#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003674.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_2003674 loop_ _publ_author_name 'H\"ubener, R.' 'Abram, U.' 'Str\"ahle, J.' _publ_section_title ;Isothiocyanato Complexes of Rhenium. V. trans-Bis(isothiocyanato)(methoxy)(phenylimido)bis(triphenylphosphine)rhenium(V) ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1284 _journal_page_last 1286 _journal_paper_doi 10.1107/S0108270195000564 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C45 H38 N3 O P2 Re S2' _chemical_formula_weight 941.1 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 93.89(3) _cell_angle_beta 99.92(3) _cell_angle_gamma 102.28(3) _cell_formula_units_Z 2 _cell_length_a 10.216(6) _cell_length_b 13.236(6) _cell_length_c 15.534(7) _cell_measurement_reflns_used 25 _cell_measurement_temperature 223 _cell_measurement_theta_max 14 _cell_measurement_theta_min 8 _cell_volume 2009.8(18) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0149 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_number 8863 _diffrn_reflns_theta_max 27 _diffrn_standards_decay_% 1.6 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.2795 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_type empirical _exptl_crystal_colour yellow-green _exptl_crystal_density_diffrn 1.568 _exptl_crystal_description lozenge _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.778 _refine_diff_density_min -0.331 _refine_ls_extinction_coef 2.1928E-9 _refine_ls_extinction_method 'Zachariasen (1963)' _refine_ls_goodness_of_fit_obs 1.305 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 488 _refine_ls_number_reflns 8096 _refine_ls_R_factor_obs 0.032 _refine_ls_shift/esd_max 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/\s^2^' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs 0.036 _reflns_number_observed 6174 _reflns_number_total 8096 _reflns_observed_criterion I>=3\s(I) _cod_data_source_file jz1024.cif _cod_data_source_block jz1024a _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value '1/\s^2^' 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^'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2009.7(17) _cod_database_code 2003674 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Re .22662(2) .23875(2) .23529(1) .2274(7) S1 .0380(2) .5292(1) .3104(1) .060(1) S2 .3183(3) -.0745(1) .1112(2) .079(1) P1 .1251(1) .1288(1) .34300(9) .0265(6) P2 .3325(1) .3504(1) .13010(8) .0271(6) O .0689(4) .1860(3) .1441(2) .032(2) N1 .1336(5) .3565(3) .2636(3) .030(2) N2 .2888(5) .1104(3) .1900(3) .032(2) N3 .3767(4) .2834(3) .3132(3) .023(2) C1 .0932(6) .4295(4) .2820(4) .034(3) C2 .3006(6) .0325(4) .1587(4) .040(3) C3 .0261(8) .1153(5) .0674(4) .049(4) C11 -.0591(6) .0822(5) .3162(4) .036(3) C12 -.1167(8) .0255(6) .2356(5) .054(4) C13 -.2600(9) -.0082(6) .2123(5) .062(5) C14 -.3406(8) .0144(6) .2691(6) .070(6) C15 -.2835(7) .0692(6) .3488(6) .071(6) C16 -.1429(6) .1032(5) .3735(5) .050(4) C21 .1900(6) .0120(4) .3601(4) .034(3) C22 .1042(7) -.0834(4) .3638(4) .043(3) C23 .1574(8) -.1686(5) .3821(5) .066(4) C24 .2951(7) -.1593(5) .3965(5) .070(4) C25 .3825(6) -.0651(5) .3934(5) .062(4) C26 .3304(6) .0204(5) .3745(4) .043(3) C31 .1624(5) .1970(4) .4543(3) .029(2) C32 .2179(6) .1543(5) .5274(4) .039(3) C33 .2440(8) .2093(6) .6103(4) .053(4) C34 .2133(8) .3058(5) .6207(4) .054(4) C35 .1578(7) .3467(5) .5495(4) .050(3) C36 .1311(6) .2942(5) .4652(4) .043(3) C41 .3655(5) .4888(4) .1634(3) .027(2) C42 .4055(6) .5276(4) .2516(4) .034(3) C43 .4351(7) .6336(5) .2772(4) .044(4) C44 .4250(7) .7019(5) .2137(5) .049(4) C45 .3879(8) .6654(5) .1275(4) .053(4) C46 .3586(7) .5594(5) .1007(4) .0045(3) C51 .2238(6) .3342(4) .0226(4) .036(3) C52 .0982(7) .3592(5) .0187(4) .048(4) C53 .0061(9) .3434(7) -.0611(5) .066(5) C54 .039(1) .3014(7) -.1350(5) .074(7) C55 .163(1) .2769(7) -.1315(5) .075(7) C56 .2578(8) .2943(6) -.0529(4) .053(4) C61 .4985(6) .3285(4) .1156(3) .034(2) C62 .5075(6) .2285(5) .0891(4) .049(3) C63 .6359(7) .2077(5) .0882(4) .060(3) C64 .7508(7) .2864(7) .1111(5) .073(5) C65 .7424(7) .3855(7) .1347(5) .060(5) C66 .6150(6) .4078(5) .1367(4) .042(3) C71 .5033(6) .3142(5) .3657(4) .037(3) C72 .6174(7) .2953(5) .3324(5) .050(4) C73 .7459(7) .3322(6) .3821(6) .056(5) C74 .7649(9) .3796(6) .4644(5) .061(5) C75 .6493(9) .4005(6) .4971(5) .053(5) C76 .5254(7) .3683(6) .4515(4) .049(4) H12 -.0593 .0089 .1954 ? H13 -.3016 -.0483 .1554 ? H14 -.4393 -.0076 .2517 ? H15 -.3412 .0848 .3893 ? H16 -.1019 .1409 .4312 ? H22 .0056 -.0896 .3527 ? H23 .0963 -.2350 .3835 ? H24 .3317 -.2192 .4093 ? H25 .4803 -.0589 .4047 ? H26 .3908 .0864 .3711 ? H32 .2381 .0865 .5201 ? H33 .2838 .1796 .6610 ? H34 .2317 .3441 .6784 ? H35 .1353 .4138 .5571 ? H36 .0912 .3244 .4147 ? H42 .4133 .4797 .2954 ? H43 .4627 .6595 .3389 ? H44 .4449 .7756 .2313 ? H45 .3815 .7139 .0838 ? H46 .3323 .5342 .0385 ? H52 .0751 .3882 .0717 ? H53 -.0825 .3628 -.0640 ? H54 -.0270 .2883 -.1903 ? H55 .1849 .2461 -.1844 ? H56 .3479 .2792 -.0510 ? H62 .4249 .1739 .0709 ? H63 .6427 .1371 .0714 ? H64 .8395 .2713 .1107 ? H65 .8245 .4410 .1504 ? H66 .6078 .4784 .1525 ? H72 .6038 .2565 .2746 ? H73 .8245 .3239 .3571 ? H74 .8560 .3990 .5013 ? H75 .6621 .4400 .5539 ? H76 .4482 .3813 .4750 ? H301 -.0669 .1141 .0413 ? H302 .0820 .1351 .0249 ? H303 .0313 .0464 .0805 ? 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 178.78(4) yes P1 Re N1 93.10(10) yes P1 Re N2 86.90(10) yes P1 Re N3 89.90(10) yes P1 Re O 92.20(10) yes P2 Re N1 86.90(10) yes P2 Re N2 93.30(10) yes P2 Re N3 88.80(10) yes P2 Re O 89.10(10) yes N1 Re N2 169.8(2) yes N1 Re N3 97.3(2) yes N2 Re N3 93.0(2) yes N1 Re O 86.0(2) yes N2 Re O 83.7(2) yes N3 Re O 175.9(2) yes Re O C3 140.2(4) yes Re N1 C1 173.5(5) yes Re N2 C2 168.4(4) yes Re N3 C71 172.2(4) yes N1 C1 S1 178.2(5) yes N2 C2 S2 177.8(6) yes Re P1 C11 115.1(3) no Re P1 C21 114.9(2) no Re P1 C31 112.6(2) no C11 P1 C21 104.6(3) no C11 P1 C31 105.7(3) no C21 P1 C31 102.7(2) no Re P2 C41 114.0(2) no Re P2 C51 112.7(2) no Re P2 C61 113.4(2) no C41 P2 C51 103.6(2) no C41 P2 C61 104.2(2) no C51 P2 C61 108.1(3) no P1 C11 C12 118.4(5) no P1 C11 C16 122.1(5) no C12 C11 C16 119.5(6) no P1 C21 C22 121.9(5) no P1 C21 C26 118.8(4) no C22 C21 C26 119.2(6) no P1 C31 C32 122.3(4) no P1 C31 C36 118.4(4) no C32 C31 C36 119.5(5) no P2 C41 C42 120.7(5) no P2 C41 C46 120.9(4) no C42 C41 C46 118.4(5) no P2 C51 C52 116.8(5) no P2 C51 C56 123.3(5) no C52 C51 C56 119.8(6) no P2 C61 C62 118.6(4) no P2 C61 C66 121.2(5) no C62 C61 C66 120.1(6) no N3 C71 C72 118.9(6) no N3 C71 C76 122.4(6) no C72 C71 C76 118.7(5) no C11 C12 C13 119.2(7) no C12 C13 C14 120.3(7) no C13 C14 C15 120.3(7) no C14 C15 C16 120.6(8) no C11 C16 C15 120.1(6) no C21 C22 C23 120.4(6) no C22 C23 C24 119.9(6) no C23 C24 C25 120.7(7) no C24 C25 C26 119.9(6) no C21 C26 C25 120.0(5) no C31 C32 C33 119.9(6) no C32 C33 C34 120.4(6) no C33 C34 C35 119.7(6) no C34 C35 C36 121.5(6) no C31 C36 C35 119.1(5) no C41 C42 C43 121.0(5) no C42 C43 C44 119.5(5) no C43 C44 C45 120.3(6) no C44 C45 C46 121.0(6) no C41 C46 C45 119.9(5) no C51 C52 C53 120.0(8) no C52 C53 C54 120.0(10) no C53 C54 C55 120.4(8) no C54 C55 C56 121.0(9) no C51 C56 C55 119.1(9) no C61 C62 C63 119.4(5) no C62 C63 C64 120.0(7) no C63 C64 C65 121.0(7) no C64 C65 C66 120.0(6) no C61 C66 C65 119.5(6) no C71 C72 C73 119.4(6) no C72 C73 C74 121.3(8) no C73 C74 C75 119.0(7) no C74 C75 C76 121.5(7) no C71 C76 C75 120.0(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Re P1 2.5060(10) yes Re P2 2.5070(10) yes Re N1 2.051(5) yes Re N2 2.057(5) yes Re N3 1.744(4) yes Re O 1.922(3) yes N1 C1 1.166(8) yes N2 C2 1.149(8) yes O C3 1.407(7) yes N3 C71 1.368(7) yes C1 S1 1.606(6) yes C2 S2 1.612(6) yes P1 C11 1.815(6) no P1 C21 1.824(6) no P1 C31 1.834(5) no P2 C41 1.812(6) no P2 C51 1.811(5) no P2 C61 1.829(6) no C11 C12 1.381(8) no C11 C16 1.400(10) no C21 C22 1.386(7) no C21 C26 1.392(8) no C31 C32 1.390(8) no C31 C36 1.396(8) no C41 C42 1.390(8) no C41 C46 1.398(8) no C51 C52 1.38(2) no C51 C56 1.380(10) no C61 C62 1.385(8) no C61 C66 1.384(7) no C71 C72 1.41(2) no C71 C76 1.429(9) no C12 C13 1.41(2) no C13 C14 1.370(10) no C14 C15 1.360(10) no C15 C16 1.387(9) no C22 C23 1.380(10) no C23 C24 1.36(2) no C24 C25 1.381(9) no C25 C26 1.380(10) no C32 C33 1.391(9) no C33 C34 1.380(10) no C34 C35 1.355(9) no C35 C36 1.395(8) no C42 C43 1.385(9) no C43 C44 1.389(9) no C44 C45 1.353(9) no C45 C46 1.389(8) no C52 C53 1.39(2) no C53 C54 1.370(10) no C54 C55 1.36(2) no C55 C56 1.39(2) no C62 C63 1.400(10) no C63 C64 1.368(9) no C64 C65 1.360(10) no C65 C66 1.40(2) no C72 C73 1.370(10) no C73 C74 1.350(10) no C74 C75 1.430(10) no C75 C76 1.310(10) no