#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:16:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180255 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/41/7114133.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_7114133
loop_
_publ_author_name
'Alonso, Pablo J.'
'Forniés, Juan'
'García-Monforte, M. Angeles'
'Martín, Antonio'
'Menjón, Babil'
_publ_section_title
;
 The first structurally characterised homoleptic σ-organotitanium(iii)
 compound
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              728
_journal_paper_doi               10.1039/b111127b
_journal_year                    2002
_chemical_formula_sum            'C41 H38 Cl22 Li O4 Ti'
_chemical_formula_weight         1429.45
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.748(5)
_cell_length_b                   19.1546(15)
_cell_length_c                   17.580(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.6
_cell_measurement_theta_min      10.2
_cell_volume                     5637.5(19)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4548
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2860
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.711
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.049
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.049
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_obs          0.0484
_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)+(0.0651P)²+20.0030P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1385
_refine_ls_wR_factor_obs         0.1202
_reflns_number_observed          3363
_reflns_number_total             4368
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b111127b.txt
_cod_data_source_block           amt186
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+20.0030P] 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^)+(0.0651P)^2^+20.0030P] 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        5637.6(18)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7114133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ti Ti 0.0000 0.17223(6) 0.2500 0.0203(3) Uani 1 d S
Cl2 Cl -0.05903(8) 0.07613(6) 0.37483(6) 0.0290(3) Uani 1 d .
Cl3 Cl -0.18971(9) -0.03924(8) 0.37814(8) 0.0478(4) Uani 1 d .
Cl4 Cl -0.28217(10) -0.07930(8) 0.22757(10) 0.0568(5) Uani 1 d .
Cl5 Cl -0.25800(10) 0.00847(8) 0.08082(8) 0.0494(4) Uani 1 d .
Cl6 Cl -0.12935(8) 0.12446(7) 0.07873(6) 0.0336(3) Uani 1 d .
Cl8 Cl -0.13056(8) 0.27368(7) 0.18385(7) 0.0306(3) Uani 1 d .
Cl9 Cl -0.12798(10) 0.38236(8) 0.05158(9) 0.0517(4) Uani 1 d .
Cl10 Cl 0.03055(11) 0.40874(8) -0.03277(8) 0.0554(5) Uani 1 d .
Cl11 Cl 0.18343(8) 0.32523(7) 0.01275(7) 0.0357(3) Uani 1 d .
Cl12 Cl 0.18087(7) 0.21864(6) 0.14443(6) 0.0286(3) Uani 1 d .
C1 C -0.0978(3) 0.0970(2) 0.2283(2) 0.0217(10) Uani 1 d .
C2 C -0.1154(3) 0.0572(2) 0.2921(3) 0.0238(11) Uani 1 d .
C3 C -0.1723(3) 0.0046(2) 0.2942(3) 0.0290(12) Uani 1 d .
C4 C -0.2147(3) -0.0111(3) 0.2280(3) 0.0348(13) Uani 1 d .
C5 C -0.2015(3) 0.0275(3) 0.1621(3) 0.0313(12) Uani 1 d .
C6 C -0.1444(3) 0.0791(2) 0.1635(3) 0.0257(11) Uani 1 d .
C7 C 0.0236(3) 0.2479(2) 0.1586(3) 0.0225(11) Uani 1 d .
C8 C -0.0427(3) 0.2873(2) 0.1342(3) 0.0246(11) Uani 1 d .
C9 C -0.0423(3) 0.3359(3) 0.0759(3) 0.0320(13) Uani 1 d .
C10 C 0.0275(3) 0.3477(3) 0.0386(3) 0.0332(13) Uani 1 d .
C11 C 0.0961(3) 0.3111(2) 0.0602(3) 0.0280(12) Uani 1 d .
C12 C 0.0927(3) 0.2624(2) 0.1190(3) 0.0224(11) Uani 1 d .
Li Li 0.0000 0.2225(7) 0.7500 0.046(4) Uani 1 d S
O1 O -0.0855(3) 0.2756(2) 0.7949(3) 0.0585(12) Uani 1 d .
C13 C -0.1545(5) 0.2379(4) 0.8208(4) 0.072(2) Uani 1 d .
H13A H -0.1530(5) 0.1896(4) 0.8008(4) 0.087 Uiso 1 calc R
H13B H -0.2036(5) 0.2604(4) 0.8000(4) 0.087 Uiso 1 calc R
C14 C -0.1578(6) 0.2356(5) 0.9038(4) 0.087(3) Uani 1 d .
H14A H -0.2053(6) 0.2096(5) 0.9185(4) 0.131 Uiso 1 calc R
H14B H -0.1604(6) 0.2832(5) 0.9238(4) 0.131 Uiso 1 calc R
H14C H -0.1098(6) 0.2123(5) 0.9246(4) 0.131 Uiso 1 calc R
C15 C -0.0998(5) 0.3486(4) 0.7938(5) 0.079(2) Uani 1 d .
H15A H -0.0477(5) 0.3728(4) 0.7988(5) 0.095 Uiso 1 calc R
H15B H -0.1308(5) 0.3608(4) 0.8390(5) 0.095 Uiso 1 calc R
C16 C -0.1437(5) 0.3765(4) 0.7239(5) 0.080(2) Uani 1 d .
H16A H -0.1505(5) 0.4271(4) 0.7288(5) 0.120 Uiso 1 calc R
H16B H -0.1963(5) 0.3541(4) 0.7190(5) 0.120 Uiso 1 calc R
H16C H -0.1129(5) 0.3662(4) 0.6787(5) 0.120 Uiso 1 calc R
O2 O 0.0516(2) 0.1608(2) 0.8223(2) 0.0425(10) Uani 1 d .
C17 C 0.1060(5) 0.1876(4) 0.8804(3) 0.074(3) Uani 1 d .
H17A H 0.1618(5) 0.1830(4) 0.8640(3) 0.089 Uiso 1 calc R
H17B H 0.0950(5) 0.2377(4) 0.8896(3) 0.089 Uiso 1 calc R
C18 C 0.0948(6) 0.1486(4) 0.9479(4) 0.090(3) Uani 1 d .
H18A H 0.0687(6) 0.1781(4) 0.9862(4) 0.108 Uiso 1 calc R
H18B H 0.1472(6) 0.1334(4) 0.9694(4) 0.108 Uiso 1 calc R
C19 C 0.0444(4) 0.0867(3) 0.9305(3) 0.0394(14) Uani 1 d .
H19A H -0.0049(4) 0.0874(3) 0.9604(3) 0.047 Uiso 1 calc R
H19B H 0.0739(4) 0.0429(3) 0.9418(3) 0.047 Uiso 1 calc R
C20 C 0.0246(3) 0.0932(3) 0.8456(3) 0.0327(13) Uani 1 d .
H20A H 0.0521(3) 0.0561(3) 0.8170(3) 0.039 Uiso 1 calc R
H20B H -0.0336(3) 0.0886(3) 0.8358(3) 0.039 Uiso 1 calc R
Cl13 Cl -0.01926(14) 0.51784(9) 0.83017(10) 0.0730(6) Uani 1 d .
C21 C 0.0000 0.5690(5) 0.7500 0.065(3) Uani 1 d S
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'
Li Li -0.0003 0.0001 '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'
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'
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
C7 Ti C1 114.0(2) 2 .
C7 Ti C1 116.8(2) 2 2
C1 Ti C1 98.5(2) . 2
C7 Ti C7 97.9(2) 2 .
C1 Ti C7 116.8(2) . .
C1 Ti C7 114.0(2) 2 .
C2 C1 C6 113.2(4) . .
C2 C1 Ti 113.0(3) . .
C6 C1 Ti 133.8(3) . .
C3 C2 C1 125.3(4) . .
C3 C2 Cl2 118.9(4) . .
C1 C2 Cl2 115.8(4) . .
C4 C3 C2 118.3(4) . .
C4 C3 Cl3 121.3(4) . .
C2 C3 Cl3 120.5(4) . .
C3 C4 C5 119.7(5) . .
C3 C4 Cl4 119.3(4) . .
C5 C4 Cl4 121.0(4) . .
C6 C5 C4 119.5(5) . .
C6 C5 Cl5 121.9(4) . .
C4 C5 Cl5 118.6(4) . .
C5 C6 C1 124.0(4) . .
C5 C6 Cl6 117.3(4) . .
C1 C6 Cl6 118.6(4) . .
C12 C7 C8 113.6(4) . .
C12 C7 Ti 131.5(3) . .
C8 C7 Ti 114.8(3) . .
C9 C8 C7 124.7(5) . .
C9 C8 Cl8 119.3(4) . .
C7 C8 Cl8 116.0(3) . .
C10 C9 C8 119.0(5) . .
C10 C9 Cl9 120.5(4) . .
C8 C9 Cl9 120.6(4) . .
C9 C10 C11 119.6(4) . .
C9 C10 Cl10 120.2(4) . .
C11 C10 Cl10 120.2(4) . .
C10 C11 C12 119.4(5) . .
C10 C11 Cl11 119.6(4) . .
C12 C11 Cl11 121.0(4) . .
C7 C12 C11 123.7(4) . .
C7 C12 Cl12 118.9(3) . .
C11 C12 Cl12 117.3(4) . .
O2 Li O2 104.2(6) . 2_556
O2 Li O1 112.1(2) . .
O2 Li O1 105.5(2) 2_556 .
O2 Li O1 105.5(2) . 2_556
O2 Li O1 112.1(2) 2_556 2_556
O1 Li O1 116.8(7) . 2_556
C15 O1 C13 111.2(6) . .
C15 O1 Li 129.6(6) . .
C13 O1 Li 118.0(5) . .
O1 C13 C14 112.4(6) . .
O1 C15 C16 115.9(7) . .
C20 O2 C17 108.5(4) . .
C20 O2 Li 127.1(4) . .
C17 O2 Li 120.8(5) . .
C18 C17 O2 108.0(5) . .
C17 C18 C19 109.7(5) . .
C18 C19 C20 104.1(4) . .
O2 C20 C19 106.9(4) . .
Cl13 C21 Cl13 112.0(5) . 2_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti C7 2.207(4) 2
Ti C1 2.207(5) .
Ti C1 2.207(5) 2
Ti C7 2.207(4) .
Cl2 C2 1.750(5) .
Cl3 C3 1.730(5) .
Cl4 C4 1.727(5) .
Cl5 C5 1.731(5) .
Cl6 C6 1.749(5) .
Cl8 C8 1.751(5) .
Cl9 C9 1.731(5) .
Cl10 C10 1.716(5) .
Cl11 C11 1.726(5) .
Cl12 C12 1.746(5) .
C1 C2 1.394(6) .
C1 C6 1.406(6) .
C2 C3 1.389(7) .
C3 C4 1.380(7) .
C4 C5 1.395(7) .
C5 C6 1.376(7) .
C7 C12 1.394(7) .
C7 C8 1.400(7) .
C8 C9 1.385(7) .
C9 C10 1.376(8) .
C10 C11 1.389(7) .
C11 C12 1.395(6) .
Li O2 1.923(9) .
Li O2 1.923(9) 2_556
Li O1 1.942(8) .
Li O1 1.942(8) 2_556
O1 C15 1.418(8) .
O1 C13 1.446(8) .
C13 C14 1.463(10) .
C15 C16 1.512(11) .
O2 C20 1.435(6) .
O2 C17 1.444(7) .
C17 C18 1.420(9) .
C18 C19 1.483(8) .
C19 C20 1.526(7) .
Cl13 C21 1.754(5) .
C21 Cl13 1.754(5) 2_556
