#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000313.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_4000313 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'C56 H84 Co Li2 O6' _chemical_formula_weight 926.04 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.1013(13) _cell_length_b 16.7999(13) _cell_length_c 19.3768(15) _cell_measurement_reflns_used ? _cell_measurement_temperature 168(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 5567.0(7) _diffrn_ambient_temperature 168(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _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 0.0866 _diffrn_reflns_av_sigmaI/netI 0.0933 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 35577 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 1.70 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type SADABS _exptl_absorpt_process_details ? _exptl_crystal_colour blue-green _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description octahedron _exptl_crystal_F_000 2004 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.5mm _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 302 _refine_ls_number_reflns 6683 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.877 _refine_ls_R_factor_all 0.1420 _refine_ls_R_factor_gt 0.0514 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1195 _refine_ls_wR_factor_ref 0.1456 _reflns_number_gt 3005 _reflns_number_total 6683 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4000313 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' 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 Li1 Li 0.1582(3) 0.2630(3) 0.2731(3) 0.0657(14) Uani 1 1 d . . . Co1 Co 0.0000 0.26369(3) 0.2500 0.03803(16) Uani 1 2 d S . . O1 O 0.09512(10) 0.30053(11) 0.20436(9) 0.0492(5) Uani 1 1 d . . . O2 O 0.07405(9) 0.22575(10) 0.31974(9) 0.0455(5) Uani 1 1 d . . . O3 O 0.26650(12) 0.26339(15) 0.28390(13) 0.0828(7) Uani 1 1 d . . . C1 C 0.12325(14) 0.33122(17) 0.14468(14) 0.0443(7) Uani 1 1 d . . . C2 C 0.15094(15) 0.28021(17) 0.09262(15) 0.0498(7) Uani 1 1 d . . . C3 C 0.18899(17) 0.3145(2) 0.03645(16) 0.0633(9) Uani 1 1 d . . . H3 H 0.2098 0.2808 0.0016 0.076 Uiso 1 1 calc R . . C4 C 0.19747(17) 0.3956(2) 0.02970(17) 0.0690(9) Uani 1 1 d . . . H4 H 0.2243 0.4174 -0.0089 0.083 Uiso 1 1 calc R . . C5 C 0.16642(16) 0.4451(2) 0.07987(16) 0.0615(8) Uani 1 1 d . . . H5 H 0.1712 0.5012 0.0748 0.074 Uiso 1 1 calc R . . C6 C 0.12853(14) 0.41453(17) 0.13738(14) 0.0470(7) Uani 1 1 d . . . C7 C 0.09586(17) 0.46770(17) 0.19329(15) 0.0554(8) Uani 1 1 d . . . H7 H 0.0498 0.4395 0.2136 0.066 Uiso 1 1 calc R . . C8 C 0.1539(2) 0.4808(2) 0.25124(17) 0.0802(10) Uani 1 1 d . . . H8A H 0.1709 0.4293 0.2695 0.120 Uiso 1 1 calc R . . H8B H 0.1290 0.5117 0.2881 0.120 Uiso 1 1 calc R . . H8C H 0.1992 0.5101 0.2336 0.120 Uiso 1 1 calc R . . C9 C 0.0666(2) 0.54845(19) 0.16687(17) 0.0786(10) Uani 1 1 d . . . H9A H 0.1105 0.5783 0.1471 0.118 Uiso 1 1 calc R . . H9B H 0.0440 0.5786 0.2053 0.118 Uiso 1 1 calc R . . H9C H 0.0267 0.5400 0.1313 0.118 Uiso 1 1 calc R . . C10 C 0.14218(16) 0.19077(18) 0.09902(15) 0.0566(8) Uani 1 1 d . . . H10 H 0.0977 0.1803 0.1313 0.068 Uiso 1 1 calc R . . C11 C 0.12305(18) 0.1502(2) 0.03085(17) 0.0744(10) Uani 1 1 d . . . H11A H 0.0785 0.1771 0.0091 0.112 Uiso 1 1 calc R . . H11B H 0.1098 0.0944 0.0393 0.112 Uiso 1 1 calc R . . H11C H 0.1685 0.1532 0.0002 0.112 Uiso 1 1 calc R . . C12 C 0.21496(19) 0.1528(2) 0.13022(17) 0.0770(10) Uani 1 1 d . . . H12A H 0.2604 0.1648 0.1012 0.116 Uiso 1 1 calc R . . H12B H 0.2078 0.0950 0.1329 0.116 Uiso 1 1 calc R . . H12C H 0.2235 0.1742 0.1767 0.116 Uiso 1 1 calc R . . C13 C 0.07443(14) 0.20002(17) 0.38577(15) 0.0465(7) Uani 1 1 d . . . C14 C 0.08115(15) 0.25489(18) 0.44012(15) 0.0530(8) Uani 1 1 d . . . C15 C 0.08983(18) 0.2256(2) 0.50680(17) 0.0751(10) Uani 1 1 d . . . H15 H 0.0956 0.2622 0.5439 0.090 Uiso 1 1 calc R . . C16 C 0.0903(2) 0.1461(3) 0.5205(2) 0.0887(13) Uani 1 1 d . . . H16 H 0.0970 0.1280 0.5665 0.106 Uiso 1 1 calc R . . C17 C 0.08096(18) 0.0916(2) 0.4675(2) 0.0785(11) Uani 1 1 d . . . H17 H 0.0805 0.0362 0.4775 0.094 Uiso 1 1 calc R . . C18 C 0.07229(16) 0.11754(18) 0.39940(17) 0.0606(8) Uani 1 1 d . . . C19 C 0.0625(2) 0.06045(18) 0.33973(19) 0.0766(10) Uani 1 1 d . . . H19 H 0.0329 0.0897 0.3032 0.092 Uiso 1 1 calc R . . C20 C 0.0148(3) -0.0138(2) 0.3570(2) 0.1151(15) Uani 1 1 d . . . H20A H 0.0428 -0.0457 0.3914 0.173 Uiso 1 1 calc R . . H20B H 0.0071 -0.0455 0.3150 0.173 Uiso 1 1 calc R . . H20C H -0.0362 0.0021 0.3755 0.173 Uiso 1 1 calc R . . C21 C 0.1411(3) 0.0378(3) 0.3082(3) 0.149(2) Uani 1 1 d . . . H21A H 0.1702 0.0863 0.2966 0.224 Uiso 1 1 calc R . . H21B H 0.1324 0.0065 0.2662 0.224 Uiso 1 1 calc R . . H21C H 0.1711 0.0063 0.3414 0.224 Uiso 1 1 calc R . . C22 C 0.08178(17) 0.34312(18) 0.42609(16) 0.0590(8) Uani 1 1 d . . . H22 H 0.0588 0.3517 0.3792 0.071 Uiso 1 1 calc R . . C23 C 0.0325(2) 0.3907(2) 0.47802(18) 0.0905(12) Uani 1 1 d . . . H23A H -0.0207 0.3692 0.4792 0.136 Uiso 1 1 calc R . . H23B H 0.0308 0.4467 0.4639 0.136 Uiso 1 1 calc R . . H23C H 0.0560 0.3866 0.5240 0.136 Uiso 1 1 calc R . . C24 C 0.16636(18) 0.3753(2) 0.42483(17) 0.0751(10) Uani 1 1 d . . . H24A H 0.1903 0.3680 0.4703 0.113 Uiso 1 1 calc R . . H24B H 0.1657 0.4321 0.4132 0.113 Uiso 1 1 calc R . . H24C H 0.1968 0.3463 0.3901 0.113 Uiso 1 1 calc R . . C25 C 0.3106(3) 0.2172(3) 0.3294(3) 0.144(2) Uani 1 1 d . . . H25A H 0.3048 0.1600 0.3183 0.173 Uiso 1 1 calc R . . H25B H 0.2932 0.2261 0.3775 0.173 Uiso 1 1 calc R . . C26 C 0.3952(4) 0.2430(4) 0.3205(4) 0.195(4) Uani 1 1 d . . . H26A H 0.4103 0.2838 0.3549 0.234 Uiso 1 1 calc R . . H26B H 0.4316 0.1973 0.3237 0.234 Uiso 1 1 calc R . . C27 C 0.3928(3) 0.2766(4) 0.2490(5) 0.208(4) Uani 1 1 d . . . H27A H 0.4341 0.3173 0.2432 0.249 Uiso 1 1 calc R . . H27B H 0.4014 0.2339 0.2146 0.249 Uiso 1 1 calc R . . C28 C 0.3163(2) 0.3121(3) 0.2395(3) 0.1279(18) Uani 1 1 d . . . H28A H 0.2994 0.3088 0.1907 0.153 Uiso 1 1 calc R . . H28B H 0.3159 0.3685 0.2543 0.153 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.045(3) 0.087(4) 0.066(3) 0.011(3) 0.003(2) -0.007(3) Co1 0.0376(3) 0.0350(3) 0.0415(3) 0.000 0.0044(3) 0.000 O1 0.0461(11) 0.0570(12) 0.0447(11) 0.0100(9) 0.0030(9) -0.0105(9) O2 0.0439(10) 0.0470(11) 0.0456(11) 0.0078(9) 0.0042(9) 0.0028(8) O3 0.0436(13) 0.120(2) 0.0845(16) -0.0161(15) 0.0021(12) -0.0046(13) C1 0.0306(14) 0.0571(19) 0.0452(17) 0.0104(14) -0.0001(12) -0.0081(12) C2 0.0402(16) 0.060(2) 0.0493(18) 0.0044(15) 0.0038(14) -0.0021(13) C3 0.0574(19) 0.075(2) 0.058(2) 0.0035(17) 0.0152(16) 0.0046(16) C4 0.064(2) 0.077(3) 0.066(2) 0.0180(19) 0.0232(17) -0.0023(17) C5 0.0552(18) 0.061(2) 0.068(2) 0.0161(17) 0.0066(17) -0.0060(15) C6 0.0387(15) 0.0537(19) 0.0486(17) 0.0101(14) 0.0005(13) -0.0049(13) C7 0.0570(18) 0.0537(19) 0.0555(19) 0.0083(15) 0.0035(16) -0.0060(14) C8 0.098(3) 0.070(2) 0.072(2) -0.002(2) -0.015(2) 0.0028(19) C9 0.089(3) 0.066(2) 0.081(2) 0.0076(19) 0.014(2) 0.0113(18) C10 0.0511(18) 0.059(2) 0.060(2) -0.0038(16) 0.0105(15) -0.0004(15) C11 0.061(2) 0.086(3) 0.077(2) -0.014(2) 0.0031(18) -0.0029(17) C12 0.083(2) 0.068(2) 0.080(2) -0.0002(19) -0.001(2) 0.0102(18) C13 0.0341(14) 0.0547(18) 0.0508(18) 0.0139(15) 0.0016(13) 0.0082(12) C14 0.0405(16) 0.071(2) 0.0479(18) 0.0073(16) -0.0072(13) 0.0039(14) C15 0.064(2) 0.109(3) 0.052(2) 0.013(2) -0.0128(17) -0.013(2) C16 0.068(2) 0.119(4) 0.078(3) 0.050(3) -0.014(2) -0.007(2) C17 0.063(2) 0.069(3) 0.103(3) 0.045(2) 0.012(2) 0.0084(18) C18 0.0489(17) 0.057(2) 0.075(2) 0.0259(18) 0.0155(16) 0.0082(15) C19 0.085(2) 0.045(2) 0.100(3) 0.0077(19) 0.037(2) 0.0052(17) C20 0.138(4) 0.066(3) 0.141(4) -0.002(2) 0.043(3) -0.028(2) C21 0.129(4) 0.094(3) 0.224(6) -0.037(4) 0.091(4) 0.007(3) C22 0.0609(19) 0.065(2) 0.0509(18) -0.0098(16) -0.0131(15) 0.0064(16) C23 0.077(2) 0.107(3) 0.088(3) -0.033(2) -0.017(2) 0.022(2) C24 0.076(2) 0.066(2) 0.083(2) -0.0045(19) -0.010(2) -0.0069(17) C25 0.092(3) 0.204(6) 0.136(4) -0.037(4) -0.050(3) 0.065(3) C26 0.099(4) 0.208(8) 0.278(10) -0.056(6) -0.110(6) 0.043(4) C27 0.043(3) 0.141(6) 0.440(15) -0.064(7) 0.004(6) -0.004(3) C28 0.067(3) 0.116(4) 0.201(5) -0.024(4) 0.035(3) -0.037(2) _journal_paper_doi 10.1021/cm020902u