#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/19/2011981.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_2011981 loop_ _publ_author_name 'Garc\'ia Font\'an, Soledad' 'Lamas Castro, Elvira' 'Rodr\'iguez Seoane, Pilar' 'V\'azquez-L\'opez, Ezequiel M.' _publ_section_title ; Tetracarbonyl(diphenyldithiophosphinato-S,S')rhenium(I) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 532 _journal_page_last 533 _journal_paper_doi 10.1107/S0108270101002190 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Re(C12 H10 PS2 )(CO)4 ]' _chemical_formula_moiety 'C16 H10 O4 P Re S2' _chemical_formula_sum 'C16 H10 O4 P Re S2' _chemical_formula_weight 547.53 _chemical_name_systematic ; Diphenyldithiophosphinato-tetracarbonylrhenium(I) ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 16.11600(10) _cell_length_b 12.8286(2) _cell_length_c 17.5930(3) _cell_measurement_temperature 293(2) _cell_volume 3637.28(9) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction 'SHELXTL (Sheldrick, 1995)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'CCD area detector' _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 .71073 _diffrn_reflns_av_R_equivalents .0848 _diffrn_reflns_av_sigmaI/netI .0598 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 23344 _diffrn_reflns_theta_full 28.30 _diffrn_reflns_theta_max 28.30 _diffrn_reflns_theta_min 2.32 _exptl_absorpt_coefficient_mu 7.015 _exptl_absorpt_correction_T_max .551 _exptl_absorpt_correction_T_min .271 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour 'light brown' _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2080 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _refine_diff_density_max 1.359 _refine_diff_density_min -3.522 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .977 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 217 _refine_ls_number_reflns 4518 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .977 _refine_ls_R_factor_all .0592 _refine_ls_R_factor_gt .0412 _refine_ls_shift/su_max .002 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0438P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0976 _reflns_number_gt 3181 _reflns_number_total 4518 _reflns_threshold_expression I>2\s(I) _cod_data_source_file jz1448.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2011981 _cod_database_fobs_code 2011981 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Re .311151(13) .025387(16) -.661550(12) .03976(9) Uani d . 1 . . Re S1 .34950(10) -.03238(10) -.52821(9) .0493(3) Uani d . 1 . . S S2 .32155(9) .19964(10) -.59206(8) .0502(3) Uani d . 1 . . S P .31646(8) .11232(10) -.49654(7) .0382(3) Uani d . 1 . . P O1 .1201(3) .0140(5) -.6340(4) .0928(17) Uani d . 1 . . O O2 .5010(3) .0495(4) -.6936(4) .0903(16) Uani d . 1 . . O O3 .3092(2) -.1966(3) -.7265(3) .0617(12) Uani d . 1 . . O O4 .2643(4) .1141(4) -.8171(3) .0886(17) Uani d . 1 . . O C1 .1895(4) .0176(5) -.6418(5) .0591(17) Uani d . 1 . . C C2 .4330(5) .0391(4) -.6818(4) .0553(15) Uani d . 1 . . C C3 .3103(3) -.1135(5) -.7022(3) .0474(13) Uani d . 1 . . C C4 .2826(4) .0827(5) -.7595(4) .0581(15) Uani d . 1 . . C C11 .2133(3) .1158(4) -.4577(3) .0403(11) Uani d . 1 . . C C12 .1807(3) .2120(5) -.4361(4) .0525(14) Uani d . 1 . . C H12 .2119 .2724 -.4419 .063 Uiso calc R 1 . . H C13 .1022(4) .2166(6) -.4063(4) .0648(17) Uani d . 1 . . C H13 .0805 .2807 -.3918 .078 Uiso calc R 1 . . H C14 .0557(4) .1301(7) -.3976(4) .075(2) Uani d . 1 . . C H14 .0027 .1351 -.3772 .090 Uiso calc R 1 . . H C15 .0868(4) .0344(6) -.4189(5) .080(2) Uani d . 1 . . C H15 .0545 -.0251 -.4130 .097 Uiso calc R 1 . . H C16 .1651(4) .0266(5) -.4489(4) .0567(15) Uani d . 1 . . C H16 .1859 -.0381 -.4634 .068 Uiso calc R 1 . . H C21 .3829(3) .1644(4) -.4238(3) .0398(11) Uani d . 1 . . C C22 .3623(4) .1583(6) -.3487(3) .0602(17) Uani d . 1 . . C H22 .3122 .1283 -.3341 .072 Uiso calc R 1 . . H C23 .4165(4) .1970(6) -.2942(4) .080(2) Uani d . 1 . . C H23 .4016 .1954 -.2431 .096 Uiso calc R 1 . . H C24 .4909(5) .2370(6) -.3149(4) .075(2) Uani d . 1 . . C H24 .5270 .2623 -.2780 .090 Uiso calc R 1 . . H C25 .5127(4) .2402(5) -.3878(5) .077(2) Uani d . 1 . . C H25 .5642 .2671 -.4013 .092 Uiso calc R 1 . . H C26 .4597(4) .2041(5) -.4436(4) .0656(17) Uani d . 1 . . C H26 .4757 .2064 -.4944 .079 Uiso calc R 1 . . H 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 Re .05144(14) .04501(14) .02284(14) .00279(9) -.00006(8) -.00227(8) S1 .0744(10) .0412(7) .0324(8) .0110(6) -.0022(7) .0023(6) S2 .0835(10) .0417(7) .0254(8) .0021(7) .0016(7) .0042(5) P .0522(7) .0410(6) .0215(7) .0024(5) -.0011(5) .0019(5) O1 .047(3) .139(5) .092(4) .001(3) .001(3) -.021(3) O2 .067(3) .090(4) .115(5) -.004(3) .017(3) .004(3) O3 .076(3) .056(2) .054(3) -.006(2) -.004(2) -.016(2) O4 .153(5) .084(3) .029(3) .023(3) -.023(3) .003(2) C1 .061(4) .066(4) .050(4) .008(3) -.001(3) -.007(3) C2 .067(4) .052(3) .047(4) -.004(3) .009(3) -.003(3) C3 .052(3) .062(3) .028(3) -.001(3) -.004(2) .001(3) C4 .085(4) .053(4) .037(4) .005(3) -.003(3) -.010(3) C11 .050(3) .048(3) .023(3) .002(2) -.005(2) .002(2) C12 .052(3) .059(3) .046(4) .006(3) -.008(3) -.004(3) C13 .055(4) .080(4) .059(5) .016(3) -.005(3) -.009(3) C14 .050(4) .111(6) .064(5) .005(4) .006(3) .004(4) C15 .068(5) .090(5) .084(6) -.021(4) .013(4) .015(4) C16 .060(3) .059(4) .051(4) -.002(3) .006(3) .006(3) C21 .046(3) .044(3) .029(3) .006(2) .000(2) -.005(2) C22 .047(3) .103(5) .030(3) .008(3) -.003(2) -.007(3) C23 .075(5) .130(6) .036(4) .030(4) -.011(3) -.024(4) C24 .071(4) .087(5) .068(5) .018(4) -.026(4) -.038(4) C25 .062(4) .088(5) .080(6) -.018(3) -.005(4) -.016(4) C26 .064(4) .089(5) .044(4) -.016(3) .000(3) -.006(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 '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_publ_flag C3 Re C4 91.1(2) y C3 Re C1 90.7(2) y C4 Re C1 86.6(3) y C3 Re C2 91.3(2) y C4 Re C2 92.4(3) y C1 Re C2 177.8(3) y C3 Re S1 94.30(17) y C4 Re S1 174.57(18) y C1 Re S1 93.6(2) y C2 Re S1 87.2(2) y C3 Re S2 172.41(17) y C4 Re S2 96.28(18) y C1 Re S2 91.43(19) y C2 Re S2 86.80(17) y S1 Re S2 78.29(4) y P S1 Re 85.52(6) ? P S2 Re 84.85(6) ? C21 P C11 105.7(2) ? C21 P S1 112.49(17) ? C11 P S1 111.92(18) ? C21 P S2 111.22(18) ? C11 P S2 109.86(18) ? S1 P S2 105.71(8) y C1 O1 C16 84.3(5) ? C1 O1 C11 71.5(5) ? C16 O1 C11 22.15(13) ? C1 O1 C15 104.8(6) ? C16 O1 C15 20.62(15) ? C11 O1 C15 37.00(14) ? C1 O1 C12 81.5(5) ? C16 O1 C12 32.45(14) ? C11 O1 C12 16.88(11) ? C15 O1 C12 38.13(15) ? C1 O1 C14 108.9(5) ? C16 O1 C14 30.71(15) ? C11 O1 C14 37.37(13) ? C15 O1 C14 16.31(14) ? C12 O1 C14 30.64(12) ? C1 O1 C13 98.0(5) ? C16 O1 C13 33.95(14) ? C11 O1 C13 29.22(11) ? C15 O1 C13 29.21(14) ? C12 O1 C13 16.53(10) ? C14 O1 C13 16.33(11) ? O1 C1 Re 176.8(7) ? O1 C1 C16 76.5(5) ? Re C1 C16 106.6(3) ? O1 C1 C11 90.7(5) ? Re C1 C11 92.1(3) ? C16 C1 C11 23.19(13) ? O1 C1 C15 60.4(5) ? Re C1 C15 122.7(3) ? C16 C1 C15 16.29(15) ? C11 C1 C15 34.10(15) ? O1 C1 C12 83.8(5) ? Re C1 C12 98.5(2) ? C16 C1 C12 32.88(14) ? C11 C1 C12 15.59(11) ? C15 C1 C12 37.02(14) ? O1 C1 C14 58.8(5) ? Re C1 C14 123.9(3) ? C16 C1 C14 24.64(14) ? C11 C1 C14 31.83(13) ? C15 C1 C14 14.30(13) ? C12 C1 C14 28.17(12) ? O1 C1 C13 69.3(5) ? Re C1 C13 113.0(3) ? C16 C1 C13 30.58(14) ? C11 C1 C13 24.66(12) ? C15 C1 C13 27.63(13) ? C12 C1 C13 14.57(10) ? C14 C1 C13 15.33(11) ? O2 C2 Re 178.1(6) ? O3 C3 Re 179.5(5) ? O4 C4 Re 178.0(6) ? C16 C11 C12 119.2(5) ? C16 C11 P 122.5(4) ? C12 C11 P 118.3(4) ? C16 C11 C1 75.2(4) ? C12 C11 C1 122.0(4) ? P C11 C1 74.9(2) ? C16 C11 O1 64.8(4) ? C12 C11 O1 112.9(4) ? P C11 O1 92.7(2) ? C1 C11 O1 17.82(13) ? C13 C12 C11 119.3(6) ? C13 C12 C1 111.7(4) ? C11 C12 C1 42.4(3) ? C13 C12 O1 97.0(4) ? C11 C12 O1 50.2(3) ? C1 C12 O1 14.71(10) ? C14 C13 C12 121.4(6) ? C14 C13 O1 71.4(4) ? C12 C13 O1 66.5(4) ? C14 C13 C1 80.4(4) ? C12 C13 C1 53.8(4) ? O1 C13 C1 12.75(9) ? C13 C14 C15 120.1(6) ? C13 C14 O1 92.2(4) ? C15 C14 O1 51.3(4) ? C13 C14 C1 84.3(4) ? C15 C14 C1 49.8(4) ? O1 C14 C1 12.28(9) ? C16 C15 C14 120.3(6) ? C16 C15 O1 59.1(4) ? C14 C15 O1 112.4(5) ? C16 C15 C1 44.3(4) ? C14 C15 C1 115.9(5) ? O1 C15 C1 14.83(11) ? C15 C16 C11 119.7(6) ? C15 C16 O1 100.3(5) ? C11 C16 O1 93.1(4) ? C15 C16 C1 119.4(5) ? C11 C16 C1 81.6(4) ? O1 C16 C1 19.18(13) ? C22 C21 C26 118.9(5) ? C22 C21 P 121.5(4) ? C26 C21 P 119.4(4) ? C21 C22 C23 119.7(6) ? C24 C23 C22 120.4(7) ? C25 C24 C23 120.3(6) ? C24 C25 C26 120.8(7) ? C25 C26 C21 119.8(6) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re C3 . 1.920(6) y Re C4 . 1.929(7) y Re C1 . 1.993(7) y Re C2 . 2.004(7) y Re S1 . 2.5366(15) y Re S2 . 2.5535(14) y S1 P . 2.0100(19) y S2 P . 2.0212(19) y P C21 . 1.798(5) ? P C11 . 1.799(5) ? O1 C1 . 1.128(7) y O1 C16 . 3.340(10) ? O1 C11 . 3.686(8) ? O1 C15 . 3.831(11) ? O1 C12 . 4.419(9) ? O1 C14 . 4.538(10) ? O1 C13 . 4.784(9) ? O2 C2 . 1.123(8) y O3 C3 . 1.148(7) y O4 C4 . 1.130(7) y C1 C16 . 3.417(10) ? C1 C11 . 3.497(9) ? C1 C15 . 4.261(12) ? C1 C12 . 4.396(10) ? C1 C14 . 5.018(10) ? C1 C13 . 5.065(10) ? C11 C16 . 1.392(7) ? C11 C12 . 1.393(8) ? C12 C13 . 1.371(8) ? C13 C14 . 1.346(9) ? C14 C15 . 1.378(10) ? C15 C16 . 1.372(9) ? C21 C22 . 1.365(7) ? C21 C26 . 1.383(7) ? C22 C23 . 1.389(9) ? C23 C24 . 1.354(10) ? C24 C25 . 1.330(10) ? C25 C26 . 1.382(9) ?