#------------------------------------------------------------------------------ #$Date: 2013-02-26 18:13:55 +0200 (Tue, 26 Feb 2013) $ #$Revision: 74361 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/72/4117292.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_4117292 loop_ _publ_author_name 'Nathan A. Siladke' 'Katie R. Meihaus' 'Joseph W. Ziller' 'Ming Fang' 'Filipp Furche' 'Jeffrey R. Long' 'William J. Evans' _publ_section_title ; Synthesis, Structure, and Magnetism of an f Element Nitrosyl Complex, (C5Me4H)3UNO ; _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 1243 _journal_page_last 1249 _journal_volume 134 _journal_year 2012 _chemical_absolute_configuration ad _chemical_formula_sum 'C27 H39 N O U' _chemical_formula_weight 631.62 _chemical_name_systematic ; ? ; _space_group_IT_number 198 _symmetry_cell_setting cubic _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _symmetry_space_group_name_H-M 'P 21 3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXTL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.4239(7) _cell_length_b 13.4239(7) _cell_length_c 13.4239(7) _cell_measurement_reflns_used 8469 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 28.27 _cell_measurement_theta_min 2.63 _cell_volume 2419.0(2) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 93(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w 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 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 21558 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 28.27 _diffrn_reflns_theta_min 1.52 _exptl_absorpt_coefficient_mu 6.728 _exptl_absorpt_correction_T_max 0.3772 _exptl_absorpt_correction_T_min 0.3323 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker SADABS' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_meas none _exptl_crystal_description irregular _exptl_crystal_F_000 1232 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.395 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.034(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 96 _refine_ls_number_reflns 1993 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0164 _refine_ls_R_factor_gt 0.0158 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+2.1163P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.0342 _reflns_number_gt 1940 _reflns_number_total 1993 _reflns_threshold_expression >2sigma(I) _journal_paper_doi 10.1021/ja2096128 _[local]_cod_data_source_file ja2096128_si_002.cif _[local]_cod_data_source_block nas35 _cod_database_code 4117292 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-y+1/2, -z, x+1/2' 'z+1/2, -x+1/2, -y' '-y, z+1/2, -x+1/2' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y+1/2, -z+1/2, -x' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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 U1 U 0.247157(5) 0.247157(5) 0.247157(5) 0.00982(4) Uani 1 3 d S N1 N 0.33375(17) 0.33375(17) 0.33375(17) 0.0155(9) Uani 1 3 d S O1 O 0.38668(15) 0.38668(15) 0.38668(15) 0.0194(8) Uani 1 3 d S C1 C 0.3016(2) 0.1358(2) 0.4111(2) 0.0160(6) Uani 1 1 d . C2 C 0.2034(2) 0.1667(2) 0.4355(2) 0.0160(7) Uani 1 1 d . C3 C 0.1356(2) 0.1172(2) 0.3706(2) 0.0148(6) Uani 1 1 d . C4 C 0.1925(2) 0.0587(2) 0.3036(2) 0.0155(6) Uani 1 1 d . C5 C 0.2942(2) 0.0706(2) 0.3295(2) 0.0150(6) Uani 1 1 d . H5A H 0.3487 0.0393 0.2969 0.018 Uiso 1 1 calc R C6 C 0.3936(2) 0.1572(3) 0.4715(3) 0.0224(7) Uani 1 1 d . H6A H 0.3871 0.1265 0.5374 0.034 Uiso 1 1 calc R H6B H 0.4015 0.2294 0.4790 0.034 Uiso 1 1 calc R H6C H 0.4520 0.1297 0.4375 0.034 Uiso 1 1 calc R C7 C 0.1771(2) 0.2315(2) 0.5236(2) 0.0232(7) Uani 1 1 d . H7A H 0.1789 0.1915 0.5846 0.035 Uiso 1 1 calc R H7B H 0.1101 0.2590 0.5144 0.035 Uiso 1 1 calc R H7C H 0.2253 0.2861 0.5288 0.035 Uiso 1 1 calc R C8 C 0.0239(2) 0.1101(2) 0.3835(2) 0.0206(6) Uani 1 1 d . H8A H -0.0092 0.1362 0.3240 0.031 Uiso 1 1 calc R H8B H 0.0036 0.1492 0.4418 0.031 Uiso 1 1 calc R H8C H 0.0049 0.0403 0.3933 0.031 Uiso 1 1 calc R C9 C 0.1486(2) -0.0125(2) 0.2279(3) 0.0240(7) Uani 1 1 d . H9A H 0.1866 -0.0748 0.2282 0.036 Uiso 1 1 calc R H9B H 0.1519 0.0176 0.1614 0.036 Uiso 1 1 calc R H9C H 0.0790 -0.0263 0.2449 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 U1 0.00982(4) 0.00982(4) 0.00982(4) 0.00009(6) 0.00009(6) 0.00009(6) N1 0.0155(9) 0.0155(9) 0.0155(9) -0.0015(9) -0.0015(9) -0.0015(9) O1 0.0194(8) 0.0194(8) 0.0194(8) -0.0040(8) -0.0040(8) -0.0040(8) C1 0.0184(15) 0.0164(16) 0.0132(14) 0.0059(12) -0.0026(12) -0.0012(12) C2 0.0195(15) 0.0163(15) 0.0123(14) 0.0020(11) -0.0004(11) -0.0032(11) C3 0.0173(14) 0.0134(14) 0.0136(14) 0.0029(11) 0.0012(11) -0.0024(10) C4 0.0179(16) 0.0118(14) 0.0167(16) 0.0012(11) -0.0005(12) -0.0033(11) C5 0.0165(15) 0.0114(13) 0.0171(15) 0.0048(12) 0.0010(11) 0.0014(11) C6 0.0213(16) 0.0251(17) 0.0208(16) 0.0057(13) -0.0063(13) -0.0053(13) C7 0.0317(17) 0.0227(16) 0.0152(13) -0.0009(13) 0.0023(12) 0.0000(14) C8 0.0169(15) 0.0219(16) 0.0229(17) 0.0065(13) 0.0021(12) -0.0044(13) C9 0.0254(15) 0.0186(14) 0.0280(17) -0.0030(13) 0.0001(14) -0.0050(12) 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' O O 0.0106 0.0060 '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 Cnt U1 N1 96.5 . . Cnt U1 Cnt 118.8 . . N1 U1 C5 97.82(6) . . N1 U1 C5 97.82(6) . 3 C5 U1 C5 118.18(3) . 3 N1 U1 C5 97.82(7) . 2 C5 U1 C5 118.18(3) . 2 C5 U1 C5 118.18(3) 3 2 N1 U1 C4 121.86(7) . . C5 U1 C4 30.24(9) . . C5 U1 C4 94.51(9) 3 . C5 U1 C4 124.76(9) 2 . N1 U1 C4 121.86(7) . 3 C5 U1 C4 124.75(9) . 3 C5 U1 C4 30.24(9) 3 3 C5 U1 C4 94.51(9) 2 3 C4 U1 C4 94.71(9) . 3 N1 U1 C4 121.86(7) . 2 C5 U1 C4 94.51(9) . 2 C5 U1 C4 124.76(9) 3 2 C5 U1 C4 30.24(9) 2 2 C4 U1 C4 94.71(9) . 2 C4 U1 C4 94.71(9) 3 2 N1 U1 C1 72.51(6) . . C5 U1 C1 29.86(9) . . C5 U1 C1 105.60(10) 3 . C5 U1 C1 136.13(9) 2 . C4 U1 C1 49.47(9) . . C4 U1 C1 127.43(9) 3 . C4 U1 C1 121.19(10) 2 . N1 U1 C1 72.51(6) . 2 C5 U1 C1 105.60(10) . 2 C5 U1 C1 136.13(9) 3 2 C5 U1 C1 29.86(9) 2 2 C4 U1 C1 127.43(9) . 2 C4 U1 C1 121.19(10) 3 2 C4 U1 C1 49.47(9) 2 2 C1 U1 C1 111.38(6) . 2 N1 U1 C1 72.51(6) . 3 C5 U1 C1 136.13(9) . 3 C5 U1 C1 29.86(9) 3 3 C5 U1 C1 105.60(10) 2 3 C4 U1 C1 121.19(10) . 3 C4 U1 C1 49.47(9) 3 3 C4 U1 C1 127.43(9) 2 3 C1 U1 C1 111.38(6) . 3 C1 U1 C1 111.38(6) 2 3 N1 U1 C2 79.81(6) . . C5 U1 C2 48.79(9) . . C5 U1 C2 76.28(9) 3 . C5 U1 C2 165.53(9) 2 . C4 U1 C2 48.77(9) . . C4 U1 C2 98.86(10) 3 . C4 U1 C2 141.73(10) 2 . C1 U1 C2 29.53(9) . . C1 U1 C2 139.09(9) 2 . C1 U1 C2 87.41(9) 3 . N1 U1 C2 79.81(6) . 3 C5 U1 C2 165.53(9) . 3 C5 U1 C2 48.79(9) 3 3 C5 U1 C2 76.28(9) 2 3 C4 U1 C2 141.73(10) . 3 C4 U1 C2 48.77(9) 3 3 C4 U1 C2 98.86(10) 2 3 C1 U1 C2 139.09(9) . 3 C1 U1 C2 87.41(9) 2 3 C1 U1 C2 29.53(9) 3 3 C2 U1 C2 116.94(4) . 3 N1 U1 C2 79.81(6) . 2 C5 U1 C2 76.28(9) . 2 C5 U1 C2 165.53(9) 3 2 C5 U1 C2 48.79(9) 2 2 C4 U1 C2 98.86(10) . 2 C4 U1 C2 141.73(10) 3 2 C4 U1 C2 48.77(9) 2 2 C1 U1 C2 87.41(9) . 2 C1 U1 C2 29.53(9) 2 2 C1 U1 C2 139.09(9) 3 2 C2 U1 C2 116.94(4) . 2 C2 U1 C2 116.94(4) 3 2 N1 U1 C3 108.83(5) . 2 C5 U1 C3 69.54(9) . 2 C5 U1 C3 151.24(8) 3 2 C5 U1 C3 48.80(9) 2 2 C4 U1 C3 80.75(8) . 2 C4 U1 C3 121.40(9) 3 2 C4 U1 C3 29.39(8) 2 2 C1 U1 C3 92.86(9) . 2 C1 U1 C3 48.69(8) 2 2 C1 U1 C3 154.33(9) 3 2 C2 U1 C3 118.23(9) . 2 C2 U1 C3 124.82(9) 3 2 C2 U1 C3 29.22(8) 2 2 N1 U1 C3 108.83(5) . 3 C5 U1 C3 151.24(8) . 3 C5 U1 C3 48.80(9) 3 3 C5 U1 C3 69.54(9) 2 3 C4 U1 C3 121.40(9) . 3 C4 U1 C3 29.39(8) 3 3 C4 U1 C3 80.75(8) 2 3 C1 U1 C3 154.33(9) . 3 C1 U1 C3 92.86(9) 2 3 C1 U1 C3 48.69(8) 3 3 C2 U1 C3 124.82(9) . 3 C2 U1 C3 29.22(8) 3 3 C2 U1 C3 118.23(9) 2 3 C3 U1 C3 110.10(5) 2 3 N1 U1 C3 108.83(5) . . C5 U1 C3 48.80(9) . . C5 U1 C3 69.54(9) 3 . C5 U1 C3 151.24(8) 2 . C4 U1 C3 29.39(8) . . C4 U1 C3 80.75(8) 3 . C4 U1 C3 121.40(9) 2 . C1 U1 C3 48.69(8) . . C1 U1 C3 154.33(9) 2 . C1 U1 C3 92.86(9) 3 . C2 U1 C3 29.22(8) . . C2 U1 C3 118.23(9) 3 . C2 U1 C3 124.82(9) 2 . C3 U1 C3 110.10(5) 2 . C3 U1 C3 110.10(5) 3 . O1 N1 U1 180.0(4) . . C5 C1 C2 107.2(3) . . C5 C1 C6 126.6(3) . . C2 C1 C6 125.5(3) . . C5 C1 U1 72.39(16) . . C2 C1 U1 77.28(18) . . C6 C1 U1 122.9(2) . . C1 C2 C3 108.3(3) . . C1 C2 C7 124.5(3) . . C3 C2 C7 126.8(3) . . C1 C2 U1 73.19(18) . . C3 C2 U1 76.24(16) . . C7 C2 U1 122.1(2) . . C4 C3 C2 107.7(3) . . C4 C3 C8 124.9(3) . . C2 C3 C8 126.3(3) . . C4 C3 U1 71.67(16) . . C2 C3 U1 74.53(16) . . C8 C3 U1 129.04(19) . . C3 C4 C5 107.5(3) . . C3 C4 C9 124.5(3) . . C5 C4 C9 127.6(3) . . C3 C4 U1 78.94(17) . . C5 C4 U1 72.94(18) . . C9 C4 U1 120.1(2) . . C1 C5 C4 109.2(3) . . C1 C5 U1 77.75(17) . . C4 C5 U1 76.82(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance U1 Cnt 2.491 U1 N1 2.013(4) U1 C5 2.691(3) U1 C4 2.741(3) U1 C1 2.759(3) U1 C2 2.812(3) U1 C3 2.834(3) N1 O1 1.231(5) C1 C5 1.406(4) C1 C2 1.421(4) C1 C6 1.505(4) C2 C3 1.424(4) C2 C7 1.509(4) C3 C4 1.417(4) C3 C8 1.513(4) C4 C5 1.417(4) C4 C9 1.515(4)