#------------------------------------------------------------------------------ #$Date: 2025-08-18 23:52:38 +0100 (Mon, 18 Aug 2025) $ #$Revision: 301791 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/34/2003467.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_2003467 loop_ _publ_author_name 'H\"ubener, R.' 'Abram, U.' 'Str\"ahle, J.' _publ_section_title ; trans-Hydroxotris(isothiocyanato)bis(triphenylphosphine)rhenium(IV) Methanol Solvate ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 876 _journal_page_last 878 _journal_paper_doi 10.1107/S0108270194008498 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety '[Re (OH) (NCS)3 (PC18H15 P)2 ],CH4 O' _chemical_formula_sum 'C40 H35 N3 O2 P2 Re S3' _chemical_formula_weight 934.08 _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_type_scat_source IntTabIV _cell_angle_alpha 90.0 _cell_angle_beta 107.74(2) _cell_angle_gamma 90.0 _cell_formula_units_Z 4 _cell_length_a 9.976(4) _cell_length_b 29.601(6) _cell_length_c 14.189(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 223 _cell_measurement_theta_max 13 _cell_measurement_theta_min 8 _cell_volume 3991(2) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0882 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10287 _diffrn_reflns_theta_max 29 _diffrn_standards_decay_% 2.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.3518 _exptl_absorpt_correction_T_max 1.2938 _exptl_absorpt_correction_T_min 0.7979 _exptl_absorpt_correction_type 'DIFABS (Walker & Stuart, 1983)' _exptl_crystal_colour brown-red _exptl_crystal_density_diffrn 1.555 _exptl_crystal_description plate _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.663 _refine_diff_density_min -0.386 _refine_ls_extinction_coef 6.5446E-9 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_obs 1.286 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 465 _refine_ls_number_reflns 9719 _refine_ls_R_factor_obs 0.032 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/\s^2^(F)' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.036 _reflns_number_observed 6797 _reflns_number_total 9901 _reflns_observed_criterion I>=3\s(I) _cod_data_source_file ka1086.cif _cod_data_source_block ka1086a _cod_depositor_comments ; Marking attached hydrogen atoms. Antanas Vaitkus, 2017-03-27 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/\s^2^(F)' 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^(F)'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 3990.9(9) _cod_original_sg_symbol_H-M 'P 21/c' _cod_original_formula_sum 'C40 H35 N3 O2 P2 Re1 S3' _cod_database_code 2003467 loop_ _symmetry_equiv_pos_as_xyz x,y,z x,1/2-y,1/2+z -x,-y,-z -x,1/2+y,1/2-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_attached_hydrogens Re .13807(2) .11593(1) .19600(1) .02177(7) 0 S1 .2038(2) -.02884(5) .0722(1) .057(1) 0 S2 -.0095(2) .26385(5) .2418(1) .0483(9) 0 S3 .6058(2) .15413(6) .3964(1) .0442(9) 0 P1 .1825(1) .15864(4) .05947(8) .0236(6) 0 P2 .0898(1) .06770(4) .32398(9) .0253(6) 0 O -.0827(4) .1095(2) .1117(3) .046(2) 0 O10 .2724(5) .6569(2) .3019(4) .077(4) 1 N1 .1710(4) .0576(1) .1351(3) .026(2) 0 N2 .0821(4) .1758(1) .2394(3) .028(2) 0 N3 .3401(4) .1252(1) .2802(3) .029(2) 0 C1 .1853(5) .0215(2) .1065(4) .027(2) 0 C2 .0422(5) .2127(2) .2410(3) .030(3) 0 C3 .4513(5) .1372(2) .3293(4) .029(2) 0 C10 .3391(8) .6946(3) .3639(7) .075(6) 3 C11 .3002(5) .1332(2) -.0016(3) .028(2) 0 C12 .4072(6) .1043(2) .0511(4) .031(3) 0 C13 .5054(6) .0882(2) .0081(4) .037(3) 0 C14 .5006(6) .1012(2) -.0863(4) .040(3) 0 C15 .3952(6) .1297(2) -.1394(4) .041(3) 0 C16 .2951(5) .1459(2) -.0977(4) .033(3) 0 C21 .2549(5) .2156(2) .0844(4) .027(2) 0 C22 .3254(6) .2294(2) .1798(4) .030(3) 0 C23 .3923(7) .2708(2) .1968(5) .041(3) 0 C24 .3906(7) .2988(2) .1190(5) .047(4) 0 C25 .3190(7) .2858(2) .0229(5) .045(3) 0 C26 .2517(6) .2445(2) .0060(4) .037(3) 0 C31 .0163(5) .1667(2) -.0390(3) .029(2) 0 C32 -.0709(6) .2024(2) -.0317(4) .039(3) 0 C33 -.2048(6) .2057(3) -.0989(5) .052(4) 0 C34 -.2500(7) .1740(3) -.1722(5) .055(5) 0 C35 -.1659(7) .1381(2) -.1789(5) .047(4) 0 C36 -.0312(6) .1341(2) -.1122(4) .037(3) 0 C41 -.0864(5) .0426(2) .2807(3) .030(2) 0 C42 -.1951(6) .0558(2) .3155(4) .038(3) 0 C43 -.3270(6) .0372(2) .2785(5) .050(4) 0 C44 -.3535(7) .0047(2) .2047(5) .044(3) 0 C45 -.2455(6) -.0089(2) .1694(4) .041(3) 0 C46 -.1129(6) .0094(2) .2072(4) .036(3) 0 C51 .2017(5) .0178(2) .3600(3) .028(2) 0 C52 .1511(6) -.0206(2) .3962(4) .040(3) 0 C53 .2371(7) -.0585(2) .4253(5) .043(3) 0 C54 .3710(7) -.0583(2) .4176(5) .044(3) 0 C55 .4209(7) -.0204(2) .3811(5) .051(3) 0 C56 .3360(6) .0172(2) .3522(4) .038(3) 0 C61 .0953(5) .0947(2) .4406(3) .031(3) 0 C62 .0232(6) .1352(2) .4380(4) .035(3) 0 C63 .0178(6) .1550(2) .5259(4) .047(3) 0 C64 .0855(7) .1352(2) .6163(4) .053(4) 0 C65 .1589(8) .0957(2) .6187(4) .050(4) 0 C66 .1645(6) .0750(2) .5314(4) .038(3) 0 H -.110(6) .076(2) .101(4) .03(1) 0 H12 .4124 .0955 .1173 5.0 0 H13 .5777 .0678 .0446 5.0 0 H14 .5701 .0902 -.1151 5.0 0 H15 .3910 .1384 -.2053 5.0 0 H16 .2221 .1659 -.1347 5.0 0 H22 .3275 .2099 .2344 5.0 0 H23 .4405 .2800 .2637 5.0 0 H24 .4399 .3271 .1315 5.0 0 H25 .3157 .3054 -.0318 5.0 0 H26 .2019 .2354 -.0605 5.0 0 H32 -.0379 .2245 .0199 5.0 0 H33 -.2657 .2303 -.0938 5.0 0 H34 -.3420 .1769 -.2198 5.0 0 H35 -.2000 .1155 -.2297 5.0 0 H36 .0292 .1090 -.1163 5.0 0 H42 -.1774 .0782 .3672 5.0 0 H43 -.4025 .0471 .3027 5.0 0 H44 -.4458 -.0083 .1791 5.0 0 H45 -.2625 -.0313 .1181 5.0 0 H46 -.0381 -.0006 .1825 5.0 0 H52 .0570 -.0206 .4014 5.0 0 H53 .2021 -.0847 .4504 5.0 0 H54 .4299 -.0844 .4372 5.0 0 H55 .5146 -.0203 .3753 5.0 0 H56 .3708 .0432 .3264 5.0 0 H62 -.0220 .1495 .3756 5.0 0 H63 -.0346 .1827 .5234 5.0 0 H64 .0810 .1488 .6768 5.0 0 H65 .2077 .0820 .6814 5.0 0 H66 .2158 .0472 .5337 5.0 0 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 P1 Re P2 175.35(5) yes P1 Re N1 90.70(10) yes P1 Re N2 85.50(10) yes P1 Re N3 90.50(10) yes P1 Re O 90.40(10) yes P2 Re N1 85.00(10) yes P2 Re N2 98.60(10) yes P2 Re N3 91.50(10) yes P2 Re O 87.80(10) yes N1 Re N2 171.80(10) yes N1 Re N3 96.10(10) yes N1 Re O 87.6(2) yes N2 Re N3 91.1(2) yes N2 Re O 85.3(2) yes N3 Re O 176.2(2) yes Re N1 C1 173.3(4) yes Re N2 C2 163.9(4) yes Re N3 C3 170.0(5) yes N1 C1 S1 177.2(6) yes N2 C2 S2 178.4(6) yes N3 C3 S3 179.4(5) yes Re O H 111(3) yes P2 C41 C46 118.6(4) no C42 C41 C46 118.4(5) no P2 C51 C52 120.0(4) no P2 C51 C56 120.9(5) no C52 C51 C56 119.1(5) no P2 C61 C62 118.8(3) no P2 C61 C66 121.7(4) no C62 C61 C66 119.5(5) no C11 C12 C13 120.1(5) no C12 C13 C14 120.8(5) no C13 C14 C15 119.7(6) no C14 C15 C16 120.3(5) no C11 C16 C15 120.1(5) no C21 C22 C23 120.4(6) no C22 C23 C24 120.5(5) no C23 C24 C25 119.9(6) no C24 C25 C26 119.6(6) no C21 C26 C25 120.9(5) no C31 C32 C33 119.6(5) no C32 C33 C34 120.0(6) no C33 C34 C35 121.0(6) no C34 C35 C36 120.1(6) no C31 C36 C35 119.1(6) no C41 C42 C43 121.0(5) no C42 C43 C44 120.4(7) no C43 C44 C45 119.1(6) no C44 C45 C46 120.5(5) no C41 C46 C45 120.5(6) no C51 C52 C53 120.1(6) no C52 C53 C54 119.9(6) no C53 C54 C55 120.0(6) no C54 C55 C56 120.3(6) no C51 C56 C55 120.6(6) no C61 C62 C63 119.9(5) no C62 C63 C64 120.7(6) no C63 C64 C65 119.3(6) no C64 C65 C66 121.1(5) no C61 C66 C65 119.7(6) no Re P1 C11 117.3(2) no Re P1 C21 118.5(2) no Re P1 C31 109.2(2) no C11 P1 C21 101.6(2) no C11 P1 C31 104.8(2) no C21 P1 C31 104.0(2) no Re P2 C41 111.7(2) no Re P2 C51 115.7(2) no Re P2 C61 117.1(2) no C41 P2 C51 102.0(2) no C41 P2 C61 104.0(3) no C51 P2 C61 104.7(2) no P1 C11 C12 119.8(4) no P1 C11 C16 120.9(4) no C12 C11 C16 118.9(5) no P1 C21 C22 121.0(4) no P1 C21 C26 120.0(4) no C22 C21 C26 118.7(5) no P1 C31 C32 118.9(4) no P1 C31 C36 120.3(5) no C32 C31 C36 120.3(4) no P2 C41 C42 122.9(4) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Re P1 2.4640(10) yes Re P2 2.4700(10) yes Re N1 2.002(4) yes Re N2 2.011(4) yes Re N3 2.024(4) yes Re O 2.171(4) yes N1 C1 1.169(7) yes N2 C2 1.164(7) yes N3 C3 1.170(6) yes O H 1.03(6) yes C1 S1 1.595(5) yes C2 S2 1.600(6) yes C3 S3 1.625(5) yes O10 C10 1.45(2) yes P1 C11 1.822(6) no P1 C21 1.827(6) no P1 C31 1.829(4) no P2 C41 1.834(6) no P2 C51 1.828(5) no P2 C61 1.823(5) no C11 C12 1.394(7) no C11 C16 1.401(7) no C21 C22 1.382(7) no C21 C26 1.397(8) no C31 C32 1.394(8) no C31 C36 1.391(7) no C41 C42 1.379(9) no C41 C46 1.398(7) no C51 C52 1.404(8) no C51 C56 1.378(8) no C61 C62 1.395(8) no C61 C66 1.392(7) no C12 C13 1.387(9) no C13 C14 1.381(9) no C14 C15 1.379(7) no C15 C16 1.392(9) no C22 C23 1.382(8) no C23 C24 1.376(9) no C24 C25 1.386(9) no C25 C26 1.380(8) no C32 C33 1.388(7) no C33 C34 1.370(10) no C34 C35 1.38(2) no C35 C36 1.394(8) no C42 C43 1.375(8) no C43 C44 1.385(9) no C44 C45 1.38(2) no C45 C46 1.377(8) no C52 C53 1.396(8) no C53 C54 1.37(2) no C54 C55 1.400(10) no C55 C56 1.382(8) no C62 C63 1.394(8) no C63 C64 1.386(8) no C64 C65 1.370(10) no C65 C66 1.398(9) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 168307582