Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Timo Hatanpaa' 'Jarno Kansikas' 'Markku Leskela' 'Ilpo Mutikainen' 'Mikko Ritala' 'Marko Vehkamaki' _publ_contact_author_name 'Mr Timo Hatanpaa' _publ_contact_author_address ; Department of Chemistry University of Helsinki P.O.Box 55 Helsinki 00014 FINLAND ; _publ_contact_author_email TIMO.HATANPAA@HELSINKI.FI _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and characterisation of cyclopentadienyl complexes of barium: precursors for atomic layer deposition of BaTiO3 ; data_2 _database_code_depnum_ccdc_archive 'CCDC 228233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2,3,4,5-pentamethylcyclopentadienyl)barium(II)dien ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H43 Ba N3' _chemical_formula_sum 'C24 H43 Ba N3' _chemical_formula_weight 510.95 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' N N 0.0061 0.0033 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.346(8) _cell_length_b 20.514(17) _cell_length_c 15.413(10) _cell_angle_alpha 90.00 _cell_angle_beta 130.50(4) _cell_angle_gamma 90.00 _cell_volume 5132(6) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 7.5 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 1.561 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details 'North etal. (1968). Acta Cryst. A24, 351-359' _exptl_special_details ; Bis(1,2,3,4,5-pentamethylcyclopentadienyl)barium(II)dien ; _diffrn_ambient_temperature 193(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 'Rigaku AFC-7S' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 4987 _diffrn_reflns_av_R_equivalents 0.0512 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.50 _reflns_number_total 4845 _reflns_number_gt 4315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7S software (1993)' _computing_cell_refinement 'TEXSAN (1993)' _computing_data_reduction 'TEXSAN (1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC v. 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0531P)^2^+12.9042P] 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 4845 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 Ba1 Ba 0.227077(8) 0.132559(8) 0.745245(12) 0.04695(5) Uani 1 1 d . . . N3 N 0.33784(18) 0.24279(17) 0.8663(3) 0.0883(11) Uani 1 1 d . A . H3A H 0.3083 0.2783 0.8586 0.106 Uiso 1 1 calc R . . H3B H 0.3764 0.2329 0.9427 0.106 Uiso 1 1 calc R . . C24 C 0.3798(2) 0.2593(2) 0.8232(3) 0.1062(17) Uani 1 1 d . . . H24A H 0.4242 0.2911 0.8753 0.127 Uiso 1 1 calc R A . H24B H 0.3402 0.2801 0.7473 0.127 Uiso 1 1 calc R . . C23 C 0.4157(2) 0.2005(3) 0.8137(3) 0.1037(17) Uani 1 1 d . A . H23A H 0.4494 0.2138 0.7934 0.124 Uiso 1 1 calc R . . H23B H 0.4521 0.1777 0.8880 0.124 Uiso 1 1 calc R . . N2 N 0.35030(15) 0.15677(18) 0.7266(2) 0.0775(9) Uani 1 1 d . A . H2A H 0.3231 0.1788 0.6579 0.093 Uiso 1 1 calc R . . C22 C 0.3813(2) 0.0964(3) 0.7145(4) 0.1224(16) Uani 1 1 d . . . H22A H 0.4177 0.1078 0.6979 0.147 Uiso 1 1 calc R A . H22B H 0.4146 0.0722 0.7875 0.147 Uiso 1 1 calc R . . C21 C 0.3143(3) 0.0544(3) 0.6231(4) 0.1500(19) Uani 1 1 d . A . H21A H 0.2818 0.0785 0.5500 0.180 Uiso 1 1 calc R . . H21B H 0.3383 0.0156 0.6161 0.180 Uiso 1 1 calc R . . N1 N 0.2604(2) 0.03342(17) 0.6430(2) 0.1037(12) Uani 1 1 d . A . H1A H 0.2834 -0.0024 0.6902 0.124 Uiso 1 1 calc R . . H1B H 0.2112 0.0205 0.5747 0.124 Uiso 1 1 calc R . . C20 C 0.10839(17) 0.03752(18) 0.8245(4) 0.0966(15) Uani 1 1 d . . . H20A H 0.1059 0.0035 0.8668 0.145 Uiso 1 1 calc R A . H20B H 0.0762 0.0239 0.7449 0.145 Uiso 1 1 calc R . . H20C H 0.0856 0.0781 0.8273 0.145 Uiso 1 1 calc R . . C19 C 0.2226(2) 0.1496(2) 0.9960(3) 0.0990(12) Uani 1 1 d . . . H19A H 0.2148 0.1300 1.0464 0.149 Uiso 1 1 calc R A . H19B H 0.1709 0.1696 0.9304 0.149 Uiso 1 1 calc R . . H19C H 0.2656 0.1830 1.0380 0.149 Uiso 1 1 calc R . . C18 C 0.4022(2) 0.1254(2) 1.0838(3) 0.1017(16) Uani 1 1 d . . . H18A H 0.4275 0.1060 1.1581 0.153 Uiso 1 1 calc R A . H18B H 0.3865 0.1706 1.0822 0.153 Uiso 1 1 calc R . . H18C H 0.4418 0.1248 1.0713 0.153 Uiso 1 1 calc R . . C17 C 0.39792(18) 0.0001(2) 0.9603(3) 0.0954(13) Uani 1 1 d . . . H17A H 0.4281 -0.0254 1.0308 0.143 Uiso 1 1 calc R A . H17B H 0.4341 0.0339 0.9691 0.143 Uiso 1 1 calc R . . H17C H 0.3796 -0.0287 0.8968 0.143 Uiso 1 1 calc R . . C16 C 0.2122(3) -0.05331(17) 0.7927(4) 0.0948(16) Uani 1 1 d . . . H16A H 0.1890 -0.0828 0.8154 0.142 Uiso 1 1 calc R A . H16B H 0.2582 -0.0749 0.8044 0.142 Uiso 1 1 calc R . . H16C H 0.1697 -0.0419 0.7120 0.142 Uiso 1 1 calc R . . C15 C 0.19710(14) 0.04840(13) 0.8777(3) 0.0543(8) Uani 1 1 d . A . C14 C 0.24792(15) 0.09768(15) 0.9550(2) 0.0560(8) Uani 1 1 d . A . C13 C 0.32701(15) 0.08706(17) 0.9913(2) 0.0575(9) Uani 1 1 d . A . C12 C 0.32413(14) 0.03155(16) 0.9359(2) 0.0556(8) Uani 1 1 d . A . C11 C 0.24283(15) 0.00767(14) 0.8641(2) 0.0547(9) Uani 1 1 d . A . C1B C 0.1018(3) 0.1762(3) 0.4926(4) 0.0486(14) Uani 0.553(2) 1 d P A 1 C2B C 0.0594(3) 0.1494(2) 0.5244(4) 0.0472(19) Uani 0.553(2) 1 d P A 1 C3B C 0.0618(2) 0.1981(3) 0.5952(4) 0.0573(16) Uani 0.553(2) 1 d P A 1 C4B C 0.1085(2) 0.2513(2) 0.6186(3) 0.0340(11) Uani 0.553(2) 1 d P A 1 C5B C 0.1304(2) 0.2380(2) 0.5441(3) 0.0362(12) Uani 0.553(2) 1 d P A 1 C6B C 0.1114(5) 0.1497(4) 0.4111(5) 0.095(3) Uani 0.553(2) 1 d P A 1 H6B1 H 0.1434 0.1092 0.4420 0.142 Uiso 0.553(2) 1 calc PR A 1 H6B2 H 0.1400 0.1817 0.4006 0.142 Uiso 0.553(2) 1 calc PR A 1 H6B3 H 0.0569 0.1407 0.3375 0.142 Uiso 0.553(2) 1 calc PR A 1 C7B C 0.0189(4) 0.0824(3) 0.4883(8) 0.111(4) Uani 0.553(2) 1 d P A 1 H7B1 H -0.0194 0.0791 0.4049 0.167 Uiso 0.553(2) 1 calc PR A 1 H7B2 H -0.0114 0.0764 0.5155 0.167 Uiso 0.553(2) 1 calc PR A 1 H7B3 H 0.0613 0.0487 0.5213 0.167 Uiso 0.553(2) 1 calc PR A 1 C8B C 0.0203(3) 0.1897(4) 0.6451(5) 0.098(2) Uani 0.553(2) 1 d P A 1 H8B1 H 0.0623 0.1845 0.7280 0.147 Uiso 0.553(2) 1 calc PR A 1 H8B2 H -0.0150 0.1510 0.6120 0.147 Uiso 0.553(2) 1 calc PR A 1 H8B3 H -0.0133 0.2282 0.6276 0.147 Uiso 0.553(2) 1 calc PR A 1 C9B C 0.1180(4) 0.3121(4) 0.6656(5) 0.079(2) Uani 0.553(2) 1 d P A 1 H9B1 H 0.0820 0.3437 0.6042 0.118 Uiso 0.553(2) 1 calc PR A 1 H9B2 H 0.1755 0.3262 0.7119 0.118 Uiso 0.553(2) 1 calc PR A 1 H9B3 H 0.1031 0.3094 0.7137 0.118 Uiso 0.553(2) 1 calc PR A 1 C10B C 0.1684(3) 0.2881(3) 0.5188(5) 0.0686(17) Uani 0.553(2) 1 d P A 1 H10A H 0.1250 0.3093 0.4458 0.103 Uiso 0.553(2) 1 calc PR A 1 H10B H 0.2074 0.2666 0.5146 0.103 Uiso 0.553(2) 1 calc PR A 1 H10C H 0.1974 0.3209 0.5796 0.103 Uiso 0.553(2) 1 calc PR A 1 C1A C 0.1128(3) 0.2137(4) 0.5320(6) 0.053(2) Uani 0.447(2) 1 d P A 2 C2A C 0.0744(3) 0.1529(4) 0.5021(4) 0.0451(19) Uani 0.447(2) 1 d P A 2 C3A C 0.0441(3) 0.1470(3) 0.5591(4) 0.0390(15) Uani 0.447(2) 1 d P A 2 C4A C 0.0634(3) 0.1976(3) 0.6264(5) 0.0345(15) Uani 0.447(2) 1 d P A 2 C5A C 0.1049(3) 0.2415(3) 0.5967(5) 0.0336(16) Uani 0.447(2) 1 d P A 2 C6A C 0.1499(4) 0.2444(5) 0.4870(7) 0.092(3) Uani 0.447(2) 1 d P A 2 H6A1 H 0.1060 0.2615 0.4102 0.138 Uiso 0.447(2) 1 calc PR A 2 H6A2 H 0.1819 0.2118 0.4837 0.138 Uiso 0.447(2) 1 calc PR A 2 H6A3 H 0.1862 0.2802 0.5374 0.138 Uiso 0.447(2) 1 calc PR A 2 C7A C 0.0604(5) 0.1068(5) 0.4163(6) 0.093(3) Uani 0.447(2) 1 d P A 2 H7A1 H 0.0068 0.1159 0.3414 0.139 Uiso 0.447(2) 1 calc PR A 2 H7A2 H 0.0611 0.0620 0.4388 0.139 Uiso 0.447(2) 1 calc PR A 2 H7A3 H 0.1040 0.1122 0.4122 0.139 Uiso 0.447(2) 1 calc PR A 2 C8A C -0.0099(4) 0.0904(4) 0.5424(6) 0.068(2) Uani 0.447(2) 1 d P A 2 H8A1 H -0.0285 0.0994 0.5850 0.102 Uiso 0.447(2) 1 calc PR A 2 H8A2 H 0.0221 0.0500 0.5704 0.102 Uiso 0.447(2) 1 calc PR A 2 H8A3 H -0.0579 0.0859 0.4611 0.102 Uiso 0.447(2) 1 calc PR A 2 C9A C 0.0392(4) 0.2133(4) 0.6967(5) 0.063(2) Uani 0.447(2) 1 d P A 2 H9A1 H -0.0006 0.1809 0.6816 0.094 Uiso 0.447(2) 1 calc PR A 2 H9A2 H 0.0142 0.2568 0.6763 0.094 Uiso 0.447(2) 1 calc PR A 2 H9A3 H 0.0882 0.2125 0.7779 0.094 Uiso 0.447(2) 1 calc PR A 2 C10A C 0.1358(6) 0.3107(4) 0.6636(11) 0.105(5) Uani 0.447(2) 1 d P A 2 H10D H 0.1783 0.3292 0.6641 0.158 Uiso 0.447(2) 1 calc PR A 2 H10E H 0.1586 0.3040 0.7423 0.158 Uiso 0.447(2) 1 calc PR A 2 H10F H 0.0890 0.3409 0.6250 0.158 Uiso 0.447(2) 1 calc PR A 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 Ba1 0.03485(6) 0.04812(9) 0.04463(6) -0.00274(6) 0.01991(5) 0.00711(6) N3 0.0787(15) 0.086(2) 0.0778(15) -0.0254(15) 0.0411(12) -0.0157(16) C24 0.091(2) 0.117(3) 0.073(2) -0.017(2) 0.0368(17) -0.053(2) C23 0.0491(13) 0.180(5) 0.0738(18) 0.010(2) 0.0361(12) -0.017(2) N2 0.0627(10) 0.117(2) 0.0588(10) 0.0185(13) 0.0422(8) 0.0251(14) C22 0.1220(15) 0.167(4) 0.1342(19) 0.048(2) 0.1080(13) 0.071(2) C21 0.233(3) 0.138(4) 0.121(2) 0.009(2) 0.1335(19) 0.078(3) N1 0.150(2) 0.086(2) 0.0667(13) -0.0031(14) 0.0664(13) 0.0343(19) C20 0.0385(12) 0.069(2) 0.144(3) 0.0442(19) 0.0424(14) 0.0096(14) C19 0.1327(17) 0.076(2) 0.145(2) -0.0232(18) 0.1151(14) -0.0090(19) C18 0.0688(16) 0.154(4) 0.0507(16) -0.0144(19) 0.0246(13) -0.058(2) C17 0.0673(12) 0.143(3) 0.0899(16) 0.0539(18) 0.0572(11) 0.0588(17) C16 0.101(2) 0.0428(18) 0.097(2) -0.0098(16) 0.0448(19) 0.0109(18) C15 0.0384(9) 0.0350(13) 0.0804(14) 0.0038(11) 0.0346(9) 0.0046(10) C14 0.0590(10) 0.0492(16) 0.0720(12) -0.0080(11) 0.0480(8) -0.0081(11) C13 0.0413(10) 0.078(2) 0.0397(10) -0.0054(12) 0.0203(8) -0.0165(12) C12 0.0354(9) 0.0752(19) 0.0465(11) 0.0150(12) 0.0224(8) 0.0174(12) C11 0.0417(11) 0.0421(14) 0.0533(13) 0.0013(11) 0.0187(10) 0.0099(11) C1B 0.0499(19) 0.043(3) 0.0422(18) 0.0018(18) 0.0250(15) 0.013(2) C2B 0.0319(18) 0.037(2) 0.047(2) 0.0025(19) 0.0143(18) -0.0035(18) C3B 0.0357(14) 0.085(3) 0.0644(18) 0.052(2) 0.0383(12) 0.0227(19) C4B 0.0470(13) 0.034(2) 0.0334(13) -0.0070(14) 0.0317(10) 0.0022(16) C5B 0.0292(13) 0.038(2) 0.0407(15) -0.0026(15) 0.0223(12) -0.0070(16) C6B 0.121(4) 0.100(5) 0.041(2) -0.001(3) 0.043(2) 0.040(4) C7B 0.074(4) 0.049(3) 0.117(6) 0.001(4) 0.020(4) -0.023(3) C8B 0.0772(18) 0.127(5) 0.138(3) 0.081(3) 0.0913(17) 0.046(3) C9B 0.079(3) 0.078(4) 0.060(3) -0.004(3) 0.037(2) 0.024(3) C10B 0.0634(19) 0.081(4) 0.079(2) 0.020(2) 0.0542(16) -0.007(3) C1A 0.026(2) 0.070(5) 0.057(3) 0.023(3) 0.0243(18) 0.003(3) C2A 0.043(2) 0.070(5) 0.0347(19) 0.010(2) 0.0306(16) 0.017(3) C3A 0.038(2) 0.039(3) 0.043(2) 0.009(2) 0.0271(16) 0.006(2) C4A 0.039(2) 0.028(2) 0.043(2) 0.0150(18) 0.0287(17) -0.0025(18) C5A 0.038(2) 0.025(3) 0.035(2) -0.0158(19) 0.0229(17) -0.0020(19) C6A 0.046(3) 0.136(7) 0.094(4) 0.067(4) 0.046(2) 0.017(4) C7A 0.071(3) 0.142(8) 0.042(3) 0.005(4) 0.027(3) 0.047(5) C8A 0.055(3) 0.054(4) 0.070(4) -0.003(3) 0.030(3) -0.016(3) C9A 0.065(2) 0.087(5) 0.051(2) 0.006(3) 0.0444(19) 0.020(3) C10A 0.081(5) 0.024(4) 0.161(9) 0.002(4) 0.056(5) -0.008(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 Ba1 N2 2.869(3) . ? Ba1 N3 2.908(4) . ? Ba1 N1 2.930(4) . ? Ba1 C2B 2.948(5) . ? Ba1 C2A 2.996(5) . ? Ba1 C3B 3.001(5) . ? Ba1 C4A 3.004(6) . ? Ba1 C3A 3.004(5) . ? Ba1 C1A 3.018(7) . ? Ba1 C11 3.038(4) . ? Ba1 C15 3.042(4) . ? Ba1 C5A 3.047(6) . ? Ba1 C14 3.048(4) . ? Ba1 C13 3.049(4) . ? Ba1 C12 3.052(3) . ? Ba1 C1B 3.097(5) . ? Ba1 C4B 3.119(5) . ? Ba1 C5B 3.200(5) . ? N3 C24 1.461(7) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? C24 C23 1.487(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C23 N2 1.457(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? N2 C22 1.472(6) . ? N2 H2A 0.9300 . ? C22 C21 1.468(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C21 N1 1.436(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? C20 C15 1.514(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C19 C14 1.508(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C18 C13 1.502(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 C12 1.506(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C16 C11 1.506(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 C14 1.393(4) . ? C15 C11 1.401(5) . ? C14 C13 1.408(4) . ? C13 C12 1.401(5) . ? C12 C11 1.408(4) . ? C1B C2B 1.393(9) . ? C1B C5B 1.407(7) . ? C1B C6B 1.499(10) . ? C2B C3B 1.456(9) . ? C2B C7B 1.525(8) . ? C3B C4B 1.358(7) . ? C3B C8B 1.513(9) . ? C4B C9B 1.390(9) . ? C4B C5B 1.520(8) . ? C5B C10B 1.507(8) . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B H7B1 0.9800 . ? C7B H7B2 0.9800 . ? C7B H7B3 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10A 0.9800 . ? C10B H10B 0.9800 . ? C10B H10C 0.9800 . ? C1A C5A 1.251(12) . ? C1A C2A 1.395(11) . ? C1A C6A 1.490(11) . ? C2A C3A 1.395(10) . ? C2A C7A 1.490(11) . ? C3A C4A 1.330(9) . ? C3A C8A 1.534(10) . ? C4A C9A 1.508(11) . ? C4A C5A 1.528(10) . ? C5A C10A 1.622(11) . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A H7A1 0.9800 . ? C7A H7A2 0.9800 . ? C7A H7A3 0.9800 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? C9A H9A1 0.9800 . ? C9A H9A2 0.9800 . ? C9A H9A3 0.9800 . ? C10A H10D 0.9800 . ? C10A H10E 0.9800 . ? C10A H10F 0.9800 . ? 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 N2 Ba1 N3 60.88(11) . . ? N2 Ba1 N1 60.49(11) . . ? N3 Ba1 N1 120.31(12) . . ? N2 Ba1 C2B 111.64(16) . . ? N3 Ba1 C2B 121.40(12) . . ? N1 Ba1 C2B 89.86(15) . . ? N2 Ba1 C2A 100.01(16) . . ? N3 Ba1 C2A 117.70(18) . . ? N1 Ba1 C2A 82.59(16) . . ? C2B Ba1 C2A 11.70(17) . . ? N2 Ba1 C3B 122.74(13) . . ? N3 Ba1 C3B 101.83(14) . . ? N1 Ba1 C3B 118.13(14) . . ? C2B Ba1 C3B 28.30(17) . . ? C2A Ba1 C3B 36.32(18) . . ? N2 Ba1 C4A 129.85(14) . . ? N3 Ba1 C4A 100.65(14) . . ? N1 Ba1 C4A 124.95(14) . . ? C2B Ba1 C4A 35.40(18) . . ? C2A Ba1 C4A 44.44(19) . . ? C3B Ba1 C4A 8.77(17) . . ? N2 Ba1 C3A 126.55(15) . . ? N3 Ba1 C3A 123.20(14) . . ? N1 Ba1 C3A 100.03(15) . . ? C2B Ba1 C3A 15.19(17) . . ? C2A Ba1 C3A 26.88(18) . . ? C3B Ba1 C3A 21.73(16) . . ? C4A Ba1 C3A 25.58(17) . . ? N2 Ba1 C1A 86.61(16) . . ? N3 Ba1 C1A 90.89(16) . . ? N1 Ba1 C1A 95.96(19) . . ? C2B Ba1 C1A 32.99(17) . . ? C2A Ba1 C1A 26.8(2) . . ? C3B Ba1 C1A 36.82(19) . . ? C4A Ba1 C1A 45.1(2) . . ? C3A Ba1 C1A 43.56(18) . . ? N2 Ba1 C11 117.17(9) . . ? N3 Ba1 C11 122.91(10) . . ? N1 Ba1 C11 76.61(12) . . ? C2B Ba1 C11 111.79(12) . . ? C2A Ba1 C11 118.45(17) . . ? C3B Ba1 C11 117.19(13) . . ? C4A Ba1 C11 111.82(14) . . ? C3A Ba1 C11 103.01(13) . . ? C1A Ba1 C11 144.69(14) . . ? N2 Ba1 C15 140.50(8) . . ? N3 Ba1 C15 116.64(11) . . ? N1 Ba1 C15 101.39(11) . . ? C2B Ba1 C15 102.39(15) . . ? C2A Ba1 C15 112.75(16) . . ? C3B Ba1 C15 96.72(13) . . ? C4A Ba1 C15 89.60(14) . . ? C3A Ba1 C15 89.26(14) . . ? C1A Ba1 C15 132.08(15) . . ? C11 Ba1 C15 26.63(9) . . ? N2 Ba1 C5A 100.98(17) . . ? N3 Ba1 C5A 81.61(14) . . ? N1 Ba1 C5A 119.56(15) . . ? C2B Ba1 C5A 40.66(14) . . ? C2A Ba1 C5A 41.65(19) . . ? C3B Ba1 C5A 24.24(17) . . ? C4A Ba1 C5A 29.25(19) . . ? C3A Ba1 C5A 42.49(16) . . ? C1A Ba1 C5A 23.8(2) . . ? C11 Ba1 C5A 141.03(16) . . ? C15 Ba1 C5A 118.07(17) . . ? N2 Ba1 C14 129.42(8) . . ? N3 Ba1 C14 90.23(10) . . ? N1 Ba1 C14 119.23(10) . . ? C2B Ba1 C14 118.92(16) . . ? C2A Ba1 C14 130.57(15) . . ? C3B Ba1 C14 102.19(14) . . ? C4A Ba1 C14 93.55(15) . . ? C3A Ba1 C14 103.88(15) . . ? C1A Ba1 C14 137.93(18) . . ? C11 Ba1 C14 43.95(9) . . ? C15 Ba1 C14 26.44(8) . . ? C5A Ba1 C14 115.70(17) . . ? N2 Ba1 C13 103.37(9) . . ? N3 Ba1 C13 79.59(10) . . ? N1 Ba1 C13 103.79(10) . . ? C2B Ba1 C13 144.69(15) . . ? C2A Ba1 C13 155.87(16) . . ? C3B Ba1 C13 128.19(14) . . ? C4A Ba1 C13 119.43(15) . . ? C3A Ba1 C13 130.07(15) . . ? C1A Ba1 C13 160.24(19) . . ? C11 Ba1 C13 43.78(8) . . ? C15 Ba1 C13 43.43(8) . . ? C5A Ba1 C13 136.50(16) . . ? C14 Ba1 C13 26.71(8) . . ? N2 Ba1 C12 96.93(9) . . ? N3 Ba1 C12 98.59(11) . . ? N1 Ba1 C12 78.25(11) . . ? C2B Ba1 C12 138.37(12) . . ? C2A Ba1 C12 143.70(17) . . ? C3B Ba1 C12 140.31(13) . . ? C4A Ba1 C12 133.00(14) . . ? C3A Ba1 C12 129.43(14) . . ? C1A Ba1 C12 170.44(15) . . ? C11 Ba1 C12 26.73(7) . . ? C15 Ba1 C12 43.59(8) . . ? C5A Ba1 C12 159.44(17) . . ? C14 Ba1 C12 43.89(9) . . ? C13 Ba1 C12 26.55(9) . . ? N2 Ba1 C1B 85.58(14) . . ? N3 Ba1 C1B 105.08(13) . . ? N1 Ba1 C1B 80.64(13) . . ? C2B Ba1 C1B 26.50(17) . . ? C2A Ba1 C1B 15.71(16) . . ? C3B Ba1 C1B 43.84(17) . . ? C4A Ba1 C1B 52.60(18) . . ? C3A Ba1 C1B 41.00(18) . . ? C1A Ba1 C1B 17.06(17) . . ? C11 Ba1 C1B 132.00(11) . . ? C15 Ba1 C1B 128.46(13) . . ? C5A Ba1 C1B 39.12(16) . . ? C14 Ba1 C1B 144.45(13) . . ? C13 Ba1 C1B 171.05(13) . . ? C12 Ba1 C1B 154.02(11) . . ? N2 Ba1 C4B 103.08(13) . . ? N3 Ba1 C4B 77.62(12) . . ? N1 Ba1 C4B 125.96(12) . . ? C2B Ba1 C4B 45.77(13) . . ? C2A Ba1 C4B 47.70(17) . . ? C3B Ba1 C4B 25.55(14) . . ? C4A Ba1 C4B 28.62(15) . . ? C3A Ba1 C4B 45.73(14) . . ? C1A Ba1 C4B 30.07(19) . . ? C11 Ba1 C4B 139.71(12) . . ? C15 Ba1 C4B 115.10(12) . . ? C5A Ba1 C4B 6.48(16) . . ? C14 Ba1 C4B 110.31(12) . . ? C13 Ba1 C4B 130.18(12) . . ? C12 Ba1 C4B 154.19(12) . . ? C1B Ba1 C4B 45.60(13) . . ? N2 Ba1 C5B 80.91(11) . . ? N3 Ba1 C5B 80.79(11) . . ? N1 Ba1 C5B 100.20(13) . . ? C2B Ba1 C5B 42.83(13) . . ? C2A Ba1 C5B 36.93(18) . . ? C3B Ba1 C5B 41.84(15) . . ? C4A Ba1 C5B 49.20(16) . . ? C3A Ba1 C5B 52.25(15) . . ? C1A Ba1 C5B 10.14(14) . . ? C11 Ba1 C5B 154.61(9) . . ? C15 Ba1 C5B 138.56(10) . . ? C5A Ba1 C5B 22.68(19) . . ? C14 Ba1 C5B 138.11(12) . . ? C13 Ba1 C5B 154.44(11) . . ? C12 Ba1 C5B 177.79(11) . . ? C1B Ba1 C5B 25.75(12) . . ? C4B Ba1 C5B 27.80(14) . . ? C24 N3 Ba1 111.9(2) . . ? C24 N3 H3A 109.2 . . ? Ba1 N3 H3A 109.2 . . ? C24 N3 H3B 109.2 . . ? Ba1 N3 H3B 109.2 . . ? H3A N3 H3B 107.9 . . ? N3 C24 C23 111.4(4) . . ? N3 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? N3 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N2 C23 C24 110.1(3) . . ? N2 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N2 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.2 . . ? C23 N2 C22 113.2(3) . . ? C23 N2 Ba1 114.0(3) . . ? C22 N2 Ba1 112.6(3) . . ? C23 N2 H2A 105.3 . . ? C22 N2 H2A 105.3 . . ? Ba1 N2 H2A 105.3 . . ? C21 C22 N2 112.1(3) . . ? C21 C22 H22A 109.2 . . ? N2 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? N2 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N1 C21 C22 112.8(4) . . ? N1 C21 H21A 109.0 . . ? C22 C21 H21A 109.0 . . ? N1 C21 H21B 109.0 . . ? C22 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C21 N1 Ba1 114.5(3) . . ? C21 N1 H1A 108.6 . . ? Ba1 N1 H1A 108.6 . . ? C21 N1 H1B 108.6 . . ? Ba1 N1 H1B 108.6 . . ? H1A N1 H1B 107.6 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C15 C11 109.2(2) . . ? C14 C15 C20 125.2(3) . . ? C11 C15 C20 125.4(3) . . ? C14 C15 Ba1 77.0(2) . . ? C11 C15 Ba1 76.5(2) . . ? C20 C15 Ba1 117.0(2) . . ? C15 C14 C13 107.1(3) . . ? C15 C14 C19 125.4(3) . . ? C13 C14 C19 127.4(3) . . ? C15 C14 Ba1 76.5(2) . . ? C13 C14 Ba1 76.69(19) . . ? C19 C14 Ba1 115.7(2) . . ? C12 C13 C14 108.5(2) . . ? C12 C13 C18 126.9(3) . . ? C14 C13 C18 124.3(3) . . ? C12 C13 Ba1 76.82(17) . . ? C14 C13 Ba1 76.61(17) . . ? C18 C13 Ba1 118.2(2) . . ? C13 C12 C11 107.8(3) . . ? C13 C12 C17 124.8(3) . . ? C11 C12 C17 127.1(3) . . ? C13 C12 Ba1 76.64(18) . . ? C11 C12 Ba1 76.10(17) . . ? C17 C12 Ba1 118.5(2) . . ? C15 C11 C12 107.3(3) . . ? C15 C11 C16 126.2(3) . . ? C12 C11 C16 126.3(3) . . ? C15 C11 Ba1 76.84(19) . . ? C12 C11 Ba1 77.17(19) . . ? C16 C11 Ba1 115.8(3) . . ? C2B C1B C5B 107.4(5) . . ? C2B C1B C6B 128.7(6) . . ? C5B C1B C6B 123.7(6) . . ? C2B C1B Ba1 70.8(3) . . ? C5B C1B Ba1 81.2(3) . . ? C6B C1B Ba1 118.2(3) . . ? C1B C2B C3B 106.2(5) . . ? C1B C2B C7B 124.9(7) . . ? C3B C2B C7B 128.9(7) . . ? C1B C2B Ba1 82.7(3) . . ? C3B C2B Ba1 77.9(2) . . ? C7B C2B Ba1 106.9(3) . . ? C4B C3B C2B 114.3(5) . . ? C4B C3B C8B 121.9(6) . . ? C2B C3B C8B 123.7(6) . . ? C4B C3B Ba1 82.1(3) . . ? C2B C3B Ba1 73.8(3) . . ? C8B C3B Ba1 109.9(3) . . ? C3B C4B C9B 133.8(7) . . ? C3B C4B C5B 100.9(4) . . ? C9B C4B C5B 122.8(6) . . ? C3B C4B Ba1 72.4(3) . . ? C9B C4B Ba1 126.2(3) . . ? C5B C4B Ba1 79.1(2) . . ? C1B C5B C10B 125.3(5) . . ? C1B C5B C4B 110.7(5) . . ? C10B C5B C4B 123.6(5) . . ? C1B C5B Ba1 73.0(3) . . ? C10B C5B Ba1 126.5(3) . . ? C4B C5B Ba1 73.1(2) . . ? C5A C1A C2A 108.5(7) . . ? C5A C1A C6A 124.3(8) . . ? C2A C1A C6A 126.9(8) . . ? C5A C1A Ba1 79.4(4) . . ? C2A C1A Ba1 75.7(4) . . ? C6A C1A Ba1 116.2(4) . . ? C3A C2A C1A 106.5(7) . . ? C3A C2A C7A 126.5(8) . . ? C1A C2A C7A 126.6(8) . . ? C3A C2A Ba1 76.9(3) . . ? C1A C2A Ba1 77.5(3) . . ? C7A C2A Ba1 116.8(4) . . ? C4A C3A C2A 112.8(6) . . ? C4A C3A C8A 122.7(7) . . ? C2A C3A C8A 124.5(7) . . ? C4A C3A Ba1 77.2(3) . . ? C2A C3A Ba1 76.3(3) . . ? C8A C3A Ba1 117.1(4) . . ? C3A C4A C9A 130.5(6) . . ? C3A C4A C5A 100.0(6) . . ? C9A C4A C5A 128.7(6) . . ? C3A C4A Ba1 77.2(3) . . ? C9A C4A Ba1 117.6(3) . . ? C5A C4A Ba1 76.9(3) . . ? C1A C5A C4A 111.9(6) . . ? C1A C5A C10A 134.3(9) . . ? C4A C5A C10A 113.6(8) . . ? C1A C5A Ba1 76.8(4) . . ? C4A C5A Ba1 73.8(3) . . ? C10A C5A Ba1 111.6(4) . . ? C1A C6A H6A1 109.5 . . ? C1A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C1A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C2A C7A H7A1 109.5 . . ? C2A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C2A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C3A C8A H8A1 109.5 . . ? C3A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C3A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C4A C9A H9A1 109.5 . . ? C4A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C4A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C5A C10A H10D 109.5 . . ? C5A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C5A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.805 _refine_diff_density_min -1.248 _refine_diff_density_rms 0.084 #===end data_4 _database_code_depnum_ccdc_archive 'CCDC 228234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2,3,4,5-pentamethylcyclopentadienyl)barium(II) diglyme ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 Ba O3' _chemical_formula_sum 'C26 H44 Ba O3' _chemical_formula_weight 541.95 _chemical_absolute_configuration unk loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.3244 2.2819 '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 tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' _cell_length_a 15.1070(10) _cell_length_b 15.1070(19) _cell_length_c 24.052(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 5489.2(10) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 22850 _cell_measurement_theta_min 5.019 _cell_measurement_theta_max 27.521 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min .700 _exptl_absorpt_correction_T_max .746 _exptl_absorpt_process_details 'sadabs (sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22801 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 5.02 _diffrn_reflns_theta_max 27.54 _reflns_number_total 6262 _reflns_number_gt 4082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'COLLECT (Nonius, 2002)' _computing_data_reduction 'COLLECT (Nonius, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0243P)^2^+1.2522P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6262 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Ba1 Ba 0.232924(18) 0.236494(19) 0.256138(8) 0.02692(8) Uani 1 1 d . . . O1 O 0.2051(3) 0.3943(3) 0.19819(16) 0.0532(12) Uani 1 1 d . . . O3 O 0.3985(3) 0.2221(3) 0.30730(15) 0.0578(12) Uani 1 1 d . . . O2 O 0.3594(3) 0.3810(3) 0.25764(17) 0.0663(13) Uani 1 1 d . . . C12 C 0.0675(4) 0.1929(5) 0.3230(3) 0.0473(19) Uani 1 1 d . . . C22 C 0.2596(7) 0.4691(5) 0.2061(3) 0.081(3) Uani 1 1 d . . . H22A H 0.2384 0.5031 0.2386 0.097 Uiso 1 1 calc R . . H22B H 0.2558 0.5079 0.1730 0.097 Uiso 1 1 calc R . . C4 C 0.3078(5) 0.0756(6) 0.1978(3) 0.065(2) Uani 1 1 d . . . C15 C 0.1692(4) 0.2686(5) 0.3735(2) 0.0474(16) Uani 1 1 d . . . C5 C 0.2190(5) 0.0635(4) 0.1970(2) 0.0435(18) Uani 1 1 d . . . C13 C 0.0586(4) 0.2810(5) 0.3117(2) 0.0431(17) Uani 1 1 d . . . C1 C 0.1815(4) 0.1228(4) 0.1600(3) 0.0412(15) Uani 1 1 d . . . C8 C 0.4247(7) 0.1731(10) 0.1483(5) 0.211(9) Uani 1 1 d . . . H8A H 0.4583 0.1803 0.1829 0.317 Uiso 1 1 calc R . . H8B H 0.4224 0.2298 0.1285 0.317 Uiso 1 1 calc R . . H8C H 0.4539 0.1288 0.1248 0.317 Uiso 1 1 calc R . . C11 C 0.1386(5) 0.1813(5) 0.3623(3) 0.055(2) Uani 1 1 d . . . C2 C 0.2508(7) 0.1734(4) 0.13760(19) 0.070(2) Uani 1 1 d . . . C26 C 0.4162(6) 0.1512(7) 0.3453(3) 0.094(3) Uani 1 1 d . . . H26A H 0.4796 0.1377 0.3450 0.140 Uiso 1 1 calc R . . H26B H 0.3827 0.0986 0.3339 0.140 Uiso 1 1 calc R . . H26C H 0.3982 0.1688 0.3828 0.140 Uiso 1 1 calc R . . C7 C 0.2452(10) 0.2426(5) 0.0918(3) 0.195(6) Uani 1 1 d . . . H7A H 0.2753 0.2206 0.0584 0.293 Uiso 1 1 calc R . . H7B H 0.2737 0.2974 0.1043 0.293 Uiso 1 1 calc R . . H7C H 0.1829 0.2544 0.0831 0.293 Uiso 1 1 calc R . . C14 C 0.1197(4) 0.3270(4) 0.3427(2) 0.0370(15) Uani 1 1 d . . . C19 C 0.1295(7) 0.4269(5) 0.3442(4) 0.093(3) Uani 1 1 d . . . H19A H 0.1803 0.4427 0.3676 0.139 Uiso 1 1 calc R . . H19B H 0.0756 0.4533 0.3597 0.139 Uiso 1 1 calc R . . H19C H 0.1390 0.4492 0.3064 0.139 Uiso 1 1 calc R . . C21 C 0.1211(6) 0.4123(6) 0.1731(3) 0.092(3) Uani 1 1 d . . . H21A H 0.0884 0.4548 0.1960 0.139 Uiso 1 1 calc R . . H21B H 0.0871 0.3572 0.1701 0.139 Uiso 1 1 calc R . . H21C H 0.1302 0.4372 0.1359 0.139 Uiso 1 1 calc R . . C20 C 0.2388(5) 0.2950(7) 0.4164(3) 0.123(4) Uani 1 1 d . . . H20A H 0.2800 0.3376 0.3998 0.185 Uiso 1 1 calc R . . H20B H 0.2715 0.2423 0.4284 0.185 Uiso 1 1 calc R . . H20C H 0.2097 0.3221 0.4486 0.185 Uiso 1 1 calc R . . C23 C 0.3495(6) 0.4432(5) 0.2147(3) 0.077(2) Uani 1 1 d . . . H23A H 0.3732 0.4178 0.1798 0.092 Uiso 1 1 calc R . . H23B H 0.3850 0.4964 0.2237 0.092 Uiso 1 1 calc R . . C3 C 0.3303(5) 0.1424(7) 0.1619(3) 0.074(3) Uani 1 1 d . . . C10 C 0.1706(7) -0.0092(5) 0.2267(3) 0.113(4) Uani 1 1 d . . . H10A H 0.2134 -0.0497 0.2437 0.169 Uiso 1 1 calc R . . H10B H 0.1338 -0.0417 0.2001 0.169 Uiso 1 1 calc R . . H10C H 0.1329 0.0164 0.2557 0.169 Uiso 1 1 calc R . . C18 C -0.0131(5) 0.3187(7) 0.2759(3) 0.111(4) Uani 1 1 d . . . H18A H -0.0140 0.2877 0.2401 0.167 Uiso 1 1 calc R . . H18B H -0.0019 0.3818 0.2697 0.167 Uiso 1 1 calc R . . H18C H -0.0704 0.3113 0.2945 0.167 Uiso 1 1 calc R . . C9 C 0.3728(8) 0.0178(8) 0.2299(4) 0.167(6) Uani 1 1 d . . . H9A H 0.3443 -0.0043 0.2638 0.251 Uiso 1 1 calc R . . H9B H 0.4250 0.0528 0.2399 0.251 Uiso 1 1 calc R . . H9C H 0.3908 -0.0324 0.2067 0.251 Uiso 1 1 calc R . . C17 C 0.0037(6) 0.1210(6) 0.3033(4) 0.138(5) Uani 1 1 d . . . H17A H -0.0530 0.1272 0.3227 0.207 Uiso 1 1 calc R . . H17B H 0.0289 0.0626 0.3113 0.207 Uiso 1 1 calc R . . H17C H -0.0059 0.1269 0.2631 0.207 Uiso 1 1 calc R . . C25 C 0.4511(6) 0.2952(6) 0.3172(4) 0.090(3) Uani 1 1 d . . . H25A H 0.5131 0.2760 0.3228 0.108 Uiso 1 1 calc R . . H25B H 0.4311 0.3253 0.3515 0.108 Uiso 1 1 calc R . . C24 C 0.4468(6) 0.3557(6) 0.2714(3) 0.097(3) Uani 1 1 d . . . H24A H 0.4814 0.4093 0.2808 0.116 Uiso 1 1 calc R . . H24B H 0.4747 0.3278 0.2385 0.116 Uiso 1 1 calc R . . C16 C 0.1650(7) 0.0943(6) 0.3873(4) 0.166(6) Uani 1 1 d . . . H16A H 0.2118 0.1039 0.4148 0.249 Uiso 1 1 calc R . . H16B H 0.1868 0.0549 0.3580 0.249 Uiso 1 1 calc R . . H16C H 0.1136 0.0672 0.4055 0.249 Uiso 1 1 calc R . . C6 C 0.0851(5) 0.1290(7) 0.1432(4) 0.135(4) Uani 1 1 d . . . H6A H 0.0596 0.1837 0.1581 0.202 Uiso 1 1 calc R . . H6B H 0.0527 0.0780 0.1581 0.202 Uiso 1 1 calc R . . H6C H 0.0806 0.1292 0.1026 0.202 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 Ba1 0.02558(16) 0.02919(18) 0.02600(14) 0.00076(15) 0.00130(15) -0.00650(10) O1 0.065(4) 0.042(3) 0.053(3) 0.011(2) -0.001(2) 0.001(2) O3 0.055(3) 0.067(4) 0.051(2) 0.009(2) -0.023(2) -0.008(3) O2 0.059(3) 0.068(3) 0.072(3) 0.014(3) -0.001(3) -0.038(2) C12 0.044(4) 0.045(5) 0.053(4) -0.021(3) 0.032(3) -0.025(3) C22 0.127(9) 0.047(5) 0.070(5) 0.027(3) 0.006(6) -0.006(6) C4 0.037(5) 0.096(7) 0.061(5) -0.037(4) -0.009(4) 0.034(4) C15 0.033(3) 0.079(5) 0.030(3) -0.008(3) 0.003(2) 0.003(4) C5 0.080(6) 0.018(3) 0.033(3) -0.002(2) 0.016(3) 0.007(3) C13 0.034(4) 0.061(6) 0.034(3) 0.002(3) 0.008(3) 0.008(3) C1 0.030(4) 0.036(4) 0.057(4) -0.019(3) -0.010(3) 0.000(3) C8 0.110(9) 0.303(19) 0.222(12) -0.177(13) 0.130(9) -0.142(11) C11 0.070(5) 0.044(5) 0.050(4) 0.027(3) 0.037(4) 0.039(4) C2 0.153(8) 0.037(4) 0.019(3) -0.004(2) 0.014(4) -0.022(5) C26 0.107(8) 0.086(7) 0.088(6) 0.001(6) -0.040(6) 0.039(6) C7 0.49(2) 0.059(5) 0.038(4) 0.012(4) 0.025(7) -0.041(11) C14 0.042(4) 0.022(3) 0.047(4) -0.010(3) 0.017(3) -0.008(3) C19 0.122(8) 0.035(5) 0.122(7) -0.026(5) 0.073(6) -0.018(5) C21 0.081(7) 0.111(9) 0.085(6) 0.050(5) -0.006(5) 0.013(6) C20 0.067(5) 0.257(11) 0.046(4) -0.032(5) -0.013(4) 0.011(7) C23 0.085(7) 0.069(6) 0.076(6) 0.029(4) 0.007(5) -0.035(5) C3 0.048(5) 0.107(8) 0.067(6) -0.051(5) 0.038(4) -0.039(5) C10 0.219(11) 0.033(4) 0.087(6) 0.006(4) 0.073(6) -0.007(6) C18 0.045(5) 0.238(11) 0.051(5) 0.020(5) -0.005(4) 0.041(6) C9 0.196(12) 0.185(11) 0.120(8) -0.085(7) -0.075(8) 0.152(10) C17 0.120(8) 0.143(9) 0.150(8) -0.104(7) 0.093(7) -0.105(7) C25 0.072(6) 0.095(8) 0.103(7) 0.018(5) -0.040(5) -0.035(5) C24 0.063(6) 0.121(8) 0.106(7) 0.008(5) -0.004(5) -0.062(5) C16 0.191(12) 0.125(9) 0.183(9) 0.115(7) 0.128(9) 0.114(8) C6 0.070(7) 0.177(10) 0.157(9) -0.096(7) -0.062(6) 0.040(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O1 2.794(4) . ? Ba1 O3 2.796(4) . ? Ba1 O2 2.901(3) . ? Ba1 C5 2.982(6) . ? Ba1 C1 2.983(5) . ? Ba1 C2 3.018(5) . ? Ba1 C14 3.021(5) . ? Ba1 C15 3.022(5) . ? Ba1 C4 3.025(7) . ? Ba1 C13 3.029(6) . ? Ba1 C11 3.042(6) . ? Ba1 C12 3.044(6) . ? Ba1 C3 3.053(6) . ? O1 C22 1.409(8) . ? O1 C21 1.432(9) . ? O3 C25 1.381(8) . ? O3 C26 1.433(8) . ? O2 C23 1.405(7) . ? O2 C24 1.414(9) . ? C12 C13 1.365(9) . ? C12 C11 1.443(9) . ? C12 C17 1.528(8) . ? C22 C23 1.429(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C4 C5 1.353(9) . ? C4 C3 1.370(11) . ? C4 C9 1.525(10) . ? C15 C14 1.375(8) . ? C15 C11 1.424(9) . ? C15 C20 1.526(8) . ? C5 C1 1.383(8) . ? C5 C10 1.501(9) . ? C13 C14 1.375(8) . ? C13 C18 1.497(9) . ? C1 C2 1.404(9) . ? C1 C6 1.515(9) . ? C8 C3 1.536(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C16 1.499(9) . ? C2 C3 1.415(10) . ? C2 C7 1.521(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C14 C19 1.516(9) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C25 C24 1.432(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 O1 Ba1 O3 114.85(13) . . ? O1 Ba1 O2 57.52(14) . . ? O3 Ba1 O2 57.57(14) . . ? O1 Ba1 C5 119.96(13) . . ? O3 Ba1 C5 101.82(17) . . ? O2 Ba1 C5 135.35(17) . . ? O1 Ba1 C1 93.77(16) . . ? O3 Ba1 C1 121.95(15) . . ? O2 Ba1 C1 127.90(15) . . ? C5 Ba1 C1 26.82(15) . . ? O1 Ba1 C2 79.14(14) . . ? O3 Ba1 C2 108.1(2) . . ? O2 Ba1 C2 100.96(18) . . ? C5 Ba1 C2 43.89(15) . . ? C1 Ba1 C2 27.06(18) . . ? O1 Ba1 C14 82.66(14) . . ? O3 Ba1 C14 103.78(15) . . ? O2 Ba1 C14 91.35(15) . . ? C5 Ba1 C14 133.27(17) . . ? C1 Ba1 C14 130.34(17) . . ? C2 Ba1 C14 147.6(2) . . ? O1 Ba1 C15 106.34(17) . . ? O3 Ba1 C15 83.45(14) . . ? O2 Ba1 C15 94.44(16) . . ? C5 Ba1 C15 124.31(19) . . ? C1 Ba1 C15 137.19(18) . . ? C2 Ba1 C15 164.1(2) . . ? C14 Ba1 C15 26.30(15) . . ? O1 Ba1 C4 120.7(2) . . ? O3 Ba1 C4 78.89(17) . . ? O2 Ba1 C4 111.3(2) . . ? C5 Ba1 C4 26.02(18) . . ? C1 Ba1 C4 43.56(18) . . ? C2 Ba1 C4 43.5(2) . . ? C14 Ba1 C4 153.5(2) . . ? C15 Ba1 C4 132.9(2) . . ? O1 Ba1 C13 84.27(16) . . ? O3 Ba1 C13 126.91(15) . . ? O2 Ba1 C13 113.58(17) . . ? C5 Ba1 C13 110.1(2) . . ? C1 Ba1 C13 104.11(17) . . ? C2 Ba1 C13 124.4(2) . . ? C14 Ba1 C13 26.26(15) . . ? C15 Ba1 C13 43.54(15) . . ? C4 Ba1 C13 135.1(2) . . ? O1 Ba1 C11 125.63(14) . . ? O3 Ba1 C11 91.62(17) . . ? O2 Ba1 C11 120.30(19) . . ? C5 Ba1 C11 97.31(19) . . ? C1 Ba1 C11 111.8(2) . . ? C2 Ba1 C11 138.5(2) . . ? C14 Ba1 C11 43.98(16) . . ? C15 Ba1 C11 27.16(17) . . ? C4 Ba1 C11 110.1(2) . . ? C13 Ba1 C11 44.17(16) . . ? O1 Ba1 C12 108.95(19) . . ? O3 Ba1 C12 119.03(17) . . ? O2 Ba1 C12 134.20(15) . . ? C5 Ba1 C12 90.25(18) . . ? C1 Ba1 C12 94.07(17) . . ? C2 Ba1 C12 120.3(2) . . ? C14 Ba1 C12 43.06(16) . . ? C15 Ba1 C12 43.94(17) . . ? C4 Ba1 C12 112.2(2) . . ? C13 Ba1 C12 25.98(16) . . ? C11 Ba1 C12 27.43(18) . . ? O1 Ba1 C3 95.7(2) . . ? O3 Ba1 C3 81.9(2) . . ? O2 Ba1 C3 92.44(18) . . ? C5 Ba1 C3 43.3(2) . . ? C1 Ba1 C3 44.09(19) . . ? C2 Ba1 C3 26.9(2) . . ? C14 Ba1 C3 174.2(2) . . ? C15 Ba1 C3 157.2(3) . . ? C4 Ba1 C3 26.1(2) . . ? C13 Ba1 C3 148.20(19) . . ? C11 Ba1 C3 136.2(2) . . ? C12 Ba1 C3 133.4(2) . . ? C22 O1 C21 115.0(6) . . ? C22 O1 Ba1 121.9(4) . . ? C21 O1 Ba1 120.4(4) . . ? C25 O3 C26 112.4(6) . . ? C25 O3 Ba1 121.9(4) . . ? C26 O3 Ba1 120.4(5) . . ? C23 O2 C24 116.9(6) . . ? C23 O2 Ba1 115.1(4) . . ? C24 O2 Ba1 114.5(4) . . ? C13 C12 C11 108.7(6) . . ? C13 C12 C17 124.8(8) . . ? C11 C12 C17 125.9(8) . . ? C13 C12 Ba1 76.4(4) . . ? C11 C12 Ba1 76.2(3) . . ? C17 C12 Ba1 120.5(4) . . ? O1 C22 C23 110.8(7) . . ? O1 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C5 C4 C3 109.6(7) . . ? C5 C4 C9 124.6(10) . . ? C3 C4 C9 125.6(10) . . ? C5 C4 Ba1 75.2(4) . . ? C3 C4 Ba1 78.1(4) . . ? C9 C4 Ba1 117.8(4) . . ? C14 C15 C11 108.4(5) . . ? C14 C15 C20 124.9(7) . . ? C11 C15 C20 126.5(7) . . ? C14 C15 Ba1 76.8(3) . . ? C11 C15 Ba1 77.2(3) . . ? C20 C15 Ba1 117.0(4) . . ? C4 C5 C1 109.1(7) . . ? C4 C5 C10 125.1(8) . . ? C1 C5 C10 125.4(8) . . ? C4 C5 Ba1 78.8(4) . . ? C1 C5 Ba1 76.6(3) . . ? C10 C5 Ba1 116.7(4) . . ? C12 C13 C14 108.7(6) . . ? C12 C13 C18 123.8(7) . . ? C14 C13 C18 127.2(7) . . ? C12 C13 Ba1 77.6(4) . . ? C14 C13 Ba1 76.5(3) . . ? C18 C13 Ba1 117.4(4) . . ? C5 C1 C2 107.1(6) . . ? C5 C1 C6 127.3(7) . . ? C2 C1 C6 125.5(8) . . ? C5 C1 Ba1 76.5(3) . . ? C2 C1 Ba1 77.8(3) . . ? C6 C1 Ba1 114.9(4) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C11 C12 104.7(5) . . ? C15 C11 C16 130.5(8) . . ? C12 C11 C16 124.6(9) . . ? C15 C11 Ba1 75.7(3) . . ? C12 C11 Ba1 76.4(3) . . ? C16 C11 Ba1 116.9(4) . . ? C1 C2 C3 107.0(5) . . ? C1 C2 C7 127.6(9) . . ? C3 C2 C7 125.1(10) . . ? C1 C2 Ba1 75.1(3) . . ? C3 C2 Ba1 77.9(3) . . ? C7 C2 Ba1 117.6(4) . . ? O3 C26 H26A 109.5 . . ? O3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C14 C15 109.4(6) . . ? C13 C14 C19 125.6(7) . . ? C15 C14 C19 124.9(7) . . ? C13 C14 Ba1 77.2(3) . . ? C15 C14 Ba1 76.9(3) . . ? C19 C14 Ba1 114.3(4) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C23 C22 113.0(6) . . ? O2 C23 H23A 109.0 . . ? C22 C23 H23A 109.0 . . ? O2 C23 H23B 109.0 . . ? C22 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C4 C3 C2 107.1(6) . . ? C4 C3 C8 125.9(11) . . ? C2 C3 C8 126.8(11) . . ? C4 C3 Ba1 75.8(4) . . ? C2 C3 Ba1 75.1(4) . . ? C8 C3 Ba1 117.7(5) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O3 C25 C24 110.6(6) . . ? O3 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? O2 C24 C25 113.3(6) . . ? O2 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? O2 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.662 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.087 #===end data_5 _database_code_depnum_ccdc_archive 'CCDC 228235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,2,3,4,5-pentamethylcyclopentadienyl)barium(II)triglyme ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H48 Ba O4' _chemical_formula_sum 'C28 H48 Ba O4' _chemical_formula_weight 586.00 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.620(5) _cell_length_b 21.738(5) _cell_length_c 16.243(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 5868(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 7.0 _exptl_crystal_description colorless _exptl_crystal_colour prismatic _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.500 _exptl_absorpt_process_details 'North etal. (1968). Acta Cryst. A24, 351-359' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 5187 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.48 _reflns_number_total 5187 _reflns_number_gt 4142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7S software (1993)' _computing_cell_refinement 'TEXSAN (1993)' _computing_data_reduction 'TEXSAN (1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC v. 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1284P)^2^+6.7236P] 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 5187 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ba1 Ba 0.295823(19) 0.141313(14) 0.495224(18) 0.03226(14) Uani 1 1 d . . . C1 C 0.2408(5) 0.0945(3) 0.3301(4) 0.061(2) Uani 1 1 d . . . C2 C 0.2763(4) 0.0427(4) 0.3682(5) 0.059(2) Uani 1 1 d . . . C3 C 0.2247(6) 0.0241(3) 0.4297(5) 0.067(2) Uani 1 1 d . . . C4 C 0.1604(4) 0.0627(4) 0.4304(5) 0.067(2) Uani 1 1 d . . . C5 C 0.1693(5) 0.1056(3) 0.3708(5) 0.063(2) Uani 1 1 d . . . C6 C 0.2731(10) 0.1278(6) 0.2559(6) 0.142(6) Uani 1 1 d . . . H6A H 0.2303 0.1325 0.2150 0.213 Uiso 1 1 calc R . . H6B H 0.3175 0.1040 0.2320 0.213 Uiso 1 1 calc R . . H6C H 0.2927 0.1684 0.2724 0.213 Uiso 1 1 calc R . . C7 C 0.3556(6) 0.0124(6) 0.3487(8) 0.137(5) Uani 1 1 d . . . H7A H 0.3510 -0.0321 0.3571 0.206 Uiso 1 1 calc R . . H7B H 0.3974 0.0289 0.3852 0.206 Uiso 1 1 calc R . . H7C H 0.3701 0.0207 0.2913 0.206 Uiso 1 1 calc R . . C8 C 0.2326(11) -0.0337(5) 0.4821(7) 0.149(6) Uani 1 1 d . . . H8A H 0.2069 -0.0683 0.4538 0.223 Uiso 1 1 calc R . . H8B H 0.2063 -0.0270 0.5353 0.223 Uiso 1 1 calc R . . H8C H 0.2897 -0.0429 0.4908 0.223 Uiso 1 1 calc R . . C9 C 0.0860(8) 0.0579(8) 0.4878(7) 0.145(6) Uani 1 1 d . . . H9A H 0.0375 0.0519 0.4545 0.218 Uiso 1 1 calc R . . H9B H 0.0808 0.0959 0.5198 0.218 Uiso 1 1 calc R . . H9C H 0.0928 0.0230 0.5252 0.218 Uiso 1 1 calc R . . C10 C 0.1091(7) 0.1551(6) 0.3453(8) 0.154(6) Uani 1 1 d . . . H10A H 0.0564 0.1362 0.3357 0.231 Uiso 1 1 calc R . . H10B H 0.1277 0.1751 0.2947 0.231 Uiso 1 1 calc R . . H10C H 0.1046 0.1858 0.3893 0.231 Uiso 1 1 calc R . . C11 C 0.4522(4) 0.1829(3) 0.4220(4) 0.0552(19) Uani 1 1 d . . . C12 C 0.4729(4) 0.1584(3) 0.4979(4) 0.0494(18) Uani 1 1 d . . . C13 C 0.4478(4) 0.1992(3) 0.5602(4) 0.0425(14) Uani 1 1 d . . . C14 C 0.4116(4) 0.2497(3) 0.5200(4) 0.0434(14) Uani 1 1 d . . . C15 C 0.4141(4) 0.2400(3) 0.4371(4) 0.0521(17) Uani 1 1 d . . . C16 C 0.4784(5) 0.1595(5) 0.3388(6) 0.095(3) Uani 1 1 d . . . H16A H 0.5265 0.1819 0.3209 0.142 Uiso 1 1 calc R . . H16B H 0.4350 0.1660 0.2988 0.142 Uiso 1 1 calc R . . H16C H 0.4906 0.1155 0.3425 0.142 Uiso 1 1 calc R . . C17 C 0.5184(5) 0.0986(4) 0.5106(6) 0.081(3) Uani 1 1 d . . . H17A H 0.5712 0.1014 0.4840 0.121 Uiso 1 1 calc R . . H17B H 0.4878 0.0646 0.4862 0.121 Uiso 1 1 calc R . . H17C H 0.5255 0.0912 0.5696 0.121 Uiso 1 1 calc R . . C18 C 0.4582(5) 0.1923(4) 0.6514(5) 0.069(2) Uani 1 1 d . . . H18A H 0.4902 0.2267 0.6726 0.104 Uiso 1 1 calc R . . H18B H 0.4859 0.1535 0.6632 0.104 Uiso 1 1 calc R . . H18C H 0.4053 0.1923 0.6781 0.104 Uiso 1 1 calc R . . C19 C 0.3792(5) 0.3060(3) 0.5634(6) 0.076(3) Uani 1 1 d . . . H19A H 0.4239 0.3289 0.5881 0.114 Uiso 1 1 calc R . . H19B H 0.3417 0.2932 0.6067 0.114 Uiso 1 1 calc R . . H19C H 0.3511 0.3322 0.5237 0.114 Uiso 1 1 calc R . . C20 C 0.3899(6) 0.2853(4) 0.3698(5) 0.086(3) Uani 1 1 d . . . H20A H 0.4373 0.3087 0.3522 0.128 Uiso 1 1 calc R . . H20B H 0.3491 0.3136 0.3912 0.128 Uiso 1 1 calc R . . H20C H 0.3679 0.2627 0.3227 0.128 Uiso 1 1 calc R . . C21 C 0.1793(6) 0.2860(4) 0.4435(7) 0.097(3) Uani 1 1 d . . . H21A H 0.1856 0.3270 0.4678 0.145 Uiso 1 1 calc R . . H21B H 0.1251 0.2821 0.4204 0.145 Uiso 1 1 calc R . . H21C H 0.2192 0.2803 0.3998 0.145 Uiso 1 1 calc R . . O1 O 0.1908(3) 0.2402(3) 0.5059(3) 0.0695(18) Uani 1 1 d . . . C22 C 0.1290(5) 0.2404(5) 0.5635(7) 0.101(4) Uani 1 1 d . . . H22A H 0.0835 0.2155 0.5424 0.121 Uiso 1 1 calc R . . H22B H 0.1097 0.2830 0.5715 0.121 Uiso 1 1 calc R . . C23 C 0.1556(7) 0.2153(4) 0.6424(7) 0.095(3) Uani 1 1 d . . . H23A H 0.1936 0.2445 0.6684 0.114 Uiso 1 1 calc R . . H23B H 0.1086 0.2109 0.6793 0.114 Uiso 1 1 calc R . . O2 O 0.1931(3) 0.1582(3) 0.6337(3) 0.0595(13) Uani 1 1 d . . . C24 C 0.2174(6) 0.1306(5) 0.7092(5) 0.085(3) Uani 1 1 d . . . H24A H 0.1713 0.1296 0.7478 0.102 Uiso 1 1 calc R . . H24B H 0.2608 0.1553 0.7345 0.102 Uiso 1 1 calc R . . C25 C 0.2460(5) 0.0683(5) 0.6949(6) 0.089(3) Uani 1 1 d . . . H25A H 0.2596 0.0488 0.7482 0.107 Uiso 1 1 calc R . . H25B H 0.2028 0.0438 0.6687 0.107 Uiso 1 1 calc R . . O3 O 0.3140(3) 0.0685(2) 0.6439(3) 0.0561(13) Uani 1 1 d . . . C26 C 0.3601(5) 0.0125(4) 0.6499(5) 0.067(2) Uani 1 1 d . . . H26A H 0.4005 0.0120 0.6052 0.080 Uiso 1 1 calc R . . H26B H 0.3236 -0.0229 0.6411 0.080 Uiso 1 1 calc R . . C27 C 0.4024(5) 0.0040(3) 0.7300(4) 0.061(2) Uani 1 1 d . . . H27A H 0.3631 0.0047 0.7757 0.073 Uiso 1 1 calc R . . H27B H 0.4304 -0.0362 0.7307 0.073 Uiso 1 1 calc R . . O4 O 0.4587(3) 0.0522(3) 0.7398(4) 0.0776(17) Uani 1 1 d . . . C28 C 0.4942(6) 0.0511(5) 0.8183(6) 0.095(3) Uani 1 1 d . . . H28A H 0.5311 0.0860 0.8238 0.143 Uiso 1 1 calc R . . H28B H 0.5241 0.0126 0.8253 0.143 Uiso 1 1 calc R . . H28C H 0.4522 0.0539 0.8604 0.143 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 Ba1 0.0227(2) 0.0285(2) 0.0456(2) 0.00051(13) 0.00208(12) 0.00055(12) C1 0.084(6) 0.052(4) 0.048(4) -0.002(3) -0.009(4) -0.031(4) C2 0.027(3) 0.068(5) 0.083(5) -0.043(4) -0.013(3) 0.009(3) C3 0.094(6) 0.032(3) 0.074(5) 0.007(3) -0.035(4) -0.029(4) C4 0.038(4) 0.090(6) 0.074(5) -0.025(4) -0.004(3) -0.026(4) C5 0.059(5) 0.049(4) 0.080(5) -0.020(4) -0.034(4) 0.022(4) C6 0.220(15) 0.144(10) 0.063(6) 0.008(6) -0.021(7) -0.119(10) C7 0.069(6) 0.150(10) 0.192(11) -0.121(9) -0.053(7) 0.038(7) C8 0.253(17) 0.055(6) 0.137(9) 0.030(6) -0.104(10) -0.075(8) C9 0.090(8) 0.208(15) 0.139(10) -0.079(9) 0.040(7) -0.091(10) C10 0.147(10) 0.123(9) 0.192(12) -0.073(8) -0.127(9) 0.084(8) C11 0.033(3) 0.067(5) 0.066(4) -0.023(4) 0.017(3) -0.019(3) C12 0.024(3) 0.032(3) 0.093(5) -0.004(3) 0.001(3) -0.004(3) C13 0.033(3) 0.043(4) 0.051(3) 0.004(3) 0.002(3) -0.012(3) C14 0.031(3) 0.033(3) 0.065(4) -0.006(3) 0.004(3) -0.003(3) C15 0.039(4) 0.053(4) 0.064(4) 0.012(3) 0.003(3) -0.011(3) C16 0.065(6) 0.120(8) 0.098(6) -0.059(6) 0.031(5) -0.051(6) C17 0.038(4) 0.044(4) 0.160(10) -0.006(5) -0.001(5) 0.006(4) C18 0.072(6) 0.074(6) 0.062(4) 0.005(4) -0.005(4) -0.024(4) C19 0.066(5) 0.041(4) 0.120(7) -0.023(4) 0.002(5) -0.007(4) C20 0.086(7) 0.093(7) 0.078(5) 0.043(5) -0.011(5) -0.021(5) C21 0.067(6) 0.074(6) 0.150(10) 0.039(6) 0.016(6) 0.023(5) O1 0.040(3) 0.048(3) 0.120(5) 0.007(3) 0.015(3) 0.017(2) C22 0.061(5) 0.102(8) 0.139(9) 0.025(7) 0.045(6) 0.052(5) C23 0.105(8) 0.059(5) 0.121(8) -0.016(5) 0.049(7) 0.022(5) O2 0.052(3) 0.062(3) 0.065(3) -0.008(2) 0.015(2) 0.013(2) C24 0.078(6) 0.122(8) 0.056(5) -0.016(5) 0.016(4) 0.011(6) C25 0.058(5) 0.117(8) 0.094(6) 0.052(6) 0.030(5) 0.024(6) O3 0.041(2) 0.069(3) 0.058(3) 0.020(2) 0.009(2) 0.003(2) C26 0.063(5) 0.056(5) 0.080(5) 0.007(4) 0.001(4) 0.010(4) C27 0.061(5) 0.050(4) 0.072(5) 0.015(3) 0.010(4) 0.015(4) O4 0.065(4) 0.076(4) 0.092(4) 0.032(3) -0.012(3) -0.006(3) C28 0.077(7) 0.113(8) 0.097(7) 0.017(6) -0.018(5) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O1 2.775(5) . ? Ba1 O2 2.848(5) . ? Ba1 O3 2.903(5) . ? Ba1 C12 2.967(7) . ? Ba1 C2 2.993(6) . ? Ba1 C11 2.998(6) . ? Ba1 C3 3.005(6) . ? Ba1 C1 3.012(7) . ? Ba1 C13 3.014(6) . ? Ba1 C4 3.016(7) . ? Ba1 C5 3.018(7) . ? Ba1 C15 3.059(6) . ? Ba1 C14 3.068(6) . ? C1 C5 1.382(11) . ? C1 C2 1.414(11) . ? C1 C6 1.505(12) . ? C2 C3 1.378(11) . ? C2 C7 1.508(11) . ? C3 C4 1.359(11) . ? C3 C8 1.522(12) . ? C4 C5 1.352(11) . ? C4 C9 1.551(13) . ? C5 C10 1.526(11) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.387(10) . ? C11 C15 1.414(10) . ? C11 C16 1.509(10) . ? C12 C13 1.409(9) . ? C12 C17 1.517(10) . ? C13 C14 1.411(9) . ? C13 C18 1.500(9) . ? C14 C15 1.363(9) . ? C14 C19 1.512(10) . ? C15 C20 1.526(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O1 1.433(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? O1 C22 1.388(10) . ? C22 C23 1.462(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 O2 1.395(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? O2 C24 1.424(11) . ? C24 C25 1.453(13) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 O3 1.401(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? O3 C26 1.443(9) . ? C26 C27 1.489(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 O4 1.414(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O4 C28 1.404(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 O1 Ba1 O2 58.22(16) . . ? O1 Ba1 O3 115.83(15) . . ? O2 Ba1 O3 58.37(15) . . ? O1 Ba1 C12 121.77(18) . . ? O2 Ba1 C12 124.53(17) . . ? O3 Ba1 C12 87.29(17) . . ? O1 Ba1 C2 121.97(19) . . ? O2 Ba1 C2 124.9(2) . . ? O3 Ba1 C2 101.2(2) . . ? C12 Ba1 C2 101.97(18) . . ? O1 Ba1 C11 109.7(2) . . ? O2 Ba1 C11 142.57(17) . . ? O3 Ba1 C11 113.85(18) . . ? C12 Ba1 C11 26.89(19) . . ? C2 Ba1 C11 92.1(2) . . ? O1 Ba1 C3 115.6(2) . . ? O2 Ba1 C3 98.8(2) . . ? O3 Ba1 C3 82.72(17) . . ? C12 Ba1 C3 120.1(2) . . ? C2 Ba1 C3 26.6(2) . . ? C11 Ba1 C3 117.2(2) . . ? O1 Ba1 C1 97.2(2) . . ? O2 Ba1 C1 124.4(2) . . ? O3 Ba1 C1 126.06(17) . . ? C12 Ba1 C1 110.9(2) . . ? C2 Ba1 C1 27.2(2) . . ? C11 Ba1 C1 90.7(2) . . ? C3 Ba1 C1 43.8(2) . . ? O1 Ba1 C13 100.48(18) . . ? O2 Ba1 C13 99.91(16) . . ? O3 Ba1 C13 81.34(15) . . ? C12 Ba1 C13 27.23(17) . . ? C2 Ba1 C13 129.17(18) . . ? C11 Ba1 C13 44.43(19) . . ? C3 Ba1 C13 143.9(2) . . ? C1 Ba1 C13 135.1(2) . . ? O1 Ba1 C4 89.5(2) . . ? O2 Ba1 C4 84.35(19) . . ? O3 Ba1 C4 93.4(2) . . ? C12 Ba1 C4 144.7(2) . . ? C2 Ba1 C4 43.3(2) . . ? C11 Ba1 C4 132.8(2) . . ? C3 Ba1 C4 26.1(2) . . ? C1 Ba1 C4 43.2(2) . . ? C13 Ba1 C4 170.0(2) . . ? O1 Ba1 C5 78.60(18) . . ? O2 Ba1 C5 98.3(2) . . ? O3 Ba1 C5 119.3(2) . . ? C12 Ba1 C5 137.2(2) . . ? C2 Ba1 C5 43.84(18) . . ? C11 Ba1 C5 114.6(2) . . ? C3 Ba1 C5 43.2(2) . . ? C1 Ba1 C5 26.5(2) . . ? C13 Ba1 C5 157.8(2) . . ? C4 Ba1 C5 25.9(2) . . ? O1 Ba1 C15 83.13(19) . . ? O2 Ba1 C15 122.58(18) . . ? O3 Ba1 C15 124.90(16) . . ? C12 Ba1 C15 43.90(19) . . ? C2 Ba1 C15 111.0(2) . . ? C11 Ba1 C15 26.98(19) . . ? C3 Ba1 C15 137.6(2) . . ? C1 Ba1 C15 99.0(2) . . ? C13 Ba1 C15 43.63(18) . . ? C4 Ba1 C15 140.3(2) . . ? C5 Ba1 C15 114.9(2) . . ? O1 Ba1 C14 77.97(19) . . ? O2 Ba1 C14 99.97(16) . . ? O3 Ba1 C14 104.13(16) . . ? C12 Ba1 C14 43.95(18) . . ? C2 Ba1 C14 135.1(2) . . ? C11 Ba1 C14 43.67(17) . . ? C3 Ba1 C14 160.8(2) . . ? C1 Ba1 C14 124.52(19) . . ? C13 Ba1 C14 26.82(17) . . ? C4 Ba1 C14 161.6(2) . . ? C5 Ba1 C14 136.2(2) . . ? C15 Ba1 C14 25.71(17) . . ? C5 C1 C2 106.8(7) . . ? C5 C1 C6 127.4(10) . . ? C2 C1 C6 125.7(10) . . ? C5 C1 Ba1 77.0(4) . . ? C2 C1 Ba1 75.7(4) . . ? C6 C1 Ba1 116.2(5) . . ? C3 C2 C1 107.0(6) . . ? C3 C2 C7 124.6(10) . . ? C1 C2 C7 128.4(10) . . ? C3 C2 Ba1 77.2(4) . . ? C1 C2 Ba1 77.1(4) . . ? C7 C2 Ba1 111.2(5) . . ? C4 C3 C2 108.3(7) . . ? C4 C3 C8 125.0(11) . . ? C2 C3 C8 126.4(11) . . ? C4 C3 Ba1 77.4(4) . . ? C2 C3 Ba1 76.2(4) . . ? C8 C3 Ba1 117.9(5) . . ? C5 C4 C3 109.6(7) . . ? C5 C4 C9 124.3(10) . . ? C3 C4 C9 126.2(10) . . ? C5 C4 Ba1 77.1(4) . . ? C3 C4 Ba1 76.5(4) . . ? C9 C4 Ba1 115.0(5) . . ? C4 C5 C1 108.4(7) . . ? C4 C5 C10 127.5(10) . . ? C1 C5 C10 123.8(9) . . ? C4 C5 Ba1 77.0(4) . . ? C1 C5 Ba1 76.5(4) . . ? C10 C5 Ba1 117.2(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 107.1(6) . . ? C12 C11 C16 126.5(8) . . ? C15 C11 C16 125.5(8) . . ? C12 C11 Ba1 75.3(4) . . ? C15 C11 Ba1 78.9(4) . . ? C16 C11 Ba1 120.2(4) . . ? C11 C12 C13 108.8(6) . . ? C11 C12 C17 125.0(7) . . ? C13 C12 C17 126.2(7) . . ? C11 C12 Ba1 77.8(4) . . ? C13 C12 Ba1 78.2(4) . . ? C17 C12 Ba1 112.9(5) . . ? C12 C13 C14 106.5(6) . . ? C12 C13 C18 127.7(7) . . ? C14 C13 C18 125.7(6) . . ? C12 C13 Ba1 74.5(4) . . ? C14 C13 Ba1 78.7(4) . . ? C18 C13 Ba1 113.6(4) . . ? C15 C14 C13 108.9(6) . . ? C15 C14 C19 126.7(7) . . ? C13 C14 C19 124.4(7) . . ? C15 C14 Ba1 76.7(4) . . ? C13 C14 Ba1 74.4(4) . . ? C19 C14 Ba1 117.3(4) . . ? C14 C15 C11 108.7(6) . . ? C14 C15 C20 126.8(7) . . ? C11 C15 C20 124.1(7) . . ? C14 C15 Ba1 77.5(4) . . ? C11 C15 Ba1 74.1(4) . . ? C20 C15 Ba1 120.3(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 H21A 109.5 . . ? O1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 O1 C21 112.1(7) . . ? C22 O1 Ba1 120.6(5) . . ? C21 O1 Ba1 125.3(5) . . ? O1 C22 C23 111.5(7) . . ? O1 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? O1 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? O2 C23 C22 112.2(8) . . ? O2 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? O2 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 O2 C24 114.5(7) . . ? C23 O2 Ba1 117.5(5) . . ? C24 O2 Ba1 117.1(5) . . ? O2 C24 C25 110.4(7) . . ? O2 C24 H24A 109.6 . . ? C25 C24 H24A 109.6 . . ? O2 C24 H24B 109.6 . . ? C25 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? O3 C25 C24 110.8(8) . . ? O3 C25 H25A 109.5 . . ? C24 C25 H25A 109.5 . . ? O3 C25 H25B 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C25 O3 C26 112.7(6) . . ? C25 O3 Ba1 114.1(4) . . ? C26 O3 Ba1 124.9(4) . . ? O3 C26 C27 114.5(7) . . ? O3 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? O3 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? O4 C27 C26 108.6(6) . . ? O4 C27 H27A 110.0 . . ? C26 C27 H27A 110.0 . . ? O4 C27 H27B 110.0 . . ? C26 C27 H27B 110.0 . . ? H27A C27 H27B 108.3 . . ? C28 O4 C27 111.6(6) . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 1.978 _refine_diff_density_min -3.503 _refine_diff_density_rms 0.165 #===end data_7 _database_code_depnum_ccdc_archive 'CCDC 228236' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(1,3,5-tritertbutylcyclopentadienyl)barium(tetrahydrofuran) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H66 Ba O' _chemical_formula_sum 'C38 H66 Ba O' _chemical_formula_weight 676.25 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' 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 'P 21/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 10.602(2) _cell_length_b 23.618(8) _cell_length_c 15.104(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.046(19) _cell_angle_gamma 90.00 _cell_volume 3781.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6162 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_process_details 'North etal. (1968). Acta Cryst. A24, 351-359' _exptl_special_details ; Bis(1,3,5-tritertbutylcyclopentadienyl)barium(tetrahydrofuran) ; _diffrn_ambient_temperature 193(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 \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _diffrn_reflns_number 7004 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.1046 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6629 _reflns_number_gt 4466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7S software (1993)' _computing_cell_refinement 'TEXSAN (1993)' _computing_data_reduction 'TEXSAN (1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PC v. 5.03 (Sheldrick, 1994)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0766P)^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 6629 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0669 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.039 _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 Ba1 Ba 0.70629(3) 0.861941(13) 0.802067(18) 0.03175(8) Uani 1 1 d . . . C1 C 0.8187(5) 0.9494(2) 0.6796(3) 0.0322(13) Uani 1 1 d . . . C2 C 0.7632(5) 0.9089(2) 0.6213(3) 0.0322(13) Uani 1 1 d . . . H2A H 0.8107 0.8878 0.5751 0.039 Uiso 1 1 calc R . . C3 C 0.6323(5) 0.9123(2) 0.6234(3) 0.0356(13) Uani 1 1 d . . . C4 C 0.6026(5) 0.9537(2) 0.6855(3) 0.0324(13) Uani 1 1 d . . . H4A H 0.5170 0.9709 0.6917 0.039 Uiso 1 1 calc R . . C5 C 0.7170(5) 0.9780(2) 0.7209(3) 0.0331(13) Uani 1 1 d . . . C6 C 0.9631(5) 0.9579(2) 0.6839(3) 0.0428(15) Uani 1 1 d . . . C7 C 1.0207(6) 0.9415(3) 0.7730(4) 0.071(2) Uani 1 1 d . . . H7A H 0.9845 0.9652 0.8194 0.106 Uiso 1 1 calc R . . H7B H 1.1122 0.9472 0.7720 0.106 Uiso 1 1 calc R . . H7C H 1.0024 0.9017 0.7852 0.106 Uiso 1 1 calc R . . C8 C 1.0267(6) 0.9185(3) 0.6174(5) 0.076(2) Uani 1 1 d . . . H8A H 1.1182 0.9245 0.6200 0.114 Uiso 1 1 calc R . . H8B H 0.9949 0.9269 0.5575 0.114 Uiso 1 1 calc R . . H8C H 1.0078 0.8791 0.6321 0.114 Uiso 1 1 calc R . . C9 C 1.0033(6) 1.0173(3) 0.6599(5) 0.070(2) Uani 1 1 d . . . H9A H 0.9696 1.0441 0.7030 0.105 Uiso 1 1 calc R . . H9B H 0.9707 1.0268 0.6006 0.105 Uiso 1 1 calc R . . H9C H 1.0956 1.0196 0.6606 0.105 Uiso 1 1 calc R . . C10 C 0.5425(5) 0.8806(2) 0.5605(3) 0.0423(15) Uani 1 1 d . . . C11 C 0.5448(7) 0.8179(3) 0.5774(4) 0.070(2) Uani 1 1 d . . . H11A H 0.6290 0.8030 0.5651 0.105 Uiso 1 1 calc R . . H11B H 0.4824 0.7992 0.5387 0.105 Uiso 1 1 calc R . . H11C H 0.5246 0.8105 0.6394 0.105 Uiso 1 1 calc R . . C12 C 0.5807(7) 0.8923(3) 0.4663(3) 0.068(2) Uani 1 1 d . . . H12A H 0.6682 0.8803 0.4584 0.101 Uiso 1 1 calc R . . H12B H 0.5732 0.9329 0.4541 0.101 Uiso 1 1 calc R . . H12C H 0.5254 0.8712 0.4254 0.101 Uiso 1 1 calc R . . C13 C 0.4060(6) 0.9025(3) 0.5704(4) 0.063(2) Uani 1 1 d . . . H13A H 0.3500 0.8825 0.5286 0.094 Uiso 1 1 calc R . . H13B H 0.4033 0.9432 0.5579 0.094 Uiso 1 1 calc R . . H13C H 0.3782 0.8956 0.6310 0.094 Uiso 1 1 calc R . . C14 C 0.7087(5) 1.0321(2) 0.7773(3) 0.0382(14) Uani 1 1 d . . . C15 C 0.7105(7) 1.0836(3) 0.7169(4) 0.070(2) Uani 1 1 d . . . H15A H 0.7158 1.1181 0.7529 0.105 Uiso 1 1 calc R . . H15B H 0.6331 1.0845 0.6805 0.105 Uiso 1 1 calc R . . H15C H 0.7838 1.0815 0.6784 0.105 Uiso 1 1 calc R . . C16 C 0.5850(6) 1.0354(3) 0.8266(5) 0.072(2) Uani 1 1 d . . . H16A H 0.5788 1.0722 0.8561 0.108 Uiso 1 1 calc R . . H16B H 0.5821 1.0051 0.8709 0.108 Uiso 1 1 calc R . . H16C H 0.5143 1.0310 0.7844 0.108 Uiso 1 1 calc R . . C17 C 0.8114(7) 1.0406(3) 0.8474(4) 0.071(2) Uani 1 1 d . . . H17A H 0.7964 1.0761 0.8791 0.106 Uiso 1 1 calc R . . H17B H 0.8937 1.0422 0.8190 0.106 Uiso 1 1 calc R . . H17C H 0.8104 1.0089 0.8893 0.106 Uiso 1 1 calc R . . C18 C 0.5060(4) 0.8355(2) 0.9347(3) 0.0311(12) Uani 1 1 d . . . C19 C 0.5838(4) 0.8767(2) 0.9776(3) 0.0298(12) Uani 1 1 d . . . H19A H 0.5524 0.9137 1.0005 0.036 Uiso 1 1 calc R . . C20 C 0.7000(4) 0.8527(2) 1.0016(3) 0.0290(12) Uani 1 1 d . . . C21 C 0.6951(4) 0.7962(2) 0.9725(3) 0.0265(12) Uani 1 1 d . . . H21A H 0.7581 0.7667 0.9905 0.032 Uiso 1 1 calc R . . C22 C 0.5755(4) 0.7838(2) 0.9326(3) 0.0292(12) Uani 1 1 d . . . C23 C 0.3682(5) 0.8504(2) 0.9077(3) 0.0364(14) Uani 1 1 d . . . C24 C 0.3341(5) 0.8303(3) 0.8131(4) 0.0503(17) Uani 1 1 d . . . H24A H 0.3888 0.8492 0.7707 0.075 Uiso 1 1 calc R . . H24B H 0.2458 0.8396 0.7994 0.075 Uiso 1 1 calc R . . H24C H 0.3461 0.7892 0.8091 0.075 Uiso 1 1 calc R . . C25 C 0.3493(5) 0.9146(3) 0.9063(4) 0.0581(18) Uani 1 1 d . . . H25A H 0.4014 0.9313 0.8602 0.087 Uiso 1 1 calc R . . H25B H 0.3740 0.9304 0.9640 0.087 Uiso 1 1 calc R . . H25C H 0.2603 0.9232 0.8938 0.087 Uiso 1 1 calc R . . C26 C 0.2744(5) 0.8267(3) 0.9744(4) 0.0487(16) Uani 1 1 d . . . H26A H 0.1886 0.8382 0.9571 0.073 Uiso 1 1 calc R . . H26B H 0.2949 0.8414 1.0335 0.073 Uiso 1 1 calc R . . H26C H 0.2797 0.7853 0.9751 0.073 Uiso 1 1 calc R . . C27 C 0.8068(5) 0.8804(2) 1.0548(3) 0.0373(14) Uani 1 1 d . . . C28 C 0.9205(7) 0.8847(5) 1.0008(6) 0.165(4) Uani 1 1 d . . . H28A H 0.9890 0.9018 1.0360 0.247 Uiso 1 1 calc R . . H28B H 0.9023 0.9083 0.9487 0.247 Uiso 1 1 calc R . . H28C H 0.9459 0.8468 0.9816 0.247 Uiso 1 1 calc R . . C29 C 0.7738(7) 0.9393(3) 1.0829(6) 0.116(3) Uani 1 1 d . . . H29A H 0.8463 0.9564 1.1140 0.174 Uiso 1 1 calc R . . H29B H 0.7017 0.9380 1.1226 0.174 Uiso 1 1 calc R . . H29C H 0.7518 0.9620 1.0306 0.174 Uiso 1 1 calc R . . C30 C 0.8336(10) 0.8471(4) 1.1355(6) 0.179(4) Uani 1 1 d . . . H30A H 0.9067 0.8632 1.1671 0.268 Uiso 1 1 calc R . . H30B H 0.8517 0.8078 1.1192 0.268 Uiso 1 1 calc R . . H30C H 0.7601 0.8481 1.1739 0.268 Uiso 1 1 calc R . . C31 C 0.5499(5) 0.7238(2) 0.8971(3) 0.0326(13) Uani 1 1 d . . . C32 C 0.4181(5) 0.7010(2) 0.9177(4) 0.0511(17) Uani 1 1 d . . . H32A H 0.3542 0.7237 0.8863 0.077 Uiso 1 1 calc R . . H32B H 0.4043 0.7032 0.9816 0.077 Uiso 1 1 calc R . . H32C H 0.4115 0.6615 0.8984 0.077 Uiso 1 1 calc R . . C33 C 0.6411(5) 0.6812(2) 0.9407(4) 0.0444(15) Uani 1 1 d . . . H33A H 0.7275 0.6895 0.9226 0.067 Uiso 1 1 calc R . . H33B H 0.6182 0.6427 0.9220 0.067 Uiso 1 1 calc R . . H33C H 0.6359 0.6841 1.0052 0.067 Uiso 1 1 calc R . . C34 C 0.5728(6) 0.7214(2) 0.7964(3) 0.0494(17) Uani 1 1 d . . . H34A H 0.5068 0.7429 0.7650 0.074 Uiso 1 1 calc R . . H34B H 0.5707 0.6819 0.7764 0.074 Uiso 1 1 calc R . . H34C H 0.6554 0.7378 0.7838 0.074 Uiso 1 1 calc R . . O1 O 0.8848(4) 0.78220(16) 0.7628(2) 0.0486(11) Uani 1 1 d . . . C35 C 0.9765(6) 0.7549(3) 0.8194(4) 0.065(2) Uani 1 1 d . . . H35A H 0.9339 0.7320 0.8649 0.078 Uiso 1 1 calc R . . H35B H 1.0302 0.7835 0.8497 0.078 Uiso 1 1 calc R . . C36 C 1.0555(7) 0.7176(3) 0.7621(4) 0.074(2) Uani 1 1 d . . . H36A H 1.1462 0.7264 0.7709 0.088 Uiso 1 1 calc R . . H36B H 1.0416 0.6772 0.7767 0.088 Uiso 1 1 calc R . . C37 C 1.0172(7) 0.7289(4) 0.6749(4) 0.090(3) Uani 1 1 d . . . H37A H 1.0096 0.6930 0.6412 0.107 Uiso 1 1 calc R . . H37B H 1.0804 0.7531 0.6458 0.107 Uiso 1 1 calc R . . C38 C 0.8950(6) 0.7579(3) 0.6762(4) 0.0583(19) Uani 1 1 d . . . H38A H 0.8910 0.7878 0.6303 0.070 Uiso 1 1 calc R . . H38B H 0.8255 0.7307 0.6648 0.070 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 Ba1 0.03508(15) 0.02935(14) 0.03085(14) 0.00140(14) 0.00156(11) 0.00200(15) C1 0.037(3) 0.033(3) 0.027(2) 0.013(2) -0.004(2) 0.006(2) C2 0.040(3) 0.033(3) 0.024(2) -0.004(2) 0.001(2) 0.003(2) C3 0.039(3) 0.038(3) 0.029(2) 0.002(2) -0.012(2) 0.004(2) C4 0.032(3) 0.031(3) 0.033(2) -0.001(2) -0.007(2) 0.002(2) C5 0.031(3) 0.032(3) 0.036(3) 0.010(2) -0.002(2) -0.002(2) C6 0.027(3) 0.053(4) 0.048(3) 0.005(3) -0.002(2) 0.001(3) C7 0.042(4) 0.092(5) 0.077(4) 0.011(4) -0.020(3) 0.003(4) C8 0.040(3) 0.086(5) 0.102(5) -0.035(4) 0.008(4) 0.005(4) C9 0.051(4) 0.061(4) 0.098(5) 0.023(4) 0.022(4) -0.010(3) C10 0.046(3) 0.038(3) 0.042(3) -0.006(2) -0.013(3) -0.001(3) C11 0.092(5) 0.042(4) 0.075(4) -0.007(3) -0.035(4) -0.010(4) C12 0.090(5) 0.079(5) 0.033(3) 0.000(3) -0.022(3) -0.009(4) C13 0.047(4) 0.071(4) 0.070(4) -0.016(3) -0.019(3) -0.005(3) C14 0.042(3) 0.022(2) 0.050(3) 0.000(2) 0.001(3) -0.005(2) C15 0.086(5) 0.039(4) 0.087(5) 0.005(3) 0.022(4) 0.007(4) C16 0.071(4) 0.052(4) 0.094(5) -0.032(4) 0.019(4) -0.020(3) C17 0.075(5) 0.075(5) 0.063(4) -0.033(3) -0.014(4) 0.005(4) C18 0.022(2) 0.037(3) 0.034(2) 0.005(2) 0.000(2) -0.006(2) C19 0.031(3) 0.032(3) 0.027(2) -0.001(2) -0.004(2) -0.002(2) C20 0.030(2) 0.034(3) 0.023(2) 0.0011(19) 0.0043(19) -0.006(2) C21 0.025(2) 0.028(2) 0.026(2) 0.0053(19) -0.0024(19) 0.001(2) C22 0.024(2) 0.032(3) 0.032(2) 0.000(2) -0.004(2) 0.000(2) C23 0.042(3) 0.028(3) 0.039(3) -0.004(2) -0.004(2) 0.006(2) C24 0.043(3) 0.054(4) 0.053(3) -0.004(3) -0.011(3) 0.005(3) C25 0.039(3) 0.064(4) 0.071(4) 0.007(3) -0.008(3) 0.015(3) C26 0.028(3) 0.054(4) 0.064(4) 0.004(3) 0.002(3) 0.003(3) C27 0.028(3) 0.045(3) 0.039(3) -0.001(2) -0.004(2) -0.005(2) C28 0.054(4) 0.271(10) 0.171(8) -0.143(7) 0.030(5) -0.078(6) C29 0.075(5) 0.084(5) 0.187(8) -0.086(5) -0.054(5) 0.017(4) C30 0.209(8) 0.167(8) 0.154(6) 0.093(6) -0.150(6) -0.125(6) C31 0.033(3) 0.024(3) 0.041(3) 0.002(2) 0.007(2) -0.002(2) C32 0.057(4) 0.030(3) 0.067(4) -0.020(3) 0.010(3) -0.011(3) C33 0.054(3) 0.027(3) 0.052(3) -0.006(2) 0.000(3) 0.003(3) C34 0.066(4) 0.039(3) 0.043(3) -0.011(3) -0.003(3) 0.002(3) O1 0.053(2) 0.043(2) 0.049(2) -0.0044(18) 0.0028(19) 0.0115(19) C35 0.054(4) 0.090(5) 0.052(4) -0.012(4) -0.002(3) 0.016(4) C36 0.061(4) 0.090(5) 0.069(4) -0.018(4) -0.006(4) 0.030(4) C37 0.094(5) 0.124(7) 0.051(4) -0.005(4) 0.014(4) 0.055(5) C38 0.069(4) 0.062(4) 0.043(3) -0.004(3) 0.003(3) 0.022(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 Ba1 O1 2.743(4) . ? Ba1 C4 2.988(5) . ? Ba1 C19 2.993(5) . ? Ba1 C5 3.006(5) . ? Ba1 C21 3.010(4) . ? Ba1 C18 3.011(5) . ? Ba1 C2 3.018(5) . ? Ba1 C20 3.024(4) . ? Ba1 C1 3.031(5) . ? Ba1 C3 3.039(5) . ? Ba1 C22 3.052(5) . ? C1 C2 1.421(7) . ? C1 C5 1.427(7) . ? C1 C6 1.544(7) . ? C2 C3 1.391(7) . ? C2 H2A 1.0000 . ? C3 C4 1.395(7) . ? C3 C10 1.528(7) . ? C4 C5 1.437(7) . ? C4 H4A 1.0000 . ? C5 C14 1.537(7) . ? C6 C9 1.513(8) . ? C6 C7 1.518(8) . ? C6 C8 1.533(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.504(8) . ? C10 C12 1.511(8) . ? C10 C13 1.546(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C17 1.518(8) . ? C14 C16 1.521(8) . ? C14 C15 1.523(8) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.425(7) . ? C18 C22 1.427(7) . ? C18 C23 1.549(7) . ? C19 C20 1.399(7) . ? C19 H19A 1.0000 . ? C20 C21 1.406(6) . ? C20 C27 1.524(7) . ? C21 C22 1.424(6) . ? C21 H21A 1.0000 . ? C22 C31 1.538(7) . ? C23 C25 1.531(8) . ? C23 C26 1.535(7) . ? C23 C24 1.542(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.471(9) . ? C27 C30 1.474(10) . ? C27 C29 1.498(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.535(7) . ? C31 C32 1.536(7) . ? C31 C34 1.546(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O1 C38 1.435(7) . ? O1 C35 1.436(7) . ? C35 C36 1.500(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.397(9) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.466(9) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? 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 O1 Ba1 C4 128.21(12) . . ? O1 Ba1 C19 125.70(12) . . ? C4 Ba1 C19 106.04(13) . . ? O1 Ba1 C5 120.46(13) . . ? C4 Ba1 C5 27.74(13) . . ? C19 Ba1 C5 105.96(13) . . ? O1 Ba1 C21 82.46(12) . . ? C4 Ba1 C21 149.07(13) . . ? C19 Ba1 C21 43.81(13) . . ? C5 Ba1 C21 145.21(13) . . ? O1 Ba1 C18 119.93(13) . . ? C4 Ba1 C18 106.62(14) . . ? C19 Ba1 C18 27.45(13) . . ? C5 Ba1 C18 119.53(14) . . ? C21 Ba1 C18 44.35(13) . . ? O1 Ba1 C2 84.63(12) . . ? C4 Ba1 C2 43.81(13) . . ? C19 Ba1 C2 148.83(13) . . ? C5 Ba1 C2 44.50(13) . . ? C21 Ba1 C2 167.08(13) . . ? C18 Ba1 C2 146.43(13) . . ? O1 Ba1 C20 101.16(12) . . ? C4 Ba1 C20 128.68(13) . . ? C19 Ba1 C20 26.87(13) . . ? C5 Ba1 C20 118.28(13) . . ? C21 Ba1 C20 26.94(12) . . ? C18 Ba1 C20 45.05(13) . . ? C2 Ba1 C20 159.50(13) . . ? O1 Ba1 C1 93.17(12) . . ? C4 Ba1 C1 44.86(13) . . ? C19 Ba1 C1 130.01(13) . . ? C5 Ba1 C1 27.34(13) . . ? C21 Ba1 C1 153.54(13) . . ? C18 Ba1 C1 146.87(13) . . ? C2 Ba1 C1 27.17(13) . . ? C20 Ba1 C1 132.33(13) . . ? O1 Ba1 C3 104.17(12) . . ? C4 Ba1 C3 26.75(13) . . ? C19 Ba1 C3 129.18(13) . . ? C5 Ba1 C3 44.95(13) . . ? C21 Ba1 C3 161.38(13) . . ? C18 Ba1 C3 119.88(13) . . ? C2 Ba1 C3 26.56(13) . . ? C20 Ba1 C3 154.61(13) . . ? C1 Ba1 C3 44.73(13) . . ? O1 Ba1 C22 92.73(12) . . ? C4 Ba1 C22 130.72(13) . . ? C19 Ba1 C22 44.68(13) . . ? C5 Ba1 C22 146.71(13) . . ? C21 Ba1 C22 27.17(12) . . ? C18 Ba1 C22 27.21(13) . . ? C2 Ba1 C22 155.12(13) . . ? C20 Ba1 C22 45.10(12) . . ? C1 Ba1 C22 174.02(13) . . ? C3 Ba1 C22 134.22(13) . . ? C2 C1 C5 106.4(4) . . ? C2 C1 C6 120.8(4) . . ? C5 C1 C6 132.6(5) . . ? C2 C1 Ba1 75.9(3) . . ? C5 C1 Ba1 75.4(3) . . ? C6 C1 Ba1 117.6(3) . . ? C3 C2 C1 110.4(4) . . ? C3 C2 Ba1 77.6(3) . . ? C1 C2 Ba1 76.9(3) . . ? C3 C2 H2A 124.0 . . ? C1 C2 H2A 124.0 . . ? Ba1 C2 H2A 124.0 . . ? C2 C3 C4 107.1(4) . . ? C2 C3 C10 124.6(4) . . ? C4 C3 C10 128.0(5) . . ? C2 C3 Ba1 75.9(3) . . ? C4 C3 Ba1 74.6(3) . . ? C10 C3 Ba1 120.6(3) . . ? C3 C4 C5 109.4(4) . . ? C3 C4 Ba1 78.6(3) . . ? C5 C4 Ba1 76.8(3) . . ? C3 C4 H4A 124.3 . . ? C5 C4 H4A 124.3 . . ? Ba1 C4 H4A 124.3 . . ? C1 C5 C4 106.7(4) . . ? C1 C5 C14 133.4(5) . . ? C4 C5 C14 118.8(4) . . ? C1 C5 Ba1 77.3(3) . . ? C4 C5 Ba1 75.4(3) . . ? C14 C5 Ba1 121.9(3) . . ? C9 C6 C7 109.7(5) . . ? C9 C6 C8 106.1(5) . . ? C7 C6 C8 104.6(5) . . ? C9 C6 C1 113.2(5) . . ? C7 C6 C1 112.7(4) . . ? C8 C6 C1 110.0(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 109.6(5) . . ? C11 C10 C3 111.6(5) . . ? C12 C10 C3 108.7(5) . . ? C11 C10 C13 109.0(5) . . ? C12 C10 C13 107.3(5) . . ? C3 C10 C13 110.5(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C17 C14 C16 105.5(5) . . ? C17 C14 C15 107.2(5) . . ? C16 C14 C15 105.8(5) . . ? C17 C14 C5 116.6(5) . . ? C16 C14 C5 111.9(4) . . ? C15 C14 C5 109.3(4) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C22 107.4(4) . . ? C19 C18 C23 120.0(4) . . ? C22 C18 C23 132.3(4) . . ? C19 C18 Ba1 75.6(3) . . ? C22 C18 Ba1 78.0(3) . . ? C23 C18 Ba1 116.8(3) . . ? C20 C19 C18 110.0(4) . . ? C20 C19 Ba1 77.8(3) . . ? C18 C19 Ba1 77.0(3) . . ? C20 C19 H19A 124.2 . . ? C18 C19 H19A 124.2 . . ? Ba1 C19 H19A 124.2 . . ? C19 C20 C21 106.0(4) . . ? C19 C20 C27 127.3(4) . . ? C21 C20 C27 126.6(4) . . ? C19 C20 Ba1 75.3(3) . . ? C21 C20 Ba1 76.0(2) . . ? C27 C20 Ba1 117.7(3) . . ? C20 C21 C22 110.9(4) . . ? C20 C21 Ba1 77.1(3) . . ? C22 C21 Ba1 78.1(3) . . ? C20 C21 H21A 123.8 . . ? C22 C21 H21A 123.8 . . ? Ba1 C21 H21A 123.8 . . ? C21 C22 C18 105.7(4) . . ? C21 C22 C31 119.2(4) . . ? C18 C22 C31 135.1(4) . . ? C21 C22 Ba1 74.8(3) . . ? C18 C22 Ba1 74.8(3) . . ? C31 C22 Ba1 114.3(3) . . ? C25 C23 C26 106.5(4) . . ? C25 C23 C24 105.3(4) . . ? C26 C23 C24 110.6(4) . . ? C25 C23 C18 110.6(4) . . ? C26 C23 C18 111.3(4) . . ? C24 C23 C18 112.2(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C30 110.4(7) . . ? C28 C27 C29 106.9(7) . . ? C30 C27 C29 107.7(6) . . ? C28 C27 C20 110.2(5) . . ? C30 C27 C20 109.7(5) . . ? C29 C27 C20 111.9(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 104.6(4) . . ? C33 C31 C22 110.4(4) . . ? C32 C31 C22 114.0(4) . . ? C33 C31 C34 106.8(4) . . ? C32 C31 C34 110.3(4) . . ? C22 C31 C34 110.3(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 O1 C35 107.6(4) . . ? C38 O1 Ba1 122.4(3) . . ? C35 O1 Ba1 130.0(3) . . ? O1 C35 C36 107.4(5) . . ? O1 C35 H35A 110.2 . . ? C36 C35 H35A 110.2 . . ? O1 C35 H35B 110.2 . . ? C36 C35 H35B 110.2 . . ? H35A C35 H35B 108.5 . . ? C37 C36 C35 106.1(6) . . ? C37 C36 H36A 110.5 . . ? C35 C36 H36A 110.5 . . ? C37 C36 H36B 110.5 . . ? C35 C36 H36B 110.5 . . ? H36A C36 H36B 108.7 . . ? C36 C37 C38 108.5(6) . . ? C36 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? C36 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? O1 C38 C37 106.3(5) . . ? O1 C38 H38A 110.5 . . ? C37 C38 H38A 110.5 . . ? O1 C38 H38B 110.5 . . ? C37 C38 H38B 110.5 . . ? H38A C38 H38B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.110 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.125 #===end data_8 _database_code_depnum_ccdc_archive 'CCDC 228237' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(N,N-dimethylaminoethyl-1,2,3,4-tetramethylcyclopentadienyl)barium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H44 Ba N2' _chemical_formula_sum 'C26 H44 Ba1 N2' _chemical_formula_weight 521.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 Hexagonal _symmetry_space_group_name_H-M 'R -3 C' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'y+2/3, x+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'y+1/3, x+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-y+2/3, -x+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-y+1/3, -x+2/3, z+1/6' _cell_length_a 17.028(5) _cell_length_b 17.028(5) _cell_length_c 47.342(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 120.000(5) _cell_volume 11888(5) _cell_formula_units_Z 18 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max .26 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4860 _exptl_absorpt_coefficient_mu 1.517 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 4526 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.26 _reflns_number_total 2400 _reflns_number_gt 2071 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'AFC7S software' _computing_cell_refinement 'AFC7S software' _computing_data_reduction 'TEXSAN (1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL Ver. 5.1 (Bruker AXS, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0676P)^2^+13.9423P] 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 2400 _refine_ls_number_parameters 132 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0588 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1139 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba Ba 0.6667 -0.01533(2) 0.0833 0.03007(18) Uani 1 2 d S . . N1 N 0.5749(3) -0.1608(3) 0.04302(9) 0.0448(10) Uani 1 1 d . . . C1 C 0.7223(4) 0.0270(3) 0.02396(9) 0.0395(11) Uani 1 1 d . . . C2 C 0.6964(3) 0.0911(3) 0.03121(9) 0.0382(10) Uani 1 1 d . . . C3 C 0.7636(4) 0.1545(3) 0.04967(10) 0.0486(13) Uani 1 1 d . . . C4 C 0.8294(3) 0.1282(4) 0.05333(11) 0.0563(15) Uani 1 1 d . . . C5 C 0.8036(4) 0.0496(4) 0.03711(12) 0.0494(13) Uani 1 1 d . . . C6 C 0.6695(4) -0.0532(4) 0.00445(10) 0.0562(15) Uani 1 1 d . . . H6A H 0.7055 -0.0835 0.0014 0.067 Uiso 1 1 calc R . . H6B H 0.6630 -0.0301 -0.0141 0.067 Uiso 1 1 calc R . . C7 C 0.5754(5) -0.1239(4) 0.01469(13) 0.0693(18) Uani 1 1 d . . . H7A H 0.5362 -0.0963 0.0151 0.083 Uiso 1 1 calc R . . H7B H 0.5488 -0.1746 0.0010 0.083 Uiso 1 1 calc R . . C8 C 0.4801(5) -0.2231(5) 0.05042(16) 0.085(2) Uani 1 1 d . . . H8A H 0.4524 -0.2707 0.0360 0.127 Uiso 1 1 calc R . . H8B H 0.4471 -0.1897 0.0513 0.127 Uiso 1 1 calc R . . H8C H 0.4772 -0.2507 0.0688 0.127 Uiso 1 1 calc R . . C9 C 0.6205(5) -0.2125(4) 0.04221(15) 0.0737(18) Uani 1 1 d . . . H9A H 0.5903 -0.2621 0.0286 0.111 Uiso 1 1 calc R . . H9B H 0.6186 -0.2377 0.0610 0.111 Uiso 1 1 calc R . . H9C H 0.6838 -0.1731 0.0366 0.111 Uiso 1 1 calc R . . C10 C 0.6140(4) 0.0934(4) 0.02074(12) 0.0565(14) Uani 1 1 d . . . H10A H 0.6294 0.1298 0.0035 0.085 Uiso 1 1 calc R . . H10B H 0.5936 0.1204 0.0352 0.085 Uiso 1 1 calc R . . H10C H 0.5653 0.0315 0.0167 0.085 Uiso 1 1 calc R . . C11 C 0.7681(6) 0.2399(4) 0.06094(12) 0.081(2) Uani 1 1 d . . . H11A H 0.8021 0.2900 0.0477 0.121 Uiso 1 1 calc R . . H11B H 0.7985 0.2552 0.0793 0.121 Uiso 1 1 calc R . . H11C H 0.7065 0.2299 0.0631 0.121 Uiso 1 1 calc R . . C12 C 0.9164(4) 0.1822(6) 0.07025(16) 0.096(3) Uani 1 1 d . . . H12A H 0.9641 0.2266 0.0579 0.144 Uiso 1 1 calc R . . H12B H 0.9353 0.1409 0.0780 0.144 Uiso 1 1 calc R . . H12C H 0.9057 0.2140 0.0857 0.144 Uiso 1 1 calc R . . C13 C 0.8600(5) 0.0037(5) 0.03392(14) 0.081(2) Uani 1 1 d . . . H13A H 0.9023 0.0312 0.0181 0.122 Uiso 1 1 calc R . . H13B H 0.8199 -0.0611 0.0302 0.122 Uiso 1 1 calc R . . H13C H 0.8942 0.0114 0.0513 0.122 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 0.0321(2) 0.0344(2) 0.0229(2) 0.00096(7) 0.00192(13) 0.01607(12) N1 0.056(3) 0.037(2) 0.037(2) -0.0037(19) 0.0006(19) 0.020(2) C1 0.049(3) 0.039(2) 0.026(2) 0.0060(19) 0.008(2) 0.019(2) C2 0.047(3) 0.039(2) 0.027(2) 0.001(2) 0.002(2) 0.020(2) C3 0.067(3) 0.029(2) 0.033(3) 0.004(2) 0.008(2) 0.011(2) C4 0.041(3) 0.060(3) 0.039(3) 0.018(3) -0.001(2) 0.003(3) C5 0.049(3) 0.058(3) 0.040(3) 0.019(2) 0.016(2) 0.025(3) C6 0.094(5) 0.047(3) 0.024(2) -0.004(2) 0.000(3) 0.033(3) C7 0.094(5) 0.046(3) 0.055(4) -0.014(3) -0.026(3) 0.025(3) C8 0.067(4) 0.059(4) 0.103(6) -0.009(4) 0.009(4) 0.013(3) C9 0.096(5) 0.067(4) 0.069(4) 0.000(3) 0.000(4) 0.048(4) C10 0.067(4) 0.064(3) 0.041(3) 0.003(3) 0.002(3) 0.034(3) C11 0.133(6) 0.037(3) 0.040(3) -0.005(3) 0.007(4) 0.018(4) C12 0.050(4) 0.102(6) 0.075(5) 0.024(4) -0.011(3) -0.007(4) C13 0.074(4) 0.131(7) 0.066(4) 0.037(4) 0.033(4) 0.072(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba N1 2.889(4) . ? Ba N1 2.889(4) 17_654 ? Ba C1 2.939(4) . ? Ba C1 2.939(4) 17_654 ? Ba C2 2.951(5) . ? Ba C2 2.951(5) 17_654 ? Ba C3 2.976(5) . ? Ba C3 2.976(5) 17_654 ? Ba C5 2.978(5) . ? Ba C5 2.978(5) 17_654 ? Ba C4 2.983(5) . ? Ba C4 2.983(5) 17_654 ? N1 C9 1.438(7) . ? N1 C8 1.463(8) . ? N1 C7 1.479(7) . ? C1 C5 1.386(8) . ? C1 C2 1.408(7) . ? C1 C6 1.517(7) . ? C2 C3 1.416(7) . ? C2 C10 1.508(7) . ? C3 C4 1.410(8) . ? C3 C11 1.515(8) . ? C4 C5 1.410(8) . ? C4 C12 1.523(8) . ? C5 C13 1.518(8) . ? C6 C7 1.524(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 N1 Ba N1 108.15(17) . 17_654 ? N1 Ba C1 63.16(13) . . ? N1 Ba C1 123.40(14) 17_654 . ? N1 Ba C1 123.40(14) . 17_654 ? N1 Ba C1 63.16(13) 17_654 17_654 ? C1 Ba C1 170.33(18) . 17_654 ? N1 Ba C2 80.05(13) . . ? N1 Ba C2 142.41(13) 17_654 . ? C1 Ba C2 27.65(13) . . ? C1 Ba C2 142.82(13) 17_654 . ? N1 Ba C2 142.42(13) . 17_654 ? N1 Ba C2 80.05(13) 17_654 17_654 ? C1 Ba C2 142.82(13) . 17_654 ? C1 Ba C2 27.65(13) 17_654 17_654 ? C2 Ba C2 116.26(18) . 17_654 ? N1 Ba C3 106.19(13) . . ? N1 Ba C3 122.43(14) 17_654 . ? C1 Ba C3 45.18(13) . . ? C1 Ba C3 126.00(14) 17_654 . ? C2 Ba C3 27.63(14) . . ? C2 Ba C3 98.77(13) 17_654 . ? N1 Ba C3 122.43(14) . 17_654 ? N1 Ba C3 106.19(13) 17_654 17_654 ? C1 Ba C3 126.00(14) . 17_654 ? C1 Ba C3 45.18(13) 17_654 17_654 ? C2 Ba C3 98.77(13) . 17_654 ? C2 Ba C3 27.64(14) 17_654 17_654 ? C3 Ba C3 92.0(2) . 17_654 ? N1 Ba C5 79.65(15) . . ? N1 Ba C5 98.95(14) 17_654 . ? C1 Ba C5 27.08(15) . . ? C1 Ba C5 153.35(15) 17_654 . ? C2 Ba C5 45.23(14) . . ? C2 Ba C5 136.54(14) 17_654 . ? C3 Ba C5 45.17(15) . . ? C3 Ba C5 137.17(15) 17_654 . ? N1 Ba C5 98.95(14) . 17_654 ? N1 Ba C5 79.65(15) 17_654 17_654 ? C1 Ba C5 153.35(15) . 17_654 ? C1 Ba C5 27.08(15) 17_654 17_654 ? C2 Ba C5 136.54(14) . 17_654 ? C2 Ba C5 45.23(14) 17_654 17_654 ? C3 Ba C5 137.17(15) . 17_654 ? C3 Ba C5 45.18(15) 17_654 17_654 ? C5 Ba C5 177.7(2) . 17_654 ? N1 Ba C4 105.70(14) . . ? N1 Ba C4 98.39(14) 17_654 . ? C1 Ba C4 44.77(14) . . ? C1 Ba C4 130.55(15) 17_654 . ? C2 Ba C4 45.16(14) . . ? C2 Ba C4 109.28(15) 17_654 . ? C3 Ba C4 27.37(15) . . ? C3 Ba C4 113.26(18) 17_654 . ? C5 Ba C4 27.37(16) . . ? C5 Ba C4 154.51(16) 17_654 . ? N1 Ba C4 98.39(14) . 17_654 ? N1 Ba C4 105.71(14) 17_654 17_654 ? C1 Ba C4 130.55(15) . 17_654 ? C1 Ba C4 44.77(14) 17_654 17_654 ? C2 Ba C4 109.28(15) . 17_654 ? C2 Ba C4 45.16(14) 17_654 17_654 ? C3 Ba C4 113.26(18) . 17_654 ? C3 Ba C4 27.37(15) 17_654 17_654 ? C5 Ba C4 154.51(16) . 17_654 ? C5 Ba C4 27.37(16) 17_654 17_654 ? C4 Ba C4 138.4(3) . 17_654 ? C9 N1 C8 107.5(5) . . ? C9 N1 C7 110.2(5) . . ? C8 N1 C7 107.2(5) . . ? C9 N1 Ba 108.5(4) . . ? C8 N1 Ba 113.0(4) . . ? C7 N1 Ba 110.5(3) . . ? C5 C1 C2 109.4(5) . . ? C5 C1 C6 125.7(5) . . ? C2 C1 C6 124.9(5) . . ? C5 C1 Ba 78.1(3) . . ? C2 C1 Ba 76.7(3) . . ? C6 C1 Ba 112.8(3) . . ? C1 C2 C3 107.2(5) . . ? C1 C2 C10 126.6(5) . . ? C3 C2 C10 126.2(5) . . ? C1 C2 Ba 75.7(3) . . ? C3 C2 Ba 77.2(3) . . ? C10 C2 Ba 114.5(3) . . ? C4 C3 C2 107.5(5) . . ? C4 C3 C11 126.5(6) . . ? C2 C3 C11 125.7(6) . . ? C4 C3 Ba 76.6(3) . . ? C2 C3 Ba 75.2(3) . . ? C11 C3 Ba 118.8(3) . . ? C3 C4 C5 108.4(5) . . ? C3 C4 C12 124.1(7) . . ? C5 C4 C12 127.4(7) . . ? C3 C4 Ba 76.0(3) . . ? C5 C4 Ba 76.1(3) . . ? C12 C4 Ba 118.0(4) . . ? C1 C5 C4 107.5(5) . . ? C1 C5 C13 127.9(6) . . ? C4 C5 C13 124.5(6) . . ? C1 C5 Ba 74.9(3) . . ? C4 C5 Ba 76.5(3) . . ? C13 C5 Ba 117.5(3) . . ? C1 C6 C7 115.7(4) . . ? C1 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? C1 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? N1 C7 C6 113.9(5) . . ? N1 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? N1 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 H12A 109.5 . . ? C4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C5 C13 H13A 109.5 . . ? C5 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C5 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ba N1 C9 -24.8(3) 17_654 . . . ? C1 Ba N1 C9 94.1(4) . . . . ? C1 Ba N1 C9 -94.1(4) 17_654 . . . ? C2 Ba N1 C9 117.3(4) . . . . ? C2 Ba N1 C9 -122.1(4) 17_654 . . . ? C3 Ba N1 C9 108.3(4) . . . . ? C3 Ba N1 C9 -148.5(4) 17_654 . . . ? C5 Ba N1 C9 71.4(4) . . . . ? C5 Ba N1 C9 -106.7(4) 17_654 . . . ? C4 Ba N1 C9 79.8(4) . . . . ? C4 Ba N1 C9 -134.4(4) 17_654 . . . ? N1 Ba N1 C8 94.3(4) 17_654 . . . ? C1 Ba N1 C8 -146.8(4) . . . . ? C1 Ba N1 C8 25.0(4) 17_654 . . . ? C2 Ba N1 C8 -123.6(4) . . . . ? C2 Ba N1 C8 -3.0(5) 17_654 . . . ? C3 Ba N1 C8 -132.6(4) . . . . ? C3 Ba N1 C8 -29.5(4) 17_654 . . . ? C5 Ba N1 C8 -169.6(4) . . . . ? C5 Ba N1 C8 12.3(4) 17_654 . . . ? C4 Ba N1 C8 -161.1(4) . . . . ? C4 Ba N1 C8 -15.4(4) 17_654 . . . ? N1 Ba N1 C7 -145.6(4) 17_654 . . . ? C1 Ba N1 C7 -26.7(4) . . . . ? C1 Ba N1 C7 145.0(4) 17_654 . . . ? C2 Ba N1 C7 -3.5(4) . . . . ? C2 Ba N1 C7 117.0(4) 17_654 . . . ? C3 Ba N1 C7 -12.6(4) . . . . ? C3 Ba N1 C7 90.6(4) 17_654 . . . ? C5 Ba N1 C7 -49.5(4) . . . . ? C5 Ba N1 C7 132.4(4) 17_654 . . . ? C4 Ba N1 C7 -41.1(4) . . . . ? C4 Ba N1 C7 104.7(4) 17_654 . . . ? N1 Ba C1 C5 -123.2(3) . . . . ? N1 Ba C1 C5 -28.3(3) 17_654 . . . ? C1 Ba C1 C5 102.2(3) 17_654 . . . ? C2 Ba C1 C5 113.5(4) . . . . ? C2 Ba C1 C5 93.4(4) 17_654 . . . ? C3 Ba C1 C5 76.1(3) . . . . ? C3 Ba C1 C5 124.8(3) 17_654 . . . ? C5 Ba C1 C5 -174.9(5) 17_654 . . . ? C4 Ba C1 C5 37.0(3) . . . . ? C4 Ba C1 C5 159.4(3) 17_654 . . . ? N1 Ba C1 C2 123.3(3) . . . . ? N1 Ba C1 C2 -141.9(3) 17_654 . . . ? C1 Ba C1 C2 -11.4(3) 17_654 . . . ? C2 Ba C1 C2 -20.1(5) 17_654 . . . ? C3 Ba C1 C2 -37.4(3) . . . . ? C3 Ba C1 C2 11.2(4) 17_654 . . . ? C5 Ba C1 C2 -113.5(4) . . . . ? C5 Ba C1 C2 71.6(4) 17_654 . . . ? C4 Ba C1 C2 -76.5(3) . . . . ? C4 Ba C1 C2 45.8(4) 17_654 . . . ? N1 Ba C1 C6 0.7(4) . . . . ? N1 Ba C1 C6 95.6(4) 17_654 . . . ? C1 Ba C1 C6 -133.9(4) 17_654 . . . ? C2 Ba C1 C6 -122.5(6) . . . . ? C2 Ba C1 C6 -142.6(4) 17_654 . . . ? C3 Ba C1 C6 -159.9(5) . . . . ? C3 Ba C1 C6 -111.3(4) 17_654 . . . ? C5 Ba C1 C6 123.9(5) . . . . ? C5 Ba C1 C6 -51.0(5) 17_654 . . . ? C4 Ba C1 C6 161.0(5) . . . . ? C4 Ba C1 C6 -76.7(4) 17_654 . . . ? C5 C1 C2 C3 -0.6(5) . . . . ? C6 C1 C2 C3 -179.9(4) . . . . ? Ba C1 C2 C3 71.4(3) . . . . ? C5 C1 C2 C10 177.9(5) . . . . ? C6 C1 C2 C10 -1.4(8) . . . . ? Ba C1 C2 C10 -110.1(5) . . . . ? C5 C1 C2 Ba -72.0(3) . . . . ? C6 C1 C2 Ba 108.7(5) . . . . ? N1 Ba C2 C1 -49.2(3) . . . . ? N1 Ba C2 C1 57.6(4) 17_654 . . . ? C1 Ba C2 C1 176.85(10) 17_654 . . . ? C2 Ba C2 C1 166.6(3) 17_654 . . . ? C3 Ba C2 C1 111.8(5) . . . . ? C3 Ba C2 C1 -170.8(3) 17_654 . . . ? C5 Ba C2 C1 36.0(3) . . . . ? C5 Ba C2 C1 -141.8(3) 17_654 . . . ? C4 Ba C2 C1 75.0(3) . . . . ? C4 Ba C2 C1 -144.7(3) 17_654 . . . ? N1 Ba C2 C3 -161.0(3) . . . . ? N1 Ba C2 C3 -54.1(4) 17_654 . . . ? C1 Ba C2 C3 -111.8(5) . . . . ? C1 Ba C2 C3 65.1(4) 17_654 . . . ? C2 Ba C2 C3 54.8(3) 17_654 . . . ? C3 Ba C2 C3 77.4(4) 17_654 . . . ? C5 Ba C2 C3 -75.8(3) . . . . ? C5 Ba C2 C3 106.4(3) 17_654 . . . ? C4 Ba C2 C3 -36.8(3) . . . . ? C4 Ba C2 C3 103.5(3) 17_654 . . . ? N1 Ba C2 C10 74.8(4) . . . . ? N1 Ba C2 C10 -178.3(3) 17_654 . . . ? C1 Ba C2 C10 124.1(5) . . . . ? C1 Ba C2 C10 -59.1(5) 17_654 . . . ? C2 Ba C2 C10 -69.3(3) 17_654 . . . ? C3 Ba C2 C10 -124.2(5) . . . . ? C3 Ba C2 C10 -46.8(4) 17_654 . . . ? C5 Ba C2 C10 160.1(4) . . . . ? C5 Ba C2 C10 -17.7(4) 17_654 . . . ? C4 Ba C2 C10 -161.0(5) . . . . ? C4 Ba C2 C10 -20.7(4) 17_654 . . . ? C1 C2 C3 C4 0.1(5) . . . . ? C10 C2 C3 C4 -178.4(5) . . . . ? Ba C2 C3 C4 70.4(3) . . . . ? C1 C2 C3 C11 174.6(5) . . . . ? C10 C2 C3 C11 -3.9(8) . . . . ? Ba C2 C3 C11 -115.1(5) . . . . ? C1 C2 C3 Ba -70.4(3) . . . . ? C10 C2 C3 Ba 111.1(5) . . . . ? N1 Ba C3 C4 -93.0(3) . . . . ? N1 Ba C3 C4 31.7(4) 17_654 . . . ? C1 Ba C3 C4 -75.1(3) . . . . ? C1 Ba C3 C4 110.2(3) 17_654 . . . ? C2 Ba C3 C4 -112.5(5) . . . . ? C2 Ba C3 C4 115.4(3) 17_654 . . . ? C3 Ba C3 C4 142.3(4) 17_654 . . . ? C5 Ba C3 C4 -36.5(3) . . . . ? C5 Ba C3 C4 143.5(3) 17_654 . . . ? C4 Ba C3 C4 160.1(3) 17_654 . . . ? N1 Ba C3 C2 19.5(3) . . . . ? N1 Ba C3 C2 144.2(3) 17_654 . . . ? C1 Ba C3 C2 37.4(3) . . . . ? C1 Ba C3 C2 -137.4(3) 17_654 . . . ? C2 Ba C3 C2 -132.1(3) 17_654 . . . ? C3 Ba C3 C2 -105.2(3) 17_654 . . . ? C5 Ba C3 C2 76.0(3) . . . . ? C5 Ba C3 C2 -104.0(3) 17_654 . . . ? C4 Ba C3 C2 112.5(5) . . . . ? C4 Ba C3 C2 -87.4(3) 17_654 . . . ? N1 Ba C3 C11 142.5(5) . . . . ? N1 Ba C3 C11 -92.9(5) 17_654 . . . ? C1 Ba C3 C11 160.4(6) . . . . ? C1 Ba C3 C11 -14.4(5) 17_654 . . . ? C2 Ba C3 C11 123.0(6) . . . . ? C2 Ba C3 C11 -9.2(5) 17_654 . . . ? C3 Ba C3 C11 17.8(4) 17_654 . . . ? C5 Ba C3 C11 -161.1(6) . . . . ? C5 Ba C3 C11 19.0(6) 17_654 . . . ? C4 Ba C3 C11 -124.5(6) . . . . ? C4 Ba C3 C11 35.6(5) 17_654 . . . ? C2 C3 C4 C5 0.5(6) . . . . ? C11 C3 C4 C5 -174.0(5) . . . . ? Ba C3 C4 C5 70.0(4) . . . . ? C2 C3 C4 C12 176.0(5) . . . . ? C11 C3 C4 C12 1.5(9) . . . . ? Ba C3 C4 C12 -114.6(5) . . . . ? C2 C3 C4 Ba -69.5(3) . . . . ? C11 C3 C4 Ba 116.1(5) . . . . ? N1 Ba C4 C3 95.0(3) . . . . ? N1 Ba C4 C3 -153.4(3) 17_654 . . . ? C1 Ba C4 C3 76.7(3) . . . . ? C1 Ba C4 C3 -91.7(3) 17_654 . . . ? C2 Ba C4 C3 37.2(3) . . . . ? C2 Ba C4 C3 -71.1(3) 17_654 . . . ? C3 Ba C4 C3 -41.7(4) 17_654 . . . ? C5 Ba C4 C3 113.3(5) . . . . ? C5 Ba C4 C3 -69.9(5) 17_654 . . . ? C4 Ba C4 C3 -28.0(3) 17_654 . . . ? N1 Ba C4 C5 -18.3(4) . . . . ? N1 Ba C4 C5 93.3(3) 17_654 . . . ? C1 Ba C4 C5 -36.6(3) . . . . ? C1 Ba C4 C5 155.0(3) 17_654 . . . ? C2 Ba C4 C5 -76.1(3) . . . . ? C2 Ba C4 C5 175.6(3) 17_654 . . . ? C3 Ba C4 C5 -113.3(5) . . . . ? C3 Ba C4 C5 -155.0(3) 17_654 . . . ? C5 Ba C4 C5 176.8(3) 17_654 . . . ? C4 Ba C4 C5 -141.4(3) 17_654 . . . ? N1 Ba C4 C12 -143.6(6) . . . . ? N1 Ba C4 C12 -32.0(6) 17_654 . . . ? C1 Ba C4 C12 -161.8(7) . . . . ? C1 Ba C4 C12 29.7(7) 17_654 . . . ? C2 Ba C4 C12 158.6(7) . . . . ? C2 Ba C4 C12 50.4(6) 17_654 . . . ? C3 Ba C4 C12 121.4(8) . . . . ? C3 Ba C4 C12 79.8(6) 17_654 . . . ? C5 Ba C4 C12 -125.2(8) . . . . ? C5 Ba C4 C12 51.6(8) 17_654 . . . ? C4 Ba C4 C12 93.4(6) 17_654 . . . ? C2 C1 C5 C4 0.9(6) . . . . ? C6 C1 C5 C4 -179.8(4) . . . . ? Ba C1 C5 C4 -70.2(4) . . . . ? C2 C1 C5 C13 -175.7(5) . . . . ? C6 C1 C5 C13 3.6(8) . . . . ? Ba C1 C5 C13 113.3(5) . . . . ? C2 C1 C5 Ba 71.1(3) . . . . ? C6 C1 C5 Ba -109.7(5) . . . . ? C3 C4 C5 C1 -0.8(6) . . . . ? C12 C4 C5 C1 -176.1(5) . . . . ? Ba C4 C5 C1 69.1(4) . . . . ? C3 C4 C5 C13 175.9(5) . . . . ? C12 C4 C5 C13 0.6(9) . . . . ? Ba C4 C5 C13 -114.3(5) . . . . ? C3 C4 C5 Ba -69.9(4) . . . . ? C12 C4 C5 Ba 114.8(6) . . . . ? N1 Ba C5 C1 49.4(3) . . . . ? N1 Ba C5 C1 156.3(3) 17_654 . . . ? C1 Ba C5 C1 -158.5(4) 17_654 . . . ? C2 Ba C5 C1 -36.8(3) . . . . ? C2 Ba C5 C1 -118.7(3) 17_654 . . . ? C3 Ba C5 C1 -76.2(3) . . . . ? C3 Ba C5 C1 -77.8(4) 17_654 . . . ? C5 Ba C5 C1 103.0(3) 17_654 . . . ? C4 Ba C5 C1 -112.7(5) . . . . ? C4 Ba C5 C1 -38.4(5) 17_654 . . . ? N1 Ba C5 C4 162.1(3) . . . . ? N1 Ba C5 C4 -91.0(3) 17_654 . . . ? C1 Ba C5 C4 112.7(5) . . . . ? C1 Ba C5 C4 -45.8(5) 17_654 . . . ? C2 Ba C5 C4 75.9(3) . . . . ? C2 Ba C5 C4 -6.0(4) 17_654 . . . ? C3 Ba C5 C4 36.5(3) . . . . ? C3 Ba C5 C4 34.8(4) 17_654 . . . ? C5 Ba C5 C4 -144.3(3) 17_654 . . . ? C4 Ba C5 C4 74.3(6) 17_654 . . . ? N1 Ba C5 C13 -75.8(5) . . . . ? N1 Ba C5 C13 31.1(5) 17_654 . . . ? C1 Ba C5 C13 -125.2(6) . . . . ? C1 Ba C5 C13 76.3(6) 17_654 . . . ? C2 Ba C5 C13 -162.0(6) . . . . ? C2 Ba C5 C13 116.1(5) 17_654 . . . ? C3 Ba C5 C13 158.6(6) . . . . ? C3 Ba C5 C13 157.0(4) 17_654 . . . ? C5 Ba C5 C13 -22.2(5) 17_654 . . . ? C4 Ba C5 C13 122.1(6) . . . . ? C4 Ba C5 C13 -163.6(4) 17_654 . . . ? C5 C1 C6 C7 117.0(6) . . . . ? C2 C1 C6 C7 -63.8(7) . . . . ? Ba C1 C6 C7 25.5(6) . . . . ? C9 N1 C7 C6 -66.6(6) . . . . ? C8 N1 C7 C6 176.7(5) . . . . ? Ba N1 C7 C6 53.2(6) . . . . ? C1 C6 C7 N1 -55.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.422 _refine_diff_density_min -1.611 _refine_diff_density_rms 0.150 #===end data_9 _database_code_depnum_ccdc_archive 'CCDC 228238' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(ethoxyethyl-1,2,3,4-tetramethylcyclopentadienyl)barium(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H42 Ba O2' _chemical_formula_sum 'C26 H42 Ba O2' _chemical_formula_weight 523.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ba Ba -0.3244 2.2819 '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 orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 15.202(3) _cell_length_b 22.907(3) _cell_length_c 15.135(3) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 5270.5(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40573 _cell_measurement_theta_min 5.026 _cell_measurement_theta_max 27.632 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.524 _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.67 _exptl_absorpt_process_details 'sadabs (sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38116 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.01 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6006 _reflns_number_gt 3923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 2002)' _computing_cell_refinement 'COLLECT (Nonius, 2002)' _computing_data_reduction 'COLLECT (Nonius, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material 'SHELX97 (Sheldrick, 1997)' _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^)+(0.0341P)^2^+12.9218P] 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 6006 _refine_ls_number_parameters 272 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.0927 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.007 _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 Ba1 Ba 0.240459(14) 0.122727(10) 0.470204(16) 0.03427(10) Uani 1 1 d . . . O2 O 0.3769(3) 0.1664(2) 0.3784(4) 0.0935(14) Uani 1 1 d . . . C4 C 0.1887(3) 0.2322(2) 0.5561(3) 0.0464(11) Uani 1 1 d . . . C18 C 0.2957(3) 0.0582(2) 0.3088(3) 0.0424(11) Uani 1 1 d . . . C23 C 0.3540(4) 0.0956(3) 0.2528(4) 0.0751(17) Uani 1 1 d U . . H23A H 0.3342 0.0934 0.1905 0.090 Uiso 1 1 calc R . . H23B H 0.4150 0.0806 0.2557 0.090 Uiso 1 1 calc R . . C16 C 0.2456(3) -0.0022(2) 0.4173(3) 0.0518(13) Uani 1 1 d . . . C1 C 0.0708(3) 0.1853(2) 0.4975(4) 0.0624(16) Uani 1 1 d . . . C14 C 0.2034(3) 0.0562(2) 0.3037(3) 0.0447(11) Uani 1 1 d . . . C5 C 0.1196(3) 0.1932(2) 0.5769(3) 0.0602(15) Uani 1 1 d . . . C22 C 0.4167(4) 0.0094(3) 0.4065(4) 0.081(2) Uani 1 1 d . . . H22A H 0.4569 0.0351 0.3740 0.122 Uiso 1 1 calc R . . H22B H 0.4307 -0.0314 0.3931 0.122 Uiso 1 1 calc R . . H22C H 0.4232 0.0163 0.4701 0.122 Uiso 1 1 calc R . . C12 C 0.2767(5) 0.0839(4) 0.7136(4) 0.097(2) Uani 1 1 d . . . H12A H 0.2599 0.0472 0.7438 0.117 Uiso 1 1 calc R . . H12B H 0.2689 0.1163 0.7562 0.117 Uiso 1 1 calc R . . C3 C 0.1822(4) 0.24622(19) 0.4681(3) 0.0523(12) Uani 1 1 d . . . C24 C 0.3525(5) 0.1605(3) 0.2837(5) 0.096(2) Uani 1 1 d U . . H24A H 0.3942 0.1834 0.2473 0.115 Uiso 1 1 calc R . . H24B H 0.2929 0.1768 0.2745 0.115 Uiso 1 1 calc R . . C25 C 0.4675(4) 0.1775(3) 0.3961(6) 0.098(2) Uani 1 1 d . . . H25A H 0.4818 0.2183 0.3801 0.117 Uiso 1 1 calc R . . H25B H 0.5043 0.1514 0.3595 0.117 Uiso 1 1 calc R . . C15 C 0.1734(3) 0.0195(2) 0.3707(3) 0.0497(12) Uani 1 1 d . . . O1 O 0.2228(3) 0.0925(2) 0.6446(3) 0.1000(16) Uani 1 1 d . . . C17 C 0.3224(3) 0.0223(2) 0.3789(3) 0.0487(12) Uani 1 1 d . . . C2 C 0.1103(4) 0.2174(2) 0.4323(4) 0.0591(14) Uani 1 1 d . . . C11 C 0.1289(6) 0.0997(5) 0.6657(6) 0.138(4) Uani 1 1 d . . . H11A H 0.1170 0.0834 0.7250 0.165 Uiso 1 1 calc R . . H11B H 0.0932 0.0778 0.6223 0.165 Uiso 1 1 calc R . . C6 C -0.0135(4) 0.1496(4) 0.4876(7) 0.140(4) Uani 1 1 d . . . H6A H -0.0566 0.1720 0.4533 0.210 Uiso 1 1 calc R . . H6B H -0.0377 0.1410 0.5462 0.210 Uiso 1 1 calc R . . H6C H -0.0003 0.1130 0.4569 0.210 Uiso 1 1 calc R . . C19 C 0.1463(4) 0.0846(3) 0.2336(4) 0.0763(18) Uani 1 1 d . . . H19A H 0.1405 0.0581 0.1830 0.114 Uiso 1 1 calc R . . H19B H 0.1735 0.1212 0.2142 0.114 Uiso 1 1 calc R . . H19C H 0.0879 0.0927 0.2582 0.114 Uiso 1 1 calc R . . C20 C 0.0772(4) 0.0023(3) 0.3851(5) 0.087(2) Uani 1 1 d . . . H20A H 0.0388 0.0331 0.3622 0.131 Uiso 1 1 calc R . . H20B H 0.0662 -0.0029 0.4485 0.131 Uiso 1 1 calc R . . H20C H 0.0649 -0.0343 0.3540 0.131 Uiso 1 1 calc R . . C9 C 0.2606(4) 0.2525(4) 0.6186(5) 0.115(3) Uani 1 1 d . . . H9A H 0.3142 0.2298 0.6078 0.173 Uiso 1 1 calc R . . H9B H 0.2415 0.2468 0.6798 0.173 Uiso 1 1 calc R . . H9C H 0.2727 0.2940 0.6084 0.173 Uiso 1 1 calc R . . C8 C 0.2429(5) 0.2886(3) 0.4196(6) 0.113(3) Uani 1 1 d . . . H8A H 0.2126 0.3041 0.3675 0.169 Uiso 1 1 calc R . . H8B H 0.2963 0.2680 0.4010 0.169 Uiso 1 1 calc R . . H8C H 0.2588 0.3207 0.4592 0.169 Uiso 1 1 calc R . . C21 C 0.2436(5) -0.0443(3) 0.4933(5) 0.098(3) Uani 1 1 d . . . H21A H 0.2354 -0.0227 0.5486 0.147 Uiso 1 1 calc R . . H21B H 0.2993 -0.0658 0.4957 0.147 Uiso 1 1 calc R . . H21C H 0.1949 -0.0718 0.4853 0.147 Uiso 1 1 calc R . . C26 C 0.4874(5) 0.1680(4) 0.4886(6) 0.117(3) Uani 1 1 d . . . H26A H 0.4542 0.1959 0.5247 0.176 Uiso 1 1 calc R . . H26B H 0.5505 0.1736 0.4986 0.176 Uiso 1 1 calc R . . H26C H 0.4709 0.1281 0.5052 0.176 Uiso 1 1 calc R . . C7 C 0.0758(6) 0.2260(3) 0.3382(4) 0.117(3) Uani 1 1 d . . . H7A H 0.0631 0.2675 0.3284 0.176 Uiso 1 1 calc R . . H7B H 0.0219 0.2032 0.3301 0.176 Uiso 1 1 calc R . . H7C H 0.1204 0.2130 0.2957 0.176 Uiso 1 1 calc R . . C13 C 0.3676(5) 0.0807(4) 0.6885(5) 0.120(3) Uani 1 1 d . . . H13A H 0.3776 0.0449 0.6543 0.181 Uiso 1 1 calc R . . H13B H 0.4044 0.0801 0.7416 0.181 Uiso 1 1 calc R . . H13C H 0.3827 0.1147 0.6523 0.181 Uiso 1 1 calc R . . C10 C 0.1021(6) 0.1641(4) 0.6639(5) 0.124(3) Uani 1 1 d . . . H10A H 0.0386 0.1671 0.6775 0.149 Uiso 1 1 calc R . . H10B H 0.1346 0.1852 0.7108 0.149 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 Ba1 0.03082(14) 0.03651(14) 0.03549(14) 0.00029(12) -0.00432(11) 0.00140(10) O2 0.058(2) 0.096(3) 0.127(4) 0.009(3) 0.027(3) -0.014(2) C4 0.047(3) 0.052(3) 0.040(3) -0.018(2) 0.000(2) 0.010(2) C18 0.035(2) 0.051(3) 0.042(3) -0.005(2) 0.005(2) 0.000(2) C23 0.057(3) 0.093(4) 0.075(4) 0.010(4) 0.023(3) 0.006(3) C16 0.080(4) 0.039(2) 0.036(3) -0.008(2) -0.001(2) -0.005(2) C1 0.027(2) 0.055(3) 0.105(5) -0.010(3) -0.004(3) 0.011(2) C14 0.036(2) 0.072(3) 0.026(2) -0.009(2) -0.0042(18) 0.006(2) C5 0.058(3) 0.073(4) 0.050(3) 0.017(3) 0.028(3) 0.032(3) C22 0.064(3) 0.077(4) 0.104(5) -0.034(4) -0.042(4) 0.029(3) C12 0.105(6) 0.126(6) 0.061(4) 0.035(4) -0.019(4) -0.001(5) C3 0.077(4) 0.034(2) 0.046(3) -0.005(2) 0.013(3) 0.006(2) C24 0.094(5) 0.110(5) 0.084(5) 0.038(4) 0.018(4) -0.007(4) C25 0.046(3) 0.094(5) 0.154(8) -0.018(5) 0.026(4) -0.031(3) C15 0.048(3) 0.056(3) 0.046(3) -0.016(2) 0.004(2) -0.013(2) O1 0.094(3) 0.133(4) 0.073(3) 0.049(3) 0.008(3) 0.029(3) C17 0.047(3) 0.050(3) 0.049(3) -0.018(2) -0.020(2) 0.013(2) C2 0.076(4) 0.052(3) 0.050(3) -0.003(3) -0.020(3) 0.025(3) C11 0.095(6) 0.179(9) 0.139(8) 0.092(7) 0.045(5) 0.022(6) C6 0.034(3) 0.101(5) 0.284(12) -0.022(7) -0.008(5) -0.003(3) C19 0.067(4) 0.117(5) 0.045(3) -0.003(3) -0.013(3) 0.017(4) C20 0.056(3) 0.104(5) 0.102(5) -0.035(4) 0.024(3) -0.034(3) C9 0.088(5) 0.131(6) 0.126(6) -0.094(6) -0.034(4) 0.026(4) C8 0.173(8) 0.047(3) 0.118(6) 0.012(4) 0.058(6) -0.011(4) C21 0.173(8) 0.043(3) 0.079(4) 0.004(3) 0.003(4) -0.004(4) C26 0.071(5) 0.137(7) 0.143(8) -0.053(6) 0.009(5) -0.044(5) C7 0.163(7) 0.113(6) 0.076(5) -0.011(4) -0.060(5) 0.071(5) C13 0.087(5) 0.162(8) 0.112(6) 0.059(6) -0.007(5) 0.019(5) C10 0.127(6) 0.156(8) 0.090(5) 0.058(5) 0.073(5) 0.069(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ba1 O2 2.689(4) . ? Ba1 O1 2.742(4) . ? Ba1 C5 2.931(4) . ? Ba1 C4 2.933(4) . ? Ba1 C17 2.958(4) . ? Ba1 C3 2.965(4) . ? Ba1 C16 2.973(5) . ? Ba1 C18 2.977(4) . ? Ba1 C1 2.979(4) . ? Ba1 C15 2.983(4) . ? Ba1 C2 2.991(5) . ? Ba1 C14 2.998(4) . ? O2 C25 1.426(7) . ? O2 C24 1.487(8) . ? C4 C3 1.374(7) . ? C4 C5 1.414(7) . ? C4 C9 1.518(7) . ? C18 C17 1.402(6) . ? C18 C14 1.405(6) . ? C18 C23 1.496(7) . ? C23 C24 1.559(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C16 C15 1.395(7) . ? C16 C17 1.420(7) . ? C16 C21 1.500(8) . ? C1 C2 1.369(8) . ? C1 C5 1.424(8) . ? C1 C6 1.527(8) . ? C14 C15 1.395(6) . ? C14 C19 1.517(7) . ? C5 C10 1.501(8) . ? C22 C17 1.522(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C12 O1 1.341(7) . ? C12 C13 1.435(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C3 C2 1.387(7) . ? C3 C8 1.527(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.448(10) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C15 C20 1.531(6) . ? O1 C11 1.472(8) . ? C2 C7 1.531(7) . ? C11 C10 1.530(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ba1 O1 131.80(16) . . ? O2 Ba1 C5 124.24(15) . . ? O1 Ba1 C5 63.12(14) . . ? O2 Ba1 C4 96.75(14) . . ? O1 Ba1 C4 76.30(15) . . ? C5 Ba1 C4 27.90(14) . . ? O2 Ba1 C17 73.96(14) . . ? O1 Ba1 C17 107.11(14) . . ? C5 Ba1 C17 161.74(16) . . ? C4 Ba1 C17 170.09(14) . . ? O2 Ba1 C3 82.51(14) . . ? O1 Ba1 C3 102.84(15) . . ? C5 Ba1 C3 44.99(14) . . ? C4 Ba1 C3 26.93(13) . . ? C17 Ba1 C3 149.64(14) . . ? O2 Ba1 C16 101.49(14) . . ? O1 Ba1 C16 91.05(15) . . ? C5 Ba1 C16 134.05(15) . . ? C4 Ba1 C16 161.76(14) . . ? C17 Ba1 C16 27.70(13) . . ? C3 Ba1 C16 157.47(15) . . ? O2 Ba1 C18 62.85(14) . . ? O1 Ba1 C18 133.79(14) . . ? C5 Ba1 C18 154.51(14) . . ? C4 Ba1 C18 149.83(13) . . ? C17 Ba1 C18 27.33(12) . . ? C3 Ba1 C18 123.34(13) . . ? C16 Ba1 C18 45.03(13) . . ? O2 Ba1 C1 124.05(16) . . ? O1 Ba1 C1 84.48(16) . . ? C5 Ba1 C1 27.87(15) . . ? C4 Ba1 C1 45.15(14) . . ? C17 Ba1 C1 143.44(14) . . ? C3 Ba1 C1 44.25(15) . . ? C16 Ba1 C1 121.55(14) . . ? C18 Ba1 C1 126.65(15) . . ? O2 Ba1 C15 107.34(14) . . ? O1 Ba1 C15 104.59(16) . . ? C5 Ba1 C15 120.06(15) . . ? C4 Ba1 C15 144.12(13) . . ? C17 Ba1 C15 44.89(13) . . ? C3 Ba1 C15 130.48(15) . . ? C16 Ba1 C15 27.09(13) . . ? C18 Ba1 C15 44.62(12) . . ? C1 Ba1 C15 98.96(14) . . ? O2 Ba1 C2 98.11(16) . . ? O1 Ba1 C2 107.66(15) . . ? C5 Ba1 C2 44.90(14) . . ? C4 Ba1 C2 44.57(13) . . ? C17 Ba1 C2 138.81(13) . . ? C3 Ba1 C2 26.94(14) . . ? C16 Ba1 C2 131.58(15) . . ? C18 Ba1 C2 112.91(13) . . ? C1 Ba1 C2 26.51(15) . . ? C15 Ba1 C2 104.60(15) . . ? O2 Ba1 C14 84.26(15) . . ? O1 Ba1 C14 131.48(16) . . ? C5 Ba1 C14 128.71(15) . . ? C4 Ba1 C14 139.19(13) . . ? C17 Ba1 C14 44.88(12) . . ? C3 Ba1 C14 114.82(14) . . ? C16 Ba1 C14 44.72(13) . . ? C18 Ba1 C14 27.21(12) . . ? C1 Ba1 C14 101.44(14) . . ? C15 Ba1 C14 26.98(13) . . ? C2 Ba1 C14 94.75(13) . . ? C25 O2 C24 116.0(6) . . ? C25 O2 Ba1 135.6(5) . . ? C24 O2 Ba1 105.8(3) . . ? C3 C4 C5 108.0(4) . . ? C3 C4 C9 125.7(6) . . ? C5 C4 C9 126.2(6) . . ? C3 C4 Ba1 77.8(3) . . ? C5 C4 Ba1 76.0(3) . . ? C9 C4 Ba1 110.1(3) . . ? C17 C18 C14 108.1(4) . . ? C17 C18 C23 126.4(4) . . ? C14 C18 C23 125.3(5) . . ? C17 C18 Ba1 75.6(3) . . ? C14 C18 Ba1 77.2(2) . . ? C23 C18 Ba1 110.3(3) . . ? C18 C23 C24 111.6(5) . . ? C18 C23 H23A 109.3 . . ? C24 C23 H23A 109.3 . . ? C18 C23 H23B 109.3 . . ? C24 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? C15 C16 C17 107.4(4) . . ? C15 C16 C21 126.9(5) . . ? C17 C16 C21 125.8(5) . . ? C15 C16 Ba1 76.8(3) . . ? C17 C16 Ba1 75.5(3) . . ? C21 C16 Ba1 114.3(3) . . ? C2 C1 C5 108.1(5) . . ? C2 C1 C6 125.8(7) . . ? C5 C1 C6 126.0(7) . . ? C2 C1 Ba1 77.2(3) . . ? C5 C1 Ba1 74.2(2) . . ? C6 C1 Ba1 117.1(4) . . ? C15 C14 C18 107.8(4) . . ? C15 C14 C19 125.4(4) . . ? C18 C14 C19 126.6(5) . . ? C15 C14 Ba1 75.9(2) . . ? C18 C14 Ba1 75.6(3) . . ? C19 C14 Ba1 118.6(3) . . ? C4 C5 C1 106.3(4) . . ? C4 C5 C10 127.4(6) . . ? C1 C5 C10 126.3(6) . . ? C4 C5 Ba1 76.1(2) . . ? C1 C5 Ba1 78.0(3) . . ? C10 C5 Ba1 110.5(4) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C12 C13 112.9(6) . . ? O1 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? O1 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C4 C3 C2 108.9(5) . . ? C4 C3 C8 124.8(6) . . ? C2 C3 C8 126.2(6) . . ? C4 C3 Ba1 75.3(3) . . ? C2 C3 Ba1 77.6(3) . . ? C8 C3 Ba1 115.5(4) . . ? O2 C24 C23 111.9(5) . . ? O2 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? O2 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? O2 C25 C26 110.9(6) . . ? O2 C25 H25A 109.5 . . ? C26 C25 H25A 109.5 . . ? O2 C25 H25B 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C14 C15 C16 109.0(4) . . ? C14 C15 C20 124.8(5) . . ? C16 C15 C20 126.0(5) . . ? C14 C15 Ba1 77.1(3) . . ? C16 C15 Ba1 76.1(3) . . ? C20 C15 Ba1 117.3(3) . . ? C12 O1 C11 116.1(6) . . ? C12 O1 Ba1 136.6(4) . . ? C11 O1 Ba1 105.9(4) . . ? C18 C17 C16 107.7(4) . . ? C18 C17 C22 126.4(5) . . ? C16 C17 C22 125.8(5) . . ? C18 C17 Ba1 77.1(2) . . ? C16 C17 Ba1 76.8(3) . . ? C22 C17 Ba1 114.8(3) . . ? C1 C2 C3 108.6(5) . . ? C1 C2 C7 126.2(6) . . ? C3 C2 C7 124.9(6) . . ? C1 C2 Ba1 76.3(3) . . ? C3 C2 Ba1 75.5(3) . . ? C7 C2 Ba1 120.0(4) . . ? O1 C11 C10 111.3(7) . . ? O1 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? O1 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C5 C10 C11 113.4(6) . . ? C5 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C5 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.990 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.086 #===end