#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007073.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_2007073 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1998 _journal_volume 54 _journal_page_first 331 _journal_page_last 333 _publ_section_title ; A Novel Cyclotriphosphazene Complex with a Short Transannular P...P Contact ; _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 'K. R. Justin Thomas' _chemical_name_common ; 2,2-di-t-butylamino-4,4,6,6-tetrakis(3,5-dimethylpyrazol-1-yl)- cycltriphosphazene cobalt(II)chloride ; _chemical_formula_sum 'C28 H48 Cl2 Co N13 P3' _chemical_formula_structural ; Co Cl~2~ N~3~P~3~(C~5~N~2~H~7~)~4~(C~4~H~10~)~2~ ; _chemical_formula_iupac '[Co Cl2 (C28 H48 N13 P3)]' _chemical_formula_weight 789.53 _symmetry_cell_setting Monoclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.503(5) _cell_length_b 17.843(5) _cell_length_c 19.132(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.51(3) _cell_angle_gamma 90.00 _cell_volume 3765(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.393 _diffrn_ambient_temperature 293(2) _refine_ls_R_factor_obs .0327 _refine_ls_wR_factor_obs .0770 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 _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Co .55847(3) .24331(2) .15788(2) .03365(10) Uani d . 1 . Co Cl1 .74390(7) .25704(5) .13860(5) .0672(2) Uani d . 1 . Cl Cl2 .55497(7) .20713(4) .27207(4) .0546(2) Uani d . 1 . Cl P1 .31744(5) .33633(3) .08323(3) .02579(13) Uani d . 1 . P P2 .31038(5) .19385(3) .03479(3) .02695(14) Uani d . 1 . P P3 .11508(5) .25225(3) .07882(3) .02656(13) Uani d . 1 . P N1 .2077(2) .32099(10) .11287(10) .0278(4) Uani d . 1 . N N2 .3940(2) .26541(10) .06815(10) .0277(4) Uani d . 1 . N N3 .1836(2) .18722(10) .04704(10) .0302(4) Uani d . 1 . N N4 .4234(2) .38947(11) .14126(10) .0317(4) Uani d . 1 . N N5 .5331(2) .35761(12) .17839(11) .0391(5) Uani d . 1 . N N6 .2764(2) .39089(11) .00747(10) .0304(4) Uani d . 1 . N N7 .1606(2) .42195(11) -.01282(11) .0351(5) Uani d . 1 . N N8 .4029(2) .12083(11) .07107(11) .0336(4) Uani d . 1 . N N9 .5180(2) .13432(12) .11607(11) .0378(5) Uani d . 1 . N N10 .2971(2) .18335(11) -.05511(10) .0314(4) Uani d . 1 . N N11 .1842(2) .16411(12) -.10143(11) .0385(5) Uani d . 1 . N N12 .0042(2) .29460(12) .02083(11) .0348(5) Uani d . 1 . N N13 .0563(2) .21346(12) .13732(11) .0335(5) Uani d . 1 . N C1 .5936(2) .4102(2) .22209(14) .0450(6) Uani d . 1 . C C2 .5249(3) .4762(2) .21472(15) .0440(6) Uani d . 1 . C C3 .4180(2) .46261(13) .16369(13) .0364(5) Uani d . 1 . C C4 .7181(3) .3955(2) .2721(2) .0821(12) Uani d . 1 . C H4A .7419(3) .3451(2) .2650(2) .16(2) Uiso calc R 1 . H H4B .7172(3) .4018(2) .3218(2) .21(3) Uiso calc R 1 . H H4C .7747(3) .4300(2) .2615(2) .19(3) Uiso calc R 1 . H C5 .3118(3) .5117(2) .1333(2) .0562(8) Uani d . 1 . C C6 .1594(2) .46865(14) -.06649(14) .0413(6) Uani d . 1 . C C7 .2717(3) .4688(2) -.0813(2) .0500(7) Uani d . 1 . C C8 .3452(2) .42014(15) -.03473(15) .0420(6) Uani d . 1 . C C9 .0482(3) .5121(2) -.1025(2) .0626(9) Uani d . 1 . C H9A -.0145(3) .5000(2) -.0803(2) .16(2) Uiso calc R 1 . H H9B .0215(3) .4996(2) -.1534(2) .102(14) Uiso calc R 1 . H H9C .0657(3) .5647(2) -.0971(2) .105(15) Uiso calc R 1 . H C10 .4743(3) .3986(2) -.0265(2) .0690(10) Uani d . 1 . C H10A .5000(3) .3624(2) .0119(2) .145(19) Uiso calc R 1 . H H10B .5249(3) .4423(2) -.0148(2) .23(3) Uiso calc R 1 . H H10C .4807(3) .3774(2) -.0714(2) .21(3) Uiso calc R 1 . H C11 .5698(3) .0677(2) .13119(15) .0456(7) Uani d . 1 . C C12 .4895(3) .0117(2) .0969(2) .0545(8) Uani d . 1 . C C13 .3846(3) .04526(14) .0589(2) .0442(6) Uani d . 1 . C C14 .6967(4) .0611(2) .1788(2) .0676(10) Uani d . 1 . C C15 .2692(4) .0135(2) .0119(2) .0644(10) Uani d . 1 . C C16 .2041(3) .15156(14) -.16495(13) .0406(6) Uani d . 1 . C C17 .3268(3) .1623(2) -.16126(14) .0424(6) Uani d . 1 . C C18 .3853(2) .18116(13) -.09137(13) .0344(5) Uani d . 1 . C C19 .1022(4) .1272(2) -.2286(2) .0606(9) Uani d . 1 . C C20 .5161(3) .1943(2) -.0559(2) .0495(7) Uani d . 1 . C C21 -.1018(2) .26819(15) -.03843(13) .0377(6) Uani d . 1 . C C22 -.1321(3) .1873(2) -.0263(2) .0584(8) Uani d . 1 . C C23 -.0728(3) .2774(3) -.1107(2) .0628(9) Uani d . 1 . C C24 -.2074(3) .3185(2) -.0366(2) .0542(8) Uani d . 1 . C C25 .0974(2) .14901(15) .18744(14) .0418(6) Uani d . 1 . C C26 .0421(4) .1600(2) .2502(2) .0621(9) Uani d . 1 . C C27 .2342(3) .1484(3) .2180(2) .0683(11) Uani d . 1 . C C28 .0503(5) .0769(2) .1469(3) .0738(11) Uani d . 1 . C H2 .547(3) .5219(18) .2381(15) .054(8) Uiso d . 1 . H H5A .328(3) .5594(19) .1555(17) .059(9) Uiso d . 1 . H H5B .247(3) .4929(19) .1426(17) .059(10) Uiso d . 1 . H H5C .290(4) .518(3) .071(3) .119(15) Uiso d . 1 . H H7 .297(3) .497(2) -.1111(18) .072(11) Uiso d . 1 . H H12N .030(2) .3368(16) .0116(14) .040(8) Uiso d . 1 . H H12 .505(3) -.037(2) .0999(18) .075(11) Uiso d . 1 . H H13N -.012(3) .2287(18) .1336(17) .056(9) Uiso d . 1 . H H14A .710(4) .093(3) .220(3) .121(17) Uiso d . 1 . H H14B .707(4) .017(3) .200(3) .115(17) Uiso d . 1 . H H14C .752(4) .068(3) .154(3) .121(19) Uiso d . 1 . H H15A .274(4) -.037(3) .008(2) .107(15) Uiso d . 1 . H H15B .245(5) .039(3) -.038(3) .15(2) Uiso d . 1 . H H15C .199(5) .031(3) .018(3) .14(2) Uiso d . 1 . H H17 .364(3) .1588(18) -.1994(17) .062(9) Uiso d . 1 . H H19A .108(4) .140(3) -.275(3) .127(18) Uiso d . 1 . H H19B .100(4) .079(3) -.227(3) .125(19) Uiso d . 1 . H H19C .030(4) .149(3) -.230(2) .104(16) Uiso d . 1 . H H20A .537(3) .232(2) -.024(2) .081(12) Uiso d . 1 . H H20B .559(4) .150(2) -.026(2) .091(13) Uiso d . 1 . H H20C .559(4) .198(2) -.089(2) .097(14) Uiso d . 1 . H H22A -.196(3) .1716(17) -.0693(17) .058(9) Uiso d . 1 . H H22B -.069(3) .1581(18) -.0308(16) .052(9) Uiso d . 1 . H H22C -.152(3) .181(2) .023(2) .079(11) Uiso d . 1 . H H23A -.142(3) .265(2) -.149(2) .080(12) Uiso d . 1 . H H23B -.003(4) .241(2) -.111(2) .091(13) Uiso d . 1 . H H23C -.049(3) .333(2) -.115(2) .085(12) Uiso d . 1 . H H24A -.223(3) .3136(19) .0103(19) .067(10) Uiso d . 1 . H H24B -.274(4) .306(2) -.078(2) .083(11) Uiso d . 1 . H H24C -.179(3) .372(2) -.0399(18) .075(11) Uiso d . 1 . H H26A .066(3) .116(2) .283(2) .086(12) Uiso d . 1 . H H26B .078(4) .203(3) .279(2) .110(17) Uiso d . 1 . H H26C -.041(3) .1676(19) .2308(18) .067(10) Uiso d . 1 . H H27A .267(4) .202(3) .241(3) .130(19) Uiso d . 1 . H H27B .269(3) .128(2) .181(2) .088(13) Uiso d . 1 . H H27C .254(3) .110(2) .256(2) .091(12) Uiso d . 1 . H H28A .080(4) .072(2) .104(2) .101(14) Uiso d . 1 . H H28B .075(3) .038(2) .180(2) .077(11) Uiso d . 1 . H H28C -.040(4) .078(3) .125(3) .114(17) Uiso d . 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 .0309(2) .0352(2) .0332(2) .00537(14) .00647(13) .00245(14) Cl1 .0443(4) .0912(6) .0730(5) .0024(4) .0278(4) .0092(5) Cl2 .0671(5) .0605(5) .0372(3) .0052(4) .0166(3) .0053(3) P1 .0274(3) .0218(3) .0275(3) .0004(2) .0067(2) -.0001(2) P2 .0301(3) .0232(3) .0293(3) .0011(2) .0111(2) -.0012(2) P3 .0284(3) .0258(3) .0270(3) -.0001(2) .0104(2) .0009(2) N1 .0305(10) .0244(10) .0301(10) .0016(8) .0110(8) -.0022(8) N2 .0275(9) .0235(9) .0324(10) .0017(8) .0089(8) -.0004(8) N3 .0332(10) .0264(10) .0346(10) -.0023(8) .0154(8) -.0052(8) N4 .0299(10) .0268(10) .0347(11) -.0004(8) .0030(8) -.0028(8) N5 .0352(11) .0355(11) .0387(11) .0002(9) -.0020(9) .0012(9) N6 .0312(10) .0284(10) .0314(10) .0019(8) .0087(8) .0048(8) N7 .0338(11) .0326(11) .0359(11) .0046(9) .0048(9) .0046(9) N8 .0399(11) .0242(10) .0373(11) .0057(8) .0120(9) .0001(8) N9 .0400(12) .0366(12) .0361(11) .0111(9) .0098(9) .0025(9) N10 .0324(10) .0329(11) .0300(10) -.0013(8) .0105(8) -.0038(8) N11 .0378(11) .0418(12) .0344(11) -.0024(9) .0080(9) -.0035(9) N12 .0329(11) .0298(11) .0390(11) -.0026(9) .0058(9) .0043(9) N13 .0335(11) .0348(11) .0367(11) .0035(9) .0175(9) .0066(9) C1 .0418(15) .0413(15) .0434(15) -.0060(12) -.0018(12) -.0021(12) C2 .050(2) .0344(15) .0426(15) -.0097(12) .0047(12) -.0077(12) C3 .0415(14) .0280(12) .0384(13) -.0035(10) .0093(11) -.0044(10) C4 .061(2) .066(2) .088(3) .000(2) -.031(2) -.012(2) C5 .054(2) .034(2) .071(2) .0074(14) .003(2) -.016(2) C6 .051(2) .0336(13) .0344(13) .0043(12) .0035(11) .0051(11) C7 .064(2) .044(2) .047(2) .0033(14) .0231(14) .0156(13) C8 .0459(15) .0375(14) .0479(15) -.0007(12) .0216(12) .0076(12) C9 .066(2) .058(2) .054(2) .019(2) .000(2) .016(2) C10 .057(2) .063(2) .102(3) .013(2) .047(2) .033(2) C11 .055(2) .0381(15) .0431(15) .0191(13) .0134(13) .0039(12) C12 .073(2) .0308(15) .059(2) .0158(14) .017(2) .0014(13) C13 .057(2) .0269(13) .052(2) .0036(12) .0209(13) -.0045(11) C14 .063(2) .061(2) .068(2) .030(2) .002(2) .005(2) C15 .068(2) .029(2) .090(3) -.0019(15) .011(2) -.010(2) C16 .055(2) .0360(14) .0305(13) .0025(12) .0112(11) -.0015(11) C17 .057(2) .0398(15) .0362(14) .0024(12) .0230(12) -.0029(11) C18 .0416(13) .0292(12) .0380(13) .0023(10) .0202(11) -.0007(10) C19 .071(2) .065(2) .036(2) -.003(2) .000(2) -.007(2) C20 .043(2) .058(2) .055(2) -.0071(14) .0255(14) -.014(2) C21 .0311(12) .0440(14) .0355(13) -.0032(11) .0055(10) .0033(11) C22 .055(2) .043(2) .066(2) -.012(2) -.001(2) -.002(2) C23 .057(2) .093(3) .038(2) -.013(2) .0125(15) -.004(2) C24 .038(2) .061(2) .058(2) .0070(14) .0053(14) .005(2) C25 .050(2) .0386(14) .0420(14) .0043(12) .0208(12) .0133(11) C26 .074(2) .070(2) .054(2) .010(2) .037(2) .025(2) C27 .054(2) .091(3) .061(2) .021(2) .019(2) .038(2) C28 .104(3) .038(2) .086(3) -.004(2) .039(3) .011(2) 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 N9 . 2.104(2) yes Co N5 . 2.113(2) yes Co N2 . 2.199(2) yes Co Cl1 . 2.2788(12) yes Co Cl2 . 2.2893(12) yes P1 N1 . 1.548(2) yes P1 N2 . 1.614(2) yes P1 N4 . 1.688(2) yes P1 N6 . 1.698(2) yes P1 P2 . 2.6992(10) yes P2 N3 . 1.546(2) yes P2 N2 . 1.617(2) yes P2 N10 . 1.693(2) yes P2 N8 . 1.701(2) yes P3 N3 . 1.615(2) yes P3 N13 . 1.618(2) yes P3 N12 . 1.620(2) yes P3 N1 . 1.634(2) yes N4 C3 . 1.381(3) ? N4 N5 . 1.382(3) ? N5 C1 . 1.317(3) ? N6 C8 . 1.383(3) ? N6 N7 . 1.392(3) ? N7 C6 . 1.319(3) ? N8 C13 . 1.374(3) ? N8 N9 . 1.380(3) ? N9 C11 . 1.324(3) ? N10 C18 . 1.383(3) ? N10 N11 . 1.392(3) ? N11 C16 . 1.318(3) ? N12 C21 . 1.486(3) ? N13 C25 . 1.486(3) ? C1 C2 . 1.403(4) ? C1 C4 . 1.502(4) ? C2 C3 . 1.357(4) ? C3 C5 . 1.482(4) ? C6 C7 . 1.399(4) ? C6 C9 . 1.488(4) ? C7 C8 . 1.354(4) ? C8 C10 . 1.498(4) ? C11 C12 . 1.392(4) ? C11 C14 . 1.489(5) ? C12 C13 . 1.357(4) ? C13 C15 . 1.487(5) ? C16 C17 . 1.407(4) ? C16 C19 . 1.495(4) ? C17 C18 . 1.357(4) ? C18 C20 . 1.483(4) ? C21 C22 . 1.517(4) ? C21 C24 . 1.518(4) ? C21 C23 . 1.521(4) ? C25 C27 . 1.515(4) ? C25 C28 . 1.521(5) ? C25 C26 . 1.523(4) ? _cod_database_code 2007073