#------------------------------------------------------------------------------
#$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $
#$Revision: 91933 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/36/2003609.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003609
loop_
_publ_author_name
'Tian, J.'
'Hu, N.-H.'
'Shen, Q.'
'Huang, B.-T.'
_publ_section_title
Dichloro(\h^5^-cyclopentadienyl){[1-(4-methoxyphenyl)cyclohexyl]-\h^5^-cyclopentadienyl}titanium(IV)
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1065
_journal_page_last               1067
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        'synthesized in our own laboratory'
_chemical_formula_sum            'C23 H26 Cl2 O Ti'
_chemical_formula_weight         437.24
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.680(5)
_cell_length_b                   12.846(5)
_cell_length_c                   16.944(6)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293
_cell_measurement_theta_max      11.7
_cell_measurement_theta_min      3.2
_cell_volume                     2107.0(16)
_diffrn_measurement_device       'Nicolet R3m/E'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1927
_diffrn_reflns_theta_max         24
_diffrn_standards_decay_%        <1.3
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.68
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       'flat slice'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.09
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     244
_refine_ls_number_reflns         1406
_refine_ls_R_factor_obs          0.066
_refine_ls_shift/esd_max         0.03
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      1/[\s^2^(F~o~)+0.0036(F~o~)^2^]
_refine_ls_wR_factor_obs         0.086
_reflns_number_observed          1406
_reflns_number_total             1904
_reflns_observed_criterion       F~o~>3\s(F~o~)
_[local]_cod_data_source_file    ta1007.cif
_[local]_cod_data_source_block   ta1007a
_cod_original_cell_volume        2107.0(10)
_cod_database_code               2003609
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,-y,1/2+z
-x,1/2+y,1/2-z
1/2+x,1/2-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Ti .5550(2) -.0025(1) .2278(1) .051(1)
Cl(1) .3512(3) .0984(2) .1966(2) .054(1)
Cl(2) .7080(3) .1430(2) .2094(1) .048(1)
C(1) .868(1) -.1178(7) .1421(5) .050(3)
C(2) .944(1) -.0301(8) .0906(6) .062(4)
C(3) 1.098(1) -.049(1) .0811(6) .073(5)
C(4) 1.123(1) -.163(1) .0457(7) .094(6)
C(5) 1.050(1) -.2477(9) .0886(7) .069(4)
C(6) .898(1) -.2259(8) .0975(6) .065(4)
C(11) .714(1) -.1029(7) .1419(5) .051(3)
C(12) .632(1) -.0354(8) .0911(6) .061(4)
C(13) .493(1) -.0608(8) .0983(7) .053(4)
C(14) .481(1) -.1454(9) .1537(8) .068(4)
C(15) .622(1) -.1700(7) .1797(7) .060(4)
C(21) .925(1) -.1216(7) .2274(6) .047(3)
C(22) .978(1) -.0351(8) .2636(6) .058(4)
C(23) 1.026(1) -.0364(8) .3422(7) .065(4)
C(24) 1.030(1) -.1303(9) .3831(6) .072(5)
C(25) .982(1) -.2207(8) .3459(7) .063(4)
C(26) .932(1) -.2129(7) .2700(6) .057(4)
C(27) 1.095(3) -.223(1) .496(1) .16(1)
O(1) 1.083(1) -.1257(6) .4565(4) .097(4)
C(31) .638(1) -.0793(9) .3451(6) .073(4)
C(32) .636(2) .0203(9) .3598(8) .097(6)
C(33) .504(1) -.1146(9) .3379(8) .091(6)
C(34) .422(1) -.026(1) .346(1) .095(6)
C(35) .506(2) .0543(9) .3573(8) .107(8)
H(2a) .8967 -.0284 .0401 .060
H(2b) .9275 .0345 .1174 .060
H(3a) 1.1335 .0010 .0449 .060
H(3b) 1.1419 -.0459 .1302 .060
H(4a) 1.2215 -.1738 .0454 .060
H(4b) 1.0918 -.1613 -.0092 .060
H(5a) 1.0658 -.3101 .0618 .060
H(5b) 1.0914 -.2500 .1410 .060
H(6a) .8571 -.2238 .0450 .060
H(6b) .8565 -.2809 .1268 .060
H(12) .5730 .0192 .0571 .060
H(13) .4148 -.0296 .0715 .060
H(14) .3958 -.1816 .1703 .060
H(15) .6448 -.2225 .2191 .060
H(22) .9786 .0302 .2355 .060
H(23) 1.0696 .0252 .3660 .060
H(25) .9776 -.2841 .3734 .060
H(26) .8992 -.2756 .2448 .060
H(27a) 1.1344 -.2165 .5482 .060
H(27b) 1.1573 -.2699 .4660 .060
H(27c) 1.0075 -.2579 .5000 .060
H(31) .7198 -.1260 .3393 .060
H(32) .7204 .0667 .3700 .060
H(33) .4677 -.1868 .3243 .060
H(34) .3188 -.0173 .3411 .060
H(35) .4770 .1292 .3641 .060
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl(1) Ti Cl(2) 93.30(10) yes
Cl(2) Ti C(11) 86.9(2) yes
Cl(2) Ti C(13) 106.2(3) yes
Cl(2) Ti C(31) 102.9(3) yes
Cl(2) Ti C(34) 122.4(4) yes
C(13) Ti C(15) 58.3(4) yes
C(32) Ti C(35) 32.8(6) yes
C(11) Ti C(33) 105.8(4) yes
C(35) Ti C(14) 132.9(5) yes
C(1) C(11) C(12) 127.9(9) yes
C(2) C(1) C(11) 111.2(8) yes
C(1) C(21) C(22) 121.7(8) yes
C(12) C(11) C(15) 107.1(9) yes
C(32) C(31) C(33) 109.2(12) yes
C(2) C(1) C(6) 105.6(8) yes
C(21) C(22) C(23) 122.4(9) yes
Cl(1) Ti C(11) 131.1(2) yes
Cl(1) Ti C(13) 76.3(3) yes
Cl(1) Ti C(31) 133.3(3) yes
Cl(1) Ti C(34) 79.0(4) yes
C(11) Ti C(14) 57.6(4) yes
C(31) Ti C(34) 55.2(5) yes
C(11) Ti C(31) 93.7(4) yes
C(35) Ti C(11) 146.3(5) yes
Ti C(11) C(1) 132.9(7) yes
C(11) C(1) C(21) 111.1(8) yes
C(6) C(1) C(11) 106.7(8) yes
C(24) O(1) C(27) 115.6(11) yes
C(12) C(13) C(14) 107.9(9) yes
C(33) C(34) C(35) 107.4(13) yes
C(3) C(4) C(5) 114.5(10) yes
C(24) C(25) C(26) 118.5(9) yes
Cl(2) Ti C(12) 79.9(3) no
C(11) Ti C(13) 57.0(3) no
Cl(1) Ti C(14) 93.2(3) no
C(13) Ti C(14) 35.4(4) no
Cl(2) Ti C(15) 119.2(3) no
C(12) Ti C(15) 56.2(4) no
C(14) Ti C(15) 36.1(4) no
C(12) Ti C(31) 127.9(4) no
C(14) Ti C(31) 103.2(4) no
Cl(1) Ti C(32) 114.1(4) no
C(11) Ti C(32) 114.1(4) no
C(13) Ti C(32) 168.1(4) no
C(15) Ti C(32) 109.9(4) no
Cl(1) Ti C(33) 108.7(3) no
C(13) Ti C(33) 118.1(4) no
C(15) Ti C(33) 77.4(4) no
C(32) Ti C(33) 54.3(4) no
C(12) Ti C(34) 157.4(5) no
C(14) Ti C(34) 100.7(5) no
C(33) Ti C(34) 33.8(5) no
Cl(2) Ti C(35) 90.3(4) no
C(12) Ti C(35) 170.2(4) no
C(31) Ti C(35) 54.2(4) no
C(33) Ti C(35) 54.7(4) no
C(6) C(1) C(21) 110.4(8) no
C(1) C(2) C(3) 113.2(9) no
C(1) C(6) C(5) 112.5(9) no
Ti C(11) C(12) 72.6(6) no
Ti C(11) C(15) 69.9(6) no
Ti C(12) C(13) 70.4(6) no
Ti C(13) C(12) 76.3(6) no
Ti C(14) C(15) 74.0(6) no
Ti C(15) C(11) 76.9(6) no
C(11) C(15) C(14) 108.8(9) no
C(1) C(21) C(26) 122.1(8) no
C(23) C(24) C(25) 119.0(10) no
C(25) C(24) O(1) 126.3(10) no
C(21) C(26) C(25) 124.5(9) no
Ti C(31) C(32) 75.4(8) no
Ti C(32) C(35) 72.4(8) no
Ti C(33) C(31) 71.2(7) no
C(31) C(33) C(34) 105.0(11) no
Ti C(34) C(35) 72.4(9) no
Ti C(35) C(32) 74.8(8) no
C(32) C(35) C(34) 109.4(12) no
Cl(1) Ti C(12) 97.8(3) no
C(11) Ti C(12) 34.2(3) no
C(12) Ti C(13) 33.3(4) no
Cl(2) Ti C(14) 136.8(3) no
C(12) Ti C(14) 57.0(4) no
Cl(1) Ti C(15) 129.0(3) no
C(11) Ti C(15) 33.2(4) no
C(13) Ti C(31) 136.6(4) no
C(15) Ti C(31) 79.5(4) no
Cl(2) Ti C(32) 79.8(3) no
C(12) Ti C(32) 142.9(5) no
C(14) Ti C(32) 134.4(4) no
C(31) Ti C(32) 31.8(4) no
Cl(2) Ti C(33) 133.8(3) no
C(12) Ti C(33) 133.4(4) no
C(14) Ti C(33) 83.3(4) no
C(31) Ti C(33) 33.7(4) no
C(11) Ti C(34) 139.3(4) no
C(13) Ti C(34) 126.1(4) no
C(15) Ti C(34) 108.5(5) no
C(32) Ti C(34) 54.1(5) no
Cl(1) Ti C(35) 82.6(4) no
C(13) Ti C(35) 153.8(5) no
C(15) Ti C(35) 130.5(4) no
C(34) Ti C(35) 32.3(5) no
C(2) C(1) C(21) 111.6(8) no
C(2) C(3) C(4) 109.5(10) no
C(4) C(5) C(6) 112.1(10) no
C(1) C(11) C(15) 123.6(9) no
Ti C(12) C(11) 73.3(6) no
C(11) C(12) C(13) 109.5(9) no
Ti C(13) C(14) 70.0(6) no
Ti C(14) C(13) 74.6(6) no
C(13) C(14) C(15) 106.7(9) no
Ti C(15) C(14) 69.9(6) no
C(22) C(21) C(26) 116.1(9) no
C(22) C(23) C(24) 119.3(10) no
C(23) C(24) O(1) 115.7(10) no
Ti C(31) C(33) 75.1(7) no
Ti C(32) C(31) 72.8(7) no
C(31) C(32) C(35) 108.9(13) no
Ti C(33) C(34) 72.6(8) no
Ti C(34) C(33) 73.6(8) no
Ti C(35) C(34) 75.3(9) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ti Cl(1) 2.419(3) yes
Ti C(11) 2.480(10) yes
Ti C(13) 2.390(10) yes
Ti C(15) 2.390(10) yes
Ti C(32) 2.390(10) yes
Ti C(34) 2.40(2) yes
C(1) C(2) 1.600(10) yes
C(1) C(11) 1.500(10) yes
C(2) C(3) 1.52(2) yes
C(4) C(5) 1.49(2) yes
C(11) C(12) 1.450(10) yes
C(12) C(13) 1.40(2) yes
C(14) C(15) 1.46(2) yes
C(21) C(26) 1.380(10) yes
C(23) C(24) 1.39(2) yes
C(25) C(26) 1.380(10) yes
O(1) C(27) 1.420(10) yes
C(31) C(33) 1.38(2) yes
C(33) C(34) 1.40(2) yes
Ti Cl(2) 2.404(3) yes
Ti C(12) 2.470(10) yes
Ti C(14) 2.330(10) yes
Ti C(31) 2.360(10) yes
Ti C(33) 2.410(10) yes
Ti C(35) 2.360(10) yes
C(1) C(6) 1.610(10) yes
C(1) C(21) 1.550(10) yes
C(3) C(4) 1.60(2) yes
C(5) C(6) 1.51(2) yes
C(11) C(15) 1.390(10) yes
C(13) C(14) 1.44(2) yes
C(21) C(22) 1.370(10) yes
C(22) C(23) 1.410(10) yes
C(24) C(25) 1.40(2) yes
O(1) C(24) 1.340(10) yes
C(31) C(32) 1.30(2) yes
C(32) C(35) 1.34(2) yes
C(34) C(35) 1.32(2) yes
_journal_paper_doi 10.1107/S0108270194013910