#------------------------------------------------------------------------------
#$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $
#$Revision: 966 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006297.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_2006297
_journal_name_full 'Acta Crystallographica Section C'
_journal_year  1997
_journal_volume 53
_journal_page_first  843
_journal_page_last  845
_publ_section_title
;
cyclo-Tetrakis(\m-oxo)tetrakis[iodo(\h^5^-methylcyclopentadienyl)titanium(IV)]
;
loop_
_publ_author_name
 'Kienitz, Carsten O.'
 'Th\"one, Carsten'
 'Jones, Peter G.'
_chemical_formula_sum  'C24 H28 I4 O4 Ti4'
_chemical_formula_weight  1079.66
_symmetry_cell_setting  orthorhombic
_symmetry_space_group_name_H-M  'P n a 21'
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'
_cell_length_a  19.239(3)
_cell_length_b  10.500(2)
_cell_length_c  15.696(2)
_cell_angle_alpha  90.00
_cell_angle_beta  90.00
_cell_angle_gamma  90.00
_cell_volume  3170.7(9)
_cell_formula_units_Z  4
_cell_measurement_temperature  143(2)
_exptl_crystal_density_diffrn  2.262
_diffrn_ambient_temperature  143(2)
_refine_ls_R_factor_obs   .0766
_refine_ls_wR_factor_obs   .1578
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
 I1  .51614(8)  .36267(15)  .28872(9)  .0345(4) Uani d . 1 . I
 Ti1  .45035(19)  .4521(4)  .4263(2)  .0180(8) Uani d U 1 . Ti
 C11  .4386(8)  .3040(15)  .5421(11)  .028(3) Uani d DU 1 . C
 C12  .5030(8)  .2810(15)  .5033(10)  .024(3) Uani d DU 1 . C
 H12  .5164  .2044  .4756  .029 Uiso calc R 1 . H
 C13  .5449(8)  .3921(16)  .5125(10)  .024(3) Uani d DU 1 . C
 H13  .5911  .4022  .4923  .029 Uiso calc R 1 . H
 C14  .5063(9)  .4832(16)  .5562(12)  .031(3) Uani d DU 1 . C
 H14  .5215  .5658  .5723  .037 Uiso calc R 1 . H
 C15  .4404(9)  .4295(15)  .5719(12)  .030(3) Uani d DU 1 . C
 H15  .4028  .4722  .5987  .036 Uiso calc R 1 . H
 C16  .3792(10)  .213(2)  .5498(16)  .045(6) Uani d DU 1 . C
 H16A  .3367  .2593  .5644  .054 Uiso calc R 1 . H
 H16B  .3893  .1502  .5946  .054 Uiso calc R 1 . H
 H16C  .3725  .1682  .4955  .054 Uiso calc R 1 . H
 O1  .3597(7)  .4191(12)  .4057(10)  .025(3) Uani d U 1 . O
 Ti2  .27221(19)  .4533(4)  .3679(2)  .0185(8) Uani d U 1 . Ti
 C21  .2849(8)  .4677(15)  .2214(11)  .031(3) Uani d DU 1 . C
 C22  .3040(8)  .3434(15)  .2456(11)  .030(3) Uani d DU 1 . C
 H22  .3492  .3075  .2414  .036 Uiso calc R 1 . H
 C23  .2439(9)  .2811(15)  .2772(12)  .031(3) Uani d DU 1 . C
 H23  .2417  .1968  .2991  .037 Uiso calc R 1 . H
 C24  .1886(8)  .3667(16)  .2703(13)  .030(3) Uani d DU 1 . C
 H24  .1419  .3499  .2861  .035 Uiso calc R 1 . H
 C25  .2135(8)  .4824(15)  .2359(12)  .026(3) Uani d DU 1 . C
 H25  .1867  .5566  .2246  .031 Uiso calc R 1 . H
 C26  .3325(12)  .568(2)  .1862(16)  .050(6) Uani d DU 1 . C
 H26A  .3329  .5623  .1238  .060 Uiso calc R 1 . H
 H26B  .3796  .5541  .2081  .060 Uiso calc R 1 . H
 H26C  .3160  .6521  .2036  .060 Uiso calc R 1 . H
 I2  .19076(7)  .36948(15)  .49362(10)  .0332(4) Uani d . 1 . I
 I3  .21575(8)  .88955(15)  .25804(10)  .0366(4) Uani d . 1 . I
 Ti3  .27159(18)  .7932(4)  .3988(2)  .0182(8) Uani d U 1 . Ti
 C31  .2639(8)  .7761(15)  .5459(11)  .032(3) Uani d DU 1 . C
 C32  .1964(8)  .7605(16)  .5139(11)  .031(3) Uani d DU 1 . C
 H32  .1694  .6850  .5178  .037 Uiso calc R 1 . H
 C33  .1747(9)  .8754(18)  .4748(12)  .036(4) Uani d DU 1 . C
 H33  .1309  .8908  .4488  .043 Uiso calc R 1 . H
 C34  .2298(10)  .9621(16)  .4815(13)  .035(3) Uani d DU 1 . C
 H34  .2310 1.0456  .4583  .042 Uiso calc R 1 . H
 C35  .2835(9)  .9027(15)  .5292(13)  .032(3) Uani d DU 1 . C
 H35  .3257  .9418  .5469  .038 Uiso calc R 1 . H
 C36  .3070(12)  .675(2)  .5881(14)  .041(5) Uani d DU 1 . C
 H36A  .3089  .5998  .5515  .050 Uiso calc R 1 . H
 H36B  .2862  .6527  .6430  .050 Uiso calc R 1 . H
 H36C  .3542  .7078  .5973  .050 Uiso calc R 1 . H
 O3  .3634(7)  .8252(12)  .3864(9)  .021(2) Uani d U 1 . O
 Ti4  .45495(18)  .7894(4)  .3871(2)  .0190(8) Uani d U 1 . Ti
 C41  .4638(8)  .9397(14)  .2727(11)  .029(3) Uani d DU 1 . C
 C42  .5211(8)  .9560(16)  .3270(11)  .030(3) Uani d DU 1 . C
 H42  .5306 1.0301  .3597  .036 Uiso calc R 1 . H
 C43  .5623(9)  .8447(17)  .3255(12)  .031(3) Uani d DU 1 . C
 H43  .6039  .8306  .3566  .037 Uiso calc R 1 . H
 C44  .5304(9)  .7598(16)  .2699(13)  .033(3) Uani d DU 1 . C
 H44  .5473  .6778  .2549  .040 Uiso calc R 1 . H
 C45  .4685(9)  .8164(15)  .2394(12)  .029(3) Uani d DU 1 . C
 H45  .4356  .7773  .2026  .035 Uiso calc R 1 . H
 C46  .4092(11) 1.040(2)  .2575(18)  .051(6) Uani d DU 1 . C
 H46A  .3718 1.0035  .2225  .061 Uiso calc R 1 . H
 H46B  .4299 1.1122  .2278  .061 Uiso calc R 1 . H
 H46C  .3901 1.0677  .3122  .061 Uiso calc R 1 . H
 I4  .49438(8)  .87831(15)  .53893(10)  .0348(4) Uani d . 1 . I
 O2  .2624(6)  .6251(14)  .3811(9)  .018(2) Uani d U 1 . O
 O4  .4599(7)  .6169(14)  .4082(9)  .022(3) Uani d U 1 . O
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
 I1  .0399(9)  .0331(9)  .0305(8)  .0100(7)  .0094(7)  -.0011(7)
 Ti1  .0186(18)  .0172(19)  .0181(17)  .0005(15)  -.0034(15)  -.0017(15)
 C11  .027(6)  .029(6)  .030(7)  .001(5)  -.004(5)  .007(5)
 C12  .025(6)  .030(5)  .018(7)  .003(5)  -.010(5)  .003(5)
 C13  .026(5)  .029(6)  .018(7)  .002(5)  -.004(4)  .012(6)
 C14  .038(7)  .031(6)  .025(6)  .001(5)  -.012(5)  -.002(5)
 C15  .035(6)  .031(6)  .023(4)  .012(5)  .000(5)  .009(5)
 C16  .039(9)  .046(10)  .051(12)  -.007(8)  .014(10)  .020(9)
 O1  .017(4)  .026(6)  .031(6)  .006(4)  -.003(4)  -.007(5)
 Ti2  .0203(18)  .0160(18)  .0193(18)  .0020(15)  -.0005(15)  -.0031(15)
 C21  .033(6)  .037(6)  .024(4)  -.002(5)  .005(6)  .002(5)
 C22  .033(6)  .032(6)  .026(6)  .006(5)  .003(6)  -.008(5)
 C23  .037(7)  .025(5)  .030(8)  -.004(5)  -.009(6)  -.005(5)
 C24  .026(5)  .031(6)  .032(8)  -.006(5)  -.007(5)  -.003(6)
 C25  .028(5)  .028(6)  .021(6)  .001(5)  -.002(5)  .000(5)
 C26  .050(11)  .058(11)  .043(10)  -.027(10)  .008(10)  .007(10)
 I2  .0299(8)  .0325(8)  .0371(8)  -.0064(7)  .0086(7)  .0049(8)
 I3  .0352(9)  .0342(8)  .0403(9)  -.0006(7)  -.0124(7)  .0137(8)
 Ti3  .0120(16)  .0193(19)  .0234(18)  .0007(15)  .0016(14)  -.0025(16)
 C31  .036(6)  .034(6)  .025(4)  -.006(6)  -.001(5)  -.001(5)
 C32  .028(6)  .034(6)  .031(7)  -.006(5)  .011(4)  -.008(5)
 C33  .027(5)  .039(7)  .041(8)  .008(5)  .007(5)  -.012(6)
 C34  .041(7)  .028(5)  .036(8)  .004(5)  .010(6)  -.009(5)
 C35  .036(6)  .026(6)  .033(6)  -.006(5)  .001(5)  -.012(5)
 C36  .051(11)  .040(10)  .034(9)  .010(9)  .004(9)  .001(9)
 O3  .018(4)  .025(5)  .021(5)  -.008(4)  -.003(4)  -.003(5)
 Ti4  .0212(18)  .0146(18)  .0211(18)  -.0010(15)  .0020(15)  -.0005(16)
 C41  .029(6)  .027(5)  .030(7)  -.002(5)  .004(5)  .009(5)
 C42  .028(6)  .028(5)  .034(7)  -.008(5)  .006(5)  .004(5)
 C43  .027(5)  .036(7)  .029(7)  -.001(5)  .006(5)  .016(6)
 C44  .033(6)  .029(6)  .038(7)  .002(5)  .015(5)  .005(5)
 C45  .033(6)  .031(6)  .023(5)  -.009(6)  .007(5)  .007(5)
 C46  .038(10)  .045(10)  .071(14)  .007(8)  .011(10)  .030(9)
 I4  .0363(8)  .0354(9)  .0327(8)  -.0023(7)  -.0087(7)  -.0069(8)
 O2  .012(5)  .017(4)  .023(5)  .001(4)  -.004(4)  .002(4)
 O4  .026(6)  .019(4)  .022(5)  .000(4)  .001(5)  .001(4)
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
 I1 Ti1 . 2.673(4) y
 Ti1 O4 . 1.763(15) y
 Ti1 O1 . 1.807(15) y
 O1 Ti2 . 1.820(14) y
 Ti2 O2 . 1.826(15) y
 Ti2 I2 . 2.669(4) y
 I3 Ti3 . 2.657(4) y
 Ti3 O2 . 1.795(15) y
 Ti3 O3 . 1.808(13) y
 O3 Ti4 . 1.801(14) y
 Ti4 O4 . 1.845(15) y
 Ti4 I4 . 2.670(4) y
 X1A Ti1 . 2.031 y
 X1B Ti2 . 2.031 y
 X1C Ti3 . 2.018 y
 X1D Ti4 . 2.041 y
 Ti1 C15 . 2.306(19) ?
 Ti1 C14 . 2.329(19) ?
 Ti1 C13 . 2.353(16) ?
 Ti1 C12 . 2.391(16) ?
 Ti1 C11 . 2.402(17) ?
 C11 C15 . 1.399(15) ?
 C11 C12 . 1.401(15) ?
 C11 C16 . 1.499(18) ?
 C12 C13 . 1.425(15) ?
 C13 C14 . 1.391(18) ?
 C14 C15 . 1.409(16) ?
 Ti2 C21 . 2.318(17) ?
 Ti2 C22 . 2.323(17) ?
 Ti2 C23 . 2.365(17) ?
 Ti2 C25 . 2.380(18) ?
 Ti2 C24 . 2.400(19) ?
 C21 C25 . 1.401(15) ?
 C21 C22 . 1.408(15) ?
 C21 C26 . 1.499(18) ?
 C22 C23 . 1.418(15) ?
 C23 C24 . 1.397(18) ?
 C24 C25 . 1.412(15) ?
 Ti3 C31 . 2.321(18) ?
 Ti3 C32 . 2.340(18) ?
 Ti3 C34 . 2.34(2)   ?
 Ti3 C35 . 2.36(2)   ?
 Ti3 C33 . 2.375(18) ?
 C31 C32 . 1.402(15) ?
 C31 C35 . 1.406(15) ?
 C31 C36 . 1.498(18) ?
 C32 C33 . 1.415(16) ?
 C33 C34 . 1.401(19) ?
 C34 C35 . 1.421(16) ?
 Ti4 C45 . 2.349(19) ?
 Ti4 C43 . 2.353(18) ?
 Ti4 C42 . 2.358(17) ?
 Ti4 C44 . 2.36(2)   ?
 Ti4 C41 . 2.397(17) ?
 C41 C45 . 1.399(15) ?
 C41 C42 . 1.403(15) ?
 C41 C46 . 1.503(18) ?
 C42 C43 . 1.412(15) ?
 C43 C44 . 1.391(19) ?
 C44 C45 . 1.415(15) ?
_cod_database_code 2006297