#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000361.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_4000361 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _publ_section_title ; Crystal structures and magnetic properties of the new alkaline zinc oxovanadium phosphates MZn(H2O)(VO)2(PO4)2(H2PO4) with M = K+, Rb+ and Cs+. ; _chemical_formula_moiety 'H2 K0.50 O7.50 P1.50 V Zn0.50' _chemical_formula_sum 'H2 K0.50 O7.50 P1.50 V Zn0.50' _chemical_formula_weight 271.65 _symmetry_cell_setting monoclinic _space_group_IT_number 11 _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _[local]_cod_cif_authors_sg_H-M 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.4459(1) _cell_length_b 9.2160(1) _cell_length_c 9.3199(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.281(1) _cell_angle_gamma 90.00 _cell_volume 619.78(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2591 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 34.972 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.911 _exptl_crystal_density_method 'Archimede's principle in CH2Cl2' _exptl_crystal_density_meas 2.88 _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 4.205 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method 'omega-phi scans' _diffrn_reflns_number 6248 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 37.05 _reflns_number_total 3318 _reflns_number_gt 2639 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0217(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3318 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 2.103 _refine_ls_restrained_S_all 2.103 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 K K 0.17803(18) 0.46586(12) -0.28118(13) 0.0311(3) Uani 0.50 1 d P . . Zn Zn 0.32949(6) 0.7500 0.38242(4) 0.01900(11) Uani 1 2 d S . . V1 V 0.55178(7) 0.2500 0.02638(6) 0.01335(11) Uani 1 2 d S . . V2 V 0.03905(7) 0.7500 -0.02190(6) 0.01428(12) Uani 1 2 d S . . P1 P 0.29673(7) 0.49026(5) 0.15043(6) 0.01223(12) Uani 1 1 d . . . P2 P 0.12789(16) 0.66193(11) -0.36731(12) 0.0150(2) Uani 0.50 1 d P . . O1 O 0.4019(3) 0.2500 -0.1279(2) 0.0234(5) Uani 1 2 d S . . O2 O 0.4672(2) 0.40379(16) 0.14086(17) 0.0199(3) Uani 1 1 d . . . O3 O 0.26093(18) 0.60822(15) 0.02580(16) 0.0153(3) Uani 1 1 d . . . O4 O 0.3364(3) 0.56088(18) 0.30204(18) 0.0311(4) Uani 1 1 d . . . O5 O 0.1234(2) 0.39978(16) 0.1316(2) 0.0249(4) Uani 1 1 d . . . O6 O 0.1734(3) 0.7500 -0.2192(2) 0.0183(4) Uani 1 2 d S . . O7 O 0.0011(3) 0.7500 0.1388(3) 0.0339(6) Uani 1 2 d S . . O8 O -0.0826(4) 0.6161(3) -0.4169(3) 0.0221(7) Uani 0.50 1 d P . . O9 O 0.1591(4) 0.7500 0.5089(3) 0.0259(5) Uani 1 2 d S . . O10 O 0.5828(5) 0.7865(3) 0.5293(4) 0.0337(9) Uani 0.50 1 d P . . O11 O 0.2367(5) 0.5160(4) -0.3564(5) 0.0347(9) Uani 0.50 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 K 0.0410(7) 0.0264(5) 0.0222(6) -0.0009(4) 0.0005(5) -0.0045(4) Zn 0.0271(2) 0.01758(17) 0.01471(19) 0.000 0.00968(17) 0.000 V1 0.0077(2) 0.0212(2) 0.0117(2) 0.000 0.00341(19) 0.000 V2 0.0076(2) 0.0233(2) 0.0122(2) 0.000 0.00297(19) 0.000 P1 0.0108(3) 0.0163(2) 0.0099(3) -0.00211(17) 0.0033(2) 0.00039(18) P2 0.0155(5) 0.0179(5) 0.0106(5) -0.0003(4) 0.0015(4) 0.0018(4) O1 0.0142(12) 0.0370(13) 0.0168(12) 0.000 -0.0002(10) 0.000 O2 0.0126(8) 0.0312(8) 0.0159(8) -0.0006(6) 0.0032(6) 0.0074(6) O3 0.0096(7) 0.0225(7) 0.0132(7) 0.0027(5) 0.0018(6) -0.0008(5) O4 0.0545(13) 0.0257(9) 0.0110(8) -0.0050(6) 0.0043(8) 0.0100(7) O5 0.0133(8) 0.0232(8) 0.0359(10) 0.0058(7) 0.0018(7) -0.0034(6) O6 0.0127(11) 0.0292(11) 0.0126(10) 0.000 0.0021(9) 0.000 O7 0.0214(14) 0.0631(17) 0.0210(13) 0.000 0.0127(12) 0.000 O8 0.0166(17) 0.0349(17) 0.0139(15) -0.0015(13) 0.0020(13) -0.0065(13) O9 0.0273(14) 0.0389(13) 0.0152(12) 0.000 0.0123(11) 0.000 O10 0.031(2) 0.027(2) 0.035(2) -0.0048(13) -0.0083(16) 0.0051(12) O11 0.037(2) 0.0255(17) 0.031(2) -0.0114(15) -0.0122(18) 0.0121(15)