#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/30/2213043.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_2213043
loop_
_publ_author_name
'Wu, Qiao-Lin'
'Su, Qing'
'Ye, Ling'
'Li, Bao'
'Mu, Ying'
_publ_section_title
μ-Oxo-bis{dichlorido[η⁵-2,3,4,5-tetramethyl-1-(4-methylphenyl)cyclopentadienyl]titanium(IV)}
_journal_coeditor_code           TK2146
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1158
_journal_page_last               m1159
_journal_paper_doi               10.1107/S1600536807012585
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ti2 (C16 H19)2 Cl4 O]'
_chemical_formula_moiety         'C32 H38 Cl4 O Ti2'
_chemical_formula_sum            'C32 H38 Cl4 O Ti2'
_chemical_formula_weight         676.22
_chemical_name_systematic
;
μ-Oxo-bis{dichlorido[η⁵-2,3,4,5-tetramethyl-1-(4-
methylphenyl)cyclopentadienyl]titanium(IV)}
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 94.61(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.268(8)
_cell_length_b                   13.459(5)
_cell_length_c                   15.019(7)
_cell_measurement_reflns_used    12659
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      55.0
_cell_measurement_theta_min      6.1
_cell_volume                     3278(3)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC Rigaku, 2002)'
_computing_molecular_graphics
'PLATON (Spek, 2003) and MERCURY (Macrae et al.,  2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15845
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0547P)²+0.938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.092
_refine_ls_wR_factor_ref         0.097
_reflns_number_gt                3009
_reflns_number_total             3747
_reflns_threshold_expression     I>\2s(I)
_cod_data_source_file            tk2146.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2213043
_cod_database_fobs_code          2213043
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'
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
Ti Ti1 0.390353(18) 0.62793(2) 0.24722(2) 0.02866(11) Uani d . 1
Cl Cl1 0.34401(4) 0.73148(5) 0.34996(4) 0.05922(18) Uani d . 1
Cl Cl2 0.38994(4) 0.48009(4) 0.31704(4) 0.05887(18) Uani d . 1
O O1 0.5000 0.65406(13) 0.2500 0.0336(4) Uani d S 1
C C1 0.38606(11) 0.63656(13) 0.09110(12) 0.0337(4) Uani d . 1
C C2 0.34556(11) 0.54726(14) 0.11310(12) 0.0361(4) Uani d . 1
C C3 0.27241(11) 0.57333(14) 0.15352(12) 0.0357(4) Uani d . 1
C C4 0.26802(11) 0.67808(14) 0.15790(12) 0.0345(4) Uani d . 1
C C5 0.33938(11) 0.71792(13) 0.12059(12) 0.0336(4) Uani d . 1
C C6 0.35965(12) 0.82425(14) 0.11071(12) 0.0367(4) Uani d . 1
C C7 0.43737(14) 0.86190(16) 0.13623(17) 0.0499(5) Uani d . 1
H H7 0.4782 0.8195 0.1609 0.060 Uiso calc R 1
C C8 0.45521(16) 0.96161(17) 0.12553(18) 0.0586(6) Uani d . 1
H H8 0.5078 0.9848 0.1434 0.070 Uiso calc R 1
C C9 0.39712(16) 1.02698(16) 0.08926(16) 0.0531(6) Uani d . 1
C C10 0.31946(17) 0.99014(16) 0.06462(16) 0.0557(6) Uani d . 1
H H10 0.2788 1.0332 0.0407 0.067 Uiso calc R 1
C C11 0.30050(14) 0.89108(15) 0.07458(15) 0.0477(5) Uani d . 1
H H11 0.2476 0.8686 0.0570 0.057 Uiso calc R 1
C C12 0.45931(13) 0.64154(16) 0.03795(14) 0.0432(5) Uani d . 1
H H12A 0.4984 0.5915 0.0586 0.065 Uiso calc R 1
H H12B 0.4844 0.7059 0.0449 0.065 Uiso calc R 1
H H12C 0.4424 0.6303 -0.0240 0.065 Uiso calc R 1
C C13 0.37300(15) 0.44444(15) 0.09157(16) 0.0504(5) Uani d . 1
H H13A 0.3396 0.3968 0.1196 0.076 Uiso calc R 1
H H13B 0.4297 0.4358 0.1132 0.076 Uiso calc R 1
H H13C 0.3673 0.4348 0.0280 0.076 Uiso calc R 1
C C14 0.20887(13) 0.50294(16) 0.18237(16) 0.0499(5) Uani d . 1
H H14A 0.1905 0.5246 0.2384 0.075 Uiso calc R 1
H H14B 0.2323 0.4377 0.1892 0.075 Uiso calc R 1
H H14C 0.1629 0.5013 0.1381 0.075 Uiso calc R 1
C C15 0.19792(13) 0.73486(17) 0.19109(16) 0.0502(5) Uani d . 1
H H15A 0.1554 0.7428 0.1435 0.075 Uiso calc R 1
H H15B 0.2169 0.7990 0.2116 0.075 Uiso calc R 1
H H15C 0.1764 0.6993 0.2395 0.075 Uiso calc R 1
C C16 0.4174(2) 1.13565(19) 0.0776(2) 0.0845(10) Uani d . 1
H H16A 0.4550 1.1425 0.0319 0.127 Uiso calc R 1
H H16B 0.4424 1.1616 0.1329 0.127 Uiso calc R 1
H H16C 0.3677 1.1718 0.0607 0.127 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'
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
O1 Ti1 Cl2 . 101.56(5)
O1 Ti1 Cl1 . 104.28(5)
Cl2 Ti1 Cl1 . 102.37(4)
O1 Ti1 C1 . 87.92(5)
Cl2 Ti1 C1 . 120.62(5)
Cl1 Ti1 C1 . 132.06(5)
O1 Ti1 C5 . 101.60(6)
Cl2 Ti1 C5 . 145.02(5)
Cl1 Ti1 C5 . 96.88(6)
C1 Ti1 C5 . 35.32(6)
O1 Ti1 C2 . 110.21(6)
Cl2 Ti1 C2 . 88.77(6)
Cl1 Ti1 C2 . 140.74(5)
C1 Ti1 C2 . 35.27(7)
C5 Ti1 C2 . 58.65(7)
O1 Ti1 C3 . 144.10(6)
Cl2 Ti1 C3 . 88.30(5)
Cl1 Ti1 C3 . 107.16(6)
C1 Ti1 C3 . 58.04(7)
C5 Ti1 C3 . 57.99(7)
C2 Ti1 C3 . 34.81(7)
O1 Ti1 C4 . 136.54(6)
Cl2 Ti1 C4 . 118.35(5)
Cl1 Ti1 C4 . 84.32(6)
C1 Ti1 C4 . 58.08(7)
C5 Ti1 C4 . 35.06(7)
C2 Ti1 C4 . 57.75(7)
C3 Ti1 C4 . 34.20(6)
Ti1 O1 Ti1 2_655 157.66(11)
C2 C1 C5 . 108.00(17)
C2 C1 C12 . 124.65(17)
C5 C1 C12 . 127.05(18)
C2 C1 Ti1 . 72.71(10)
C5 C1 Ti1 . 72.57(10)
C12 C1 Ti1 . 125.33(13)
C1 C2 C3 . 108.04(16)
C1 C2 C13 . 125.39(19)
C3 C2 C13 . 126.45(18)
C1 C2 Ti1 . 72.02(10)
C3 C2 Ti1 . 74.51(11)
C13 C2 Ti1 . 122.30(13)
C4 C3 C2 . 108.23(17)
C4 C3 C14 . 125.54(19)
C2 C3 C14 . 126.17(19)
C4 C3 Ti1 . 73.05(10)
C2 C3 Ti1 . 70.68(10)
C14 C3 Ti1 . 124.31(14)
C3 C4 C5 . 108.03(16)
C3 C4 C15 . 124.71(18)
C5 C4 C15 . 127.17(18)
C3 C4 Ti1 . 72.75(10)
C5 C4 Ti1 . 70.32(10)
C15 C4 Ti1 . 125.30(14)
C1 C5 C4 . 107.64(16)
C1 C5 C6 . 125.76(18)
C4 C5 C6 . 126.56(17)
C1 C5 Ti1 . 72.11(10)
C4 C5 Ti1 . 74.63(10)
C6 C5 Ti1 . 120.88(12)
C7 C6 C11 . 117.19(19)
C7 C6 C5 . 122.10(17)
C11 C6 C5 . 120.71(18)
C8 C7 C6 . 121.1(2)
C8 C7 H7 . 119.4
C6 C7 H7 . 119.4
C9 C8 C7 . 121.6(2)
C9 C8 H8 . 119.2
C7 C8 H8 . 119.2
C8 C9 C10 . 117.6(2)
C8 C9 C16 . 121.1(2)
C10 C9 C16 . 121.3(2)
C11 C10 C9 . 121.7(2)
C11 C10 H10 . 119.1
C9 C10 H10 . 119.1
C10 C11 C6 . 120.8(2)
C10 C11 H11 . 119.6
C6 C11 H11 . 119.6
C1 C12 H12A . 109.5
C1 C12 H12B . 109.5
H12A C12 H12B . 109.5
C1 C12 H12C . 109.5
H12A C12 H12C . 109.5
H12B C12 H12C . 109.5
C2 C13 H13A . 109.5
C2 C13 H13B . 109.5
H13A C13 H13B . 109.5
C2 C13 H13C . 109.5
H13A C13 H13C . 109.5
H13B C13 H13C . 109.5
C3 C14 H14A . 109.5
C3 C14 H14B . 109.5
H14A C14 H14B . 109.5
C3 C14 H14C . 109.5
H14A C14 H14C . 109.5
H14B C14 H14C . 109.5
C4 C15 H15A . 109.5
C4 C15 H15B . 109.5
H15A C15 H15B . 109.5
C4 C15 H15C . 109.5
H15A C15 H15C . 109.5
H15B C15 H15C . 109.5
C9 C16 H16A . 109.5
C9 C16 H16B . 109.5
H16A C16 H16B . 109.5
C9 C16 H16C . 109.5
H16A C16 H16C . 109.5
H16B C16 H16C . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ti1 O1 . 1.8153(10)
Ti1 Cl2 . 2.2495(9)
Ti1 Cl1 . 2.2535(9)
Ti1 C1 . 2.343(2)
Ti1 C5 . 2.3491(19)
Ti1 C2 . 2.3520(19)
Ti1 C3 . 2.4018(19)
Ti1 C4 . 2.4056(19)
O1 Ti1 2_655 1.8153(10)
C1 C2 . 1.422(3)
C1 C5 . 1.423(3)
C1 C12 . 1.488(3)
C2 C3 . 1.423(3)
C2 C13 . 1.497(3)
C3 C4 . 1.413(3)
C3 C14 . 1.492(3)
C4 C5 . 1.433(3)
C4 C15 . 1.491(3)
C5 C6 . 1.479(3)
C6 C7 . 1.387(3)
C6 C11 . 1.395(3)
C7 C8 . 1.385(3)
C7 H7 . 0.9300
C8 C9 . 1.372(3)
C8 H8 . 0.9300
C9 C10 . 1.380(4)
C9 C16 . 1.512(3)
C10 C11 . 1.379(3)
C10 H10 . 0.9300
C11 H11 . 0.9300
C12 H12A . 0.9600
C12 H12B . 0.9600
C12 H12C . 0.9600
C13 H13A . 0.9600
C13 H13B . 0.9600
C13 H13C . 0.9600
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
