#------------------------------------------------------------------------------ #$Date: 2014-07-11 23:16:09 +0100 (Fri, 11 Jul 2014) $ #$Revision: 120081 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/85/4308551.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_4308551 loop_ _publ_author_name 'Jean-Claude Berthet' 'Pierre Thu\'ery' 'Michel Ephritikhine' _publ_contact_author_address ; CEA/Saclay, SCM (CNRS URA 331) B\^at. 125 91191 Gif-sur-Yvette France ; _publ_contact_author_email ephri@drecam.cea.fr _publ_contact_author_fax '33 (1) 69 08 66 40' _publ_contact_author_name 'M. Ephritikhine' _publ_contact_author_phone '33 (1) 69 08 64 36' _publ_section_title ; New Efficient Synthesis of [UI4(MeCN)4]. X-ray Crystal Structures of [UI2(MeCN)7][UI6], [UI4(py)3], and [U(dmf)9]I4 ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1142 _journal_page_last 1146 _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C15 H15 I4 N3 U' _chemical_formula_weight 982.93 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary patter _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 107.094(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.3294(3) _cell_length_b 13.1236(5) _cell_length_c 15.4734(6) _cell_measurement_reflns_used 14135 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.68 _cell_measurement_theta_min 3.06 _cell_volume 2198.99(14) _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'Kappa-CCD software (Nonius B.V., 1998)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1999)' _computing_publication_material 'SHELXTL (Sheldrick, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.896 _diffrn_measured_fraction_theta_max 0.896 _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 14135 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 3.06 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _exptl_absorpt_coefficient_mu 12.999 _exptl_absorpt_correction_T_max 0.349 _exptl_absorpt_correction_T_min 0.168 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details 'program DELABS from PLATON (Spek, 2000)' _exptl_crystal_colour 'translucent dark red' _exptl_crystal_density_diffrn 2.969 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 1720 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.784 _refine_diff_density_min -0.921 _refine_diff_density_rms 0.131 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3741 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.107 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0255 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+6.7946P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.0603 _reflns_number_gt 3558 _reflns_number_total 3741 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic048603psi20041007_101646_3.cif _[local]_cod_data_source_block 3 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 4308551 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' 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 U U 0.741839(18) 0.122340(15) 0.802055(13) 0.02101(8) Uani 1 1 d . . . I1 I 0.74853(4) -0.08953(3) 0.87364(2) 0.02736(10) Uani 1 1 d . . . I2 I 0.88800(3) 0.19397(3) 0.99017(2) 0.02652(10) Uani 1 1 d . . . I3 I 0.48945(3) 0.07745(3) 0.67459(2) 0.02946(10) Uani 1 1 d . . . I4 I 0.73667(4) 0.33097(3) 0.72906(3) 0.03260(11) Uani 1 1 d . . . N1 N 0.9716(5) 0.1274(4) 0.8024(3) 0.0244(10) Uani 1 1 d . . . N2 N 0.7870(5) 0.0320(4) 0.6631(3) 0.0258(10) Uani 1 1 d . . . N3 N 0.5828(5) 0.1852(4) 0.8805(3) 0.0270(10) Uani 1 1 d . . . C1 C 1.0104(6) 0.1755(5) 0.7378(4) 0.0281(13) Uani 1 1 d . . . H1A H 0.9536 0.2149 0.6953 0.034 Uiso 1 1 calc R . . C2 C 1.1278(6) 0.1691(5) 0.7317(4) 0.0323(14) Uani 1 1 d . . . H2A H 1.1498 0.2032 0.6861 0.039 Uiso 1 1 calc R . . C3 C 1.2144(6) 0.1108(5) 0.7949(4) 0.0343(14) Uani 1 1 d . . . H3A H 1.2954 0.1055 0.7930 0.041 Uiso 1 1 calc R . . C4 C 1.1759(6) 0.0615(5) 0.8603(4) 0.0335(14) Uani 1 1 d . . . H4A H 1.2316 0.0217 0.9032 0.040 Uiso 1 1 calc R . . C5 C 1.0555(5) 0.0702(4) 0.8629(4) 0.0247(12) Uani 1 1 d . . . H5A H 1.0316 0.0357 0.9075 0.030 Uiso 1 1 calc R . . C6 C 0.7454(6) 0.0731(5) 0.5807(4) 0.0306(13) Uani 1 1 d . . . H6A H 0.6932 0.1293 0.5727 0.037 Uiso 1 1 calc R . . C7 C 0.7767(6) 0.0356(5) 0.5062(4) 0.0312(13) Uani 1 1 d . . . H7A H 0.7468 0.0667 0.4500 0.037 Uiso 1 1 calc R . . C8 C 0.8532(6) -0.0489(5) 0.5172(4) 0.0367(15) Uani 1 1 d . . . H8A H 0.8749 -0.0759 0.4685 0.044 Uiso 1 1 calc R . . C9 C 0.8958(6) -0.0915(5) 0.6012(4) 0.0349(14) Uani 1 1 d . . . H9A H 0.9473 -0.1482 0.6101 0.042 Uiso 1 1 calc R . . C10 C 0.8630(6) -0.0507(5) 0.6727(4) 0.0292(13) Uani 1 1 d . . . H10A H 0.8935 -0.0804 0.7295 0.035 Uiso 1 1 calc R . . C11 C 0.5136(6) 0.2697(5) 0.8575(4) 0.0318(13) Uani 1 1 d . . . H11A H 0.5225 0.3084 0.8095 0.038 Uiso 1 1 calc R . . C12 C 0.4311(6) 0.3019(5) 0.9005(5) 0.0350(14) Uani 1 1 d . . . H12A H 0.3852 0.3609 0.8819 0.042 Uiso 1 1 calc R . . C13 C 0.4166(6) 0.2457(5) 0.9721(4) 0.0329(14) Uani 1 1 d . . . H13A H 0.3608 0.2658 1.0025 0.039 Uiso 1 1 calc R . . C14 C 0.4872(6) 0.1583(5) 0.9975(4) 0.0311(13) Uani 1 1 d . . . H14A H 0.4794 0.1188 1.0454 0.037 Uiso 1 1 calc R . . C15 C 0.5689(6) 0.1308(5) 0.9513(4) 0.0303(13) Uani 1 1 d . . . H15A H 0.6165 0.0725 0.9692 0.036 Uiso 1 1 calc R . . 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 U 0.02108(14) 0.02123(12) 0.02131(11) 0.00076(7) 0.00713(8) 0.00038(7) I1 0.0330(2) 0.0229(2) 0.02931(19) 0.00289(14) 0.01387(15) 0.00204(15) I2 0.0261(2) 0.0302(2) 0.02298(18) -0.00325(14) 0.00685(13) 0.00065(14) I3 0.0226(2) 0.0343(2) 0.0302(2) -0.00330(15) 0.00566(14) -0.00138(15) I4 0.0365(2) 0.0279(2) 0.0345(2) 0.00590(15) 0.01221(16) 0.00189(16) N1 0.025(3) 0.026(3) 0.023(2) -0.0014(18) 0.0074(18) 0.0011(19) N2 0.026(3) 0.027(3) 0.025(2) -0.0043(19) 0.0079(18) -0.006(2) N3 0.030(3) 0.026(3) 0.027(2) -0.0014(19) 0.0108(19) -0.003(2) C1 0.030(4) 0.032(3) 0.025(3) -0.001(2) 0.011(2) -0.004(2) C2 0.038(4) 0.030(3) 0.033(3) -0.008(2) 0.017(3) -0.011(3) C3 0.025(4) 0.040(4) 0.042(4) -0.010(3) 0.016(3) -0.005(3) C4 0.031(4) 0.037(4) 0.032(3) -0.006(3) 0.008(2) 0.004(3) C5 0.028(3) 0.027(3) 0.021(3) -0.002(2) 0.009(2) 0.000(2) C6 0.026(3) 0.030(3) 0.034(3) -0.002(2) 0.007(2) -0.009(2) C7 0.036(4) 0.036(3) 0.023(3) -0.005(2) 0.010(2) -0.011(3) C8 0.037(4) 0.044(4) 0.036(3) -0.012(3) 0.020(3) -0.007(3) C9 0.032(4) 0.036(4) 0.041(4) -0.006(3) 0.017(3) -0.003(3) C10 0.028(3) 0.029(3) 0.032(3) -0.004(2) 0.010(2) -0.002(2) C11 0.028(4) 0.030(3) 0.039(3) 0.006(3) 0.013(2) 0.005(2) C12 0.031(4) 0.028(3) 0.053(4) 0.003(3) 0.022(3) 0.005(3) C13 0.029(4) 0.033(4) 0.042(3) -0.016(3) 0.018(3) -0.005(3) C14 0.029(4) 0.036(4) 0.028(3) 0.002(2) 0.008(2) 0.002(3) C15 0.029(4) 0.030(3) 0.029(3) 0.000(2) 0.004(2) 0.007(2) 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 0.0000 0.0000 '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' I I -0.4742 1.8119 '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 _geom_angle_publ_flag N3 U N1 145.64(15) . . ? N3 U N2 148.89(15) . . ? N1 U N2 65.10(15) . . ? N3 U I4 86.87(11) . . ? N1 U I4 83.38(11) . . ? N2 U I4 95.27(11) . . ? N3 U I1 93.92(11) . . ? N1 U I1 96.12(11) . . ? N2 U I1 83.90(11) . . ? I4 U I1 179.157(13) . . ? N3 U I3 73.24(11) . . ? N1 U I3 139.63(10) . . ? N2 U I3 75.68(11) . . ? I4 U I3 91.293(12) . . ? I1 U I3 88.654(12) . . ? N3 U I2 73.21(11) . . ? N1 U I2 74.17(10) . . ? N2 U I2 137.55(11) . . ? I4 U I2 91.342(12) . . ? I1 U I2 89.170(12) . . ? I3 U I2 146.135(12) . . ? C5 N1 C1 117.0(5) . . ? C5 N1 U 119.2(4) . . ? C1 N1 U 123.3(4) . . ? C6 N2 C10 117.3(5) . . ? C6 N2 U 119.9(4) . . ? C10 N2 U 122.5(4) . . ? C11 N3 C15 116.8(5) . . ? C11 N3 U 124.9(4) . . ? C15 N3 U 118.3(4) . . ? N1 C1 C2 123.7(6) . . ? C1 C2 C3 119.0(6) . . ? C4 C3 C2 117.7(6) . . ? C3 C4 C5 120.8(6) . . ? N1 C5 C4 121.8(6) . . ? N2 C6 C7 122.9(6) . . ? C8 C7 C6 118.9(6) . . ? C9 C8 C7 118.5(6) . . ? C8 C9 C10 120.2(6) . . ? N2 C10 C9 122.2(6) . . ? N3 C11 C12 123.8(6) . . ? C11 C12 C13 119.1(6) . . ? C12 C13 C14 118.3(6) . . ? C15 C14 C13 119.4(6) . . ? N3 C15 C14 122.6(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U N3 2.586(5) . ? U N1 2.602(5) . ? U N2 2.634(5) . ? U I4 2.9558(4) . ? U I1 2.9857(4) . ? U I3 3.0163(4) . ? U I2 3.0438(4) . ? N1 C5 1.349(8) . ? N1 C1 1.361(7) . ? N2 C6 1.337(8) . ? N2 C10 1.366(8) . ? N3 C11 1.343(8) . ? N3 C15 1.355(8) . ? C1 C2 1.363(9) . ? C2 C3 1.393(10) . ? C3 C4 1.375(9) . ? C4 C5 1.381(9) . ? C6 C7 1.392(9) . ? C7 C8 1.386(10) . ? C8 C9 1.367(10) . ? C9 C10 1.375(9) . ? C11 C12 1.365(9) . ? C12 C13 1.380(9) . ? C13 C14 1.387(9) . ? C14 C15 1.374(9) . ? _journal_paper_doi 10.1021/ic048603p