#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000488.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_4000488 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_sum 'C15 H16 Co N3 O8 V2' _chemical_formula_weight 527.12 _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 106.5390(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 30.4457(13) _cell_length_b 11.3540(5) _cell_length_c 11.5836(5) _cell_measurement_reflns_used 6444 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.3 _cell_measurement_theta_min 2.5 _cell_volume 3838.6(3) _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '20s frmes at 0.3 deg omega increments'' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 18787 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.857 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.803 _exptl_absorpt_correction_type none _exptl_absorpt_process_details 'computed via SADABS' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.824 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description lath _exptl_crystal_F_000 2112 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _refine_ls_extinction_coef none _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4544 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.163 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0404 _refine_ls_shift/su_max 0.098 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.055P)^2^+25.0P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1232 _refine_ls_wR_factor_ref 0.1259 _reflns_number_gt 4091 _reflns_number_total 4544 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M C2/c _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_database_code 4000488 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 0.2500 0.0000 0.00962(14) Uani 1 2 d S . . Co2 Co 0.5000 0.0000 0.5000 0.01422(15) Uani 1 2 d S . . V1 V 0.355188(17) 0.09031(5) 0.06062(4) 0.01183(13) Uani 1 1 d . . . V2 V 0.392386(17) -0.08915(4) 0.31860(4) 0.01123(13) Uani 1 1 d . . . O1 O 0.29969(7) 0.1266(2) 0.02713(19) 0.0141(4) Uani 1 1 d . . . O2 O 0.36697(9) -0.0184(2) 0.1765(2) 0.0240(5) Uani 1 1 d . . . O3 O 0.38764(10) 0.2043(3) 0.1051(2) 0.0293(6) Uani 1 1 d . . . O4 O 0.38123(11) -0.2284(2) 0.3029(2) 0.0282(6) Uani 1 1 d . . . O5 O 0.36663(8) -0.0306(2) 0.4284(2) 0.0189(5) Uani 1 1 d . . . O6 O 0.44908(8) -0.0709(2) 0.3629(2) 0.0223(5) Uani 1 1 d . . . O7 O 0.52687(9) 0.0836(3) 0.3680(3) 0.0349(7) Uani 1 1 d . . . N1 N 0.30004(9) 0.3878(2) -0.0020(2) 0.0128(5) Uani 1 1 d . . . N2 N 0.26095(9) 0.2686(2) 0.2006(2) 0.0123(5) Uani 1 1 d . . . N3 N 0.45737(9) 0.1509(3) 0.4941(3) 0.0173(5) Uani 1 1 d . . . C1 C 0.30818(11) 0.4767(3) 0.0784(3) 0.0168(6) Uani 1 1 d . . . H1 H 0.2919 0.4784 0.1352 0.020 Uiso 1 1 calc R . . C2 C 0.33958(12) 0.5659(3) 0.0806(3) 0.0184(6) Uani 1 1 d . . . H2 H 0.3444 0.6248 0.1387 0.022 Uiso 1 1 calc R . . C3 C 0.36392(11) 0.5665(3) -0.0052(3) 0.0157(6) Uani 1 1 d . . . C4 C 0.35580(12) 0.4739(3) -0.0875(3) 0.0182(6) Uani 1 1 d . . . H4 H 0.3714 0.4700 -0.1458 0.022 Uiso 1 1 calc R . . C5 C 0.32428(11) 0.3876(3) -0.0818(3) 0.0179(6) Uani 1 1 d . . . H5 H 0.3197 0.3259 -0.1367 0.021 Uiso 1 1 calc R . . C6 C 0.23717(10) 0.3482(3) 0.2441(3) 0.0133(6) Uani 1 1 d . . . H6 H 0.2229 0.4091 0.1935 0.016 Uiso 1 1 calc R . . C7 C 0.23253(10) 0.3454(3) 0.3600(3) 0.0145(6) Uani 1 1 d . . . H7 H 0.2158 0.4035 0.3852 0.017 Uiso 1 1 calc R . . C8 C 0.25309(11) 0.2549(3) 0.4384(3) 0.0136(6) Uani 1 1 d . . . C9 C 0.27941(12) 0.1755(3) 0.3951(3) 0.0207(7) Uani 1 1 d . . . H9 H 0.2951 0.1157 0.4449 0.025 Uiso 1 1 calc R . . C10 C 0.28255(12) 0.1848(3) 0.2780(3) 0.0174(6) Uani 1 1 d . . . H10 H 0.3005 0.1303 0.2520 0.021 Uiso 1 1 calc R . . C11 C 0.43306(11) 0.2014(3) 0.3914(3) 0.0187(6) Uani 1 1 d . . . H11 H 0.4367 0.1728 0.3194 0.022 Uiso 1 1 calc R . . C12 C 0.40277(11) 0.2941(3) 0.3861(3) 0.0185(6) Uani 1 1 d . . . H12 H 0.3867 0.3262 0.3123 0.022 Uiso 1 1 calc R . . C13 C 0.39690(11) 0.3382(3) 0.4929(3) 0.0173(6) Uani 1 1 d . . . C14 C 0.42269(15) 0.2866(4) 0.5995(3) 0.0328(9) Uani 1 1 d . . . H14 H 0.4206 0.3149 0.6731 0.039 Uiso 1 1 calc R . . C15 C 0.45144(14) 0.1933(4) 0.5961(3) 0.0317(9) Uani 1 1 d . . . H15 H 0.4674 0.1582 0.6684 0.038 Uiso 1 1 calc R . . O11 O 0.5000 0.519(3) 0.7500 0.092(3) Uiso 0.310(17) 2 d SP . . O12 O 0.5031(9) 0.498(2) 0.659(3) 0.092(3) Uiso 0.233(10) 1 d P . . O13 O 0.4794(5) 0.4192(13) -0.0297(14) 0.092(3) Uiso 0.395(10) 1 d P . . O14 O 0.4650(9) 0.319(2) 0.110(2) 0.092(3) Uiso 0.236(10) 1 d P . . 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 Co1 0.0105(3) 0.0105(3) 0.0087(3) 0.00056(19) 0.0042(2) 0.00086(19) Co2 0.0096(3) 0.0194(3) 0.0128(3) 0.0014(2) 0.0018(2) 0.0038(2) V1 0.0101(2) 0.0171(3) 0.0084(2) 0.00111(18) 0.00284(18) -0.00051(18) V2 0.0116(2) 0.0131(2) 0.0087(2) 0.00187(17) 0.00242(18) 0.00026(18) O1 0.0140(10) 0.0174(11) 0.0117(10) 0.0023(8) 0.0046(8) 0.0046(8) O2 0.0226(12) 0.0327(14) 0.0162(11) 0.0097(10) 0.0049(10) 0.0093(11) O3 0.0331(14) 0.0340(15) 0.0194(12) -0.0042(11) 0.0052(11) -0.0189(12) O4 0.0449(16) 0.0190(12) 0.0244(13) -0.0026(10) 0.0159(12) -0.0100(11) O5 0.0210(11) 0.0227(12) 0.0163(11) -0.0006(9) 0.0106(9) -0.0028(9) O6 0.0124(10) 0.0306(13) 0.0214(12) -0.0065(10) 0.0008(9) 0.0032(10) O7 0.0171(12) 0.060(2) 0.0261(14) 0.0195(13) 0.0038(11) -0.0046(12) N1 0.0132(12) 0.0125(12) 0.0135(12) 0.0003(9) 0.0049(10) 0.0005(9) N2 0.0132(11) 0.0146(12) 0.0098(11) 0.0000(9) 0.0045(9) -0.0018(10) N3 0.0144(12) 0.0208(14) 0.0162(13) 0.0010(10) 0.0035(10) 0.0040(10) C1 0.0182(15) 0.0181(15) 0.0167(14) -0.0025(12) 0.0092(12) -0.0032(12) C2 0.0216(16) 0.0182(15) 0.0179(15) -0.0055(12) 0.0095(13) -0.0051(13) C3 0.0157(14) 0.0158(14) 0.0161(14) -0.0009(12) 0.0052(12) -0.0025(12) C4 0.0211(15) 0.0191(15) 0.0184(15) -0.0040(12) 0.0121(13) -0.0051(13) C5 0.0207(15) 0.0163(15) 0.0195(15) -0.0039(12) 0.0105(13) -0.0029(12) C6 0.0143(13) 0.0147(14) 0.0104(13) 0.0011(11) 0.0028(11) 0.0025(11) C7 0.0147(13) 0.0176(14) 0.0118(14) -0.0008(11) 0.0049(11) 0.0041(12) C8 0.0158(14) 0.0167(14) 0.0090(13) 0.0008(11) 0.0048(11) 0.0015(11) C9 0.0290(17) 0.0215(16) 0.0143(15) 0.0073(12) 0.0105(13) 0.0123(14) C10 0.0227(15) 0.0177(15) 0.0148(14) 0.0020(12) 0.0104(12) 0.0080(12) C11 0.0201(15) 0.0217(16) 0.0134(14) -0.0014(12) 0.0033(12) 0.0062(13) C12 0.0198(15) 0.0200(15) 0.0143(14) 0.0015(12) 0.0023(12) 0.0062(13) C13 0.0181(14) 0.0182(15) 0.0182(15) 0.0019(12) 0.0093(12) 0.0032(12) C14 0.040(2) 0.045(2) 0.0153(16) 0.0044(16) 0.0104(15) 0.0240(19) C15 0.035(2) 0.044(2) 0.0164(16) 0.0069(16) 0.0065(15) 0.0240(18) _journal_paper_doi 10.1021/cm049071d