#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:30:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179974 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/68/7026822.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_7026822
loop_
_publ_author_name
'Jura, Marek'
'Levason, William'
'Petts, Edmund'
'Reid, Gillian'
'Webster, Michael'
'Zhang, Wenjian'
_publ_section_title
;
 Taking TiF4 complexes to extremes--the first examples with phosphine
 co-ligands.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10264
_journal_page_last               10271
_journal_paper_doi               10.1039/c0dt00747a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C36 H30 As2 F4 O2 Ti, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H34 As2 Cl4 F4 O2 Ti'
_chemical_formula_weight         938.19
_chemical_name_systematic
;
tetrafluorobis(triphenylarsine oxide)titanium(IV)
dichloromethane solvate
;
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2010-05-07
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.091(3)
_cell_length_b                   16.284(5)
_cell_length_c                   16.152(2)
_cell_measurement_reflns_used    2435
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      61.98
_cell_measurement_theta_min      2.71
_cell_volume                     3969.2(15)
_computing_cell_refinement
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)'
_computing_data_collection
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)'
_computing_data_reduction
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Sapphire3 (Gemini Cu)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7366
_diffrn_reflns_theta_full        61.76
_diffrn_reflns_theta_max         61.76
_diffrn_reflns_theta_min         3.99
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.599
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0740P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                2346
_reflns_number_total             3046
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c0dt00747a.txt
_cod_data_source_block           09mj44
_cod_original_cell_volume        3969.3(15)
_cod_database_code               7026822
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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 0.5000 0.11829(5) 0.2500 0.0295(2) Uani 1 2 d S
As1 As 0.55919(2) 0.26061(2) 0.10881(2) 0.03247(16) Uani 1 1 d .
F1 F 0.57525(13) 0.12549(13) 0.33983(13) 0.0444(5) Uani 1 1 d .
F2 F 0.57113(13) 0.04053(13) 0.20333(14) 0.0466(5) Uani 1 1 d .
O1 O 0.57246(15) 0.20613(15) 0.19535(15) 0.0372(6) Uani 1 1 d .
C1 C 0.4620(3) 0.3363(2) 0.1128(2) 0.0437(9) Uani 1 1 d .
C2 C 0.3764(3) 0.3085(3) 0.1094(2) 0.0497(10) Uani 1 1 d .
H2 H 0.3651 0.2523 0.1082 0.060 Uiso 1 1 calc R
C3 C 0.3069(3) 0.3638(3) 0.1077(3) 0.0639(13) Uani 1 1 d .
H3 H 0.2489 0.3447 0.1057 0.077 Uiso 1 1 calc R
C4 C 0.3224(4) 0.4449(4) 0.1091(3) 0.0817(17) Uani 1 1 d .
H4 H 0.2753 0.4817 0.1079 0.098 Uiso 1 1 calc R
C5 C 0.4076(4) 0.4732(4) 0.1122(5) 0.115(3) Uani 1 1 d .
H5 H 0.4182 0.5294 0.1131 0.138 Uiso 1 1 calc R
C6 C 0.4784(4) 0.4188(3) 0.1138(4) 0.089(2) Uani 1 1 d .
H6 H 0.5363 0.4383 0.1156 0.106 Uiso 1 1 calc R
C7 C 0.5467(2) 0.1951(2) 0.0115(2) 0.0357(8) Uani 1 1 d .
C8 C 0.5132(3) 0.2312(2) -0.0592(2) 0.0484(10) Uani 1 1 d .
H8 H 0.4909 0.2844 -0.0576 0.058 Uiso 1 1 calc R
C9 C 0.5132(3) 0.1875(3) -0.1321(3) 0.0597(12) Uani 1 1 d .
H9 H 0.4913 0.2115 -0.1802 0.072 Uiso 1 1 calc R
C10 C 0.5453(3) 0.1085(3) -0.1344(3) 0.0529(12) Uani 1 1 d .
H10 H 0.5463 0.0798 -0.1842 0.063 Uiso 1 1 calc R
C11 C 0.5755(3) 0.0724(3) -0.0641(3) 0.0473(10) Uani 1 1 d .
H11 H 0.5955 0.0184 -0.0657 0.057 Uiso 1 1 calc R
C12 C 0.5769(2) 0.1155(2) 0.0105(2) 0.0399(9) Uani 1 1 d .
H12 H 0.5978 0.0909 0.0586 0.048 Uiso 1 1 calc R
C13 C 0.6662(3) 0.3225(2) 0.0967(2) 0.0377(9) Uani 1 1 d .
C14 C 0.7047(3) 0.3332(2) 0.0196(3) 0.0474(10) Uani 1 1 d .
H14 H 0.6788 0.3103 -0.0272 0.057 Uiso 1 1 calc R
C15 C 0.7815(3) 0.3779(2) 0.0131(3) 0.0550(11) Uani 1 1 d .
H15 H 0.8075 0.3863 -0.0384 0.066 Uiso 1 1 calc R
C16 C 0.8201(3) 0.4105(3) 0.0837(3) 0.0573(12) Uani 1 1 d .
H16 H 0.8725 0.4402 0.0792 0.069 Uiso 1 1 calc R
C17 C 0.7822(3) 0.3996(3) 0.1597(3) 0.0634(13) Uani 1 1 d .
H17 H 0.8082 0.4225 0.2065 0.076 Uiso 1 1 calc R
C18 C 0.7056(3) 0.3545(3) 0.1669(3) 0.0545(11) Uani 1 1 d .
H18 H 0.6804 0.3457 0.2186 0.065 Uiso 1 1 calc R
Cl1 Cl 0.81701(18) 0.11544(17) 0.11776(12) 0.1546(10) Uani 1 1 d .
Cl2 Cl 0.83398(13) 0.17817(11) 0.28361(11) 0.1136(6) Uani 1 1 d .
C19 C 0.7736(4) 0.1221(4) 0.2137(4) 0.0946(19) Uani 1 1 d .
H19A H 0.7664 0.0669 0.2353 0.114 Uiso 1 1 calc R
H19B H 0.7150 0.1462 0.2094 0.114 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
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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
F2 Ti1 F2 92.02(14) 3_655 .
F2 Ti1 F1 94.67(10) 3_655 .
F2 Ti1 F1 90.39(10) . .
F2 Ti1 F1 90.39(10) 3_655 3_655
F2 Ti1 F1 94.67(10) . 3_655
F1 Ti1 F1 172.72(14) . 3_655
F2 Ti1 O1 89.56(10) 3_655 3_655
F2 Ti1 O1 176.88(10) . 3_655
F1 Ti1 O1 86.80(10) . 3_655
F1 Ti1 O1 88.01(10) 3_655 3_655
F2 Ti1 O1 176.88(10) 3_655 .
F2 Ti1 O1 89.56(10) . .
F1 Ti1 O1 88.01(10) . .
F1 Ti1 O1 86.80(10) 3_655 .
O1 Ti1 O1 88.99(15) 3_655 .
O1 As1 C7 113.85(14) . .
O1 As1 C1 113.92(14) . .
C7 As1 C1 108.19(16) . .
O1 As1 C13 105.33(14) . .
C7 As1 C13 107.07(15) . .
C1 As1 C13 108.09(17) . .
As1 O1 Ti1 133.08(14) . .
C2 C1 C6 119.8(4) . .
C2 C1 As1 120.5(3) . .
C6 C1 As1 119.6(3) . .
C1 C2 C3 120.0(4) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C4 C3 C2 120.6(5) . .
C4 C3 H3 119.7 . .
C2 C3 H3 119.7 . .
C3 C4 C5 119.7(5) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C4 C5 C6 120.7(5) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C1 C6 C5 119.2(5) . .
C1 C6 H6 120.4 . .
C5 C6 H6 120.4 . .
C12 C7 C8 120.8(4) . .
C12 C7 As1 120.4(3) . .
C8 C7 As1 118.6(3) . .
C9 C8 C7 119.2(4) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C10 C9 C8 120.5(4) . .
C10 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C11 C10 C9 120.0(4) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.6(4) . .
C10 C11 H11 119.7 . .
C12 C11 H11 119.7 . .
C7 C12 C11 118.8(4) . .
C7 C12 H12 120.6 . .
C11 C12 H12 120.6 . .
C18 C13 C14 120.6(4) . .
C18 C13 As1 118.6(3) . .
C14 C13 As1 120.8(3) . .
C15 C14 C13 119.4(4) . .
C15 C14 H14 120.3 . .
C13 C14 H14 120.3 . .
C14 C15 C16 119.7(4) . .
C14 C15 H15 120.1 . .
C16 C15 H15 120.1 . .
C17 C16 C15 120.9(4) . .
C17 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
C16 C17 C18 119.8(4) . .
C16 C17 H17 120.1 . .
C18 C17 H17 120.1 . .
C17 C18 C13 119.7(4) . .
C17 C18 H18 120.2 . .
C13 C18 H18 120.2 . .
Cl1 C19 Cl2 115.6(3) . .
Cl1 C19 H19A 108.4 . .
Cl2 C19 H19A 108.4 . .
Cl1 C19 H19B 108.4 . .
Cl2 C19 H19B 108.4 . .
H19A C19 H19B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 F2 1.823(2) 3_655
Ti1 F2 1.823(2) .
Ti1 F1 1.846(2) .
Ti1 F1 1.846(2) 3_655
Ti1 O1 2.005(2) 3_655
Ti1 O1 2.005(2) .
As1 O1 1.668(2) .
As1 C7 1.909(4) .
As1 C1 1.917(4) .
As1 C13 1.913(4) .
C1 C2 1.370(5) .
C1 C6 1.366(6) .
C2 C3 1.384(6) .
C2 H2 0.9300 .
C3 C4 1.341(7) .
C3 H3 0.9300 .
C4 C5 1.367(8) .
C4 H4 0.9300 .
C5 C6 1.389(7) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C12 1.373(5) .
C7 C8 1.382(5) .
C8 C9 1.376(6) .
C8 H8 0.9300 .
C9 C10 1.375(7) .
C9 H9 0.9300 .
C10 C11 1.358(6) .
C10 H10 0.9300 .
C11 C12 1.394(5) .
C11 H11 0.9300 .
C12 H12 0.9300 .
C13 C18 1.382(5) .
C13 C14 1.385(5) .
C14 C15 1.372(5) .
C14 H14 0.9300 .
C15 C16 1.386(6) .
C15 H15 0.9300 .
C16 C17 1.367(6) .
C16 H16 0.9300 .
C17 C18 1.374(6) .
C17 H17 0.9300 .
C18 H18 0.9300 .
Cl1 C19 1.685(6) .
Cl2 C19 1.715(6) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
