#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/49/2004999.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_2004999 loop_ _publ_author_name 'Kettmann, V.' 'Dunaj-Jur\tert-Butylbis(dimethylglyoximato-N,N')(triphenylphosphine-P)rhodium _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1399 _journal_page_last 1401 _journal_volume 52 _journal_year 1996 _chemical_formula_iupac '[Rh (C4 H7 N2 O2)2 (C4 H9)(C18 H15 P1)]' _chemical_formula_sum 'C30 H38 N4 O4 P Rh' _chemical_formula_weight 652.54 _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 76.63(5) _cell_angle_beta 87.31(6) _cell_angle_gamma 72.23(5) _cell_formula_units_Z 2 _cell_length_a 8.696(3) _cell_length_b 10.421(4) _cell_length_c 17.113(8) _cell_measurement_reflns_used 15 _cell_measurement_temperature 293 _cell_measurement_theta_max 17 _cell_measurement_theta_min 6 _cell_volume 1436.3(11) _computing_cell_refinement 'Syntex P2~1~ diffractometer software' _computing_data_collection 'Syntex P2~1~ diffractometer software' _computing_data_reduction 'XP21 (Pavel\2\s(I) _[local]_cod_data_source_file hr1052.cif _[local]_cod_data_source_block hr1052a _cod_original_cell_volume 1436.3(8) _cod_database_code 2004999 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_B_iso_or_equiv Rh(1) .14588(3) .08969(2) .229150(10) 2.720(10) P(1) .13492(9) .30437(7) .27280(4) 2.58(2) O(1) .4961(3) -.0029(2) .23740(10) 4.14(6) O(2) -.0455(3) .2690(2) .09260(10) 4.14(7) O(3) -0.2045(3) .1753(3) .22130(10) 4.42(8) O(4) .3394(3) -.0994(2) .36270(10) 3.91(6) N(1) .3619(3) .0753(2) .19080(10) 3.05(7) N(2) .1013(3) .2045(2) .11880(10) 3.16(7) N(3) -.0690(3) .0964(3) .26600(10) 3.16(8) N(4) .1937(3) -.0350(2) .33750(10) 3.36(8) C(1) .3773(4) .1381(3) .1173(2) 3.43(8) C(2) .2262(4) .2109(3) .0753(2) 3.64(9) C(3) .5352(5) .1323(4) .0814(2) 5.12(13) C(4) .2096(5) .2833(4) -.0104(2) 4.89(13) C(5) -.0830(4) .0227(4) .3360(2) 3.87(10) C(6) .0669(4) -.0550(3) .3774(2) 3.74(9) C(7) -0.2424(5) .0133(5) .3690(3) 5.81(15) C(8) .0848(6) -0.1556(4) .4545(2) 5.39(13) C(9) .2422(4) .4020(3) .2020(2) 3.03(8) C(10) .3999(4) .3918(3) .2194(2) 3.51(9) C(11) .4866(4) .4561(4) .1639(2) 4.01(9) C(12) .4197(5) .5315(3) .0911(2) 4.10(10) C(13) .2647(5) .5411(3) .0725(2) 4.18(10) C(14) .1771(4) .4738(3) .1267(2) 3.40(9) C(15) -.0664(4) .4203(3) .2798(2) 3.24(8) C(16) -0.1667(4) .3702(4) .3334(2) 3.99(10) C(17) -0.3154(5) .4535(5) .3484(2) 5.12(14) C(18) -0.3617(4) .5904(5) .3077(2) 5.62(14) C(19) -0.2679(5) .6409(4) .2559(3) 5.19(12) C(20) -0.1148(5) .5590(3) .2406(2) 4.33(10) C(21) .2218(4) .2996(3) .3686(2) 3.02(8) C(22) .3406(4) .1870(3) .4057(2) 3.17(8) C(23) .4148(4) .1894(3) .4741(2) 3.66(10) C(24) .3698(5) .3046(4) .5051(2) 4.57(11) C(25) .2472(6) .4147(5) .4693(3) 6.84(17) C(26) .1717(6) .4137(4) .4009(2) 5.83(14) C(27) .1447(4) -.0875(3) .1786(2) 3.85(10) C(28) .2846(7) -0.1228(5) .1238(3) 7.2(2) C(29) -.0071(6) -.0545(5) .1336(3) 6.59(17) C(30) .1631(5) -0.2171(4) .2447(3) 5.18(13) HO1 .4337 -0.0456 .2855 4.5 HO3 -0.1476 .2057 .1845 4.8 H31 .6025 .1732 .1117 5.4 H32 .6059 .0321 .0828 5.4 H33 .5256 .1855 .0231 5.4 H41 .1509 .2409 -0.0426 5.1 H42 .1525 .3847 -0.0178 5.1 H43 .3241 .2726 -0.0352 5.1 H71 -0.3156 .1108 .3754 6.3 H72 -0.3042 -0.0194 .3337 6.3 H73 -0.2295 -0.0495 .4253 6.3 H81 .1579 -0.2521 .4499 5.7 H82 .1381 -0.1281 .4983 5.7 H83 -0.0231 -0.1659 .4755 5.7 H10 .4486 .3531 .2701 4.0 H11 .5984 .4374 .1765 4.3 H12 .4930 .5647 .0494 4.5 H13 .2087 .6022 .0149 4.5 H14 .0562 .4757 .1170 3.8 H16 -0.1204 .2770 .3590 4.4 H17 -0.4010 .4392 .3821 5.4 H18 -0.4771 .6273 .3253 5.2 H19 -0.3053 .7256 .2336 5.3 H20 -0.0391 .5840 .2033 4.6 H22 .3667 .1000 .3816 3.5 H23 .5022 .1131 .5000 4.0 H24 .4340 .3077 .5573 5.1 H25 .2090 .4856 .4978 6.3 H26 .0940 .5040 .3706 5.6 H128 .2988 -0.2028 .1001 6.9 H228 .2372 -0.0383 .0711 6.9 H328 .4013 -0.1455 .1576 6.9 H129 -0.0902 -0.0744 .1815 6.6 H229 -0.0038 -0.1208 .1115 6.6 H329 -0.0562 .0519 .0972 6.6 H130 .2740 -0.2490 .2753 5.8 H230 .1952 -0.2951 .2161 5.8 H330 .0662 -0.1944 .2810 5.8 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 Rh(1) 0.04076 0.03054 0.02836 -0.00224 -0.00562 -0.00104 P(1) 0.04635 0.02882 0.02818 -0.00229 -0.00566 0.00020 O(1) 0.04659 0.05411 0.05561 -0.00779 -0.01053 0.00676 O(2) 0.05434 0.05855 0.04018 0.00464 -0.01855 -0.00007 O(3) 0.04698 0.06697 0.05414 -0.00503 -0.01227 -0.00017 O(4) 0.06150 0.03681 0.04430 0.00323 -0.01753 0.00398 N(1) 0.04184 0.03681 0.04381 -0.00532 -0.00173 0.00177 N(2) 0.05322 0.04041 0.03305 -0.00508 -0.01005 0.00062 N(3) 0.04047 0.04369 0.04436 -0.00536 -0.00466 -0.00160 N(4) 0.05549 0.03622 0.03313 0.00107 -0.01073 0.00389 C(1) 0.06023 0.04207 0.03843 -0.00954 0.00579 -0.00774 C(2) 0.06111 0.04275 0.03252 -0.00585 -0.00316 -0.00914 C(3) 0.06510 0.07591 0.05822 -0.01911 0.01900 -0.01901 C(4) 0.09197 0.06290 0.03101 -0.00165 0.00136 -0.02557 C(5) 0.05532 0.05868 0.03975 -0.00756 0.00314 -0.01226 C(6) 0.06709 0.04640 0.03401 -0.00130 0.00039 -0.01206 C(7) 0.06882 0.11523 0.06300 -0.01081 0.01953 -0.04240 C(8) 0.10040 0.06880 0.04500 0.01196 0.00158 -0.02399 C(9) 0.05568 0.02856 0.03009 -0.00199 -0.00768 -0.00464 C(10) 0.05439 0.04390 0.04038 -0.00100 -0.00541 -0.00674 C(11) 0.06221 0.04778 0.05623 -0.01186 0.00869 -0.01832 C(12) 0.07924 0.04258 0.04147 -0.00786 0.00840 -0.01352 C(13) 0.08135 0.04134 0.03453 -0.00248 -0.00334 -0.01333 C(14) 0.06286 0.04079 0.03253 -0.00132 -0.00664 -0.00185 C(15) 0.05443 0.04360 0.03312 -0.01249 -0.00329 0.00282 C(16) 0.05979 0.05954 0.04752 -0.01518 0.00741 -0.00675 C(17) 0.06080 0.09113 0.05629 -0.03500 0.00841 -0.01351 C(18) 0.04876 0.09617 0.05825 -0.03919 -0.00634 0.01166 C(19) 0.07896 0.05328 0.07446 -0.02516 -0.02011 0.01485 C(20) 0.06379 0.04385 0.05387 -0.00696 -0.01175 0.00753 C(21) 0.05075 0.04098 0.02757 -0.00705 -0.00297 -0.00775 C(22) 0.05135 0.04233 0.03120 -0.00643 -0.00655 -0.00372 C(23) 0.06224 0.04934 0.03374 -0.00030 -0.01350 -0.00721 C(24) 0.07678 0.06962 0.03522 -0.01353 -0.01547 -0.00864 C(25) 0.11376 0.06535 0.06559 -0.03589 -0.03525 0.00944 C(26) 0.09897 0.04973 0.05893 -0.02682 -0.02903 0.00831 C(27) 0.06432 0.03843 0.05452 -0.01183 -0.00253 -0.00852 C(28) 0.11683 0.07546 0.11812 -0.06398 0.06031 -0.03951 C(29) 0.09069 0.07559 0.09333 -0.03415 -0.03553 -0.01999 C(30) 0.09229 0.04523 0.08226 -0.01862 -0.01882 -0.01816 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 N(1) Rh(1) N(2) 78.40(10) yes N(3) Rh(1) N(4) 78.80(10) yes P(1) Rh(1) N(1) 90.20(10) yes P(1) Rh(1) N(2) 87.30(10) yes P(1) Rh(1) N(3) 92.40(10) yes P(1) Rh(1) N(4) 95.80(10) yes N(1) Rh(1) C(27) 90.00(10) yes N(2) Rh(1) C(27) 87.10(10) yes N(3) Rh(1) C(27) 87.40(10) yes N(4) Rh(1) C(27) 89.90(10) yes P(1) Rh(1) C(27) 174.20(10) yes Rh(1) P(1) C(9) 109.10(10) yes Rh(1) P(1) C(15) 115.40(10) yes Rh(1) P(1) C(21) 122.20(10) yes C(9) P(1) C(15) 106.90(10) yes C(9) P(1) C(21) 102.00(10) yes C(15) P(1) C(21) 99.70(10) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Rh(1) P(1) 2.4920(10) yes Rh(1) C(27) 2.216(3) yes Rh(1) N(1) 1.934(3) yes Rh(1) N(2) 1.973(2) yes Rh(1) N(3) 1.930(3) yes Rh(1) N(4) 1.982(2) yes P(1) C(9) 1.810(3) yes P(1) C(15) 1.815(3) yes P(1) C(21) 1.822(3) yes N(1) O(1) 1.367(3) yes N(2) O(2) 1.293(4) yes N(3) O(3) 1.361(3) yes N(4) O(4) 1.281(4) yes N(1) C(1) 1.298(4) no C(1) C(2) 1.430(5) no C(1) C(3) 1.468(6) no N(2) C(2) 1.297(4) no C(2) C(4) 1.478(4) no N(3) C(5) 1.288(4) no C(5) C(6) 1.426(5) no C(5) C(7) 1.495(6) no N(4) C(6) 1.315(5) no C(6) C(8) 1.465(5) no C(27) C(28) 1.509(7) no C(27) C(29) 1.467(7) no C(27) C(30) 1.518(5) no C(9) C(10) 1.385(5) no C(10) C(11) 1.366(5) no C(11) C(12) 1.358(5) no C(12) C(13) 1.368(6) no C(13) C(14) 1.375(5) no C(14) C(9) 1.380(4) no C(15) C(16) 1.362(5) no C(16) C(17) 1.371(6) no C(17) C(18) 1.378(7) no C(18) C(19) 1.306(6) no C(19) C(20) 1.396(6) no C(20) C(15) 1.386(5) no C(21) C(22) 1.350(4) no C(22) C(23) 1.372(4) no C(23) C(24) 1.365(5) no C(24) C(25) 1.348(6) no C(25) C(26) 1.372(7) no C(26) C(21) 1.369(5) no _journal_paper_doi 10.1107/S0108270195010912