#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000363.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_4000363 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_moiety 'Cs0.50 H2 O7.50 P1.50 V Zn0.50' _chemical_formula_sum 'Cs0.5 H2 O7.5 P1.5 V Zn0.5' _[local]_cod_chemical_formula_sum_orig 'Cs0.50 H2 O7.50 P1.50 V Zn0.50' _chemical_formula_weight 318.55 _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 7.5159(1) _cell_length_b 9.1994(1) _cell_length_c 9.5465(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.912(1) _cell_angle_gamma 90.00 _cell_volume 650.21(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 34.99 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 3.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 6.447 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.103 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; _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 5187 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 34.99 _reflns_number_total 2998 _reflns_number_gt 2620 _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 0.051(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2998 _refine_ls_number_parameters 131 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 2.477 _refine_ls_restrained_S_all 2.477 _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 Cs Cs 0.18953(5) 0.44868(4) 0.68882(4) 0.02335(12) Uani 0.50 1 d P . . V1 V 0.55189(7) 0.2500 0.02674(7) 0.01095(14) Uani 1 2 d S . . V2 V 0.95908(7) 0.2500 0.02510(7) 0.01486(15) Uani 1 2 d S . . Zn Zn 0.67404(6) 0.2500 0.62647(5) 0.01754(13) Uani 1 2 d S . . P1 P 0.71811(8) 0.50893(7) 0.85479(8) 0.01409(16) Uani 1 1 d . . . P2 P 0.82993(16) 0.15480(15) 0.35322(16) 0.0158(3) Uani 0.50 1 d P . . O1 O 0.7434(2) 0.39307(17) 0.9764(2) 0.0154(4) Uani 1 1 d . . . O2 O 0.5506(2) 0.5989(2) 0.8653(2) 0.0196(4) Uani 1 1 d . . . O3 O 0.4237(3) 0.2500 0.8762(3) 0.0241(6) Uani 1 2 d S . . O4 O 0.2026(3) 0.7500 0.7889(3) 0.0256(7) Uani 1 2 d S . . O5 O 0.8891(2) 0.5997(2) 0.8681(2) 0.0241(5) Uani 1 1 d . . . O6 O 0.6865(3) 0.4371(2) 0.7091(2) 0.0288(5) Uani 1 1 d . . . O7 O 0.8183(5) 0.2500 0.4778(4) 0.0311(7) Uani 1 2 d S . . O8 O 0.4169(5) 0.2500 0.5049(5) 0.0849(18) Uani 1 2 d S . . O9 O 0.0173(4) 0.2500 0.8733(3) 0.0288(7) Uani 1 2 d S . . O10 O 0.0192(7) 0.0859(8) 0.3834(5) 0.074(2) Uani 0.50 1 d P . . O11 O 0.6943(8) 0.0268(5) 0.3533(6) 0.062(2) 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 Cs 0.0284(2) 0.01927(19) 0.0207(2) 0.00192(13) -0.00068(15) -0.00146(13) V1 0.0070(2) 0.0149(3) 0.0113(3) 0.000 0.00231(19) 0.000 V2 0.0074(2) 0.0157(3) 0.0223(4) 0.000 0.0051(2) 0.000 Zn 0.0268(2) 0.01105(19) 0.0171(3) 0.000 0.01008(18) 0.000 P1 0.0127(3) 0.0121(3) 0.0186(4) -0.0053(2) 0.0059(2) 0.0002(2) P2 0.0158(6) 0.0155(5) 0.0147(7) -0.0034(5) -0.0010(5) 0.0024(5) O1 0.0118(7) 0.0125(7) 0.0223(11) -0.0024(7) 0.0038(7) -0.0017(6) O2 0.0117(7) 0.0247(9) 0.0227(11) -0.0055(8) 0.0039(7) 0.0047(7) O3 0.0141(11) 0.0383(16) 0.0179(16) 0.000 -0.0027(10) 0.000 O4 0.0127(11) 0.0490(18) 0.0145(16) 0.000 0.0007(10) 0.000 O5 0.0136(8) 0.0210(9) 0.0383(14) 0.0008(9) 0.0058(8) -0.0041(7) O6 0.0522(14) 0.0171(9) 0.0178(12) -0.0077(8) 0.0084(10) 0.0022(9) O7 0.056(2) 0.0171(12) 0.0274(19) 0.000 0.0269(16) 0.000 O8 0.033(2) 0.174(5) 0.046(3) 0.000 0.002(2) 0.000 O9 0.0211(13) 0.0383(16) 0.031(2) 0.000 0.0157(13) 0.000 O10 0.056(3) 0.150(6) 0.018(3) 0.010(3) 0.008(2) 0.080(4) O11 0.087(4) 0.034(2) 0.048(4) 0.020(3) -0.033(3) -0.039(3) _cod_database_code 4000363 _journal_paper_doi 10.1021/cm031090k