#------------------------------------------------------------------------------ #$Date: 2016-03-20 23:21:50 +0000 (Sun, 20 Mar 2016) $ #$Revision: 178377 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/04/4000489.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_4000489 _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/cm049071d _journal_year 2004 _chemical_formula_sum 'C10 H8 Co N2 O6 V2' _chemical_formula_weight 412.99 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 87.0170(10) _cell_angle_beta 75.9610(10) _cell_angle_gamma 75.1740(10) _cell_formula_units_Z 2 _cell_length_a 8.1517(4) _cell_length_b 8.5794(4) _cell_length_c 10.1233(5) _cell_measurement_reflns_used 5773 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.21 _cell_measurement_theta_min 2.46 _cell_volume 663.94(6) _diffrn_ambient_temperature 173(2) _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '25s frames 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 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6894 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_theta_min 2.07 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count n/a _diffrn_standards_interval_time n/a _diffrn_standards_number n/a _exptl_absorpt_coefficient_mu 2.640 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'computed via SADABS' _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 406 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _refine_ls_extinction_coef n/a _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 3068 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0242 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.035P)^2^+0.65P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.0669 _reflns_number_gt 2919 _reflns_number_total 3068 _reflns_threshold_expression >2sigma(I) _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'multi-scan ' changed to 'multi-scan' 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 The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'none' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 4000489 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -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 Co1 Co 0.84373(3) 0.83910(3) 0.44210(2) 0.01105(8) Uani 1 1 d . . . V1 V 1.23116(4) 0.72646(4) 0.53016(3) 0.01209(8) Uani 1 1 d . . . V2 V 0.62618(4) 0.58995(4) 0.30192(3) 0.01119(8) Uani 1 1 d . . . O1 O 1.04046(18) 0.70562(18) 0.51304(15) 0.0191(3) Uani 1 1 d . . . O2 O 1.21782(19) 0.92141(16) 0.54741(14) 0.0191(3) Uani 1 1 d . . . O3 O 0.72873(18) 0.69764(17) 0.37047(14) 0.0181(3) Uani 1 1 d . . . O4 O 0.39509(18) 0.64362(17) 0.38456(15) 0.0190(3) Uani 1 1 d . . . O5 O 0.6509(2) 0.62957(18) 0.14134(14) 0.0213(3) Uani 1 1 d . . . O6 O 0.71825(18) 0.37755(16) 0.32221(14) 0.0178(3) Uani 1 1 d . . . N1 N 0.6668(2) 0.83587(19) 0.63407(16) 0.0142(3) Uani 1 1 d . . . N2 N 0.0206(2) 0.8458(2) 1.24873(16) 0.0160(3) Uani 1 1 d . . . C1 C 0.6723(3) 0.7027(2) 0.7109(2) 0.0171(4) Uani 1 1 d . . . H1A H 0.7613 0.6107 0.6812 0.021 Uiso 1 1 calc R . . C2 C 0.5507(3) 0.6967(2) 0.8327(2) 0.0173(4) Uani 1 1 d . . . H2A H 0.5585 0.6022 0.8828 0.021 Uiso 1 1 calc R . . C3 C 0.4169(2) 0.8336(2) 0.87903(19) 0.0146(3) Uani 1 1 d . . . C4 C 0.4117(3) 0.9714(2) 0.7998(2) 0.0185(4) Uani 1 1 d . . . H4A H 0.3250 1.0654 0.8274 0.022 Uiso 1 1 calc R . . C5 C 0.5374(3) 0.9668(2) 0.6794(2) 0.0178(4) Uani 1 1 d . . . H5A H 0.5318 1.0596 0.6271 0.021 Uiso 1 1 calc R . . C6 C 0.2810(2) 0.8356(2) 1.00718(19) 0.0154(4) Uani 1 1 d . . . C7 C 0.2116(3) 0.7037(2) 1.0483(2) 0.0204(4) Uani 1 1 d . . . H7A H 0.2509 0.6096 0.9959 0.025 Uiso 1 1 calc R . . C8 C 0.0833(3) 0.7140(2) 1.1680(2) 0.0206(4) Uani 1 1 d . . . H8A H 0.0381 0.6250 1.1938 0.025 Uiso 1 1 calc R . . C9 C 0.0877(3) 0.9729(3) 1.2080(2) 0.0234(4) Uani 1 1 d . . . H9A H 0.0458 1.0656 1.2621 0.028 Uiso 1 1 calc R . . C10 C 0.2152(3) 0.9734(3) 1.0901(2) 0.0230(4) Uani 1 1 d . . . H10A H 0.2570 1.0646 1.0661 0.028 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 Co1 0.00941(13) 0.01135(13) 0.01112(13) -0.00096(9) 0.00019(9) -0.00264(9) V1 0.00859(15) 0.01101(15) 0.01449(16) 0.00008(11) -0.00017(11) -0.00102(11) V2 0.01008(15) 0.01181(15) 0.01044(15) -0.00118(11) -0.00053(11) -0.00208(11) O1 0.0111(6) 0.0249(7) 0.0203(7) 0.0041(6) -0.0025(5) -0.0044(5) O2 0.0205(7) 0.0131(6) 0.0184(7) -0.0005(5) 0.0042(6) -0.0030(5) O3 0.0160(7) 0.0187(7) 0.0197(7) -0.0036(5) -0.0025(6) -0.0057(5) O4 0.0125(6) 0.0200(7) 0.0219(7) -0.0057(6) 0.0010(5) -0.0029(5) O5 0.0272(8) 0.0205(7) 0.0135(7) 0.0002(5) -0.0031(6) -0.0031(6) O6 0.0195(7) 0.0140(6) 0.0194(7) -0.0005(5) -0.0067(6) -0.0013(5) N1 0.0121(7) 0.0153(7) 0.0132(7) -0.0008(6) 0.0010(6) -0.0038(6) N2 0.0142(7) 0.0185(8) 0.0130(7) -0.0008(6) 0.0013(6) -0.0041(6) C1 0.0147(9) 0.0143(9) 0.0186(9) -0.0011(7) 0.0011(7) -0.0016(7) C2 0.0174(9) 0.0151(9) 0.0168(9) 0.0020(7) 0.0004(7) -0.0042(7) C3 0.0128(8) 0.0182(9) 0.0123(8) -0.0020(7) 0.0001(7) -0.0056(7) C4 0.0154(9) 0.0163(9) 0.0184(9) -0.0014(7) 0.0030(7) -0.0008(7) C5 0.0152(9) 0.0164(9) 0.0173(9) 0.0026(7) 0.0019(7) -0.0022(7) C6 0.0124(8) 0.0195(9) 0.0121(8) -0.0005(7) 0.0012(7) -0.0036(7) C7 0.0224(10) 0.0155(9) 0.0184(9) -0.0034(7) 0.0049(8) -0.0043(8) C8 0.0204(10) 0.0168(9) 0.0202(10) -0.0005(7) 0.0045(8) -0.0053(7) C9 0.0243(10) 0.0227(10) 0.0203(10) -0.0095(8) 0.0073(8) -0.0106(8) C10 0.0249(10) 0.0213(10) 0.0211(10) -0.0059(8) 0.0069(8) -0.0133(8)