#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/4/4000105.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_4000105 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'H5 B Fe N O9 P2' _chemical_formula_weight 291.65 _symmetry_cell_setting 'monoclinic' _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.3698(11) _cell_length_b 8.3092(15) _cell_length_c 9.6800(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.049(13) _cell_angle_gamma 90.00 _cell_volume 737.04(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'rod-shaped' _exptl_crystal_colour 'pale-pink' _exptl_crystal_size_max '0.4' _exptl_crystal_size_mid '0.1' _exptl_crystal_size_min '0.1' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 11236 _diffrn_reflns_av_R_equivalents 0.1086 _diffrn_reflns_av_sigmaI/netI 0.1174 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.71 _reflns_number_total 2849 _reflns_number_gt 1761 _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^)+(0.0207P)^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_number_reflns 2849 _refine_ls_number_parameters 138 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0891 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_restrained_S_all 0.862 _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 0.78816(4) 0.15318(5) 0.57040(5) 0.00408(9) Uani 1 1 d . . . B1 B 0.6667(3) 0.5627(4) 0.8096(4) 0.0065(6) Uani 1 1 d . . . P1 P 0.92451(7) 0.06225(9) 0.29564(8) 0.00376(14) Uani 1 1 d . . . P2 P 0.57801(7) 0.24272(9) 0.78467(8) 0.00407(14) Uani 1 1 d . . . O1 O 0.9090(2) 0.1658(3) 0.4219(2) 0.0083(4) Uani 1 1 d . . . O2 O 0.9229(2) 0.0059(2) 0.6917(2) 0.0081(4) Uani 1 1 d . . . O3 O 0.8883(2) 0.3462(3) 0.6559(2) 0.0081(4) Uani 1 1 d . . . O4 O 0.6547(2) 0.1286(2) 0.7022(2) 0.0091(4) Uani 1 1 d . . . O5 O 0.5923(2) 0.4202(2) 0.7380(2) 0.0069(4) Uani 1 1 d . . . O6 O 0.8145(2) -0.0820(2) 0.2830(2) 0.0076(4) Uani 1 1 d . . . O7 O 0.4104(2) 0.2107(2) 0.7447(2) 0.0082(4) Uani 1 1 d . . . O8 O 0.6292(2) 0.2764(3) 0.4425(2) 0.0099(4) Uani 1 1 d . . . O9 O 0.6814(2) 0.5525(3) 0.9644(2) 0.0086(4) Uani 1 1 d . . . H1 H 0.610(4) 0.578(4) 0.991(4) 0.013 Uiso 1 1 d . . . N1 N 0.8167(3) 0.5967(4) 0.4388(4) 0.0211(7) Uiso 1 1 d D . . H2 H 0.827(3) 0.520(3) 0.495(3) 0.025 Uiso 1 1 d D . . H3 H 0.875(3) 0.666(3) 0.470(3) 0.025 Uiso 1 1 d D . . H4 H 0.734(2) 0.625(4) 0.421(3) 0.025 Uiso 1 1 d D . . H5 H 0.840(3) 0.562(4) 0.365(3) 0.025 Uiso 1 1 d D . . 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 0.00494(16) 0.00384(17) 0.0032(2) -0.00057(18) 0.00028(13) 0.00052(16) B1 0.0074(12) 0.0056(13) 0.0060(17) 0.0025(12) 0.0005(11) 0.0012(11) P1 0.0036(3) 0.0039(3) 0.0035(4) 0.0008(3) -0.0001(2) 0.0009(2) P2 0.0034(3) 0.0041(3) 0.0045(4) -0.0007(3) 0.0003(2) -0.0013(2) O1 0.0116(9) 0.0094(10) 0.0050(11) -0.0015(9) 0.0044(8) -0.0019(8) O2 0.0049(8) 0.0108(10) 0.0088(12) 0.0053(9) 0.0015(8) 0.0026(7) O3 0.0107(8) 0.0086(9) 0.0049(11) -0.0020(9) 0.0015(7) -0.0024(8) O4 0.0096(9) 0.0081(10) 0.0119(12) 0.0006(8) 0.0075(8) 0.0002(7) O5 0.0087(9) 0.0040(9) 0.0067(11) 0.0007(8) -0.0018(8) -0.0022(7) O6 0.0057(8) 0.0056(9) 0.0117(12) -0.0010(9) 0.0023(8) 0.0002(7) O7 0.0055(8) 0.0046(9) 0.0129(12) -0.0031(8) -0.0014(8) -0.0006(7) O8 0.0129(9) 0.0100(10) 0.0050(12) 0.0006(8) -0.0018(8) 0.0069(8) O9 0.0093(9) 0.0088(10) 0.0074(12) 0.0001(9) 0.0012(8) 0.0042(8)