#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/34/2213438.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_2213438
loop_
_publ_author_name
'Wu, Qiao-Lin'
'Ye, Ling'
'Li, Bao'
'Mu, Ying'
_publ_section_title
μ-Oxido-bis({η⁵-1-[3,5-bis(trifluoromethyl)phenyl]-2,3,4,5-tetramethylcyclopentadienyl}dichloridotitanium(IV))
_journal_coeditor_code           LH2331
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1194
_journal_page_last               m1195
_journal_paper_doi               10.1107/S1600536807013360
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ti2 (C17 H15 F6)2 Cl4 O]'
_chemical_formula_moiety         'C34 H30 Cl4 F12 O Ti2'
_chemical_formula_sum            'C34 H30 Cl4 F12 O Ti2'
_chemical_formula_weight         920.18
_chemical_name_systematic
;
μ-Oxido-bis(dichlorido{η⁵-2,3,4,5-tetramethyl-1-[3,5-
bis(trifluoromethyl)phenyl]cyclopentadienyl}titanium(IV))
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.63(3)
_cell_angle_beta                 71.28(3)
_cell_angle_gamma                69.52(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6637(17)
_cell_length_b                   10.551(2)
_cell_length_c                   11.630(2)
_cell_measurement_reflns_used    7837
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.02
_cell_measurement_theta_min      7.19
_cell_volume                     938.9(4)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction
'CrystalStructure (Rigaku/MSC and Rigaku, 2002)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9309
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_T_max  0.8632
_exptl_absorpt_correction_T_min  0.8075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.769
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4265
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0682P)²+1.1255P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1371
_reflns_number_gt                3604
_reflns_number_total             4265
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2331.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2213438
_cod_database_fobs_code          2213438
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_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
Ti Ti1 0.54968(5) 0.84204(4) 0.59532(4) 0.02522(14) Uani d . 1 . .
Cl Cl1 0.83760(10) 0.76724(9) 0.54386(12) 0.0629(3) Uani d . 1 . .
Cl Cl2 0.47997(13) 0.91446(10) 0.78012(7) 0.0534(2) Uani d . 1 . .
F F1 -0.0596(7) 1.2372(5) 0.7544(6) 0.0615(16) Uani d PU 0.553(12) A 1
F F2 -0.1350(10) 1.1969(6) 0.9500(5) 0.0722(17) Uani d PU 0.553(12) A 1
F F3 -0.3060(8) 1.2167(6) 0.8442(7) 0.0693(16) Uani d PU 0.553(12) A 1
F F1' -0.2680(10) 1.2354(7) 0.7981(8) 0.069(2) Uani d PU 0.447(12) A 2
F F2' -0.0204(9) 1.2279(7) 0.8010(8) 0.069(2) Uani d PU 0.447(12) A 2
F F3' -0.2078(11) 1.1887(6) 0.9661(6) 0.0640(19) Uani d PU 0.447(12) A 2
F F4 -0.3655(3) 0.7703(4) 1.0341(3) 0.1030(11) Uani d . 1 . .
F F5 -0.2117(5) 0.6134(4) 0.9194(3) 0.1001(11) Uani d . 1 . .
F F6 -0.1357(4) 0.6334(3) 1.0667(3) 0.0877(9) Uani d . 1 . .
O O1 0.5000 1.0000 0.5000 0.0374(6) Uani d S 1 . .
C C1 0.3134(3) 0.7572(3) 0.6592(2) 0.0274(5) Uani d . 1 . .
C C2 0.4523(3) 0.6488(3) 0.6914(3) 0.0319(6) Uani d . 1 . .
C C3 0.5792(3) 0.6100(3) 0.5820(3) 0.0339(6) Uani d . 1 . .
C C4 0.5222(3) 0.6938(3) 0.4825(3) 0.0322(6) Uani d . 1 . .
C C5 0.3558(3) 0.7829(3) 0.5298(2) 0.0280(5) Uani d . 1 . .
C C6 0.1459(3) 0.8215(3) 0.7447(2) 0.0305(5) Uani d . 1 . .
C C7 0.0811(3) 0.9612(3) 0.7533(3) 0.0334(6) Uani d . 1 . .
H H7 0.1434 1.0175 0.7040 0.040 Uiso calc R 1 . .
C C8 -0.0753(4) 1.0167(3) 0.8349(3) 0.0385(6) Uani d . 1 A .
C C9 -0.1711(4) 0.9350(4) 0.9087(3) 0.0441(7) Uani d . 1 . .
H H9 -0.2758 0.9726 0.9637 0.053 Uiso calc R 1 . .
C C10 -0.1087(4) 0.7973(4) 0.8991(3) 0.0412(7) Uani d . 1 . .
C C11 0.0493(4) 0.7398(3) 0.8180(3) 0.0366(6) Uani d . 1 . .
H H11 0.0902 0.6464 0.8131 0.044 Uiso calc R 1 . .
C C12 -0.1399(4) 1.1660(4) 0.8473(3) 0.0488(8) Uani d . 1 . .
C C13 -0.2063(5) 0.7049(5) 0.9795(4) 0.0593(10) Uani d . 1 . .
C C14 0.4597(5) 0.5868(3) 0.8178(3) 0.0450(7) Uani d . 1 . .
H H14A 0.4183 0.5097 0.8374 0.068 Uiso calc R 1 . .
H H14B 0.3896 0.6527 0.8749 0.068 Uiso calc R 1 . .
H H14C 0.5760 0.5583 0.8220 0.068 Uiso calc R 1 . .
C C15 0.7420(4) 0.4938(3) 0.5718(4) 0.0530(9) Uani d . 1 . .
H H15A 0.7824 0.4844 0.6418 0.079 Uiso calc R 1 . .
H H15B 0.8270 0.5109 0.4993 0.079 Uiso calc R 1 . .
H H15C 0.7210 0.4114 0.5679 0.079 Uiso calc R 1 . .
C C16 0.6179(5) 0.6865(4) 0.3502(3) 0.0491(8) Uani d . 1 . .
H H16A 0.7352 0.6791 0.3395 0.074 Uiso calc R 1 . .
H H16B 0.5665 0.7673 0.3039 0.074 Uiso calc R 1 . .
H H16C 0.6132 0.6084 0.3223 0.074 Uiso calc R 1 . .
C C17 0.2401(4) 0.8775(3) 0.4569(3) 0.0356(6) Uani d . 1 . .
H H17A 0.1690 0.8319 0.4446 0.053 Uiso calc R 1 . .
H H17B 0.3077 0.9055 0.3793 0.053 Uiso calc R 1 . .
H H17C 0.1692 0.9558 0.5000 0.053 Uiso calc R 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Ti1 Cl1 . 103.97(5) yes
O1 Ti1 Cl2 . 102.20(4) yes
Cl1 Ti1 Cl2 . 103.15(6) yes
O1 Ti1 C4 . 100.56(8) n
Cl1 Ti1 C4 . 95.33(8) n
Cl2 Ti1 C4 . 146.06(8) n
O1 Ti1 C5 . 86.88(7) ?
Cl1 Ti1 C5 . 130.27(7) ?
Cl2 Ti1 C5 . 122.03(7) ?
C4 Ti1 C5 . 35.15(9) ?
O1 Ti1 C1 . 109.52(7) ?
Cl1 Ti1 C1 . 140.20(7) ?
Cl2 Ti1 C1 . 90.35(8) ?
C4 Ti1 C1 . 58.25(9) ?
C5 Ti1 C1 . 35.13(9) ?
O1 Ti1 C3 . 135.31(8) ?
Cl1 Ti1 C3 . 83.67(8) ?
Cl2 Ti1 C3 . 119.08(9) ?
C4 Ti1 C3 . 34.85(11) ?
C5 Ti1 C3 . 57.86(10) ?
C1 Ti1 C3 . 57.41(9) ?
O1 Ti1 C2 . 143.40(7) ?
Cl1 Ti1 C2 . 107.02(8) ?
Cl2 Ti1 C2 . 89.30(8) ?
C4 Ti1 C2 . 57.87(10) ?
C5 Ti1 C2 . 58.17(10) ?
C1 Ti1 C2 . 34.91(9) ?
C3 Ti1 C2 . 34.07(10) ?
Ti1 O1 Ti1 2_676 180 y
C5 C1 C2 . 108.4(2) ?
C5 C1 C6 . 125.4(2) ?
C2 C1 C6 . 125.9(2) ?
C5 C1 Ti1 . 72.02(14) ?
C2 C1 Ti1 . 74.39(15) ?
C6 C1 Ti1 . 124.64(18) ?
C3 C2 C1 . 107.3(2) ?
C3 C2 C14 . 126.4(3) ?
C1 C2 C14 . 126.3(3) ?
C3 C2 Ti1 . 72.60(15) ?
C1 C2 Ti1 . 70.70(14) ?
C14 C2 Ti1 . 122.9(2) ?
C2 C3 C4 . 108.7(2) ?
C2 C3 C15 . 125.6(3) ?
C4 C3 C15 . 125.6(3) ?
C2 C3 Ti1 . 73.33(16) ?
C4 C3 Ti1 . 70.35(15) ?
C15 C3 Ti1 . 125.2(2) ?
C5 C4 C3 . 108.1(2) ?
C5 C4 C16 . 125.6(3) ?
C3 C4 C16 . 126.2(3) ?
C5 C4 Ti1 . 72.73(15) ?
C3 C4 Ti1 . 74.80(16) ?
C16 C4 Ti1 . 120.0(2) ?
C4 C5 C1 . 107.5(2) ?
C4 C5 C17 . 126.2(3) ?
C1 C5 C17 . 126.2(2) ?
C4 C5 Ti1 . 72.12(15) ?
C1 C5 Ti1 . 72.85(15) ?
C17 C5 Ti1 . 124.61(18) ?
C11 C6 C7 . 118.7(3) ?
C11 C6 C1 . 118.9(3) ?
C7 C6 C1 . 122.4(2) ?
C8 C7 C6 . 120.5(3) ?
C8 C7 H7 . 119.8 ?
C6 C7 H7 . 119.8 ?
C7 C8 C9 . 120.8(3) ?
C7 C8 C12 . 120.0(3) ?
C9 C8 C12 . 119.1(3) ?
C10 C9 C8 . 118.8(3) ?
C10 C9 H9 . 120.6 ?
C8 C9 H9 . 120.6 ?
C9 C10 C11 . 120.9(3) ?
C9 C10 C13 . 120.5(3) ?
C11 C10 C13 . 118.5(3) ?
C6 C11 C10 . 120.3(3) ?
C6 C11 H11 . 119.9 ?
C10 C11 H11 . 119.9 ?
F2 C12 F2' . 81.8(5) ?
F2 C12 F1' . 121.2(5) ?
F2' C12 F1' . 106.5(5) ?
F2 C12 F1 . 108.8(5) ?
F1' C12 F1 . 80.3(5) ?
F2' C12 F3' . 107.2(5) ?
F1' C12 F3' . 103.5(5) ?
F1 C12 F3' . 129.8(5) ?
F2 C12 F3 . 106.7(4) ?
F2' C12 F3 . 126.8(5) ?
F1 C12 F3 . 103.9(4) ?
F3' C12 F3 . 83.5(4) ?
F2 C12 C8 . 113.6(4) ?
F2' C12 C8 . 114.0(4) ?
F1' C12 C8 . 114.7(4) ?
F1 C12 C8 . 113.2(3) ?
F3' C12 C8 . 110.2(4) ?
F3 C12 C8 . 109.8(4) ?
F4 C13 F5 . 106.9(4) ?
F4 C13 F6 . 106.4(3) ?
F5 C13 F6 . 104.8(4) ?
F4 C13 C10 . 113.1(4) ?
F5 C13 C10 . 112.6(3) ?
F6 C13 C10 . 112.4(3) ?
C2 C14 H14A . 109.5 ?
C2 C14 H14B . 109.5 ?
H14A C14 H14B . 109.5 ?
C2 C14 H14C . 109.5 ?
H14A C14 H14C . 109.5 ?
H14B C14 H14C . 109.5 ?
C3 C15 H15A . 109.5 ?
C3 C15 H15B . 109.5 ?
H15A C15 H15B . 109.5 ?
C3 C15 H15C . 109.5 ?
H15A C15 H15C . 109.5 ?
H15B C15 H15C . 109.5 ?
C4 C16 H16A . 109.5 ?
C4 C16 H16B . 109.5 ?
H16A C16 H16B . 109.5 ?
C4 C16 H16C . 109.5 ?
H16A C16 H16C . 109.5 ?
H16B C16 H16C . 109.5 ?
C5 C17 H17A . 109.5 ?
C5 C17 H17B . 109.5 ?
H17A C17 H17B . 109.5 ?
C5 C17 H17C . 109.5 ?
H17A C17 H17C . 109.5 ?
H17B C17 H17C . 109.5 ?
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
Ti1 O1 . 1.8077(8) y
Ti1 Cl1 . 2.2481(11) y
Ti1 Cl2 . 2.2492(11) y
Ti1 C4 . 2.344(3) y
Ti1 C5 . 2.352(3) y
Ti1 C1 . 2.363(3) y
Ti1 C3 . 2.402(3) y
Ti1 C2 . 2.412(3) y
F1 C12 . 1.334(6) n
F2 C12 . 1.315(6) n
F3 C12 . 1.358(6) n
F1' C12 . 1.330(8) ?
F2' C12 . 1.328(7) ?
F3' C12 . 1.350(7) ?
F4 C13 . 1.314(5) n
F5 C13 . 1.320(5) n
F6 C13 . 1.321(5) n
O1 Ti1 2_676 1.8077(8) ?
C1 C5 . 1.423(4) ?
C1 C2 . 1.433(4) ?
C1 C6 . 1.486(4) ?
C2 C3 . 1.410(4) ?
C2 C14 . 1.498(4) ?
C3 C4 . 1.423(4) ?
C3 C15 . 1.499(4) ?
C4 C5 . 1.418(4) ?
C4 C16 . 1.499(4) ?
C5 C17 . 1.493(4) ?
C6 C11 . 1.388(4) ?
C6 C7 . 1.393(4) ?
C7 C8 . 1.385(4) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.386(5) ?
C8 C12 . 1.496(5) ?
C9 C10 . 1.375(5) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.396(4) ?
C10 C13 . 1.500(5) ?
C11 H11 . 0.9300 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
