#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/4/11/64/4116492.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_4116492 loop_ _publ_author_name 'P. S. Halasyamani' 'S. M. Walker' 'D. O'Hare' _publ_section_title ; The First Open Framework Actinide Material (C4N2H12)U2O4F6 (MUF-1) ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7415 _journal_page_last 7416 _journal_paper_doi 10.1021/ja9912271 _journal_volume 121 _journal_year 1999 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'C4 H12 F6 N2 O2 U2' _chemical_formula_structural 'C4 N2 H12 U2 O2 F6' _chemical_formula_sum 'C4 H12 F6 N2 O2 U2' _chemical_formula_weight 744.23 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_creation_date 1999-02-23T10:25:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 97.0230(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.1080(10) _cell_length_b 10.0590(10) _cell_length_c 13.6330(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 150.0(1) _cell_measurement_theta_max 2.49 _cell_measurement_theta_min 2.49 _cell_measurement_wavelength 0.71073 _cell_volume 1239.6(2) _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.03 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2312 _diffrn_reflns_theta_max 26.51 _diffrn_reflns_theta_min 3.01 _exptl_absorpt_coefficient_mu 26.179 _exptl_absorpt_correction_T_max 0.1205 _exptl_absorpt_correction_T_min 0.0601 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 3.988 _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 1288 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _refine_diff_density_max 2.486 _refine_diff_density_min -3.269 _refine_diff_density_rms 0.407 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.103 _refine_ls_goodness_of_fit_gt 1.103 _refine_ls_matrix_type full _refine_ls_number_parameters 71 _refine_ls_number_reflns 1234 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.103 _refine_ls_restrained_S_obs 1.103 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0399 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+117.9577P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1031 _refine_ls_wR_factor_gt 0.1029 _reflns_number_gt 1227 _reflns_number_total 1234 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ja9912271.cif _[local]_cod_data_source_block JA9912271-112 _[local]_cod_cif_authors_sg_H-M 'C 2/c' _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+117.9577P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+117.9577P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 4116492 #BEGIN Tags that were not found in dictionaries: _exptl_absorpt_factor_mur 2.398 _exptl_absorpt_correction_t_ave 0.0918 #END Tags that were not found in dictionaries loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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_calc_flag _atom_site_refinement_flags U1 U 0.41310(4) 0.38489(4) 0.09271(3) 0.0060(2) Uani 1 d . F1 F 0.5755(9) 0.5582(8) 0.0721(6) 0.019(2) Uani 1 d . F2 F 0.25 0.25 0 0.033(3) Uani 1 d S F3 F 0.3286(10) 0.2506(8) 0.1998(6) 0.023(2) Uani 1 d . F4 F 0.5 0.4697(10) 0.25 0.015(2) Uani 1 d S O1 O 0.5599(10) 0.2717(10) 0.0833(8) 0.019(2) Uani 1 d . O2 O 0.2657(12) 0.4996(10) 0.0986(8) 0.026(2) Uani 1 d . N1 N 0.5 0.025(3) 0.25 0.058(7) Uiso 1 d S H1A H 0.5714 0.082(3) 0.2252 0.073 Uiso 0.5 calc PR H1B H 0.4286 0.082(3) 0.2748 0.073 Uiso 0.5 calc PR N2 N 0.537(2) 0.748(2) 0.2421(19) 0.016(5) Uiso 0.5 d P C1 C 0.4252(17) -0.0410(15) 0.1673(12) 0.026(3) Uiso 1 d . H1C H 0.4657(17) -0.0097(15) 0.1097(12) 0.033 Uiso 1 calc R H1D H 0.3236(17) -0.0135(15) 0.1609(12) 0.033 Uiso 1 calc R C2 C 0.4278(18) 0.8127(17) 0.1653(13) 0.029(3) Uiso 1 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 U1 0.0063(2) 0.0061(3) 0.0056(3) 0.00058(14) 0.0006(2) -0.00184(14) F1 0.032(4) 0.014(4) 0.011(4) 0.000(3) -0.001(3) -0.018(3) F2 0.043(8) 0.040(8) 0.014(6) 0.004(5) -0.001(5) -0.035(6) F3 0.036(5) 0.017(4) 0.018(4) 0.004(3) 0.012(4) -0.013(3) F4 0.026(6) 0.010(5) 0.008(5) 0 0.002(4) 0 O1 0.014(4) 0.018(5) 0.023(5) -0.006(4) -0.002(4) 0.009(4) O2 0.023(5) 0.021(5) 0.032(6) -0.004(4) -0.002(4) 0.017(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 U1 O2 178.4(5) . . O1 U1 F3 89.0(4) . . O2 U1 F3 92.4(5) . . O1 U1 F2 91.4(3) . . O2 U1 F2 88.1(4) . . F3 U1 F2 75.2(2) . . O1 U1 F1 88.6(4) . . O2 U1 F1 90.8(4) . . F3 U1 F1 145.2(3) . . F2 U1 F1 139.6(2) . . O1 U1 F1 88.0(4) . 5_665 O2 U1 F1 90.4(4) . 5_665 F3 U1 F1 148.4(3) . 5_665 F2 U1 F1 73.4(2) . 5_665 F1 U1 F1 66.2(3) . 5_665 O1 U1 F4 97.3(3) . . O2 U1 F4 84.0(4) . . F3 U1 F4 73.9(3) . . F2 U1 F4 147.74(13) . . F1 U1 F4 71.9(3) . . F1 U1 F4 137.6(3) 5_665 . O1 U1 U1 88.0(3) . 5_665 O2 U1 U1 90.7(4) . 5_665 F3 U1 U1 176.6(2) . 5_665 F2 U1 U1 106.42(2) . 5_665 F1 U1 U1 33.2(2) . 5_665 F1 U1 U1 33.0(2) 5_665 5_665 F4 U1 U1 104.9(2) . 5_665 U1 F1 U1 113.8(3) . 5_665 U1 F2 U1 180 . 7 U1 F4 U1 137.5(5) 2_655 . C1 N1 C1 124(3) 2_655 . N2 N2 C2 82(4) 2_655 2_655 N2 N2 C2 70(3) 2_655 . C2 N2 C2 118.5(19) 2_655 . N1 C1 C2 118.5(16) . 1_545 N2 C2 C1 116.4(15) 2_655 1_565 N2 C2 N2 28.8(15) 2_655 . C1 C2 N2 115.6(15) 1_565 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 U1 O1 1.773(9) . U1 O2 1.779(9) . U1 F1 2.325(7) . U1 F1 2.334(8) 5_665 U1 F2 2.2774(4) . U1 F3 2.196(8) . U1 F4 2.353(4) . U1 U1 3.9035(8) 5_665 F1 U1 2.334(8) 5_665 F2 U1 2.2774(4) 7 F4 U1 2.353(4) 2_655 N1 C1 1.41(2) 2_655 N1 C1 1.41(2) . N2 N2 0.73(4) 2_655 N2 C2 1.42(3) 2_655 N2 C2 1.50(3) . C1 C2 1.47(2) 1_545 C2 N2 1.42(3) 2_655 C2 C1 1.47(2) 1_565