#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000314.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_4000314 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm020902u _journal_year 2003 _chemical_formula_sum 'C48 H48 Co Li2 N4 O4' _chemical_formula_weight 817.71 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/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 93.043(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 18.372(6) _cell_length_b 10.291(3) _cell_length_c 23.219(7) _cell_measurement_temperature 168(2) _cell_volume 4384(2) _diffrn_ambient_temperature 168(2) _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 0.1592 _diffrn_reflns_av_sigmaI/netI 0.2156 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 22987 _diffrn_reflns_theta_max 23.28 _diffrn_reflns_theta_min 1.76 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type SADABS _exptl_absorpt_process_details ? _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rhombohedra _exptl_crystal_F_000 1716 _exptl_crystal_size_max .14 _exptl_crystal_size_mid ? _exptl_crystal_size_min .19 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 511 _refine_ls_number_reflns 6306 _refine_ls_number_restraints 70 _refine_ls_restrained_S_all 0.849 _refine_ls_R_factor_all 0.1817 _refine_ls_R_factor_gt 0.0654 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1141 _refine_ls_wR_factor_ref 0.1437 _reflns_number_gt 2585 _reflns_number_total 6306 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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_original_sg_symbol_H-M P2(1)/c _cod_database_code 4000314 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.7515(6) 0.3097(10) 0.6882(4) 0.041(3) Uani 1 1 d . . . Li2 Li 0.7386(6) 0.5343(10) 0.4713(5) 0.046(3) Uani 1 1 d . . . Co1 Co 0.74564(5) 0.42373(8) 0.58138(4) 0.0362(3) Uani 1 1 d . . . N1 N 0.7917(3) 0.3991(5) 0.7653(3) 0.0575(17) Uani 1 1 d D . . N2 N 0.7176(3) 0.1191(5) 0.7041(2) 0.0387(15) Uani 1 1 d D . . N3 N 0.8206(3) 0.5329(5) 0.4135(3) 0.0439(15) Uani 1 1 d D . . N4 N 0.6489(3) 0.6299(5) 0.4322(2) 0.0449(16) Uani 1 1 d D . . O1 O 0.8116(2) 0.3034(4) 0.62380(17) 0.0366(11) Uani 1 1 d . . . O2 O 0.6884(2) 0.4375(4) 0.64953(16) 0.0358(11) Uani 1 1 d . . . O3 O 0.7846(2) 0.5799(4) 0.54557(17) 0.0392(11) Uani 1 1 d . . . O4 O 0.7002(2) 0.3776(4) 0.50689(18) 0.0413(12) Uani 1 1 d . . . C1 C 0.8722(4) 0.2577(6) 0.6003(3) 0.0345(18) Uani 1 1 d . . . C2 C 0.9295(4) 0.2112(6) 0.6357(3) 0.0398(18) Uani 1 1 d . . . C3 C 0.9903(4) 0.1651(6) 0.6096(4) 0.053(2) Uani 1 1 d . . . H3 H 1.0297 0.1327 0.6336 0.064 Uiso 1 1 calc R . . C4 C 0.9968(4) 0.1637(7) 0.5510(4) 0.056(2) Uani 1 1 d . . . H4 H 1.0402 0.1332 0.5352 0.068 Uiso 1 1 calc R . . C5 C 0.9394(5) 0.2069(7) 0.5154(3) 0.057(2) Uani 1 1 d . . . H5 H 0.9420 0.2051 0.4746 0.069 Uiso 1 1 calc R . . C6 C 0.8776(4) 0.2530(6) 0.5405(3) 0.0436(19) Uani 1 1 d . . . H6 H 0.8377 0.2824 0.5163 0.052 Uiso 1 1 calc R . . C7 C 0.9259(3) 0.2163(6) 0.7002(3) 0.055(2) Uani 1 1 d . . . H7A H 0.9719 0.1843 0.7183 0.083 Uiso 1 1 calc R . . H7B H 0.8856 0.1617 0.7120 0.083 Uiso 1 1 calc R . . H7C H 0.9179 0.3062 0.7122 0.083 Uiso 1 1 calc R . . C8 C 0.6330(4) 0.5220(6) 0.6521(3) 0.0374(18) Uani 1 1 d . . . C9 C 0.5859(4) 0.5210(6) 0.6972(3) 0.0432(19) Uani 1 1 d . . . C10 C 0.5287(4) 0.6107(7) 0.6973(3) 0.049(2) Uani 1 1 d . . . H10 H 0.4970 0.6098 0.7283 0.059 Uiso 1 1 calc R . . C11 C 0.5169(4) 0.7002(7) 0.6537(3) 0.054(2) Uani 1 1 d . . . H11 H 0.4776 0.7599 0.6548 0.065 Uiso 1 1 calc R . . C12 C 0.5626(4) 0.7025(6) 0.6082(3) 0.052(2) Uani 1 1 d . . . H12 H 0.5545 0.7631 0.5777 0.063 Uiso 1 1 calc R . . C13 C 0.6202(3) 0.6163(6) 0.6075(3) 0.0387(18) Uani 1 1 d . . . H13 H 0.6520 0.6197 0.5766 0.046 Uiso 1 1 calc R . . C14 C 0.5937(3) 0.4230(6) 0.7437(3) 0.055(2) Uani 1 1 d . . . H14A H 0.5906 0.3357 0.7269 0.082 Uiso 1 1 calc R . . H14B H 0.5546 0.4344 0.7704 0.082 Uiso 1 1 calc R . . H14C H 0.6410 0.4339 0.7647 0.082 Uiso 1 1 calc R . . C15 C 0.8280(4) 0.6636(6) 0.5756(3) 0.0363(18) Uani 1 1 d . . . C16 C 0.8343(4) 0.7923(6) 0.5559(3) 0.045(2) Uani 1 1 d . . . C17 C 0.8807(4) 0.8753(7) 0.5865(4) 0.052(2) Uani 1 1 d . . . H17 H 0.8856 0.9613 0.5724 0.062 Uiso 1 1 calc R . . C18 C 0.9203(4) 0.8415(7) 0.6362(4) 0.065(2) Uani 1 1 d . . . H18 H 0.9519 0.9017 0.6560 0.078 Uiso 1 1 calc R . . C19 C 0.9119(4) 0.7131(7) 0.6564(4) 0.069(3) Uani 1 1 d . . . H19 H 0.9371 0.6861 0.6912 0.083 Uiso 1 1 calc R . . C20 C 0.8672(4) 0.6270(7) 0.6258(3) 0.053(2) Uani 1 1 d . . . H20 H 0.8631 0.5404 0.6394 0.064 Uiso 1 1 calc R . . C21 C 0.7893(4) 0.8370(6) 0.5035(3) 0.062(2) Uani 1 1 d . . . H21A H 0.7957 0.9308 0.4984 0.093 Uiso 1 1 calc R . . H21B H 0.7377 0.8181 0.5087 0.093 Uiso 1 1 calc R . . H21C H 0.8051 0.7913 0.4693 0.093 Uiso 1 1 calc R . . C22 C 0.6675(3) 0.2595(6) 0.4985(3) 0.0355(18) Uani 1 1 d . . . C23 C 0.6549(4) 0.2107(7) 0.4445(3) 0.0441(19) Uani 1 1 d . . . C24 C 0.6202(4) 0.0896(7) 0.4372(3) 0.0502(19) Uani 1 1 d . . . H24 H 0.6108 0.0554 0.3996 0.060 Uiso 1 1 calc R . . C25 C 0.5995(4) 0.0201(7) 0.4848(4) 0.057(2) Uani 1 1 d . . . H25 H 0.5762 -0.0618 0.4795 0.069 Uiso 1 1 calc R . . C26 C 0.6124(4) 0.0681(7) 0.5391(3) 0.055(2) Uani 1 1 d . . . H26 H 0.5987 0.0201 0.5717 0.066 Uiso 1 1 calc R . . C27 C 0.6459(4) 0.1881(7) 0.5459(3) 0.052(2) Uani 1 1 d . . . H27 H 0.6544 0.2226 0.5836 0.062 Uiso 1 1 calc R . . C28 C 0.6764(4) 0.2848(6) 0.3915(3) 0.061(2) Uani 1 1 d . . . H28A H 0.6469 0.3640 0.3873 0.091 Uiso 1 1 calc R . . H28B H 0.6680 0.2302 0.3572 0.091 Uiso 1 1 calc R . . H28C H 0.7281 0.3082 0.3958 0.091 Uiso 1 1 calc R . . C29 C 0.8181(5) 0.3419(9) 0.8141(4) 0.098(3) Uiso 1 1 d D . . H29 H 0.8239 0.2504 0.8167 0.117 Uiso 1 1 calc R . . C30 C 0.8375(5) 0.4261(9) 0.8631(4) 0.114(3) Uiso 1 1 d D . . H30 H 0.8554 0.3943 0.8995 0.137 Uiso 1 1 calc R . . C31 C 0.8277(4) 0.5505(9) 0.8518(4) 0.095(3) Uiso 1 1 d D . . H31 H 0.8389 0.6047 0.8842 0.113 Uiso 1 1 calc R . . C32 C 0.8062(5) 0.6150(11) 0.8062(4) 0.134(4) Uiso 1 1 d D . . H32 H 0.8038 0.7069 0.8028 0.160 Uiso 1 1 calc R . . C33 C 0.7873(4) 0.5271(8) 0.7634(4) 0.085(3) Uiso 1 1 d D . . H33 H 0.7687 0.5631 0.7279 0.102 Uiso 1 1 calc R . . C34 C 0.7437(4) 0.0269(6) 0.6709(3) 0.044(2) Uani 1 1 d D . . H34 H 0.7772 0.0513 0.6431 0.053 Uiso 1 1 calc R . . C35 C 0.7247(4) -0.1025(6) 0.6747(3) 0.050(2) Uani 1 1 d D . . H35 H 0.7456 -0.1657 0.6508 0.060 Uiso 1 1 calc R . . C36 C 0.6749(4) -0.1377(6) 0.7138(3) 0.051(2) Uani 1 1 d D . . H36 H 0.6599 -0.2256 0.7167 0.061 Uiso 1 1 calc R . . C37 C 0.6472(4) -0.0447(6) 0.7486(3) 0.0451(19) Uani 1 1 d D . . H37 H 0.6135 -0.0669 0.7766 0.054 Uiso 1 1 calc R . . C38 C 0.6696(4) 0.0824(7) 0.7418(3) 0.0486(19) Uani 1 1 d D . . H38 H 0.6495 0.1473 0.7654 0.058 Uiso 1 1 calc R . . C39 C 0.8891(4) 0.5235(6) 0.4353(3) 0.051(2) Uani 1 1 d D . . H39 H 0.8968 0.5195 0.4761 0.061 Uiso 1 1 calc R . . C40 C 0.9485(4) 0.5191(7) 0.4028(4) 0.066(2) Uani 1 1 d D . . H40 H 0.9959 0.5126 0.4210 0.079 Uiso 1 1 calc R . . C41 C 0.9400(5) 0.5243(7) 0.3437(4) 0.065(2) Uani 1 1 d D . . H41 H 0.9805 0.5201 0.3201 0.078 Uiso 1 1 calc R . . C42 C 0.8706(5) 0.5356(6) 0.3207(3) 0.056(2) Uani 1 1 d D . . H42 H 0.8616 0.5410 0.2801 0.067 Uiso 1 1 calc R . . C43 C 0.8140(4) 0.5391(6) 0.3565(3) 0.052(2) Uani 1 1 d D . . H43 H 0.7662 0.5465 0.3392 0.063 Uiso 1 1 calc R . . C44 C 0.6504(4) 0.7230(6) 0.3924(3) 0.054(2) Uani 1 1 d D . . H44 H 0.6967 0.7554 0.3831 0.065 Uiso 1 1 calc R . . C45 C 0.5897(5) 0.7761(7) 0.3637(3) 0.055(2) Uani 1 1 d D . . H45 H 0.5945 0.8392 0.3342 0.066 Uiso 1 1 calc R . . C46 C 0.5224(5) 0.7351(7) 0.3789(3) 0.066(2) Uani 1 1 d D . . H46 H 0.4791 0.7713 0.3613 0.079 Uiso 1 1 calc R . . C47 C 0.5190(4) 0.6394(7) 0.4208(3) 0.063(2) Uani 1 1 d D . . H47 H 0.4733 0.6085 0.4324 0.076 Uiso 1 1 calc R . . C48 C 0.5826(4) 0.5903(7) 0.4450(3) 0.054(2) Uani 1 1 d D . . H48 H 0.5794 0.5233 0.4729 0.065 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 0.062(9) 0.029(6) 0.033(7) -0.002(5) -0.003(6) -0.009(6) Li2 0.042(8) 0.047(8) 0.050(8) 0.009(6) 0.010(6) -0.005(6) Co1 0.0439(6) 0.0252(5) 0.0397(6) 0.0019(5) 0.0048(4) 0.0006(5) N1 0.058(4) 0.043(4) 0.072(5) -0.003(3) 0.013(3) -0.002(3) N2 0.054(4) 0.028(3) 0.035(4) -0.007(3) 0.008(3) 0.001(3) N3 0.039(4) 0.040(4) 0.053(5) 0.003(3) 0.005(3) -0.003(3) N4 0.051(5) 0.034(4) 0.050(4) 0.012(3) 0.004(3) 0.002(3) O1 0.035(3) 0.030(3) 0.045(3) 0.006(2) 0.005(2) 0.005(2) O2 0.039(3) 0.022(2) 0.047(3) 0.006(2) 0.004(2) 0.008(2) O3 0.046(3) 0.028(2) 0.044(3) 0.004(3) 0.001(2) -0.003(2) O4 0.047(3) 0.027(3) 0.050(3) 0.006(2) 0.006(2) -0.002(2) C1 0.033(5) 0.021(4) 0.049(5) 0.003(4) 0.005(4) -0.007(3) C2 0.035(5) 0.032(4) 0.052(5) 0.002(4) 0.001(4) -0.002(4) C3 0.036(5) 0.051(5) 0.071(6) -0.002(5) -0.005(5) 0.006(4) C4 0.046(6) 0.045(5) 0.079(7) -0.011(5) 0.019(5) 0.003(4) C5 0.061(6) 0.048(5) 0.064(6) -0.009(4) 0.016(5) 0.000(5) C6 0.044(5) 0.032(4) 0.055(6) 0.000(4) 0.003(4) 0.002(4) C7 0.048(5) 0.066(5) 0.050(6) 0.017(4) -0.013(4) 0.004(4) C8 0.037(5) 0.035(4) 0.040(5) -0.009(4) 0.003(4) -0.010(4) C9 0.050(5) 0.028(4) 0.051(5) 0.002(4) 0.000(4) -0.008(4) C10 0.047(5) 0.039(5) 0.061(6) -0.002(4) 0.007(4) -0.001(4) C11 0.043(5) 0.040(5) 0.080(6) -0.009(5) 0.017(5) 0.007(4) C12 0.066(6) 0.034(5) 0.058(5) 0.004(4) 0.014(5) 0.010(4) C13 0.037(5) 0.031(4) 0.048(5) -0.009(4) 0.003(4) 0.005(3) C14 0.058(5) 0.050(5) 0.056(5) 0.004(5) 0.006(4) -0.008(4) C15 0.038(5) 0.035(5) 0.037(5) -0.010(4) 0.013(4) -0.004(4) C16 0.058(5) 0.026(5) 0.053(6) -0.009(4) 0.014(4) -0.007(4) C17 0.055(6) 0.034(5) 0.068(6) -0.001(5) 0.017(5) -0.002(4) C18 0.057(6) 0.042(6) 0.096(7) -0.022(5) -0.007(5) -0.007(4) C19 0.070(6) 0.043(5) 0.091(7) -0.013(5) -0.029(5) 0.007(5) C20 0.063(6) 0.037(5) 0.058(6) 0.001(4) -0.017(5) 0.001(4) C21 0.099(7) 0.034(5) 0.053(6) 0.007(4) 0.006(5) -0.007(4) C22 0.035(5) 0.027(4) 0.046(5) 0.000(4) 0.005(4) 0.006(3) C23 0.039(5) 0.038(5) 0.056(6) -0.003(4) 0.006(4) -0.004(4) C24 0.068(5) 0.052(5) 0.030(5) -0.003(4) -0.004(4) -0.001(5) C25 0.072(6) 0.040(5) 0.059(6) -0.001(5) -0.008(5) -0.009(4) C26 0.072(6) 0.047(5) 0.046(5) 0.015(5) 0.010(4) -0.013(5) C27 0.066(6) 0.047(5) 0.044(5) 0.000(4) 0.008(4) -0.013(4) C28 0.086(6) 0.045(5) 0.053(5) 0.002(4) 0.013(5) -0.009(4) C34 0.052(5) 0.036(5) 0.044(5) -0.003(4) 0.007(4) -0.012(4) C35 0.056(5) 0.028(5) 0.068(6) -0.007(4) 0.023(4) -0.006(4) C36 0.056(6) 0.028(4) 0.068(6) -0.001(4) -0.003(5) -0.011(4) C37 0.060(5) 0.039(5) 0.037(5) 0.007(4) 0.008(4) 0.004(4) C38 0.068(5) 0.033(5) 0.045(5) 0.001(4) 0.015(4) 0.008(4) C39 0.054(6) 0.047(5) 0.053(5) 0.002(4) 0.008(5) -0.007(4) C40 0.047(6) 0.084(6) 0.067(7) -0.010(5) 0.003(5) -0.004(4) C41 0.050(6) 0.065(6) 0.083(7) -0.007(5) 0.030(5) -0.010(5) C42 0.074(6) 0.041(5) 0.054(6) -0.003(4) 0.026(6) -0.003(4) C43 0.063(6) 0.047(5) 0.047(6) 0.011(4) 0.002(5) 0.002(4) C44 0.068(6) 0.038(5) 0.056(6) 0.004(4) 0.014(5) 0.001(4) C45 0.077(7) 0.037(5) 0.050(5) 0.006(4) -0.002(5) 0.015(5) C46 0.066(7) 0.056(6) 0.073(7) -0.012(5) -0.019(5) 0.020(5) C47 0.049(6) 0.055(5) 0.086(7) 0.003(5) 0.000(5) -0.001(4) C48 0.045(5) 0.050(5) 0.067(6) 0.009(4) 0.005(5) 0.005(5)