#------------------------------------------------------------------------------ #$Date: 2009-11-18 14:56:34 +0000 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000104.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_4000104 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _publ_section_title ; Open-Framework Borophosphates: (NH4)0.4Fe1.05(H2O)2[BP2O8]*0.6H2O and NH4Fe[BP2O8(OH)] ; loop_ _publ_author_name 'Huang, Ya-Xi' 'Sch\"afer, Gerd' 'Carrillo-Carbrera, Wilder' 'Cardoso, Raul' 'Schnelle, Walter' 'Zhao, Jing-Tai' 'Kniep, R\"udiger' _chemical_formula_sum 'B Fe1.05 H0 N0.41 O10.59 P2' _[local]_cod_chemical_formula_sum_orig 'H0 B Fe1.05 N0.41 O10.59 P2' _chemical_formula_weight 306.58 _symmetry_cell_setting 'hexagonal' _symmetry_space_group_name_H-M 'P 65' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z+2/3' 'y, -x+y, z+1/6' '-x+y, -x, z+1/3' 'x-y, x, z+5/6' _cell_length_a 9.483(4) _cell_length_b 9.483(4) _cell_length_c 15.697(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1222.5(8) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _exptl_crystal_description 'hexagonal bipyramide' _exptl_crystal_colour 'black' _exptl_crystal_size_max '0.2' _exptl_crystal_size_mid '0.2' _exptl_crystal_size_min '0.2' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 899 _exptl_absorpt_coefficient_mu 1.229 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.56087 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 16047 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.99 _reflns_number_total 2589 _reflns_number_gt 2348 _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^)+(0.0427P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 2589 _refine_ls_number_parameters 126 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.002 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 Fe1 Fe 0.44705(19) 0.55221(19) 0.08185(15) 0.01183(8) Uani 1 1 d . . . P1 P 0.6152(3) 0.7836(3) 0.24577(8) 0.0085(4) Uani 1 1 d . . . P2 P 0.2162(3) 0.3845(3) -0.08242(7) 0.0103(4) Uani 1 1 d . . . B1 B 0.3002(3) 0.1509(13) -0.0841(9) 0.0101(4) Uiso 1 1 d . . . O1 O 0.7930(7) 0.8151(7) 0.2290(4) 0.0126(11) Uani 1 1 d . . . O2 O 0.1917(7) 0.2140(7) -0.0666(4) 0.0135(12) Uani 1 1 d . . . O3 O 0.2346(8) 0.4132(8) -0.1808(4) 0.0169(13) Uani 1 1 d . . . O4 O 0.5874(7) 0.7649(7) 0.3439(3) 0.0095(10) Uani 1 1 d . . . O5 O 0.4884(8) 0.6281(9) 0.2040(4) 0.0200(12) Uani 1 1 d . . . O6 O 0.3769(8) 0.5130(8) -0.0459(4) 0.0175(12) Uani 1 1 d . . . O7 O 0.0679(7) 0.3859(8) -0.0494(4) 0.0188(14) Uani 1 1 d . . . O8 O 0.6813(7) 0.6165(8) 0.0452(4) 0.0187(13) Uani 1 1 d . . . O9 O 0.5008(5) 0.7948(4) 0.0546(2) 0.0230(9) Uiso 1 1 d . . . O10 O 0.1846(4) 0.4690(5) 0.1213(2) 0.0203(7) Uiso 1 1 d . . . O11 O 0.1093(15) 0.1690(14) 0.2721(7) 0.077(3) Uiso 0.598(12) 1 d P . . N1 N 0.147(3) 0.262(2) 0.244(2) 0.077(3) Uiso 0.402(12) 1 d P . . Fe2 Fe 0.044(2) 0.370(2) 0.2470(12) 0.042(6) Uiso 0.051(4) 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 Fe1 0.0116(5) 0.0137(6) 0.01119(14) -0.0031(3) -0.0047(4) 0.00705(12) P1 0.0086(9) 0.0081(9) 0.0096(10) -0.0016(8) -0.0013(7) 0.0047(8) P2 0.0124(10) 0.0119(10) 0.0077(10) -0.0032(7) -0.0025(8) 0.0070(9) O1 0.012(2) 0.016(2) 0.013(3) 0.001(2) 0.0068(18) 0.010(2) O2 0.011(2) 0.013(2) 0.016(3) -0.0021(19) 0.0049(19) 0.005(2) O3 0.019(3) 0.017(3) 0.015(3) -0.007(2) -0.009(2) 0.010(2) O4 0.008(2) 0.014(3) 0.004(2) 0.002(2) 0.0041(19) 0.004(2) O5 0.017(3) 0.021(3) 0.019(2) -0.007(2) -0.003(2) 0.007(2) O6 0.012(2) 0.019(3) 0.013(2) -0.010(2) -0.0026(18) 0.002(2) O7 0.010(2) 0.031(3) 0.022(3) -0.006(3) -0.002(2) 0.015(2) O8 0.013(3) 0.018(3) 0.016(3) 0.002(2) -0.004(2) 0.001(2)