#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/35/2003572.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_2003572 loop_ _publ_author_name 'Abram, S.' 'Abram, U.' 'Schulz-Lang, E.' 'Str\"ahle, J.' _publ_section_title ; trans-Dichlorooxo(2-propoxido)bis(triphenylphosphine)rhenium(V) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1078 _journal_page_last 1080 _journal_volume 51 _journal_year 1995 _chemical_formula_moiety 'C39 H37 Cl2 O2 P2 Re1' _chemical_formula_sum 'C39 H37 Cl2 O2 P2 Re' _chemical_formula_weight 856.73 _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 109.71(2) _cell_angle_beta 99.13(3) _cell_angle_gamma 105.90(3) _cell_formula_units_Z 2 _cell_length_a 9.594(5) _cell_length_b 12.430(5) _cell_length_c 16.893(9) _cell_measurement_reflns_used 25 _cell_measurement_temperature 213(2) _cell_measurement_theta_max 14 _cell_measurement_theta_min 8 _cell_volume 1752.4(16) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \w/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0164 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_number 8360 _diffrn_reflns_theta_max 27 _diffrn_standards_decay_% 2.3 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 3.754 _exptl_absorpt_correction_T_max 0.9996 _exptl_absorpt_correction_T_min 0.8959 _exptl_absorpt_correction_type 'empirical via \y scan' _exptl_crystal_colour violet _exptl_crystal_density_diffrn 1.624 _exptl_crystal_description column _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.685 _refine_diff_density_min -0.638 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.108 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 535 _refine_ls_number_reflns 7580 _refine_ls_R_factor_obs 0.0207 _refine_ls_shift/esd_max 0.000 _refine_ls_structure_factor_coef F^2^ _refine_ls_weighting_scheme ; w = 1/[\s^2^(F~o~^2^) + (0.0282P)^2^ + 0.8269P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_wR_factor_obs 0.0509 _reflns_number_observed 7115 _reflns_number_total 7580 _reflns_observed_criterion I>=2\s(I) _[local]_cod_data_source_file jz1019.cif _[local]_cod_data_source_block jz1019a _[local]_cod_chemical_formula_sum_orig 'C39 H37 Cl2 O2 P2 Re1' _cod_original_cell_volume 1753(2) _cod_database_code 2003572 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 .1676(1) .2282(1) .2465(1) .021(1) P(1) .0812(1) .3838(1) .2092(1) .023(1) P(2) .2258(1) .0603(1) .2807(1) .023(1) Cl(1) .2112(1) .1485(1) .1053(1) .028(1) Cl(2) .1559(1) .3231(1) .3941(1) .037(1) O(1) -.0171(2) .1389(2) .2160(1) .029(1) O(2) .3708(2) .3350(2) .2917(1) .031(1) C(1) .4842(4) .4295(3) .3682(2) .053(1) C(2) .5797(5) .3777(4) .4101(3) .074(1) C(3) .5682(6) .5307(4) .3490(4) .094(2) C(11) .0809(3) .5094(2) .3034(2) .028(1) C(12) .1845(4) .6271(3) .3320(2) .038(1) C(13) .1876(5) .7181(3) .4085(2) .052(1) C(14) .0890(4) .6932(4) .4567(2) .051(1) C(15) -.0134(4) .5771(3) .4282(2) .046(1) C(16) -.0171(4) .4859(3) .3531(2) .037(1) C(21) .1843(3) .4593(2) .1499(2) .027(1) C(22) .3245(3) .4539(3) .1440(2) .035(1) C(23) .4057(4) .5179(3) .1024(2) .044(1) C(24) .3488(4) .5870(3) .0681(2) .047(1) C(25) .2093(4) .5918(3) .0729(2) .046(1) C(26) .1258(4) .5283(3) .1133(2) .039(1) C(31) -.1128(3) .3098(2) .1393(2) .027(1) C(32) -.1476(3) .2010(3) .0668(2) .032(1) C(33) -.2926(4) .1390(3) .0126(2) .038(1) C(34) -.4072(3) .1815(3) .0318(2) .039(1) C(35) -.3748(3) .2887(3) .1029(2) .040(1) C(36) -.2277(3) .3543(3) .1561(2) .034(1) C(41) .2543(3) .0830(2) .3952(2) .028(1) C(42) .1365(4) .0954(3) .4326(2) .036(1) C(43) .1526(4) .1162(3) .5196(2) .045(1) C(44) .2838(5) .1234(4) .5701(2) .053(1) C(45) .4008(5) .1125(4) .5349(2) .054(1) C(46) .3881(4) .0932(3) .4475(2) .039(1) C(51) .3851(3) .0210(2) .2504(2) .027(1) C(52) .4955(3) .1010(3) .2330(2) .034(1) C(53) .6210(4) .0731(3) .2144(2) .043(1) C(54) .6347(4) -.0349(3) .2125(2) .044(1) C(55) .5232(4) -.1168(3) .2269(2) .040(1) C(56) .3977(3) -.0899(3) .2456(2) .035(1) C(61) .0652(3) -.0833(2) .2236(2) .027(1) C(62) .0155(4) -.1603(3) .2645(2) .039(1) C(63) -.1036(4) -.2703(3) .2185(3) .049(1) C(64) -.1707(4) -.3039(3) .1316(3) .049(1) C(65) -.1218(4) -.2290(3) .0899(2) .045(1) C(66) -.0040(3) -.1182(3) .1360(2) .035(1) H(1) .4309(4) .4624(3) .4100(2) .063 H(2A) .5170(5) .3121(4) .4206(3) .111 H(2B) .6469(5) .4401(4) .4646(3) .111 H(2C) .6374(5) .3474(4) .3722(3) .111 H(3A) .4990(6) .5595(4) .3220(4) .141 H(3B) .6257(6) .5032(4) .3100(4) .141 H(3C) .6352(6) .5959(4) .4025(4) .141 H(12) .2542(41) .6464(32) .2972(24) .047(10) H(13) .2494(45) .7900(37) .4255(26) .054(11) H(14) .1022(47) .7577(39) .5097(29) .068(13) H(15) -.0858(50) .5579(38) .4625(29) .069(13) H(16) -.0840(39) .4078(32) .3390(23) .040(9) H(22) .3619(34) .4067(28) .1680(20) .029(8) H(23) .4899(47) .5183(37) .0988(27) .059(12) H(24) .4048(42) .6233(34) .0387(25) .051(11) H(25) .1721(44) .6335(36) .0514(26) .054(11) H(26) .0355(40) .5327(31) .1164(22) .040(9) H(32) -.0742(43) .1757(34) .0566(25) .051(11) H(33) -.3165(41) .0709(34) -.0301(25) .048(10) H(34) -.5032(38) .1403(30) -.0039(22) .035(8) H(35) -.4533(42) .3145(33) .1173(24) .049(10) H(36) -.2081(35) .4307(29) .2072(21) .033(8) H(42) .0452(43) .0851(33) .3970(25) .050(10) H(43) .0692(41) .1279(32) .5392(24) .044(10) H(44) .2988(43) .1421(34) .6304(26) .053(11) H(45) .4957(49) .1198(38) .5694(28) .066(13) H(46) .4678(38) .0874(29) .4244(22) .035(9) H(52) .4811(34) .1757(28) .2316(20) .031(8) H(53) .6899(44) .1218(35) .2027(26) .054(11) H(54) .7136(39) -.0533(31) .1985(22) .039(9) H(55) .5225(41) -.1853(34) .2234(24) .046(10) H(56) .3231(37) -.1420(29) .2535(21) .033(8) H(62) .0615(37) -.1396(30) .3205(23) .037(9) H(63) -.1405(39) -.3159(32) .2432(23) .041(9) H(64) -.2489(47) -.3811(38) .0997(27) .061(12) H(65) -.1688(39) -.2487(32) .0345(24) .041(9) H(66) .0312(48) -.0729(39) .1031(29) .069(13) 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 O(1) Re O(2) 174.25(9) yes O(1) Re Cl(2) 90.38(8) yes O(2) Re Cl(2) 83.88(7) yes O(1) Re Cl(1) 96.59(8) yes O(2) Re Cl(1) 89.16(7) yes Cl(2) Re Cl(1) 173.03(3) yes O(1) Re P(2) 86.66(7) yes O(2) Re P(2) 93.53(7) yes Cl(2) Re P(2) 90.12(4) yes O(1) Re P(1) 87.51(7) yes O(2) Re P(1) 92.21(7) yes Cl(2) Re P(1) 89.34(4) yes Cl(1) Re P(1) 91.26(4) yes P(2) Re P(1) 174.14(2) yes C(1) O(2) Re 145.3(2) yes O(2) C(1) C(3) 111.6(4) yes O(2) C(1) C(2) 110.5(3) yes C(3) C(1) C(2) 114.2(4) yes C(11) P(1) C(21) 103.64(13) no C(11) P(1) C(31) 106.25(13) no C(21) P(1) C(31) 104.63(13) no C(11) P(1) Re 114.25(10) no C(21) P(1) Re 117.81(9) no C(31) P(1) Re 109.27(9) no C(41) P(2) C(51) 105.17(13) no C(41) P(2) C(61) 103.28(13) no C(51) P(2) C(61) 103.96(13) no C(41) P(2) Re 114.55(9) no C(51) P(2) Re 118.14(9) no C(61) P(2) Re 110.25(10) no C(12) C(11) C(16) 118.6(3) no C(12) C(11) P(1) 121.9(2) no C(16) C(11) P(1) 119.2(2) no C(13) C(12) C(11) 119.8(3) no C(14) C(13) C(12) 120.8(4) no C(15) C(14) C(13) 119.3(3) no C(14) C(15) C(16) 120.6(3) no C(15) C(16) C(11) 120.9(3) no C(22) C(21) C(26) 119.2(3) no C(22) C(21) P(1) 120.5(2) no C(26) C(21) P(1) 120.2(2) no C(21) C(22) C(23) 119.8(3) no C(24) C(23) C(22) 120.7(3) no C(23) C(24) C(25) 119.9(3) no C(24) C(25) C(26) 120.6(3) no C(25) C(26) C(21) 119.8(3) no C(36) C(31) C(32) 118.6(3) no C(36) C(31) P(1) 123.4(2) no C(32) C(31) P(1) 117.9(2) no C(33) C(32) C(31) 120.9(3) no C(32) C(33) C(34) 120.1(3) no C(35) C(34) C(33) 119.7(3) no C(34) C(35) C(36) 120.6(3) no C(31) C(36) C(35) 120.1(3) no C(46) C(41) C(42) 118.8(3) no C(46) C(41) P(2) 123.3(2) no C(42) C(41) P(2) 117.8(2) no C(43) C(42) C(41) 120.6(3) no C(44) C(43) C(42) 120.1(3) no C(43) C(44) C(45) 120.0(3) no C(44) C(45) C(46) 120.9(3) no C(41) C(46) C(45) 119.4(3) no C(52) C(51) C(56) 119.3(3) no C(52) C(51) P(2) 120.7(2) no C(56) C(51) P(2) 120.0(2) no C(51) C(52) C(53) 120.4(3) no C(54) C(53) C(52) 119.9(3) no C(53) C(54) C(55) 120.2(3) no C(54) C(55) C(56) 120.4(3) no C(55) C(56) C(51) 119.9(3) no C(66) C(61) C(62) 119.2(3) no C(66) C(61) P(2) 118.8(2) no C(62) C(61) P(2) 121.9(2) no C(61) C(62) C(63) 120.4(3) no C(64) C(63) C(62) 119.8(3) no C(63) C(64) C(65) 120.6(3) no C(64) C(65) C(66) 119.9(3) no C(61) C(66) C(65) 120.2(3) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Re O(1) 1.698(2) yes Re O(2) 1.890(2) yes Re Cl(2) 2.4071(14) yes Re Cl(1) 2.4076(13) yes Re P(2) 2.5201(11) yes Re P(1) 2.5208(11) yes O(2) C(1) 1.436(4) yes C(1) C(3) 1.463(6) yes C(1) C(2) 1.476(6) yes P(1) C(11) 1.816(3) no P(1) C(21) 1.818(3) no P(1) C(31) 1.827(3) no P(2) C(41) 1.822(3) no P(2) C(51) 1.824(3) no P(2) C(61) 1.830(3) no C(11) C(12) 1.391(4) no C(11) C(16) 1.393(4) no C(12) C(13) 1.390(5) no C(13) C(14) 1.381(6) no C(14) C(15) 1.372(6) no C(15) C(16) 1.375(4) no C(21) C(22) 1.383(4) no C(21) C(26) 1.394(4) no C(22) C(23) 1.394(4) no C(23) C(24) 1.365(5) no C(24) C(25) 1.370(5) no C(25) C(26) 1.387(5) no C(31) C(36) 1.390(4) no C(31) C(32) 1.394(4) no C(32) C(33) 1.379(4) no C(33) C(34) 1.381(5) no C(34) C(35) 1.375(5) no C(35) C(36) 1.391(4) no C(41) C(46) 1.385(4) no C(41) C(42) 1.400(4) no C(42) C(43) 1.378(4) no C(43) C(44) 1.366(5) no C(44) C(45) 1.368(6) no C(45) C(46) 1.393(5) no C(51) C(52) 1.384(4) no C(51) C(56) 1.392(4) no C(52) C(53) 1.395(4) no C(53) C(54) 1.374(5) no C(54) C(55) 1.376(5) no C(55) C(56) 1.389(4) no C(61) C(66) 1.385(4) no C(61) C(62) 1.387(4) no C(62) C(63) 1.388(5) no C(63) C(64) 1.371(5) no C(64) C(65) 1.376(5) no C(65) C(66) 1.388(4) no