#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203372.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2203372 loop_ _publ_author_name 'Dro\&s, Thomas' 'Glaum, Robert' _publ_section_title ; The langbeinite-type barium vanadium(III) orthophosphate, Ba~3~V~4~(PO~4~)~6~ ; _journal_issue 4 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first i58 _journal_page_last i60 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'Ba3 V4 (P O4)6' _chemical_formula_structural 'Ba3 V4 (P O4)6' _chemical_formula_sum 'Ba3 O24 P6 V4' _chemical_formula_weight 1185.58 _chemical_name_systematic ; ; _symmetry_cell_setting cubic _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P 21 3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.8825(7) _cell_length_b 9.8825(7) _cell_length_c 9.8825(7) _cell_measurement_reflns_used 29 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.97 _cell_measurement_theta_min 2.91 _cell_volume 965.16(12) _computing_cell_refinement 'COLLECT and DENZO (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 2001)' _computing_data_reduction 'COLLECT and DENZO' _computing_molecular_graphics 'ATOMS (Dowty, 2002)' _computing_publication_material 'WinGX (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 22794 _diffrn_reflns_theta_full 29.97 _diffrn_reflns_theta_max 29.97 _diffrn_reflns_theta_min 2.91 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.494 _exptl_absorpt_correction_T_max 0.7074 _exptl_absorpt_correction_T_min 0.5970 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(HABITUS; Herrendorf, 1993)' _exptl_crystal_colour yellow--green _exptl_crystal_density_diffrn 4.08 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1084 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 2.024 _refine_diff_density_min -1.903 _refine_ls_abs_structure_details 'Flack (1983), 393 Friedel pairs' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_extinction_coef 0.0237(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_matrix_type full _refine_ls_number_parameters 61 _refine_ls_number_reflns 930 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.130 _refine_ls_R_factor_all 0.027 _refine_ls_R_factor_gt 0.027 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+7.2584P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.059 _reflns_number_gt 930 _reflns_number_total 930 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file br6140.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z, x+1/2' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' 'z, x, y' '-z, x+1/2, -y+1/2' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 '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_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Ba1 0.06743(4) 0.06743(4) 0.06743(4) 0.0182(2) Uani d SP 0.772(2) Ba Ba2 0.29438(6) 0.29438(6) 0.29438(6) 0.0282(3) Uani d SP 0.728(2) Ba V1 0.58620(7) 0.58620(7) 0.58620(7) 0.0073(2) Uani d S 1 V V2 0.85303(7) 0.85303(7) 0.85303(7) 0.0086(2) Uani d S 1 V P 0.62570(10) 0.46081(10) 0.27168(10) 0.0067(2) Uani d . 1 P O1 0.6530(4) 0.5015(4) 0.4170(4) 0.0216(7) Uani d . 1 O O2 0.7572(4) 0.4841(4) 0.1930(4) 0.0279(9) Uani d . 1 O O3 0.5776(4) 0.3136(3) 0.2618(4) 0.0218(7) Uani d . 1 O O4 0.5218(4) 0.5517(4) 0.2037(4) 0.0238(8) Uani d . 1 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ba1 0.0182(2) 0.0182(2) 0.0182(2) 0.00074(13) 0.00074(13) 0.00074(13) Ba2 0.0282(3) 0.0282(3) 0.0282(3) 0.0107(2) 0.0107(2) 0.0107(2) V1 0.0073(2) 0.0073(2) 0.0073(2) -0.0006(2) -0.0006(2) -0.0006(2) V2 0.0086(2) 0.0086(2) 0.0086(2) 0.0010(2) 0.0010(2) 0.0010(2) P 0.0068(4) 0.0065(4) 0.0068(4) 0.0016(3) 0.0005(3) 0.0002(3) O1 0.0250(17) 0.0280(18) 0.0118(15) 0.0032(15) -0.0028(13) -0.0119(14) O2 0.0211(17) 0.032(2) 0.031(2) 0.0097(15) 0.0193(15) 0.0087(16) O3 0.0254(18) 0.0099(14) 0.0300(18) -0.0046(13) -0.0131(16) 0.0040(13) O4 0.0232(17) 0.0212(18) 0.0270(18) 0.0125(14) -0.0084(15) 0.0011(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ba1 O1 11_564 2.843(4) Y Ba1 O1 7_456 2.843(4) ? Ba1 O1 4_645 2.843(4) ? Ba1 O4 10_545 2.961(4) Y Ba1 O4 6_554 2.961(4) ? Ba1 O4 3_455 2.961(4) ? Ba1 O2 11_564 3.047(5) Y Ba1 O2 7_456 3.047(5) ? Ba1 O2 4_645 3.047(5) ? Ba1 O2 10_545 3.225(5) Y Ba1 O2 6_554 3.225(5) ? Ba1 O2 3_455 3.225(5) ? Ba2 O3 . 2.824(4) Y Ba2 O3 9 2.824(4) ? Ba2 O3 5 2.824(4) ? Ba2 O4 11_564 3.009(4) Y Ba2 O4 7_456 3.009(4) ? Ba2 O4 4_645 3.009(4) ? Ba2 O2 11_564 3.111(4) Y Ba2 O2 7_456 3.111(4) ? Ba2 O2 4_645 3.111(4) ? Ba2 P 11_564 3.4521(11) Y Ba2 P 4_645 3.4521(11) ? Ba2 P 7_456 3.4521(11) ? V1 O1 9 1.983(3) Y V1 O1 5 1.983(3) ? V1 O1 . 1.983(3) ? V1 O2 8_656 1.998(4) Y V1 O2 12_566 1.998(4) ? V1 O2 2_665 1.998(4) ? V1 Ba1 2_565 3.7492(5) ? V1 Ba1 3_556 3.7492(5) ? V1 Ba1 4_655 3.7492(5) ? V2 O4 10_656 1.996(3) Y V2 O4 6_665 1.996(3) ? V2 O4 3_566 1.996(4) ? V2 O3 12_566 1.999(3) Y V2 O3 8_656 1.999(4) ? V2 O3 2_665 1.999(3) ? V2 Ba1 1_666 3.6699(14) ? V2 Ba2 4_656 3.8209(6) ? V2 Ba2 3_566 3.8210(5) ? V2 Ba2 2_665 3.8210(6) ? P O1 . 1.516(3) Y P O4 . 1.521(3) Y P O2 . 1.531(4) Y P O3 . 1.534(3) Y P Ba1 3 3.4118(11) ? P Ba2 4_655 3.4521(11) ? P Ba1 4_655 3.5826(11) ? O1 Ba1 4_655 2.843(4) ? O2 V1 2_664 1.998(4) ? O2 Ba1 4_655 3.047(5) ? O2 Ba2 4_655 3.111(4) ? O2 Ba1 3 3.225(5) ? O3 V2 2_664 1.999(3) ? O4 V2 3_466 1.996(3) ? O4 Ba1 3 2.961(4) ? O4 Ba2 4_655 3.009(4) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Ba1 O1 11_564 7_456 100.53(10) ? O1 Ba1 O1 11_564 4_645 100.53(10) ? O1 Ba1 O1 7_456 4_645 100.53(10) ? O1 Ba1 O4 11_564 10_545 96.08(10) ? O1 Ba1 O4 7_456 10_545 100.78(11) ? O1 Ba1 O4 4_645 10_545 149.99(10) ? O1 Ba1 O4 11_564 6_554 149.99(10) ? O1 Ba1 O4 7_456 6_554 96.08(10) ? O1 Ba1 O4 4_645 6_554 100.78(11) ? O4 Ba1 O4 10_545 6_554 56.07(11) ? O1 Ba1 O4 11_564 3_455 100.78(11) ? O1 Ba1 O4 7_456 3_455 149.99(10) ? O1 Ba1 O4 4_645 3_455 96.08(10) ? O4 Ba1 O4 10_545 3_455 56.07(11) ? O4 Ba1 O4 6_554 3_455 56.07(11) ? O1 Ba1 O2 11_564 11_564 48.95(10) ? O1 Ba1 O2 7_456 11_564 114.21(11) ? O1 Ba1 O2 4_645 11_564 52.41(10) ? O4 Ba1 O2 10_545 11_564 133.01(11) ? O4 Ba1 O2 6_554 11_564 141.46(11) ? O4 Ba1 O2 3_455 11_564 95.73(10) ? O1 Ba1 O2 11_564 7_456 52.41(10) ? O1 Ba1 O2 7_456 7_456 48.95(10) ? O1 Ba1 O2 4_645 7_456 114.21(11) ? O4 Ba1 O2 10_545 7_456 95.73(10) ? O4 Ba1 O2 6_554 7_456 133.01(11) ? O4 Ba1 O2 3_455 7_456 141.46(11) ? O2 Ba1 O2 11_564 7_456 85.52(11) ? O1 Ba1 O2 11_564 4_645 114.21(11) ? O1 Ba1 O2 7_456 4_645 52.41(10) ? O1 Ba1 O2 4_645 4_645 48.95(10) ? O4 Ba1 O2 10_545 4_645 141.46(11) ? O4 Ba1 O2 6_554 4_645 95.73(10) ? O4 Ba1 O2 3_455 4_645 133.01(11) ? O2 Ba1 O2 11_564 4_645 85.52(11) ? O2 Ba1 O2 7_456 4_645 85.52(11) ? O1 Ba1 O2 11_564 10_545 56.07(10) ? O1 Ba1 O2 7_456 10_545 86.51(10) ? O1 Ba1 O2 4_645 10_545 156.56(10) ? O4 Ba1 O2 10_545 10_545 45.87(9) ? O4 Ba1 O2 6_554 10_545 100.65(10) ? O4 Ba1 O2 3_455 10_545 88.09(10) ? O2 Ba1 O2 11_564 10_545 104.277(10) ? O2 Ba1 O2 7_456 10_545 54.72(14) ? O2 Ba1 O2 4_645 10_545 137.20(7) ? O1 Ba1 O2 11_564 6_554 156.56(10) ? O1 Ba1 O2 7_456 6_554 56.07(10) ? O1 Ba1 O2 4_645 6_554 86.51(10) ? O4 Ba1 O2 10_545 6_554 88.09(10) ? O4 Ba1 O2 6_554 6_554 45.87(9) ? O4 Ba1 O2 3_455 6_554 100.65(10) ? O2 Ba1 O2 11_564 6_554 137.20(7) ? O2 Ba1 O2 7_456 6_554 104.277(10) ? O2 Ba1 O2 4_645 6_554 54.72(14) ? O2 Ba1 O2 10_545 6_554 115.46(5) ? O1 Ba1 O2 11_564 3_455 86.51(10) ? O1 Ba1 O2 7_456 3_455 156.56(10) ? O1 Ba1 O2 4_645 3_455 56.07(10) ? O4 Ba1 O2 10_545 3_455 100.65(10) ? O4 Ba1 O2 6_554 3_455 88.09(10) ? O4 Ba1 O2 3_455 3_455 45.87(9) ? O2 Ba1 O2 11_564 3_455 54.72(14) ? O2 Ba1 O2 7_456 3_455 137.20(7) ? O2 Ba1 O2 4_645 3_455 104.277(10) ? O2 Ba1 O2 10_545 3_455 115.46(5) ? O2 Ba1 O2 6_554 3_455 115.46(5) ? O3 Ba2 O3 . 9 93.11(11) ? O3 Ba2 O3 . 5 93.11(11) ? O3 Ba2 O3 9 5 93.11(11) ? O3 Ba2 O4 . 11_564 82.07(11) ? O3 Ba2 O4 9 11_564 57.03(9) ? O3 Ba2 O4 5 11_564 149.16(10) ? O3 Ba2 O4 . 7_456 149.16(10) ? O3 Ba2 O4 9 7_456 82.07(11) ? O3 Ba2 O4 5 7_456 57.03(9) ? O4 Ba2 O4 11_564 7_456 118.85(2) ? O3 Ba2 O4 . 4_645 57.03(9) ? O3 Ba2 O4 9 4_645 149.16(10) ? O3 Ba2 O4 5 4_645 82.07(11) ? O4 Ba2 O4 11_564 4_645 118.85(2) ? O4 Ba2 O4 7_456 4_645 118.85(2) ? O3 Ba2 O2 . 11_564 81.88(11) ? O3 Ba2 O2 9 11_564 103.48(10) ? O3 Ba2 O2 5 11_564 162.86(10) ? O4 Ba2 O2 11_564 11_564 46.60(10) ? O4 Ba2 O2 7_456 11_564 128.91(11) ? O4 Ba2 O2 4_645 11_564 81.46(10) ? O3 Ba2 O2 . 7_456 162.86(10) ? O3 Ba2 O2 9 7_456 81.88(11) ? O3 Ba2 O2 5 7_456 103.48(10) ? O4 Ba2 O2 11_564 7_456 81.46(10) ? O4 Ba2 O2 7_456 7_456 46.60(10) ? O4 Ba2 O2 4_645 7_456 128.91(11) ? O2 Ba2 O2 11_564 7_456 83.37(13) ? O3 Ba2 O2 . 4_645 103.48(10) ? O3 Ba2 O2 9 4_645 162.86(10) ? O3 Ba2 O2 5 4_645 81.88(11) ? O4 Ba2 O2 11_564 4_645 128.91(11) ? O4 Ba2 O2 7_456 4_645 81.46(10) ? O4 Ba2 O2 4_645 4_645 46.60(10) ? O2 Ba2 O2 11_564 4_645 83.37(13) ? O2 Ba2 O2 7_456 4_645 83.37(13) ? O1 V1 O1 9 5 93.73(16) Y O1 V1 O1 9 . 93.73(16) ? O1 V1 O1 5 . 93.73(16) ? O1 V1 O2 9 8_656 81.84(18) Y O1 V1 O2 5 8_656 92.35(17) Y O1 V1 O2 . 8_656 172.71(18) Y O1 V1 O2 9 12_566 92.35(17) ? O1 V1 O2 5 12_566 172.71(18) ? O1 V1 O2 . 12_566 81.84(18) ? O2 V1 O2 8_656 12_566 92.50(16) Y O1 V1 O2 9 2_665 172.71(18) ? O1 V1 O2 5 2_665 81.84(18) ? O1 V1 O2 . 2_665 92.35(17) ? O2 V1 O2 8_656 2_665 92.50(16) ? O2 V1 O2 12_566 2_665 92.50(16) ? O4 V2 O4 10_656 6_665 88.44(17) Y O4 V2 O4 10_656 3_566 88.44(17) ? O4 V2 O4 6_665 3_566 88.44(17) ? O4 V2 O3 10_656 12_566 88.61(15) Y O4 V2 O3 6_665 12_566 176.20(17) Y O4 V2 O3 3_566 12_566 89.08(17) Y O4 V2 O3 10_656 8_656 89.08(17) ? O4 V2 O3 6_665 8_656 88.61(15) ? O4 V2 O3 3_566 8_656 176.20(17) ? O3 V2 O3 12_566 8_656 93.75(17) Y O4 V2 O3 10_656 2_665 176.20(17) ? O4 V2 O3 6_665 2_665 89.08(17) ? O4 V2 O3 3_566 2_665 88.61(15) ? O3 V2 O3 12_566 2_665 93.75(17) ? O3 V2 O3 8_656 2_665 93.75(17) ? O1 P O4 . . 112.5(2) ? O1 P O2 . . 106.9(2) ? O4 P O2 . . 105.1(2) ? O1 P O3 . . 111.5(2) ? O4 P O3 . . 108.8(2) ? O2 P O3 . . 111.9(2) ? _cod_database_code 2203372