#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:22:03 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178604 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/15/4071560.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_4071560
loop_
_publ_author_name
'Lorber, Christian'
'Choukroun, Robert'
'Vendier, Laure'
_publ_section_title
;
 Reactivity of B(C6F5)3with Simple Early Transition Metal Alkoxides:
 Alkoxide-Aryl Exchange, THF Ring-Opening, or Acetonitrile CC Coupling
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5017
_journal_paper_doi               10.1021/om800234z
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H42 F10 O6 Ti2'
_chemical_formula_sum            'C30 H42 F10 O6 Ti2'
_chemical_formula_weight         784.38
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.564(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9690(7)
_cell_length_b                   16.8220(14)
_cell_length_c                   12.0463(10)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.62
_cell_measurement_wavelength     0.71073
_cell_volume                     1805.6(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       ω-φ
_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  0.0466
_diffrn_reflns_av_unetI/netI     0.061
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16234
_diffrn_reflns_theta_full        30.55
_diffrn_reflns_theta_max         30.55
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0957
_reflns_number_gt                3226
_reflns_number_total             5078
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om800234z_si_002.cif
_cod_data_source_block           (1)
_cod_database_code               4071560
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.47922(4) 0.915029(18) 0.43776(2) 0.02433(10) Uani 1 1 d .
F22 F 0.76918(13) 0.99768(7) 0.35803(9) 0.0453(3) Uani 1 1 d .
F33 F 0.88434(15) 1.01357(8) 0.16193(11) 0.0588(4) Uani 1 1 d .
F44 F 0.73154(16) 0.95587(8) -0.02881(10) 0.0608(4) Uani 1 1 d .
F55 F 0.46610(15) 0.87857(8) -0.02133(9) 0.0579(4) Uani 1 1 d .
F66 F 0.35634(14) 0.85800(8) 0.17445(10) 0.0524(3) Uani 1 1 d .
O1 O 0.28519(14) 0.89394(7) 0.41868(10) 0.0321(3) Uani 1 1 d .
O2 O 0.55783(14) 0.81941(7) 0.45411(10) 0.0324(3) Uani 1 1 d .
O3 O 0.56480(13) 0.96336(7) 0.57706(9) 0.0250(3) Uani 1 1 d .
C1 C 0.5581(2) 0.92755(10) 0.27439(14) 0.0283(4) Uani 1 1 d .
C2 C 0.6908(2) 0.96655(11) 0.26479(15) 0.0331(4) Uani 1 1 d .
C3 C 0.7524(2) 0.97587(11) 0.16565(17) 0.0383(5) Uani 1 1 d .
C4 C 0.6760(3) 0.94595(12) 0.06971(16) 0.0404(5) Uani 1 1 d .
C5 C 0.5426(2) 0.90732(12) 0.07385(15) 0.0386(5) Uani 1 1 d .
C6 C 0.4874(2) 0.89840(11) 0.17497(16) 0.0351(4) Uani 1 1 d .
C7 C 0.1851(2) 0.82771(13) 0.41476(19) 0.0462(5) Uani 1 1 d .
H7 H 0.2331 0.7815 0.3805 0.055 Uiso 1 1 calc R
C8 C 0.0442(3) 0.84966(17) 0.3414(2) 0.0737(8) Uani 1 1 d .
H8A H -0.0081 0.892 0.3772 0.111 Uiso 1 1 calc R
H8B H -0.0212 0.803 0.3303 0.111 Uiso 1 1 calc R
H8C H 0.0701 0.8683 0.269 0.111 Uiso 1 1 calc R
C9 C 0.1584(3) 0.80599(15) 0.5319(2) 0.0688(8) Uani 1 1 d .
H9A H 0.2537 0.791 0.5747 0.103 Uiso 1 1 calc R
H9B H 0.0884 0.7611 0.5298 0.103 Uiso 1 1 calc R
H9C H 0.1155 0.8517 0.5676 0.103 Uiso 1 1 calc R
C10 C 0.6252(2) 0.74247(11) 0.44776(17) 0.0413(5) Uani 1 1 d .
H10 H 0.7242 0.7429 0.4952 0.05 Uiso 1 1 calc R
C11 C 0.5269(3) 0.68086(13) 0.4933(2) 0.0583(7) Uani 1 1 d .
H11A H 0.5084 0.6958 0.5692 0.087 Uiso 1 1 calc R
H11B H 0.5772 0.6291 0.4951 0.087 Uiso 1 1 calc R
H11C H 0.4312 0.6776 0.4454 0.087 Uiso 1 1 calc R
C12 C 0.6523(3) 0.72623(13) 0.3295(2) 0.0550(6) Uani 1 1 d .
H12A H 0.556 0.7241 0.2821 0.082 Uiso 1 1 calc R
H12B H 0.7043 0.6753 0.3257 0.082 Uiso 1 1 calc R
H12C H 0.7142 0.7688 0.3033 0.082 Uiso 1 1 calc R
C13 C 0.6658(2) 0.93258(11) 0.66943(14) 0.0335(4) Uani 1 1 d .
H13 H 0.6835 0.976 0.7262 0.04 Uiso 1 1 calc R
C14 C 0.5928(3) 0.86414(12) 0.72397(16) 0.0476(6) Uani 1 1 d .
H14A H 0.4963 0.8815 0.7465 0.071 Uiso 1 1 calc R
H14B H 0.6584 0.8465 0.79 0.071 Uiso 1 1 calc R
H14C H 0.5762 0.82 0.6708 0.071 Uiso 1 1 calc R
C15 C 0.8155(2) 0.91168(13) 0.63128(18) 0.0465(5) Uani 1 1 d .
H15A H 0.8029 0.8669 0.579 0.07 Uiso 1 1 calc R
H15B H 0.8862 0.8969 0.6961 0.07 Uiso 1 1 calc R
H15C H 0.8547 0.9577 0.594 0.07 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
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 O1 101.99(6) . .
O2 Ti1 O3 99.90(5) . .
O1 Ti1 O3 118.88(5) . .
O2 Ti1 O3 167.35(6) . 3_676
O1 Ti1 O3 90.66(5) . 3_676
O3 Ti1 O3 73.52(5) . 3_676
O2 Ti1 C1 91.30(6) . .
O1 Ti1 C1 108.62(7) . .
O3 Ti1 C1 127.13(6) . .
O3 Ti1 C1 84.56(5) 3_676 .
O2 Ti1 Ti1 137.23(4) . 3_676
O1 Ti1 Ti1 107.33(4) . 3_676
O3 Ti1 Ti1 38.31(3) . 3_676
O3 Ti1 Ti1 35.21(3) 3_676 3_676
C1 Ti1 Ti1 107.55(5) . 3_676
C7 O1 Ti1 140.14(13) . .
C10 O2 Ti1 170.29(12) . .
C13 O3 Ti1 131.69(10) . .
C13 O3 Ti1 120.82(10) . 3_676
Ti1 O3 Ti1 106.48(5) . 3_676
C2 C1 C6 114.37(16) . .
C2 C1 Ti1 119.75(13) . .
C6 C1 Ti1 125.87(14) . .
F22 C2 C1 118.99(16) . .
F22 C2 C3 116.78(18) . .
C1 C2 C3 124.22(18) . .
F33 C3 C4 120.05(18) . .
F33 C3 C2 121.45(19) . .
C4 C3 C2 118.50(19) . .
F44 C4 C5 120.25(19) . .
F44 C4 C3 119.8(2) . .
C5 C4 C3 119.92(18) . .
F55 C5 C4 119.91(18) . .
F55 C5 C6 120.76(19) . .
C4 C5 C6 119.33(18) . .
F66 C6 C5 116.77(17) . .
F66 C6 C1 119.58(17) . .
C5 C6 C1 123.65(19) . .
O1 C7 C8 108.08(19) . .
O1 C7 C9 109.03(18) . .
C8 C7 C9 113.5(2) . .
O2 C10 C12 109.27(16) . .
O2 C10 C11 109.54(17) . .
C12 C10 C11 112.80(18) . .
O3 C13 C15 110.47(15) . .
O3 C13 C14 110.03(16) . .
C15 C13 C14 113.56(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O2 1.7585(12) .
Ti1 O1 1.7650(13) .
Ti1 O3 1.9415(11) .
Ti1 O3 2.0875(11) 3_676
Ti1 C1 2.1764(17) .
Ti1 Ti1 3.2289(7) 3_676
F22 C2 1.360(2) .
F33 C3 1.348(2) .
F44 C4 1.349(2) .
F55 C5 1.356(2) .
F66 C6 1.357(2) .
O1 C7 1.428(2) .
O2 C10 1.434(2) .
O3 C13 1.448(2) .
O3 Ti1 2.0875(11) 3_676
C1 C2 1.376(3) .
C1 C6 1.379(3) .
C2 C3 1.381(3) .
C3 C4 1.370(3) .
C4 C5 1.367(3) .
C5 C6 1.375(3) .
C7 C8 1.503(3) .
C7 C9 1.504(3) .
C10 C12 1.498(3) .
C10 C11 1.504(3) .
C13 C15 1.510(3) .
C13 C14 1.512(3) .
