Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'L. Cronin' 'S. J. Clark' 'S. Parsons' 'T. Nakamura' 'N. Robertson' _publ_contact_author_name 'Dr Neil Robertson' _publ_contact_author_address ; Dr Neil Robertson Department of Chemistry Imperial College of Science, Technology & Medicine Exhibtion Road London SW7 2AY UNITED KINGDOM ; _publ_contact_author_email 'neil.robertson2@ic.ac.uk' data_rb-cath _database_code_CSD 158412 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H72 Ni O12 Rb2 S10' _chemical_formula_weight 1367.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Rb' 'Rb' -0.9393 2.9676 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 14.636(7) _cell_length_b 8.484(6) _cell_length_c 24.440(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.71(3) _cell_angle_gamma 90.00 _cell_volume 3024(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 2.318 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 6966 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.66 _reflns_number_total 6966 _reflns_number_gt 4187 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+1.5000P] 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 6966 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1549 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Rb Rb 0.10882(3) 1.06337(5) 0.135707(17) 0.05700(14) Uani 1 1 d . . . Ni Ni 0.0000 1.0000 0.0000 0.0528(2) Uani 1 2 d S . . S1 S -0.41745(11) 0.9243(3) 0.12983(7) 0.1083(6) Uani 1 1 d . . . S2 S -0.23140(9) 0.81383(18) 0.10925(5) 0.0792(4) Uani 1 1 d . . . S3 S -0.29543(9) 1.10486(17) 0.06068(6) 0.0765(4) Uani 1 1 d . . . S4 S -0.05173(8) 0.82690(15) 0.05555(5) 0.0696(3) Uani 1 1 d . . . S5 S -0.12409(8) 1.14550(14) -0.00105(5) 0.0653(3) Uani 1 1 d . . . O1 O -0.0287(2) 1.0919(4) 0.22118(13) 0.0646(8) Uani 1 1 d . . . O2 O 0.1203(2) 0.8994(4) 0.24252(13) 0.0649(8) Uani 1 1 d . . . O3 O 0.26870(19) 0.8974(4) 0.17955(12) 0.0631(7) Uani 1 1 d . . . O4 O 0.3106(2) 1.1555(3) 0.10839(11) 0.0583(7) Uani 1 1 d . . . O5 O 0.1658(2) 1.3593(3) 0.09372(13) 0.0674(8) Uani 1 1 d . . . O6 O 0.0123(2) 1.3585(4) 0.15519(13) 0.0678(8) Uani 1 1 d . . . C1 C -0.3200(3) 0.9470(7) 0.1015(2) 0.0746(13) Uani 1 1 d . . . C2 C -0.1559(3) 0.9087(5) 0.06832(18) 0.0597(11) Uani 1 1 d . . . C3 C -0.1872(3) 1.0438(5) 0.04477(18) 0.0580(10) Uani 1 1 d . . . C4 C -0.1659(4) 0.8760(8) 0.2633(2) 0.0912(17) Uani 1 1 d . . . H4A H -0.2206 0.8522 0.2817 0.109 Uiso 1 1 calc R . . H4B H -0.1846 0.9312 0.2294 0.109 Uiso 1 1 calc R . . C5 C -0.1179(4) 0.7239(7) 0.2502(3) 0.0936(17) Uani 1 1 d . . . H5A H -0.1573 0.6635 0.2242 0.112 Uiso 1 1 calc R . . H5B H -0.1077 0.6619 0.2835 0.112 Uiso 1 1 calc R . . C6 C -0.0253(3) 0.7532(6) 0.2262(2) 0.0737(13) Uani 1 1 d . . . H6A H 0.0059 0.6536 0.2222 0.088 Uiso 1 1 calc R . . H6B H -0.0359 0.8006 0.1901 0.088 Uiso 1 1 calc R . . C7 C 0.0343(3) 0.8616(5) 0.26340(18) 0.0612(10) Uani 1 1 d . . . H7 H 0.0471 0.8083 0.2988 0.073 Uiso 1 1 calc R . . C8 C 0.1838(3) 0.7745(6) 0.2463(2) 0.0718(12) Uani 1 1 d . . . H8A H 0.1630 0.6913 0.2211 0.086 Uiso 1 1 calc R . . H8B H 0.1879 0.7316 0.2833 0.086 Uiso 1 1 calc R . . C9 C 0.2760(3) 0.8306(6) 0.23295(19) 0.0655(11) Uani 1 1 d . . . H9A H 0.2989 0.9089 0.2596 0.079 Uiso 1 1 calc R . . H9B H 0.3188 0.7430 0.2344 0.079 Uiso 1 1 calc R . . C10 C 0.3551(3) 0.9241(5) 0.15843(19) 0.0605(11) Uani 1 1 d . . . H10A H 0.3873 0.8248 0.1558 0.073 Uiso 1 1 calc R . . H10B H 0.3920 0.9928 0.1830 0.073 Uiso 1 1 calc R . . C11 C 0.3407(3) 0.9983(5) 0.10285(18) 0.0624(11) Uani 1 1 d . . . H11A H 0.3976 0.9971 0.0851 0.075 Uiso 1 1 calc R . . H11B H 0.2952 0.9391 0.0802 0.075 Uiso 1 1 calc R . . C12 C 0.2922(3) 1.2360(6) 0.05653(17) 0.0640(11) Uani 1 1 d . . . H12 H 0.2497 1.1721 0.0327 0.077 Uiso 1 1 calc R . . C13 C 0.3795(4) 1.2649(7) 0.02729(19) 0.0802(14) Uani 1 1 d . . . H13A H 0.4098 1.1652 0.0218 0.096 Uiso 1 1 calc R . . H13B H 0.3632 1.3113 -0.0085 0.096 Uiso 1 1 calc R . . C14 C 0.4450(4) 1.3746(7) 0.0607(2) 0.0864(16) Uani 1 1 d . . . H14A H 0.4652 1.3246 0.0953 0.104 Uiso 1 1 calc R . . H14B H 0.4986 1.3939 0.0408 0.104 Uiso 1 1 calc R . . C15 C 0.3992(4) 1.5292(7) 0.0717(2) 0.0891(17) Uani 1 1 d . . . H15A H 0.3846 1.5841 0.0373 0.107 Uiso 1 1 calc R . . H15B H 0.4411 1.5947 0.0946 0.107 Uiso 1 1 calc R . . C16 C 0.3116(4) 1.5034(6) 0.1004(2) 0.0733(13) Uani 1 1 d . . . H16A H 0.3270 1.4602 0.1367 0.088 Uiso 1 1 calc R . . H16B H 0.2811 1.6037 0.1045 0.088 Uiso 1 1 calc R . . C17 C 0.2469(3) 1.3914(5) 0.06768(18) 0.0649(11) Uani 1 1 d . . . H17 H 0.2289 1.4410 0.0322 0.078 Uiso 1 1 calc R . . C18 C 0.1034(4) 1.4882(6) 0.0933(3) 0.0872(16) Uani 1 1 d . . . H18A H 0.1016 1.5420 0.0582 0.105 Uiso 1 1 calc R . . H18B H 0.1236 1.5628 0.1218 0.105 Uiso 1 1 calc R . . C19 C 0.0105(4) 1.4282(6) 0.1028(2) 0.0812(15) Uani 1 1 d . . . H19A H -0.0332 1.5144 0.1002 0.097 Uiso 1 1 calc R . . H19B H -0.0088 1.3509 0.0749 0.097 Uiso 1 1 calc R . . C20 C -0.0767(3) 1.3129(6) 0.1681(2) 0.0789(14) Uani 1 1 d . . . H20A H -0.1022 1.2369 0.1414 0.095 Uiso 1 1 calc R . . H20B H -0.1167 1.4041 0.1671 0.095 Uiso 1 1 calc R . . C21 C -0.0704(4) 1.2420(6) 0.2238(2) 0.0814(15) Uani 1 1 d . . . H21A H -0.0341 1.3092 0.2493 0.098 Uiso 1 1 calc R . . H21B H -0.1311 1.2316 0.2365 0.098 Uiso 1 1 calc R . . C22 C -0.0135(3) 1.0142(6) 0.27358(18) 0.0635(11) Uani 1 1 d . . . H22 H 0.0264 1.0799 0.2984 0.076 Uiso 1 1 calc R . . C23 C -0.1027(4) 0.9811(7) 0.2999(2) 0.0841(16) Uani 1 1 d . . . H23A H -0.0888 0.9300 0.3351 0.101 Uiso 1 1 calc R . . H23B H -0.1334 1.0799 0.3063 0.101 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 Rb 0.0551(2) 0.0489(2) 0.0676(3) 0.00603(18) 0.00891(18) 0.00331(17) Ni 0.0492(4) 0.0524(4) 0.0569(4) 0.0069(3) 0.0046(3) -0.0023(3) S1 0.0725(9) 0.1542(18) 0.1032(11) 0.0029(11) 0.0368(8) -0.0109(10) S2 0.0629(7) 0.1027(10) 0.0729(8) 0.0242(7) 0.0117(6) -0.0083(7) S3 0.0606(7) 0.0800(8) 0.0910(9) -0.0052(7) 0.0195(6) 0.0051(6) S4 0.0567(6) 0.0670(7) 0.0860(8) 0.0257(6) 0.0124(6) 0.0033(5) S5 0.0581(6) 0.0562(6) 0.0830(8) 0.0121(6) 0.0136(5) 0.0013(5) O1 0.0629(18) 0.0602(18) 0.0727(19) 0.0011(14) 0.0180(15) 0.0080(14) O2 0.0615(17) 0.0602(18) 0.0752(19) 0.0172(15) 0.0191(15) 0.0044(14) O3 0.0500(15) 0.0678(18) 0.0727(19) 0.0171(15) 0.0111(13) 0.0070(14) O4 0.0669(18) 0.0476(15) 0.0619(16) 0.0003(13) 0.0149(13) 0.0011(13) O5 0.0705(19) 0.0485(17) 0.084(2) 0.0169(15) 0.0112(16) 0.0002(14) O6 0.0615(18) 0.0568(18) 0.085(2) 0.0066(16) 0.0040(15) 0.0053(15) C1 0.061(3) 0.098(4) 0.066(3) -0.006(3) 0.012(2) -0.009(3) C2 0.050(2) 0.070(3) 0.060(2) 0.008(2) 0.0049(18) -0.009(2) C3 0.052(2) 0.060(3) 0.062(2) -0.001(2) 0.0093(19) -0.0068(19) C4 0.058(3) 0.115(5) 0.102(4) 0.006(4) 0.020(3) -0.019(3) C5 0.084(4) 0.091(4) 0.106(4) 0.018(3) 0.007(3) -0.033(3) C6 0.080(3) 0.057(3) 0.085(3) 0.004(2) 0.012(3) -0.009(2) C7 0.055(2) 0.065(3) 0.064(3) 0.014(2) 0.0101(19) -0.006(2) C8 0.079(3) 0.056(3) 0.083(3) 0.015(2) 0.023(2) 0.009(2) C9 0.063(3) 0.063(3) 0.071(3) 0.016(2) 0.007(2) 0.015(2) C10 0.045(2) 0.054(2) 0.083(3) -0.002(2) 0.012(2) 0.0084(18) C11 0.057(2) 0.062(3) 0.070(3) -0.004(2) 0.016(2) 0.005(2) C12 0.076(3) 0.065(3) 0.051(2) 0.000(2) 0.006(2) -0.013(2) C13 0.099(4) 0.083(3) 0.062(3) 0.001(3) 0.029(3) -0.012(3) C14 0.081(3) 0.103(4) 0.078(3) 0.003(3) 0.026(3) -0.025(3) C15 0.101(4) 0.080(4) 0.089(4) 0.001(3) 0.026(3) -0.035(3) C16 0.089(4) 0.057(3) 0.075(3) -0.003(2) 0.015(3) -0.015(3) C17 0.081(3) 0.054(2) 0.060(2) 0.014(2) 0.006(2) -0.009(2) C18 0.095(4) 0.051(3) 0.118(4) 0.025(3) 0.018(3) 0.007(3) C19 0.073(3) 0.064(3) 0.106(4) 0.027(3) 0.002(3) 0.015(2) C20 0.057(3) 0.069(3) 0.112(4) 0.008(3) 0.013(3) 0.017(2) C21 0.068(3) 0.077(3) 0.102(4) 0.000(3) 0.027(3) 0.018(3) C22 0.058(2) 0.072(3) 0.062(3) 0.000(2) 0.014(2) -0.009(2) C23 0.066(3) 0.111(4) 0.079(3) 0.001(3) 0.024(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 Rb O5 2.862(3) . ? Rb O3 2.863(3) . ? Rb O6 2.933(3) . ? Rb O2 2.950(3) . ? Rb O1 3.027(3) . ? Rb O4 3.178(3) . ? Rb C19 3.480(5) . ? Rb S4 3.5538(19) . ? Rb C20 3.582(5) . ? Rb C11 3.593(5) . ? Rb Ni 3.5999(12) . ? Rb C12 3.734(5) . ? Ni S4 2.1776(14) 3_575 ? Ni S4 2.1776(14) . ? Ni S5 2.1944(14) 3_575 ? Ni S5 2.1944(14) . ? Ni Rb 3.5999(12) 3_575 ? S1 C1 1.647(5) . ? S2 C1 1.719(6) . ? S2 C2 1.747(4) . ? S3 C1 1.725(6) . ? S3 C3 1.741(4) . ? S4 C2 1.727(5) . ? S5 C3 1.738(4) . ? S5 Rb 3.7605(17) 3_575 ? O1 C21 1.416(6) . ? O1 C22 1.441(5) . ? O2 C8 1.408(5) . ? O2 C7 1.433(5) . ? O3 C9 1.419(5) . ? O3 C10 1.422(5) . ? O4 C11 1.414(5) . ? O4 C12 1.445(5) . ? O5 C17 1.418(5) . ? O5 C18 1.424(6) . ? O6 C19 1.409(6) . ? O6 C20 1.419(6) . ? C2 C3 1.346(6) . ? C4 C5 1.515(8) . ? C4 C23 1.522(8) . ? C5 C6 1.541(7) . ? C6 C7 1.518(6) . ? C7 C22 1.503(7) . ? C8 C9 1.493(6) . ? C10 C11 1.497(6) . ? C12 C17 1.510(7) . ? C12 C13 1.534(6) . ? C13 C14 1.525(7) . ? C14 C15 1.507(8) . ? C15 C16 1.527(7) . ? C16 C17 1.521(6) . ? C18 C19 1.489(7) . ? C20 C21 1.483(7) . ? C22 C23 1.527(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 O5 Rb O3 108.19(9) . . ? O5 Rb O6 57.84(10) . . ? O3 Rb O6 138.49(9) . . ? O5 Rb O2 137.18(9) . . ? O3 Rb O2 56.74(8) . . ? O6 Rb O2 104.60(9) . . ? O5 Rb O1 114.02(9) . . ? O3 Rb O1 110.51(9) . . ? O6 Rb O1 57.54(9) . . ? O2 Rb O1 54.54(8) . . ? O5 Rb O4 53.54(8) . . ? O3 Rb O4 56.94(8) . . ? O6 Rb O4 107.00(9) . . ? O2 Rb O4 108.38(8) . . ? O1 Rb O4 143.82(8) . . ? O5 Rb C19 42.62(11) . . ? O3 Rb C19 146.51(11) . . ? O6 Rb C19 23.46(11) . . ? O2 Rb C19 128.06(12) . . ? O1 Rb C19 78.62(11) . . ? O4 Rb C19 96.12(11) . . ? O5 Rb S4 119.77(7) . . ? O3 Rb S4 114.33(8) . . ? O6 Rb S4 105.42(8) . . ? O2 Rb S4 102.05(8) . . ? O1 Rb S4 88.78(7) . . ? O4 Rb S4 127.36(6) . . ? C19 Rb S4 97.60(11) . . ? O5 Rb C20 79.02(11) . . ? O3 Rb C20 144.97(11) . . ? O6 Rb C20 22.45(10) . . ? O2 Rb C20 94.13(11) . . ? O1 Rb C20 40.64(10) . . ? O4 Rb C20 129.44(11) . . ? C19 Rb C20 38.65(12) . . ? S4 Rb C20 88.66(10) . . ? O5 Rb C11 75.30(10) . . ? O3 Rb C11 41.42(9) . . ? O6 Rb C11 130.06(10) . . ? O2 Rb C11 97.99(10) . . ? O1 Rb C11 149.32(10) . . ? O4 Rb C11 23.08(9) . . ? C19 Rb C11 117.73(11) . . ? S4 Rb C11 112.58(8) . . ? C20 Rb C11 152.49(12) . . ? O5 Rb Ni 85.45(7) . . ? O3 Rb Ni 123.90(7) . . ? O6 Rb Ni 95.42(7) . . ? O2 Rb Ni 137.19(7) . . ? O1 Rb Ni 112.26(7) . . ? O4 Rb Ni 101.05(6) . . ? C19 Rb Ni 77.07(10) . . ? S4 Rb Ni 35.44(2) . . ? C20 Rb Ni 90.34(10) . . ? C11 Rb Ni 97.22(8) . . ? O5 Rb C12 39.40(10) . . ? O3 Rb C12 77.68(10) . . ? O6 Rb C12 97.21(11) . . ? O2 Rb C12 130.71(9) . . ? O1 Rb C12 150.82(9) . . ? O4 Rb C12 22.33(8) . . ? C19 Rb C12 80.36(12) . . ? S4 Rb C12 113.98(7) . . ? C20 Rb C12 118.22(12) . . ? C11 Rb C12 38.04(11) . . ? Ni Rb C12 82.15(7) . . ? S4 Ni S4 180.00(5) 3_575 . ? S4 Ni S5 93.26(6) 3_575 3_575 ? S4 Ni S5 86.74(6) . 3_575 ? S4 Ni S5 86.74(6) 3_575 . ? S4 Ni S5 93.26(6) . . ? S5 Ni S5 180.00(3) 3_575 . ? S4 Ni Rb 71.13(4) 3_575 3_575 ? S4 Ni Rb 108.87(4) . 3_575 ? S5 Ni Rb 103.30(4) 3_575 3_575 ? S5 Ni Rb 76.70(4) . 3_575 ? S4 Ni Rb 108.87(4) 3_575 . ? S4 Ni Rb 71.13(4) . . ? S5 Ni Rb 76.70(4) 3_575 . ? S5 Ni Rb 103.30(4) . . ? Rb Ni Rb 180.000(6) 3_575 . ? C1 S2 C2 98.1(2) . . ? C1 S3 C3 97.7(2) . . ? C2 S4 Ni 101.46(16) . . ? C2 S4 Rb 103.11(16) . . ? Ni S4 Rb 73.44(5) . . ? C3 S5 Ni 101.32(16) . . ? C3 S5 Rb 113.76(15) . 3_575 ? Ni S5 Rb 68.69(4) . 3_575 ? C21 O1 C22 114.0(4) . . ? C21 O1 Rb 114.6(3) . . ? C22 O1 Rb 121.0(2) . . ? C8 O2 C7 113.7(3) . . ? C8 O2 Rb 113.8(2) . . ? C7 O2 Rb 115.7(2) . . ? C9 O3 C10 113.3(3) . . ? C9 O3 Rb 122.6(2) . . ? C10 O3 Rb 120.6(2) . . ? C11 O4 C12 113.5(3) . . ? C11 O4 Rb 95.2(2) . . ? C12 O4 Rb 101.0(2) . . ? C17 O5 C18 114.1(3) . . ? C17 O5 Rb 127.5(3) . . ? C18 O5 Rb 118.1(3) . . ? C19 O6 C20 111.6(4) . . ? C19 O6 Rb 100.6(3) . . ? C20 O6 Rb 105.4(3) . . ? S1 C1 S2 123.2(3) . . ? S1 C1 S3 124.2(3) . . ? S2 C1 S3 112.5(3) . . ? C3 C2 S4 122.7(3) . . ? C3 C2 S2 115.3(3) . . ? S4 C2 S2 121.8(3) . . ? C2 C3 S5 121.2(3) . . ? C2 C3 S3 116.2(3) . . ? S5 C3 S3 122.5(3) . . ? C5 C4 C23 110.6(5) . . ? C4 C5 C6 112.4(4) . . ? C7 C6 C5 110.4(4) . . ? O2 C7 C22 107.5(4) . . ? O2 C7 C6 113.6(4) . . ? C22 C7 C6 111.6(4) . . ? O2 C8 C9 110.4(4) . . ? O2 C8 Rb 46.11(19) . . ? C9 C8 Rb 81.4(2) . . ? O3 C9 C8 109.1(4) . . ? O3 C10 C11 109.5(3) . . ? O4 C11 C10 109.4(3) . . ? O4 C11 Rb 61.74(19) . . ? C10 C11 Rb 85.8(2) . . ? O4 C12 C17 107.9(3) . . ? O4 C12 C13 112.4(4) . . ? C17 C12 C13 109.8(4) . . ? O4 C12 Rb 56.66(19) . . ? C17 C12 Rb 84.5(2) . . ? C13 C12 Rb 164.9(3) . . ? C14 C13 C12 111.1(4) . . ? C15 C14 C13 110.9(5) . . ? C14 C15 C16 111.1(4) . . ? C17 C16 C15 111.1(4) . . ? O5 C17 C12 108.0(3) . . ? O5 C17 C16 113.1(4) . . ? C12 C17 C16 112.2(4) . . ? O5 C18 C19 109.3(4) . . ? O5 C18 Rb 42.3(2) . . ? C19 C18 Rb 68.1(2) . . ? O6 C19 C18 109.6(4) . . ? O6 C19 Rb 55.9(2) . . ? C18 C19 Rb 88.5(3) . . ? O6 C20 C21 109.0(4) . . ? O6 C20 Rb 52.1(2) . . ? C21 C20 Rb 88.4(3) . . ? O1 C21 C20 108.6(4) . . ? O1 C22 C7 106.7(3) . . ? O1 C22 C23 112.6(4) . . ? C7 C22 C23 109.7(4) . . ? C4 C23 C22 111.1(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.66 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.991 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.079 #===END data_nrrbo1 _database_code_CSD 158413 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H36 Ni O6 Rb S10' _chemical_formula_weight 909.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.706(3) _cell_length_b 10.846(3) _cell_length_c 16.196(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.999(17) _cell_angle_gamma 90.00 _cell_volume 1798.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 64 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Black _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 930 _exptl_absorpt_coefficient_mu 8.168 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.109 _exptl_absorpt_correction_T_max 0.291 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 3245 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.43 _diffrn_reflns_theta_max 70.19 _reflns_number_total 3234 _reflns_number_gt 2885 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.3821P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3234 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1282 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.5000 0.0270(2) Uani 1 2 d S . . S1 S 0.13156(8) -0.10588(7) 0.44829(5) 0.0345(2) Uani 1 1 d . . . C2 C 0.1505(3) -0.0099(3) 0.3685(2) 0.0307(7) Uani 1 1 d . . . S3 S 0.24409(8) -0.04813(8) 0.29960(5) 0.0403(2) Uani 1 1 d . . . C4 C 0.2161(3) 0.0862(3) 0.2386(2) 0.0377(7) Uani 1 1 d . . . S4 S 0.27955(10) 0.11521(11) 0.15908(6) 0.0541(3) Uani 1 1 d . . . S5 S 0.11444(8) 0.18812(8) 0.26943(5) 0.0382(2) Uani 1 1 d . . . C6 C 0.0887(3) 0.1007(3) 0.35296(19) 0.0305(6) Uani 1 1 d . . . S7 S -0.01233(7) 0.14896(6) 0.41091(5) 0.0309(2) Uani 1 1 d . . . Rb1 Rb 1.0000 0.0000 0.0000 0.0513(2) Uani 1 2 d S . . C1C C 0.9886(3) 0.3250(3) -0.0343(2) 0.0382(7) Uani 1 1 d . . . H1C1 H 1.0604 0.3289 0.0204 0.046 Uiso 1 1 calc R . . H1C2 H 0.9491 0.4081 -0.0463 0.046 Uiso 1 1 calc R . . O2C O 0.8928(2) 0.2390(2) -0.02626(15) 0.0345(5) Uani 1 1 d . . . C3C C 0.8370(3) 0.2715(3) 0.0404(2) 0.0374(7) Uani 1 1 d . . . H3C1 H 0.7936 0.3528 0.0277 0.045 Uiso 1 1 calc R . . H3C2 H 0.9064 0.2775 0.0962 0.045 Uiso 1 1 calc R . . C4C C 0.7390(3) 0.1751(3) 0.0464(2) 0.0373(7) Uani 1 1 d . . . H4C1 H 0.6821 0.2079 0.0796 0.045 Uiso 1 1 calc R . . H4C2 H 0.6834 0.1537 -0.0122 0.045 Uiso 1 1 calc R . . O5C O 0.8052(2) 0.0675(2) 0.08795(14) 0.0341(5) Uani 1 1 d . . . C6C C 0.7185(3) -0.0355(3) 0.0835(2) 0.0329(7) Uani 1 1 d . . . H6C H 0.6769 -0.0574 0.0216 0.039 Uiso 1 1 calc R . . C7C C 0.6112(3) -0.0088(3) 0.1262(2) 0.0378(7) Uani 1 1 d . . . H7C1 H 0.5604 0.0640 0.0983 0.045 Uiso 1 1 calc R . . H7C2 H 0.5509 -0.0800 0.1173 0.045 Uiso 1 1 calc R . . C8C C 0.6677(4) 0.0154(3) 0.2227(2) 0.0447(8) Uani 1 1 d . . . H8C1 H 0.7203 0.0920 0.2318 0.054 Uiso 1 1 calc R . . H8C2 H 0.5956 0.0270 0.2488 0.054 Uiso 1 1 calc R . . C9C C 0.7529(4) -0.0919(3) 0.2665(2) 0.0449(8) Uani 1 1 d . . . H9C1 H 0.6980 -0.1663 0.2627 0.054 Uiso 1 1 calc R . . H9C2 H 0.7926 -0.0724 0.3283 0.054 Uiso 1 1 calc R . . C10C C 0.8605(3) -0.1186(3) 0.2251(2) 0.0388(7) Uani 1 1 d . . . H10A H 0.9117 -0.1911 0.2532 0.047 Uiso 1 1 calc R . . H10B H 0.9203 -0.0471 0.2329 0.047 Uiso 1 1 calc R . . C11C C 0.7999(3) -0.1441(3) 0.12896(19) 0.0317(6) Uani 1 1 d . . . H11C H 0.7410 -0.2172 0.1229 0.038 Uiso 1 1 calc R . . O12C O 0.8947(2) -0.1705(2) 0.08541(14) 0.0339(5) Uani 1 1 d . . . C13C C 0.9583(3) -0.2868(3) 0.1063(2) 0.0398(7) Uani 1 1 d . . . H13A H 0.8954 -0.3492 0.1143 0.048 Uiso 1 1 calc R . . H13B H 1.0303 -0.2801 0.1608 0.048 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 0.0257(4) 0.0282(4) 0.0281(4) 0.0007(3) 0.0095(3) 0.0027(2) S1 0.0378(4) 0.0347(4) 0.0345(4) 0.0050(3) 0.0161(3) 0.0103(3) C2 0.0284(15) 0.0369(16) 0.0271(15) -0.0037(11) 0.0083(12) 0.0002(11) S3 0.0396(4) 0.0497(5) 0.0364(4) 0.0006(3) 0.0188(3) 0.0068(3) C4 0.0344(16) 0.0500(19) 0.0286(16) -0.0003(13) 0.0093(13) -0.0071(14) S4 0.0595(6) 0.0721(7) 0.0394(5) -0.0014(4) 0.0284(4) -0.0101(5) S5 0.0401(4) 0.0414(4) 0.0345(4) 0.0053(3) 0.0131(3) -0.0030(3) C6 0.0276(14) 0.0317(15) 0.0305(15) -0.0005(11) 0.0057(12) -0.0021(11) S7 0.0303(4) 0.0286(4) 0.0351(4) 0.0028(3) 0.0116(3) 0.0033(3) Rb1 0.0541(4) 0.0326(3) 0.0823(4) 0.0137(2) 0.0436(3) 0.00858(19) C1C 0.0392(17) 0.0299(16) 0.0446(18) 0.0039(13) 0.0110(14) 0.0013(12) O2C 0.0339(11) 0.0319(11) 0.0389(12) 0.0007(9) 0.0123(9) 0.0009(9) C3C 0.0388(16) 0.0375(17) 0.0356(16) 0.0007(13) 0.0101(13) 0.0047(13) C4C 0.0325(15) 0.0378(17) 0.0416(17) 0.0053(13) 0.0110(13) 0.0069(13) O5C 0.0278(10) 0.0353(11) 0.0362(11) 0.0058(9) 0.0050(9) 0.0016(8) C6C 0.0252(14) 0.0385(16) 0.0314(15) -0.0032(12) 0.0025(12) -0.0014(12) C7C 0.0306(16) 0.0368(17) 0.0455(19) -0.0061(13) 0.0103(14) -0.0036(12) C8C 0.052(2) 0.0449(19) 0.0422(19) -0.0090(15) 0.0221(17) -0.0073(15) C9C 0.056(2) 0.0455(19) 0.0336(18) -0.0050(14) 0.0130(16) -0.0090(16) C10C 0.0390(17) 0.0390(17) 0.0326(16) 0.0008(13) 0.0014(13) -0.0069(14) C11C 0.0278(14) 0.0342(15) 0.0320(15) -0.0017(12) 0.0070(12) -0.0029(11) O12C 0.0334(11) 0.0354(11) 0.0360(11) 0.0068(9) 0.0149(9) 0.0039(9) C13C 0.0400(17) 0.0361(17) 0.0440(18) 0.0104(14) 0.0133(14) 0.0050(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 Ni1 S7 2.1444(8) . ? Ni1 S7 2.1444(8) 3_556 ? Ni1 S1 2.1665(8) . ? Ni1 S1 2.1665(8) 3_556 ? S1 C2 1.717(3) . ? C2 C6 1.358(4) . ? C2 S3 1.754(3) . ? S3 C4 1.737(4) . ? C4 S4 1.652(3) . ? C4 S5 1.724(4) . ? S4 Rb1 3.5564(13) 1_455 ? S5 C6 1.739(3) . ? C6 S7 1.708(3) . ? Rb1 O12C 2.742(2) 3_755 ? Rb1 O12C 2.742(2) . ? Rb1 O2C 2.816(2) 3_755 ? Rb1 O2C 2.816(2) . ? Rb1 O5C 2.941(2) 3_755 ? Rb1 O5C 2.941(2) . ? Rb1 S4 3.5564(13) 3_655 ? Rb1 S4 3.5564(13) 1_655 ? Rb1 C1C 3.565(3) . ? Rb1 C1C 3.565(3) 3_755 ? Rb1 C3C 3.579(3) 3_755 ? Rb1 C3C 3.579(3) . ? C1C O2C 1.420(4) . ? C1C C13C 1.496(5) 3_755 ? O2C C3C 1.423(4) . ? C3C C4C 1.504(5) . ? C4C O5C 1.427(4) . ? O5C C6C 1.441(4) . ? C6C C11C 1.521(4) . ? C6C C7C 1.531(5) . ? C7C C8C 1.525(5) . ? C8C C9C 1.520(5) . ? C9C C10C 1.520(5) . ? C10C C11C 1.527(4) . ? C11C O12C 1.424(4) . ? O12C C13C 1.426(4) . ? C13C C1C 1.496(5) 3_755 ? 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 S7 Ni1 S7 180.0 . 3_556 ? S7 Ni1 S1 93.34(3) . . ? S7 Ni1 S1 86.66(3) 3_556 . ? S7 Ni1 S1 86.66(3) . 3_556 ? S7 Ni1 S1 93.34(3) 3_556 3_556 ? S1 Ni1 S1 180.00(3) . 3_556 ? C2 S1 Ni1 101.71(11) . . ? C6 C2 S1 121.1(3) . . ? C6 C2 S3 115.4(2) . . ? S1 C2 S3 123.44(18) . . ? C4 S3 C2 97.37(16) . . ? S4 C4 S5 122.8(2) . . ? S4 C4 S3 124.1(2) . . ? S5 C4 S3 113.05(19) . . ? C4 S4 Rb1 92.71(12) . 1_455 ? C4 S5 C6 97.64(16) . . ? C2 C6 S7 121.4(2) . . ? C2 C6 S5 116.5(2) . . ? S7 C6 S5 122.03(18) . . ? C6 S7 Ni1 102.39(11) . . ? O12C Rb1 O12C 180.00(11) 3_755 . ? O12C Rb1 O2C 119.18(6) 3_755 3_755 ? O12C Rb1 O2C 60.82(6) . 3_755 ? O12C Rb1 O2C 60.82(6) 3_755 . ? O12C Rb1 O2C 119.18(6) . . ? O2C Rb1 O2C 180.00(9) 3_755 . ? O12C Rb1 O5C 57.94(6) 3_755 3_755 ? O12C Rb1 O5C 122.06(6) . 3_755 ? O2C Rb1 O5C 61.89(6) 3_755 3_755 ? O2C Rb1 O5C 118.11(6) . 3_755 ? O12C Rb1 O5C 122.06(6) 3_755 . ? O12C Rb1 O5C 57.94(6) . . ? O2C Rb1 O5C 118.11(6) 3_755 . ? O2C Rb1 O5C 61.89(6) . . ? O5C Rb1 O5C 180.00(7) 3_755 . ? O12C Rb1 S4 104.75(5) 3_755 3_655 ? O12C Rb1 S4 75.25(5) . 3_655 ? O2C Rb1 S4 90.31(5) 3_755 3_655 ? O2C Rb1 S4 89.69(5) . 3_655 ? O5C Rb1 S4 97.31(5) 3_755 3_655 ? O5C Rb1 S4 82.69(5) . 3_655 ? O12C Rb1 S4 75.25(5) 3_755 1_655 ? O12C Rb1 S4 104.75(5) . 1_655 ? O2C Rb1 S4 89.69(5) 3_755 1_655 ? O2C Rb1 S4 90.31(5) . 1_655 ? O5C Rb1 S4 82.69(5) 3_755 1_655 ? O5C Rb1 S4 97.31(5) . 1_655 ? S4 Rb1 S4 180.00(3) 3_655 1_655 ? O12C Rb1 C1C 41.81(7) 3_755 . ? O12C Rb1 C1C 138.19(7) . . ? O2C Rb1 C1C 158.05(7) 3_755 . ? O2C Rb1 C1C 21.95(7) . . ? O5C Rb1 C1C 99.63(7) 3_755 . ? O5C Rb1 C1C 80.37(7) . . ? S4 Rb1 C1C 104.55(6) 3_655 . ? S4 Rb1 C1C 75.45(6) 1_655 . ? O12C Rb1 C1C 138.19(7) 3_755 3_755 ? O12C Rb1 C1C 41.81(7) . 3_755 ? O2C Rb1 C1C 21.95(7) 3_755 3_755 ? O2C Rb1 C1C 158.05(7) . 3_755 ? O5C Rb1 C1C 80.37(7) 3_755 3_755 ? O5C Rb1 C1C 99.63(7) . 3_755 ? S4 Rb1 C1C 75.45(6) 3_655 3_755 ? S4 Rb1 C1C 104.55(6) 1_655 3_755 ? C1C Rb1 C1C 180.0 . 3_755 ? O12C Rb1 C3C 99.69(7) 3_755 3_755 ? O12C Rb1 C3C 80.31(7) . 3_755 ? O2C Rb1 C3C 21.80(7) 3_755 3_755 ? O2C Rb1 C3C 158.20(7) . 3_755 ? O5C Rb1 C3C 41.76(7) 3_755 3_755 ? O5C Rb1 C3C 138.24(7) . 3_755 ? S4 Rb1 C3C 86.01(6) 3_655 3_755 ? S4 Rb1 C3C 93.99(6) 1_655 3_755 ? C1C Rb1 C3C 141.36(8) . 3_755 ? C1C Rb1 C3C 38.64(8) 3_755 3_755 ? O12C Rb1 C3C 80.31(7) 3_755 . ? O12C Rb1 C3C 99.69(7) . . ? O2C Rb1 C3C 158.20(7) 3_755 . ? O2C Rb1 C3C 21.80(7) . . ? O5C Rb1 C3C 138.24(7) 3_755 . ? O5C Rb1 C3C 41.76(7) . . ? S4 Rb1 C3C 93.99(6) 3_655 . ? S4 Rb1 C3C 86.01(6) 1_655 . ? C1C Rb1 C3C 38.64(8) . . ? C1C Rb1 C3C 141.36(8) 3_755 . ? C3C Rb1 C3C 180.00(12) 3_755 . ? O2C C1C C13C 109.8(3) . 3_755 ? O2C C1C Rb1 47.86(13) . . ? C13C C1C Rb1 81.02(18) 3_755 . ? C1C O2C C3C 112.5(2) . . ? C1C O2C Rb1 110.19(17) . . ? C3C O2C Rb1 110.87(18) . . ? O2C C3C C4C 109.4(3) . . ? O2C C3C Rb1 47.32(14) . . ? C4C C3C Rb1 80.00(18) . . ? O5C C4C C3C 109.8(3) . . ? O5C C4C Rb1 50.56(14) . . ? C3C C4C Rb1 75.95(18) . . ? C4C O5C C6C 112.7(2) . . ? C4C O5C Rb1 107.43(18) . . ? C6C O5C Rb1 108.69(17) . . ? O5C C6C C11C 107.8(2) . . ? O5C C6C C7C 112.8(3) . . ? C11C C6C C7C 109.1(3) . . ? O5C C6C Rb1 49.45(14) . . ? C11C C6C Rb1 80.99(17) . . ? C7C C6C Rb1 162.3(2) . . ? C8C C7C C6C 111.8(3) . . ? C9C C8C C7C 110.5(3) . . ? C8C C9C C10C 111.7(3) . . ? C9C C10C C11C 109.4(3) . . ? O12C C11C C6C 107.9(3) . . ? O12C C11C C10C 112.9(2) . . ? C6C C11C C10C 111.5(3) . . ? O12C C11C Rb1 36.93(13) . . ? C6C C11C Rb1 75.36(17) . . ? C10C C11C Rb1 110.58(18) . . ? C11C O12C C13C 114.9(2) . . ? C11C O12C Rb1 124.88(18) . . ? C13C O12C Rb1 118.53(18) . . ? O12C C13C C1C 108.9(3) . 3_755 ? O12C C13C Rb1 41.37(14) . . ? C1C C13C Rb1 75.05(17) 3_755 . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 70.19 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.020 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.107 #===END data_cs-cath _database_code_CSD 158414 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H72 Cs2 Ni O12 S10' _chemical_formula_weight 1462.17 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' 'S' 'S' 0.1246 0.1234 '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' 'Cs' 'Cs' -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 14.628(2) _cell_length_b 8.3769(9) _cell_length_c 24.692(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.631(11) _cell_angle_gamma 90.00 _cell_volume 3019.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 1.908 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _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 5324 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5324 _reflns_number_gt 3482 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^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 5324 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.011 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 Cs1 Cs 0.89089(2) 0.02670(4) 0.371268(13) 0.03698(11) Uani 1 1 d . . . Ni1 Ni 1.0000 0.0000 0.5000 0.0376(3) Uani 1 2 d S . . S4 S 1.11837(11) 0.15363(17) 0.48758(6) 0.0469(4) Uani 1 1 d . . . S5 S 1.05909(11) -0.20471(18) 0.46004(6) 0.0480(4) Uani 1 1 d . . . S3 S 1.23339(11) -0.2320(2) 0.40007(7) 0.0569(5) Uani 1 1 d . . . S2 S 1.28566(11) 0.0923(2) 0.42325(7) 0.0587(5) Uani 1 1 d . . . S1 S 1.40968(13) -0.1127(3) 0.36203(8) 0.0799(6) Uani 1 1 d . . . O3 O 0.6764(2) 0.1173(4) 0.38900(14) 0.0393(9) Uani 1 1 d . . . O6 O 1.0251(2) 0.0781(4) 0.28098(14) 0.0414(9) Uani 1 1 d . . . O1 O 0.8812(2) -0.1243(4) 0.25640(14) 0.0391(9) Uani 1 1 d . . . O2 O 0.7286(2) -0.1443(4) 0.31872(14) 0.0436(9) Uani 1 1 d . . . O4 O 0.8126(3) 0.3397(4) 0.40365(15) 0.0483(10) Uani 1 1 d . . . O5 O 0.9690(3) 0.3554(4) 0.34218(14) 0.0446(10) Uani 1 1 d . . . C23 C 0.9712(4) -0.1588(7) 0.2388(2) 0.0428(14) Uani 1 1 d . . . H23 H 0.9635 -0.2139 0.2038 0.051 Uiso 1 1 calc R . . C2 C 1.1825(4) 0.0305(7) 0.4481(2) 0.0430(14) Uani 1 1 d . . . C3 C 1.1573(4) -0.1207(7) 0.4366(2) 0.0413(14) Uani 1 1 d . . . C8 C 0.6897(4) 0.1967(7) 0.4403(2) 0.0460(15) Uani 1 1 d . . . H8 H 0.7341 0.1360 0.4634 0.055 Uiso 1 1 calc R . . C18 C 1.0183(4) -0.0013(6) 0.2294(2) 0.0421(14) Uani 1 1 d . . . H18 H 0.9808 0.0626 0.2033 0.051 Uiso 1 1 calc R . . C5 C 0.7257(4) -0.2037(7) 0.2643(2) 0.0442(15) Uani 1 1 d . . . H5A H 0.7037 -0.1210 0.2393 0.053 Uiso 1 1 calc R . . H5B H 0.6839 -0.2936 0.2606 0.053 Uiso 1 1 calc R . . C6 C 0.6411(3) -0.1180(6) 0.3378(2) 0.0414(14) Uani 1 1 d . . . H6A H 0.6084 -0.2185 0.3391 0.050 Uiso 1 1 calc R . . H6B H 0.6064 -0.0472 0.3131 0.050 Uiso 1 1 calc R . . C19 C 1.1121(4) -0.0345(8) 0.2069(2) 0.0571(16) Uani 1 1 d . . . H19A H 1.1033 -0.0877 0.1721 0.068 Uiso 1 1 calc R . . H19B H 1.1432 0.0659 0.2013 0.068 Uiso 1 1 calc R . . C12 C 0.6618(4) 0.4672(7) 0.3980(2) 0.0563(17) Uani 1 1 d . . . H12A H 0.6492 0.4232 0.3620 0.068 Uiso 1 1 calc R . . H12B H 0.6886 0.5721 0.3942 0.068 Uiso 1 1 calc R . . C7 C 0.6496(4) -0.0454(7) 0.3932(2) 0.0469(15) Uani 1 1 d . . . H7A H 0.5914 -0.0520 0.4099 0.056 Uiso 1 1 calc R . . H7B H 0.6949 -0.1032 0.4159 0.056 Uiso 1 1 calc R . . C4 C 0.8194(4) -0.2548(6) 0.2513(2) 0.0458(15) Uani 1 1 d . . . H4A H 0.8404 -0.3398 0.2757 0.055 Uiso 1 1 calc R . . H4B H 0.8177 -0.2958 0.2145 0.055 Uiso 1 1 calc R . . C1 C 1.3147(4) -0.0847(7) 0.3931(2) 0.0558(17) Uani 1 1 d . . . C22 C 1.0281(4) -0.2668(6) 0.2777(2) 0.0466(15) Uani 1 1 d . . . H22A H 1.0349 -0.2174 0.3133 0.056 Uiso 1 1 calc R . . H22B H 0.9971 -0.3682 0.2814 0.056 Uiso 1 1 calc R . . C15 C 0.9642(4) 0.4334(7) 0.3935(2) 0.0562(17) Uani 1 1 d . . . H15A H 1.0030 0.5274 0.3948 0.067 Uiso 1 1 calc R . . H15B H 0.9858 0.3619 0.4224 0.067 Uiso 1 1 calc R . . C16 C 1.0599(4) 0.3121(7) 0.3334(2) 0.0533(17) Uani 1 1 d . . . H16A H 1.0828 0.2395 0.3616 0.064 Uiso 1 1 calc R . . H16B H 1.0985 0.4065 0.3348 0.064 Uiso 1 1 calc R . . C13 C 0.7291(4) 0.3602(7) 0.4300(2) 0.0486(16) Uani 1 1 d . . . H13 H 0.7440 0.4108 0.4652 0.058 Uiso 1 1 calc R . . C14 C 0.8672(4) 0.4805(7) 0.4010(2) 0.0562(17) Uani 1 1 d . . . H14A H 0.8641 0.5416 0.4342 0.067 Uiso 1 1 calc R . . H14B H 0.8443 0.5467 0.3709 0.067 Uiso 1 1 calc R . . C20 C 1.1716(4) -0.1389(8) 0.2458(3) 0.067(2) Uani 1 1 d . . . H20A H 1.2294 -0.1614 0.2301 0.080 Uiso 1 1 calc R . . H20B H 1.1845 -0.0826 0.2797 0.080 Uiso 1 1 calc R . . C17 C 1.0638(4) 0.2333(7) 0.2791(2) 0.0530(17) Uani 1 1 d . . . H17A H 1.0300 0.2966 0.2516 0.064 Uiso 1 1 calc R . . H17B H 1.1269 0.2260 0.2694 0.064 Uiso 1 1 calc R . . C11 C 0.5730(5) 0.4823(9) 0.4261(3) 0.078(2) Uani 1 1 d . . . H11A H 0.5294 0.5442 0.4035 0.093 Uiso 1 1 calc R . . H11B H 0.5844 0.5386 0.4602 0.093 Uiso 1 1 calc R . . C21 C 1.1221(4) -0.2947(8) 0.2563(3) 0.0658(19) Uani 1 1 d . . . H21A H 1.1152 -0.3554 0.2229 0.079 Uiso 1 1 calc R . . H21B H 1.1590 -0.3575 0.2825 0.079 Uiso 1 1 calc R . . C10 C 0.5323(5) 0.3192(9) 0.4370(3) 0.075(2) Uani 1 1 d . . . H10A H 0.5146 0.2674 0.4028 0.090 Uiso 1 1 calc R . . H10B H 0.4777 0.3321 0.4569 0.090 Uiso 1 1 calc R . . C9 C 0.6014(4) 0.2144(8) 0.4697(2) 0.0643(19) Uani 1 1 d . . . H9A H 0.6152 0.2618 0.5051 0.077 Uiso 1 1 calc R . . H9B H 0.5749 0.1098 0.4750 0.077 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 Cs1 0.0418(2) 0.03307(18) 0.03521(18) -0.00079(17) -0.00414(13) -0.00275(18) Ni1 0.0403(6) 0.0400(7) 0.0315(5) -0.0061(4) -0.0054(4) 0.0014(5) S4 0.0504(10) 0.0404(9) 0.0503(9) -0.0057(7) 0.0067(8) 0.0011(7) S5 0.0460(9) 0.0450(9) 0.0525(9) -0.0162(7) -0.0008(8) 0.0000(7) S3 0.0518(10) 0.0677(11) 0.0509(10) -0.0198(8) 0.0012(8) 0.0093(9) S2 0.0523(10) 0.0616(11) 0.0636(11) 0.0049(9) 0.0134(9) 0.0025(8) S1 0.0594(13) 0.1087(16) 0.0739(13) -0.0084(12) 0.0226(10) 0.0110(11) O3 0.049(2) 0.032(2) 0.037(2) -0.0001(17) 0.0030(18) 0.0011(18) O6 0.043(2) 0.038(2) 0.042(2) 0.0011(17) -0.0027(18) -0.0095(18) O1 0.039(2) 0.034(2) 0.044(2) -0.0067(17) 0.0018(18) 0.0016(18) O2 0.035(2) 0.049(2) 0.046(2) -0.0120(19) 0.0010(18) -0.0045(19) O4 0.059(3) 0.033(2) 0.052(3) -0.0060(19) -0.003(2) 0.002(2) O5 0.054(3) 0.037(2) 0.042(2) -0.0033(18) -0.004(2) -0.012(2) C23 0.044(4) 0.048(4) 0.036(3) -0.005(3) -0.002(3) 0.009(3) C2 0.039(3) 0.058(4) 0.032(3) 0.004(3) -0.002(2) 0.001(3) C3 0.039(3) 0.050(4) 0.034(3) -0.005(3) -0.008(3) 0.004(3) C8 0.058(4) 0.051(4) 0.029(3) -0.001(3) -0.004(3) 0.011(3) C18 0.040(3) 0.045(4) 0.041(3) 0.006(3) -0.001(2) 0.007(3) C5 0.042(4) 0.043(3) 0.046(4) -0.009(3) -0.003(3) -0.014(3) C6 0.030(3) 0.037(3) 0.056(4) -0.003(3) 0.001(3) -0.001(3) C19 0.048(4) 0.069(4) 0.056(4) -0.002(4) 0.014(3) 0.004(4) C12 0.071(4) 0.043(3) 0.053(4) -0.009(3) -0.011(3) 0.018(3) C7 0.047(4) 0.043(4) 0.052(4) 0.006(3) 0.007(3) -0.002(3) C4 0.057(4) 0.034(3) 0.045(4) -0.010(3) 0.001(3) -0.009(3) C1 0.057(4) 0.067(4) 0.044(4) -0.004(3) 0.003(3) 0.009(3) C22 0.046(4) 0.035(3) 0.058(4) 0.002(3) 0.000(3) 0.003(3) C15 0.073(5) 0.038(4) 0.055(4) -0.011(3) -0.011(3) -0.018(3) C16 0.051(4) 0.043(4) 0.065(4) -0.001(3) -0.006(3) -0.021(3) C13 0.060(4) 0.045(4) 0.041(3) -0.012(3) 0.003(3) 0.009(3) C14 0.082(5) 0.031(3) 0.054(4) -0.009(3) -0.006(3) -0.003(3) C20 0.037(4) 0.081(5) 0.083(5) 0.014(4) 0.005(4) 0.017(4) C17 0.044(4) 0.056(4) 0.060(4) 0.003(3) 0.002(3) -0.013(3) C11 0.082(5) 0.072(5) 0.077(5) -0.016(4) -0.004(4) 0.034(5) C21 0.058(5) 0.057(4) 0.082(5) 0.007(4) 0.004(4) 0.022(4) C10 0.062(5) 0.110(6) 0.054(4) -0.012(4) 0.007(4) 0.032(5) C9 0.072(5) 0.088(5) 0.034(4) -0.005(3) 0.015(3) 0.003(4) _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 Cs1 O4 2.990(4) . ? Cs1 O2 2.997(3) . ? Cs1 O5 3.083(3) . ? Cs1 O6 3.093(4) . ? Cs1 O1 3.101(3) . ? Cs1 O3 3.284(4) . ? Cs1 Ni1 3.4726(6) . ? Cs1 C15 3.603(5) . ? Cs1 C16 3.606(6) . ? Cs1 C7 3.655(6) . ? Cs1 S5 3.7327(16) . ? Cs1 C8 3.772(6) . ? Ni1 S5 2.1838(15) 3_756 ? Ni1 S5 2.1838(15) . ? Ni1 S4 2.1945(16) 3_756 ? Ni1 S4 2.1945(16) . ? Ni1 Cs1 3.4725(6) 3_756 ? S4 C2 1.735(6) . ? S4 Cs1 3.8090(16) 3_756 ? S5 C3 1.732(6) . ? S3 C1 1.730(7) . ? S3 C3 1.746(6) . ? S2 C1 1.725(6) . ? S2 C2 1.744(6) . ? S1 C1 1.645(6) . ? O3 C7 1.424(6) . ? O3 C8 1.432(6) . ? O6 C17 1.420(6) . ? O6 C18 1.434(6) . ? O1 C4 1.419(6) . ? O1 C23 1.441(6) . ? O2 C6 1.409(6) . ? O2 C5 1.431(6) . ? O4 C14 1.428(6) . ? O4 C13 1.430(6) . ? O5 C16 1.409(7) . ? O5 C15 1.430(6) . ? C23 C18 1.513(7) . ? C23 C22 1.528(7) . ? C2 C3 1.345(7) . ? C8 C13 1.513(8) . ? C8 C9 1.529(8) . ? C18 C19 1.537(7) . ? C5 C4 1.491(7) . ? C6 C7 1.496(7) . ? C19 C20 1.529(8) . ? C12 C13 1.516(7) . ? C12 C11 1.516(9) . ? C22 C21 1.522(8) . ? C15 C14 1.495(8) . ? C16 C17 1.499(8) . ? C20 C21 1.523(8) . ? C11 C10 1.520(9) . ? C10 C9 1.530(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 O4 Cs1 O2 103.21(10) . . ? O4 Cs1 O5 55.46(10) . . ? O2 Cs1 O5 128.38(10) . . ? O4 Cs1 O6 110.01(10) . . ? O2 Cs1 O6 106.03(9) . . ? O5 Cs1 O6 56.38(9) . . ? O4 Cs1 O1 127.32(9) . . ? O2 Cs1 O1 54.55(9) . . ? O5 Cs1 O1 98.48(9) . . ? O6 Cs1 O1 52.53(9) . . ? O4 Cs1 O3 51.42(10) . . ? O2 Cs1 O3 55.31(9) . . ? O5 Cs1 O3 101.29(10) . . ? O6 Cs1 O3 136.01(9) . . ? O1 Cs1 O3 103.16(9) . . ? O4 Cs1 Ni1 88.47(7) . . ? O2 Cs1 Ni1 132.16(7) . . ? O5 Cs1 Ni1 96.61(6) . . ? O6 Cs1 Ni1 113.13(6) . . ? O1 Cs1 Ni1 143.39(6) . . ? O3 Cs1 Ni1 106.29(6) . . ? O4 Cs1 C15 41.02(12) . . ? O2 Cs1 C15 137.53(12) . . ? O5 Cs1 C15 23.07(11) . . ? O6 Cs1 C15 77.39(12) . . ? O1 Cs1 C15 121.39(11) . . ? O3 Cs1 C15 92.22(12) . . ? Ni1 Cs1 C15 78.85(10) . . ? O4 Cs1 C16 76.61(13) . . ? O2 Cs1 C16 137.90(12) . . ? O5 Cs1 C16 22.64(11) . . ? O6 Cs1 C16 40.84(11) . . ? O1 Cs1 C16 91.46(11) . . ? O3 Cs1 C16 123.92(12) . . ? Ni1 Cs1 C16 89.85(10) . . ? C15 Cs1 C16 37.83(14) . . ? O4 Cs1 C7 73.46(12) . . ? O2 Cs1 C7 40.48(11) . . ? O5 Cs1 C7 123.89(11) . . ? O6 Cs1 C7 142.48(11) . . ? O1 Cs1 C7 94.58(11) . . ? O3 Cs1 C7 22.88(10) . . ? Ni1 Cs1 C7 104.22(9) . . ? C15 Cs1 C7 114.48(14) . . ? C16 Cs1 C7 146.37(14) . . ? O4 Cs1 S5 123.21(7) . . ? O2 Cs1 S5 118.73(7) . . ? O5 Cs1 S5 111.13(7) . . ? O6 Cs1 S5 94.05(7) . . ? O1 Cs1 S5 108.39(7) . . ? O3 Cs1 S5 129.90(6) . . ? Ni1 Cs1 S5 35.05(2) . . ? C15 Cs1 S5 102.89(10) . . ? C16 Cs1 S5 93.41(10) . . ? C7 Cs1 S5 115.71(9) . . ? O4 Cs1 C8 39.21(12) . . ? O2 Cs1 C8 75.91(11) . . ? O5 Cs1 C8 94.54(12) . . ? O6 Cs1 C8 145.30(11) . . ? O1 Cs1 C8 125.13(10) . . ? O3 Cs1 C8 22.06(10) . . ? Ni1 Cs1 C8 86.41(8) . . ? C15 Cs1 C8 78.89(14) . . ? C16 Cs1 C8 115.74(13) . . ? C7 Cs1 C8 37.52(12) . . ? S5 Cs1 C8 115.79(8) . . ? S5 Ni1 S5 180.00(7) 3_756 . ? S5 Ni1 S4 93.38(6) 3_756 3_756 ? S5 Ni1 S4 86.62(6) . 3_756 ? S5 Ni1 S4 86.62(6) 3_756 . ? S5 Ni1 S4 93.38(6) . . ? S4 Ni1 S4 180.00(8) 3_756 . ? S5 Ni1 Cs1 79.00(4) 3_756 3_756 ? S5 Ni1 Cs1 101.00(4) . 3_756 ? S4 Ni1 Cs1 98.93(4) 3_756 3_756 ? S4 Ni1 Cs1 81.07(4) . 3_756 ? S5 Ni1 Cs1 101.00(4) 3_756 . ? S5 Ni1 Cs1 79.00(4) . . ? S4 Ni1 Cs1 81.07(4) 3_756 . ? S4 Ni1 Cs1 98.93(4) . . ? Cs1 Ni1 Cs1 180.0 3_756 . ? C2 S4 Ni1 100.9(2) . . ? C2 S4 Cs1 109.27(18) . 3_756 ? Ni1 S4 Cs1 64.24(4) . 3_756 ? C3 S5 Ni1 101.1(2) . . ? C3 S5 Cs1 97.02(19) . . ? Ni1 S5 Cs1 65.95(4) . . ? C1 S3 C3 97.8(3) . . ? C1 S2 C2 98.0(3) . . ? C7 O3 C8 113.7(4) . . ? C7 O3 Cs1 93.4(3) . . ? C8 O3 Cs1 98.5(3) . . ? C17 O6 C18 113.6(4) . . ? C17 O6 Cs1 115.1(3) . . ? C18 O6 Cs1 124.3(3) . . ? C4 O1 C23 114.1(4) . . ? C4 O1 Cs1 112.8(3) . . ? C23 O1 Cs1 111.6(3) . . ? C6 O2 C5 113.2(4) . . ? C6 O2 Cs1 119.5(3) . . ? C5 O2 Cs1 123.3(3) . . ? C14 O4 C13 114.7(4) . . ? C14 O4 Cs1 119.2(3) . . ? C13 O4 Cs1 125.4(3) . . ? C16 O5 C15 110.7(4) . . ? C16 O5 Cs1 100.0(3) . . ? C15 O5 Cs1 99.3(3) . . ? O1 C23 C18 107.8(4) . . ? O1 C23 C22 113.7(4) . . ? C18 C23 C22 112.2(4) . . ? O1 C23 Cs1 48.2(2) . . ? C18 C23 Cs1 86.9(3) . . ? C22 C23 Cs1 83.6(3) . . ? C3 C2 S4 121.9(4) . . ? C3 C2 S2 115.9(4) . . ? S4 C2 S2 122.2(4) . . ? C2 C3 S5 122.2(4) . . ? C2 C3 S3 115.9(4) . . ? S5 C3 S3 121.7(3) . . ? O3 C8 C13 107.7(4) . . ? O3 C8 C9 113.2(5) . . ? C13 C8 C9 109.5(5) . . ? O3 C8 Cs1 59.4(2) . . ? C13 C8 Cs1 87.1(3) . . ? C9 C8 Cs1 163.4(4) . . ? O6 C18 C23 105.9(4) . . ? O6 C18 C19 113.0(4) . . ? C23 C18 C19 108.9(5) . . ? O2 C5 C4 109.2(4) . . ? O2 C6 C7 110.2(4) . . ? O2 C6 Cs1 42.1(2) . . ? C7 C6 Cs1 69.9(3) . . ? C20 C19 C18 111.2(5) . . ? C13 C12 C11 111.0(5) . . ? O3 C7 C6 109.2(4) . . ? O3 C7 Cs1 63.8(3) . . ? C6 C7 Cs1 87.5(3) . . ? O1 C4 C5 110.4(4) . . ? O1 C4 Cs1 47.5(2) . . ? C5 C4 Cs1 82.4(3) . . ? S1 C1 S2 124.2(4) . . ? S1 C1 S3 123.5(4) . . ? S2 C1 S3 112.3(3) . . ? C21 C22 C23 109.9(5) . . ? O5 C15 C14 109.3(5) . . ? O5 C15 Cs1 57.6(2) . . ? C14 C15 Cs1 89.6(3) . . ? O5 C16 C17 109.9(5) . . ? O5 C16 Cs1 57.4(2) . . ? C17 C16 Cs1 90.3(3) . . ? O4 C13 C8 108.2(4) . . ? O4 C13 C12 112.3(5) . . ? C8 C13 C12 112.4(5) . . ? O4 C14 C15 109.0(5) . . ? O4 C14 Cs1 42.2(2) . . ? C15 C14 Cs1 67.8(3) . . ? C21 C20 C19 109.9(5) . . ? O6 C17 C16 109.6(5) . . ? O6 C17 Cs1 45.7(3) . . ? C16 C17 Cs1 67.2(3) . . ? C12 C11 C10 111.2(5) . . ? C22 C21 C20 112.2(5) . . ? C11 C10 C9 110.8(6) . . ? C8 C9 C10 110.8(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.570 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.089 #===END data_xcsnis _database_code_CSD 158415 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Cs(Crown)1.5][Ni(dmit)2]6 _chemical_formula_sum 'C66 H54 Cs Ni6 O9 S60' _chemical_formula_weight 3399.86 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' 'S' 'S' 0.1246 0.1234 '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' 'Cs' 'Cs' -0.3680 2.1192 '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 11.633(6) _cell_length_b 12.150(6) _cell_length_c 23.778(12) _cell_angle_alpha 80.07(3) _cell_angle_beta 80.11(3) _cell_angle_gamma 69.10(3) _cell_volume 3070(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _exptl_crystal_description plate _exptl_crystal_colour Black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.839 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1705 _exptl_absorpt_coefficient_mu 2.261 _exptl_absorpt_correction_type Integration _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.911 _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 ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% ? _diffrn_reflns_number 7619 _diffrn_reflns_av_R_equivalents 0.1482 _diffrn_reflns_av_sigmaI/netI 0.2042 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 20.10 _reflns_number_total 5749 _reflns_number_gt 1776 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1835P)^2^+55.0952P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5749 _refine_ls_number_parameters 470 _refine_ls_number_restraints 374 _refine_ls_R_factor_all 0.2883 _refine_ls_R_factor_gt 0.1179 _refine_ls_wR_factor_ref 0.4330 _refine_ls_wR_factor_gt 0.3382 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.003 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 Ni1A Ni 0.0000 0.0000 1.0000 0.029(2) Uani 1 2 d S . . S1A S 0.0481(10) -0.0831(7) 0.9219(4) 0.036(3) Uani 1 1 d D . . S2A S 0.0349(9) 0.1586(8) 0.9566(3) 0.032(3) Uani 1 1 d D . . C1A C 0.082(4) 0.025(2) 0.8725(6) 0.049(14) Uiso 1 1 d D . . C2A C 0.079(3) 0.1271(18) 0.8879(6) 0.032(11) Uiso 1 1 d D . . S3A S 0.1162(10) 0.2283(7) 0.8321(3) 0.032(3) Uani 1 1 d D . . C4A C 0.148(4) 0.1415(17) 0.7765(7) 0.041(13) Uiso 1 1 d D . . S4A S 0.1878(15) 0.1848(12) 0.7102(4) 0.070(5) Uani 1 1 d D . . S5A S 0.1242(11) 0.0057(8) 0.7992(3) 0.040(3) Uani 1 1 d D . . Ni1B Ni 0.0000 -0.5000 1.0000 0.038(2) Uani 1 2 d S . . S1B S 0.1347(10) -0.5919(8) 0.9334(4) 0.042(3) Uani 1 1 d D . . S2B S -0.0562(10) -0.3369(8) 0.9445(4) 0.042(3) Uani 1 1 d D . . C1B C 0.114(3) -0.4816(16) 0.8764(8) 0.043(13) Uiso 1 1 d D . . C2B C 0.037(3) -0.3705(15) 0.8824(7) 0.031(11) Uiso 1 1 d D . . S3B S 0.0269(9) -0.2682(8) 0.8201(4) 0.043(3) Uani 1 1 d D . . C4B C 0.143(3) -0.3606(15) 0.7755(8) 0.035(12) Uiso 1 1 d D . . S4B S 0.1908(13) -0.3164(12) 0.7104(4) 0.069(5) Uani 1 1 d D . . S5B S 0.2090(10) -0.5035(9) 0.8103(4) 0.048(3) Uani 1 1 d D . . Ni2 Ni 0.7003(5) 0.0272(5) 0.9542(2) 0.0323(16) Uani 1 1 d . . . S1C S 0.6654(10) -0.1287(8) 0.9962(4) 0.041(3) Uani 1 1 d D . . S2C S 0.6565(9) 0.1089(7) 1.0326(4) 0.035(3) Uani 1 1 d D . . C1C C 0.625(3) -0.0989(18) 1.0661(6) 0.031(11) Uiso 1 1 d D . . C2C C 0.620(3) 0.0041(18) 1.0817(6) 0.032(11) Uiso 1 1 d D . . S3C S 0.5742(10) 0.0203(8) 1.1551(4) 0.040(3) Uani 1 1 d D . . C4C C 0.545(3) -0.1131(18) 1.1761(7) 0.035(11) Uiso 1 1 d D . . S4C S 0.5109(14) -0.1605(11) 1.2425(4) 0.067(4) Uani 1 1 d D . . S5C S 0.5793(10) -0.1994(8) 1.1197(4) 0.039(3) Uani 1 1 d D . . S1D S 0.7447(10) -0.0569(8) 0.8769(4) 0.039(3) Uani 1 1 d D . . S2D S 0.7303(11) 0.1866(9) 0.9085(4) 0.046(3) Uani 1 1 d D . . C1D C 0.780(3) 0.0488(17) 0.8262(6) 0.030(10) Uiso 1 1 d D . . C2D C 0.779(3) 0.1511(17) 0.8406(6) 0.029(10) Uiso 1 1 d D . . S3D S 0.8026(12) 0.2549(8) 0.7824(4) 0.060(4) Uani 1 1 d D . . C4D C 0.842(5) 0.162(2) 0.7286(8) 0.085(19) Uiso 1 1 d D . . S4D S 0.8855(16) 0.2019(15) 0.6622(4) 0.093(6) Uani 1 1 d D . . S5D S 0.8249(12) 0.0243(9) 0.7537(4) 0.053(4) Uani 1 1 d D . . Ni3 Ni 0.6998(5) -0.4715(5) 0.9539(3) 0.0350(16) Uani 1 1 d . . . S1E S 0.8297(10) -0.5609(8) 0.8861(4) 0.038(3) Uani 1 1 d D . . S2E S 0.6389(10) -0.3060(9) 0.8987(4) 0.044(3) Uani 1 1 d D . . C1E C 0.813(3) -0.4474(16) 0.8307(7) 0.043(12) Uiso 1 1 d D . . C2E C 0.727(2) -0.3396(14) 0.8355(7) 0.014(8) Uiso 1 1 d D . . S3E S 0.7241(10) -0.2342(8) 0.7746(4) 0.050(3) Uani 1 1 d D . . C4E C 0.832(3) -0.3286(15) 0.7284(8) 0.046(13) Uiso 1 1 d D . . S4E S 0.8802(14) -0.2828(12) 0.6637(4) 0.077(5) Uani 1 1 d D . . S5E S 0.8992(11) -0.4717(8) 0.7627(4) 0.058(4) Uani 1 1 d D . . S1F S 0.7586(8) -0.6363(8) 1.0097(4) 0.029(3) Uani 1 1 d D . . S2F S 0.5644(10) -0.3844(7) 1.0206(4) 0.038(3) Uani 1 1 d D . . C1F C 0.665(3) -0.6010(16) 1.0727(7) 0.030(10) Uiso 1 1 d D . . C2F C 0.580(3) -0.4927(16) 1.0770(7) 0.031(11) Uiso 1 1 d D . . S3F S 0.4883(9) -0.4714(7) 1.1439(4) 0.040(3) Uani 1 1 d D . . C4F C 0.552(3) -0.6153(17) 1.1775(9) 0.061(15) Uiso 1 1 d D . . S4F S 0.5129(12) -0.6594(11) 1.2439(4) 0.059(4) Uani 1 1 d D . . S5F S 0.6712(9) -0.7071(7) 1.1335(4) 0.040(3) Uani 1 1 d D . . Cs1 Cs 0.5601(10) 0.8886(11) 0.4997(4) 0.048(4) Uani 0.25 1 d PD . 1 Cs2 Cs 0.4373(12) 0.6021(13) 0.5035(5) 0.068(4) Uani 0.25 1 d PD . 2 C11 C 0.255(4) 0.896(4) 0.4679(19) 0.149(6) Uiso 0.75 1 d PD . 1 H11 H 0.1888 0.9262 0.4430 0.179 Uiso 0.75 1 calc PR . 1 C21 C 0.307(5) 0.764(4) 0.471(3) 0.149(6) Uiso 0.75 1 d PD A 1 H21A H 0.3709 0.7330 0.4965 0.179 Uiso 0.75 1 calc PR A 1 H21B H 0.3426 0.7408 0.4333 0.179 Uiso 0.75 1 calc PR A 1 C31 C 0.203(6) 0.719(5) 0.494(3) 0.149(6) Uiso 0.75 1 d PD A 1 H31A H 0.2314 0.6337 0.4932 0.179 Uiso 0.75 1 calc PR A 1 H31B H 0.1367 0.7551 0.4695 0.179 Uiso 0.75 1 calc PR A 1 C41 C 0.158(6) 0.748(6) 0.553(2) 0.149(6) Uiso 0.75 1 d PD A 1 H41A H 0.0953 0.7130 0.5700 0.179 Uiso 0.75 1 calc PR A 1 H41B H 0.2258 0.7174 0.5765 0.179 Uiso 0.75 1 calc PR A 1 C51 C 0.105(4) 0.879(6) 0.551(3) 0.149(6) Uiso 0.75 1 d PD A 1 H51A H 0.0381 0.9099 0.5269 0.179 Uiso 0.75 1 calc PR A 1 H51B H 0.0717 0.9010 0.5892 0.179 Uiso 0.75 1 calc PR A 1 C61 C 0.204(4) 0.929(4) 0.5269(18) 0.149(6) Uiso 0.75 1 d PD A 1 H61 H 0.1708 1.0153 0.5252 0.179 Uiso 0.75 1 calc PR A 1 O71 O 0.305(3) 0.882(4) 0.5642(18) 0.149(6) Uiso 0.75 1 d PD . 1 C81 C 0.266(4) 0.947(6) 0.615(2) 0.149(6) Uiso 0.75 1 d PD . 1 H81A H 0.2318 1.0316 0.6032 0.179 Uiso 0.75 1 calc PR . 1 H81B H 0.2031 0.9223 0.6407 0.179 Uiso 0.75 1 calc PR . 1 C91 C 0.376(6) 0.921(6) 0.645(2) 0.149(6) Uiso 0.75 1 d PD . 1 H91A H 0.4252 0.8375 0.6457 0.179 Uiso 0.75 1 calc PR . 1 H91B H 0.3500 0.9388 0.6844 0.179 Uiso 0.75 1 calc PR . 1 O101 O 0.452(4) 0.994(4) 0.6147(13) 0.149(6) Uiso 0.75 1 d PD . 1 C111 C 0.563(5) 0.964(7) 0.644(3) 0.149(6) Uiso 0.75 1 d PD . 1 H11A H 0.6156 0.8827 0.6399 0.179 Uiso 0.75 1 calc PR . 1 H11B H 0.5382 0.9703 0.6849 0.179 Uiso 0.75 1 calc PR . 1 C121 C 0.632(6) 1.045(7) 0.6194(17) 0.149(6) Uiso 0.75 1 d PD . 1 H12A H 0.5880 1.1231 0.6319 0.179 Uiso 0.75 1 calc PR . 1 H12B H 0.7133 1.0156 0.6325 0.179 Uiso 0.75 1 calc PR . 1 O131 O 0.645(5) 1.055(4) 0.5560(17) 0.149(6) Uiso 0.75 1 d PD . 1 C12 C 0.796(4) 0.558(4) 0.4691(18) 0.149(6) Uiso 0.75 1 d PD . 2 H12 H 0.8390 0.4723 0.4702 0.179 Uiso 0.75 1 calc PR . 2 C22 C 0.879(4) 0.622(6) 0.439(2) 0.149(6) Uiso 0.75 1 d PD B 2 H22A H 0.9038 0.6027 0.3996 0.179 Uiso 0.75 1 calc PR B 2 H22B H 0.9536 0.5968 0.4578 0.179 Uiso 0.75 1 calc PR B 2 C32 C 0.818(7) 0.751(6) 0.438(2) 0.149(6) Uiso 0.75 1 d PD B 2 H32A H 0.7466 0.7776 0.4170 0.179 Uiso 0.75 1 calc PR B 2 H32B H 0.8747 0.7920 0.4193 0.179 Uiso 0.75 1 calc PR B 2 C42 C 0.777(7) 0.781(5) 0.498(3) 0.149(6) Uiso 0.75 1 d PD B 2 H42A H 0.7375 0.8663 0.4976 0.179 Uiso 0.75 1 calc PR B 2 H42B H 0.8478 0.7557 0.5192 0.179 Uiso 0.75 1 calc PR B 2 C52 C 0.688(5) 0.720(4) 0.526(3) 0.149(6) Uiso 0.75 1 d PD B 2 H52A H 0.6534 0.7450 0.5635 0.179 Uiso 0.75 1 calc PR B 2 H52B H 0.6206 0.7397 0.5027 0.179 Uiso 0.75 1 calc PR B 2 C62 C 0.757(4) 0.591(4) 0.5307(19) 0.149(6) Uiso 0.75 1 d PD B 2 H62 H 0.8297 0.5713 0.5512 0.179 Uiso 0.75 1 calc PR B 2 O72 O 0.674(3) 0.526(4) 0.5594(17) 0.149(6) Uiso 0.75 1 d PD . 2 C82 C 0.628(6) 0.550(6) 0.619(2) 0.149(6) Uiso 0.75 1 d PD C 2 H82A H 0.5665 0.6292 0.6198 0.179 Uiso 0.75 1 calc PR C 2 H82B H 0.6957 0.5468 0.6391 0.179 Uiso 0.75 1 calc PR C 2 C92 C 0.572(5) 0.460(6) 0.648(2) 0.149(6) Uiso 0.75 1 d PD C 2 H92A H 0.6264 0.3816 0.6396 0.179 Uiso 0.75 1 calc PR C 2 H92B H 0.5602 0.4608 0.6894 0.179 Uiso 0.75 1 calc PR C 2 O102 O 0.452(5) 0.488(5) 0.6268(16) 0.149(6) Uiso 0.75 1 d PD . 2 C112 C 0.395(6) 0.396(5) 0.648(2) 0.149(6) Uiso 0.75 1 d PD . 2 H11C H 0.3746 0.3919 0.6898 0.179 Uiso 0.75 1 calc PR . 2 H11D H 0.4525 0.3187 0.6393 0.179 Uiso 0.75 1 calc PR . 2 C122 C 0.281(4) 0.424(7) 0.621(2) 0.149(6) Uiso 0.75 1 d PD D 2 H12C H 0.2282 0.5057 0.6249 0.179 Uiso 0.75 1 calc PR D 2 H12D H 0.2347 0.3724 0.6395 0.179 Uiso 0.75 1 calc PR D 2 O132 O 0.317(4) 0.408(4) 0.5594(18) 0.149(6) Uiso 0.75 1 d PD . 2 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 Ni1A 0.030(5) 0.019(5) 0.032(5) -0.003(4) 0.000(4) -0.002(4) S1A 0.048(7) 0.014(6) 0.041(7) -0.007(5) -0.002(6) -0.006(5) S2A 0.028(6) 0.022(6) 0.045(7) 0.000(5) 0.008(6) -0.015(5) S3A 0.032(6) 0.036(7) 0.035(7) -0.006(5) 0.003(5) -0.021(5) S4A 0.111(13) 0.083(12) 0.030(9) 0.004(8) 0.012(8) -0.063(10) S5A 0.049(8) 0.037(7) 0.037(7) -0.017(6) 0.014(6) -0.020(6) Ni1B 0.050(6) 0.023(5) 0.036(6) -0.008(4) 0.011(4) -0.012(4) S1B 0.030(7) 0.020(7) 0.064(9) 0.004(6) -0.009(6) 0.001(5) S2B 0.042(8) 0.032(7) 0.037(8) -0.006(6) 0.006(6) 0.002(6) S3B 0.045(8) 0.049(8) 0.038(7) 0.003(6) 0.002(6) -0.026(6) S4B 0.082(11) 0.078(12) 0.042(9) 0.001(8) 0.014(8) -0.034(9) S5B 0.040(8) 0.065(9) 0.033(7) -0.007(6) 0.010(6) -0.016(7) Ni2 0.033(3) 0.026(4) 0.033(4) -0.004(3) 0.004(3) -0.009(3) S1C 0.040(7) 0.023(6) 0.049(8) -0.009(5) 0.000(6) 0.002(6) S2C 0.024(6) 0.016(6) 0.059(8) -0.006(5) 0.002(6) -0.003(5) S3C 0.037(7) 0.031(7) 0.048(8) -0.005(6) -0.006(6) -0.007(6) S4C 0.087(11) 0.065(11) 0.043(10) -0.007(8) 0.022(8) -0.031(8) S5C 0.031(7) 0.043(7) 0.042(7) -0.009(6) 0.010(5) -0.017(6) S1D 0.030(7) 0.043(7) 0.039(7) 0.001(6) -0.001(6) -0.010(6) S2D 0.045(8) 0.035(7) 0.048(8) 0.001(6) 0.005(6) -0.010(6) S3D 0.073(10) 0.050(8) 0.051(9) 0.010(7) 0.006(7) -0.029(7) S4D 0.113(14) 0.142(17) 0.039(10) 0.006(10) 0.006(9) -0.077(13) S5D 0.061(9) 0.056(9) 0.042(8) 0.002(6) 0.004(7) -0.029(7) Ni3 0.029(3) 0.019(4) 0.051(4) -0.004(3) -0.001(3) -0.003(3) S1E 0.035(7) 0.032(7) 0.041(7) -0.008(5) 0.008(6) -0.011(5) S2E 0.055(8) 0.047(8) 0.034(7) -0.005(6) 0.000(6) -0.025(7) S3E 0.075(9) 0.044(8) 0.040(8) 0.007(6) -0.015(7) -0.031(7) S4E 0.083(11) 0.083(12) 0.043(9) 0.011(8) 0.012(8) -0.019(9) S5E 0.074(10) 0.060(9) 0.044(8) 0.001(7) 0.009(7) -0.040(8) S1F 0.022(6) 0.029(6) 0.033(7) 0.001(5) -0.007(5) -0.004(5) S2F 0.043(7) 0.023(7) 0.042(7) -0.015(5) 0.014(6) -0.004(5) S3F 0.045(7) 0.034(7) 0.047(8) -0.017(6) 0.005(6) -0.020(6) S4F 0.075(10) 0.083(11) 0.028(8) -0.002(7) 0.010(7) -0.046(8) S5F 0.049(8) 0.034(7) 0.035(7) -0.008(5) 0.002(6) -0.014(6) Cs1 0.044(7) 0.067(9) 0.009(6) -0.021(6) -0.012(5) 0.021(6) Cs2 0.074(10) 0.078(10) 0.037(8) -0.031(7) -0.010(7) 0.005(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 Ni1A S1A 2.160(9) 2_557 ? Ni1A S1A 2.160(9) . ? Ni1A S2A 2.161(9) . ? Ni1A S2A 2.161(9) 2_557 ? S1A C1A 1.711(12) . ? S2A C2A 1.693(12) . ? C1A C2A 1.342(19) . ? C1A S5A 1.760(12) . ? C2A S3A 1.755(12) . ? S3A C4A 1.743(12) . ? C4A S4A 1.616(16) . ? C4A S5A 1.747(12) . ? Ni1B S2B 2.137(10) 2_547 ? Ni1B S2B 2.137(10) . ? Ni1B S1B 2.172(10) 2_547 ? Ni1B S1B 2.172(10) . ? S1B C1B 1.718(13) . ? S2B C2B 1.690(13) . ? C1B C2B 1.343(19) . ? C1B S5B 1.763(13) . ? C2B S3B 1.755(13) . ? S3B C4B 1.744(13) . ? C4B S4B 1.620(16) . ? C4B S5B 1.749(13) . ? Ni2 S1C 2.123(11) . ? Ni2 S1D 2.154(11) . ? Ni2 S2C 2.161(11) . ? Ni2 S2D 2.163(11) . ? S1C C1C 1.713(13) . ? S2C C2C 1.694(13) . ? C1C C2C 1.343(19) . ? C1C S5C 1.757(13) . ? C2C S3C 1.758(13) . ? S3C C4C 1.744(13) . ? C4C S4C 1.618(16) . ? C4C S5C 1.750(13) . ? S1D C1D 1.713(13) . ? S2D C2D 1.693(13) . ? C1D C2D 1.343(19) . ? C1D S5D 1.759(13) . ? C2D S3D 1.757(13) . ? S3D C4D 1.743(13) . ? C4D S4D 1.618(16) . ? C4D S5D 1.751(13) . ? Ni3 S1E 2.158(11) . ? Ni3 S1F 2.157(11) . ? Ni3 S2F 2.156(10) . ? Ni3 S2E 2.159(11) . ? S1E C1E 1.717(13) . ? S2E C2E 1.691(13) . ? C1E C2E 1.342(19) . ? C1E S5E 1.761(13) . ? C2E S3E 1.756(12) . ? S3E C4E 1.743(13) . ? C4E S4E 1.618(16) . ? C4E S5E 1.749(13) . ? S1F C1F 1.715(13) . ? S2F C2F 1.693(13) . ? C1F C2F 1.343(19) . ? C1F S5F 1.756(13) . ? C2F S3F 1.760(13) . ? S3F C4F 1.744(13) . ? C4F S4F 1.618(16) . ? C4F S5F 1.751(13) . ? Cs1 Cs1 2.57(2) 2_676 ? Cs1 O131 2.74(5) 2_676 ? Cs1 O101 2.85(4) 2_676 ? Cs1 O101 3.09(3) . ? Cs1 O131 3.11(3) . ? Cs1 O71 3.12(3) . ? Cs1 O71 3.66(5) 2_676 ? Cs1 C121 3.71(5) 2_676 ? Cs1 C111 3.71(7) . ? Cs1 C91 3.74(6) . ? Cs1 C11 3.72(5) . ? Cs1 C111 3.83(5) 2_676 ? Cs2 Cs2 2.41(3) 2_666 ? Cs2 O132 2.96(4) 2_666 ? Cs2 O72 3.04(3) . ? Cs2 O102 3.02(3) . ? Cs2 O72 3.04(4) 2_666 ? Cs2 O132 3.15(3) . ? Cs2 O102 3.36(5) 2_666 ? Cs2 C12 3.78(5) 2_666 ? Cs2 C112 3.80(7) 2_666 ? Cs2 C82 3.66(7) . ? Cs2 C122 3.84(6) . ? Cs2 C62 3.84(4) . ? C11 O131 1.479(10) 2_676 ? C11 C21 1.481(10) . ? C11 C61 1.49(3) . ? C21 C31 1.481(10) . ? C31 C41 1.481(10) . ? C41 C51 1.479(10) . ? C51 C61 1.479(10) . ? C61 O71 1.480(10) . ? O71 C81 1.480(10) . ? O71 Cs1 3.66(5) 2_676 ? C81 C91 1.479(10) . ? C81 Cs1 3.82(7) 2_676 ? C91 O101 1.481(10) . ? C91 Cs1 3.92(5) 2_676 ? O101 C111 1.476(10) . ? O101 Cs1 2.85(4) 2_676 ? C111 C121 1.477(10) . ? C111 Cs1 3.83(5) 2_676 ? C121 O131 1.478(10) . ? C121 Cs1 3.71(5) 2_676 ? O131 C11 1.479(10) 2_676 ? O131 Cs1 2.74(5) 2_676 ? C12 C22 1.474(10) . ? C12 O132 1.478(10) 2_666 ? C12 C62 1.54(4) . ? C12 Cs2 3.78(5) 2_666 ? C22 C32 1.476(10) . ? C32 C42 1.480(10) . ? C42 C52 1.481(10) . ? C52 C62 1.480(10) . ? C62 O72 1.473(10) . ? O72 C82 1.475(10) . ? O72 Cs2 3.04(4) 2_666 ? C82 C92 1.483(10) . ? C92 O102 1.472(10) . ? O102 C112 1.476(10) . ? O102 Cs2 3.36(5) 2_666 ? C112 C122 1.480(10) . ? C112 Cs2 3.80(7) 2_666 ? C122 O132 1.482(10) . ? O132 C12 1.478(10) 2_666 ? O132 Cs2 2.96(4) 2_666 ? 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 S1A Ni1A S1A 180.000(2) 2_557 . ? S1A Ni1A S2A 87.2(3) 2_557 . ? S1A Ni1A S2A 92.8(3) . . ? S1A Ni1A S2A 92.8(3) 2_557 2_557 ? S1A Ni1A S2A 87.2(3) . 2_557 ? S2A Ni1A S2A 180.0(2) . 2_557 ? C1A S1A Ni1A 101.6(6) . . ? C2A S2A Ni1A 102.2(6) . . ? C2A C1A S1A 121.6(9) . . ? C2A C1A S5A 116.9(8) . . ? S1A C1A S5A 121.5(9) . . ? C1A C2A S2A 121.7(8) . . ? C1A C2A S3A 116.1(8) . . ? S2A C2A S3A 122.2(8) . . ? C4A S3A C2A 97.4(7) . . ? S4A C4A S3A 123.6(8) . . ? S4A C4A S5A 123.5(8) . . ? S3A C4A S5A 112.9(9) . . ? C4A S5A C1A 96.8(7) . . ? S2B Ni1B S2B 180.0(4) 2_547 . ? S2B Ni1B S1B 93.0(3) 2_547 2_547 ? S2B Ni1B S1B 87.0(3) . 2_547 ? S2B Ni1B S1B 87.0(3) 2_547 . ? S2B Ni1B S1B 93.0(3) . . ? S1B Ni1B S1B 180.0(4) 2_547 . ? C1B S1B Ni1B 101.0(6) . . ? C2B S2B Ni1B 102.8(6) . . ? C2B C1B S1B 121.5(10) . . ? C2B C1B S5B 116.7(10) . . ? S1B C1B S5B 121.1(10) . . ? C1B C2B S2B 121.4(10) . . ? C1B C2B S3B 115.7(9) . . ? S2B C2B S3B 122.6(9) . . ? C2B S3B C4B 97.6(7) . . ? S4B C4B S3B 123.6(9) . . ? S4B C4B S5B 123.6(10) . . ? S3B C4B S5B 112.6(9) . . ? C4B S5B C1B 96.8(7) . . ? S1C Ni2 S1D 85.9(4) . . ? S1C Ni2 S2C 93.3(4) . . ? S1D Ni2 S2C 179.1(5) . . ? S1C Ni2 S2D 177.3(5) . . ? S1D Ni2 S2D 92.4(4) . . ? S2C Ni2 S2D 88.4(4) . . ? C1C S1C Ni2 102.0(6) . . ? C2C S2C Ni2 102.0(6) . . ? C2C C1C S1C 121.8(10) . . ? C2C C1C S5C 117.4(9) . . ? S1C C1C S5C 120.7(9) . . ? C1C C2C S2C 120.9(10) . . ? C1C C2C S3C 115.6(9) . . ? S2C C2C S3C 123.5(9) . . ? C4C S3C C2C 97.4(7) . . ? S4C C4C S3C 123.1(10) . . ? S4C C4C S5C 123.3(9) . . ? S3C C4C S5C 112.9(9) . . ? C1C S5C C4C 96.5(7) . . ? C1D S1D Ni2 102.1(6) . . ? C2D S2D Ni2 102.6(6) . . ? C2D C1D S1D 121.6(10) . . ? C2D C1D S5D 117.3(9) . . ? S1D C1D S5D 121.1(9) . . ? C1D C2D S2D 121.0(10) . . ? C1D C2D S3D 115.3(9) . . ? S2D C2D S3D 122.5(9) . . ? C4D S3D C2D 97.4(7) . . ? S4D C4D S3D 123.5(10) . . ? S4D C4D S5D 123.7(10) . . ? S3D C4D S5D 112.8(9) . . ? C1D S5D C4D 96.5(7) . . ? S1E Ni3 S1F 87.7(4) . . ? S1E Ni3 S2F 177.7(5) . . ? S1F Ni3 S2F 92.3(4) . . ? S1E Ni3 S2E 92.9(4) . . ? S1F Ni3 S2E 179.3(5) . . ? S2F Ni3 S2E 87.1(4) . . ? C1E S1E Ni3 101.3(6) . . ? C2E S2E Ni3 102.4(6) . . ? C2E C1E S1E 121.9(10) . . ? C2E C1E S5E 117.0(9) . . ? S1E C1E S5E 120.8(9) . . ? C1E C2E S2E 121.2(10) . . ? C1E C2E S3E 115.7(9) . . ? S2E C2E S3E 122.8(9) . . ? C4E S3E C2E 97.5(7) . . ? S4E C4E S3E 123.0(10) . . ? S4E C4E S5E 123.7(10) . . ? S3E C4E S5E 112.7(9) . . ? C4E S5E C1E 96.7(7) . . ? C1F S1F Ni3 102.1(6) . . ? C2F S2F Ni3 103.1(6) . . ? C2F C1F S1F 121.6(10) . . ? C2F C1F S5F 117.0(9) . . ? S1F C1F S5F 121.4(9) . . ? C1F C2F S2F 120.9(10) . . ? C1F C2F S3F 116.2(9) . . ? S2F C2F S3F 122.9(9) . . ? C4F S3F C2F 97.1(7) . . ? S4F C4F S3F 124.4(10) . . ? S4F C4F S5F 122.4(10) . . ? S3F C4F S5F 113.1(9) . . ? C1F S5F C4F 96.7(7) . . ? Cs1 Cs1 O131 71.6(10) 2_676 2_676 ? Cs1 Cs1 O101 69.5(9) 2_676 2_676 ? O131 Cs1 O101 57.8(12) 2_676 2_676 ? Cs1 Cs1 O101 59.5(9) 2_676 . ? O131 Cs1 O101 103.2(13) 2_676 . ? O101 Cs1 O101 129.0(7) 2_676 . ? Cs1 Cs1 O131 56.8(11) 2_676 . ? O131 Cs1 O131 128.4(7) 2_676 . ? O101 Cs1 O131 100.4(12) 2_676 . ? O101 Cs1 O131 51.7(11) . . ? Cs1 Cs1 O71 79.5(11) 2_676 . ? O131 Cs1 O71 57.6(12) 2_676 . ? O101 Cs1 O71 114.0(11) 2_676 . ? O101 Cs1 O71 58.2(11) . . ? O131 Cs1 O71 108.8(12) . . ? Cs1 Cs1 O71 56.9(7) 2_676 2_676 ? O131 Cs1 O71 103.6(11) 2_676 2_676 ? O101 Cs1 O71 53.6(10) 2_676 2_676 ? O101 Cs1 O71 95.3(10) . 2_676 ? O131 Cs1 O71 48.8(9) . 2_676 ? O71 Cs1 O71 136.4(6) . 2_676 ? Cs1 Cs1 C121 77.6(13) 2_676 2_676 ? O131 Cs1 C121 20.2(10) 2_676 2_676 ? O101 Cs1 C121 40.6(8) 2_676 2_676 ? O101 Cs1 C121 121.3(12) . 2_676 ? O131 Cs1 C121 130.6(15) . 2_676 ? O71 Cs1 C121 77.3(9) . 2_676 ? O71 Cs1 C121 92.1(9) 2_676 2_676 ? Cs1 Cs1 C111 72.7(11) 2_676 . ? O131 Cs1 C111 126.0(13) 2_676 . ? O101 Cs1 C111 137.2(11) 2_676 . ? O101 Cs1 C111 22.8(8) . . ? O131 Cs1 C111 40.2(8) . . ? O71 Cs1 C111 77.1(10) . . ? O71 Cs1 C111 88.9(9) 2_676 . ? C121 Cs1 C111 143.6(11) 2_676 . ? Cs1 Cs1 C91 74.1(11) 2_676 . ? O131 Cs1 C91 93.7(11) 2_676 . ? O101 Cs1 C91 139.2(12) 2_676 . ? O101 Cs1 C91 22.6(7) . . ? O131 Cs1 C91 73.6(10) . . ? O71 Cs1 C91 39.6(7) . . ? O71 Cs1 C91 117.7(8) 2_676 . ? C121 Cs1 C91 113.8(10) 2_676 . ? C111 Cs1 C91 37.6(6) . . ? Cs1 Cs1 C11 80.8(8) 2_676 . ? O131 Cs1 C11 20.0(7) 2_676 . ? O101 Cs1 C11 77.4(10) 2_676 . ? O101 Cs1 C11 93.9(10) . . ? O131 Cs1 C11 134.2(11) . . ? O71 Cs1 C11 40.3(6) . . ? O71 Cs1 C11 122.5(7) 2_676 . ? C121 Cs1 C11 37.7(6) 2_676 . ? C111 Cs1 C11 115.5(9) . . ? C91 Cs1 C11 79.1(6) . . ? Cs1 Cs1 C111 67.6(14) 2_676 2_676 ? O131 Cs1 C111 38.7(7) 2_676 2_676 ? O101 Cs1 C111 19.1(7) 2_676 2_676 ? O101 Cs1 C111 123.6(15) . 2_676 ? O131 Cs1 C111 112.0(15) . 2_676 ? O71 Cs1 C111 95.4(10) . 2_676 ? O71 Cs1 C111 69.7(9) 2_676 2_676 ? C121 Cs1 C111 22.5(3) 2_676 2_676 ? C111 Cs1 C111 140.3(7) . 2_676 ? C91 Cs1 C111 125.7(13) . 2_676 ? C11 Cs1 C111 58.4(6) . 2_676 ? Cs2 Cs2 O132 71.0(9) 2_666 2_666 ? Cs2 Cs2 O72 66.7(10) 2_666 . ? O132 Cs2 O72 55.6(11) 2_666 . ? Cs2 Cs2 O102 75.4(13) 2_666 . ? O132 Cs2 O102 112.8(12) 2_666 . ? O72 Cs2 O102 58.0(12) . . ? Cs2 Cs2 O72 66.7(9) 2_666 2_666 ? O132 Cs2 O72 107.9(11) 2_666 2_666 ? O72 Cs2 O72 133.4(7) . 2_666 ? O102 Cs2 O72 109.2(12) . 2_666 ? Cs2 Cs2 O132 62.7(10) 2_666 . ? O132 Cs2 O132 133.7(7) 2_666 . ? O72 Cs2 O132 103.2(12) . . ? O102 Cs2 O132 56.1(12) . . ? O72 Cs2 O132 53.7(11) 2_666 . ? Cs2 Cs2 O102 60.7(9) 2_666 2_666 ? O132 Cs2 O102 54.4(11) 2_666 2_666 ? O72 Cs2 O102 101.2(12) . 2_666 ? O102 Cs2 O102 136.1(8) . 2_666 ? O72 Cs2 O102 54.5(11) 2_666 2_666 ? O132 Cs2 O102 100.0(12) . 2_666 ? Cs2 Cs2 C12 76.2(10) 2_666 2_666 ? O132 Cs2 C12 142.2(11) 2_666 2_666 ? O72 Cs2 C12 125.6(10) . 2_666 ? O102 Cs2 C12 75.4(10) . 2_666 ? O72 Cs2 C12 39.6(7) 2_666 2_666 ? O132 Cs2 C12 22.3(5) . 2_666 ? O102 Cs2 C12 93.2(10) 2_666 2_666 ? Cs2 Cs2 C112 75.7(10) 2_666 2_666 ? O132 Cs2 C112 39.1(8) 2_666 2_666 ? O72 Cs2 C112 93.7(10) . 2_666 ? O102 Cs2 C112 145.8(12) . 2_666 ? O72 Cs2 C112 75.0(10) 2_666 2_666 ? O132 Cs2 C112 122.7(10) . 2_666 ? O102 Cs2 C112 22.7(6) 2_666 2_666 ? C12 Cs2 C112 114.5(8) 2_666 2_666 ? Cs2 Cs2 C82 80.2(12) 2_666 . ? O132 Cs2 C82 77.0(10) 2_666 . ? O72 Cs2 C82 23.1(8) . . ? O102 Cs2 C82 40.6(8) . . ? O72 Cs2 C82 141.6(12) 2_666 . ? O132 Cs2 C82 94.6(10) . . ? O102 Cs2 C82 124.2(10) 2_666 . ? C12 Cs2 C82 115.6(8) 2_666 . ? C112 Cs2 C82 115.9(8) 2_666 . ? Cs2 Cs2 C122 75.3(12) 2_666 . ? O132 Cs2 C122 141.6(12) 2_666 . ? O72 Cs2 C122 94.2(10) . . ? O102 Cs2 C122 38.8(7) . . ? O72 Cs2 C122 74.1(10) 2_666 . ? O132 Cs2 C122 21.7(8) . . ? O102 Cs2 C122 121.4(10) 2_666 . ? C12 Cs2 C122 36.8(5) 2_666 . ? C112 Cs2 C122 144.0(9) 2_666 . ? C82 Cs2 C122 79.4(6) . . ? Cs2 Cs2 C62 77.1(10) 2_666 . ? O132 Cs2 C62 39.5(7) 2_666 . ? O72 Cs2 C62 20.9(6) . . ? O102 Cs2 C62 77.4(10) . . ? O72 Cs2 C62 139.2(9) 2_666 . ? O132 Cs2 C62 123.6(10) . . ? O102 Cs2 C62 92.1(10) 2_666 . ? C12 Cs2 C62 145.7(8) 2_666 . ? C112 Cs2 C62 78.6(7) 2_666 . ? C82 Cs2 C62 38.1(6) . . ? C122 Cs2 C62 114.8(8) . . ? O131 C11 C21 109(2) 2_676 . ? O131 C11 C61 110(2) 2_676 . ? C21 C11 C61 109(2) . . ? O131 C11 Cs1 39.3(18) 2_676 . ? C21 C11 Cs1 88(3) . . ? C61 C11 Cs1 87.2(14) . . ? C11 C21 C31 107(2) . . ? C21 C31 C41 109(2) . . ? C51 C41 C31 108(2) . . ? C61 C51 C41 108.2(19) . . ? C51 C61 O71 109.5(19) . . ? C51 C61 C11 110(2) . . ? O71 C61 C11 109(2) . . ? C61 O71 C81 108.3(19) . . ? C61 O71 Cs1 113(2) . . ? C81 O71 Cs1 112(3) . . ? C61 O71 Cs1 93(2) . 2_676 ? C81 O71 Cs1 85(3) . 2_676 ? Cs1 O71 Cs1 43.6(6) . 2_676 ? C91 C81 O71 108(2) . . ? C91 C81 Cs1 82(2) . 2_676 ? O71 C81 Cs1 72(3) . 2_676 ? C81 C91 O101 110(2) . . ? C81 C91 Cs1 86.2(19) . . ? O101 C91 Cs1 53(3) . . ? C81 C91 Cs1 76(2) . 2_676 ? O101 C91 Cs1 35.7(16) . 2_676 ? Cs1 C91 Cs1 39.1(6) . 2_676 ? C111 O101 C91 108.7(19) . . ? C111 O101 Cs1 122(2) . 2_676 ? C91 O101 Cs1 127(2) . 2_676 ? C111 O101 Cs1 103(4) . . ? C91 O101 Cs1 104(3) . . ? Cs1 O101 Cs1 51.0(7) 2_676 . ? O101 C111 C121 110(2) . . ? O101 C111 Cs1 54(3) . . ? C121 C111 Cs1 91(2) . . ? O101 C111 Cs1 39.2(18) . 2_676 ? C121 C111 Cs1 74.0(16) . 2_676 ? Cs1 C111 Cs1 39.7(7) . 2_676 ? O131 C121 C111 109(2) . . ? O131 C121 Cs1 40(3) . 2_676 ? C111 C121 Cs1 83.5(16) . 2_676 ? C121 O131 C11 108.6(18) . 2_676 ? C121 O131 Cs1 120(4) . 2_676 ? C11 O131 Cs1 121(2) 2_676 2_676 ? C121 O131 Cs1 119(2) . . ? C11 O131 Cs1 127(2) 2_676 . ? Cs1 O131 Cs1 51.6(7) 2_676 . ? C22 C12 O132 111.0(19) . 2_666 ? C22 C12 C62 108(2) . . ? O132 C12 C62 108(2) 2_666 . ? C22 C12 Cs2 161(2) . 2_666 ? O132 C12 Cs2 54.1(19) 2_666 2_666 ? C62 C12 Cs2 88.8(15) . 2_666 ? C22 C12 Cs2 140(2) . . ? O132 C12 Cs2 38.6(15) 2_666 . ? C62 C12 Cs2 74.0(14) . . ? Cs2 C12 Cs2 36.1(6) 2_666 . ? C12 C22 C32 111(2) . . ? C22 C32 C42 110(2) . . ? C32 C42 C52 109(2) . . ? C62 C52 C42 107(2) . . ? O72 C62 C52 110(2) . . ? O72 C62 C12 107(2) . . ? C52 C62 C12 107(2) . . ? O72 C62 Cs2 47.3(18) . . ? C52 C62 Cs2 78(2) . . ? C12 C62 Cs2 83.4(15) . . ? C62 O72 C82 112.7(19) . . ? C62 O72 Cs2 112(2) . . ? C82 O72 Cs2 103(3) . . ? C62 O72 Cs2 124(2) . 2_666 ? C82 O72 Cs2 122(2) . 2_666 ? Cs2 O72 Cs2 46.6(7) . 2_666 ? O72 C82 C92 108(2) . . ? O72 C82 Cs2 54(3) . . ? C92 C82 Cs2 87.5(19) . . ? O102 C92 C82 108(2) . . ? C92 O102 C112 113(2) . . ? C92 O102 Cs2 115(3) . . ? C112 O102 Cs2 119(3) . . ? C92 O102 Cs2 97(4) . 2_666 ? C112 O102 Cs2 96(4) . 2_666 ? Cs2 O102 Cs2 43.9(8) . 2_666 ? O102 C112 C122 109(2) . . ? O102 C112 Cs2 61(3) . 2_666 ? C122 C112 Cs2 86.1(19) . 2_666 ? C112 C122 O132 108(2) . . ? C112 C122 Cs2 83.7(18) . . ? O132 C122 Cs2 52(3) . . ? C12 O132 C122 108.9(19) 2_666 . ? C12 O132 Cs2 123(2) 2_666 2_666 ? C122 O132 Cs2 124(2) . 2_666 ? C12 O132 Cs2 104(2) 2_666 . ? C122 O132 Cs2 107(3) . . ? Cs2 O132 Cs2 46.3(7) 2_666 . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 20.10 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.179 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.207