#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000414.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_4000414 _journal_name_full 'Chemistry of Materials' _journal_year 2004 _chemical_formula_moiety 'F15 Fe5, 2(K), 1.254(K0.50)' _chemical_formula_structural 'F60 Fe20 K10.5' _chemical_formula_sum 'F15 Fe5 K2.63' _chemical_formula_weight 666.97 _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P42bc' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,z 3 -y,x,z+1/2 4 y,-x,z+1/2 5 -x+1/2,y+1/2,z 6 x+1/2,-y+1/2,z 7 y+1/2,x+1/2,z+1/2 8 -y+1/2,-x+1/2,z+1/2 _cell_length_a 12.6340(10) _cell_length_b 12.6340(10) _cell_length_c 7.9030(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1261.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 412 _cell_measurement_theta_min 5.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description 'prism' _exptl_crystal_colour 'brown' _exptl_crystal_size_max .113 _exptl_crystal_size_mid .064 _exptl_crystal_size_min .048 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.512 _exptl_crystal_density_method ? _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 6.653 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.606 _exptl_absorpt_correction_T_max 0.727 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker AXS 100 CCD' _diffrn_measurement_method '/f and /w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6625 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1395 _reflns_number_observed 834 _reflns_observed_criterion 'I>2sigma(I)' 'SMART Program Package (Bruker AXS Inc., 1998)' 'SMART Program Package (Bruker AXS Inc., 1998)' 'SAINT Program Package (Bruker AXS Inc., 1998)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00103(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(4) _refine_ls_number_reflns 1272 _refine_ls_number_parameters 110 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_obs 0.0209 _refine_ls_wR_factor_all 0.0613 _refine_ls_wR_factor_obs 0.0544 _refine_ls_goodness_of_fit_all 0.978 _refine_ls_goodness_of_fit_obs 1.141 _refine_ls_restrained_S_all 0.965 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/esd_max 1.290 _refine_ls_shift/esd_mean 0.199 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.5000 0.0000 0.2104(4) 0.01151(14) Uani 1 d S . Fe2 Fe 0.21305(3) -0.07416(3) 0.7105(2) 0.01151(15) Uani 1 d . . Fe3 Fe 0.21096(3) -0.07425(3) 0.2096(2) 0.01150(15) Uani 1 d . . K1 K 0.1719(2) -0.3273(2) 0.4597(8) 0.0422(3) Uani 1.000(3) d . . K2 K 0.0000 0.0000 -0.0394(12) 0.0177(4) Uani 0.627(3) d SP . F1 F 0.27590(14) -0.21431(13) 0.2055(15) 0.0230(5) Uani 1 d . . F2 F 0.34418(14) -0.00107(15) 0.2036(15) 0.0405(10) Uani 1 d . . F3 F 0.51460(15) -0.15305(13) 0.2101(15) 0.0294(6) Uani 1 d . . F4 F 0.1490(2) 0.0672(2) 0.2052(13) 0.0328(7) Uani 1 d . . F5 F 0.07321(15) -0.13734(14) 0.2049(13) 0.0308(6) Uani 1 d . . F6 F 0.2077(5) -0.0747(5) 0.4482(15) 0.044(2) Uani 1 d . . F7 F 0.2102(5) -0.0783(5) -0.0394(16) 0.042(2) Uani 1 d . . F8 F 0.5000 0.0000 0.4573(27) 0.0526(9) Uani 1 d S . 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 Fe1 0.0116(4) 0.0100(3) 0.0130(3) 0.000 0.000 0.0002(2) Fe2 0.0117(2) 0.0108(2) 0.0120(3) 0.0010(10) -0.0004(11) -0.0007(2) Fe3 0.0115(2) 0.0104(3) 0.0126(3) 0.0009(11) 0.0006(11) 0.0001(2) K1 0.052(2) 0.051(2) 0.0236(4) 0.003(2) 0.000(2) -0.0263(4) K2 0.019(3) 0.014(3) 0.0202(7) 0.000 0.000 0.004(3) F1 0.0208(11) 0.0156(11) 0.0325(14) -0.002(4) -0.005(4) 0.0046(7) F2 0.0163(12) 0.0282(12) 0.077(3) 0.013(6) 0.003(5) -0.0054(9) F3 0.0230(10) 0.0125(10) 0.053(2) 0.002(5) -0.002(6) -0.0043(8) F4 0.0293(12) 0.0166(9) 0.053(2) -0.003(4) -0.009(5) 0.0054(10) F5 0.0158(9) 0.0255(11) 0.051(2) 0.003(5) -0.002(4) -0.0082(10) F6 0.035(4) 0.082(6) 0.014(4) -0.002(4) 0.000(3) 0.021(3) F7 0.051(5) 0.070(5) 0.006(3) 0.006(4) 0.001(4) 0.024(3) F8 0.065(8) 0.074(9) 0.018(2) 0.000 0.000 0.006(2)