#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:47:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179764 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/60/7006078.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_7006078
loop_
_publ_author_name
'Reid, Stuart D.'
'Hector, Andrew L.'
'Levason, William'
'Reid, Gillian'
'Waller, Benjamin J.'
'Webster, Michael'
_publ_section_title
;
 Thio- and seleno-ether complexes with Group 4 tetrahalides and tin
 tetrachloride: preparation and use in CVD for metal chalcogenide
 films.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4769
_journal_page_last               4777
_journal_paper_doi               10.1039/b708809d
_journal_year                    2007
_chemical_formula_moiety         '(C17 H19 Se1 1+)2, Cl6 Ti1 2-, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H42 Cl10 Se2 Ti'
_chemical_formula_weight         1035.02
_chemical_name_systematic
;
Bis(6-methyl-5,7,12,13-tetrahydrodibenzo[c,g]selenoninium)
hexachlorotitanate(IV) dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2006-08-27
_audit_creation_method           'SHELXL-97 + hand edit'
_audit_update_record
; 2007-06-09 Moved cation into unit cell.
Relabelled CH2Cl2 atoms (removed S).
Relabelled HnA to Hn where only one H on C. (mw)
;
_cell_angle_alpha                97.211(10)
_cell_angle_beta                 109.899(10)
_cell_angle_gamma                93.532(10)
_cell_formula_units_Z            1
_cell_length_a                   9.0027(10)
_cell_length_b                   9.955(2)
_cell_length_c                   12.413(3)
_cell_measurement_reflns_used    4211
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1031.3(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15187
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.647
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             518
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0266P)²+0.9361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                3971
_reflns_number_total             4638
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b708809d.txt
_cod_data_source_block           06sdr003
_cod_original_cell_volume        1031.3(3)
_cod_database_code               7006078
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.5000 0.5000 0.0000 0.01320(12) Uani 1 2 d S . .
Se1 Se 0.05158(2) 0.42461(2) 0.162801(18) 0.01686(7) Uani 1 1 d . . .
Cl1 Cl 0.70001(6) 0.61323(6) 0.16564(5) 0.02152(13) Uani 1 1 d . . .
Cl2 Cl 0.30661(6) 0.59563(6) 0.06469(5) 0.02024(12) Uani 1 1 d . . .
Cl3 Cl 0.51461(6) 0.69058(6) -0.09194(5) 0.01877(12) Uani 1 1 d . . .
C1 C 0.2594(3) 0.4110(2) 0.27929(19) 0.0193(5) Uani 1 1 d . . .
H1A H 0.2634 0.3180 0.2998 0.023 Uiso 1 1 calc R . .
H1B H 0.3445 0.4288 0.2475 0.023 Uiso 1 1 calc R . .
C2 C 0.2848(2) 0.5133(2) 0.38518(19) 0.0183(5) Uani 1 1 d . . .
C3 C 0.3033(3) 0.6518(3) 0.3772(2) 0.0230(5) Uani 1 1 d . . .
H3 H 0.2984 0.6785 0.3053 0.028 Uiso 1 1 calc R . .
C4 C 0.3287(3) 0.7508(3) 0.4726(2) 0.0263(5) Uani 1 1 d . . .
H4 H 0.3397 0.8446 0.4661 0.032 Uiso 1 1 calc R . .
C5 C 0.3379(3) 0.7107(3) 0.5780(2) 0.0256(5) Uani 1 1 d . . .
H5 H 0.3556 0.7775 0.6441 0.031 Uiso 1 1 calc R . .
C6 C 0.3214(3) 0.5750(3) 0.5864(2) 0.0223(5) Uani 1 1 d . . .
H6 H 0.3297 0.5495 0.6593 0.027 Uiso 1 1 calc R . .
C7 C 0.2929(2) 0.4727(2) 0.4912(2) 0.0192(5) Uani 1 1 d . . .
C8 C 0.2739(3) 0.3261(2) 0.5083(2) 0.0212(5) Uani 1 1 d . . .
H8A H 0.3335 0.3194 0.5904 0.025 Uiso 1 1 calc R . .
H8B H 0.3224 0.2706 0.4600 0.025 Uiso 1 1 calc R . .
C9 C 0.0987(3) 0.2649(3) 0.4771(2) 0.0217(5) Uani 1 1 d . . .
H9A H 0.0919 0.2188 0.5417 0.026 Uiso 1 1 calc R . .
H9B H 0.0320 0.3410 0.4720 0.026 Uiso 1 1 calc R . .
C10 C 0.0282(3) 0.1645(2) 0.3655(2) 0.0200(5) Uani 1 1 d . . .
C11 C 0.0469(3) 0.0264(3) 0.3714(2) 0.0242(5) Uani 1 1 d . . .
H11 H 0.1106 0.0014 0.4427 0.029 Uiso 1 1 calc R . .
C12 C -0.0241(3) -0.0745(3) 0.2768(2) 0.0276(6) Uani 1 1 d . . .
H12 H -0.0076 -0.1670 0.2832 0.033 Uiso 1 1 calc R . .
C13 C -0.1196(3) -0.0400(3) 0.1727(2) 0.0278(6) Uani 1 1 d . . .
H13 H -0.1726 -0.1091 0.1082 0.033 Uiso 1 1 calc R . .
C14 C -0.1373(3) 0.0952(3) 0.1631(2) 0.0241(5) Uani 1 1 d . . .
H14 H -0.2016 0.1187 0.0912 0.029 Uiso 1 1 calc R . .
C15 C -0.0620(3) 0.1984(2) 0.2575(2) 0.0190(5) Uani 1 1 d . . .
C16 C -0.0851(3) 0.3418(2) 0.2383(2) 0.0210(5) Uani 1 1 d . . .
H16A H -0.0653 0.3986 0.3142 0.025 Uiso 1 1 calc R . .
H16B H -0.1975 0.3446 0.1900 0.025 Uiso 1 1 calc R . .
C17 C 0.0583(3) 0.2787(2) 0.0472(2) 0.0218(5) Uani 1 1 d . . .
H17A H 0.1244 0.3112 0.0052 0.033 Uiso 1 1 calc R . .
H17B H -0.0497 0.2482 -0.0074 0.033 Uiso 1 1 calc R . .
H17C H 0.1037 0.2025 0.0851 0.033 Uiso 1 1 calc R . .
C18 C 0.4794(3) 0.9496(3) 0.1813(2) 0.0296(6) Uani 1 1 d . . .
H18A H 0.4783 0.8682 0.1262 0.036 Uiso 1 1 calc R . .
H18B H 0.5298 1.0292 0.1610 0.036 Uiso 1 1 calc R . .
Cl4 Cl 0.28249(8) 0.97588(8) 0.16873(7) 0.04241(18) Uani 1 1 d . . .
Cl5 Cl 0.59072(9) 0.92667(8) 0.32323(6) 0.03980(17) Uani 1 1 d . . .
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'
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'
Se Se -0.0929 2.2259 '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
_geom_angle_publ_flag
Cl1 Ti1 Cl1 180.00(3) . 2_665 ?
Cl1 Ti1 Cl3 89.07(2) . . ?
Cl1 Ti1 Cl3 90.93(2) 2_665 . ?
Cl1 Ti1 Cl3 90.93(2) . 2_665 ?
Cl1 Ti1 Cl3 89.07(2) 2_665 2_665 ?
Cl3 Ti1 Cl3 180.00(2) . 2_665 ?
Cl1 Ti1 Cl2 90.30(2) . . ?
Cl1 Ti1 Cl2 89.70(2) 2_665 . ?
Cl3 Ti1 Cl2 89.07(2) . . ?
Cl3 Ti1 Cl2 90.93(2) 2_665 . ?
Cl1 Ti1 Cl2 89.70(2) . 2_665 ?
Cl1 Ti1 Cl2 90.30(2) 2_665 2_665 ?
Cl3 Ti1 Cl2 90.93(2) . 2_665 ?
Cl3 Ti1 Cl2 89.07(2) 2_665 2_665 ?
Cl2 Ti1 Cl2 180.00(2) . 2_665 ?
C17 Se1 C1 97.19(10) . . ?
C17 Se1 C16 104.02(10) . . ?
C1 Se1 C16 98.53(10) . . ?
C2 C1 Se1 109.11(15) . . ?
C2 C1 H1A 109.9 . . ?
Se1 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
Se1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C3 C2 C7 120.0(2) . . ?
C3 C2 C1 118.5(2) . . ?
C7 C2 C1 121.5(2) . . ?
C4 C3 C2 121.0(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.1(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 120.1(2) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 122.2(2) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 H6 118.9 . . ?
C6 C7 C2 117.6(2) . . ?
C6 C7 C8 118.5(2) . . ?
C2 C7 C8 123.9(2) . . ?
C7 C8 C9 114.28(19) . . ?
C7 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C8 116.33(19) . . ?
C10 C9 H9A 108.2 . . ?
C8 C9 H9A 108.2 . . ?
C10 C9 H9B 108.2 . . ?
C8 C9 H9B 108.2 . . ?
H9A C9 H9B 107.4 . . ?
C11 C10 C15 117.4(2) . . ?
C11 C10 C9 117.7(2) . . ?
C15 C10 C9 124.8(2) . . ?
C12 C11 C10 122.2(2) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 119.6(2) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 119.7(2) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 121.0(2) . . ?
C13 C14 H14 119.5 . . ?
C15 C14 H14 119.5 . . ?
C14 C15 C10 119.9(2) . . ?
C14 C15 C16 117.3(2) . . ?
C10 C15 C16 122.8(2) . . ?
C15 C16 Se1 115.53(15) . . ?
C15 C16 H16A 108.4 . . ?
Se1 C16 H16A 108.4 . . ?
C15 C16 H16B 108.4 . . ?
Se1 C16 H16B 108.4 . . ?
H16A C16 H16B 107.5 . . ?
Se1 C17 H17A 109.5 . . ?
Se1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Se1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Cl5 C18 Cl4 110.75(14) . . ?
Cl5 C18 H18A 109.5 . . ?
Cl4 C18 H18A 109.5 . . ?
Cl5 C18 H18B 109.5 . . ?
Cl4 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 Cl1 2.3213(7) . ?
Ti1 Cl1 2.3213(7) 2_665 ?
Ti1 Cl3 2.3526(7) . ?
Ti1 Cl3 2.3526(7) 2_665 ?
Ti1 Cl2 2.3551(6) . ?
Ti1 Cl2 2.3551(6) 2_665 ?
Se1 C17 1.929(2) . ?
Se1 C1 1.962(2) . ?
Se1 C16 1.981(2) . ?
C1 C2 1.499(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.399(3) . ?
C2 C7 1.405(3) . ?
C3 C4 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.371(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.399(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.508(3) . ?
C8 C9 1.554(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.515(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.403(3) . ?
C10 C15 1.406(3) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.492(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 Cl5 1.757(3) . ?
C18 Cl4 1.765(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
