Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Kessler, Vadim' 'Gohil, Surresh' 'Parola, Stephane' _publ_contact_author_name 'Dr Vadim Kessler' _publ_contact_author_address ; Department of Chemistry Swedish University of Agricultural Sciences Box 7015 Uppsala 75007 SWEDEN ; _publ_contact_author_email 'VADIM.KESSLER@KEMI.SLU.SE' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Interaction of some divalent metal acetylacetonates with aluminium, titanium, niobium and tantalum isopropoxides. Factors influencing the formation and stability of heterometallic alkoxide complexes ; data_cotipr5m _database_code_CSD 168879 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 Co2 O10' _chemical_formula_weight 634.47 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' _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 9.4213(14) _cell_length_b 8.4980(13) _cell_length_c 19.315(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.481(3) _cell_angle_gamma 90.00 _cell_volume 1533.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 999(I>2sigma(I)) _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 28.96 _exptl_crystal_description prism _exptl_crystal_colour 'pinkish violet' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 1.131 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.6300 _exptl_absorpt_correction_T_max 0.8054 _exptl_absorpt_process_details ? _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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9452 _diffrn_reflns_av_R_equivalents 0.0659 _diffrn_reflns_av_sigmaI/netI 0.1016 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 28.96 _reflns_number_total 3723 _reflns_number_gt 1798 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3723 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1431 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 0.55302(5) 0.92436(7) 0.07578(3) 0.0428(2) Uani 1 1 d . . . O1 O 0.4440(3) 0.7218(4) 0.02785(18) 0.0554(9) Uani 1 1 d . . . O2 O 0.3846(3) 1.0564(3) 0.02754(14) 0.0431(7) Uani 1 1 d . . . O3 O 0.4590(3) 0.9206(4) 0.16492(15) 0.0551(8) Uani 1 1 d . . . O4 O 0.7128(3) 0.7977(3) 0.12769(14) 0.0495(7) Uani 1 1 d . . . O5 O 0.6671(3) 1.1262(3) 0.09871(15) 0.0514(8) Uani 1 1 d . . . C10 C 0.3634(4) 0.5914(6) 0.0492(3) 0.0586(12) Uani 1 1 d . . . H10A H 0.3599 0.5109 0.0127 0.070 Uiso 1 1 calc R . . C11 C 0.4435(5) 0.5243(6) 0.1138(3) 0.0772(16) Uani 1 1 d . . . H11A H 0.5389 0.4978 0.1055 0.116 Uiso 1 1 calc R . . H11B H 0.3957 0.4313 0.1269 0.116 Uiso 1 1 calc R . . H11C H 0.4477 0.6003 0.1508 0.116 Uiso 1 1 calc R . . C12 C 0.2138(5) 0.6368(7) 0.0560(3) 0.0893(18) Uani 1 1 d . . . H12A H 0.1690 0.6790 0.0125 0.134 Uiso 1 1 calc R . . H12B H 0.2138 0.7149 0.0919 0.134 Uiso 1 1 calc R . . H12C H 0.1618 0.5459 0.0681 0.134 Uiso 1 1 calc R . . C21 C 0.1570(4) 1.1754(6) 0.0087(3) 0.0711(15) Uani 1 1 d . . . H21A H 0.1865 1.1886 -0.0367 0.107 Uiso 1 1 calc R . . H21B H 0.1393 1.2767 0.0279 0.107 Uiso 1 1 calc R . . H21C H 0.0711 1.1137 0.0048 0.107 Uiso 1 1 calc R . . C22 C 0.2723(4) 1.0936(5) 0.0555(2) 0.0445(10) Uani 1 1 d . . . C23 C 0.2519(4) 1.0631(5) 0.1230(2) 0.0534(11) Uani 1 1 d . . . H23A H 0.1680 1.1025 0.1369 0.064 Uiso 1 1 calc R . . C24 C 0.3413(5) 0.9804(5) 0.1735(2) 0.0485(11) Uani 1 1 d . . . C25 C 0.2922(5) 0.9556(6) 0.2436(2) 0.0651(14) Uani 1 1 d . . . H25A H 0.3636 0.8974 0.2731 0.098 Uiso 1 1 calc R . . H25B H 0.2039 0.8978 0.2380 0.098 Uiso 1 1 calc R . . H25C H 0.2778 1.0558 0.2646 0.098 Uiso 1 1 calc R . . C31 C 0.9131(5) 0.7340(6) 0.2076(3) 0.0668(14) Uani 1 1 d . . . H31A H 0.8798 0.6299 0.1951 0.100 Uiso 1 1 calc R . . H31B H 0.9152 0.7484 0.2571 0.100 Uiso 1 1 calc R . . H31C H 1.0078 0.7478 0.1952 0.100 Uiso 1 1 calc R . . C32 C 0.8141(4) 0.8527(6) 0.1695(2) 0.0484(11) Uani 1 1 d . . . C33 C 0.8434(4) 1.0127(6) 0.1804(2) 0.0528(12) Uani 1 1 d . . . H33A H 0.9172 1.0371 0.2155 0.063 Uiso 1 1 calc R . . C34 C 0.7758(4) 1.1385(6) 0.1453(2) 0.0510(11) Uani 1 1 d . . . C35 C 0.8322(5) 1.3010(6) 0.1601(3) 0.0692(14) Uani 1 1 d . . . H35A H 0.7738 1.3751 0.1316 0.104 Uiso 1 1 calc R . . H35B H 0.9289 1.3071 0.1496 0.104 Uiso 1 1 calc R . . H35C H 0.8301 1.3254 0.2085 0.104 Uiso 1 1 calc R . . H1 H 0.407(5) 0.754(6) -0.007(2) 0.067(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0373(3) 0.0495(4) 0.0405(3) 0.0005(3) 0.0009(2) 0.0028(3) O1 0.059(2) 0.054(2) 0.050(2) 0.0113(16) -0.0046(16) -0.0073(16) O2 0.0325(14) 0.0524(18) 0.0444(16) 0.0026(14) 0.0051(12) 0.0019(13) O3 0.0478(17) 0.072(2) 0.0460(17) 0.0025(16) 0.0063(13) 0.0066(17) O4 0.0419(16) 0.0549(19) 0.0486(18) 0.0043(14) -0.0054(14) 0.0040(14) O5 0.0516(17) 0.0504(18) 0.0487(18) 0.0023(14) -0.0069(14) 0.0003(14) C10 0.051(3) 0.053(3) 0.071(3) 0.005(3) 0.007(2) -0.002(2) C11 0.085(4) 0.069(4) 0.081(4) 0.023(3) 0.021(3) 0.003(3) C12 0.066(4) 0.099(5) 0.104(5) -0.002(4) 0.017(3) -0.003(3) C21 0.050(3) 0.100(4) 0.065(3) 0.013(3) 0.014(2) 0.033(3) C22 0.037(2) 0.046(3) 0.050(3) -0.008(2) 0.0062(19) 0.002(2) C23 0.043(2) 0.070(3) 0.049(3) -0.004(2) 0.014(2) 0.012(2) C24 0.052(3) 0.048(3) 0.046(3) -0.008(2) 0.008(2) -0.011(2) C25 0.065(3) 0.084(4) 0.048(3) -0.002(3) 0.014(2) -0.002(3) C31 0.055(3) 0.064(3) 0.076(4) 0.013(3) -0.013(2) 0.008(3) C32 0.041(2) 0.063(3) 0.041(3) 0.005(2) 0.006(2) 0.006(2) C33 0.046(3) 0.058(3) 0.050(3) -0.003(2) -0.011(2) -0.003(2) C34 0.045(3) 0.059(3) 0.047(3) -0.008(2) 0.001(2) -0.001(2) C35 0.069(3) 0.062(3) 0.072(4) -0.011(3) -0.010(3) -0.008(3) _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 2.009(3) . ? Co1 O3 2.037(3) . ? Co1 O5 2.042(3) . ? Co1 O2 2.064(3) . ? Co1 O1 2.151(3) . ? Co1 O2 2.159(3) 3_675 ? O1 C10 1.434(5) . ? O2 C22 1.288(4) . ? O2 Co1 2.159(3) 3_675 ? O3 C24 1.250(5) . ? O4 C32 1.257(5) . ? O5 C34 1.276(5) . ? C10 C12 1.484(6) . ? C10 C11 1.485(6) . ? C21 C22 1.491(6) . ? C22 C23 1.367(6) . ? C23 C24 1.394(6) . ? C24 C25 1.502(6) . ? C31 C32 1.501(6) . ? C32 C33 1.397(6) . ? C33 C34 1.377(6) . ? C34 C35 1.494(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 O3 87.13(11) . . ? O4 Co1 O5 90.16(11) . . ? O3 Co1 O5 96.00(12) . . ? O4 Co1 O2 176.90(11) . . ? O3 Co1 O2 89.82(11) . . ? O5 Co1 O2 89.61(11) . . ? O4 Co1 O1 94.06(13) . . ? O3 Co1 O1 96.61(12) . . ? O5 Co1 O1 166.88(12) . . ? O2 Co1 O1 86.84(12) . . ? O4 Co1 O2 103.03(11) . 3_675 ? O3 Co1 O2 169.57(10) . 3_675 ? O5 Co1 O2 86.45(11) . 3_675 ? O2 Co1 O2 80.04(10) . 3_675 ? O1 Co1 O2 80.50(12) . 3_675 ? C10 O1 Co1 137.4(3) . . ? C22 O2 Co1 124.7(3) . . ? C22 O2 Co1 134.9(3) . 3_675 ? Co1 O2 Co1 99.96(10) . 3_675 ? C24 O3 Co1 126.6(3) . . ? C32 O4 Co1 125.3(3) . . ? C34 O5 Co1 125.0(3) . . ? O1 C10 C12 111.7(4) . . ? O1 C10 C11 108.0(4) . . ? C12 C10 C11 114.2(5) . . ? O2 C22 C23 125.3(4) . . ? O2 C22 C21 115.7(4) . . ? C23 C22 C21 119.0(4) . . ? C22 C23 C24 128.0(4) . . ? O3 C24 C23 125.3(4) . . ? O3 C24 C25 116.4(4) . . ? C23 C24 C25 118.2(4) . . ? O4 C32 C33 125.2(4) . . ? O4 C32 C31 115.9(4) . . ? C33 C32 C31 118.8(4) . . ? C34 C33 C32 127.7(4) . . ? O5 C34 C33 124.1(4) . . ? O5 C34 C35 116.3(4) . . ? C33 C34 C35 119.6(4) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 28.96 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 0.432 _refine_diff_density_min -0.323 _refine_diff_density_rms 0.069 data_mgtics _database_code_CSD 168880 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H84 Co2 O14 Ti2' _chemical_formula_weight 1002.73 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.953(5) _cell_length_b 10.004(6) _cell_length_c 15.639(10) _cell_angle_alpha 83.275(9) _cell_angle_beta 79.323(15) _cell_angle_gamma 64.758(9) _cell_volume 1382.8(15) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 933(I>2sigma(I)) _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 18.00 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 534 _exptl_absorpt_coefficient_mu 0.919 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.7392 _exptl_absorpt_correction_T_max 0.9555 _exptl_absorpt_process_details ? _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 ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1640 _diffrn_reflns_av_R_equivalents 0.1283 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 18.00 _reflns_number_total 1639 _reflns_number_gt 933 _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^)+(0.1174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1634 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1166 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 0.838 _refine_ls_restrained_S_all 0.838 _refine_ls_shift/su_max 0.003 _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 0.2549(3) -0.1529(2) -0.26839(14) 0.0603(10) Uani 1 1 d . . . Co1 Co 0.0864(2) -0.05754(19) -0.08535(12) 0.0546(8) Uani 1 1 d . . . O1 O 0.2893(11) -0.1296(8) -0.1497(5) 0.054(3) Uani 1 1 d . . . O2 O 0.2125(10) -0.1976(10) -0.3632(6) 0.080(3) Uani 1 1 d . . . O3 O 0.4798(11) -0.2443(12) -0.3067(6) 0.073(3) Uani 1 1 d . . . O4 O 0.3000(12) -0.3714(12) -0.2227(5) 0.074(3) Uani 1 1 d . . . O5 O 0.2458(10) 0.0243(9) -0.3060(6) 0.077(3) Uani 1 1 d . . . O6 O 0.0281(8) -0.1291(9) 0.0285(5) 0.063(3) Uani 1 1 d . . . O7 O 0.0556(11) -0.0985(9) -0.1974(6) 0.065(3) Uani 1 1 d . . . C1 C 0.583(2) -0.374(3) -0.3028(11) 0.087(6) Uani 1 1 d . . . C2 C 0.4029(18) -0.6267(16) -0.1840(10) 0.125(7) Uani 1 1 d . . . H2A H 0.2995 -0.6029 -0.1605 0.187 Uiso 1 1 calc R . . H2B H 0.4629 -0.6637 -0.1379 0.187 Uiso 1 1 calc R . . H2C H 0.4365 -0.7008 -0.2264 0.187 Uiso 1 1 calc R . . C3 C 0.418(3) -0.4907(18) -0.2265(11) 0.092(6) Uani 1 1 d . . . C4 C 0.738(2) -0.3888(19) -0.3438(11) 0.133(7) Uani 1 1 d . . . H4A H 0.8081 -0.4905 -0.3399 0.200 Uiso 1 1 calc R . . H4B H 0.7676 -0.3297 -0.3138 0.200 Uiso 1 1 calc R . . H4C H 0.7371 -0.3555 -0.4039 0.200 Uiso 1 1 calc R . . C5 C 0.559(2) -0.494(2) -0.2661(12) 0.101(6) Uani 1 1 d . . . H5A H 0.6412 -0.5854 -0.2673 0.121 Uiso 1 1 calc R . . C10 C 0.269(3) 0.094(2) -0.3808(13) 0.121(7) Uani 1 1 d . . . H10A H 0.2857 0.0280 -0.4271 0.145 Uiso 1 1 calc R . . C11 C 0.400(3) 0.125(3) -0.3915(14) 0.220(13) Uani 1 1 d . . . H11A H 0.4876 0.0338 -0.3867 0.330 Uiso 1 1 calc R . . H11B H 0.3888 0.1891 -0.3472 0.330 Uiso 1 1 calc R . . H11C H 0.4118 0.1716 -0.4479 0.330 Uiso 1 1 calc R . . C12 C 0.152(3) 0.231(3) -0.3999(18) 0.31(2) Uani 1 1 d . . . H12A H 0.0626 0.2169 -0.4008 0.458 Uiso 1 1 calc R . . H12B H 0.1807 0.2701 -0.4558 0.458 Uiso 1 1 calc R . . H12C H 0.1325 0.2992 -0.3560 0.458 Uiso 1 1 calc R . . C20 C -0.071(2) -0.1020(19) -0.2228(10) 0.099(6) Uani 1 1 d . . . H20A H -0.0361 -0.1445 -0.2804 0.119 Uiso 1 1 calc R . . C21 C -0.184(2) 0.038(2) -0.2357(17) 0.235(15) Uani 1 1 d . . . H21A H -0.1415 0.0991 -0.2711 0.353 Uiso 1 1 calc R . . H21B H -0.2319 0.0812 -0.1804 0.353 Uiso 1 1 calc R . . H21C H -0.2573 0.0291 -0.2644 0.353 Uiso 1 1 calc R . . C22 C -0.122(3) -0.207(3) -0.1661(14) 0.214(13) Uani 1 1 d . . . H22A H -0.0383 -0.3017 -0.1627 0.320 Uiso 1 1 calc R . . H22B H -0.1983 -0.2187 -0.1904 0.320 Uiso 1 1 calc R . . H22C H -0.1623 -0.1699 -0.1089 0.320 Uiso 1 1 calc R . . C30 C 0.265(4) -0.314(3) -0.4296(17) 0.242(16) Uani 1 1 d . . . H30A H 0.3622 -0.3957 -0.4224 0.290 Uiso 1 1 calc R . . C31 C 0.267(4) -0.236(4) -0.507(2) 0.322(19) Uiso 1 1 d . . . H31A H 0.2986 -0.3018 -0.5544 0.483 Uiso 1 1 calc R . . H31B H 0.3355 -0.1907 -0.5106 0.483 Uiso 1 1 calc R . . H31C H 0.1679 -0.1609 -0.5119 0.483 Uiso 1 1 calc R . . C32 C 0.157(3) -0.356(3) -0.4198(17) 0.249(14) Uiso 1 1 d . . . H32A H 0.1823 -0.4338 -0.4588 0.373 Uiso 1 1 calc R . . H32B H 0.0664 -0.2742 -0.4325 0.373 Uiso 1 1 calc R . . H32C H 0.1411 -0.3925 -0.3609 0.373 Uiso 1 1 calc R . . C40 C 0.057(3) -0.269(2) 0.0617(11) 0.202(13) Uani 1 1 d . . . H40 H -0.0347 -0.2673 0.0460 0.243 Uiso 1 1 calc R . . C41 C 0.0155(19) -0.2941(18) 0.1487(11) 0.132(6) Uiso 1 1 d . . . H41A H -0.0519 -0.2019 0.1743 0.198 Uiso 1 1 calc R . . H41B H 0.1032 -0.3381 0.1770 0.198 Uiso 1 1 calc R . . H41C H -0.0338 -0.3597 0.1555 0.198 Uiso 1 1 calc R . . C42 C 0.1530(19) -0.3880(18) 0.0055(11) 0.123(6) Uiso 1 1 d . . . H42A H 0.1627 -0.4807 0.0349 0.184 Uiso 1 1 calc R . . H42B H 0.2503 -0.3863 -0.0095 0.184 Uiso 1 1 calc R . . H42C H 0.1101 -0.3762 -0.0466 0.184 Uiso 1 1 calc R . . C50 C 0.4156(19) -0.1279(16) -0.1253(9) 0.067(4) Uani 1 1 d . . . H50A H 0.4934 -0.1528 -0.1767 0.081 Uiso 1 1 calc R . . C52 C 0.3915(18) 0.0190(18) -0.1003(12) 0.135(7) Uani 1 1 d . . . H52A H 0.3559 0.0905 -0.1466 0.202 Uiso 1 1 calc R . . H52B H 0.4846 0.0159 -0.0892 0.202 Uiso 1 1 calc R . . H52C H 0.3184 0.0463 -0.0486 0.202 Uiso 1 1 calc R . . C51 C 0.4786(18) -0.2403(18) -0.0549(12) 0.142(7) Uani 1 1 d . . . H51A H 0.4979 -0.3367 -0.0720 0.214 Uiso 1 1 calc R . . H51B H 0.4077 -0.2171 -0.0021 0.214 Uiso 1 1 calc R . . H51C H 0.5707 -0.2394 -0.0453 0.214 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 Ti1 0.057(2) 0.066(2) 0.055(2) -0.0075(15) -0.0078(15) -0.0221(15) Co1 0.0530(16) 0.0576(13) 0.0503(13) -0.0082(9) -0.0033(9) -0.0203(10) O1 0.057(9) 0.077(6) 0.047(6) -0.006(4) -0.022(6) -0.040(5) O2 0.080(8) 0.105(8) 0.069(7) -0.030(6) -0.021(6) -0.039(6) O3 0.051(9) 0.075(8) 0.085(8) -0.017(6) -0.012(6) -0.013(6) O4 0.073(9) 0.059(7) 0.085(7) -0.006(5) -0.003(6) -0.026(6) O5 0.089(8) 0.066(6) 0.064(7) 0.022(5) 0.001(5) -0.032(5) O6 0.077(8) 0.052(6) 0.064(6) 0.008(5) 0.001(5) -0.037(5) O7 0.054(9) 0.084(7) 0.065(7) -0.004(5) -0.026(6) -0.030(6) C1 0.069(19) 0.096(17) 0.070(12) -0.028(12) -0.008(11) -0.002(16) C2 0.164(19) 0.061(12) 0.131(15) 0.005(11) -0.007(12) -0.038(11) C3 0.12(2) 0.052(14) 0.082(13) -0.015(10) -0.013(13) -0.013(14) C4 0.090(18) 0.153(18) 0.117(15) -0.035(12) -0.007(13) -0.008(13) C5 0.09(2) 0.072(15) 0.104(15) -0.007(11) 0.006(12) -0.007(13) C10 0.17(2) 0.094(15) 0.118(18) 0.028(13) -0.035(16) -0.077(15) C11 0.25(4) 0.30(3) 0.18(2) 0.08(2) -0.05(2) -0.19(3) C12 0.21(3) 0.32(4) 0.32(4) 0.24(3) -0.07(3) -0.09(3) C20 0.086(19) 0.108(14) 0.070(12) -0.022(10) -0.038(12) 0.006(13) C21 0.10(2) 0.15(2) 0.46(5) -0.02(2) -0.15(2) -0.016(15) C22 0.28(3) 0.32(3) 0.16(2) 0.08(2) -0.08(2) -0.24(3) C30 0.40(4) 0.32(4) 0.19(3) 0.11(3) -0.22(3) -0.29(4) C40 0.34(3) 0.090(15) 0.073(14) -0.018(11) 0.128(17) -0.049(16) C50 0.071(16) 0.076(12) 0.054(11) -0.017(9) 0.008(9) -0.033(10) C52 0.117(18) 0.104(15) 0.21(2) 0.000(14) -0.086(15) -0.053(12) C51 0.137(19) 0.134(16) 0.18(2) 0.031(15) -0.097(16) -0.060(13) _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 O2 1.768(10) . ? Ti1 O5 1.770(9) . ? Ti1 O7 1.966(10) . ? Ti1 O1 2.005(9) . ? Ti1 O3 2.023(10) . ? Ti1 O4 2.099(10) . ? Ti1 Co1 3.068(4) . ? Co1 O6 1.921(8) . ? Co1 O6 1.943(8) 2 ? Co1 O7 1.952(9) . ? Co1 O1 1.945(9) . ? Co1 Co1 2.957(4) 2 ? O1 C50 1.387(15) . ? O2 C30 1.51(3) . ? O3 C1 1.269(17) . ? O4 C3 1.266(17) . ? O5 C10 1.325(17) . ? O6 C40 1.365(16) . ? O6 Co1 1.943(8) 2 ? O7 C20 1.407(18) . ? C1 C5 1.37(2) . ? C1 C4 1.51(2) . ? C2 C3 1.498(19) . ? C3 C5 1.41(2) . ? C10 C11 1.44(2) . ? C10 C12 1.42(2) . ? C20 C21 1.39(2) . ? C20 C22 1.49(2) . ? C30 C32 1.29(3) . ? C30 C31 1.37(3) . ? C40 C41 1.372(18) . ? C40 C42 1.435(19) . ? C50 C52 1.473(16) . ? C50 C51 1.495(17) . ? 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 O2 Ti1 O5 97.2(4) . . ? O2 Ti1 O7 97.7(4) . . ? O5 Ti1 O7 100.6(4) . . ? O2 Ti1 O1 169.4(4) . . ? O5 Ti1 O1 92.6(4) . . ? O7 Ti1 O1 76.4(4) . . ? O2 Ti1 O3 94.6(4) . . ? O5 Ti1 O3 90.6(4) . . ? O7 Ti1 O3 162.2(4) . . ? O1 Ti1 O3 89.4(4) . . ? O2 Ti1 O4 86.9(4) . . ? O5 Ti1 O4 171.3(4) . . ? O7 Ti1 O4 86.4(4) . . ? O1 Ti1 O4 84.0(3) . . ? O3 Ti1 O4 81.4(4) . . ? O2 Ti1 Co1 135.9(3) . . ? O5 Ti1 Co1 95.1(3) . . ? O7 Ti1 Co1 38.3(3) . . ? O1 Ti1 Co1 38.4(3) . . ? O3 Ti1 Co1 127.5(3) . . ? O4 Ti1 Co1 87.2(3) . . ? O6 Co1 O6 80.2(4) . 2 ? O6 Co1 O7 127.9(4) . . ? O6 Co1 O7 124.1(4) 2 . ? O6 Co1 O1 125.6(3) . . ? O6 Co1 O1 128.2(3) 2 . ? O7 Co1 O1 78.1(4) . . ? O6 Co1 Co1 40.4(2) . 2 ? O6 Co1 Co1 39.8(2) 2 2 ? O7 Co1 Co1 140.2(3) . 2 ? O1 Co1 Co1 141.7(3) . 2 ? O6 Co1 Ti1 143.9(3) . . ? O6 Co1 Ti1 135.9(2) 2 . ? O7 Co1 Ti1 38.6(3) . . ? O1 Co1 Ti1 39.8(3) . . ? Co1 Co1 Ti1 175.63(11) 2 . ? C50 O1 Co1 127.5(8) . . ? C50 O1 Ti1 128.7(8) . . ? Co1 O1 Ti1 101.9(5) . . ? C30 O2 Ti1 143.7(12) . . ? C1 O3 Ti1 134.6(13) . . ? C3 O4 Ti1 133.7(12) . . ? C10 O5 Ti1 138.4(10) . . ? C40 O6 Co1 131.1(8) . . ? C40 O6 Co1 129.0(8) . 2 ? Co1 O6 Co1 99.8(4) . 2 ? C20 O7 Ti1 126.3(9) . . ? C20 O7 Co1 130.4(9) . . ? Ti1 O7 Co1 103.1(5) . . ? O3 C1 C5 124.0(18) . . ? O3 C1 C4 115(2) . . ? C5 C1 C4 121.1(18) . . ? O4 C3 C5 121.5(16) . . ? O4 C3 C2 117(2) . . ? C5 C3 C2 121.3(18) . . ? C1 C5 C3 124.8(17) . . ? O5 C10 C11 114.4(19) . . ? O5 C10 C12 116.9(19) . . ? C11 C10 C12 104.6(19) . . ? O7 C20 C21 113.5(18) . . ? O7 C20 C22 111.7(14) . . ? C21 C20 C22 115(2) . . ? C32 C30 C31 109(2) . . ? C32 C30 O2 104(3) . . ? C31 C30 O2 103(3) . . ? O6 C40 C41 120.3(15) . . ? O6 C40 C42 116.8(12) . . ? C41 C40 C42 122.0(17) . . ? O1 C50 C52 113.1(12) . . ? O1 C50 C51 114.0(12) . . ? C52 C50 C51 109.3(14) . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 18.00 _diffrn_measured_fraction_theta_full 0.857 _refine_diff_density_max 0.285 _refine_diff_density_min -0.292 _refine_diff_density_rms 0.056 data_cotapr1m _database_code_CSD 189538 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H98 Co2 O14 Ta2' _chemical_formula_weight 1306.96 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' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.586(6) _cell_length_b 10.551(6) _cell_length_c 15.938(10) _cell_angle_alpha 83.624(15) _cell_angle_beta 78.361(13) _cell_angle_gamma 68.940(14) _cell_volume 1472.0(16) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1202(I>2sigma(I)) _cell_measurement_theta_min 1.31 _cell_measurement_theta_max 20.00 _exptl_crystal_description flake _exptl_crystal_colour pink _exptl_crystal_size_max 1.10 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 662 _exptl_absorpt_coefficient_mu 4.308 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0878 _exptl_absorpt_correction_T_max 0.8134 _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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3813 _diffrn_reflns_av_R_equivalents 0.1055 _diffrn_reflns_av_sigmaI/netI 0.3139 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2667 _reflns_number_gt 1194 _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^)+(0.0837P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2667 _refine_ls_number_parameters 167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1790 _refine_ls_R_factor_gt 0.0827 _refine_ls_wR_factor_ref 0.1893 _refine_ls_wR_factor_gt 0.1671 _refine_ls_goodness_of_fit_ref 0.829 _refine_ls_restrained_S_all 0.829 _refine_ls_shift/su_max 0.981 _refine_ls_shift/su_mean 0.006 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 Ta1 Ta -0.09716(17) -0.21820(14) 0.26567(11) 0.0530(8) Uani 1 1 d . . . Co1 Co -0.0314(5) -0.0694(4) 0.0839(3) 0.0572(13) Uani 1 1 d . . . O1 O -0.136(2) -0.1865(18) 0.1460(12) 0.065(6) Uani 1 1 d . . . O2 O 0.017(2) -0.107(2) 0.2003(12) 0.092(8) Uani 1 1 d . . . O3 O -0.229(2) -0.318(2) 0.2982(12) 0.078(7) Uani 1 1 d . . . O4 O -0.017(3) -0.232(2) 0.353(2) 0.119(11) Uani 1 1 d . . . O5 O -0.254(2) -0.0510(19) 0.2972(17) 0.107(9) Uani 1 1 d . . . O6 O -0.102(2) 0.1064(16) 0.0253(12) 0.074(6) Uani 1 1 d . . . O7 O 0.070(2) -0.380(2) 0.2244(17) 0.117(9) Uani 1 1 d . . . C1 C -0.246(5) -0.227(4) 0.117(2) 0.105(13) Uiso 1 1 d . . . H1A H -0.3103 -0.2559 0.1658 0.126 Uiso 1 1 calc R . . C11 C -0.340(6) -0.116(5) 0.061(3) 0.22(2) Uiso 1 1 d . . . H11A H -0.4062 -0.0413 0.0958 0.331 Uiso 1 1 calc R . . H11B H -0.4002 -0.1516 0.0356 0.331 Uiso 1 1 calc R . . H11C H -0.2742 -0.0850 0.0171 0.331 Uiso 1 1 calc R . . C12 C -0.154(5) -0.343(4) 0.060(3) 0.18(2) Uiso 1 1 d . . . H12A H -0.0925 -0.4168 0.0919 0.272 Uiso 1 1 calc R . . H12B H -0.0893 -0.3128 0.0138 0.272 Uiso 1 1 calc R . . H12C H -0.2208 -0.3728 0.0361 0.272 Uiso 1 1 calc R . . C2 C 0.123(4) -0.052(3) 0.235(2) 0.086(11) Uiso 1 1 d . . . H2A H 0.1547 -0.1087 0.2854 0.103 Uiso 1 1 calc R . . C21 C 0.261(7) -0.070(5) 0.167(3) 0.24(3) Uiso 1 1 d . . . H21A H 0.3298 -0.0376 0.1874 0.359 Uiso 1 1 calc R . . H21B H 0.2316 -0.0183 0.1162 0.359 Uiso 1 1 calc R . . H21C H 0.3095 -0.1640 0.1552 0.359 Uiso 1 1 calc R . . C22 C 0.033(5) 0.090(4) 0.264(3) 0.19(2) Uiso 1 1 d . . . H22A H -0.0463 0.0872 0.3107 0.278 Uiso 1 1 calc R . . H22B H -0.0102 0.1449 0.2171 0.278 Uiso 1 1 calc R . . H22C H 0.0991 0.1274 0.2820 0.278 Uiso 1 1 calc R . . C3 C -0.283(8) -0.428(7) 0.328(5) 0.23(3) Uiso 1 1 d . . . H3A H -0.3799 -0.3803 0.3078 0.278 Uiso 1 1 calc R . . C31 C -0.262(8) -0.521(7) 0.293(4) 0.30(4) Uiso 1 1 d . . . H31A H -0.3295 -0.5671 0.3217 0.444 Uiso 1 1 calc R . . H31B H -0.1589 -0.5802 0.2920 0.444 Uiso 1 1 calc R . . H31C H -0.2797 -0.4955 0.2353 0.444 Uiso 1 1 calc R . . C32 C -0.360(7) -0.402(6) 0.425(4) 0.26(3) Uiso 1 1 d . . . H32A H -0.4140 -0.4639 0.4453 0.393 Uiso 1 1 calc R . . H32B H -0.4302 -0.3103 0.4305 0.393 Uiso 1 1 calc R . . H32C H -0.2835 -0.4164 0.4593 0.393 Uiso 1 1 calc R . . C4 C -0.032(5) -0.218(4) 0.420(3) 0.108(17) Uiso 1 1 d . . . H4 H -0.1012 -0.1230 0.4207 0.130 Uiso 1 1 calc R . . C41 C -0.097(6) -0.266(5) 0.509(3) 0.21(2) Uiso 1 1 d . . . H41A H -0.1867 -0.2842 0.5066 0.316 Uiso 1 1 calc R . . H41B H -0.1215 -0.1956 0.5493 0.316 Uiso 1 1 calc R . . H41C H -0.0223 -0.3467 0.5282 0.316 Uiso 1 1 calc R . . C42 C 0.096(6) -0.199(5) 0.459(3) 0.20(2) Uiso 1 1 d . . . H42A H 0.1620 -0.1678 0.4151 0.295 Uiso 1 1 calc R . . H42B H 0.1536 -0.2843 0.4840 0.295 Uiso 1 1 calc R . . H42C H 0.0511 -0.1332 0.5029 0.295 Uiso 1 1 calc R . . C5 C -0.366(5) -0.001(4) 0.368(2) 0.106(13) Uiso 1 1 d . . . H5A H -0.3448 -0.0626 0.4182 0.127 Uiso 1 1 calc R . . C51 C -0.389(5) 0.124(4) 0.386(2) 0.146(16) Uiso 1 1 d . . . H51A H -0.2998 0.1273 0.4030 0.220 Uiso 1 1 calc R . . H51B H -0.4738 0.1535 0.4317 0.220 Uiso 1 1 calc R . . H51C H -0.4094 0.1831 0.3360 0.220 Uiso 1 1 calc R . . C52 C -0.506(6) 0.002(5) 0.344(3) 0.20(2) Uiso 1 1 d . . . H52A H -0.5880 0.0327 0.3912 0.305 Uiso 1 1 calc R . . H52B H -0.4953 -0.0882 0.3307 0.305 Uiso 1 1 calc R . . H52C H -0.5260 0.0622 0.2951 0.305 Uiso 1 1 calc R . . C6 C -0.214(6) 0.224(5) 0.065(3) 0.157(18) Uiso 1 1 d . . . H6 H -0.1508 0.2566 0.0927 0.188 Uiso 1 1 calc R . . C61 C -0.328(6) 0.220(5) 0.135(3) 0.18(2) Uiso 1 1 d . . . H61A H -0.3924 0.3109 0.1493 0.269 Uiso 1 1 calc R . . H61B H -0.2827 0.1735 0.1832 0.269 Uiso 1 1 calc R . . H61C H -0.3874 0.1723 0.1195 0.269 Uiso 1 1 calc R . . C62 C -0.248(7) 0.326(5) -0.002(3) 0.22(3) Uiso 1 1 d . . . H62A H -0.1603 0.3116 -0.0463 0.337 Uiso 1 1 calc R . . H62B H -0.2778 0.4140 0.0202 0.337 Uiso 1 1 calc R . . H62C H -0.3301 0.3193 -0.0258 0.337 Uiso 1 1 calc R . . C7 C 0.166(6) -0.509(5) 0.262(3) 0.157(19) Uiso 1 1 d . . . H7A H 0.1179 -0.5381 0.3172 0.189 Uiso 1 1 calc R . . C71 C 0.195(5) -0.601(4) 0.192(3) 0.174(19) Uiso 1 1 d . . . H71A H 0.2589 -0.6900 0.2075 0.261 Uiso 1 1 calc R . . H71B H 0.2436 -0.5672 0.1406 0.261 Uiso 1 1 calc R . . H71C H 0.1001 -0.6043 0.1832 0.261 Uiso 1 1 calc R . . C72 C 0.314(9) -0.501(8) 0.261(5) 0.35(4) Uiso 1 1 d . . . H72A H 0.3076 -0.4450 0.3064 0.530 Uiso 1 1 calc R . . H72B H 0.3480 -0.4619 0.2070 0.530 Uiso 1 1 calc R . . H72C H 0.3858 -0.5905 0.2696 0.530 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 Ta1 0.0387(10) 0.0476(9) 0.0728(14) -0.0033(7) -0.0118(7) -0.0137(7) Co1 0.042(3) 0.055(3) 0.072(3) -0.009(2) -0.015(2) -0.009(2) O1 0.033(13) 0.080(15) 0.084(17) -0.045(12) 0.025(12) -0.030(12) O2 0.076(18) 0.14(2) 0.038(15) -0.019(13) 0.026(13) -0.022(15) O3 0.057(16) 0.117(18) 0.065(16) 0.012(13) -0.021(12) -0.036(14) O4 0.17(3) 0.11(2) 0.07(2) 0.011(17) -0.02(2) -0.046(19) O5 0.027(14) 0.080(16) 0.20(3) -0.083(17) 0.028(16) -0.001(12) O6 0.071(16) 0.021(11) 0.100(17) -0.010(11) 0.001(13) 0.015(11) O7 0.051(17) 0.049(15) 0.23(3) -0.055(16) -0.033(18) 0.025(12) _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 Ta1 O4 1.69(3) . ? Ta1 O3 1.88(2) . ? Ta1 O5 1.902(18) . ? Ta1 O7 1.939(19) . ? Ta1 O2 1.96(2) . ? Ta1 O1 1.99(2) . ? Co1 O6 1.926(19) 2 ? Co1 O6 1.934(17) . ? Co1 O1 1.934(17) . ? Co1 O2 1.97(2) . ? Co1 Co1 2.963(8) 2 ? O1 C1 1.43(4) . ? O2 C2 1.54(4) . ? O3 C3 1.43(6) . ? O4 C4 1.06(4) . ? O5 C5 1.39(4) . ? O6 C6 1.43(5) . ? O6 Co1 1.926(19) 2 ? O7 C7 1.49(5) . ? C1 C12 1.50(5) . ? C1 C11 1.53(5) . ? C2 C22 1.50(5) . ? C2 C21 1.50(5) . ? C3 C31 1.12(8) . ? C3 C32 1.59(7) . ? C4 C41 1.54(5) . ? C4 C42 1.57(5) . ? C5 C51 1.32(4) . ? C5 C52 1.45(5) . ? C6 C61 1.40(5) . ? C6 C62 1.43(5) . ? C7 C72 1.46(8) . ? C7 C71 1.46(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Ta1 O3 103.8(10) . . ? O4 Ta1 O5 94.0(13) . . ? O3 Ta1 O5 92.7(9) . . ? O4 Ta1 O7 88.2(12) . . ? O3 Ta1 O7 91.4(10) . . ? O5 Ta1 O7 174.7(12) . . ? O4 Ta1 O2 93.0(11) . . ? O3 Ta1 O2 163.2(9) . . ? O5 Ta1 O2 86.2(9) . . ? O7 Ta1 O2 88.9(9) . . ? O4 Ta1 O1 162.5(10) . . ? O3 Ta1 O1 92.9(7) . . ? O5 Ta1 O1 90.5(10) . . ? O7 Ta1 O1 85.9(10) . . ? O2 Ta1 O1 70.4(8) . . ? O6 Co1 O6 79.7(8) 2 . ? O6 Co1 O1 125.2(7) 2 . ? O6 Co1 O1 132.4(9) . . ? O6 Co1 O2 129.7(9) 2 . ? O6 Co1 O2 127.0(9) . . ? O1 Co1 O2 71.5(9) . . ? O6 Co1 Co1 40.0(5) 2 2 ? O6 Co1 Co1 39.8(6) . 2 ? O1 Co1 Co1 144.6(6) . 2 ? O2 Co1 Co1 143.9(7) . 2 ? C1 O1 Co1 127(2) . . ? C1 O1 Ta1 123.4(19) . . ? Co1 O1 Ta1 109.2(9) . . ? C2 O2 Ta1 126.0(18) . . ? C2 O2 Co1 125.1(18) . . ? Ta1 O2 Co1 108.8(12) . . ? C3 O3 Ta1 161(3) . . ? C4 O4 Ta1 148(4) . . ? C5 O5 Ta1 137(2) . . ? C6 O6 Co1 136(2) . 2 ? C6 O6 Co1 124(2) . . ? Co1 O6 Co1 100.3(8) 2 . ? C7 O7 Ta1 137(3) . . ? O1 C1 C12 105(3) . . ? O1 C1 C11 112(3) . . ? C12 C1 C11 106(3) . . ? C22 C2 C21 117(4) . . ? C22 C2 O2 109(3) . . ? C21 C2 O2 107(3) . . ? C31 C3 O3 127(8) . . ? C31 C3 C32 126(8) . . ? O3 C3 C32 106(6) . . ? O4 C4 C41 143(5) . . ? O4 C4 C42 121(5) . . ? C41 C4 C42 89(4) . . ? C51 C5 O5 115(3) . . ? C51 C5 C52 106(4) . . ? O5 C5 C52 105(3) . . ? C61 C6 C62 120(5) . . ? C61 C6 O6 124(4) . . ? C62 C6 O6 106(4) . . ? C72 C7 C71 103(5) . . ? C72 C7 O7 108(5) . . ? C71 C7 O7 100(4) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.856 _refine_diff_density_min -1.286 _refine_diff_density_rms 0.177 data_ninb3cs _database_code_CSD 189539 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 Nb2 Ni O12' _chemical_formula_weight 953.56 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.509(7) _cell_length_b 9.536(2) _cell_length_c 18.973(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.790(4) _cell_angle_gamma 90.00 _cell_volume 5083(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 995(I>2sigma(I)) _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 20.00 _exptl_crystal_description needle _exptl_crystal_colour 'bluish violet' _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.5473 _exptl_absorpt_correction_T_max 0.8823 _exptl_absorpt_process_details ? _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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6252 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2303 _reflns_number_gt 1427 _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^)+(0.1271P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2303 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.005 _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 0.0000 0.3207(2) 0.2500 0.0904(7) Uani 1 2 d S . . Nb1 Nb 0.11085(3) 0.31922(12) 0.26346(5) 0.0855(6) Uani 1 1 d . . . O1 O 0.0576(5) 0.2206(13) 0.3039(7) 0.080(4) Uani 0.502(6) 1 d P . . O2 O 0.0452(5) 0.406(2) 0.2113(8) 0.106(6) Uani 0.502(6) 1 d P . . O3 O 0.0449(4) 0.2420(16) 0.2051(7) 0.075(4) Uani 0.498(6) 1 d P . . O4 O 0.0587(4) 0.4136(16) 0.3066(8) 0.094(5) Uani 0.498(6) 1 d P . . O5 O 0.1205(6) 0.1898(19) 0.3293(9) 0.111(6) Uani 0.498(6) 1 d P . . O6 O 0.1234(7) 0.437(2) 0.3366(8) 0.107(5) Uani 0.502(6) 1 d P . . O7 O 0.0979(6) 0.169(2) 0.1900(9) 0.127(6) Uani 0.502(6) 1 d P . . O8 O 0.1573(6) 0.1851(18) 0.3257(9) 0.116(6) Uani 0.502(6) 1 d P . . O9 O 0.1600(6) 0.4359(19) 0.3312(9) 0.114(6) Uani 0.498(6) 1 d P . . O10 O 0.1013(6) 0.4780(18) 0.1982(7) 0.106(5) Uani 0.498(6) 1 d P . . O11 O 0.1445(6) 0.4166(19) 0.2141(9) 0.112(5) Uani 0.502(6) 1 d P . . O12 O 0.1430(6) 0.230(2) 0.2080(8) 0.108(6) Uani 0.498(6) 1 d P . . C1A C 0.0596(11) 0.119(4) 0.3538(17) 0.133(10) Uiso 0.502(6) 1 d P . . C1B C 0.0791(12) 0.160(3) 0.4323(19) 0.170(12) Uiso 0.502(6) 1 d P . . C1C C 0.0660(16) -0.028(5) 0.334(2) 0.230(18) Uiso 0.502(6) 1 d P . . C2A C 0.0367(11) 0.507(4) 0.1611(19) 0.145(11) Uiso 0.502(6) 1 d P . . C2B C 0.0199(17) 0.464(6) 0.090(3) 0.26(2) Uiso 0.502(6) 1 d P . . C2C C -0.001(2) 0.614(7) 0.175(3) 0.31(3) Uiso 0.502(6) 1 d P . . C3A C 0.0346(10) 0.149(3) 0.1500(15) 0.116(9) Uiso 0.498(6) 1 d P . . C3B C 0.0333(11) 0.199(3) 0.0730(17) 0.146(10) Uiso 0.498(6) 1 d P . . C3C C -0.0057(17) 0.034(5) 0.158(2) 0.228(18) Uiso 0.498(6) 1 d P . . C4A C 0.0612(13) 0.502(4) 0.361(2) 0.157(12) Uiso 0.498(6) 1 d P . . C4B C 0.0814(13) 0.460(4) 0.437(2) 0.190(14) Uiso 0.498(6) 1 d P . . C4C C 0.074(3) 0.622(9) 0.350(5) 0.36(4) Uiso 0.498(6) 1 d P . . C5A C 0.1324(19) 0.027(6) 0.358(3) 0.25(2) Uiso 0.498(6) 1 d P . . C5B C 0.183(3) 0.012(9) 0.359(5) 0.36(4) Uiso 0.498(6) 1 d P . . C5C C 0.1385(17) 0.042(6) 0.443(3) 0.27(2) Uiso 0.498(6) 1 d P . . C6A C 0.136(3) 0.580(7) 0.365(4) 0.29(3) Uiso 0.502(6) 1 d P . . C6B C 0.194(2) 0.623(6) 0.382(4) 0.28(3) Uiso 0.502(6) 1 d P . . C6C C 0.145(2) 0.567(7) 0.456(3) 0.32(3) Uiso 0.502(6) 1 d P . . C7A C 0.099(2) 0.045(8) 0.148(4) 0.27(2) Uiso 0.502(6) 1 d P . . C7B C 0.125(3) -0.062(9) 0.176(4) 0.36(4) Uiso 0.502(6) 1 d P . . C7C C 0.0721(18) 0.061(6) 0.067(3) 0.28(2) Uiso 0.502(6) 1 d P . . C8A C 0.1986(14) 0.183(4) 0.390(2) 0.175(13) Uiso 0.502(6) 1 d P . . C8B C 0.2045(12) 0.042(4) 0.429(2) 0.186(13) Uiso 0.502(6) 1 d P . . C8C C 0.2437(14) 0.255(5) 0.3743(19) 0.172(13) Uiso 0.502(6) 1 d P . . C9A C 0.1988(12) 0.431(4) 0.3957(17) 0.147(10) Uiso 0.498(6) 1 d P . . C9B C 0.2058(12) 0.565(4) 0.438(2) 0.170(12) Uiso 0.498(6) 1 d P . . C9C C 0.2431(13) 0.368(4) 0.3751(18) 0.164(13) Uiso 0.498(6) 1 d P . . C10A C 0.1085(18) 0.602(6) 0.169(3) 0.214(18) Uiso 0.498(6) 1 d P . . C10B C 0.073(2) 0.662(6) 0.092(4) 0.31(3) Uiso 0.498(6) 1 d P . . C10C C 0.135(3) 0.699(10) 0.203(5) 0.40(5) Uiso 0.498(6) 1 d P . . C11A C 0.1637(14) 0.434(5) 0.150(2) 0.188(13) Uiso 0.502(6) 1 d P . . C11B C 0.2144(17) 0.362(5) 0.191(2) 0.20(2) Uiso 0.502(6) 1 d P . . C11C C 0.1587(13) 0.569(5) 0.126(2) 0.197(14) Uiso 0.502(6) 1 d P . . C12A C 0.1648(14) 0.233(4) 0.149(2) 0.163(12) Uiso 0.498(6) 1 d P . . C12B C 0.1571(13) 0.096(4) 0.112(2) 0.193(14) Uiso 0.498(6) 1 d P . . C12C C 0.2112(12) 0.289(4) 0.1729(17) 0.126(11) Uiso 0.498(6) 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 Ni1 0.0548(11) 0.1201(16) 0.0999(14) 0.000 0.0292(10) 0.000 Nb1 0.0569(7) 0.1144(9) 0.0883(8) -0.0040(8) 0.0267(5) 0.0013(6) O1 0.086(9) 0.065(11) 0.095(10) 0.017(8) 0.039(7) 0.003(7) O2 0.067(9) 0.157(19) 0.095(11) 0.043(12) 0.025(8) 0.006(10) O3 0.070(9) 0.066(10) 0.080(9) -0.033(7) 0.010(7) -0.010(7) O4 0.061(8) 0.118(14) 0.097(11) -0.032(10) 0.014(7) -0.002(8) O5 0.068(10) 0.136(14) 0.135(13) 0.021(12) 0.040(10) 0.042(11) O6 0.099(13) 0.129(15) 0.110(11) 0.014(11) 0.055(10) 0.007(12) O7 0.115(14) 0.135(14) 0.129(13) -0.032(12) 0.036(10) 0.010(12) O8 0.074(11) 0.113(12) 0.136(13) -0.025(11) -0.004(10) 0.035(11) O9 0.067(10) 0.120(14) 0.140(14) -0.015(11) 0.010(11) -0.018(11) O10 0.103(12) 0.114(13) 0.100(10) 0.048(10) 0.030(9) 0.023(10) O11 0.087(12) 0.137(17) 0.130(12) 0.020(11) 0.062(10) -0.010(11) O12 0.084(11) 0.150(18) 0.107(11) -0.018(11) 0.052(9) -0.005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.890(14) . ? Ni1 O2 1.890(14) 2 ? Ni1 O3 1.933(13) 2 ? Ni1 O3 1.933(13) . ? Ni1 O1 1.944(12) . ? Ni1 O1 1.944(12) 2 ? Ni1 O4 1.949(12) . ? Ni1 O4 1.949(12) 2 ? Nb1 O5 1.717(17) . ? Nb1 O6 1.734(18) . ? Nb1 O11 1.814(14) . ? Nb1 O12 1.830(15) . ? Nb1 O10 1.922(15) . ? Nb1 O9 1.964(15) . ? Nb1 O7 1.955(18) . ? Nb1 O8 1.979(16) . ? Nb1 O2 2.059(14) . ? Nb1 O3 2.059(12) . ? Nb1 O4 2.149(14) . ? Nb1 O1 2.164(13) . ? O1 C1A 1.34(3) . ? O1 O3 1.807(19) . ? O1 O5 1.79(2) . ? O2 C2A 1.33(3) . ? O2 O3 1.56(2) . ? O2 O4 1.73(2) . ? O3 C3A 1.33(3) . ? O4 C4A 1.32(4) . ? O4 O6 1.83(2) . ? O5 O8 1.109(18) . ? O5 C5A 1.65(5) . ? O6 O9 1.117(17) . ? O6 C6A 1.48(7) . ? O7 O12 1.40(2) . ? O7 C7A 1.42(6) . ? O7 C3A 1.80(3) . ? O8 C8A 1.44(4) . ? O8 C5A 1.86(6) . ? O8 C5B 1.85(8) . ? O9 C9A 1.40(3) . ? O9 C6A 1.76(7) . ? O10 O11 1.350(18) . ? O10 C10A 1.35(5) . ? O10 C2A 1.84(4) . ? O11 C11A 1.50(4) . ? O11 O12 1.79(2) . ? O12 C12A 1.46(4) . ? C1A C1B 1.48(4) . ? C1A C1C 1.48(5) . ? C1A C3C 1.74(5) 2 ? C2A C2B 1.35(5) . ? C2A C2C 1.59(6) . ? C3A C3C 1.66(5) . ? C3A C3B 1.53(4) . ? C3B C7C 1.78(6) . ? C3C C1A 1.74(5) 2 ? C4A C4C 1.23(8) . ? C4A C4B 1.45(4) . ? C4B C6C 2.07(6) . ? C4C C6A 1.82(8) . ? C5A C5B 1.50(8) . ? C5A C5C 1.56(6) . ? C5B C8B 1.33(8) . ? C5B C8A 1.75(8) . ? C5C C8B 2.04(6) . ? C6A C6C 1.67(7) . ? C6A C6B 1.67(7) . ? C6A C9B 2.10(8) . ? C6A C9A 2.26(7) . ? C6B C9B 1.14(6) . ? C6B C9A 1.85(7) . ? C6C C9B 1.93(6) . ? C7A C7B 1.29(8) . ? C7A C7C 1.52(6) . ? C8A C8B 1.52(5) . ? C8A C8C 1.60(5) . ? C8C C9C 1.08(4) . ? C9A C9B 1.49(4) . ? C9A C9C 1.59(4) . ? C10A C10C 1.25(9) . ? C10A C10B 1.62(7) . ? C10A C11C 1.93(5) . ? C11A C11C 1.36(5) . ? C11A C11B 1.61(5) . ? C11A C12A 1.91(5) . ? C11A C12C 1.92(5) . ? C11B C12C 0.77(5) . ? C11B C12A 1.89(6) . ? C12A C12C 1.41(4) . ? C12A C12B 1.47(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O2 129.3(12) . 2 ? O2 Ni1 O3 176.3(8) . 2 ? O2 Ni1 O3 48.3(6) 2 2 ? O2 Ni1 O3 48.3(6) . . ? O2 Ni1 O3 176.3(8) 2 . ? O3 Ni1 O3 134.3(9) 2 . ? O2 Ni1 O1 78.9(6) . . ? O2 Ni1 O1 127.8(6) 2 . ? O3 Ni1 O1 100.6(5) 2 . ? O3 Ni1 O1 55.6(6) . . ? O2 Ni1 O1 127.8(6) . 2 ? O2 Ni1 O1 78.9(6) 2 2 ? O3 Ni1 O1 55.6(6) 2 2 ? O3 Ni1 O1 100.6(5) . 2 ? O1 Ni1 O1 121.2(7) . 2 ? O2 Ni1 O4 53.5(6) . . ? O2 Ni1 O4 101.8(6) 2 . ? O3 Ni1 O4 123.2(6) 2 . ? O3 Ni1 O4 78.8(5) . . ? O1 Ni1 O4 56.4(6) . . ? O1 Ni1 O4 177.5(6) 2 . ? O2 Ni1 O4 101.8(6) . 2 ? O2 Ni1 O4 53.5(6) 2 2 ? O3 Ni1 O4 78.8(5) 2 2 ? O3 Ni1 O4 123.2(6) . 2 ? O1 Ni1 O4 177.5(6) . 2 ? O1 Ni1 O4 56.4(6) 2 2 ? O4 Ni1 O4 125.9(9) . 2 ? O5 Nb1 O6 86.3(8) . . ? O5 Nb1 O11 138.4(8) . . ? O6 Nb1 O11 93.7(8) . . ? O5 Nb1 O12 94.8(8) . . ? O6 Nb1 O12 137.8(8) . . ? O11 Nb1 O12 58.7(8) . . ? O5 Nb1 O10 174.0(7) . . ? O6 Nb1 O10 87.7(7) . . ? O11 Nb1 O10 42.2(6) . . ? O12 Nb1 O10 89.8(7) . . ? O5 Nb1 O9 90.4(8) . . ? O6 Nb1 O9 34.5(6) . . ? O11 Nb1 O9 68.7(7) . . ? O12 Nb1 O9 103.4(8) . . ? O10 Nb1 O9 84.7(7) . . ? O5 Nb1 O7 86.8(8) . . ? O6 Nb1 O7 173.1(8) . . ? O11 Nb1 O7 91.5(8) . . ? O12 Nb1 O7 43.1(7) . . ? O10 Nb1 O7 99.2(7) . . ? O9 Nb1 O7 145.8(8) . . ? O5 Nb1 O8 34.0(7) . . ? O6 Nb1 O8 90.1(8) . . ? O11 Nb1 O8 104.5(9) . . ? O12 Nb1 O8 69.9(8) . . ? O10 Nb1 O8 146.3(8) . . ? O9 Nb1 O8 74.8(7) . . ? O7 Nb1 O8 84.3(7) . . ? O5 Nb1 O2 124.0(7) . . ? O6 Nb1 O2 93.7(8) . . ? O11 Nb1 O2 97.5(7) . . ? O12 Nb1 O2 119.2(7) . . ? O10 Nb1 O2 56.2(7) . . ? O9 Nb1 O2 119.1(8) . . ? O7 Nb1 O2 90.0(7) . . ? O8 Nb1 O2 157.4(8) . . ? O5 Nb1 O3 93.1(7) . . ? O6 Nb1 O3 126.7(7) . . ? O11 Nb1 O3 118.8(6) . . ? O12 Nb1 O3 95.5(7) . . ? O10 Nb1 O3 90.4(6) . . ? O9 Nb1 O3 160.5(7) . . ? O7 Nb1 O3 53.6(6) . . ? O8 Nb1 O3 117.2(7) . . ? O2 Nb1 O3 44.6(6) . . ? O5 Nb1 O4 90.1(7) . . ? O6 Nb1 O4 55.0(7) . . ? O11 Nb1 O4 123.4(7) . . ? O12 Nb1 O4 166.4(6) . . ? O10 Nb1 O4 86.2(7) . . ? O9 Nb1 O4 89.2(7) . . ? O7 Nb1 O4 124.9(6) . . ? O8 Nb1 O4 119.3(7) . . ? O2 Nb1 O4 48.5(6) . . ? O3 Nb1 O4 71.6(5) . . ? O5 Nb1 O1 53.6(7) . . ? O6 Nb1 O1 89.9(7) . . ? O11 Nb1 O1 167.6(6) . . ? O12 Nb1 O1 124.2(7) . . ? O10 Nb1 O1 126.3(6) . . ? O9 Nb1 O1 119.1(7) . . ? O7 Nb1 O1 85.9(7) . . ? O8 Nb1 O1 87.3(7) . . ? O2 Nb1 O1 70.4(5) . . ? O3 Nb1 O1 50.6(5) . . ? O4 Nb1 O1 50.5(5) . . ? C1A O1 O3 139.9(16) . . ? C1A O1 O5 82.7(15) . . ? O3 O1 O5 99.6(10) . . ? C1A O1 Ni1 124.6(15) . . ? O3 O1 Ni1 61.9(6) . . ? O5 O1 Ni1 152.6(9) . . ? C1A O1 Nb1 133.1(15) . . ? O3 O1 Nb1 61.7(6) . . ? O5 O1 Nb1 50.4(7) . . ? Ni1 O1 Nb1 102.3(5) . . ? C2A O2 O3 132.8(19) . . ? C2A O2 O4 130(2) . . ? O3 O2 O4 96.7(11) . . ? C2A O2 Ni1 126.2(17) . . ? O3 O2 Ni1 67.3(8) . . ? O4 O2 Ni1 65.0(7) . . ? C2A O2 Nb1 125.5(17) . . ? O3 O2 Nb1 67.7(7) . . ? O4 O2 Nb1 68.5(7) . . ? Ni1 O2 Nb1 108.3(7) . . ? C3A O3 O2 135.8(16) . . ? C3A O3 O1 131.5(15) . . ? O2 O3 O1 92.3(9) . . ? C3A O3 Ni1 125.5(14) . . ? O2 O3 Ni1 64.4(7) . . ? O1 O3 Ni1 62.5(6) . . ? C3A O3 Nb1 127.7(14) . . ? O2 O3 Nb1 67.7(7) . . ? O1 O3 Nb1 67.7(6) . . ? Ni1 O3 Nb1 106.7(6) . . ? C4A O4 O2 142(2) . . ? C4A O4 O6 82.8(18) . . ? O2 O4 O6 102.4(10) . . ? C4A O4 Ni1 123.4(18) . . ? O2 O4 Ni1 61.5(7) . . ? O6 O4 Ni1 153.2(10) . . ? C4A O4 Nb1 133.7(18) . . ? O2 O4 Nb1 63.0(7) . . ? O6 O4 Nb1 50.9(7) . . ? Ni1 O4 Nb1 102.7(6) . . ? O8 O5 C5A 82(2) . . ? O8 O5 Nb1 86.0(15) . . ? C5A O5 Nb1 153(2) . . ? O8 O5 O1 160.3(18) . . ? C5A O5 O1 110(2) . . ? Nb1 O5 O1 76.1(7) . . ? O9 O6 C6A 84(3) . . ? O9 O6 Nb1 84.1(14) . . ? C6A O6 Nb1 149(3) . . ? O9 O6 O4 156.5(18) . . ? C6A O6 O4 111(3) . . ? Nb1 O6 O4 74.1(8) . . ? O12 O7 C7A 108(3) . . ? O12 O7 C3A 159.6(18) . . ? C7A O7 C3A 82(3) . . ? O12 O7 Nb1 63.6(10) . . ? C7A O7 Nb1 166(3) . . ? C3A O7 Nb1 109.2(12) . . ? O5 O8 C8A 123(2) . . ? O5 O8 C5A 61(2) . . ? C8A O8 C5A 91(2) . . ? O5 O8 C5B 109(3) . . ? C8A O8 C5B 63(3) . . ? C5A O8 C5B 48(2) . . ? O5 O8 Nb1 60.0(12) . . ? C8A O8 Nb1 140.3(19) . . ? C5A O8 Nb1 117(2) . . ? C5B O8 Nb1 157(3) . . ? O6 O9 C9A 118(2) . . ? O6 O9 C6A 57(3) . . ? C9A O9 C6A 91(3) . . ? O6 O9 Nb1 61.4(12) . . ? C9A O9 Nb1 142.7(19) . . ? C6A O9 Nb1 113(3) . . ? O11 O10 C10A 103(3) . . ? O11 O10 C2A 161.4(18) . . ? C10A O10 C2A 89(3) . . ? O11 O10 Nb1 64.6(8) . . ? C10A O10 Nb1 161(3) . . ? C2A O10 Nb1 107.2(14) . . ? O10 O11 C11A 110(2) . . ? O10 O11 O12 114.6(13) . . ? C11A O11 O12 94(2) . . ? O10 O11 Nb1 73.1(9) . . ? C11A O11 Nb1 151(2) . . ? O12 O11 Nb1 61.1(7) . . ? O7 O12 C12A 116(2) . . ? O7 O12 O11 115.7(15) . . ? C12A O12 O11 91.2(19) . . ? O7 O12 Nb1 73.2(10) . . ? C12A O12 Nb1 149.6(19) . . ? O11 O12 Nb1 60.2(7) . . ? O1 C1A C1B 116(3) . . ? O1 C1A C1C 119(3) . . ? C1B C1A C1C 118(3) . . ? O1 C1A C3C 114(3) . 2 ? C1B C1A C3C 108(3) . 2 ? C1C C1A C3C 73(3) . 2 ? O2 C2A C2B 115(4) . . ? O2 C2A C2C 109(3) . . ? C2B C2A C2C 108(4) . . ? O2 C2A O10 70.7(17) . . ? C2B C2A O10 111(3) . . ? C2C C2A O10 137(3) . . ? O3 C3A C3C 111(2) . . ? O3 C3A C3B 118(2) . . ? C3C C3A C3B 119(3) . . ? O3 C3A O7 68.9(14) . . ? C3C C3A O7 135(2) . . ? C3B C3A O7 95.1(19) . . ? C3A C3B C7C 90(3) . . ? C3A C3C C1A 109(3) . 2 ? O4 C4A C4C 114(5) . . ? O4 C4A C4B 121(3) . . ? C4C C4A C4B 111(6) . . ? C4A C4B C6C 96(3) . . ? C4A C4C C6A 97(6) . . ? O5 C5A C5B 102(5) . . ? O5 C5A C5C 102(4) . . ? C5B C5A C5C 101(5) . . ? O5 C5A O8 36.2(13) . . ? C5B C5A O8 66(4) . . ? C5C C5A O8 109(4) . . ? C8B C5B C5A 99(6) . . ? C8B C5B C8A 57(4) . . ? C5A C5B C8A 94(5) . . ? C8B C5B O8 100(5) . . ? C5A C5B O8 67(4) . . ? C8A C5B O8 47(2) . . ? C5A C5C C8B 72(3) . . ? O6 C6A C6C 104(5) . . ? O6 C6A C6B 115(5) . . ? C6C C6A C6B 89(5) . . ? O6 C6A O9 39.3(18) . . ? C6C C6A O9 111(5) . . ? C6B C6A O9 77(4) . . ? O6 C6A C4C 91(5) . . ? C6C C6A C4C 90(5) . . ? C6B C6A C4C 153(6) . . ? O9 C6A C4C 128(5) . . ? O6 C6A C9B 105(4) . . ? C6C C6A C9B 60(3) . . ? C6B C6A C9B 33(3) . . ? O9 C6A C9B 76(3) . . ? C4C C6A C9B 149(5) . . ? O6 C6A C9A 67(3) . . ? C6C C6A C9A 80(4) . . ? C6B C6A C9A 54(3) . . ? O9 C6A C9A 38.1(16) . . ? C4C C6A C9A 152(5) . . ? C9B C6A C9A 39.7(17) . . ? C9B C6B C6A 94(5) . . ? C9B C6B C9A 53(3) . . ? C6A C6B C9A 80(4) . . ? C6A C6C C9B 71(4) . . ? C6A C6C C4B 91(4) . . ? C9B C6C C4B 144(4) . . ? O7 C7A C7B 122(7) . . ? O7 C7A C7C 113(6) . . ? C7B C7A C7C 124(7) . . ? C7A C7C C3B 98(5) . . ? C8B C8A C8C 119(3) . . ? C8B C8A O8 112(3) . . ? C8C C8A O8 112(3) . . ? C8B C8A C5B 47(3) . . ? C8C C8A C5B 119(4) . . ? O8 C8A C5B 70(3) . . ? C5B C8B C8A 76(4) . . ? C5B C8B C5C 87(4) . . ? C8A C8B C5C 95(3) . . ? C9C C8C C8A 114(4) . . ? O9 C9A C9B 112(3) . . ? O9 C9A C9C 108(3) . . ? C9B C9A C9C 118(3) . . ? O9 C9A C6B 80(3) . . ? C9B C9A C6B 38(2) . . ? C9C C9A C6B 112(3) . . ? O9 C9A C6A 51(2) . . ? C9B C9A C6A 64(2) . . ? C9C C9A C6A 147(3) . . ? C6B C9A C6A 47(2) . . ? C6B C9B C9A 88(4) . . ? C6B C9B C6A 53(4) . . ? C9A C9B C6A 76(3) . . ? C6B C9B C6C 97(5) . . ? C9A C9B C6C 97(3) . . ? C6A C9B C6C 49(2) . . ? C8C C9C C9A 113(4) . . ? O10 C10A C10C 126(6) . . ? O10 C10A C10B 122(5) . . ? C10C C10A C10B 110(7) . . ? O10 C10A C11C 106(3) . . ? C10C C10A C11C 85(5) . . ? C10B C10A C11C 92(3) . . ? O11 C11A C11C 110(3) . . ? O11 C11A C11B 95(3) . . ? C11C C11A C11B 123(4) . . ? O11 C11A C12A 85(3) . . ? C11C C11A C12A 161(4) . . ? C11B C11A C12A 64(2) . . ? O11 C11A C12C 100(3) . . ? C11C C11A C12C 139(4) . . ? C11B C11A C12C 23.2(19) . . ? C12A C11A C12C 43.1(15) . . ? C12C C11B C11A 101(6) . . ? C12C C11B C12A 41(4) . . ? C11A C11B C12A 66(3) . . ? C11A C11C C10A 92(3) . . ? O12 C12A C12C 112(3) . . ? O12 C12A C12B 108(3) . . ? C12C C12A C12B 119(4) . . ? O12 C12A C11B 99(2) . . ? C12C C12A C11B 21(2) . . ? C12B C12A C11B 140(4) . . ? O12 C12A C11A 90(2) . . ? C12C C12A C11A 69(2) . . ? C12B C12A C11A 154(3) . . ? C11B C12A C11A 50.1(17) . . ? C11B C12C C12A 118(6) . . ? C11B C12C C11A 55(5) . . ? C12A C12C C11A 68(2) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.501 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.082 data_coal3 _database_code_CSD 189540 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Al2 Co O12' _chemical_formula_weight 745.66 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' 'Al' 'Al' 0.0645 0.0514 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.451(9) _cell_length_b 15.407(9) _cell_length_c 14.656(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.288(17) _cell_angle_gamma 90.00 _cell_volume 3941(4) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 998(I>2sigma(I)) _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour 'reddish violet' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 0.534 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.8351 _exptl_absorpt_process_details ? _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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6050 _diffrn_reflns_av_R_equivalents 0.1268 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 20.00 _reflns_number_total 1826 _reflns_number_gt 1108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0624P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1826 _refine_ls_number_parameters 213 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1254 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 0.5000 0.24999(8) 0.7500 0.0506(4) Uani 1 2 d S . . Al1 Al 0.49994(9) 0.25010(14) 0.95017(10) 0.0540(6) Uani 1 1 d . . . O1 O 0.4570(2) 0.3111(2) 0.8539(2) 0.0516(10) Uani 1 1 d . . . O2 O 0.4570(2) 0.1888(2) 0.6460(2) 0.0521(10) Uani 1 1 d . . . O3 O 0.4545(2) 0.3190(3) 1.0424(2) 0.0638(12) Uani 1 1 d . . . O4 O 0.5455(2) 0.1812(3) 1.0424(2) 0.0649(12) Uani 1 1 d . . . O5 O 0.5853(2) 0.3266(3) 0.9547(3) 0.0608(12) Uani 1 1 d . . . O6 O 0.4151(2) 0.1733(3) 0.9548(3) 0.0634(12) Uani 1 1 d . . . C1 C 0.4032(4) 0.3802(5) 0.8581(4) 0.069(2) Uani 1 1 d . . . H1A H 0.3701 0.3708 0.9110 0.083 Uiso 1 1 calc R . . C11 C 0.4467(5) 0.4656(5) 0.8718(5) 0.110(3) Uani 1 1 d . . . H11A H 0.4774 0.4620 0.9262 0.165 Uiso 1 1 calc R . . H11B H 0.4107 0.5124 0.8776 0.165 Uiso 1 1 calc R . . H11C H 0.4792 0.4760 0.8203 0.165 Uiso 1 1 calc R . . C12 C 0.3543(4) 0.3821(5) 0.7744(5) 0.094(2) Uani 1 1 d . . . H12A H 0.3280 0.3276 0.7680 0.141 Uiso 1 1 calc R . . H12B H 0.3860 0.3917 0.7219 0.141 Uiso 1 1 calc R . . H12C H 0.3175 0.4281 0.7793 0.141 Uiso 1 1 calc R . . C2 C 0.4025(4) 0.1193(4) 0.6420(4) 0.070(2) Uani 1 1 d . . . H2A H 0.3693 0.1287 0.5888 0.084 Uiso 1 1 calc R . . C21 C 0.3530(4) 0.1181(5) 0.7262(5) 0.097(3) Uani 1 1 d . . . H21A H 0.3271 0.1728 0.7320 0.146 Uiso 1 1 calc R . . H21B H 0.3846 0.1084 0.7790 0.146 Uiso 1 1 calc R . . H21C H 0.3159 0.0723 0.7210 0.146 Uiso 1 1 calc R . . C22 C 0.4457(5) 0.0338(5) 0.6285(5) 0.110(3) Uani 1 1 d . . . H22A H 0.4763 0.0374 0.5744 0.165 Uiso 1 1 calc R . . H22B H 0.4096 -0.0128 0.6223 0.165 Uiso 1 1 calc R . . H22C H 0.4782 0.0232 0.6803 0.165 Uiso 1 1 calc R . . C31 C 0.6984(4) 0.3986(5) 0.9971(5) 0.091(2) Uani 1 1 d . . . H31A H 0.6840 0.4347 0.9464 0.136 Uiso 1 1 calc R . . H31B H 0.7474 0.3728 0.9856 0.136 Uiso 1 1 calc R . . H31C H 0.7012 0.4333 1.0515 0.136 Uiso 1 1 calc R . . C32 C 0.6389(4) 0.3276(4) 1.0096(5) 0.0590(17) Uani 1 1 d . . . C33 C 0.6498(4) 0.2687(5) 1.0800(5) 0.072(2) Uani 1 1 d . . . H33A H 0.6907 0.2766 1.1200 0.086 Uiso 1 1 calc R . . C34 C 0.6018(4) 0.1987(4) 1.0923(4) 0.0618(18) Uani 1 1 d . . . C35 C 0.6169(4) 0.1347(5) 1.1679(4) 0.092(2) Uani 1 1 d . . . H35A H 0.5783 0.0904 1.1668 0.138 Uiso 1 1 calc R . . H35B H 0.6157 0.1642 1.2255 0.138 Uiso 1 1 calc R . . H35C H 0.6664 0.1088 1.1595 0.138 Uiso 1 1 calc R . . C41 C 0.3024(4) 0.1007(5) 0.9968(5) 0.091(2) Uani 1 1 d . . . H41A H 0.3176 0.0652 0.9462 0.136 Uiso 1 1 calc R . . H41B H 0.2530 0.1255 0.9846 0.136 Uiso 1 1 calc R . . H41C H 0.3000 0.0657 1.0510 0.136 Uiso 1 1 calc R . . C42 C 0.3602(4) 0.1724(4) 1.0106(5) 0.0607(18) Uani 1 1 d . . . C43 C 0.3499(4) 0.2317(5) 1.0802(4) 0.0696(19) Uani 1 1 d . . . H43A H 0.3092 0.2237 1.1201 0.084 Uiso 1 1 calc R . . C44 C 0.3975(4) 0.3026(5) 1.0932(4) 0.0659(19) Uani 1 1 d . . . C45 C 0.3828(4) 0.3649(5) 1.1692(4) 0.094(2) Uani 1 1 d . . . H45A H 0.4208 0.4098 1.1685 0.141 Uiso 1 1 calc R . . H45B H 0.3851 0.3347 1.2265 0.141 Uiso 1 1 calc R . . H45C H 0.3329 0.3902 1.1616 0.141 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 Co1 0.0445(7) 0.0482(7) 0.0591(7) 0.000 0.0002(5) 0.000 Al1 0.0471(12) 0.0541(12) 0.0609(11) 0.0002(11) 0.0011(9) -0.0114(9) O1 0.044(2) 0.048(3) 0.063(2) 0.000(2) 0.0031(19) 0.003(2) O2 0.049(2) 0.046(2) 0.062(2) 0.001(2) -0.0032(19) 0.000(2) O3 0.066(3) 0.066(3) 0.060(2) -0.008(2) 0.010(2) -0.020(2) O4 0.065(3) 0.068(3) 0.061(3) 0.000(2) -0.006(2) -0.019(3) O5 0.054(3) 0.059(3) 0.069(3) -0.002(2) -0.008(2) -0.016(2) O6 0.052(3) 0.065(3) 0.073(3) 0.000(2) 0.003(2) -0.017(2) C1 0.059(5) 0.083(6) 0.066(4) 0.011(4) 0.014(4) 0.012(4) C11 0.156(8) 0.060(5) 0.113(6) -0.015(5) 0.008(6) 0.008(6) C12 0.072(5) 0.102(6) 0.109(5) 0.008(5) 0.004(5) 0.032(5) C2 0.067(5) 0.073(6) 0.069(4) 0.003(4) -0.016(4) -0.012(4) C21 0.078(6) 0.108(7) 0.105(5) 0.006(5) 0.006(5) -0.032(5) C22 0.150(8) 0.063(5) 0.118(6) -0.009(5) -0.010(6) -0.010(6) C31 0.058(5) 0.088(5) 0.126(6) -0.003(5) -0.005(4) -0.031(4) C32 0.051(5) 0.056(4) 0.070(4) -0.014(4) 0.004(4) -0.011(4) C33 0.050(4) 0.082(6) 0.083(5) -0.002(5) -0.021(4) -0.019(4) C34 0.072(5) 0.055(5) 0.058(4) -0.012(4) -0.001(4) 0.004(4) C35 0.093(6) 0.099(6) 0.084(5) 0.023(5) -0.026(4) -0.017(5) C41 0.057(5) 0.089(5) 0.126(6) -0.013(5) 0.006(4) -0.033(4) C42 0.049(4) 0.057(5) 0.076(5) 0.020(5) -0.006(4) -0.010(4) C43 0.065(5) 0.068(5) 0.075(5) -0.001(4) 0.018(4) -0.010(4) C44 0.071(5) 0.069(5) 0.057(4) 0.008(4) -0.004(4) -0.006(4) C45 0.102(6) 0.100(7) 0.081(5) -0.026(5) 0.021(4) -0.016(5) _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 O2 1.940(4) . ? Co1 O2 1.940(4) 2_656 ? Co1 O1 1.944(4) . ? Co1 O1 1.944(4) 2_656 ? Co1 Al1 2.934(2) . ? Co1 Al1 2.934(2) 2_656 ? Al1 O1 1.851(4) . ? Al1 O2 1.859(4) 2_656 ? Al1 O4 1.892(4) . ? Al1 O3 1.896(4) . ? Al1 O6 1.897(5) . ? Al1 O5 1.900(4) . ? O1 C1 1.421(7) . ? O2 C2 1.433(7) . ? O2 Al1 1.859(4) 2_656 ? O3 C44 1.271(7) . ? O4 C34 1.250(7) . ? O5 C32 1.231(7) . ? O6 C42 1.262(7) . ? C1 C12 1.492(8) . ? C1 C11 1.533(9) . ? C2 C21 1.510(8) . ? C2 C22 1.531(9) . ? C31 C32 1.520(8) . ? C32 C33 1.386(8) . ? C33 C34 1.378(9) . ? C34 C35 1.505(8) . ? C41 C42 1.509(8) . ? C42 C43 1.383(8) . ? C43 C44 1.384(8) . ? C44 C45 1.494(8) . ? 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 O2 Co1 O2 121.9(2) . 2_656 ? O2 Co1 O1 134.53(15) . . ? O2 Co1 O1 76.67(15) 2_656 . ? O2 Co1 O1 76.67(15) . 2_656 ? O2 Co1 O1 134.53(15) 2_656 2_656 ? O1 Co1 O1 122.0(2) . 2_656 ? O2 Co1 Al1 141.61(12) . . ? O2 Co1 Al1 38.44(12) 2_656 . ? O1 Co1 Al1 38.23(12) . . ? O1 Co1 Al1 141.72(12) 2_656 . ? O2 Co1 Al1 38.44(12) . 2_656 ? O2 Co1 Al1 141.61(12) 2_656 2_656 ? O1 Co1 Al1 141.72(12) . 2_656 ? O1 Co1 Al1 38.23(12) 2_656 2_656 ? Al1 Co1 Al1 179.93(9) . 2_656 ? O1 Al1 O2 80.98(16) . 2_656 ? O1 Al1 O4 175.8(2) . . ? O2 Al1 O4 94.98(19) 2_656 . ? O1 Al1 O3 95.16(19) . . ? O2 Al1 O3 175.9(2) 2_656 . ? O4 Al1 O3 88.91(18) . . ? O1 Al1 O6 91.81(17) . . ? O2 Al1 O6 91.67(19) 2_656 . ? O4 Al1 O6 87.11(19) . . ? O3 Al1 O6 89.7(2) . . ? O1 Al1 O5 91.45(19) . . ? O2 Al1 O5 91.22(18) 2_656 . ? O4 Al1 O5 89.81(19) . . ? O3 Al1 O5 87.61(19) . . ? O6 Al1 O5 175.94(19) . . ? O1 Al1 Co1 40.54(12) . . ? O2 Al1 Co1 40.44(11) 2_656 . ? O4 Al1 Co1 135.41(15) . . ? O3 Al1 Co1 135.68(15) . . ? O6 Al1 Co1 92.28(13) . . ? O5 Al1 Co1 91.77(13) . . ? C1 O1 Al1 127.7(4) . . ? C1 O1 Co1 130.9(3) . . ? Al1 O1 Co1 101.23(19) . . ? C2 O2 Al1 128.2(3) . 2_656 ? C2 O2 Co1 130.5(4) . . ? Al1 O2 Co1 101.12(19) 2_656 . ? C44 O3 Al1 129.6(4) . . ? C34 O4 Al1 128.5(4) . . ? C32 O5 Al1 128.6(4) . . ? C42 O6 Al1 128.7(4) . . ? O1 C1 C12 110.7(5) . . ? O1 C1 C11 108.8(5) . . ? C12 C1 C11 111.8(6) . . ? O2 C2 C21 110.9(5) . . ? O2 C2 C22 108.8(5) . . ? C21 C2 C22 112.2(6) . . ? O5 C32 C33 125.4(6) . . ? O5 C32 C31 116.6(6) . . ? C33 C32 C31 118.0(6) . . ? C34 C33 C32 121.9(6) . . ? O4 C34 C33 124.6(6) . . ? O4 C34 C35 115.0(6) . . ? C33 C34 C35 120.3(7) . . ? O6 C42 C43 124.9(6) . . ? O6 C42 C41 115.5(6) . . ? C43 C42 C41 119.5(7) . . ? C42 C43 C44 122.9(6) . . ? O3 C44 C43 123.2(6) . . ? O3 C44 C45 116.6(6) . . ? C43 C44 C45 120.2(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.184 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.050 data_nial2n _database_code_CSD 189541 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Al2 Ni O12' _chemical_formula_weight 745.44 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' 'Al' 'Al' 0.0645 0.0514 '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 Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 15.479(3) _cell_length_b 17.480(4) _cell_length_c 14.666(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3968.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1020(I>2sigma(I)) _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 23.00 _exptl_crystal_description cubooctahedron _exptl_crystal_colour 'bluish violet' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.8436 _exptl_absorpt_correction_T_max 0.8436 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius Kappa CCD' _diffrn_measurement_method 'Nonius Collect' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5142 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 23.00 _reflns_number_total 1378 _reflns_number_gt 1020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Nonius Denzo' _computing_data_reduction 'Nonius Denzo' _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^)+(0.1028P)^2^+0.9695P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0061(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1378 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0721 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1592 _refine_ls_wR_factor_gt 0.1496 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.0000 0.2500 0.7500 0.0575(5) Uani 1 4 d S . . Al1 Al 0.0000 0.2500 0.95044(11) 0.0580(5) Uani 1 2 d S . . O1 O -0.06901(16) 0.20501(13) 1.04282(16) 0.0703(8) Uani 1 1 d . . . O2 O 0.07627(15) 0.16447(13) 0.95575(17) 0.0698(8) Uani 1 1 d . . . O3 O 0.06096(15) 0.29259(12) 0.85378(14) 0.0603(7) Uani 1 1 d . . . C1 C 0.1298(3) 0.3465(2) 0.8564(3) 0.0781(12) Uani 1 1 d . . . H1A H 0.1204 0.3802 0.9089 0.094 Uiso 1 1 calc R . . C11 C 0.1308(4) 0.3953(3) 0.7719(3) 0.1062(16) Uani 1 1 d . . . H11A H 0.0760 0.4205 0.7654 0.159 Uiso 1 1 calc R . . H11B H 0.1413 0.3636 0.7196 0.159 Uiso 1 1 calc R . . H11C H 0.1757 0.4329 0.7769 0.159 Uiso 1 1 calc R . . C12 C 0.2148(3) 0.3052(4) 0.8704(4) 0.1185(19) Uani 1 1 d . . . H12A H 0.2117 0.2747 0.9248 0.178 Uiso 1 1 calc R . . H12B H 0.2606 0.3419 0.8763 0.178 Uiso 1 1 calc R . . H12C H 0.2261 0.2727 0.8190 0.178 Uiso 1 1 calc R . . C21 C 0.1483(3) 0.0523(2) 0.9974(3) 0.0933(13) Uani 1 1 d . . . H21A H 0.1838 0.0680 0.9471 0.140 Uiso 1 1 calc R . . H21B H 0.1234 0.0032 0.9845 0.140 Uiso 1 1 calc R . . H21C H 0.1829 0.0490 1.0516 0.140 Uiso 1 1 calc R . . C22 C 0.0778(2) 0.10966(19) 1.0117(3) 0.0663(10) Uani 1 1 d . . . C23 C 0.0174(3) 0.0998(2) 1.0810(3) 0.0795(12) Uani 1 1 d . . . H23A H 0.0248 0.0591 1.1210 0.095 Uiso 1 1 calc R . . C24 C -0.0529(2) 0.1472(2) 1.0934(2) 0.0677(10) Uani 1 1 d . . . C25 C -0.1160(3) 0.1332(3) 1.1683(3) 0.1023(15) Uani 1 1 d . . . H25A H -0.1603 0.1716 1.1665 0.153 Uiso 1 1 calc R . . H25B H -0.0867 0.1353 1.2259 0.153 Uiso 1 1 calc R . . H25C H -0.1416 0.0836 1.1606 0.153 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 0.0592(7) 0.0546(6) 0.0587(7) 0.000 0.000 0.000 Al1 0.0597(10) 0.0536(9) 0.0606(10) 0.000 0.000 0.0121(6) O1 0.0716(17) 0.0717(16) 0.0677(16) 0.0067(13) 0.0065(13) 0.0173(12) O2 0.0691(17) 0.0610(15) 0.0792(17) -0.0041(13) 0.0014(13) 0.0170(12) O3 0.0597(15) 0.0552(15) 0.0658(16) -0.0028(10) -0.0017(11) -0.0021(11) C1 0.090(3) 0.073(2) 0.071(2) -0.0186(19) 0.010(2) -0.018(2) C11 0.112(4) 0.084(3) 0.122(4) 0.005(3) 0.011(3) -0.035(3) C12 0.064(3) 0.167(5) 0.124(4) -0.016(4) -0.009(3) -0.015(3) C21 0.088(3) 0.073(2) 0.119(3) 0.000(2) -0.009(3) 0.029(2) C22 0.073(2) 0.052(2) 0.074(2) -0.0015(18) -0.014(2) 0.0089(18) C23 0.094(3) 0.065(2) 0.079(3) 0.015(2) -0.011(2) 0.014(2) C24 0.078(3) 0.067(2) 0.059(2) 0.0027(18) -0.0041(19) -0.0001(19) C25 0.106(4) 0.108(3) 0.092(3) 0.026(3) 0.019(3) 0.012(3) _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 O3 1.939(2) 6_455 ? Ni1 O3 1.939(2) . ? Ni1 O3 1.939(2) 3_556 ? Ni1 O3 1.939(2) 8_456 ? Ni1 Al1 2.9397(17) . ? Ni1 Al1 2.9397(17) 3_556 ? Al1 O3 1.859(2) 6_455 ? Al1 O3 1.859(2) . ? Al1 O1 1.896(3) 6_455 ? Al1 O1 1.896(3) . ? Al1 O2 1.907(2) 6_455 ? Al1 O2 1.907(2) . ? O1 C24 1.278(4) . ? O2 C22 1.261(4) . ? O3 C1 1.423(4) . ? C1 C11 1.504(6) . ? C1 C12 1.516(6) . ? C21 C22 1.496(5) . ? C22 C23 1.391(5) . ? C23 C24 1.380(5) . ? C24 C25 1.490(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 O3 Ni1 O3 76.60(13) 6_455 . ? O3 Ni1 O3 121.77(14) 6_455 3_556 ? O3 Ni1 O3 134.86(12) . 3_556 ? O3 Ni1 O3 134.86(12) 6_455 8_456 ? O3 Ni1 O3 121.77(14) . 8_456 ? O3 Ni1 O3 76.60(13) 3_556 8_456 ? O3 Ni1 Al1 38.30(7) 6_455 . ? O3 Ni1 Al1 38.30(7) . . ? O3 Ni1 Al1 141.70(7) 3_556 . ? O3 Ni1 Al1 141.70(7) 8_456 . ? O3 Ni1 Al1 141.70(7) 6_455 3_556 ? O3 Ni1 Al1 141.70(7) . 3_556 ? O3 Ni1 Al1 38.30(7) 3_556 3_556 ? O3 Ni1 Al1 38.30(7) 8_456 3_556 ? Al1 Ni1 Al1 180.0 . 3_556 ? O3 Al1 O3 80.58(14) 6_455 . ? O3 Al1 O1 175.70(11) 6_455 6_455 ? O3 Al1 O1 95.33(10) . 6_455 ? O3 Al1 O1 95.33(10) 6_455 . ? O3 Al1 O1 175.70(11) . . ? O1 Al1 O1 88.79(16) 6_455 . ? O3 Al1 O2 91.77(11) 6_455 6_455 ? O3 Al1 O2 91.80(10) . 6_455 ? O1 Al1 O2 89.68(11) 6_455 6_455 ? O1 Al1 O2 86.98(10) . 6_455 ? O3 Al1 O2 91.80(10) 6_455 . ? O3 Al1 O2 91.77(11) . . ? O1 Al1 O2 86.98(10) 6_455 . ? O1 Al1 O2 89.68(11) . . ? O2 Al1 O2 175.32(17) 6_455 . ? O3 Al1 Ni1 40.29(7) 6_455 . ? O3 Al1 Ni1 40.29(7) . . ? O1 Al1 Ni1 135.60(8) 6_455 . ? O1 Al1 Ni1 135.60(8) . . ? O2 Al1 Ni1 92.34(9) 6_455 . ? O2 Al1 Ni1 92.34(9) . . ? C24 O1 Al1 129.2(2) . . ? C22 O2 Al1 129.3(2) . . ? C1 O3 Al1 128.7(2) . . ? C1 O3 Ni1 129.8(2) . . ? Al1 O3 Ni1 101.41(11) . . ? O3 C1 C11 111.2(3) . . ? O3 C1 C12 109.7(3) . . ? C11 C1 C12 111.9(4) . . ? O2 C22 C23 123.8(3) . . ? O2 C22 C21 115.6(4) . . ? C23 C22 C21 120.6(3) . . ? C24 C23 C22 123.5(4) . . ? O1 C24 C23 123.5(3) . . ? O1 C24 C25 115.5(3) . . ? C23 C24 C25 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.381 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.100 data_mgal2n _database_code_CSD 189542 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Al2 Mg O12' _chemical_formula_weight 711.04 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' 'Al' 'Al' 0.0645 0.0514 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Ccca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1, -y+1/2, z' '-x+1/2, y+1/2, -z+1/2' 'x+1, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x, -y, z-1/2' '-x-1/2, y, z-1/2' '-x+1/2, -y+1/2, -z' 'x, y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' '-x, y+1/2, z-1/2' _cell_length_a 15.4139(17) _cell_length_b 17.417(2) _cell_length_c 14.6913(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3944.2(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 995(I>2sigma(I)) _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 19.98 _exptl_crystal_description cubooctahedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.9582 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4706 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 19.98 _reflns_number_total 925 _reflns_number_gt 685 _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^)+(0.0807P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 925 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1178 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _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 0.0000 0.2500 0.7500 0.0484(8) Uani 1 4 d S . . Al1 Al 0.0000 0.2500 0.94769(10) 0.0525(6) Uani 1 2 d S . . O1 O -0.06840(17) 0.20520(15) 1.04085(16) 0.0630(9) Uani 1 1 d . . . O2 O 0.07643(16) 0.16451(15) 0.95270(17) 0.0598(9) Uani 1 1 d . . . O3 O 0.06194(15) 0.29385(14) 0.85211(15) 0.0513(8) Uani 1 1 d . . . C1 C 0.1313(3) 0.3473(2) 0.8588(3) 0.0680(13) Uani 1 1 d . . . H1A H 0.1208 0.3798 0.9122 0.082 Uiso 1 1 calc R . . C11 C 0.1327(3) 0.3984(3) 0.7757(3) 0.0946(16) Uani 1 1 d . . . H11A H 0.0777 0.4236 0.7695 0.142 Uiso 1 1 calc R . . H11B H 0.1437 0.3678 0.7226 0.142 Uiso 1 1 calc R . . H11C H 0.1777 0.4361 0.7822 0.142 Uiso 1 1 calc R . . C12 C 0.2159(3) 0.3056(3) 0.8729(3) 0.1065(18) Uani 1 1 d . . . H12A H 0.2119 0.2740 0.9263 0.160 Uiso 1 1 calc R . . H12B H 0.2618 0.3422 0.8806 0.160 Uiso 1 1 calc R . . H12C H 0.2278 0.2739 0.8209 0.160 Uiso 1 1 calc R . . C21 C 0.1492(3) 0.0525(2) 0.9947(3) 0.0856(15) Uani 1 1 d . . . H21A H 0.1839 0.0675 0.9434 0.128 Uiso 1 1 calc R . . H21B H 0.1244 0.0028 0.9835 0.128 Uiso 1 1 calc R . . H21C H 0.1849 0.0503 1.0482 0.128 Uiso 1 1 calc R . . C22 C 0.0783(3) 0.1097(2) 1.0087(3) 0.0600(12) Uani 1 1 d . . . C23 C 0.0191(3) 0.1008(2) 1.0788(3) 0.0702(13) Uani 1 1 d . . . H23A H 0.0273 0.0604 1.1193 0.084 Uiso 1 1 calc R . . C24 C -0.0514(3) 0.1483(3) 1.0921(3) 0.0607(12) Uani 1 1 d . . . C25 C -0.1133(3) 0.1347(3) 1.1680(3) 0.0874(15) Uani 1 1 d . . . H25A H -0.1579 0.1732 1.1667 0.131 Uiso 1 1 calc R . . H25B H -0.0829 0.1373 1.2250 0.131 Uiso 1 1 calc R . . H25C H -0.1391 0.0848 1.1613 0.131 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 Mg1 0.0510(16) 0.0438(15) 0.0504(16) 0.000 0.000 0.000 Al1 0.0570(12) 0.0480(11) 0.0524(11) 0.000 0.000 0.0114(8) O1 0.0697(19) 0.065(2) 0.0540(18) 0.0101(15) 0.0074(14) 0.0178(16) O2 0.0647(19) 0.0487(18) 0.0661(19) 0.0012(15) -0.0006(14) 0.0153(14) O3 0.0525(16) 0.0459(16) 0.0554(17) -0.0061(11) -0.0003(12) -0.0021(14) C1 0.082(3) 0.062(3) 0.059(3) -0.018(2) 0.008(2) -0.017(3) C11 0.110(4) 0.079(3) 0.095(3) -0.001(3) 0.011(3) -0.034(3) C12 0.058(3) 0.153(5) 0.109(4) -0.006(4) -0.008(3) -0.008(4) C21 0.088(3) 0.062(3) 0.107(3) -0.004(3) -0.012(3) 0.032(3) C22 0.070(3) 0.045(3) 0.065(3) -0.003(2) -0.015(3) 0.012(2) C23 0.081(3) 0.063(3) 0.067(3) 0.018(2) -0.003(3) 0.015(3) C24 0.070(3) 0.062(3) 0.050(3) 0.001(2) -0.004(2) 0.000(3) C25 0.101(4) 0.094(4) 0.067(3) 0.020(3) 0.019(3) 0.011(3) _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 O3 1.935(2) . ? Mg1 O3 1.935(2) 8_456 ? Mg1 O3 1.935(2) 3_556 ? Mg1 O3 1.935(2) 6_455 ? Mg1 Al1 2.9043(16) 3_556 ? Mg1 Al1 2.9043(16) . ? Al1 O3 1.862(3) . ? Al1 O3 1.862(3) 6_455 ? Al1 O1 1.896(3) 6_455 ? Al1 O1 1.896(3) . ? Al1 O2 1.900(3) . ? Al1 O2 1.900(3) 6_455 ? O1 C24 1.272(5) . ? O2 C22 1.260(4) . ? O3 C1 1.421(5) . ? C1 C12 1.507(6) . ? C1 C11 1.510(6) . ? C21 C22 1.494(5) . ? C22 C23 1.385(5) . ? C23 C24 1.380(5) . ? C24 C25 1.486(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Mg1 O3 120.88(14) . 8_456 ? O3 Mg1 O3 133.51(14) . 3_556 ? O3 Mg1 O3 78.36(14) 8_456 3_556 ? O3 Mg1 O3 78.36(14) . 6_455 ? O3 Mg1 O3 133.51(14) 8_456 6_455 ? O3 Mg1 O3 120.88(14) 3_556 6_455 ? O3 Mg1 Al1 140.82(7) . 3_556 ? O3 Mg1 Al1 39.18(7) 8_456 3_556 ? O3 Mg1 Al1 39.18(7) 3_556 3_556 ? O3 Mg1 Al1 140.82(7) 6_455 3_556 ? O3 Mg1 Al1 39.18(7) . . ? O3 Mg1 Al1 140.82(7) 8_456 . ? O3 Mg1 Al1 140.82(7) 3_556 . ? O3 Mg1 Al1 39.18(7) 6_455 . ? Al1 Mg1 Al1 180.0 3_556 . ? O3 Al1 O3 82.10(15) . 6_455 ? O3 Al1 O1 95.19(11) . 6_455 ? O3 Al1 O1 176.90(11) 6_455 6_455 ? O3 Al1 O1 176.90(11) . . ? O3 Al1 O1 95.19(11) 6_455 . ? O1 Al1 O1 87.57(16) 6_455 . ? O3 Al1 O2 91.87(12) . . ? O3 Al1 O2 91.48(11) 6_455 . ? O1 Al1 O2 87.12(11) 6_455 . ? O1 Al1 O2 89.67(12) . . ? O3 Al1 O2 91.48(11) . 6_455 ? O3 Al1 O2 91.87(12) 6_455 6_455 ? O1 Al1 O2 89.67(12) 6_455 6_455 ? O1 Al1 O2 87.12(11) . 6_455 ? O2 Al1 O2 175.56(18) . 6_455 ? O3 Al1 Mg1 41.05(8) . . ? O3 Al1 Mg1 41.05(8) 6_455 . ? O1 Al1 Mg1 136.22(8) 6_455 . ? O1 Al1 Mg1 136.22(8) . . ? O2 Al1 Mg1 92.22(9) . . ? O2 Al1 Mg1 92.22(9) 6_455 . ? C24 O1 Al1 129.3(3) . . ? C22 O2 Al1 129.3(3) . . ? C1 O3 Al1 127.0(2) . . ? C1 O3 Mg1 133.1(2) . . ? Al1 O3 Mg1 99.77(12) . . ? O3 C1 C12 110.1(4) . . ? O3 C1 C11 109.9(3) . . ? C12 C1 C11 112.5(4) . . ? O2 C22 C23 123.8(4) . . ? O2 C22 C21 115.6(4) . . ? C23 C22 C21 120.6(4) . . ? C24 C23 C22 123.8(4) . . ? O1 C24 C23 123.1(4) . . ? O1 C24 C25 115.9(4) . . ? C23 C24 C25 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 19.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.236 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.037 data_znal21 _database_code_CSD 189543 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H70 Al2 O14 Zn2' _chemical_formula_weight 935.64 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.044(3) _cell_length_b 30.978(6) _cell_length_c 11.788(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.10(3) _cell_angle_gamma 90.00 _cell_volume 5490.4(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1702(I>2sigma(I)) _cell_measurement_theta_min 1.90 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type 'Integration' _exptl_absorpt_correction_T_min 0.7626 _exptl_absorpt_correction_T_max 0.8700 _exptl_absorpt_process_details 'Nonius MaXus' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nonius Kappa-CCD' _diffrn_measurement_method 'Nonius Collect' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8023 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2545 _reflns_number_gt 1696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement 'Nonius Denzo' _computing_data_reduction 'Nonius Denzo' _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^)+(0.1600P)^2^+11.3688P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2545 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2589 _refine_ls_wR_factor_gt 0.2372 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 Zn1 Zn 0.07807(7) 0.13768(3) 0.22852(9) 0.0672(6) Uani 1 1 d . . . Al1 Al 0.2341(2) 0.13752(8) 0.1841(3) 0.0640(9) Uani 1 1 d . . . O1 O 0.2281(5) 0.1981(2) 0.1547(6) 0.0728(19) Uani 1 1 d . . . O2 O 0.3576(5) 0.1414(2) 0.2902(6) 0.0772(19) Uani 1 1 d . . . O3 O 0.2531(5) 0.1320(2) 0.0379(6) 0.0725(19) Uani 1 1 d . . . O4 O 0.2475(4) 0.0767(2) 0.2092(6) 0.0779(19) Uani 1 1 d . . . O5 O 0.1101(4) 0.13345(16) 0.0896(5) 0.0648(17) Uani 1 1 d . . . O6 O 0.2077(4) 0.14232(17) 0.3203(5) 0.0649(17) Uani 1 1 d . . . O7 O 0.0000 0.0963(3) 0.2500 0.074(2) Uani 1 2 d S . . O8 O 0.0000 0.1789(2) 0.2500 0.075(3) Uani 1 2 d S . . C1 C 0.2903(11) 0.2253(3) 0.1975(11) 0.082(3) Uani 1 1 d . . . C2 C 0.2621(8) 0.2719(3) 0.1582(11) 0.105(4) Uani 1 1 d . . . H2A H 0.2145 0.2726 0.0715 0.157 Uiso 1 1 calc R . . H2B H 0.3117 0.2881 0.1636 0.157 Uiso 1 1 calc R . . H2C H 0.2422 0.2843 0.2148 0.157 Uiso 1 1 calc R . . C3 C 0.3785(11) 0.2148(4) 0.2790(13) 0.109(4) Uani 1 1 d . . . H3 H 0.4194 0.2373 0.3068 0.131 Uiso 1 1 calc R . . C4 C 0.4107(9) 0.1740(5) 0.3224(11) 0.092(3) Uani 1 1 d . . . C5 C 0.5052(7) 0.1665(5) 0.4161(12) 0.124(4) Uani 1 1 d . . . H5A H 0.5372 0.1579 0.3710 0.186 Uiso 1 1 calc R . . H5B H 0.5092 0.1441 0.4749 0.186 Uiso 1 1 calc R . . H5C H 0.5306 0.1926 0.4629 0.186 Uiso 1 1 calc R . . C6 C 0.2618(7) 0.0985(4) -0.0146(9) 0.081(3) Uani 1 1 d . . . C7 C 0.2704(8) 0.1058(4) -0.1329(10) 0.104(4) Uani 1 1 d . . . H7A H 0.2330 0.0858 -0.1983 0.156 Uiso 1 1 calc R . . H7B H 0.3312 0.1016 -0.1140 0.156 Uiso 1 1 calc R . . H7C H 0.2527 0.1348 -0.1629 0.156 Uiso 1 1 calc R . . C8 C 0.2621(8) 0.0574(3) 0.0313(10) 0.089(3) Uani 1 1 d . . . H8 H 0.2664 0.0343 -0.0159 0.107 Uiso 1 1 calc R . . C9 C 0.2567(7) 0.0481(3) 0.1395(11) 0.081(3) Uani 1 1 d . . . C10 C 0.2595(10) 0.0024(3) 0.1836(12) 0.120(4) Uani 1 1 d . . . H10A H 0.3073 -0.0008 0.2695 0.180 Uiso 1 1 calc R . . H10B H 0.2688 -0.0168 0.1271 0.180 Uiso 1 1 calc R . . H10C H 0.2042 -0.0045 0.1823 0.180 Uiso 1 1 calc R . . C11 C 0.0533(7) 0.1326(3) -0.0438(9) 0.076(3) Uani 1 1 d . . . H11 H 0.0907 0.1327 -0.0863 0.092 Uiso 1 1 calc R . . C12 C -0.0035(10) 0.1733(5) -0.0853(12) 0.149(6) Uani 1 1 d . . . H12A H -0.0343 0.1764 -0.0354 0.224 Uiso 1 1 calc R . . H12B H -0.0459 0.1713 -0.1748 0.224 Uiso 1 1 calc R . . H12C H 0.0340 0.1980 -0.0718 0.224 Uiso 1 1 calc R . . C13 C -0.0011(10) 0.0925(4) -0.0837(11) 0.138(5) Uani 1 1 d . . . H13A H 0.0374 0.0678 -0.0599 0.207 Uiso 1 1 calc R . . H13B H -0.0384 0.0927 -0.1752 0.207 Uiso 1 1 calc R . . H13C H -0.0375 0.0910 -0.0417 0.207 Uiso 1 1 calc R . . C14 C 0.2670(7) 0.1417(3) 0.4562(9) 0.079(3) Uani 1 1 d . . . H14 H 0.3283 0.1413 0.4699 0.095 Uiso 1 1 calc R . . C15 C 0.2544(13) 0.1801(6) 0.5137(19) 0.208(8) Uiso 1 1 d . . . H15A H 0.2504 0.2046 0.4615 0.312 Uiso 1 1 calc R . . H15B H 0.3039 0.1837 0.5980 0.312 Uiso 1 1 calc R . . H15C H 0.2006 0.1776 0.5203 0.312 Uiso 1 1 calc R . . C16 C 0.2517(12) 0.1030(5) 0.5126(15) 0.169(6) Uiso 1 1 d . . . H16A H 0.1990 0.1066 0.5217 0.253 Uiso 1 1 calc R . . H16B H 0.3017 0.0981 0.5956 0.253 Uiso 1 1 calc R . . H16C H 0.2444 0.0788 0.4579 0.253 Uiso 1 1 calc R . . C17 C -0.0148(16) 0.0510(6) 0.2070(17) 0.090(7) Uiso 0.50 1 d P . . C18 C 0.0743(10) 0.0292(4) 0.2426(17) 0.154(7) Uani 1 1 d . . . C19 C 0.0200(18) 0.2234(6) 0.284(2) 0.095(7) Uiso 0.50 1 d P . . C20 C 0.0599(10) 0.2462(4) 0.2139(13) 0.122(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0795(11) 0.0625(9) 0.0674(9) -0.0015(5) 0.0411(7) -0.0017(6) Al1 0.078(2) 0.0534(18) 0.0678(19) -0.0001(13) 0.0405(17) 0.0006(14) O1 0.087(5) 0.058(4) 0.080(4) -0.004(3) 0.045(4) -0.006(4) O2 0.081(5) 0.073(5) 0.083(5) 0.001(4) 0.043(4) -0.004(4) O3 0.093(5) 0.061(4) 0.077(4) -0.005(3) 0.050(4) 0.005(3) O4 0.099(5) 0.055(4) 0.088(4) 0.005(4) 0.051(4) 0.006(4) O5 0.080(5) 0.063(4) 0.055(4) -0.003(3) 0.035(4) -0.004(3) O6 0.072(5) 0.066(4) 0.054(4) 0.000(3) 0.026(3) -0.002(3) O7 0.082(7) 0.060(6) 0.090(6) 0.000 0.048(5) 0.000 O8 0.105(8) 0.042(5) 0.093(6) 0.000 0.061(6) 0.000 C1 0.125(12) 0.057(8) 0.087(8) -0.004(6) 0.068(8) -0.002(8) C2 0.145(12) 0.059(7) 0.129(9) 0.003(6) 0.080(9) -0.010(7) C3 0.122(13) 0.081(10) 0.123(10) -0.013(8) 0.056(10) -0.028(9) C4 0.113(12) 0.090(10) 0.085(8) 0.002(7) 0.057(8) -0.004(9) C5 0.057(9) 0.156(13) 0.138(11) -0.022(9) 0.028(8) -0.015(8) C6 0.088(8) 0.091(9) 0.069(7) -0.003(7) 0.042(6) 0.004(6) C7 0.136(11) 0.096(8) 0.096(8) -0.006(7) 0.069(8) 0.005(8) C8 0.126(10) 0.070(8) 0.089(8) -0.015(6) 0.065(7) 0.010(6) C9 0.098(9) 0.056(7) 0.098(8) -0.001(6) 0.052(7) -0.001(6) C10 0.167(13) 0.066(8) 0.146(11) 0.009(7) 0.090(10) 0.018(8) C11 0.074(7) 0.092(8) 0.056(7) 0.006(5) 0.025(6) 0.023(6) C12 0.186(16) 0.163(14) 0.099(9) 0.016(9) 0.066(10) 0.059(12) C13 0.147(13) 0.140(12) 0.094(9) -0.026(8) 0.031(9) -0.045(10) C14 0.086(8) 0.088(8) 0.073(7) -0.001(5) 0.046(6) -0.011(6) C18 0.161(15) 0.067(9) 0.30(2) 0.017(9) 0.160(16) 0.023(8) C20 0.169(14) 0.074(8) 0.186(14) 0.000(7) 0.135(12) -0.015(8) _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 Zn1 O8 1.946(5) . ? Zn1 O7 1.949(5) . ? Zn1 O6 1.954(6) . ? Zn1 O5 1.959(6) . ? Zn1 Zn1 2.934(2) 2 ? Zn1 Al1 2.942(3) . ? Al1 O6 1.866(6) . ? Al1 O5 1.872(7) . ? Al1 O2 1.879(8) . ? Al1 O1 1.901(7) . ? Al1 O4 1.906(6) . ? Al1 O3 1.906(7) . ? O1 C1 1.258(13) . ? O2 C4 1.289(13) . ? O3 C6 1.252(11) . ? O4 C9 1.265(11) . ? O5 C11 1.406(11) . ? O6 C14 1.436(11) . ? O7 C17 1.47(2) 2 ? O7 C17 1.47(2) . ? O7 Zn1 1.949(5) 2 ? O8 C19 1.428(19) . ? O8 C19 1.428(19) 2 ? O8 Zn1 1.946(5) 2 ? C1 C3 1.388(16) . ? C1 C2 1.525(14) . ? C3 C4 1.377(16) . ? C4 C5 1.481(15) . ? C6 C8 1.385(13) . ? C6 C7 1.488(13) . ? C8 C9 1.352(13) . ? C9 C10 1.502(14) . ? C11 C13 1.488(14) . ? C11 C12 1.525(15) . ? C14 C15 1.433(18) . ? C14 C16 1.453(16) . ? C17 C17 0.89(3) 2 ? C17 C18 1.53(3) . ? C17 C18 1.55(3) 2 ? C18 C17 1.55(3) 2 ? C19 C19 0.76(4) 2 ? C19 C20 1.47(3) . ? C19 C20 1.55(3) 2 ? C20 C19 1.55(3) 2 ? 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 O8 Zn1 O7 82.2(3) . . ? O8 Zn1 O6 122.9(2) . . ? O7 Zn1 O6 129.75(19) . . ? O8 Zn1 O5 129.0(2) . . ? O7 Zn1 O5 122.7(2) . . ? O6 Zn1 O5 77.3(3) . . ? O8 Zn1 Zn1 41.07(17) . 2 ? O7 Zn1 Zn1 41.17(18) . 2 ? O6 Zn1 Zn1 141.73(17) . 2 ? O5 Zn1 Zn1 141.0(2) . 2 ? O8 Zn1 Al1 139.03(18) . . ? O7 Zn1 Al1 138.73(19) . . ? O6 Zn1 Al1 38.55(17) . . ? O5 Zn1 Al1 38.8(2) . . ? Zn1 Zn1 Al1 179.71(8) 2 . ? O6 Al1 O5 81.7(3) . . ? O6 Al1 O2 94.1(3) . . ? O5 Al1 O2 175.7(3) . . ? O6 Al1 O1 93.7(3) . . ? O5 Al1 O1 90.6(3) . . ? O2 Al1 O1 90.3(3) . . ? O6 Al1 O4 90.3(3) . . ? O5 Al1 O4 92.6(3) . . ? O2 Al1 O4 86.8(3) . . ? O1 Al1 O4 175.2(3) . . ? O6 Al1 O3 176.3(3) . . ? O5 Al1 O3 94.7(3) . . ? O2 Al1 O3 89.6(3) . . ? O1 Al1 O3 86.6(3) . . ? O4 Al1 O3 89.6(3) . . ? O6 Al1 Zn1 40.7(2) . . ? O5 Al1 Zn1 40.94(18) . . ? O2 Al1 Zn1 134.8(2) . . ? O1 Al1 Zn1 93.2(2) . . ? O4 Al1 Zn1 91.5(2) . . ? O3 Al1 Zn1 135.6(2) . . ? C1 O1 Al1 128.7(7) . . ? C4 O2 Al1 131.0(8) . . ? C6 O3 Al1 129.1(6) . . ? C9 O4 Al1 129.3(6) . . ? C11 O5 Al1 131.0(6) . . ? C11 O5 Zn1 128.3(6) . . ? Al1 O5 Zn1 100.3(3) . . ? C14 O6 Al1 129.1(6) . . ? C14 O6 Zn1 129.4(5) . . ? Al1 O6 Zn1 100.7(3) . . ? C17 O7 C17 35.4(14) 2 . ? C17 O7 Zn1 130.9(10) 2 . ? C17 O7 Zn1 126.8(10) . . ? C17 O7 Zn1 126.8(10) 2 2 ? C17 O7 Zn1 130.9(10) . 2 ? Zn1 O7 Zn1 97.7(4) . 2 ? C19 O8 C19 31.0(17) . 2 ? C19 O8 Zn1 133.3(12) . 2 ? C19 O8 Zn1 125.5(12) 2 2 ? C19 O8 Zn1 125.5(12) . . ? C19 O8 Zn1 133.3(12) 2 . ? Zn1 O8 Zn1 97.9(3) 2 . ? O1 C1 C3 123.7(10) . . ? O1 C1 C2 115.2(12) . . ? C3 C1 C2 121.0(13) . . ? C4 C3 C1 125.7(12) . . ? O2 C4 C3 120.6(12) . . ? O2 C4 C5 117.6(11) . . ? C3 C4 C5 121.6(14) . . ? O3 C6 C8 123.4(9) . . ? O3 C6 C7 115.1(10) . . ? C8 C6 C7 121.5(10) . . ? C9 C8 C6 125.1(9) . . ? O4 C9 C8 123.2(9) . . ? O4 C9 C10 115.4(9) . . ? C8 C9 C10 121.4(10) . . ? O5 C11 C13 111.6(8) . . ? O5 C11 C12 109.9(8) . . ? C13 C11 C12 112.5(11) . . ? C15 C14 O6 109.5(11) . . ? C15 C14 C16 111.6(13) . . ? O6 C14 C16 109.7(10) . . ? C17 C17 O7 72.3(7) 2 . ? C17 C17 C18 75(3) 2 . ? O7 C17 C18 109.9(16) . . ? C17 C17 C18 72(3) 2 2 ? O7 C17 C18 108.7(15) . 2 ? C18 C17 C18 116.5(16) . 2 ? C17 C18 C17 33.7(13) . 2 ? C19 C19 O8 74.5(9) 2 . ? C19 C19 C20 81(4) 2 . ? O8 C19 C20 114.9(18) . . ? C19 C19 C20 70(4) 2 2 ? O8 C19 C20 110.4(18) . 2 ? C20 C19 C20 115.7(16) . 2 ? C19 C20 C19 29.2(16) . 2 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.558 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.090 data_nial10 _database_code_CSD 189544 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H44 Ni2 O10' _chemical_formula_weight 634.03 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' '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 9.335(7) _cell_length_b 8.508(6) _cell_length_c 19.213(14) _cell_angle_alpha 90.00 _cell_angle_beta 97.51(2) _cell_angle_gamma 90.00 _cell_volume 1513.0(19) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1263 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 20.00 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 1.294 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min 0.6601 _exptl_absorpt_correction_T_max 0.7818 _exptl_absorpt_process_details ? _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 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2209 _diffrn_reflns_av_R_equivalents 0.1163 _diffrn_reflns_av_sigmaI/netI 0.1671 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 20.00 _reflns_number_total 1263 _reflns_number_gt 665 _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^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1263 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1354 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1350 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _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 0.55142(16) 0.92629(18) 0.07561(8) 0.0417(7) Uani 1 1 d . . . O1 O 0.4452(8) 0.7236(9) 0.0252(4) 0.048(2) Uani 1 1 d . . . O2 O 0.4636(9) 0.9175(10) 0.1632(4) 0.054(3) Uani 1 1 d . . . O3 O 0.3830(8) 1.0528(9) 0.0257(4) 0.036(2) Uani 1 1 d . . . O4 O 0.7120(9) 0.8007(9) 0.1264(5) 0.050(3) Uani 1 1 d . . . O5 O 0.6600(9) 1.1281(8) 0.1006(4) 0.046(2) Uani 1 1 d . . . C10 C 0.3629(14) 0.5998(18) 0.0507(7) 0.065(4) Uani 1 1 d . . . H10A H 0.3579 0.5183 0.0144 0.078 Uiso 1 1 calc R . . C11 C 0.4399(14) 0.5277(14) 0.1123(7) 0.073(5) Uani 1 1 d . . . H11A H 0.3826 0.4443 0.1279 0.110 Uiso 1 1 calc R . . H11B H 0.4588 0.6048 0.1488 0.110 Uiso 1 1 calc R . . H11C H 0.5297 0.4857 0.1012 0.110 Uiso 1 1 calc R . . C12 C 0.2126(14) 0.6420(15) 0.0549(7) 0.093(6) Uani 1 1 d . . . H12A H 0.1631 0.5536 0.0717 0.139 Uiso 1 1 calc R . . H12B H 0.1664 0.6714 0.0092 0.139 Uiso 1 1 calc R . . H12C H 0.2094 0.7287 0.0866 0.139 Uiso 1 1 calc R . . C21 C 0.8288(12) 1.3033(16) 0.1613(6) 0.074(5) Uani 1 1 d . . . H21A H 0.7675 1.3775 0.1341 0.111 Uiso 1 1 calc R . . H21B H 0.9253 1.3117 0.1495 0.111 Uiso 1 1 calc R . . H21C H 0.8293 1.3252 0.2103 0.111 Uiso 1 1 calc R . . C22 C 0.7733(14) 1.141(2) 0.1457(7) 0.047(4) Uani 1 1 d . . . C23 C 0.8445(14) 1.013(2) 0.1790(7) 0.049(5) Uani 1 1 d . . . H23A H 0.9219 1.0355 0.2131 0.059 Uiso 1 1 calc R . . C24 C 0.8139(14) 0.858(2) 0.1674(7) 0.042(4) Uani 1 1 d . . . C25 C 0.9137(13) 0.7357(14) 0.2039(7) 0.073(5) Uani 1 1 d . . . H25A H 0.8781 0.6328 0.1904 0.109 Uiso 1 1 calc R . . H25B H 0.9178 0.7476 0.2538 0.109 Uiso 1 1 calc R . . H25C H 1.0087 0.7487 0.1908 0.109 Uiso 1 1 calc R . . C31 C 0.2969(12) 0.9546(14) 0.2449(6) 0.060(4) Uani 1 1 d . . . H31A H 0.3675 0.8939 0.2742 0.090 Uiso 1 1 calc R . . H31B H 0.2058 0.9006 0.2398 0.090 Uiso 1 1 calc R . . H31C H 0.2864 1.0555 0.2660 0.090 Uiso 1 1 calc R . . C32 C 0.3453(17) 0.9763(15) 0.1736(7) 0.047(4) Uani 1 1 d . . . C33 C 0.2547(14) 1.0620(17) 0.1242(8) 0.057(4) Uani 1 1 d . . . H33A H 0.1720 1.1039 0.1392 0.069 Uiso 1 1 calc R . . C34 C 0.2742(13) 1.0920(14) 0.0549(8) 0.041(4) Uani 1 1 d . . . C35 C 0.1568(12) 1.1767(15) 0.0075(7) 0.074(5) Uani 1 1 d . . . H35A H 0.1860 1.1890 -0.0383 0.112 Uiso 1 1 calc R . . H35B H 0.1408 1.2783 0.0268 0.112 Uiso 1 1 calc R . . H35C H 0.0691 1.1167 0.0039 0.112 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 0.0385(10) 0.0345(12) 0.0493(11) 0.0023(11) -0.0049(7) 0.0024(12) O1 0.058(6) 0.020(6) 0.064(6) 0.009(5) -0.002(5) -0.018(5) O2 0.047(6) 0.058(7) 0.055(6) 0.005(5) -0.008(5) 0.013(6) O3 0.025(5) 0.028(6) 0.054(6) 0.004(5) 0.005(4) 0.017(5) O4 0.039(6) 0.040(6) 0.067(6) 0.009(5) -0.011(5) 0.014(5) O5 0.058(6) 0.024(6) 0.054(6) -0.003(4) -0.007(5) -0.008(5) C10 0.054(10) 0.066(13) 0.072(11) 0.029(9) -0.007(9) -0.004(10) C11 0.101(11) 0.052(11) 0.072(11) 0.022(9) 0.033(10) -0.010(9) C12 0.046(10) 0.100(14) 0.131(16) -0.005(10) 0.011(10) -0.020(9) C21 0.070(11) 0.047(13) 0.093(13) -0.012(9) -0.033(9) -0.018(10) C22 0.034(9) 0.045(15) 0.057(11) -0.019(10) -0.013(8) -0.007(9) C23 0.056(11) 0.022(14) 0.061(11) -0.001(9) -0.024(8) -0.005(10) C24 0.033(9) 0.045(14) 0.041(10) 0.009(9) -0.016(8) 0.010(9) C25 0.065(10) 0.058(11) 0.088(11) 0.011(9) -0.017(9) 0.019(9) C31 0.060(9) 0.070(11) 0.049(9) 0.005(9) 0.006(8) -0.006(9) C32 0.064(11) 0.024(11) 0.051(11) 0.010(8) 0.002(10) -0.014(8) C33 0.057(10) 0.069(11) 0.051(10) -0.010(10) 0.027(9) -0.005(10) C34 0.022(8) 0.022(10) 0.075(12) 0.003(9) -0.006(9) 0.004(8) C35 0.045(9) 0.111(13) 0.069(10) 0.011(10) 0.014(8) 0.034(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.968(9) . ? Ni1 O4 1.990(8) . ? Ni1 O5 2.019(8) . ? Ni1 O3 2.038(7) . ? Ni1 O3 2.123(8) 3_675 ? Ni1 O1 2.154(8) . ? O1 C10 1.427(13) . ? O2 C32 1.252(14) . ? O3 C34 1.268(13) . ? O3 Ni1 2.123(8) 3_675 ? O4 C24 1.253(14) . ? O5 C22 1.281(13) . ? C10 C11 1.439(15) . ? C10 C12 1.462(15) . ? C21 C22 1.494(14) . ? C22 C23 1.387(15) . ? C23 C24 1.359(15) . ? C24 C25 1.509(14) . ? C31 C32 1.509(15) . ? C32 C33 1.392(16) . ? C33 C34 1.390(15) . ? C34 C35 1.513(15) . ? 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 O2 Ni1 O4 86.1(4) . . ? O2 Ni1 O5 94.7(3) . . ? O4 Ni1 O5 91.0(3) . . ? O2 Ni1 O3 92.3(3) . . ? O4 Ni1 O3 178.3(3) . . ? O5 Ni1 O3 89.7(3) . . ? O2 Ni1 O3 171.8(3) . 3_675 ? O4 Ni1 O3 101.9(3) . 3_675 ? O5 Ni1 O3 87.2(3) . 3_675 ? O3 Ni1 O3 79.7(3) . 3_675 ? O2 Ni1 O1 97.8(3) . . ? O4 Ni1 O1 93.6(3) . . ? O5 Ni1 O1 167.0(3) . . ? O3 Ni1 O1 86.0(3) . . ? O3 Ni1 O1 80.0(3) 3_675 . ? C10 O1 Ni1 132.4(8) . . ? C32 O2 Ni1 126.5(9) . . ? C34 O3 Ni1 123.0(8) . . ? C34 O3 Ni1 136.7(8) . 3_675 ? Ni1 O3 Ni1 100.3(3) . 3_675 ? C24 O4 Ni1 124.0(9) . . ? C22 O5 Ni1 125.2(9) . . ? C11 C10 C12 116.1(13) . . ? C11 C10 O1 111.3(10) . . ? C12 C10 O1 113.6(12) . . ? O5 C22 C23 123.4(13) . . ? O5 C22 C21 116.6(13) . . ? C23 C22 C21 120.0(12) . . ? C24 C23 C22 127.3(13) . . ? O4 C24 C23 127.5(13) . . ? O4 C24 C25 113.2(14) . . ? C23 C24 C25 119.3(14) . . ? O2 C32 C33 124.9(13) . . ? O2 C32 C31 118.1(13) . . ? C33 C32 C31 117.1(13) . . ? C34 C33 C32 127.2(12) . . ? O3 C34 C33 126.0(11) . . ? O3 C34 C35 114.7(13) . . ? C33 C34 C35 119.3(13) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.407 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.089