#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000144.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4000144 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm0111130 _journal_year 2002 _chemical_formula_sum 'C28 H46 Ba O2' _chemical_formula_weight 551.99 _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 129.45(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 22.054(4) _cell_length_b 20.556(4) _cell_length_c 16.087(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 193(2) _cell_measurement_theta_max 7.5 _cell_measurement_theta_min 3.0 _cell_volume 5631.1(19) _diffrn_ambient_temperature 193(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method omega-2theta _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 4258 _diffrn_reflns_theta_max 24.04 _diffrn_reflns_theta_min 2.55 _diffrn_standards_decay_% <2.0 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.430 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8734 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'North etal. (1968). Acta Cryst. A24, 351-359' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 2288 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 4133 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0409 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+17.6983P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1042 _refine_ls_wR_factor_ref 0.1076 _reflns_number_gt 3724 _reflns_number_total 4133 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M C2/c _cod_database_code 4000144 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' 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ba1 Ba 0.225010(15) 0.134195(14) 0.25156(2) 0.03013(12) Uani 1 d . . . C1 C 0.3238(3) 0.0467(3) 0.4418(4) 0.0391(12) Uani 1 d . . . C2 C 0.2497(3) 0.0157(3) 0.3781(4) 0.0404(12) Uani 1 d . . . C3 C 0.1990(3) 0.0544(3) 0.3827(4) 0.0392(12) Uani 1 d . . . C4 C 0.2409(3) 0.1079(3) 0.4494(4) 0.0377(12) Uani 1 d . . . C5 C 0.3188(3) 0.1025(3) 0.4865(4) 0.0390(12) Uani 1 d . . . C6 C 0.3978(3) 0.0228(3) 0.4633(5) 0.0556(16) Uani 1 d . . . H6A H 0.4416 0.0233 0.5409 0.083 Uiso 1 calc R . . H6B H 0.4100 0.0513 0.4268 0.083 Uiso 1 calc R . . H6C H 0.3895 -0.0217 0.4359 0.083 Uiso 1 calc R . . C7 C 0.2282(4) -0.0473(3) 0.3183(5) 0.0601(17) Uani 1 d . . . H7A H 0.2032 -0.0761 0.3373 0.090 Uiso 1 calc R . . H7B H 0.2757 -0.0682 0.3380 0.090 Uiso 1 calc R . . H7C H 0.1917 -0.0389 0.2407 0.090 Uiso 1 calc R . . C8 C 0.1144(3) 0.0367(3) 0.3322(5) 0.0599(17) Uani 1 d . . . H8A H 0.1140 0.0144 0.3857 0.090 Uiso 1 calc R . . H8B H 0.0924 0.0080 0.2704 0.090 Uiso 1 calc R . . H8C H 0.0828 0.0765 0.3083 0.090 Uiso 1 calc R . . C9 C 0.2108(4) 0.1577(3) 0.4838(6) 0.0588(16) Uani 1 d . . . H9A H 0.2354 0.1508 0.5596 0.088 Uiso 1 calc R . . H9B H 0.1537 0.1535 0.4394 0.088 Uiso 1 calc R . . H9C H 0.2237 0.2014 0.4749 0.088 Uiso 1 calc R . . C10 C 0.3857(4) 0.1495(3) 0.5642(5) 0.0564(16) Uani 1 d . . . H10A H 0.4081 0.1390 0.6382 0.085 Uiso 1 calc R . . H10B H 0.3656 0.1942 0.5473 0.085 Uiso 1 calc R . . H10C H 0.4265 0.1455 0.5571 0.085 Uiso 1 calc R . . C11 C 0.0671(3) 0.1984(2) 0.1219(4) 0.0330(11) Uani 1 d . . . C12 C 0.1129(3) 0.2468(2) 0.1229(4) 0.0309(10) Uani 1 d . . . C13 C 0.1312(3) 0.2248(2) 0.0578(4) 0.0323(11) Uani 1 d . . . C14 C 0.0966(3) 0.1637(3) 0.0172(4) 0.0374(12) Uani 1 d . . . C15 C 0.0573(3) 0.1471(2) 0.0579(4) 0.0385(12) Uani 1 d . . . C16 C 0.0311(3) 0.2044(3) 0.1770(5) 0.0515(15) Uani 1 d . . . H16A H -0.0122 0.2357 0.1377 0.077 Uiso 1 calc R . . H16B H 0.0712 0.2195 0.2512 0.077 Uiso 1 calc R . . H16C H 0.0113 0.1619 0.1775 0.077 Uiso 1 calc R . . C17 C 0.1301(3) 0.3129(3) 0.1733(5) 0.0478(14) Uani 1 d . . . H17A H 0.0808 0.3366 0.1388 0.072 Uiso 1 calc R . . H17B H 0.1635 0.3372 0.1636 0.072 Uiso 1 calc R . . H17C H 0.1574 0.3082 0.2504 0.072 Uiso 1 calc R . . C18 C 0.1728(3) 0.2639(3) 0.0284(5) 0.0529(15) Uani 1 d . . . H18A H 0.1440 0.3045 -0.0064 0.079 Uiso 1 calc R . . H18B H 0.1752 0.2388 -0.0211 0.079 Uiso 1 calc R . . H18C H 0.2262 0.2740 0.0937 0.079 Uiso 1 calc R . . C19 C 0.0971(4) 0.1229(4) -0.0611(5) 0.069(2) Uani 1 d . . . H19A H 0.0461 0.1265 -0.1333 0.104 Uiso 1 calc R . . H19B H 0.1072 0.0773 -0.0381 0.104 Uiso 1 calc R . . H19C H 0.1385 0.1386 -0.0624 0.104 Uiso 1 calc R . . C20 C 0.0120(4) 0.0860(3) 0.0340(5) 0.0669(19) Uani 1 d . . . H20A H -0.0231 0.0775 -0.0436 0.100 Uiso 1 calc R . . H20B H -0.0191 0.0908 0.0579 0.100 Uiso 1 calc R . . H20C H 0.0485 0.0495 0.0722 0.100 Uiso 1 calc R . . O1 O 0.3518(2) 0.2134(2) 0.3326(3) 0.0514(10) Uani 1 d . . . C21 C 0.4272(3) 0.1935(3) 0.3662(5) 0.0553(16) Uani 1 d . . . H21A H 0.4253(3) 0.148(2) 0.3447(10) 0.066 Uiso 1 calc R . . H21B H 0.4683(18) 0.1972(3) 0.445(3) 0.066 Uiso 1 calc R . . C22 C 0.4432(3) 0.2396(3) 0.3090(5) 0.0536(16) Uani 1 d . . . H22A H 0.4260(8) 0.2200(9) 0.239(3) 0.064 Uiso 1 calc R . . H22B H 0.501(2) 0.2507(5) 0.356(2) 0.064 Uiso 1 calc R . . C23 C 0.3951(3) 0.2994(3) 0.2875(5) 0.0554(16) Uani 1 d . . . H23A H 0.4288(15) 0.3376(17) 0.3232(16) 0.066 Uiso 1 calc R . . H23B H 0.3564(17) 0.3081(5) 0.210(3) 0.066 Uiso 1 calc R . . C24 C 0.3553(4) 0.2826(3) 0.3337(5) 0.0560(16) Uani 1 d . . . H24A H 0.3827(13) 0.2976(8) 0.400(3) 0.067 Uiso 1 calc R . . H24B H 0.308(2) 0.2995(9) 0.2939(19) 0.067 Uiso 1 calc R . . O2 O 0.2861(2) 0.0671(2) 0.1684(3) 0.0498(10) Uani 1 d . . . C25 C 0.3120(5) 0.0024(4) 0.1745(6) 0.073(2) Uani 1 d . . . H25A H 0.2730(19) -0.0216(12) 0.100(3) 0.088 Uiso 1 calc R . . H25B H 0.3169(5) -0.0244(14) 0.234(3) 0.088 Uiso 1 calc R . . C26 C 0.3924(4) 0.0115(5) 0.2036(6) 0.082(3) Uani 1 d . . . H26A H 0.431(2) 0.0141(5) 0.277(4) 0.099 Uiso 1 calc R . . H26B H 0.4034(8) -0.023(2) 0.1777(15) 0.099 Uiso 1 calc R . . C27 C 0.3848(4) 0.0746(4) 0.1497(6) 0.073(2) Uani 1 d . . . H27A H 0.3838(4) 0.0664(5) 0.086(3) 0.088 Uiso 1 calc R . . H27B H 0.430(2) 0.1056(16) 0.203(3) 0.088 Uiso 1 calc R . . C28 C 0.3070(3) 0.1023(4) 0.1118(5) 0.0576(16) Uani 1 d . . . H28A H 0.3125(4) 0.150(2) 0.1288(8) 0.069 Uiso 1 calc R . . H28B H 0.2655(18) 0.0965(4) 0.032(3) 0.069 Uiso 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 0.02293(17) 0.03887(19) 0.02516(18) 0.00396(12) 0.01367(14) 0.00272(12) C1 0.034(3) 0.052(3) 0.024(2) 0.006(2) 0.015(2) 0.011(2) C2 0.042(3) 0.041(3) 0.028(3) 0.007(2) 0.017(2) 0.003(2) C3 0.033(3) 0.045(3) 0.036(3) 0.014(2) 0.020(2) 0.001(2) C4 0.039(3) 0.039(3) 0.035(3) 0.004(2) 0.023(2) 0.005(2) C5 0.037(3) 0.048(3) 0.026(2) 0.001(2) 0.017(2) -0.004(2) C6 0.046(3) 0.075(4) 0.046(3) 0.017(3) 0.029(3) 0.024(3) C7 0.070(4) 0.047(3) 0.053(4) -0.004(3) 0.035(4) -0.001(3) C8 0.040(3) 0.064(4) 0.069(4) 0.020(3) 0.031(3) -0.003(3) C9 0.069(4) 0.055(4) 0.067(4) 0.002(3) 0.050(4) 0.009(3) C10 0.051(4) 0.071(4) 0.038(3) -0.013(3) 0.024(3) -0.020(3) C11 0.027(2) 0.040(3) 0.036(3) 0.011(2) 0.022(2) 0.008(2) C12 0.022(2) 0.038(3) 0.023(2) 0.003(2) 0.010(2) 0.002(2) C13 0.026(2) 0.043(3) 0.025(2) 0.003(2) 0.014(2) -0.002(2) C14 0.031(3) 0.049(3) 0.022(2) -0.003(2) 0.012(2) 0.006(2) C15 0.026(3) 0.036(3) 0.038(3) 0.006(2) 0.013(2) 0.002(2) C16 0.040(3) 0.073(4) 0.053(3) 0.018(3) 0.035(3) 0.014(3) C17 0.044(3) 0.040(3) 0.043(3) -0.006(2) 0.020(3) -0.002(2) C18 0.039(3) 0.083(4) 0.039(3) 0.014(3) 0.026(3) -0.002(3) C19 0.051(4) 0.092(5) 0.040(3) -0.020(3) 0.017(3) 0.023(4) C20 0.051(4) 0.047(4) 0.062(4) 0.005(3) 0.017(3) -0.010(3) O1 0.041(2) 0.067(3) 0.046(2) -0.0092(19) 0.0278(19) -0.017(2) C21 0.035(3) 0.069(4) 0.041(3) -0.006(3) 0.014(3) 0.003(3) C22 0.038(3) 0.075(4) 0.051(3) -0.018(3) 0.030(3) -0.020(3) C23 0.041(3) 0.070(4) 0.046(3) -0.002(3) 0.023(3) -0.015(3) C24 0.039(3) 0.069(4) 0.053(4) -0.011(3) 0.026(3) -0.008(3) O2 0.043(2) 0.066(3) 0.042(2) -0.0062(19) 0.0272(19) 0.0053(19) C25 0.088(5) 0.068(5) 0.051(4) -0.008(3) 0.038(4) 0.014(4) C26 0.056(4) 0.130(8) 0.048(4) -0.008(4) 0.028(4) 0.039(5) C27 0.044(4) 0.106(6) 0.070(4) -0.023(4) 0.036(4) 0.002(4) C28 0.043(3) 0.089(5) 0.050(3) -0.008(3) 0.033(3) -0.001(3)