# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1652 # Please find below the CIF data for two crystal structures reported in the # manuscript entitled: # Tetraphenoxoborate complexes of barium: crystal structures of the # metalloborates [Ba(thf)4{B(OPh)4}2] and [Ba(dme)2{B(OPh)4}2] # by R.J.Errington, M.Tombul, G.L.P.Walker, W.Clegg, S.L.Heath and L.Horsburgh # which is being sent to you today by Dr. Errington # # CIF supplied by W.Clegg@ncl.ac.uk # data_rje99 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C72 H88 B2 Ba O14' _chemical_formula_weight 1336.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'Ba' 'Ba' -0.3244 2.2819 '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 11.0751(9) _cell_length_b 11.7693(10) _cell_length_c 13.5004(11) _cell_angle_alpha 104.461(2) _cell_angle_beta 104.083(2) _cell_angle_gamma 93.135(2) _cell_volume 1640.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 10079 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 28.41 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4948 _exptl_absorpt_correction_T_max 0.5979 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10382 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.42 _reflns_number_total 7185 _reflns_number_observed 7163 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+1.1879P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0032(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7185 _refine_ls_number_parameters 395 _refine_ls_number_restraints 308 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_obs 0.0289 _refine_ls_wR_factor_all 0.0785 _refine_ls_wR_factor_obs 0.0783 _refine_ls_goodness_of_fit_all 1.076 _refine_ls_goodness_of_fit_obs 1.076 _refine_ls_restrained_S_all 1.108 _refine_ls_restrained_S_obs 1.108 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ba Ba 0.5000 0.5000 0.5000 0.01899(6) Uani 1 d S . O1 O 0.37533(13) 0.49079(13) 0.28988(10) 0.0255(3) Uani 1 d . . C1 C 0.4034(2) 0.4332(2) 0.1982(2) 0.0270(4) Uani 1 d . . C2 C 0.4745(2) 0.3395(2) 0.2023(2) 0.0376(5) Uani 1 d . . H2 H 0.4996(2) 0.3170(2) 0.2664(2) 0.045 Uiso 1 calc R . C3 C 0.5088(2) 0.2791(2) 0.1130(2) 0.0457(6) Uani 1 d . . H3 H 0.5587(2) 0.2164(2) 0.1169(2) 0.055 Uiso 1 calc R . C4 C 0.4711(3) 0.3092(2) 0.0185(2) 0.0478(6) Uani 1 d . . H4 H 0.4941(3) 0.2673(2) -0.0427(2) 0.057 Uiso 1 calc R . C5 C 0.3996(3) 0.4009(3) 0.0146(2) 0.0478(6) Uani 1 d . . H5 H 0.3734(3) 0.4221(3) -0.0501(2) 0.057 Uiso 1 calc R . C6 C 0.3648(2) 0.4631(2) 0.1030(2) 0.0377(5) Uani 1 d . . H6 H 0.3150(2) 0.5258(2) 0.0985(2) 0.045 Uiso 1 calc R . B B 0.3092(2) 0.5985(2) 0.2985(2) 0.0233(4) Uani 1 d . . O2 O 0.39274(13) 0.69522(14) 0.29345(12) 0.0299(3) Uani 1 d . . C7 C 0.3877(2) 0.7720(2) 0.2330(2) 0.0254(4) Uani 1 d . . C8 C 0.4952(2) 0.8532(2) 0.2585(2) 0.0315(4) Uani 1 d . . H8 H 0.5650(2) 0.8516(2) 0.3151(2) 0.038 Uiso 1 calc R . C9 C 0.5009(2) 0.9359(2) 0.2020(2) 0.0370(5) Uani 1 d . . H9 H 0.5744(2) 0.9906(2) 0.2204(2) 0.044 Uiso 1 calc R . C10 C 0.4003(3) 0.9396(2) 0.1188(2) 0.0390(5) Uani 1 d . . H10 H 0.4044(3) 0.9960(2) 0.0799(2) 0.047 Uiso 1 calc R . C11 C 0.2942(2) 0.8598(2) 0.0937(2) 0.0373(5) Uani 1 d . . H11 H 0.2249(2) 0.8619(2) 0.0368(2) 0.045 Uiso 1 calc R . C12 C 0.2864(2) 0.7762(2) 0.1499(2) 0.0303(4) Uani 1 d . . H12 H 0.2123(2) 0.7224(2) 0.1315(2) 0.036 Uiso 1 calc R . O3 O 0.18895(13) 0.58366(13) 0.22155(11) 0.0259(3) Uani 1 d . . C13 C 0.0907(2) 0.5015(2) 0.20720(15) 0.0246(4) Uani 1 d . . C14 C -0.0209(2) 0.5065(2) 0.1342(2) 0.0317(4) Uani 1 d . . H14 H -0.0254(2) 0.5653(2) 0.0968(2) 0.038 Uiso 1 calc R . C15 C -0.1255(2) 0.4259(2) 0.1159(2) 0.0395(5) Uani 1 d . . H15 H -0.2014(2) 0.4302(2) 0.0665(2) 0.047 Uiso 1 calc R . C16 C -0.1201(2) 0.3393(2) 0.1692(2) 0.0421(5) Uani 1 d . . H16 H -0.1918(2) 0.2843(2) 0.1567(2) 0.051 Uiso 1 calc R . C17 C -0.0092(2) 0.3336(2) 0.2407(2) 0.0429(6) Uani 1 d . . H17 H -0.0049(2) 0.2739(2) 0.2771(2) 0.052 Uiso 1 calc R . C18 C 0.0959(2) 0.4141(2) 0.2600(2) 0.0343(5) Uani 1 d . . H18 H 0.1715(2) 0.4093(2) 0.3095(2) 0.041 Uiso 1 calc R . O4 O 0.30217(13) 0.61916(12) 0.41092(10) 0.0237(3) Uani 1 d . . C19 C 0.2473(2) 0.7110(2) 0.4591(2) 0.0253(4) Uani 1 d . . C20 C 0.1823(2) 0.7864(2) 0.4068(2) 0.0317(4) Uani 1 d . . H20 H 0.1736(2) 0.7757(2) 0.3332(2) 0.038 Uiso 1 calc R . C21 C 0.1299(2) 0.8777(2) 0.4634(2) 0.0429(6) Uani 1 d . . H21 H 0.0847(2) 0.9284(2) 0.4273(2) 0.052 Uiso 1 calc R . C22 C 0.1423(3) 0.8957(2) 0.5707(2) 0.0477(6) Uani 1 d . . H22 H 0.1072(3) 0.9588(2) 0.6085(2) 0.057 Uiso 1 calc R . C23 C 0.2069(2) 0.8203(3) 0.6224(2) 0.0459(6) Uani 1 d . . H23 H 0.2160(2) 0.8319(3) 0.6962(2) 0.055 Uiso 1 calc R . C24 C 0.2584(2) 0.7280(2) 0.5673(2) 0.0363(5) Uani 1 d . . H24 H 0.3013(2) 0.6762(2) 0.6033(2) 0.044 Uiso 1 calc R . O5 O 0.4086(2) 0.25893(14) 0.41017(15) 0.0399(4) Uani 1 d DU . C25 C 0.2842(5) 0.2229(5) 0.3559(5) 0.035(2) Uani 0.412(9) d PDU 1 H25A H 0.2672(5) 0.2422(5) 0.2869(5) 0.042 Uiso 0.412(9) calc PR 1 H25B H 0.2303(5) 0.2660(5) 0.3973(5) 0.042 Uiso 0.412(9) calc PR 1 C26 C 0.25293(8) 0.09365(8) 0.33747(7) 0.0496(6) Uani 1 d DU . H26A H 0.27085(8) 0.04756(8) 0.27166(7) 0.060 Uiso 0.412(9) calc PR 1 H26B H 0.16436(8) 0.07254(8) 0.33524(7) 0.060 Uiso 0.412(9) calc PR 1 H26C H 0.23442(8) 0.01931(8) 0.27952(7) 0.060 Uiso 0.588(9) calc PR 2 H26D H 0.17319(8) 0.11641(8) 0.35263(7) 0.060 Uiso 0.588(9) calc PR 2 C27 C 0.34352(8) 0.07752(8) 0.43672(7) 0.0564(8) Uani 1 d RDU . H27A H 0.30760(8) 0.09705(8) 0.49840(7) 0.068 Uiso 1 calc R . H27B H 0.36475(8) -0.00455(8) 0.42532(7) 0.068 Uiso 1 calc R . C28 C 0.45808(8) 0.16454(8) 0.45281(7) 0.0502(7) Uani 1 d RDU . H28A H 0.50235(8) 0.19510(8) 0.52909(7) 0.060 Uiso 1 calc R . H28B H 0.51712(8) 0.12642(8) 0.41431(7) 0.060 Uiso 1 calc R . C25A C 0.31780(8) 0.19102(8) 0.30628(7) 0.0431(14) Uani 0.588(9) d PRDU 2 H25C H 0.36251(8) 0.15798(8) 0.25243(7) 0.052 Uiso 0.588(9) calc PR 2 H25D H 0.25721(8) 0.24163(8) 0.27836(7) 0.052 Uiso 0.588(9) calc PR 2 O6 O 0.69379(8) 0.55313(8) 0.41258(7) 0.0369(4) Uani 1 d RD . C29 C 0.81291(8) 0.59107(8) 0.47891(7) 0.0316(12) Uani 0.499(9) d PRDU 1 H29A H 0.84505(8) 0.52742(8) 0.51019(7) 0.038 Uiso 0.499(9) calc PR 1 H29B H 0.81099(8) 0.66055(8) 0.53739(7) 0.038 Uiso 0.499(9) calc PR 1 C29A C 0.83076(8) 0.52947(8) 0.44060(7) 0.049(2) Uani 0.501(9) d PRDU 2 H29C H 0.86096(8) 0.53310(8) 0.51677(7) 0.059 Uiso 0.501(9) calc PR 2 H29D H 0.84129(8) 0.45101(8) 0.39762(7) 0.059 Uiso 0.501(9) calc PR 2 C30 C 0.89718(8) 0.62364(8) 0.41547(7) 0.0574(8) Uani 1 d RDU . H30A H 0.92830(8) 0.55353(8) 0.37640(7) 0.069 Uiso 0.499(9) calc PR 1 H30B H 0.96905(8) 0.68285(8) 0.46038(7) 0.069 Uiso 0.499(9) calc PR 1 H30C H 0.96226(8) 0.59213(8) 0.38098(7) 0.069 Uiso 0.501(9) calc PR 2 H30D H 0.93900(8) 0.68593(8) 0.48137(7) 0.069 Uiso 0.501(9) calc PR 2 C31 C 0.80458(8) 0.67506(8) 0.34181(7) 0.0656(9) Uani 1 d RDU . H31A H 0.82989(8) 0.67227(8) 0.27586(7) 0.079 Uiso 1 calc R . H31B H 0.79655(8) 0.75791(8) 0.37657(7) 0.079 Uiso 1 calc R . C32 C 0.68298(8) 0.59512(8) 0.31898(7) 0.0558(8) Uani 1 d RDU . H32A H 0.60992(8) 0.63970(8) 0.30750(7) 0.067 Uiso 1 calc R . H32B H 0.67337(8) 0.52820(8) 0.25523(7) 0.067 Uiso 1 calc R . O7 O 0.08327(8) 1.20406(8) 0.96490(7) 0.1253(14) Uani 1 d RD . C33 C 0.07187(8) 1.17601(8) 0.85187(7) 0.109(4) Uani 0.611(11) d PRDU 1 H33A H -0.01383(8) 1.18487(8) 0.81334(7) 0.131 Uiso 0.611(11) calc PR 1 H33B H 0.13235(8) 1.23060(8) 0.83730(7) 0.131 Uiso 0.611(11) calc PR 1 C33A C 0.02544(8) 1.14916(8) 0.85302(7) 0.078(4) Uani 0.389(11) d PRDU 2 H33C H -0.06235(8) 1.11611(8) 0.84238(7) 0.094 Uiso 0.389(11) calc PR 2 H33D H 0.02503(8) 1.20848(8) 0.81232(7) 0.094 Uiso 0.389(11) calc PR 2 C34 C 0.09725(8) 1.05586(8) 0.81682(7) 0.0924(14) Uani 1 d RDU . H34A H 0.02009(8) 0.99980(8) 0.79828(7) 0.111 Uiso 0.611(11) calc PR 1 H34B H 0.13124(8) 1.04485(8) 0.75414(7) 0.111 Uiso 0.611(11) calc PR 1 H34C H 0.17258(8) 1.08736(8) 0.80038(7) 0.111 Uiso 0.389(11) calc PR 2 H34D H 0.04590(8) 0.99494(8) 0.75357(7) 0.111 Uiso 0.389(11) calc PR 2 C35 C 0.18572(8) 1.03907(8) 0.90322(7) 0.090(3) Uani 0.611(11) d PRDU 1 H35A H 0.27166(8) 1.06227(8) 0.89997(7) 0.108 Uiso 0.611(11) calc PR 1 H35B H 0.17794(8) 0.95501(8) 0.90367(7) 0.108 Uiso 0.611(11) calc PR 1 C35A C 0.13158(8) 1.00841(8) 0.91096(7) 0.119(5) Uani 0.389(11) d PRDU 2 H35C H 0.20662(8) 0.96638(8) 0.91106(7) 0.142 Uiso 0.389(11) calc PR 2 H35D H 0.06147(8) 0.95368(8) 0.91270(7) 0.142 Uiso 0.389(11) calc PR 2 C36 C 0.15853(8) 1.11828(8) 1.00396(7) 0.0908(14) Uani 1 d RDU . H36A H 0.11138(8) 1.07107(8) 1.03670(7) 0.109 Uiso 0.611(11) calc PR 1 H36B H 0.23745(8) 1.15836(8) 1.05694(7) 0.109 Uiso 0.611(11) calc PR 1 H36C H 0.13397(8) 1.10083(8) 1.06490(7) 0.109 Uiso 0.389(11) calc PR 2 H36D H 0.24886(8) 1.14876(8) 1.02661(7) 0.109 Uiso 0.389(11) calc PR 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 Ba 0.01762(9) 0.02049(9) 0.01883(9) 0.00635(5) 0.00393(5) 0.00166(5) O1 0.0273(7) 0.0297(7) 0.0192(6) 0.0063(5) 0.0051(5) 0.0089(5) C1 0.0243(9) 0.0292(10) 0.0238(9) 0.0020(7) 0.0051(7) 0.0016(7) C2 0.0358(11) 0.0391(12) 0.0312(11) 0.0011(9) 0.0036(9) 0.0120(9) C3 0.0407(13) 0.0423(13) 0.0461(14) -0.0046(11) 0.0119(11) 0.0128(10) C4 0.056(2) 0.0466(14) 0.0397(13) -0.0035(11) 0.0269(12) 0.0035(12) C5 0.069(2) 0.0482(14) 0.0293(11) 0.0077(10) 0.0214(12) 0.0089(13) C6 0.0496(13) 0.0390(12) 0.0279(10) 0.0097(9) 0.0143(10) 0.0122(10) B 0.0221(10) 0.0264(10) 0.0216(9) 0.0079(8) 0.0044(8) 0.0040(8) O2 0.0249(7) 0.0367(8) 0.0289(7) 0.0166(6) 0.0018(6) -0.0013(6) C7 0.0295(10) 0.0247(9) 0.0231(9) 0.0065(7) 0.0092(7) 0.0035(7) C8 0.0325(10) 0.0315(10) 0.0281(10) 0.0058(8) 0.0077(8) -0.0016(8) C9 0.0438(12) 0.0274(10) 0.0395(12) 0.0058(9) 0.0159(10) -0.0042(9) C10 0.0538(14) 0.0273(10) 0.0410(12) 0.0147(9) 0.0166(11) 0.0053(10) C11 0.0434(13) 0.0322(11) 0.0379(12) 0.0166(9) 0.0061(10) 0.0064(9) C12 0.0318(10) 0.0284(10) 0.0306(10) 0.0106(8) 0.0057(8) 0.0032(8) O3 0.0225(7) 0.0281(7) 0.0267(7) 0.0121(5) 0.0015(5) 0.0017(5) C13 0.0234(9) 0.0257(9) 0.0228(9) 0.0048(7) 0.0046(7) 0.0030(7) C14 0.0285(10) 0.0349(11) 0.0292(10) 0.0108(8) 0.0009(8) 0.0045(8) C15 0.0264(10) 0.0474(13) 0.0365(12) 0.0085(10) -0.0028(9) -0.0009(9) C16 0.0311(11) 0.0451(13) 0.0440(13) 0.0106(11) 0.0033(10) -0.0088(10) C17 0.0378(12) 0.0412(13) 0.0495(14) 0.0212(11) 0.0042(10) -0.0057(10) C18 0.0280(10) 0.0365(11) 0.0382(11) 0.0180(9) 0.0007(9) 0.0004(8) O4 0.0242(6) 0.0269(7) 0.0220(6) 0.0080(5) 0.0072(5) 0.0076(5) C19 0.0198(8) 0.0253(9) 0.0301(10) 0.0044(7) 0.0083(7) 0.0024(7) C20 0.0300(10) 0.0279(10) 0.0421(12) 0.0131(9) 0.0144(9) 0.0057(8) C21 0.0386(12) 0.0294(11) 0.070(2) 0.0165(11) 0.0264(12) 0.0110(9) C22 0.0407(13) 0.0356(12) 0.065(2) -0.0026(11) 0.0277(12) 0.0067(10) C23 0.0374(12) 0.057(2) 0.0381(12) -0.0038(11) 0.0165(10) 0.0070(11) C24 0.0295(10) 0.0480(13) 0.0298(11) 0.0048(9) 0.0094(8) 0.0103(9) O5 0.0404(9) 0.0253(7) 0.0488(10) 0.0033(7) 0.0111(7) -0.0040(6) C25 0.034(3) 0.038(3) 0.033(3) 0.012(2) 0.008(2) 0.001(2) C26 0.0479(15) 0.0410(14) 0.0481(15) 0.0027(11) 0.0043(12) -0.0119(11) C27 0.060(2) 0.049(2) 0.054(2) 0.0186(13) 0.0041(13) -0.0213(13) C28 0.052(2) 0.0455(14) 0.0455(14) 0.0194(12) -0.0027(12) -0.0171(12) C25A 0.047(3) 0.031(2) 0.041(3) 0.005(2) -0.001(2) 0.000(2) O6 0.0322(8) 0.0429(9) 0.0372(8) 0.0095(7) 0.0156(7) -0.0049(7) C29 0.029(2) 0.030(2) 0.033(2) 0.005(2) 0.007(2) 0.002(2) C29A 0.027(2) 0.066(4) 0.063(4) 0.033(3) 0.012(2) 0.005(2) C30 0.0321(13) 0.073(2) 0.075(2) 0.029(2) 0.0197(13) 0.0009(12) C31 0.044(2) 0.072(2) 0.099(3) 0.052(2) 0.025(2) -0.0018(14) C32 0.0327(12) 0.072(2) 0.079(2) 0.050(2) 0.0142(13) 0.0041(12) O7 0.131(3) 0.115(3) 0.121(3) 0.026(2) 0.016(3) 0.049(3) C33 0.168(9) 0.116(6) 0.065(5) 0.039(5) 0.047(6) 0.068(7) C33A 0.094(8) 0.084(7) 0.059(7) 0.032(5) 0.008(5) 0.029(6) C34 0.113(4) 0.094(3) 0.059(2) -0.004(2) 0.022(2) 0.037(3) C35 0.105(6) 0.067(5) 0.096(5) 0.010(4) 0.029(4) 0.039(4) C35A 0.119(11) 0.045(5) 0.171(10) 0.027(6) 0.001(10) 0.026(7) C36 0.109(3) 0.087(3) 0.069(2) 0.026(2) -0.001(2) 0.035(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 Ba O6 2.80 2_666 ? Ba O6 2.80 . ? Ba O1 2.8087(13) . ? Ba O1 2.8088(13) 2_666 ? Ba O5 2.813(2) . ? Ba O5 2.813(2) 2_666 ? Ba O4 2.8478(13) . ? Ba O4 2.8479(13) 2_666 ? O1 C1 1.372(2) . ? O1 B 1.492(2) . ? C1 C6 1.390(3) . ? C1 C2 1.393(3) . ? C2 C3 1.389(3) . ? C3 C4 1.382(4) . ? C4 C5 1.377(4) . ? C5 C6 1.388(3) . ? B O3 1.448(2) . ? B O2 1.453(3) . ? B O4 1.498(2) . ? O2 C7 1.355(2) . ? C7 C12 1.393(3) . ? C7 C8 1.401(3) . ? C8 C9 1.385(3) . ? C9 C10 1.388(4) . ? C10 C11 1.379(4) . ? C11 C12 1.395(3) . ? O3 C13 1.358(2) . ? C13 C18 1.387(3) . ? C13 C14 1.396(3) . ? C14 C15 1.389(3) . ? C15 C16 1.382(4) . ? C16 C17 1.381(4) . ? C17 C18 1.389(3) . ? O4 C19 1.369(2) . ? C19 C20 1.393(3) . ? C19 C24 1.397(3) . ? C20 C21 1.396(3) . ? C21 C22 1.383(4) . ? C22 C23 1.386(4) . ? C23 C24 1.390(3) . ? O5 C25 1.380(6) . ? O5 C28 1.449(2) . ? O5 C25A 1.511(2) . ? C25 C26 1.485(6) . ? C26 C25A 1.52 . ? C26 C27 1.53 . ? C27 C28 1.52 . ? O6 C29 1.38 . ? O6 C32 1.45 . ? O6 C29A 1.53 . ? C29 C30 1.51 . ? C29A C30 1.45 . ? C30 C31 1.51 . ? C31 C32 1.52 . ? O7 C33 1.45 . ? O7 C33A 1.45 . ? O7 C36 1.46 . ? C33 C34 1.44 . ? C33A C34 1.45 . ? C34 C35 1.39 . ? C34 C35A 1.49 . ? C35 C36 1.55 . ? C35A C36 1.52 . ? 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 O6 Ba O6 180.0 2_666 . ? O6 Ba O1 103.77(3) 2_666 . ? O6 Ba O1 76.23(3) . . ? O6 Ba O1 76.23(3) 2_666 2_666 ? O6 Ba O1 103.77(3) . 2_666 ? O1 Ba O1 179.999(1) . 2_666 ? O6 Ba O5 71.86(4) 2_666 . ? O6 Ba O5 108.14(4) . . ? O1 Ba O5 77.01(5) . . ? O1 Ba O5 102.99(5) 2_666 . ? O6 Ba O5 108.14(4) 2_666 2_666 ? O6 Ba O5 71.86(4) . 2_666 ? O1 Ba O5 102.99(5) . 2_666 ? O1 Ba O5 77.01(5) 2_666 2_666 ? O5 Ba O5 180.0 . 2_666 ? O6 Ba O4 76.25(3) 2_666 . ? O6 Ba O4 103.75(3) . . ? O1 Ba O4 47.32(4) . . ? O1 Ba O4 132.68(4) 2_666 . ? O5 Ba O4 103.97(5) . . ? O5 Ba O4 76.03(5) 2_666 . ? O6 Ba O4 103.75(3) 2_666 2_666 ? O6 Ba O4 76.25(3) . 2_666 ? O1 Ba O4 132.68(4) . 2_666 ? O1 Ba O4 47.32(4) 2_666 2_666 ? O5 Ba O4 76.03(5) . 2_666 ? O5 Ba O4 103.97(5) 2_666 2_666 ? O4 Ba O4 180.0 . 2_666 ? C1 O1 B 122.5(2) . . ? C1 O1 Ba 128.39(11) . . ? B O1 Ba 104.78(10) . . ? O1 C1 C6 123.6(2) . . ? O1 C1 C2 117.2(2) . . ? C6 C1 C2 119.2(2) . . ? C3 C2 C1 120.2(2) . . ? C4 C3 C2 120.7(2) . . ? C5 C4 C3 118.8(2) . . ? C4 C5 C6 121.6(2) . . ? C5 C6 C1 119.6(2) . . ? O3 B O2 111.3(2) . . ? O3 B O1 114.8(2) . . ? O2 B O1 108.6(2) . . ? O3 B O4 114.4(2) . . ? O2 B O4 108.1(2) . . ? O1 B O4 98.83(14) . . ? C7 O2 B 136.2(2) . . ? O2 C7 C12 125.8(2) . . ? O2 C7 C8 115.5(2) . . ? C12 C7 C8 118.7(2) . . ? C9 C8 C7 120.7(2) . . ? C8 C9 C10 120.6(2) . . ? C11 C10 C9 118.8(2) . . ? C10 C11 C12 121.4(2) . . ? C7 C12 C11 119.8(2) . . ? C13 O3 B 125.5(2) . . ? O3 C13 C18 123.9(2) . . ? O3 C13 C14 117.1(2) . . ? C18 C13 C14 119.0(2) . . ? C15 C14 C13 120.3(2) . . ? C16 C15 C14 120.5(2) . . ? C17 C16 C15 119.3(2) . . ? C16 C17 C18 120.8(2) . . ? C13 C18 C17 120.1(2) . . ? C19 O4 B 122.39(15) . . ? C19 O4 Ba 130.00(11) . . ? B O4 Ba 102.86(10) . . ? O4 C19 C20 123.9(2) . . ? O4 C19 C24 116.8(2) . . ? C20 C19 C24 119.3(2) . . ? C19 C20 C21 119.5(2) . . ? C22 C21 C20 121.3(2) . . ? C21 C22 C23 119.0(2) . . ? C22 C23 C24 120.5(2) . . ? C23 C24 C19 120.4(2) . . ? C25 O5 C28 108.3(3) . . ? C28 O5 C25A 101.97(11) . . ? C25 O5 Ba 121.3(3) . . ? C28 O5 Ba 124.31(10) . . ? C25A O5 Ba 133.17(10) . . ? O5 C25 C26 110.9(4) . . ? C25 C26 C27 99.1(2) . . ? C25A C26 C27 106.3 . . ? C28 C27 C26 103.1 . . ? O5 C28 C27 104.82(7) . . ? O5 C25A C26 102.43(7) . . ? C29 O6 C32 108.7 . . ? C32 O6 C29A 103.0 . . ? C29 O6 Ba 118.8 . . ? C32 O6 Ba 127.3 . . ? C29A O6 Ba 129.3 . . ? O6 C29 C30 108.7 . . ? C30 C29A O6 103.7 . . ? C29A C30 C31 109.0 . . ? C29 C30 C31 99.0 . . ? C30 C31 C32 103.1 . . ? O6 C32 C31 104.9 . . ? C33 O7 C36 106.0 . . ? C33A O7 C36 106.2 . . ? C34 C33 O7 108.4 . . ? C34 C33A O7 108.1 . . ? C35 C34 C33 104.5 . . ? C33A C34 C35A 101.3 . . ? C34 C35 C36 106.4 . . ? C34 C35A C36 103.5 . . ? O7 C36 C35A 105.3 . . ? O7 C36 C35 104.1 . . ? _refine_diff_density_max 0.728 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.073 #===END data_rje215 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H65 B2 Ba O13' _chemical_formula_weight 1129.06 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' 'B' 'B' 0.0013 0.0007 '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' 'Ba' 'Ba' -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2348(6) _cell_length_b 20.0431(11) _cell_length_c 25.0246(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.881(2) _cell_angle_gamma 90.00 _cell_volume 5634.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 15851 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 28.68 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2332 _exptl_absorpt_coefficient_mu 0.77 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 35072 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.88 _reflns_number_total 13367 _reflns_number_gt 8751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0416P)^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 0.00019(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13367 _refine_ls_number_parameters 645 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba Ba 0.273558(15) 0.254310(9) 0.146774(7) 0.01926(6) Uani 1 1 d . . . O1 O 0.44525(18) 0.20384(10) 0.07805(9) 0.0245(5) Uani 1 1 d . . . C1 C 0.4413(3) 0.17921(17) 0.02670(14) 0.0289(8) Uani 1 1 d . . . C2 C 0.4308(3) 0.2216(2) -0.01645(15) 0.0413(10) Uani 1 1 d . . . H2 H 0.4320 0.2685 -0.0109 0.050 Uiso 1 1 calc R . . C3 C 0.4188(4) 0.1967(3) -0.06770(17) 0.0580(12) Uani 1 1 d . . . H3 H 0.4115 0.2266 -0.0971 0.070 Uiso 1 1 calc R . . C4 C 0.4171(4) 0.1297(3) -0.0764(2) 0.0656(15) Uani 1 1 d . . . H4 H 0.4070 0.1130 -0.1117 0.079 Uiso 1 1 calc R . . C5 C 0.4299(4) 0.0868(2) -0.0348(2) 0.0614(14) Uani 1 1 d . . . H5 H 0.4308 0.0400 -0.0412 0.074 Uiso 1 1 calc R . . C6 C 0.4419(3) 0.11113(19) 0.01789(17) 0.0459(10) Uani 1 1 d . . . H6 H 0.4504 0.0810 0.0470 0.055 Uiso 1 1 calc R . . O2 O 0.51354(17) 0.24056(10) 0.15826(9) 0.0244(5) Uani 1 1 d . . . C7 C 0.5855(3) 0.26222(16) 0.19973(13) 0.0242(7) Uani 1 1 d . . . C8 C 0.6075(3) 0.22084(19) 0.24279(15) 0.0363(9) Uani 1 1 d . . . H8 H 0.5792 0.1762 0.2420 0.044 Uiso 1 1 calc R . . C9 C 0.6705(3) 0.2438(2) 0.28724(15) 0.0444(10) Uani 1 1 d . . . H9 H 0.6857 0.2149 0.3166 0.053 Uiso 1 1 calc R . . C10 C 0.7112(3) 0.3093(2) 0.28857(16) 0.0418(10) Uani 1 1 d . . . H10 H 0.7524 0.3258 0.3192 0.050 Uiso 1 1 calc R . . C11 C 0.6912(3) 0.34990(19) 0.24498(16) 0.0396(10) Uani 1 1 d . . . H11 H 0.7205 0.3944 0.2454 0.047 Uiso 1 1 calc R . . C12 C 0.6289(3) 0.32687(17) 0.20049(15) 0.0309(8) Uani 1 1 d . . . H12 H 0.6160 0.3553 0.1706 0.037 Uiso 1 1 calc R . . O3 O 0.25576(18) 0.38370(10) 0.11800(9) 0.0239(5) Uani 1 1 d . . . C13 C 0.2824(3) 0.40883(15) 0.06836(13) 0.0247(7) Uani 1 1 d . . . C14 C 0.1957(3) 0.44012(17) 0.03781(14) 0.0317(8) Uani 1 1 d . . . H14 H 0.1188 0.4474 0.0519 0.038 Uiso 1 1 calc R . . C15 C 0.2216(4) 0.46092(18) -0.01389(15) 0.0416(10) Uani 1 1 d . . . H15 H 0.1615 0.4813 -0.0354 0.050 Uiso 1 1 calc R . . C16 C 0.3346(4) 0.45196(19) -0.03401(15) 0.0422(10) Uani 1 1 d . . . H16 H 0.3523 0.4663 -0.0692 0.051 Uiso 1 1 calc R . . C17 C 0.4209(3) 0.42219(18) -0.00278(15) 0.0380(9) Uani 1 1 d . . . H17 H 0.4986 0.4165 -0.0165 0.046 Uiso 1 1 calc R . . C18 C 0.3969(3) 0.40018(16) 0.04855(14) 0.0307(8) Uani 1 1 d . . . H18 H 0.4573 0.3796 0.0698 0.037 Uiso 1 1 calc R . . O4 O 0.26509(18) 0.36905(10) 0.20771(9) 0.0224(5) Uani 1 1 d . . . C19 C 0.2787(3) 0.38457(15) 0.26122(13) 0.0236(7) Uani 1 1 d . . . C20 C 0.3901(3) 0.38906(18) 0.28440(15) 0.0375(9) Uani 1 1 d . . . H20 H 0.4587 0.3845 0.2630 0.045 Uiso 1 1 calc R . . C21 C 0.4029(4) 0.40019(19) 0.33891(16) 0.0468(10) Uani 1 1 d . . . H21 H 0.4801 0.4027 0.3547 0.056 Uiso 1 1 calc R . . C22 C 0.3052(4) 0.40758(18) 0.36976(16) 0.0473(11) Uani 1 1 d . . . H22 H 0.3142 0.4157 0.4070 0.057 Uiso 1 1 calc R . . C23 C 0.1942(4) 0.4033(2) 0.34708(16) 0.0496(11) Uani 1 1 d . . . H23 H 0.1261 0.4081 0.3688 0.059 Uiso 1 1 calc R . . C24 C 0.1795(3) 0.39194(19) 0.29204(15) 0.0396(9) Uani 1 1 d . . . H24 H 0.1021 0.3894 0.2764 0.047 Uiso 1 1 calc R . . B1 B 0.5599(3) 0.22234(18) 0.10483(16) 0.0241(8) Uani 1 1 d . . . O5 O 0.61422(18) 0.28130(10) 0.08181(9) 0.0269(5) Uani 1 1 d . . . C25 C 0.6836(3) 0.28703(15) 0.03852(14) 0.0233(7) Uani 1 1 d . . . C26 C 0.7242(3) 0.35087(16) 0.02626(15) 0.0300(8) Uani 1 1 d . . . H26 H 0.7046 0.3872 0.0489 0.036 Uiso 1 1 calc R . . C27 C 0.7927(3) 0.36214(18) -0.01836(16) 0.0374(9) Uani 1 1 d . . . H27 H 0.8196 0.4060 -0.0259 0.045 Uiso 1 1 calc R . . C28 C 0.8224(3) 0.31055(19) -0.05201(15) 0.0374(9) Uani 1 1 d . . . H28 H 0.8694 0.3184 -0.0826 0.045 Uiso 1 1 calc R . . C29 C 0.7823(3) 0.24711(18) -0.04025(14) 0.0343(8) Uani 1 1 d . . . H29 H 0.8018 0.2113 -0.0633 0.041 Uiso 1 1 calc R . . C30 C 0.7143(3) 0.23447(16) 0.00441(14) 0.0287(8) Uani 1 1 d . . . H30 H 0.6886 0.1903 0.0119 0.034 Uiso 1 1 calc R . . O6 O 0.64822(18) 0.16902(10) 0.10686(9) 0.0265(5) Uani 1 1 d . . . C31 C 0.6379(3) 0.11181(15) 0.13545(14) 0.0252(7) Uani 1 1 d . . . C32 C 0.7411(3) 0.07535(18) 0.14509(15) 0.0357(9) Uani 1 1 d . . . H32 H 0.8147 0.0909 0.1317 0.043 Uiso 1 1 calc R . . C33 C 0.7377(3) 0.01644(18) 0.17418(17) 0.0433(10) Uani 1 1 d . . . H33 H 0.8090 -0.0082 0.1801 0.052 Uiso 1 1 calc R . . C34 C 0.6322(3) -0.00668(18) 0.19457(16) 0.0404(10) Uani 1 1 d . . . H34 H 0.6302 -0.0466 0.2150 0.048 Uiso 1 1 calc R . . C35 C 0.5304(3) 0.02895(16) 0.18489(15) 0.0336(9) Uani 1 1 d . . . H35 H 0.4574 0.0132 0.1988 0.040 Uiso 1 1 calc R . . C36 C 0.5309(3) 0.08746(16) 0.15522(15) 0.0337(9) Uani 1 1 d . . . H36 H 0.4587 0.1108 0.1484 0.040 Uiso 1 1 calc R . . B2 B 0.2832(3) 0.42274(17) 0.16717(16) 0.0235(8) Uani 1 1 d . . . O7 O 0.20746(18) 0.48052(10) 0.17430(9) 0.0252(5) Uani 1 1 d . . . C37 C 0.0881(3) 0.48208(16) 0.16628(13) 0.0253(7) Uani 1 1 d . . . C38 C 0.0152(3) 0.42557(17) 0.16632(15) 0.0322(8) Uani 1 1 d . . . H38 H 0.0491 0.3826 0.1717 0.039 Uiso 1 1 calc R . . C39 C -0.1066(3) 0.4323(2) 0.15856(15) 0.0409(10) Uani 1 1 d . . . H39 H -0.1552 0.3935 0.1582 0.049 Uiso 1 1 calc R . . C40 C -0.1582(3) 0.4932(2) 0.15140(16) 0.0470(11) Uani 1 1 d . . . H40 H -0.2420 0.4970 0.1467 0.056 Uiso 1 1 calc R . . C41 C -0.0874(4) 0.5490(2) 0.15113(17) 0.0488(11) Uani 1 1 d . . . H41 H -0.1229 0.5916 0.1463 0.059 Uiso 1 1 calc R . . C42 C 0.0351(3) 0.54419(18) 0.15782(15) 0.0357(9) Uani 1 1 d . . . H42 H 0.0830 0.5832 0.1566 0.043 Uiso 1 1 calc R . . O8 O 0.40621(18) 0.44436(10) 0.16962(9) 0.0250(5) Uani 1 1 d . . . C43 C 0.4466(3) 0.50860(15) 0.16714(13) 0.0226(7) Uani 1 1 d . . . C44 C 0.5372(3) 0.52680(16) 0.20252(14) 0.0286(8) Uani 1 1 d . . . H44 H 0.5664 0.4952 0.2278 0.034 Uiso 1 1 calc R . . C45 C 0.5858(3) 0.59013(17) 0.20163(16) 0.0360(9) Uani 1 1 d . . . H45 H 0.6473 0.6019 0.2263 0.043 Uiso 1 1 calc R . . C46 C 0.5449(3) 0.63592(17) 0.16502(16) 0.0357(9) Uani 1 1 d . . . H46 H 0.5782 0.6795 0.1643 0.043 Uiso 1 1 calc R . . C47 C 0.4543(3) 0.61860(16) 0.12876(14) 0.0307(8) Uani 1 1 d . . . H47 H 0.4257 0.6504 0.1036 0.037 Uiso 1 1 calc R . . C48 C 0.4062(3) 0.55491(16) 0.12955(13) 0.0263(8) Uani 1 1 d . . . H48 H 0.3457 0.5429 0.1044 0.032 Uiso 1 1 calc R . . O9 O 0.2224(2) 0.11864(11) 0.14887(9) 0.0296(5) Uani 1 1 d . . . C49 C 0.1777(3) 0.09094(17) 0.19698(15) 0.0361(9) Uani 1 1 d . . . H49A H 0.1822 0.0417 0.1954 0.043 Uiso 1 1 calc R . . H49B H 0.0931 0.1037 0.2010 0.043 Uiso 1 1 calc R . . C50 C 0.2483(3) 0.11564(16) 0.24364(15) 0.0341(9) Uani 1 1 d . . . H50A H 0.2134 0.0987 0.2771 0.041 Uiso 1 1 calc R . . H50B H 0.3310 0.0990 0.2416 0.041 Uiso 1 1 calc R . . O10 O 0.2482(2) 0.18704(11) 0.24401(9) 0.0307(6) Uani 1 1 d . . . C51 C 0.1726(4) 0.0895(2) 0.10164(16) 0.0536(12) Uani 1 1 d . . . H51A H 0.1931 0.0420 0.1005 0.080 Uiso 1 1 calc R . . H51B H 0.2045 0.1119 0.0702 0.080 Uiso 1 1 calc R . . H51C H 0.0858 0.0944 0.1018 0.080 Uiso 1 1 calc R . . C52 C 0.2913(4) 0.21195(18) 0.29434(15) 0.0412(10) Uani 1 1 d . . . H52A H 0.2424 0.1941 0.3231 0.062 Uiso 1 1 calc R . . H52B H 0.2868 0.2608 0.2944 0.062 Uiso 1 1 calc R . . H52C H 0.3742 0.1980 0.2999 0.062 Uiso 1 1 calc R . . O11 O 0.02765(19) 0.25332(12) 0.16531(10) 0.0365(6) Uani 1 1 d . . . C53 C -0.0527(3) 0.2474(2) 0.12080(19) 0.0530(11) Uani 1 1 d . . . H53A H -0.1290 0.2693 0.1293 0.064 Uiso 1 1 calc R . . H53B H -0.0688 0.1996 0.1136 0.064 Uiso 1 1 calc R . . C54 C -0.0018(3) 0.2787(3) 0.07278(18) 0.0576(13) Uani 1 1 d . . . H54A H -0.0580 0.2739 0.0422 0.069 Uiso 1 1 calc R . . H54B H 0.0113 0.3268 0.0793 0.069 Uiso 1 1 calc R . . O12 O 0.1084(2) 0.24723(13) 0.06063(10) 0.0411(6) Uani 1 1 d . . . C55 C -0.0274(4) 0.2423(2) 0.21517(19) 0.0636(14) Uani 1 1 d . . . H55A H -0.0902 0.2755 0.2203 0.095 Uiso 1 1 calc R . . H55B H 0.0322 0.2463 0.2440 0.095 Uiso 1 1 calc R . . H55C H -0.0622 0.1975 0.2157 0.095 Uiso 1 1 calc R . . C56 C 0.1381(4) 0.2605(3) 0.00634(18) 0.0710(15) Uani 1 1 d . . . H56A H 0.0717 0.2472 -0.0172 0.107 Uiso 1 1 calc R . . H56B H 0.2094 0.2351 -0.0030 0.107 Uiso 1 1 calc R . . H56C H 0.1537 0.3082 0.0019 0.107 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 Ba 0.01909(9) 0.01989(9) 0.01875(10) 0.00087(10) -0.00137(7) 0.00093(8) O1 0.0234(12) 0.0282(12) 0.0217(13) -0.0046(10) -0.0015(10) 0.0011(9) C1 0.0211(17) 0.0356(19) 0.030(2) -0.0088(17) -0.0018(16) 0.0022(14) C2 0.044(2) 0.050(2) 0.030(2) -0.0021(19) -0.0052(19) -0.0067(18) C3 0.051(3) 0.095(4) 0.028(2) -0.004(3) -0.005(2) -0.005(3) C4 0.050(3) 0.104(4) 0.042(3) -0.036(3) -0.010(2) 0.007(3) C5 0.059(3) 0.058(3) 0.067(4) -0.034(3) -0.012(3) 0.012(2) C6 0.052(2) 0.037(2) 0.049(3) -0.014(2) -0.008(2) 0.0047(18) O2 0.0184(10) 0.0307(12) 0.0238(12) 0.0007(11) -0.0034(9) -0.0005(9) C7 0.0143(14) 0.0335(19) 0.0246(18) -0.0040(15) -0.0008(13) 0.0029(13) C8 0.037(2) 0.040(2) 0.031(2) -0.0001(18) -0.0068(18) -0.0063(17) C9 0.042(2) 0.061(3) 0.030(2) 0.004(2) -0.0118(18) -0.001(2) C10 0.029(2) 0.063(3) 0.033(2) -0.016(2) -0.0063(18) -0.0012(18) C11 0.033(2) 0.039(2) 0.047(3) -0.016(2) -0.0046(19) -0.0027(16) C12 0.0298(19) 0.0326(19) 0.030(2) -0.0049(16) -0.0048(17) -0.0002(15) O3 0.0349(13) 0.0207(11) 0.0162(12) 0.0019(10) -0.0002(11) 0.0004(9) C13 0.036(2) 0.0213(16) 0.0165(18) -0.0033(14) 0.0010(16) 0.0014(14) C14 0.039(2) 0.0333(19) 0.0230(19) 0.0013(16) 0.0017(17) 0.0108(16) C15 0.056(3) 0.046(2) 0.023(2) 0.0111(18) -0.005(2) 0.0210(19) C16 0.058(3) 0.047(2) 0.022(2) 0.0076(18) 0.006(2) 0.014(2) C17 0.045(2) 0.045(2) 0.024(2) 0.0000(18) 0.0071(19) 0.0118(18) C18 0.039(2) 0.0313(19) 0.0216(19) -0.0016(16) -0.0011(17) 0.0108(15) O4 0.0270(12) 0.0233(11) 0.0169(12) 0.0000(10) 0.0015(10) -0.0004(9) C19 0.0326(19) 0.0197(15) 0.0184(18) 0.0030(14) 0.0023(16) 0.0009(13) C20 0.041(2) 0.042(2) 0.029(2) 0.0029(18) 0.0010(19) -0.0026(17) C21 0.063(3) 0.046(2) 0.031(2) 0.005(2) -0.015(2) -0.008(2) C22 0.088(3) 0.035(2) 0.019(2) 0.0014(17) -0.002(2) 0.001(2) C23 0.061(3) 0.056(3) 0.033(2) 0.001(2) 0.020(2) 0.013(2) C24 0.040(2) 0.053(2) 0.026(2) 0.0024(19) 0.0035(19) 0.0112(18) B1 0.0228(19) 0.0235(18) 0.026(2) 0.0010(17) 0.0012(17) 0.0030(15) O5 0.0302(13) 0.0212(11) 0.0297(14) 0.0011(10) 0.0074(11) 0.0018(9) C25 0.0190(16) 0.0250(17) 0.0257(19) 0.0070(15) -0.0036(15) -0.0015(13) C26 0.0283(18) 0.0257(17) 0.036(2) 0.0059(16) -0.0040(17) 0.0021(14) C27 0.035(2) 0.034(2) 0.043(2) 0.0176(19) -0.0031(19) -0.0037(16) C28 0.033(2) 0.050(2) 0.029(2) 0.0121(19) 0.0020(18) -0.0018(17) C29 0.0331(18) 0.043(2) 0.0266(18) -0.0072(19) -0.0012(15) 0.0010(17) C30 0.0272(17) 0.0262(18) 0.033(2) 0.0011(15) 0.0017(16) -0.0025(13) O6 0.0236(12) 0.0240(12) 0.0321(14) 0.0068(10) 0.0051(11) 0.0043(9) C31 0.0276(18) 0.0233(16) 0.0246(19) -0.0005(15) -0.0003(15) 0.0042(13) C32 0.0265(19) 0.038(2) 0.043(2) 0.0022(18) -0.0068(18) 0.0042(15) C33 0.042(2) 0.035(2) 0.053(3) 0.009(2) -0.016(2) 0.0106(17) C34 0.055(3) 0.0291(19) 0.036(2) 0.0071(18) -0.012(2) 0.0013(18) C35 0.044(2) 0.0254(18) 0.031(2) 0.0025(16) 0.0057(18) -0.0029(15) C36 0.034(2) 0.0265(18) 0.040(2) 0.0039(17) 0.0017(18) 0.0055(15) B2 0.029(2) 0.0205(18) 0.022(2) 0.0014(16) 0.0013(17) 0.0031(15) O7 0.0219(12) 0.0212(11) 0.0327(14) -0.0004(10) 0.0005(11) 0.0019(9) C37 0.0284(18) 0.0299(17) 0.0176(18) -0.0011(15) 0.0012(15) 0.0063(14) C38 0.0279(19) 0.0332(19) 0.036(2) 0.0023(17) 0.0016(17) 0.0031(15) C39 0.029(2) 0.057(3) 0.036(2) 0.001(2) -0.0014(18) -0.0025(18) C40 0.031(2) 0.080(3) 0.030(2) -0.007(2) -0.0086(19) 0.017(2) C41 0.053(3) 0.051(3) 0.042(3) -0.009(2) -0.020(2) 0.029(2) C42 0.042(2) 0.0333(19) 0.032(2) -0.0053(17) -0.0111(18) 0.0115(16) O8 0.0216(12) 0.0238(11) 0.0294(14) 0.0021(10) -0.0017(10) 0.0004(9) C43 0.0205(17) 0.0263(17) 0.0211(18) -0.0029(15) 0.0057(15) 0.0024(13) C44 0.0270(18) 0.0294(18) 0.029(2) -0.0015(16) -0.0023(16) 0.0057(14) C45 0.0288(19) 0.038(2) 0.041(2) -0.0094(19) -0.0060(18) -0.0024(16) C46 0.035(2) 0.0315(19) 0.041(2) -0.0082(18) 0.0098(19) -0.0067(16) C47 0.036(2) 0.0293(18) 0.027(2) 0.0041(16) 0.0119(17) 0.0006(15) C48 0.0284(18) 0.0331(18) 0.0176(18) 0.0003(15) 0.0031(15) -0.0028(14) O9 0.0387(13) 0.0255(12) 0.0244(14) 0.0023(11) -0.0012(12) -0.0050(10) C49 0.045(2) 0.0289(19) 0.034(2) 0.0050(17) 0.0088(19) -0.0099(16) C50 0.051(2) 0.0260(18) 0.025(2) 0.0073(16) 0.0059(19) -0.0015(16) O10 0.0448(14) 0.0257(12) 0.0215(13) 0.0049(11) -0.0023(12) -0.0005(10) C51 0.088(3) 0.042(2) 0.031(2) -0.006(2) -0.014(2) -0.014(2) C52 0.063(3) 0.031(2) 0.029(2) 0.0031(17) -0.006(2) -0.0011(18) O11 0.0249(12) 0.0447(14) 0.0400(15) 0.0114(14) 0.0054(11) 0.0031(11) C53 0.0245(19) 0.066(3) 0.068(3) -0.014(3) -0.006(2) -0.005(2) C54 0.035(2) 0.092(3) 0.045(3) -0.009(3) -0.014(2) 0.020(2) O12 0.0288(12) 0.0571(16) 0.0372(15) -0.0090(15) -0.0084(11) 0.0109(12) C55 0.049(2) 0.076(3) 0.067(3) 0.028(3) 0.029(2) 0.018(2) C56 0.059(3) 0.115(4) 0.039(3) -0.009(3) -0.010(2) 0.015(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 Ba O3 2.698(2) . ? Ba O2 2.721(2) . ? Ba O4 2.762(2) . ? Ba O9 2.780(2) . ? Ba O1 2.794(2) . ? Ba O10 2.800(2) . ? Ba O11 2.808(2) . ? Ba O12 2.826(2) . ? O1 C1 1.377(4) . ? O1 B1 1.490(4) . ? C1 C2 1.377(5) . ? C1 C6 1.382(5) . ? C2 C3 1.381(5) . ? C3 C4 1.360(6) . ? C4 C5 1.357(7) . ? C5 C6 1.411(6) . ? O2 C7 1.376(4) . ? O2 B1 1.488(4) . ? C7 C8 1.379(5) . ? C7 C12 1.384(4) . ? C8 C9 1.388(5) . ? C9 C10 1.390(5) . ? C10 C11 1.377(5) . ? C11 C12 1.385(5) . ? O3 C13 1.378(4) . ? O3 B2 1.486(4) . ? C13 C14 1.380(4) . ? C13 C18 1.396(4) . ? C14 C15 1.394(5) . ? C15 C16 1.384(5) . ? C16 C17 1.372(5) . ? C17 C18 1.388(5) . ? O4 C19 1.381(4) . ? O4 B2 1.495(4) . ? C19 C24 1.373(5) . ? C19 C20 1.374(5) . ? C20 C21 1.388(5) . ? C21 C22 1.359(6) . ? C22 C23 1.364(6) . ? C23 C24 1.403(5) . ? B1 O5 1.453(4) . ? B1 O6 1.459(4) . ? O5 C25 1.349(4) . ? C25 C26 1.394(4) . ? C25 C30 1.402(4) . ? C26 C27 1.384(5) . ? C27 C28 1.378(5) . ? C28 C29 1.382(5) . ? C29 C30 1.387(5) . ? O6 C31 1.357(4) . ? C31 C32 1.388(4) . ? C31 C36 1.396(4) . ? C32 C33 1.388(5) . ? C33 C34 1.379(5) . ? C34 C35 1.366(5) . ? C35 C36 1.388(5) . ? B2 O8 1.449(4) . ? B2 O7 1.450(4) . ? O7 C37 1.354(4) . ? C37 C42 1.394(4) . ? C37 C38 1.398(4) . ? C38 C39 1.385(5) . ? C39 C40 1.362(5) . ? C40 C41 1.372(6) . ? C41 C42 1.388(5) . ? O8 C43 1.367(3) . ? C43 C44 1.388(4) . ? C43 C48 1.392(4) . ? C44 C45 1.382(5) . ? C45 C46 1.371(5) . ? C46 C47 1.397(5) . ? C47 C48 1.387(4) . ? O9 C49 1.424(4) . ? O9 C51 1.425(4) . ? C49 C50 1.486(5) . ? C50 O10 1.431(4) . ? O10 C52 1.432(4) . ? O11 C55 1.418(4) . ? O11 C53 1.428(5) . ? C53 C54 1.478(6) . ? C54 O12 1.426(4) . ? O12 C56 1.429(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 Ba O2 101.23(6) . . ? O3 Ba O4 49.00(6) . . ? O2 Ba O4 93.93(6) . . ? O3 Ba O9 158.55(7) . . ? O2 Ba O9 95.96(6) . . ? O4 Ba O9 142.67(6) . . ? O3 Ba O1 103.46(6) . . ? O2 Ba O1 48.39(6) . . ? O4 Ba O1 132.18(6) . . ? O9 Ba O1 78.60(6) . . ? O3 Ba O10 133.36(6) . . ? O2 Ba O10 88.47(6) . . ? O4 Ba O10 85.20(6) . . ? O9 Ba O10 59.26(7) . . ? O1 Ba O10 116.17(6) . . ? O3 Ba O11 88.96(6) . . ? O2 Ba O11 163.23(7) . . ? O4 Ba O11 82.67(7) . . ? O9 Ba O11 77.62(7) . . ? O1 Ba O11 142.13(7) . . ? O10 Ba O11 74.90(7) . . ? O3 Ba O12 78.44(7) . . ? O2 Ba O12 135.51(7) . . ? O4 Ba O12 115.80(7) . . ? O9 Ba O12 80.31(7) . . ? O1 Ba O12 87.92(6) . . ? O10 Ba O12 124.35(7) . . ? O11 Ba O12 59.31(7) . . ? C1 O1 B1 121.6(2) . . ? C1 O1 Ba 133.79(18) . . ? B1 O1 Ba 103.50(18) . . ? O1 C1 C2 120.8(3) . . ? O1 C1 C6 120.2(3) . . ? C2 C1 C6 119.0(4) . . ? C1 C2 C3 120.8(4) . . ? C4 C3 C2 120.4(5) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 120.3(4) . . ? C1 C6 C5 119.4(4) . . ? C7 O2 B1 123.0(2) . . ? C7 O2 Ba 128.15(17) . . ? B1 O2 Ba 106.86(18) . . ? O2 C7 C8 119.7(3) . . ? O2 C7 C12 120.6(3) . . ? C8 C7 C12 119.6(3) . . ? C7 C8 C9 120.6(3) . . ? C8 C9 C10 119.7(4) . . ? C11 C10 C9 119.3(4) . . ? C10 C11 C12 120.9(4) . . ? C7 C12 C11 119.8(3) . . ? C13 O3 B2 120.6(2) . . ? C13 O3 Ba 125.16(17) . . ? B2 O3 Ba 105.75(17) . . ? O3 C13 C14 120.3(3) . . ? O3 C13 C18 119.3(3) . . ? C14 C13 C18 120.4(3) . . ? C13 C14 C15 119.6(3) . . ? C16 C15 C14 120.3(3) . . ? C17 C16 C15 119.5(3) . . ? C16 C17 C18 121.3(3) . . ? C17 C18 C13 118.8(3) . . ? C19 O4 B2 118.8(2) . . ? C19 O4 Ba 135.96(17) . . ? B2 O4 Ba 102.61(18) . . ? C24 C19 C20 119.8(3) . . ? C24 C19 O4 119.4(3) . . ? C20 C19 O4 120.7(3) . . ? C19 C20 C21 120.4(4) . . ? C22 C21 C20 120.2(4) . . ? C21 C22 C23 119.8(4) . . ? C22 C23 C24 120.8(4) . . ? C19 C24 C23 119.0(4) . . ? O5 B1 O6 108.7(3) . . ? O5 B1 O2 108.1(3) . . ? O6 B1 O2 113.3(3) . . ? O5 B1 O1 112.9(3) . . ? O6 B1 O1 114.6(3) . . ? O2 B1 O1 98.8(2) . . ? C25 O5 B1 129.7(3) . . ? O5 C25 C26 116.7(3) . . ? O5 C25 C30 125.1(3) . . ? C26 C25 C30 118.1(3) . . ? C27 C26 C25 121.0(3) . . ? C28 C27 C26 120.9(3) . . ? C27 C28 C29 118.5(3) . . ? C28 C29 C30 121.7(3) . . ? C29 C30 C25 119.8(3) . . ? C31 O6 B1 125.0(3) . . ? O6 C31 C32 117.3(3) . . ? O6 C31 C36 124.3(3) . . ? C32 C31 C36 118.4(3) . . ? C33 C32 C31 120.7(3) . . ? C34 C33 C32 120.7(3) . . ? C35 C34 C33 118.7(3) . . ? C34 C35 C36 121.8(3) . . ? C35 C36 C31 119.7(3) . . ? O8 B2 O7 108.5(3) . . ? O8 B2 O3 112.2(3) . . ? O7 B2 O3 114.1(3) . . ? O8 B2 O4 109.0(3) . . ? O7 B2 O4 113.9(3) . . ? O3 B2 O4 98.9(2) . . ? C37 O7 B2 125.6(2) . . ? O7 C37 C42 117.5(3) . . ? O7 C37 C38 124.1(3) . . ? C42 C37 C38 118.4(3) . . ? C39 C38 C37 119.9(3) . . ? C40 C39 C38 121.5(4) . . ? C39 C40 C41 119.0(4) . . ? C40 C41 C42 121.2(4) . . ? C41 C42 C37 120.0(4) . . ? C43 O8 B2 126.6(2) . . ? O8 C43 C44 117.3(3) . . ? O8 C43 C48 123.6(3) . . ? C44 C43 C48 118.9(3) . . ? C45 C44 C43 121.1(3) . . ? C46 C45 C44 119.8(3) . . ? C45 C46 C47 120.1(3) . . ? C48 C47 C46 120.0(3) . . ? C47 C48 C43 120.0(3) . . ? C49 O9 C51 113.7(3) . . ? C49 O9 Ba 118.23(19) . . ? C51 O9 Ba 117.7(2) . . ? O9 C49 C50 110.1(3) . . ? O10 C50 C49 109.7(3) . . ? C50 O10 C52 110.7(3) . . ? C50 O10 Ba 118.41(19) . . ? C52 O10 Ba 123.97(19) . . ? C55 O11 C53 113.2(3) . . ? C55 O11 Ba 126.1(2) . . ? C53 O11 Ba 118.9(2) . . ? O11 C53 C54 110.6(3) . . ? O12 C54 C53 109.5(4) . . ? C54 O12 C56 109.7(3) . . ? C54 O12 Ba 112.2(2) . . ? C56 O12 Ba 123.7(2) . . ? _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.618 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.100 #===END