ti2 O4 Co1 105.09(9) . . ? C9 O5 C9 44.6(8) 4 . ? C9 O5 C9 44.6(8) 4 2 ? C9 O5 C9 64.9(13) . 2 ? C9 O5 C9 64.9(13) 4 3 ? C9 O5 C9 44.6(8) . 3 ? C9 O5 C9 44.6(8) 2 3 ? C9 O5 Ti2 147.6(6) 4 . ? C9 O5 Ti2 147.6(6) . . ? C9 O5 Ti2 147.6(6) 2 . ? C9 O5 Ti2 147.6(6) 3 . ? O4 C6 C7 111.9(3) . . ? O2 C2 C3 125.3(4) . . ? O2 C2 C1 117.8(4) . . ? C3 C2 C1 116.9(4) . . ? C6 C7 C8 111.5(4) . . ? C2 C3 C4 127.5(5) . . ? O3 C4 C3 126.4(5) . . ? O3 C4 C5 113.7(6) . . ? C3 C4 C5 119.9(5) . . ? C10 C11 C11 45.8(2) . 3 ? C10 C11 C11 45.8(2) . 4 ? C11 C11 C11 90.000(4) 3 4 ? C10 C11 C9 52.4(15) . 4 ? C11 C11 C9 35.9(14) 3 4 ? C11 C11 C9 78.8(11) 4 4 ? C11 C10 C11 88.5(5) . 3 ? C11 C10 C11 88.5(5) . 4 ? C11 C10 C11 161(3) 3 4 ? C11 C10 C11 161(3) . 2 ? C11 C10 C11 88.5(5) 3 2 ? C11 C10 C11 88.5(5) 4 2 ? C11 C10 C9 90(3) . 3 ? C11 C10 C9 112.6(16) 3 3 ? C11 C10 C9 49(2) 4 3 ? C11 C10 C9 74(3) 2 3 ? C11 C10 C9 49(2) . 2 ? C11 C10 C9 90(3) 3 2 ? C11 C10 C9 74(3) 4 2 ? C11 C10 C9 112.6(16) 2 2 ? C9 C10 C9 45.5(8) 3 2 ? C11 C10 C9 74(3) . 4 ? C11 C10 C9 49(2) 3 4 ? C11 C10 C9 112.6(15) 4 4 ? C11 C10 C9 90(3) 2 4 ? C9 C10 C9 66.3(13) 3 4 ? C9 C10 C9 45.5(8) 2 4 ? C11 C10 C9 112.6(16) . . ? C11 C10 C9 74(3) 3 . ? C11 C10 C9 90(3) 4 . ? C11 C10 C9 49(2) 2 . ? C9 C10 C9 45.5(8) 3 . ? C9 C10 C9 66.3(13) 2 . ? C9 C10 C9 45.5(8) 4 . ? C9 C9 C9 90.000(11) 4 3 ? C9 C9 C10 67.3(4) 4 . ? C9 C9 C10 67.3(4) 3 . ? C9 C9 O5 67.7(4) 4 . ? C9 C9 O5 67.7(4) 3 . ? C10 C9 O5 114.4(12) . . ? C9 C9 C11 43(4) 4 3 ? C9 C9 C11 113(3) 3 3 ? C10 C9 C11 53.6(17) . 3 ? O5 C9 C11 110(4) . 3 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.288 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.053