#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/32/2013260.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2013260 loop_ _publ_author_name 'Clark, Robert W.' 'Guzei, Ilia A.' 'Jin, Wiechang C.' 'Landis, Clark R.' _publ_section_title ; A 1,2,4-diazaphospholane complex of rhodium ; _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m144 _journal_page_last m145 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Rh (C8 H12) (C24 H23 N2 O4 P) Cl] , C H2 Cl2' _chemical_formula_moiety 'C32 H35 Cl N2 O4 P Rh , C H2 Cl2' _chemical_formula_sum 'C33 H37 Cl3 N2 O4 P Rh' _chemical_formula_weight 765.88 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 102.261(10) _cell_angle_beta 103.030(10) _cell_angle_gamma 95.789(10) _cell_formula_units_Z 2 _cell_length_a 11.6420(5) _cell_length_b 11.8755(5) _cell_length_c 12.7087(6) _cell_measurement_temperature 173(2) _cell_volume 1652.21(17) _diffrn_ambient_temperature 173(2) _exptl_crystal_density_diffrn 1.539 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_geom_bond_publ_flag' value 'Y' changed to 'y' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2013260 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 _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 Rh 0.275305(15) 0.173446(15) 0.961962(14) 0.02008(8) Uani d . 1 . . Rh P 0.16239(5) 0.25500(5) 0.83422(5) 0.01927(13) Uani d . 1 . . P Cl1 0.45876(5) 0.26706(6) 0.94431(6) 0.03173(15) Uani d . 1 . . Cl Cl2 0.25111(8) 0.90356(8) 0.64874(8) 0.0566(2) Uani d . 1 . . Cl Cl3 0.47067(10) 1.04469(13) 0.65436(11) 0.0907(4) Uani d . 1 . . Cl O1 0.29847(16) 0.25175(16) 0.51988(15) 0.0311(4) Uani d . 1 . . O O2 0.3692(2) 0.4348(2) 0.5184(2) 0.0597(7) Uani d . 1 . . O O3 0.14376(16) 0.63148(15) 0.84877(16) 0.0300(4) Uani d . 1 . . O O4 0.00898(15) 0.37233(15) 1.02488(14) 0.0259(4) Uani d . 1 . . O H4 -0.0373 0.3767 1.0671 0.039 Uiso calc R 1 . . H N1 0.31141(18) 0.40651(18) 0.78875(17) 0.0232(4) Uani d D 1 . . N H1 0.3696(17) 0.391(2) 0.8413(16) 0.028 Uiso d D 1 . . H N2 0.23813(17) 0.47493(17) 0.84293(16) 0.0215(4) Uani d . 1 . . N C1 0.3652(2) 0.1696(2) 1.1325(2) 0.0293(6) Uani d . 1 . . C H1A 0.4401 0.2274 1.1659 0.035 Uiso calc R 1 . . H C2 0.3799(2) 0.0694(2) 1.0649(2) 0.0297(6) Uani d . 1 . . C H2 0.4632 0.0675 1.0568 0.036 Uiso calc R 1 . . H C3 0.3096(3) -0.0493(2) 1.0522(2) 0.0349(6) Uani d . 1 . . C H3A 0.2834 -0.0505 1.1209 0.042 Uiso calc R 1 . . H H3B 0.3618 -0.1094 1.0423 0.042 Uiso calc R 1 . . H C4 0.2000(3) -0.0788(2) 0.9524(2) 0.0328(6) Uani d . 1 . . C H4A 0.2237 -0.1162 0.8849 0.039 Uiso calc R 1 . . H H4B 0.1397 -0.1359 0.9652 0.039 Uiso calc R 1 . . H C5 0.1440(2) 0.0262(2) 0.9320(2) 0.0254(5) Uani d . 1 . . C H5 0.0846 0.0107 0.8582 0.030 Uiso calc R 1 . . H C6 0.1220(2) 0.1149(2) 1.0126(2) 0.0231(5) Uani d . 1 . . C H6 0.0503 0.1506 0.9854 0.028 Uiso calc R 1 . . H C7 0.1487(2) 0.1174(2) 1.1362(2) 0.0280(5) Uani d . 1 . . C H7A 0.1387 0.0363 1.1446 0.034 Uiso calc R 1 . . H H7B 0.0901 0.1579 1.1688 0.034 Uiso calc R 1 . . H C8 0.2755(2) 0.1788(2) 1.2013(2) 0.0306(6) Uani d . 1 . . C H8A 0.2728 0.2623 1.2313 0.037 Uiso calc R 1 . . H H8B 0.3023 0.1443 1.2654 0.037 Uiso calc R 1 . . H C9 0.2338(2) 0.2956(2) 0.72495(19) 0.0229(5) Uani d . 1 . . C H9 0.2853 0.2364 0.7044 0.027 Uiso calc R 1 . . H C10 0.1602(2) 0.41415(19) 0.89699(19) 0.0201(5) Uani d . 1 . . C H10 0.0773 0.4317 0.8738 0.024 Uiso calc R 1 . . H C11 0.0109(2) 0.1831(2) 0.76125(19) 0.0238(5) Uani d . 1 . . C C12 0.0016(2) 0.0844(2) 0.6755(2) 0.0299(6) Uani d . 1 . . C H12 0.0718 0.0579 0.6602 0.036 Uiso calc R 1 . . H C13 -0.1097(3) 0.0251(2) 0.6127(2) 0.0379(7) Uani d . 1 . . C H13 -0.1157 -0.0417 0.5541 0.046 Uiso calc R 1 . . H C14 -0.2119(3) 0.0629(3) 0.6352(2) 0.0390(7) Uani d . 1 . . C H14 -0.2881 0.0225 0.5919 0.047 Uiso calc R 1 . . H C15 -0.2034(2) 0.1595(3) 0.7206(2) 0.0350(6) Uani d . 1 . . C H15 -0.2738 0.1851 0.7361 0.042 Uiso calc R 1 . . H C16 -0.0925(2) 0.2195(2) 0.7839(2) 0.0277(5) Uani d . 1 . . C H16 -0.0872 0.2856 0.8430 0.033 Uiso calc R 1 . . H C17 0.1522(2) 0.3105(2) 0.6195(2) 0.0236(5) Uani d . 1 . . C C18 0.0421(2) 0.3493(2) 0.6149(2) 0.0277(5) Uani d . 1 . . C H18 0.0168 0.3700 0.6815 0.033 Uiso calc R 1 . . H C19 -0.0306(3) 0.3585(2) 0.5161(2) 0.0324(6) Uani d . 1 . . C H19 -0.1053 0.3846 0.5152 0.039 Uiso calc R 1 . . H C20 0.0052(3) 0.3295(3) 0.4179(2) 0.0365(6) Uani d . 1 . . C H20 -0.0457 0.3335 0.3494 0.044 Uiso calc R 1 . . H C21 0.1143(3) 0.2950(2) 0.4208(2) 0.0345(6) Uani d . 1 . . C H21 0.1403 0.2765 0.3543 0.041 Uiso calc R 1 . . H C22 0.1869(2) 0.2873(2) 0.5207(2) 0.0270(5) Uani d . 1 . . C C23 0.3848(3) 0.3366(3) 0.5149(2) 0.0394(7) Uani d . 1 . . C C24 0.4964(3) 0.2877(3) 0.5041(3) 0.0549(9) Uani d . 1 . . C H24A 0.5480 0.3419 0.4798 0.082 Uiso calc R 1 . . H H24B 0.4756 0.2124 0.4492 0.082 Uiso calc R 1 . . H H24C 0.5385 0.2768 0.5764 0.082 Uiso calc R 1 . . H C25 0.2201(2) 0.5778(2) 0.8182(2) 0.0232(5) Uani d . 1 . . C C26 0.2995(2) 0.6241(2) 0.7537(2) 0.0332(6) Uani d . 1 . . C H26A 0.2807 0.7003 0.7434 0.050 Uiso calc R 1 . . H H26B 0.2863 0.5698 0.6808 0.050 Uiso calc R 1 . . H H26C 0.3832 0.6326 0.7948 0.050 Uiso calc R 1 . . H C27 0.2024(2) 0.44839(19) 1.02271(19) 0.0217(5) Uani d . 1 . . C C28 0.3175(2) 0.5021(2) 1.0798(2) 0.0326(6) Uani d . 1 . . C H28 0.3736 0.5188 1.0392 0.039 Uiso calc R 1 . . H C29 0.3520(3) 0.5318(3) 1.1953(2) 0.0417(7) Uani d . 1 . . C H29 0.4318 0.5670 1.2331 0.050 Uiso calc R 1 . . H C30 0.2706(3) 0.5103(3) 1.2551(2) 0.0385(7) Uani d . 1 . . C H30 0.2940 0.5312 1.3342 0.046 Uiso calc R 1 . . H C31 0.1542(2) 0.4579(2) 1.1997(2) 0.0293(6) Uani d . 1 . . C H31 0.0978 0.4439 1.2408 0.035 Uiso calc R 1 . . H C32 0.1207(2) 0.4262(2) 1.0843(2) 0.0222(5) Uani d . 1 . . C C33 0.3886(3) 0.9835(3) 0.7328(3) 0.0543(9) Uani d . 1 . . C H33A 0.3740 1.0462 0.7910 0.065 Uiso calc R 1 . . H H33B 0.4351 0.9313 0.7702 0.065 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 Rh 0.02073(11) 0.01997(11) 0.02029(11) 0.00314(7) 0.00422(7) 0.00757(7) P 0.0213(3) 0.0184(3) 0.0181(3) 0.0022(2) 0.0041(2) 0.0058(2) Cl1 0.0223(3) 0.0366(3) 0.0400(4) 0.0030(3) 0.0067(3) 0.0194(3) Cl2 0.0517(5) 0.0661(6) 0.0541(5) 0.0065(4) 0.0065(4) 0.0277(4) Cl3 0.0603(7) 0.1134(10) 0.0835(8) -0.0229(6) 0.0200(6) 0.0069(7) O1 0.0345(10) 0.0339(10) 0.0267(9) 0.0056(8) 0.0138(8) 0.0050(8) O2 0.0591(15) 0.0464(14) 0.0784(18) -0.0038(12) 0.0293(14) 0.0185(13) O3 0.0350(10) 0.0235(9) 0.0383(10) 0.0078(8) 0.0173(8) 0.0118(8) O4 0.0255(9) 0.0287(9) 0.0238(9) 0.0000(7) 0.0103(7) 0.0049(7) N1 0.0226(10) 0.0243(10) 0.0252(11) 0.0052(8) 0.0089(8) 0.0079(8) N2 0.0240(10) 0.0211(10) 0.0222(10) 0.0031(8) 0.0096(8) 0.0072(8) C1 0.0227(12) 0.0409(15) 0.0234(13) 0.0020(11) -0.0011(10) 0.0147(11) C2 0.0248(13) 0.0401(15) 0.0315(14) 0.0140(11) 0.0076(11) 0.0199(12) C3 0.0379(15) 0.0338(15) 0.0447(16) 0.0174(12) 0.0170(13) 0.0219(13) C4 0.0464(16) 0.0209(12) 0.0354(15) 0.0072(11) 0.0154(12) 0.0100(11) C5 0.0298(13) 0.0216(12) 0.0240(12) -0.0010(10) 0.0059(10) 0.0075(10) C6 0.0235(12) 0.0238(12) 0.0235(12) 0.0007(9) 0.0065(10) 0.0096(10) C7 0.0288(13) 0.0334(14) 0.0242(13) 0.0052(11) 0.0087(10) 0.0094(11) C8 0.0337(14) 0.0370(14) 0.0210(12) 0.0059(11) 0.0051(11) 0.0085(11) C9 0.0284(12) 0.0228(12) 0.0212(12) 0.0076(10) 0.0101(10) 0.0075(9) C10 0.0214(11) 0.0191(11) 0.0218(12) 0.0029(9) 0.0083(9) 0.0061(9) C11 0.0291(13) 0.0217(12) 0.0194(11) 0.0012(10) 0.0005(9) 0.0101(9) C12 0.0373(15) 0.0238(12) 0.0267(13) 0.0019(11) 0.0036(11) 0.0083(10) C13 0.0528(18) 0.0276(14) 0.0247(14) -0.0053(13) -0.0010(12) 0.0046(11) C14 0.0344(15) 0.0428(16) 0.0303(15) -0.0127(13) -0.0070(12) 0.0137(13) C15 0.0278(14) 0.0428(16) 0.0336(15) -0.0008(12) 0.0021(11) 0.0167(12) C16 0.0284(13) 0.0302(13) 0.0231(12) 0.0005(10) 0.0028(10) 0.0094(10) C17 0.0310(13) 0.0193(11) 0.0213(12) 0.0024(10) 0.0069(10) 0.0068(9) C18 0.0362(14) 0.0264(13) 0.0244(13) 0.0068(11) 0.0111(11) 0.0098(10) C19 0.0347(14) 0.0319(14) 0.0352(15) 0.0095(11) 0.0083(12) 0.0166(12) C20 0.0413(16) 0.0417(16) 0.0246(13) 0.0032(13) 0.0001(12) 0.0138(12) C21 0.0462(17) 0.0355(15) 0.0226(13) 0.0033(12) 0.0108(12) 0.0080(11) C22 0.0321(13) 0.0234(12) 0.0253(13) 0.0017(10) 0.0079(10) 0.0063(10) C23 0.0397(16) 0.0468(18) 0.0279(14) -0.0021(13) 0.0104(12) 0.0037(13) C24 0.0373(18) 0.072(2) 0.0475(19) 0.0001(16) 0.0139(15) -0.0020(17) C25 0.0255(12) 0.0213(12) 0.0224(12) 0.0002(10) 0.0054(10) 0.0066(9) C26 0.0353(15) 0.0294(14) 0.0440(16) 0.0055(11) 0.0187(13) 0.0189(12) C27 0.0272(12) 0.0174(11) 0.0211(12) 0.0039(9) 0.0069(10) 0.0049(9) C28 0.0325(14) 0.0354(14) 0.0278(13) -0.0021(11) 0.0109(11) 0.0029(11) C29 0.0338(15) 0.0527(18) 0.0270(14) -0.0090(13) 0.0005(12) -0.0001(13) C30 0.0450(17) 0.0438(16) 0.0201(13) -0.0019(13) 0.0060(12) 0.0002(12) C31 0.0360(14) 0.0304(13) 0.0238(13) 0.0032(11) 0.0121(11) 0.0075(10) C32 0.0264(12) 0.0168(11) 0.0246(12) 0.0056(9) 0.0071(10) 0.0058(9) C33 0.060(2) 0.055(2) 0.0416(18) 0.0155(17) -0.0002(16) 0.0102(16) 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 Rh C5 . 2.111(2) ? Rh C6 . 2.130(2) ? Rh C1 . 2.197(2) ? Rh C2 . 2.235(2) ? Rh P . 2.2943(6) y Rh Cl1 . 2.3856(7) y P C11 . 1.823(2) ? P C9 . 1.891(2) ? P C10 . 1.894(2) ? Cl2 C33 . 1.759(4) ? Cl3 C33 . 1.741(4) ? O1 C23 . 1.372(4) ? O1 C22 . 1.408(3) ? O2 C23 . 1.191(4) ? O3 C25 . 1.230(3) ? O4 C32 . 1.361(3) ? O4 H4 . 0.8400 ? N1 N2 . 1.425(3) ? N1 C9 . 1.478(3) ? N1 H1 . 0.90(2) ? N2 C25 . 1.349(3) ? N2 C10 . 1.475(3) ? C1 C2 . 1.362(4) y C1 C8 . 1.504(4) ? C1 H1A . 1.0000 ? C2 C3 . 1.514(4) ? C2 H2 . 1.0000 ? C3 C4 . 1.533(4) ? C3 H3A . 0.9900 ? C3 H3B . 0.9900 ? C4 C5 . 1.507(3) ? C4 H4A . 0.9900 ? C4 H4B . 0.9900 ? C5 C6 . 1.392(3) y C5 H5 . 1.0000 ? C6 C7 . 1.524(3) ? C6 H6 . 1.0000 ? C7 C8 . 1.539(4) ? C7 H7A . 0.9900 ? C7 H7B . 0.9900 ? C8 H8A . 0.9900 ? C8 H8B . 0.9900 ? C9 C17 . 1.514(3) ? C9 H9 . 1.0000 ? C10 C27 . 1.513(3) ? C10 H10 . 1.0000 ? C11 C16 . 1.387(4) ? C11 C12 . 1.396(3) ? C12 C13 . 1.387(4) ? C12 H12 . 0.9500 ? C13 C14 . 1.381(4) ? C13 H13 . 0.9500 ? C14 C15 . 1.379(4) ? C14 H14 . 0.9500 ? C15 C16 . 1.387(4) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? C17 C22 . 1.385(3) ? C17 C18 . 1.399(4) ? C18 C19 . 1.379(4) ? C18 H18 . 0.9500 ? C19 C20 . 1.389(4) ? C19 H19 . 0.9500 ? C20 C21 . 1.369(4) ? C20 H20 . 0.9500 ? C21 C22 . 1.384(4) ? C21 H21 . 0.9500 ? C23 C24 . 1.497(4) ? C24 H24A . 0.9800 ? C24 H24B . 0.9800 ? C24 H24C . 0.9800 ? C25 C26 . 1.504(3) ? C26 H26A . 0.9800 ? C26 H26B . 0.9800 ? C26 H26C . 0.9800 ? C27 C28 . 1.385(4) ? C27 C32 . 1.400(3) ? C28 C29 . 1.387(4) ? C28 H28 . 0.9500 ? C29 C30 . 1.379(4) ? C29 H29 . 0.9500 ? C30 C31 . 1.390(4) ? C30 H30 . 0.9500 ? C31 C32 . 1.387(4) ? C31 H31 . 0.9500 ? C33 H33A . 0.9900 ? C33 H33B . 0.9900 ?