#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:54:20 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178587 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/98/4069869.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_4069869
loop_
_publ_author_name
'Yang, Hsu-Tang'
'Zhou, Shuangliu'
'Chang, Feng-Shuo'
'Chen, Chi-Ren'
'Gau, Han-Mou'
_publ_section_title
;
 Synthesis, Structures, and Characterizations of [ArTi(O-i-Pr)3]2and
 Efficient Room-Temperature Aryl−Aryl Coupling of Aryl Bromides
 with [ArTi(O-i-Pr)3]2Catalyzed by the Economic Pd(OAc)2/PCy3System
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5715
_journal_paper_doi               10.1021/om900460u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C17 H30 O3 Ti'
_chemical_formula_weight         330.31
_chemical_name_common            (3,5-Me2C6H4)Ti(OiPr)3
_chemical_name_systematic
; 
 ? 
;
_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                70.697(5)
_cell_angle_beta                 72.451(4)
_cell_angle_gamma                77.055(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8985(3)
_cell_length_b                   9.6752(5)
_cell_length_c                   11.9733(7)
_cell_measurement_reflns_used    4557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.0085
_cell_measurement_theta_min      3.0562
_cell_volume                     918.71(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXS97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7499
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0571P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                2850
_reflns_number_total             3581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900460u_si_003.cif
_cod_data_source_block           gau002(1g)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4069869
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ti1 Ti 0.98629(4) 0.97649(4) 0.64260(3) 0.01190(12) Uani 1 1 d .
O1 O 0.96584(15) 0.87551(15) 0.53379(12) 0.0134(3) Uani 1 1 d .
O2 O 0.90296(16) 0.85747(16) 0.78790(12) 0.0162(3) Uani 1 1 d .
O3 O 1.17644(16) 0.99243(16) 0.65772(13) 0.0180(3) Uani 1 1 d .
C1 C 0.8099(2) 1.1512(2) 0.68541(19) 0.0164(5) Uani 1 1 d .
C2 C 0.6768(2) 1.1873(2) 0.63673(19) 0.0184(5) Uani 1 1 d .
H2A H 0.6737 1.1404 0.5812 0.022 Uiso 1 1 calc R
C3 C 0.5484(2) 1.2919(2) 0.6692(2) 0.0188(5) Uani 1 1 d .
C4 C 0.5557(2) 1.3617(2) 0.7510(2) 0.0187(5) Uani 1 1 d .
H4A H 0.4713 1.4320 0.7729 0.022 Uiso 1 1 calc R
C5 C 0.6854(2) 1.3300(2) 0.80161(19) 0.0177(5) Uani 1 1 d .
C6 C 0.8113(2) 1.2241(2) 0.76717(19) 0.0161(5) Uani 1 1 d .
H6A H 0.8988 1.2018 0.8003 0.019 Uiso 1 1 calc R
C7 C 0.4059(3) 1.3290(3) 0.6154(2) 0.0294(6) Uani 1 1 d .
H7A H 0.4214 1.2709 0.5605 0.044 Uiso 1 1 calc R
H7B H 0.3940 1.4321 0.5717 0.044 Uiso 1 1 calc R
H7C H 0.3119 1.3075 0.6799 0.044 Uiso 1 1 calc R
C8 C 0.6907(3) 1.4065(3) 0.8907(2) 0.0254(5) Uani 1 1 d .
H8A H 0.7891 1.3716 0.9150 0.038 Uiso 1 1 calc R
H8B H 0.6032 1.3855 0.9613 0.038 Uiso 1 1 calc R
H8C H 0.6831 1.5112 0.8528 0.038 Uiso 1 1 calc R
C9 C 0.9149(2) 0.7356(2) 0.55335(19) 0.0166(5) Uani 1 1 d .
H9A H 0.9285 0.7223 0.4731 0.020 Uiso 1 1 calc R
C10 C 1.0187(3) 0.6100(2) 0.6204(2) 0.0268(6) Uani 1 1 d .
H10A H 1.1279 0.6125 0.5753 0.040 Uiso 1 1 calc R
H10B H 0.9875 0.5177 0.6287 0.040 Uiso 1 1 calc R
H10C H 1.0070 0.6199 0.6999 0.040 Uiso 1 1 calc R
C11 C 0.7394(3) 0.7416(3) 0.6168(2) 0.0221(5) Uani 1 1 d .
H11A H 0.6804 0.8233 0.5692 0.033 Uiso 1 1 calc R
H11B H 0.7227 0.7542 0.6961 0.033 Uiso 1 1 calc R
H11C H 0.7039 0.6511 0.6254 0.033 Uiso 1 1 calc R
C12 C 0.8149(2) 0.8377(3) 0.91200(19) 0.0206(5) Uani 1 1 d .
H12A H 0.8329 0.9158 0.9399 0.025 Uiso 1 1 calc R
C13 C 0.6393(3) 0.8539(3) 0.9220(2) 0.0286(6) Uani 1 1 d .
H13A H 0.6058 0.9494 0.8718 0.043 Uiso 1 1 calc R
H13B H 0.5815 0.8442 1.0055 0.043 Uiso 1 1 calc R
H13C H 0.6187 0.7783 0.8952 0.043 Uiso 1 1 calc R
C14 C 0.8769(3) 0.6910(3) 0.9897(2) 0.0302(6) Uani 1 1 d .
H14A H 0.9885 0.6871 0.9808 0.045 Uiso 1 1 calc R
H14B H 0.8605 0.6127 0.9640 0.045 Uiso 1 1 calc R
H14C H 0.8211 0.6799 1.0737 0.045 Uiso 1 1 calc R
C15 C 1.2877(2) 0.9265(2) 0.7307(2) 0.0194(5) Uani 1 1 d .
H15A H 1.3878 0.9669 0.6865 0.023 Uiso 1 1 calc R
C16 C 1.3202(3) 0.7611(3) 0.7496(2) 0.0254(5) Uani 1 1 d .
H16A H 1.3590 0.7410 0.6717 0.038 Uiso 1 1 calc R
H16B H 1.2236 0.7190 0.7928 0.038 Uiso 1 1 calc R
H16C H 1.3985 0.7183 0.7962 0.038 Uiso 1 1 calc R
C17 C 1.2275(3) 0.9682(3) 0.8493(2) 0.0263(5) Uani 1 1 d .
H17A H 1.2088 1.0739 0.8320 0.039 Uiso 1 1 calc R
H17B H 1.3056 0.9284 0.8964 0.039 Uiso 1 1 calc R
H17C H 1.1301 0.9286 0.8948 0.039 Uiso 1 1 calc R
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Ti1 O3 102.82(7) . .
O2 Ti1 O1 101.14(6) . .
O3 Ti1 O1 122.46(6) . .
O2 Ti1 O1 167.53(6) . 2_776
O3 Ti1 O1 89.39(6) . 2_776
O1 Ti1 O1 73.78(6) . 2_776
O2 Ti1 C1 88.90(7) . .
O3 Ti1 C1 111.76(8) . .
O1 Ti1 C1 120.23(8) . .
O1 Ti1 C1 84.14(7) 2_776 .
O2 Ti1 Ti1 138.68(5) . 2_776
O3 Ti1 Ti1 108.34(5) . 2_776
O1 Ti1 Ti1 38.67(4) . 2_776
O1 Ti1 Ti1 35.11(4) 2_776 2_776
C1 Ti1 Ti1 103.60(6) . 2_776
C9 O1 Ti1 133.45(12) . .
C9 O1 Ti1 120.09(12) . 2_776
Ti1 O1 Ti1 106.22(6) . 2_776
C12 O2 Ti1 149.86(14) . .
C15 O3 Ti1 142.64(14) . .
C6 C1 C2 117.61(18) . .
C6 C1 Ti1 123.86(15) . .
C2 C1 Ti1 118.30(16) . .
C3 C2 C1 121.9(2) . .
C3 C2 H2A 119.1 . .
C1 C2 H2A 119.1 . .
C2 C3 C4 118.3(2) . .
C2 C3 C7 120.9(2) . .
C4 C3 C7 120.82(19) . .
C5 C4 C3 121.98(19) . .
C5 C4 H4A 119.0 . .
C3 C4 H4A 119.0 . .
C6 C5 C4 118.0(2) . .
C6 C5 C8 120.9(2) . .
C4 C5 C8 121.14(19) . .
C1 C6 C5 122.3(2) . .
C1 C6 H6A 118.9 . .
C5 C6 H6A 118.9 . .
C3 C7 H7A 109.5 . .
C3 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C3 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C5 C8 H8A 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C5 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O1 C9 C11 109.33(16) . .
O1 C9 C10 110.37(17) . .
C11 C9 C10 113.82(18) . .
O1 C9 H9A 107.7 . .
C11 C9 H9A 107.7 . .
C10 C9 H9A 107.7 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C9 C11 H11A 109.5 . .
C9 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C9 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
O2 C12 C13 110.50(18) . .
O2 C12 C14 109.51(18) . .
C13 C12 C14 112.9(2) . .
O2 C12 H12A 107.9 . .
C13 C12 H12A 107.9 . .
C14 C12 H12A 107.9 . .
C12 C13 H13A 109.5 . .
C12 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C12 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C12 C14 H14A 109.5 . .
C12 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C12 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
O3 C15 C17 109.54(16) . .
O3 C15 C16 110.18(19) . .
C17 C15 C16 113.0(2) . .
O3 C15 H15A 108.0 . .
C17 C15 H15A 108.0 . .
C16 C15 H15A 108.0 . .
C15 C16 H16A 109.5 . .
C15 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C15 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C15 C17 H17A 109.5 . .
C15 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C15 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_distance
_geom_bond_site_symmetry_2
Ti1 O2 1.7840(14) .
Ti1 O3 1.7999(15) .
Ti1 O1 1.9362(15) .
Ti1 O1 2.1032(14) 2_776
Ti1 C1 2.118(2) .
Ti1 Ti1 3.2322(8) 2_776
O1 C9 1.447(2) .
O1 Ti1 2.1032(14) 2_776
O2 C12 1.427(2) .
O3 C15 1.422(2) .
C1 C6 1.386(3) .
C1 C2 1.400(3) .
C2 C3 1.398(3) .
C2 H2A 0.9300 .
C3 C4 1.384(3) .
C3 C7 1.513(3) .
C4 C5 1.390(3) .
C4 H4A 0.9300 .
C5 C6 1.400(3) .
C5 C8 1.502(3) .
C6 H6A 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C11 1.514(3) .
C9 C10 1.508(3) .
C9 H9A 0.9800 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.507(3) .
C12 C14 1.506(3) .
C12 H12A 0.9800 .
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 C17 1.513(3) .
C15 C16 1.513(3) .
C15 H15A 0.9800 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
