#------------------------------------------------------------------------------ #$Date: 2025-08-20 20:19:29 +0100 (Wed, 20 Aug 2025) $ #$Revision: 301836 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/83/4308323.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_4308323 loop_ _publ_author_name 'Marina A. Petrukhina' 'Colin Henck' 'Bo Li' 'Eric Block' 'Jin Jin' 'Shao-Zhong Zhang' 'Rodolphe Clerac' _publ_section_title ; Spirocyclic Sulfur and Selenium Ligands as Molecular Rigid Rods in Coordination of Transition Metal Centers ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 77 _journal_page_last 84 _journal_paper_doi 10.1021/ic040102g _journal_volume 44 _journal_year 2005 _chemical_formula_moiety ; [(Co (C5 O2 F6 H)2) (O H2)2] ; _chemical_formula_sum 'C10 H6 Co F12 O6' _chemical_formula_weight 509.08 _chemical_melting_point ? _chemical_name_systematic ; bis(hexafluoroacetylacetonato)-cobalt(II) dihydrate ; _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 difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 95.4830(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 21.2490(12) _cell_length_b 8.0736(4) _cell_length_c 9.6680(5) _cell_measurement_reflns_used 5649 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.20 _cell_measurement_theta_min 2.70 _cell_volume 1651.01(15) _computing_cell_refinement 'SMART, SAINT' _computing_data_collection SMART _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXP-93 (Sheldrick, 1993)' _computing_publication_material 'SHELXCIF-93 (Sheldrick, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.951 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measurement_device_type 'Brucker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _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 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0158 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6943 _diffrn_reflns_theta_full 28.24 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_min 1.93 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_number 'none (area dectector data)' _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_T_max 0.9209 _exptl_absorpt_correction_T_min 0.8045 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 996 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.431 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.084 _refine_ls_extinction_coef noref _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 144 _refine_ls_number_reflns 1941 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0311 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0477P)^2^+1.9589P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.0820 _reflns_number_gt 1851 _reflns_number_total 1941 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic040102g_4.cif _cod_data_source_block '[Co(C5O2F6H)2(H2O)2]_(5)' _cod_depositor_comments ; The following automatic conversions were performed: _chemical_melting_point value 'not measured' changed to '?' - value is undefined or not given. Automatic conversion script Id: cif_fix_values 1382 2010-08-28 14:56:29Z saulius ; _cod_database_code 4308323 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 0.5000 0.57300(4) 0.2500 0.01993(11) Uani 1 2 d S . . O1 O 0.53989(6) 0.74361(16) 0.39315(13) 0.0283(3) Uani 1 1 d . . . O2 O 0.58339(6) 0.57881(14) 0.15996(12) 0.0236(3) Uani 1 1 d . . . C1 C 0.59638(8) 0.7892(2) 0.40611(17) 0.0246(3) Uani 1 1 d . . . C2 C 0.64481(8) 0.7458(2) 0.32565(18) 0.0273(3) Uani 1 1 d . . . H2 H 0.6845(11) 0.790(3) 0.350(2) 0.037(6) Uiso 1 1 d . . . C3 C 0.63451(7) 0.6436(2) 0.21055(16) 0.0227(3) Uani 1 1 d . . . C4 C 0.61180(10) 0.9111(2) 0.5276(2) 0.0344(4) Uani 1 1 d . . . F1 F 0.58552(10) 1.05535(17) 0.4981(2) 0.0759(6) Uani 1 1 d . . . F2 F 0.59006(9) 0.8552(2) 0.64167(14) 0.0710(5) Uani 1 1 d . . . F3 F 0.67281(7) 0.9374(2) 0.55744(17) 0.0627(5) Uani 1 1 d . . . C5 C 0.69096(9) 0.5980(2) 0.1303(2) 0.0310(4) Uani 1 1 d . . . F4 F 0.74289(6) 0.6801(2) 0.16975(16) 0.0659(5) Uani 1 1 d . . . F5 F 0.67718(6) 0.6243(2) -0.00505(13) 0.0490(3) Uani 1 1 d . . . F6 F 0.70299(7) 0.43700(18) 0.14268(19) 0.0591(4) Uani 1 1 d . . . O3 O 0.46695(7) 0.38135(17) 0.11818(13) 0.0271(3) Uani 1 1 d . . . H3A H 0.4925(14) 0.324(4) 0.099(3) 0.055(9) Uiso 1 1 d . . . H3B H 0.4443(13) 0.399(3) 0.051(3) 0.048(8) Uiso 1 1 d . . . 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 0.01775(17) 0.02518(18) 0.01660(16) 0.000 0.00038(11) 0.000 O1 0.0266(6) 0.0306(6) 0.0281(6) -0.0079(5) 0.0038(5) -0.0019(5) O2 0.0204(5) 0.0305(6) 0.0198(5) -0.0017(4) 0.0013(4) -0.0030(4) C1 0.0302(8) 0.0200(7) 0.0228(7) 0.0002(6) -0.0019(6) -0.0020(6) C2 0.0244(8) 0.0299(8) 0.0270(8) -0.0009(7) -0.0009(6) -0.0064(6) C3 0.0215(7) 0.0244(7) 0.0219(7) 0.0048(6) 0.0014(6) -0.0017(6) C4 0.0419(11) 0.0285(9) 0.0322(9) -0.0073(7) 0.0006(8) -0.0056(7) F1 0.1095(14) 0.0324(7) 0.0788(12) -0.0225(7) -0.0278(11) 0.0191(8) F2 0.1066(14) 0.0770(11) 0.0320(7) -0.0214(7) 0.0195(8) -0.0429(10) F3 0.0478(8) 0.0776(11) 0.0605(9) -0.0365(8) -0.0056(7) -0.0167(7) C5 0.0237(8) 0.0392(9) 0.0305(9) -0.0007(7) 0.0044(7) -0.0030(7) F4 0.0292(6) 0.1072(13) 0.0641(9) -0.0349(9) 0.0182(6) -0.0291(7) F5 0.0440(7) 0.0755(9) 0.0295(6) 0.0017(6) 0.0144(5) 0.0034(7) F6 0.0493(8) 0.0498(8) 0.0820(11) 0.0123(7) 0.0265(8) 0.0223(6) O3 0.0287(6) 0.0323(6) 0.0197(6) -0.0037(5) -0.0007(5) -0.0025(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 177.37(6) . 2_655 n O2 Co1 O1 87.33(5) . . n O2 Co1 O1 90.93(5) 2_655 . n O2 Co1 O1 90.93(5) . 2_655 n O2 Co1 O1 87.33(5) 2_655 2_655 n O1 Co1 O1 96.84(7) . 2_655 n O2 Co1 O3 90.67(5) . . n O2 Co1 O3 91.28(5) 2_655 . n O1 Co1 O3 173.31(5) . . n O1 Co1 O3 89.58(5) 2_655 . n O2 Co1 O3 91.28(5) . 2_655 n O2 Co1 O3 90.67(5) 2_655 2_655 n O1 Co1 O3 89.58(5) . 2_655 n O1 Co1 O3 173.31(5) 2_655 2_655 n O3 Co1 O3 84.08(8) . 2_655 y C1 O1 Co1 126.10(11) . . n C3 O2 Co1 126.34(11) . . n O1 C1 C2 128.58(15) . . n O1 C1 C4 113.33(15) . . n C2 C1 C4 118.08(16) . . n C3 C2 C1 121.97(15) . . n O2 C3 C2 128.50(16) . . n O2 C3 C5 112.97(14) . . n C2 C3 C5 118.54(15) . . n F1 C4 F2 108.1(2) . . n F1 C4 F3 107.10(18) . . n F2 C4 F3 106.75(19) . . n F1 C4 C1 110.25(17) . . n F2 C4 C1 110.68(15) . . n F3 C4 C1 113.72(17) . . n F4 C5 F6 108.57(18) . . n F4 C5 F5 107.78(16) . . n F6 C5 F5 105.50(17) . . n F4 C5 C3 114.10(16) . . n F6 C5 C3 110.02(15) . . n F5 C5 C3 110.48(15) . . n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.0480(12) . y Co1 O2 2.0480(12) 2_655 n Co1 O1 2.0754(12) . y Co1 O1 2.0754(12) 2_655 n Co1 O3 2.0834(13) . y Co1 O3 2.0834(13) 2_655 n O1 C1 1.250(2) . n O2 C3 1.2615(19) . n C1 C2 1.393(2) . n C1 C4 1.543(2) . n C2 C3 1.386(2) . n C3 C5 1.534(2) . n C4 F1 1.311(2) . n C4 F2 1.316(2) . n C4 F3 1.318(3) . n C5 F4 1.312(2) . n C5 F6 1.328(2) . n C5 F5 1.330(2) . n loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168337005