#------------------------------------------------------------------------------ #$Date: 2009-11-16 03:43:51 +0200 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2016303.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2016303 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M P21/n loop_ _publ_author_name 'Franziska Emmerling' 'Werner Kraus' 'Bernhard Noll' 'Steffi Noll' 'Hans-J\"urgen Pietzsch' _publ_section_title ;\ Two mononuclear Tc complexes: [2,2'-(3-phenylpropylimino)- and [2,2'-(propylimino)bis(ethanethiolato)](4-methoxybenzenethiolato)\ oxidotechnate(V) ; _journal_coeditor_code BG3060 _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m579 _journal_page_last m582 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Tc (C7 H15 N S2) (C7 H7 O S) O]' _chemical_formula_moiety 'C14 H22 N O2 S3 Tc' _chemical_formula_sum 'C14 H22 N O2 S3 Tc' _chemical_formula_weight 430.51 _chemical_name_systematic ; (4-methoxybenzenethiolato-\kS)oxido[2,2'-(propylimino)bis(ethanethiolato)- \k^3^S,N,S']technetium(V) ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 90.574(15) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.610(7) _cell_length_b 10.356(7) _cell_length_c 16.296(11) _cell_measurement_reflns_used 907 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 24.351 _cell_measurement_theta_min 3.021 _cell_volume 1790(2) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXTL (Bruker, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method \w _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 0.0921 _diffrn_reflns_av_sigmaI/netI 0.1264 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 10232 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_min 2.28 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.923 _refine_diff_density_min -0.601 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.864 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 4031 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.873 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0617 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0371P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.0954 _reflns_number_gt 1809 _reflns_number_total 4031 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bg3060.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Tc Tc1 0.76655(4) 0.24888(5) 0.15162(3) 0.05211(17) Uani d . 1 S S1 0.89303(16) 0.08218(15) 0.11159(12) 0.0775(5) Uani d . 1 S S2 0.60719(13) 0.21855(13) 0.24244(10) 0.0629(4) Uani d . 1 S S3 0.63174(15) 0.16995(16) 0.05143(10) 0.0729(5) Uani d . 1 O O1 0.8032(3) 0.3985(3) 0.1219(2) 0.0648(10) Uani d . 1 O O2 0.1240(4) 0.4098(5) 0.0654(3) 0.0811(13) Uani d . 1 N N1 0.8856(4) 0.2457(4) 0.2630(3) 0.0565(11) Uani d . 1 C C1 0.9964(5) 0.0625(6) 0.2008(5) 0.083(2) Uani d . 1 H H1B 1.0166 -0.0282 0.2082 0.099 Uiso calc R 1 H H1C 1.0744 0.1091 0.1922 0.099 Uiso calc R 1 C C2 0.9322(5) 0.1132(6) 0.2764(4) 0.0718(18) Uani d . 1 H H2A 0.8622 0.0573 0.2901 0.086 Uiso calc R 1 H H2B 0.9913 0.1127 0.3222 0.086 Uiso calc R 1 C C3 0.6871(5) 0.2281(6) 0.3424(3) 0.0665(17) Uani d . 1 H H3A 0.6345 0.2753 0.3804 0.080 Uiso calc R 1 H H3B 0.6993 0.1417 0.3640 0.080 Uiso calc R 1 C C4 0.8121(5) 0.2941(6) 0.3358(4) 0.0701(17) Uani d . 1 H H4A 0.8607 0.2790 0.3857 0.084 Uiso calc R 1 H H4B 0.7991 0.3864 0.3305 0.084 Uiso calc R 1 C C5 0.4808(5) 0.2437(6) 0.0622(3) 0.0604(14) Uani d . 1 C C6 0.4681(5) 0.3750(6) 0.0706(4) 0.0656(17) Uani d . 1 H H6A 0.5402 0.4257 0.0751 0.079 Uiso calc R 1 C C7 0.3506(6) 0.4341(6) 0.0726(4) 0.0668(17) Uani d . 1 H H7A 0.3445 0.5230 0.0794 0.080 Uiso calc R 1 C C8 0.2429(5) 0.3597(7) 0.0644(3) 0.0586(15) Uani d . 1 C C9 0.2546(6) 0.2278(6) 0.0560(4) 0.0670(17) Uani d . 1 H H9A 0.1824 0.1774 0.0508 0.080 Uiso calc R 1 C C10 0.3700(7) 0.1698(6) 0.0552(3) 0.0673(17) Uani d . 1 H H10A 0.3755 0.0806 0.0500 0.081 Uiso calc R 1 C C11 0.1083(5) 0.5442(7) 0.0804(4) 0.088(2) Uani d . 1 H H11A 0.0201 0.5652 0.0790 0.132 Uiso calc R 1 H H11B 0.1511 0.5927 0.0390 0.132 Uiso calc R 1 H H11C 0.1429 0.5653 0.1334 0.132 Uiso calc R 1 C C12 0.9946(5) 0.3386(5) 0.2497(3) 0.0617(16) Uani d D 1 H H12A 1.0377 0.3149 0.1997 0.074 Uiso calc R 1 H H12B 0.9612 0.4251 0.2423 0.074 Uiso calc R 1 C C13 1.0879(6) 0.3397(6) 0.3194(4) 0.096(2) Uani d D 1 H H13A 1.0699 0.4143 0.3534 0.115 Uiso calc R 1 H H13B 1.0730 0.2636 0.3526 0.115 Uiso calc R 1 C C14 1.2210(6) 0.3429(12) 0.2996(5) 0.181(5) Uani d D 1 H H14A 1.2701 0.3413 0.3494 0.271 Uiso calc R 1 H H14B 1.2392 0.4204 0.2697 0.271 Uiso calc R 1 H H14C 1.2416 0.2691 0.2667 0.271 Uiso calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Tc1 0.0671(3) 0.0422(3) 0.0469(3) 0.0030(3) -0.0028(2) -0.0003(3) S1 0.0841(11) 0.0586(10) 0.0901(14) 0.0114(9) 0.0079(10) -0.0129(9) S2 0.0671(9) 0.0645(11) 0.0569(10) -0.0041(7) -0.0024(8) -0.0008(8) S3 0.0894(11) 0.0705(11) 0.0586(11) 0.0107(9) -0.0136(9) -0.0207(9) O1 0.092(3) 0.046(2) 0.056(3) -0.005(2) -0.005(2) 0.008(2) O2 0.063(3) 0.102(4) 0.078(3) -0.002(3) -0.003(2) -0.006(3) N1 0.066(3) 0.050(3) 0.053(3) -0.004(3) -0.003(2) 0.008(3) C1 0.068(4) 0.057(4) 0.123(7) 0.011(3) -0.001(4) 0.009(4) C2 0.072(4) 0.061(4) 0.082(5) 0.005(3) -0.003(4) 0.024(4) C3 0.074(4) 0.077(5) 0.049(4) -0.005(3) -0.002(3) 0.011(3) C4 0.078(4) 0.080(4) 0.052(4) -0.003(3) -0.006(3) 0.003(3) C5 0.073(4) 0.060(4) 0.047(3) -0.008(4) -0.012(3) -0.007(3) C6 0.062(4) 0.063(4) 0.071(5) -0.007(3) -0.017(3) -0.005(3) C7 0.074(4) 0.063(4) 0.063(5) 0.002(3) -0.016(3) -0.009(3) C8 0.062(4) 0.080(5) 0.033(4) -0.001(3) -0.005(3) 0.002(3) C9 0.073(4) 0.070(5) 0.057(4) -0.022(4) -0.005(3) -0.005(3) C10 0.102(5) 0.057(4) 0.042(4) -0.013(4) -0.003(4) -0.005(3) C11 0.071(4) 0.109(6) 0.084(5) 0.020(4) 0.000(4) 0.002(5) C12 0.073(4) 0.058(4) 0.054(4) -0.010(3) -0.008(3) 0.007(3) C13 0.122(6) 0.076(5) 0.090(6) -0.036(4) -0.028(5) 0.012(4) C14 0.100(6) 0.323(15) 0.120(8) -0.076(8) -0.026(6) 0.035(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Tc1 O1 1.671(3) yes Tc1 N1 2.201(4) yes Tc1 S2 2.2801(19) yes Tc1 S1 2.2856(19) yes Tc1 S3 2.3093(19) yes S1 C1 1.824(7) ? S2 C3 1.831(6) ? S3 C5 1.785(6) ? O2 C8 1.364(6) ? O2 C11 1.424(7) ? N1 C2 1.474(6) ? N1 C4 1.512(7) ? N1 C12 1.521(6) ? C1 C2 1.508(8) ? C1 H1B 0.9700 ? C1 H1C 0.9700 ? C2 H2A 0.9700 ? C2 H2B 0.9700 ? C3 C4 1.497(7) ? C3 H3A 0.9700 ? C3 H3B 0.9700 ? C4 H4A 0.9700 ? C4 H4B 0.9700 ? C5 C6 1.373(7) ? C5 C10 1.406(7) ? C6 C7 1.389(7) ? C6 H6A 0.9300 ? C7 C8 1.383(7) ? C7 H7A 0.9300 ? C8 C9 1.379(8) ? C9 C10 1.364(7) ? C9 H9A 0.9300 ? C10 H10A 0.9300 ? C11 H11A 0.9600 ? C11 H11B 0.9600 ? C11 H11C 0.9600 ? C12 C13 1.499(6) ? C12 H12A 0.9700 ? C12 H12B 0.9700 ? C13 C14 1.452(5) ? C13 H13A 0.9700 ? C13 H13B 0.9700 ? C14 H14A 0.9600 ? C14 H14B 0.9600 ? C14 H14C 0.9600 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 Tc1 N1 96.88(17) O1 Tc1 S2 119.49(14) N1 Tc1 S2 83.45(13) O1 Tc1 S1 118.61(15) N1 Tc1 S1 83.70(13) S2 Tc1 S1 121.50(7) O1 Tc1 S3 105.52(14) N1 Tc1 S3 157.51(13) S2 Tc1 S3 87.25(8) S1 Tc1 S3 83.81(7) C1 S1 Tc1 102.0(2) C3 S2 Tc1 103.31(19) C5 S3 Tc1 109.2(2) C8 O2 C11 118.9(5) C2 N1 C4 111.5(5) C2 N1 C12 110.8(4) C4 N1 C12 107.5(4) C2 N1 Tc1 109.0(3) C4 N1 Tc1 110.3(3) C12 N1 Tc1 107.7(3) C2 C1 S1 109.8(4) C2 C1 H1B 109.7 S1 C1 H1B 109.7 C2 C1 H1C 109.7 S1 C1 H1C 109.7 H1B C1 H1C 108.2 N1 C2 C1 110.9(5) N1 C2 H2A 109.5 C1 C2 H2A 109.5 N1 C2 H2B 109.5 C1 C2 H2B 109.5 H2A C2 H2B 108.1 C4 C3 S2 111.3(4) C4 C3 H3A 109.4 S2 C3 H3A 109.4 C4 C3 H3B 109.4 S2 C3 H3B 109.4 H3A C3 H3B 108.0 C3 C4 N1 111.7(4) C3 C4 H4A 109.3 N1 C4 H4A 109.3 C3 C4 H4B 109.3 N1 C4 H4B 109.3 H4A C4 H4B 107.9 C6 C5 C10 117.6(5) C6 C5 S3 121.5(4) C10 C5 S3 120.6(5) C5 C6 C7 121.8(5) C5 C6 H6A 119.1 C7 C6 H6A 119.1 C8 C7 C6 119.6(6) C8 C7 H7A 120.2 C6 C7 H7A 120.2 O2 C8 C9 117.5(6) O2 C8 C7 123.4(6) C9 C8 C7 119.1(6) C10 C9 C8 121.2(5) C10 C9 H9A 119.4 C8 C9 H9A 119.4 C9 C10 C5 120.7(5) C9 C10 H10A 119.7 C5 C10 H10A 119.7 O2 C11 H11A 109.5 O2 C11 H11B 109.5 H11A C11 H11B 109.5 O2 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C13 C12 N1 113.2(5) C13 C12 H12A 108.9 N1 C12 H12A 108.9 C13 C12 H12B 108.9 N1 C12 H12B 108.9 H12A C12 H12B 107.7 C14 C13 C12 117.9(6) C14 C13 H13A 107.8 C12 C13 H13A 107.8 C14 C13 H13B 107.8 C12 C13 H13B 107.8 H13A C13 H13B 107.2 C13 C14 H14A 109.5 C13 C14 H14B 109.5 H14A C14 H14B 109.5 C13 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C3 H3B O1 2_645 0.97 2.53 3.464(7) 162 C12 H12A O2 1_655 0.97 2.58 3.396(7) 142