#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/22/8102225.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_8102225
loop_
_publ_author_name
'Anke Spannenberg'
'Vladimir V. Burlakov'
'Uwe Rosenthal'
_publ_section_title
;
 Crystal structures of
 tribromo(η5-3,6-di-tert-butyl-9,10,11-trimethyl-bicyclo(6.3.0)undeca-4-en-8,10-dienyl)titanium(IV),
 Ti(C22H35)Br3, and
 tribromo((η5-4,5-dibromo-3,6-di-tert-butyl-9,10,11-trimethyl-bicyclo(6.3.0)undeca-8,10-dienyl)titanium(IV),
 Ti(C22H35Br2)Br3
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              57
_journal_volume                  223
_journal_year                    2008
_chemical_formula_structural     Ti(C22H35)Br3
_chemical_formula_sum            'C22 H35 Br3 Ti'
_chemical_formula_weight         587.13
_chemical_name_systematic
; 
tribromo-(η⁵-3,6-di-tert-butyl-9,10,11-trimethyl-bicyclo(6.3.0)undeca-
4-en-8,10-dienyl)-titanium
;
_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
_cell_angle_alpha                102.23(3)
_cell_angle_beta                 97.71(3)
_cell_angle_gamma                112.32(3)
_cell_formula_units_Z            2
_cell_length_a                   9.621(2)
_cell_length_b                   11.796(2)
_cell_length_c                   12.232(2)
_cell_measurement_reflns_used    4400
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1219.2(6)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe IPDS I'
_diffrn_measurement_method       phi
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3626
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         1.75
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    5.272
_exptl_absorpt_correction_type   'MEAN IMAGING PLATE INTENSITY METHOD'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.042
_refine_diff_density_min         -1.344
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.895
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3626
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_restrained_S_obs      1.072
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_obs          0.0578
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0821P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1459
_refine_ls_wR_factor_obs         0.1340
_reflns_number_observed          2206
_reflns_number_total             3626
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            1267-2163.cff
_cod_data_source_block           255
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0821P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1219.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102225
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_thermal_displace_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C 0.3020(9) 0.1513(8) 0.7023(6) 0.038(2) Uani 1 2 i d . .
C2 C 0.2471(8) 0.2214(7) 0.7824(6) 0.037(2) Uani 1 2 i d . .
C3 C 0.2197(8) 0.3386(8) 0.7775(6) 0.039(2) Uani 1 2 i d . .
H3A H 0.2923 0.3888 0.7397 0.046 Uiso 1 2 i calc R .
H3B H 0.2379 0.3911 0.8552 0.046 Uiso 1 2 i calc R .
C4 C 0.0549(9) 0.3017(8) 0.7123(7) 0.039(2) Uani 1 2 i d . .
H4 H -0.0112 0.2580 0.7585 0.047 Uiso 1 2 i calc R .
C5 C 0.0070(8) 0.2028(7) 0.5964(7) 0.037(2) Uani 1 2 i d . .
H5 H -0.0987 0.1513 0.5717 0.045 Uiso 1 2 i calc R .
C6 C 0.0887(9) 0.1765(8) 0.5240(7) 0.040(2) Uani 1 2 i d . .
H6 H 0.0313 0.1081 0.4587 0.048 Uiso 1 2 i calc R .
C7 C 0.2585(9) 0.2388(8) 0.5298(6) 0.038(2) Uani 1 2 i d . .
H7 H 0.2958 0.3285 0.5744 0.046 Uiso 1 2 i calc R .
C8 C 0.3495(10) 0.1808(9) 0.5957(7) 0.054(2) Uani 1 2 i d . .
H8A H 0.3396 0.1024 0.5434 0.065 Uiso 1 2 i calc R .
H8B H 0.4581 0.2398 0.6173 0.065 Uiso 1 2 i calc R .
C9 C 0.2064(9) 0.1544(8) 0.8662(7) 0.046(2) Uani 1 2 i d . .
C10 C 0.2362(10) 0.0442(8) 0.8367(7) 0.048(2) Uani 1 2 i d . .
C11 C 0.2943(9) 0.0420(8) 0.7360(7) 0.046(2) Uani 1 2 i d . .
C12 C 0.3234(13) -0.0682(9) 0.6699(8) 0.070(3) Uani 1 2 i d . .
H12A H 0.3103 -0.1296 0.7125 0.105 Uiso 1 2 i calc R .
H12B H 0.4270 -0.0362 0.6594 0.105 Uiso 1 2 i calc R .
H12C H 0.2513 -0.1083 0.5961 0.105 Uiso 1 2 i calc R .
C13 C 0.2939(10) 0.2392(8) 0.4074(6) 0.043(2) Uani 1 2 i d . .
C14 C 0.2334(12) 0.1053(9) 0.3247(8) 0.066(3) Uani 1 2 i d . .
H14A H 0.2816 0.0575 0.3559 0.098 Uiso 1 2 i calc R .
H14B H 0.2571 0.1113 0.2518 0.098 Uiso 1 2 i calc R .
H14C H 0.1234 0.0628 0.3143 0.098 Uiso 1 2 i calc R .
C15 C 0.0168(9) 0.4179(8) 0.7078(7) 0.042(2) Uani 1 2 i d . .
C16 C 0.0334(12) 0.4958(10) 0.8312(8) 0.065(3) Uani 1 2 i d . .
H16A H 0.1377 0.5266 0.8749 0.097 Uiso 1 2 i calc R .
H16B H -0.0364 0.4422 0.8673 0.097 Uiso 1 2 i calc R .
H16C H 0.0091 0.5670 0.8280 0.097 Uiso 1 2 i calc R .
C17 C 0.1306(10) 0.1881(10) 0.9594(7) 0.061(3) Uani 1 2 i d . .
H17A H 0.1250 0.2679 0.9605 0.092 Uiso 1 2 i calc R .
H17B H 0.1900 0.1958 1.0324 0.092 Uiso 1 2 i calc R .
H17C H 0.0281 0.1221 0.9449 0.092 Uiso 1 2 i calc R .
C18 C 0.1224(11) 0.5066(9) 0.6493(8) 0.059(3) Uani 1 2 i d . .
H18A H 0.2282 0.5374 0.6898 0.089 Uiso 1 2 i calc R .
H18B H 0.0965 0.5778 0.6504 0.089 Uiso 1 2 i calc R .
H18C H 0.1087 0.4604 0.5711 0.089 Uiso 1 2 i calc R .
C19 C -0.1489(10) 0.3712(9) 0.6420(8) 0.056(2) Uani 1 2 i d . .
H19A H -0.2171 0.3152 0.6774 0.085 Uiso 1 2 i calc R .
H19B H -0.1612 0.3256 0.5638 0.085 Uiso 1 2 i calc R .
H19C H -0.1734 0.4430 0.6432 0.085 Uiso 1 2 i calc R .
C20 C 0.2038(12) -0.0574(10) 0.8989(9) 0.070(3) Uani 1 2 i d . .
H20A H 0.1653 -0.0336 0.9644 0.105 Uiso 1 2 i calc R .
H20B H 0.2975 -0.0656 0.9241 0.105 Uiso 1 2 i calc R .
H20C H 0.1279 -0.1376 0.8477 0.105 Uiso 1 2 i calc R .
C21 C 0.4702(11) 0.3083(10) 0.4222(8) 0.067(3) Uani 1 2 i d . .
H21A H 0.5198 0.2613 0.4532 0.101 Uiso 1 2 i calc R .
H21B H 0.5083 0.3929 0.4738 0.101 Uiso 1 2 i calc R .
H21C H 0.4922 0.3138 0.3487 0.101 Uiso 1 2 i calc R .
C22 C 0.2183(13) 0.3149(10) 0.3585(8) 0.067(3) Uani 1 2 i d . .
H22A H 0.2566 0.3991 0.4107 0.101 Uiso 1 2 i calc R .
H22B H 0.1083 0.2725 0.3481 0.101 Uiso 1 2 i calc R .
H22C H 0.2420 0.3210 0.2856 0.101 Uiso 1 2 i calc R .
Ti Ti 0.4748(2) 0.22505(14) 0.88329(11) 0.0381(4) Uani 1 2 i d . .
Br1 Br 0.60187(10) 0.43937(9) 0.87439(9) 0.0591(3) Uani 1 2 i d . .
Br2 Br 0.65956(11) 0.14223(10) 0.84112(9) 0.0628(3) Uani 1 2 i d . .
Br3 Br 0.49964(12) 0.24752(12) 1.08485(8) 0.0716(4) Uani 1 2 i 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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C11 C1 C2 107.9(6) . . ?
C11 C1 C8 124.8(7) . . ?
C2 C1 C8 127.2(7) . . ?
C11 C1 Ti 73.1(4) . . ?
C2 C1 Ti 72.1(4) . . ?
C8 C1 Ti 123.8(6) . . ?
C9 C2 C1 107.9(6) . . ?
C9 C2 C3 123.8(7) . . ?
C1 C2 C3 128.1(6) . . ?
C9 C2 Ti 72.7(4) . . ?
C1 C2 Ti 72.3(4) . . ?
C3 C2 Ti 125.0(5) . . ?
C2 C3 C4 111.3(7) . . ?
C5 C4 C3 113.2(6) . . ?
C5 C4 C15 113.7(6) . . ?
C3 C4 C15 114.0(7) . . ?
C6 C5 C4 131.5(7) . . ?
C5 C6 C7 130.8(8) . . ?
C6 C7 C8 112.0(6) . . ?
C6 C7 C13 112.7(7) . . ?
C8 C7 C13 111.8(6) . . ?
C1 C8 C7 116.4(6) . . ?
C10 C9 C2 107.3(7) . . ?
C10 C9 C17 126.9(7) . . ?
C2 C9 C17 125.5(7) . . ?
C10 C9 Ti 72.5(5) . . ?
C2 C9 Ti 71.9(4) . . ?
C17 C9 Ti 125.9(6) . . ?
C11 C10 C9 108.8(6) . . ?
C11 C10 C20 125.6(8) . . ?
C9 C10 C20 125.5(8) . . ?
C11 C10 Ti 72.8(5) . . ?
C9 C10 Ti 72.4(5) . . ?
C20 C10 Ti 123.2(6) . . ?
C1 C11 C10 108.0(7) . . ?
C1 C11 C12 126.9(7) . . ?
C10 C11 C12 124.7(7) . . ?
C1 C11 Ti 72.0(5) . . ?
C10 C11 Ti 72.3(5) . . ?
C12 C11 Ti 127.0(6) . . ?
C22 C13 C14 109.6(8) . . ?
C22 C13 C21 108.6(7) . . ?
C14 C13 C21 109.4(7) . . ?
C22 C13 C7 107.1(6) . . ?
C14 C13 C7 113.0(6) . . ?
C21 C13 C7 109.0(7) . . ?
C19 C15 C18 108.2(7) . . ?
C19 C15 C16 107.8(7) . . ?
C18 C15 C16 108.7(8) . . ?
C19 C15 C4 109.9(7) . . ?
C18 C15 C4 112.5(6) . . ?
C16 C15 C4 109.7(6) . . ?
C2 Ti C1 35.5(2) . . ?
C2 Ti C9 35.4(2) . . ?
C1 Ti C9 58.9(3) . . ?
C2 Ti C10 58.4(3) . . ?
C1 Ti C10 58.3(3) . . ?
C9 Ti C10 35.1(3) . . ?
C2 Ti C11 58.5(3) . . ?
C1 Ti C11 34.9(3) . . ?
C9 Ti C11 58.5(3) . . ?
C10 Ti C11 35.0(3) . . ?
C2 Ti Br1 86.9(2) . . ?
C1 Ti Br1 95.0(2) . . ?
C9 Ti Br1 114.0(2) . . ?
C10 Ti Br1 145.3(2) . . ?
C11 Ti Br1 128.7(2) . . ?
C2 Ti Br3 116.4(2) . . ?
C1 Ti Br3 145.7(2) . . ?
C9 Ti Br3 87.1(2) . . ?
C10 Ti Br3 91.7(2) . . ?
C11 Ti Br3 124.4(2) . . ?
Br1 Ti Br3 103.92(8) . . ?
C2 Ti Br2 137.2(2) . . ?
C1 Ti Br2 101.6(2) . . ?
C9 Ti Br2 140.1(2) . . ?
C10 Ti Br2 105.3(2) . . ?
C11 Ti Br2 85.3(2) . . ?
Br1 Ti Br2 101.39(6) . . ?
Br3 Ti Br2 102.38(6) . . ?
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
C1 C11 1.414(10) . ?
C1 C2 1.433(10) . ?
C1 C8 1.503(10) . ?
C1 Ti 2.349(7) . ?
C2 C9 1.429(10) . ?
C2 C3 1.513(10) . ?
C2 Ti 2.346(7) . ?
C3 C4 1.526(10) . ?
C4 C5 1.516(11) . ?
C4 C15 1.557(10) . ?
C5 C6 1.325(10) . ?
C6 C7 1.499(11) . ?
C7 C8 1.543(10) . ?
C7 C13 1.581(9) . ?
C9 C10 1.419(11) . ?
C9 C17 1.497(11) . ?
C9 Ti 2.356(8) . ?
C10 C11 1.418(11) . ?
C10 C20 1.510(11) . ?
C10 Ti 2.358(9) . ?
C11 C12 1.521(11) . ?
C11 Ti 2.364(9) . ?
C13 C22 1.512(11) . ?
C13 C14 1.525(12) . ?
C13 C21 1.542(12) . ?
C15 C19 1.514(11) . ?
C15 C18 1.531(10) . ?
C15 C16 1.544(12) . ?
Ti Br1 2.388(2) . ?
Ti Br3 2.392(2) . ?
Ti Br2 2.394(2) . ?
