#------------------------------------------------------------------------------ #$Date: 2016-03-23 00:49:28 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179130 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/30/92/4309273.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_4309273 loop_ _publ_author_name 'Fiona H. Fry' 'Brenda A. Dougan' 'Nichola McCann' 'Christopher J. Ziegler' 'Nicola E. Brasch' _publ_section_title ; Characterization of Novel Vanadium(III)/Acetate Clusters Formed in Aqueous Solution ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 5197 _journal_page_last 5199 _journal_paper_doi 10.1021/ic050336f _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C8 H38 Cl4 O23 V4' _chemical_formula_weight 847.95 _chemical_name_systematic ; ? ; _space_group_IT_number 136 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall '-P 4n 2n' _symmetry_space_group_name_H-M 'P 42/m n m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 17.7698(11) _cell_length_b 17.7698(11) _cell_length_c 11.3900(14) _cell_measurement_reflns_used 6035 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.14 _cell_measurement_theta_min 2.29 _cell_volume 3596.6(5) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0659 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 25213 _diffrn_reflns_theta_full 24.98 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_min 1.62 _exptl_absorpt_coefficient_mu 1.376 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_correction_T_min 0.6836 _exptl_absorpt_correction_type SADABS _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1724 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _platon_squeeze_details ' ?' _refine_diff_density_max 0.743 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.142 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 142 _refine_ls_number_reflns 1752 _refine_ls_number_restraints 54 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0843 _refine_ls_shift/su_max 0.109 _refine_ls_shift/su_mean 0.013 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+76.1637P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2104 _refine_ls_wR_factor_ref 0.2126 _reflns_number_gt 1620 _reflns_number_total 1752 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic050336from20050609_015251_3.cif _cod_data_source_block '[V4(mu-OOCCH3)4(mu-OH)4(OH2)8]Cl4.3H2O' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal' 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 4309273 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y-1/2, -x-1/2, -z-1/2' '-y-1/2, x-1/2, -z-1/2' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'y, x, 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 C1 C 0.0816(4) 0.0816(4) 0.3169(10) 0.027(2) Uani 1 2 d S . . H1A H 0.0338 0.1073 0.3320 0.041 Uiso 0.50 1 calc PR . . H1B H 0.1041 0.0660 0.3915 0.041 Uiso 0.50 1 calc PR . . H1C H 0.0726 0.0372 0.2678 0.041 Uiso 0.50 1 calc PR . . C2 C 0.1343(4) 0.1343(4) 0.2543(9) 0.020(2) Uani 1 2 d S . . C3 C 0.1941(5) 0.4252(6) 0.0000 0.019(2) Uani 1 2 d S . . C4 C 0.2210(7) 0.5063(7) 0.0000 0.032(3) Uani 1 2 d S . . H4A H 0.2229 0.5250 -0.0809 0.048 Uiso 0.50 1 calc PR . . H4B H 0.2713 0.5090 0.0349 0.048 Uiso 0.50 1 calc PR . . H4C H 0.1861 0.5372 0.0460 0.048 Uiso 0.50 1 calc PR . . Cl1 Cl 0.20938(17) 0.20938(17) 0.5000 0.0284(14) Uani 0.998(18) 4 d SP A 1 Cl2 Cl 0.0160(7) 0.1193(6) 0.0000 0.029(4) Uani 0.51(4) 2 d SP B 1 Cl3 Cl 0.6228(6) 0.6228(6) 0.8871(15) 0.032(4) Uani 0.56(5) 2 d SP C 1 O1 O 0.1099(3) 0.1996(3) 0.2298(4) 0.0250(12) Uani 1 1 d U . . O2 O 0.2531(3) 0.2531(3) 0.1453(6) 0.0266(16) Uani 1.05 2 d SPDU . . O3 O 0.1743(3) 0.3330(3) 0.3202(4) 0.0274(12) Uani 1 1 d DU . . O4 O 0.1842(3) 0.3947(3) 0.0978(4) 0.0235(11) Uani 1 1 d U . . O5 O 0.0463(3) 0.3344(4) 0.1840(5) 0.0359(14) Uani 1 1 d DU . . O6 O 0.1217(5) 0.2569(5) 0.0000 0.0316(19) Uani 1 2 d SDU . . V1 V 0.15184(7) 0.29251(7) 0.15463(10) 0.0191(4) Uani 1 1 d . . . H2 H 0.2869(10) 0.2869(10) 0.15(2) 0.17(11) Uiso 1 2 d SD . . H6 H 0.079(3) 0.236(6) 0.0000 0.03(3) Uiso 1 2 d SD . . O1W O -0.011(3) 0.137(2) 0.0000 0.088(17) Uani 0.50(8) 2 d SPU D 2 O2W O 0.628(7) 0.649(8) 0.840(4) 0.07(4) Uani 0.25(5) 1 d PU E 2 H5A H 0.021(4) 0.290(3) 0.168(8) 0.04(3) Uiso 1 1 d D . . H5B H 0.042(7) 0.3865(17) 0.196(12) 0.10(5) Uiso 1 1 d D . . H3A H 0.208(6) 0.374(5) 0.324(13) 0.11(5) Uiso 1 1 d D . . H3B H 0.180(7) 0.292(5) 0.372(9) 0.09(4) Uiso 1 1 d 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 C1 0.025(3) 0.025(3) 0.031(6) 0.008(3) 0.008(3) -0.004(4) C2 0.020(3) 0.020(3) 0.020(5) -0.001(3) -0.001(3) -0.001(4) C3 0.013(5) 0.027(6) 0.017(5) 0.000 0.000 0.002(4) C4 0.044(7) 0.032(6) 0.021(5) 0.000 0.000 -0.009(5) Cl1 0.0367(18) 0.0367(18) 0.0118(19) 0.000 0.000 0.0002(18) Cl2 0.039(6) 0.024(5) 0.026(3) 0.000 0.000 0.003(3) Cl3 0.026(4) 0.026(4) 0.044(7) -0.006(3) -0.006(3) -0.003(2) O1 0.026(3) 0.032(3) 0.017(2) 0.001(2) 0.004(2) -0.011(2) O2 0.026(2) 0.026(2) 0.029(4) 0.000(2) 0.000(2) -0.023(3) O3 0.041(3) 0.024(3) 0.017(2) 0.006(2) 0.000(2) -0.002(2) O4 0.030(3) 0.023(3) 0.017(2) 0.002(2) 0.000(2) -0.006(2) O5 0.030(3) 0.047(4) 0.030(3) 0.006(3) 0.005(3) -0.004(3) O6 0.027(4) 0.048(5) 0.019(4) 0.000 0.000 -0.018(4) V1 0.0206(7) 0.0245(7) 0.0123(6) 0.0002(5) 0.0013(5) -0.0043(5) O1W 0.12(3) 0.11(3) 0.031(13) 0.000 0.000 0.09(3) O2W 0.12(8) 0.06(4) 0.04(2) 0.00(3) 0.02(3) -0.07(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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 O1 C2 O1 125.2(9) 16 . ? O1 C2 C1 117.4(5) 16 . ? O1 C2 C1 117.4(5) . . ? O4 C3 O4 125.9(10) 10 . ? O4 C3 C4 117.1(5) 10 . ? O4 C3 C4 117.1(5) . . ? C2 O1 V1 136.0(5) . . ? V1 O2 V1 132.2(4) . 16 ? C3 O4 V1 135.8(5) . . ? V1 O6 V1 129.6(4) . 10 ? O2 V1 O6 95.1(3) . . ? O2 V1 O1 94.1(2) . . ? O6 V1 O1 90.9(3) . . ? O2 V1 O4 92.5(2) . . ? O6 V1 O4 94.7(3) . . ? O1 V1 O4 171.0(2) . . ? O2 V1 O5 173.7(3) . . ? O6 V1 O5 90.8(3) . . ? O1 V1 O5 83.6(2) . . ? O4 V1 O5 89.3(2) . . ? O2 V1 O3 89.8(3) . . ? O6 V1 O3 175.1(3) . . ? O1 V1 O3 88.2(2) . . ? O4 V1 O3 85.6(2) . . ? O5 V1 O3 84.3(2) . . ? 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 C1 C2 1.504(14) . ? C2 O1 1.269(7) 16 ? C2 O1 1.269(7) . ? C3 O4 1.251(7) 10 ? C3 O4 1.251(7) . ? C3 C4 1.518(15) . ? O1 V1 2.004(5) . ? O2 V1 1.933(3) . ? O2 V1 1.933(3) 16 ? O3 V1 2.057(5) . ? O4 V1 2.012(5) . ? O5 V1 2.046(6) . ? O6 V1 1.947(4) . ? O6 V1 1.947(4) 10 ? O2W O2W 0.5(4) 16 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.098 0.399 -0.136 624.4 145.3 2 0.500 0.500 0.000 9.3 -1.3 3 0.000 0.000 0.500 9.2 -2.1