#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2006119.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_2006119 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1997 _journal_volume 53 _journal_page_first 579 _journal_page_last 581 _publ_section_title ; 2:1 Complex of N,N',N''-Trimethylnitrilotriacetamide and Pb(NO~3~)~2~ ; _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name _publ_author_footnote 'Skrzypczak-Jankun, Ewa' 'Smith, Douglas, A.' _chemical_formula_sum 'C18 H36 N10 O12 Pb' _chemical_formula_structural '[ N(CH~2~CONHCH~3~)~3~]~2~, Pb(NO~3~)~2~' _chemical_formula_iupac '[Pb (C9 H18 N4 O3)2] (N O3)2' _chemical_formula_weight 791.74 _symmetry_cell_setting monoclinic 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' _cell_length_a 12.148(2) _cell_length_b 20.749(3) _cell_length_c 13.026(2) _cell_angle_alpha 90 _cell_angle_beta 113.680(10) _cell_angle_gamma 90 _cell_volume 3007.0(10) _cell_formula_units_z 4 _cell_measurement_temperature 294 _exptl_crystal_density_diffrn 1.75 _refine_ls_R_factor_obs .028 _refine_ls_wR_factor_obs .035 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Pb .076500(10) .085580(10) .127400(10) .03537(4) Uani ? N1 .2863(3) .1074(2) .3264(3) .0380(10) Uani ? C2 .2615(4) .0864(3) .4229(4) .0450(10) Uani ? C3 .1852(4) .0266(3) .3957(4) .0440(10) Uani ? O4 .1173(3) .0117(2) .2989(3) .0580(10) Uani ? N5 .1887(4) -.0071(2) .4836(3) .057(2) Uani ? C6 .1106(6) -.0624(3) .4737(5) .076(2) Uani ? C7 .3092(4) .1772(2) .3337(4) .0420(10) Uani ? C8 .2977(4) .2046(2) .2213(4) .0390(10) Uani ? O9 .2097(3) .1896(2) .1344(3) .0550(10) Uani ? N10 .3817(4) .2442(2) .2243(3) .0540(10) Uani ? C11 .3838(6) .2738(3) .1235(5) .082(2) Uani ? C12 .3865(4) .0711(3) .3202(4) .048(2) Uani ? C13 .3812(4) .0696(3) .2021(4) .045(2) Uani ? O14 .2917(3) .0471(2) .1265(3) .0560(10) Uani ? N15 .4732(4) .0941(2) .1868(4) .0560(10) Uani ? C16 .4759(5) .0949(4) .0770(5) .090(3) Uani ? N17 -.1580(3) .0931(2) .1129(3) .0360(10) Uani ? C18 -.1699(4) .0370(2) .1758(4) .0420(10) Uani ? C19 -.1294(4) -.0245(2) .1365(4) .0370(10) Uani ? O20 -.0643(3) -.0226(2) .0833(2) .0410(10) Uani ? N21 -.1664(4) -.0777(2) .1675(3) .0460(10) Uani ? C22 -.1298(5) -.1421(3) .1470(5) .065(2) Uani ? C23 -.2442(4) .0908(3) -.0048(4) .046(2) Uani ? C24 -.1976(4) .1251(3) -.0811(4) .0400(10) Uani ? O25 -.0931(3) .1444(2) -.0486(3) .0470(10) Uani ? N26 -.2777(4) .1311(2) -.1850(3) .0550(10) Uani ? C27 -.2484(5) .1571(4) -.2746(4) .078(2) Uani ? C28 -.1724(4) .1529(3) .1669(4) .0420(10) Uani ? C29 -.0607(4) .1673(2) .2694(4) .0390(10) Uani ? O30 .0398(3) .1581(2) .2701(3) .0550(10) Uani ? N31 -.0769(3) .1897(2) .3579(3) .0460(10) Uani ? C32 .0239(5) .2097(3) .4609(4) .061(2) Uani ? N33 -.5845(4) .0687(3) -.2606(3) .058(2) Uani ? O34 -.5205(3) .0618(2) -.3133(3) .0720(10) Uani ? O35 -.5456(5) .0966(3) -.1708(4) .120(2) Uani ? O36 -.6898(4) .0495(3) -.2991(3) .0800(10) Uani ? N37 -.3243(4) .2865(3) -.0749(3) .057(2) Uani ? O38 -.4084(4) .2609(3) -.0596(4) .096(2) Uani ? O39 -.2222(3) .2797(2) -.0038(3) .078(2) Uani ? O40 -.3387(4) .3158(3) -.1627(3) .091(2) Uani ? HN5 .2445 .0031 .5650 .0746 Uiso calc HN10 .4571 .2520 .2901 .0674 Uiso calc HN15 .5389 .1116 .2488 .0641 Uiso calc HN21 -.2186 -.0823 .2040 .0609 Uiso calc HN26 -.3589 .1165 -.2140 .0700 Uiso calc HN31 -.1627 .1940 .3554 .0643 Uiso calc HC21 .2209 .1198 .4434 .0576 Uiso calc HC22 .3357 .0774 .4838 .0576 Uiso calc HC61 .0618 -.0692 .3966 .0986 Uiso calc HC62 .1567 -.1001 .5042 .0986 Uiso calc HC63 .0609 -.0534 .5127 .0986 Uiso calc HC71 .3882 .1849 .3880 .0548 Uiso calc HC72 .2527 .1981 .3558 .0548 Uiso calc HC111 .3104 .2658 .0609 .1019 Uiso calc HC112 .3947 .3189 .1356 .1019 Uiso calc HC113 .4487 .2565 .1094 .1019 Uiso calc HC121 .3832 .0281 .3439 .0623 Uiso calc HC122 .4601 .0904 .3684 .0623 Uiso calc HC161 .4067 .0740 .0242 .1154 Uiso calc HC162 .4771 .1385 .0554 .1154 Uiso calc HC163 .5461 .0735 .0795 .1154 Uiso calc HC181 -.2517 .0323 .1647 .0541 Uiso calc HC182 -.1219 .0432 .2533 .0541 Uiso calc HC221 -.0767 -.1386 .1101 .0807 Uiso calc HC222 -.0903 -.1639 .2165 .0807 Uiso calc HC223 -.1992 -.1658 .1013 .0807 Uiso calc HC231 -.3171 .1107 -.0112 .0595 Uiso calc HC232 -.2592 .0470 -.0275 .0595 Uiso calc HC271 -.1673 .1715 -.2447 .0996 Uiso calc HC272 -.2587 .1247 -.3291 .0996 Uiso calc HC273 -.3002 .1924 -.3087 .0996 Uiso calc HC281 -.2386 .1485 .1877 .0550 Uiso calc HC282 -.1873 .1876 .1154 .0550 Uiso calc HC321 .0978 .2036 .4534 .0755 Uiso calc HC322 .0150 .2539 .4748 .0755 Uiso calc HC323 .0235 .1845 .5216 .0755 Uiso calc 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 Pb .03367(7) .04146(9) .03067(7) -.00335(9) .01260(5) -.00224(9) N1 .038(2) .041(2) .035(2) -.003(2) .0150(10) -.001(2) C2 .048(2) .056(3) .030(2) -.002(3) .015(2) .004(2) C3 .052(3) .043(3) .035(2) .005(2) .015(2) .003(2) O4 .071(2) .055(2) .038(2) -.020(2) .0120(10) .000(2) N5 .081(3) .053(3) .036(2) -.011(2) .023(2) .006(2) C6 .101(4) .067(4) .068(3) -.017(4) .043(2) .006(3) C7 .039(2) .048(3) .033(2) -.012(2) .007(2) -.006(2) C8 .038(2) .034(3) .039(2) -.001(2) .010(2) .001(2) O9 .048(2) .054(2) .047(2) -.009(2) .0040(10) .007(2) N10 .052(2) .056(3) .044(2) -.018(2) .007(2) .008(2) C11 .093(4) .081(4) .065(3) -.030(4) .023(3) .016(3) C12 .043(2) .053(4) .044(2) .009(2) .013(2) -.001(2) C13 .035(2) .057(3) .041(2) .004(2) .012(2) -.010(2) O14 .041(2) .073(3) .051(2) -.010(2) .0150(10) -.028(2) N15 .033(2) .084(4) .048(2) -.007(2) .014(2) -.012(2) C16 .062(3) .161(8) .055(3) -.016(4) .032(2) -.012(4) N17 .036(2) .037(2) .035(2) -.003(2) .0150(10) .001(2) C18 .045(2) .047(3) .037(2) -.001(2) .018(2) .004(2) C19 .037(2) .040(3) .034(2) -.006(2) .012(2) .001(2) O20 .0390(10) .052(2) .0360(10) -.005(2) .0190(10) -.0070(10) N21 .053(2) .044(3) .049(2) -.010(2) .0280(10) -.003(2) C22 .075(3) .045(3) .083(3) -.009(3) .040(2) -.003(3) C23 .037(2) .055(3) .040(2) -.005(2) .011(2) -.001(2) C24 .037(2) .043(3) .037(2) .002(2) .010(2) -.001(2) O25 .038(2) .059(2) .044(2) -.007(2) .0150(10) .005(2) N26 .047(2) .078(3) .034(2) -.007(2) .008(2) .005(2) C27 .076(4) .110(6) .045(3) -.007(4) .020(2) .011(3) C28 .038(2) .049(3) .043(2) .007(2) .018(2) .003(2) C29 .045(2) .030(3) .047(2) .002(2) .022(2) -.001(2) O30 .036(2) .074(3) .058(2) -.010(2) .0220(10) -.028(2) N31 .044(2) .050(3) .043(2) .001(2) .0180(10) -.008(2) C32 .059(3) .068(4) .055(3) -.005(3) .021(2) -.023(3) N33 .051(2) .077(3) .039(2) -.004(2) .013(2) .003(2) O34 .055(2) .093(3) .076(2) .019(2) .0330(10) .016(2) O35 .099(3) .196(6) .059(2) -.040(4) .025(2) -.041(3) O36 .060(2) .128(4) .055(2) -.036(2) .0270(10) -.021(2) N37 .045(2) .079(3) .046(2) .006(2) .016(2) .007(2) O38 .055(2) .160(5) .072(2) -.007(3) .026(2) .019(3) O39 .045(2) .096(3) .079(3) .004(2) .011(2) .028(2) O40 .070(2) .131(4) .068(2) .027(3) .024(2) .043(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 C2 1.471(7) yes N1 C7 1.469(7) yes N1 C12 1.462(7) yes C2 C3 1.503(7) no C2 HC21 .9500 no C2 HC22 .9500 no C3 O4 1.237(5) yes C3 N5 1.328(7) yes N5 C6 1.462(8) no N5 HN5 1.0255 no C6 HC61 .9500 no C6 HC62 .9500 no C6 HC63 .9500 no C7 C8 1.523(7) no C7 HC71 .9500 no C7 HC72 .9500 no C8 O9 1.245(5) yes C8 N10 1.299(7) yes N10 C11 1.458(8) no N10 HN10 .9844 no C11 HC111 .9500 no C11 HC112 .9500 no C11 HC113 .9500 no C12 C13 1.514(8) no C12 HC121 .9500 no C12 HC122 .9500 no C13 O14 1.228(5) yes C13 N15 1.315(8) yes N15 C16 1.443(8) no N15 HN15 .9452 no C16 HC161 .9500 no C16 HC162 .9500 no C16 HC163 .9500 no N17 C18 1.464(7) yes N17 C23 1.469(5) yes N17 C28 1.472(7) yes C18 C19 1.527(7) no C18 HC181 .9500 no C18 HC182 .9500 no C19 O20 1.243(7) yes C19 N21 1.315(7) yes N21 C22 1.467(7) no N21 HN21 .9382 no C22 HC221 .9500 no C22 HC222 .9500 no C22 HC223 .9500 no C23 C24 1.506(8) no C23 HC231 .9500 no C23 HC232 .9500 no C24 O25 1.233(6) yes C24 N26 1.317(5) yes N26 C27 1.455(9) no N26 HN26 .9533 no C27 HC271 .9500 no C27 HC272 .9500 no C27 HC273 .9500 no C28 C29 1.503(5) no C28 HC281 .9500 no C28 HC282 .9500 no C29 O30 1.232(6) yes C29 N31 1.328(7) yes N31 C32 1.466(6) yes N31 HN31 1.0347 no C32 HC321 .9500 no C32 HC322 .9500 no C32 HC323 .9500 no N33 O34 1.235(8) no N33 O35 1.217(7) no N33 O36 1.238(6) no N37 O38 1.237(7) no N37 O39 1.222(5) no N37 O40 1.243(7) no