#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2200431.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_2200431 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2001 _journal_volume 57 _journal_page_first m399 _journal_page_last m401 _publ_section_title ; Dichloro[2,2-diphenyl-4,4,6,6-tetrakis(3,5-dimethylpyrazol-1-yl)- cyclotriphosphazene]cobalt(II) ; _space_group_IT_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _[local]_cod_cif_authors_sg_H-M 'C 2/c' loop_ _publ_author_name 'Prabakaran, P.' 'Justin Thomas, K. R.' 'Thomas Muthiah, P.' 'Bocelli, G.' 'Righi, L.' _chemical_name_common ; Dichloro(2,2-diphenyl-4,4,6,6-tetrakis(3,5-dimethylpyrazol-1-yl)- cyclotriphosphazeneCobalt(II) ; _chemical_formula_moiety 'C32 H38 Cl2 Co N11 P3' _chemical_formula_sum 'C32 H38 Cl2 Co N11 P3' _chemical_formula_structural '[N3P3(C5H7N2)4(Ph)2].CoCl2' _chemical_formula_iupac '[Co Cl2 (C32 H38 N11 P3)]' _chemical_formula_weight 799.47 _chemical_melting_point '221 dec' _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.755(3) _cell_length_b 9.378(3) _cell_length_c 22.043(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.19(3) _cell_angle_gamma 90.00 _cell_volume 7611(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.395 _diffrn_ambient_temperature 293(2) 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 Co .107332(15) .08260(6) .64398(2) .03451(16) Uani d . 1 . . Co Cl1 .14970(3) .15821(13) .73627(5) .0531(3) Uani d . 1 . . Cl Cl2 .06071(3) -.05287(13) .65412(6) .0611(4) Uani d . 1 . . Cl N5 .14187(8) -.0842(4) .62750(14) .0353(9) Uani d . 1 . . N N4 .15796(8) -.0591(3) .58043(14) .0320(9) Uani d . 1 . . N C13 .18335(11) -.1631(5) .5821(2) .0425(12) Uani d . 1 . . C C14 .18313(11) -.2520(5) .6304(2) .0447(12) Uani d . 1 . . C H14 .1976 -.3325 .6435 .050 Uiso calc . 1 . . H C15 .15756(11) -.2015(5) .6568(2) .0379(12) Uani d . 1 . . C C16 .20494(12) -.1613(5) .5363(2) .0620(15) Uani d . 1 . . C H16A .1976 -.0816 .5079 .050 Uiso calc . 1 . . H H16B .2008 -.2481 .5121 .050 Uiso calc . 1 . . H H16C .2303 -.1529 .5597 .050 Uiso calc . 1 . . H C17 .14715(12) -.2648(5) .7112(2) .0621(15) Uani d . 1 . . C H17A .1285 -.2078 .7192 .050 Uiso calc . 1 . . H H17B .1680 -.2670 .7487 .050 Uiso calc . 1 . . H H17C .1383 -.3601 .7003 .050 Uiso calc . 1 . . H P2 .14202(3) .07504(13) .52784(5) .0301(3) Uani d . 1 . . P N6 .12074(8) -.0100(3) .45962(15) .0359(9) Uani d . 1 . . N N7 .09186(10) -.0971(4) .46213(16) .0538(11) Uani d . 1 . . N C18 .07513(13) -.1289(5) .4023(2) .0599(16) Uani d . 1 . . C C19 .09191(13) -.0699(6) .36077(19) .0630(15) Uani d . 1 . . C H19 .0851 -.0815 .3167 .050 Uiso calc . 1 . . H C20 .12039(12) .0083(5) .3976(2) .0471(13) Uani d . 1 . . C C21 .04142(14) -.2185(6) .3855(2) .105(2) Uani d . 1 . . C H21A .0363 -.2455 .4238 .050 Uiso calc . 1 . . H H21B .0450 -.3026 .3633 .050 Uiso calc . 1 . . H H21C .0214 -.1648 .3585 .050 Uiso calc . 1 . . H C22 .14643(13) .0969(6) .37685(19) .0749(17) Uani d . 1 . . C H22A .1637 .1393 .4135 .050 Uiso calc . 1 . . H H22B .1335 .1707 .3487 .050 Uiso calc . 1 . . H H22C .1590 .0381 .3549 .050 Uiso calc . 1 . . H N1 .17303(8) .1696(3) .51749(14) .0321(9) Uani d . 1 . . N P1 .17412(3) .34171(13) .52595(5) .0332(3) Uani d . 1 . . P N3 .13776(7) .4112(3) .53470(13) .0317(8) Uani d . 1 . . N P3 .10493(3) .31585(12) .53502(5) .0306(3) Uani d . 1 . . P N2 .11321(7) .1508(3) .55672(12) .0269(8) Uani d . 1 . . N N8 .08363(8) .3769(4) .58572(15) .0368(10) Uani d . 1 . . N N9 .07925(9) .2867(4) .63302(15) .0379(10) Uani d . 1 . . N C23 .06250(12) .3661(5) .6638(2) .0477(14) Uani d . 1 . . C C24 .05621(13) .5042(5) .6393(2) .0606(16) Uani d . 1 . . C H24 .0449 .5779 .6541 .050 Uiso calc . 1 . . H C25 .06984(12) .5098(5) .5898(2) .0452(13) Uani d . 1 . . C C26 .05355(12) .3046(5) .7204(2) .0687(16) Uani d . 1 . . C H26A .0613 .2069 .7263 .050 Uiso calc . 1 . . H H26B .0278 .3095 .7129 .050 Uiso calc . 1 . . H H26C .0659 .3583 .7580 .050 Uiso calc . 1 . . H C27 .07229(13) .6285(5) .5467(2) .0753(17) Uani d . 1 . . C H27A .0843 .5956 .5172 .050 Uiso calc . 1 . . H H27B .0859 .7057 .5715 .050 Uiso calc . 1 . . H H27C .0483 .6609 .5234 .050 Uiso calc . 1 . . H N10 .07212(8) .3221(3) .46325(14) .0325(9) Uani d . 1 . . N N11 .08347(9) .3548(4) .41048(16) .0435(10) Uani d . 1 . . N C28 .05688(13) .3084(5) .3613(2) .0520(14) Uani d . 1 . . C C29 .02938(12) .2420(5) .3792(2) .0557(14) Uani d . 1 . . C H29 .0084 .1999 .3524 .050 Uiso calc . 1 . . H C30 .03948(11) .2512(5) .4435(2) .0448(12) Uani d . 1 . . C C31 .05900(13) .3244(6) .2954(2) .093(2) Uani d . 1 . . C H31A .0810 .3735 .2969 .050 Uiso calc . 1 . . H H31B .0385 .3781 .2700 .050 Uiso calc . 1 . . H H31C .0589 .2318 .2767 .050 Uiso calc . 1 . . H C32 .02140(11) .1944(6) .4894(2) .096(2) Uani d . 1 . . C H32A .0359 .2168 .5323 .050 Uiso calc . 1 . . H H32B .0189 .0928 .4847 .050 Uiso calc . 1 . . H H32C -.0022 .2371 .4808 .050 Uiso calc . 1 . . H C1 .18243(10) .4223(5) .45740(18) .0364(11) Uani d . 1 . . C C2 .16117(12) .5368(5) .4268(2) .0543(14) Uani d . 1 . . C H2 .1430 .5730 .4418 .050 Uiso calc . 1 . . H C3 .16748(13) .5948(6) .3749(2) .0693(16) Uani d . 1 . . C H3 .1537 .6726 .3550 .050 Uiso calc . 1 . . H C4 .19313(15) .5432(7) .3512(2) .0757(19) Uani d . 1 . . C H4 .1965 .5843 .3150 .050 Uiso calc . 1 . . H C5 .21421(13) .4304(6) .3803(2) .0664(16) Uani d . 1 . . C H5 .2322 .3952 .3646 .050 Uiso calc . 1 . . H C6 .20845(12) .3699(5) .4329(2) .0518(14) Uani d . 1 . . C H6 .2224 .2921 .4524 .050 Uiso calc . 1 . . H C7 .21172(10) .3846(4) .59637(19) .0311(11) Uani d . 1 . . C C8 .24038(11) .4716(5) .59429(19) .0425(12) Uani d . 1 . . C H8 .2418 .5057 .5555 .050 Uiso calc . 1 . . H C9 .26703(11) .5068(5) .6514(3) .0593(15) Uani d . 1 . . C H9 .2859 .5671 .6506 .050 Uiso calc . 1 . . H C10 .26580(12) .4545(6) .7079(2) .0598(16) Uani d . 1 . . C H10 .2837 .4792 .7456 .050 Uiso calc . 1 . . H C11 .23810(13) .3652(5) .7097(2) .0578(15) Uani d . 1 . . C H11 .2376 .3275 .7485 .050 Uiso calc . 1 . . H C12 .21079(11) .3311(5) .6540(2) .0464(13) Uani d . 1 . . C H12 .1918 .2719 .6555 .050 Uiso calc . 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 Co .0360(3) .0357(4) .0297(3) .0022(4) .0071(3) .0041(3) Cl1 .0518(8) .0597(9) .0373(7) .0056(7) -.0010(6) -.0052(7) Cl2 .0524(8) .0583(10) .0779(9) -.0117(7) .0278(7) .0034(8) N5 .042(2) .036(2) .027(2) .008(2) .0108(17) .010(2) N4 .039(2) .026(2) .033(2) .0096(19) .0127(17) .0018(18) C13 .044(3) .029(3) .053(3) .009(3) .012(3) -.005(3) C14 .057(3) .027(3) .045(3) .012(3) .008(3) .010(3) C15 .048(3) .028(3) .033(3) .003(2) .006(2) .001(2) C16 .071(4) .041(3) .081(4) .020(3) .034(3) .005(3) C17 .078(4) .055(4) .051(3) .015(3) .016(3) .012(3) P2 .0349(7) .0254(7) .0292(6) .0027(7) .0089(5) -.0001(6) N6 .043(2) .034(2) .027(2) -.010(2) .0057(18) -.0031(19) N7 .068(3) .050(3) .040(2) -.027(2) .012(2) -.006(2) C18 .066(4) .066(4) .041(3) -.036(3) .007(3) -.010(3) C19 .084(4) .068(4) .033(3) -.034(4) .013(3) -.015(3) C20 .068(4) .045(3) .038(3) -.010(3) .030(3) -.007(3) C21 .114(5) .136(6) .053(4) -.067(5) .007(4) .000(4) C22 .101(4) .098(5) .037(3) -.020(4) .039(3) -.015(3) N1 .030(2) .029(2) .039(2) -.0011(18) .0124(17) .0049(19) P1 .0333(7) .0277(7) .0376(7) .0000(6) .0096(6) .0011(6) N3 .0275(19) .0236(19) .040(2) -.0023(19) .0052(16) .0012(19) P3 .0298(7) .0298(7) .0312(7) .0061(6) .0079(6) .0025(6) N2 .0285(19) .028(2) .0255(18) -.0002(17) .0097(15) .0013(17) N8 .049(2) .032(2) .033(2) .0124(19) .0172(19) .0042(18) N9 .044(2) .043(3) .027(2) .004(2) .0118(18) .006(2) C23 .054(3) .060(4) .035(3) .012(3) .021(3) .004(3) C24 .092(4) .044(3) .061(4) .037(3) .044(3) .007(3) C25 .057(3) .034(3) .049(3) .023(3) .021(3) .006(3) C26 .089(4) .074(4) .052(3) .020(3) .035(3) .003(3) C27 .118(5) .038(4) .077(4) .037(3) .043(3) .014(3) N10 .025(2) .041(2) .026(2) .0004(19) .0002(17) .0069(19) N11 .050(2) .051(3) .028(2) -.002(2) .0102(19) .006(2) C28 .063(4) .063(4) .026(3) -.005(3) .008(3) .006(3) C29 .044(3) .068(4) .042(3) -.007(3) -.005(3) .004(3) C30 .037(3) .063(3) .035(3) -.003(3) .012(2) .008(3) C31 .107(5) .120(5) .043(3) -.020(4) .011(3) .002(4) C32 .037(3) .166(6) .075(4) -.035(4) .003(3) .020(4) C1 .035(3) .037(3) .037(3) -.010(3) .012(2) .000(3) C2 .055(3) .051(4) .063(4) .002(3) .027(3) .017(3) C3 .072(4) .063(4) .068(4) .004(3) .015(3) .034(4) C4 .080(4) .094(6) .059(4) -.020(4) .032(3) .028(4) C5 .075(4) .074(4) .064(4) -.007(4) .043(3) .000(4) C6 .059(3) .048(4) .053(3) .005(3) .026(3) .007(3) C7 .024(2) .028(3) .039(3) .004(2) .007(2) -.006(2) C8 .037(3) .046(3) .043(3) .005(3) .010(2) -.005(3) C9 .026(3) .061(4) .085(4) -.006(3) .009(3) -.009(3) C10 .045(3) .073(5) .050(3) .006(3) -.002(3) -.018(3) C11 .060(4) .070(4) .038(3) .002(3) .008(3) .005(3) C12 .041(3) .055(3) .043(3) -.007(3) .012(2) .002(3) 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 Co N2 . 2.106(3) yes Co N5 . 2.162(3) yes Co N9 . 2.177(3) yes Co Cl2 . 2.2760(13) yes Co Cl1 . 2.2917(14) yes N5 C15 . 1.324(5) ? N5 N4 . 1.387(4) ? N4 C13 . 1.378(4) ? N4 P2 . 1.692(3) ? C13 C14 . 1.356(5) ? C13 C16 . 1.498(5) ? C14 C15 . 1.380(5) ? C14 H14 . .930 ? C15 C17 . 1.501(5) ? C16 H16A . .960 ? C16 H16B . .960 ? C16 H16C . .960 ? C17 H17A . .960 ? C17 H17B . .960 ? C17 H17C . .960 ? P2 N1 . 1.567(3) yes P2 N2 . 1.612(3) yes P2 N6 . 1.674(3) ? N6 C20 . 1.373(5) ? N6 N7 . 1.400(4) ? N7 C18 . 1.310(5) ? C18 C19 . 1.392(6) ? C18 C21 . 1.500(6) ? C19 C20 . 1.363(5) ? C19 H19 . .930 ? C20 C22 . 1.485(5) ? C21 H21A . .960 ? C21 H21B . .960 ? C21 H21C . .960 ? C22 H22A . .960 ? C22 H22B . .960 ? C22 H22C . .960 ? N1 P1 . 1.624(3) yes P1 N3 . 1.618(3) yes P1 C1 . 1.806(4) ? P1 C7 . 1.812(4) ? N3 P3 . 1.557(3) yes P3 N2 . 1.622(3) yes P3 N8 . 1.683(3) ? P3 N10 . 1.693(3) ? N8 C25 . 1.370(5) ? N8 N9 . 1.394(4) ? N9 C23 . 1.308(5) ? C23 C24 . 1.395(6) ? C23 C26 . 1.512(6) ? C24 C25 . 1.353(5) ? C24 H24 . .930 ? C25 C27 . 1.487(6) ? C26 H26A . .960 ? C26 H26B . .960 ? C26 H26C . .960 ? C27 H27A . .960 ? C27 H27B . .960 ? C27 H27C . .960 ? N10 C30 . 1.374(4) ? N10 N11 . 1.400(4) ? N11 C28 . 1.315(5) ? C28 C29 . 1.394(5) ? C28 C31 . 1.488(5) ? C29 C30 . 1.350(5) ? C29 H29 . .930 ? C30 C32 . 1.498(5) ? C31 H31A . .960 ? C31 H31B . .960 ? C31 H31C . .960 ? C32 H32A . .960 ? C32 H32B . .960 ? C32 H32C . .960 ? C1 C6 . 1.375(5) ? C1 C2 . 1.393(5) ? C2 C3 . 1.357(6) ? C2 H2 . .930 ? C3 C4 . 1.349(6) ? C3 H3 . .930 ? C4 C5 . 1.368(6) ? C4 H4 . .930 ? C5 C6 . 1.370(6) ? C5 H5 . .930 ? C6 H6 . .930 ? C7 C12 . 1.376(5) ? C7 C8 . 1.390(5) ? C8 C9 . 1.396(5) ? C8 H8 . .930 ? C9 C10 . 1.353(6) ? C9 H9 . .930 ? C10 C11 . 1.372(6) ? C10 H10 . .930 ? C11 C12 . 1.386(5) ? C11 H11 . .930 ? C12 H12 . .930 ?