#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010109.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_7010109
loop_
_publ_author_name
'Carmalt, Claire J.'
'Dinnage, Christopher W.'
'Parkin, Ivan P.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Synthesis and structural characterisation of titanium(IV) thiolate
 compounds
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3500
_journal_paper_doi               10.1039/b006115h
_journal_year                    2000
_chemical_formula_sum            'C32 H22 F20 N2 S4 Ti'
_chemical_formula_weight         990.66
_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                 91.179(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2002(12)
_cell_length_b                   17.6154(12)
_cell_length_c                   14.117(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      10.59
_cell_volume                     3779.1(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3219
_diffrn_reflns_theta_max         63.59
_diffrn_reflns_theta_min         3.84
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.184
_exptl_absorpt_correction_T_max  0.2352
_exptl_absorpt_correction_T_min  0.0844
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00018(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.061
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         2979
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.108
_refine_ls_restrained_S_obs      1.089
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_obs          0.0552
_refine_ls_shift/esd_max         0.004
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1123P)²+0.7417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1595
_refine_ls_wR_factor_obs         0.1427
_reflns_number_observed          2598
_reflns_number_total             3093
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b006115h.txt
_cod_data_source_block           CC0001
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+0.7417P] 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^)+(0.1123P)^2^+0.7417P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C32 H22 N2 F20 S4 Ti'
_cod_database_code               7010109
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
_atom_site_disorder_group
Ti Ti 0.0000 0.26647(4) 0.7500 0.0400(3) Uani 1 d S .
S1 S 0.06773(5) 0.33478(5) 0.88081(6) 0.0501(3) Uani 1 d . .
S2 S 0.13183(5) 0.30423(5) 0.66804(6) 0.0476(3) Uani 1 d . .
N N 0.0000 0.1615(2) 0.7500 0.0537(10) Uani 1 d S .
C1 C 0.1836(2) 0.3362(2) 0.8813(2) 0.0475(7) Uani 1 d . .
C2 C 0.2282(2) 0.4047(2) 0.8845(3) 0.0531(8) Uani 1 d . .
F2 F 0.1826(2) 0.47029(15) 0.8793(2) 0.0713(7) Uani 1 d . .
C3 C 0.3187(2) 0.4092(3) 0.8909(3) 0.0583(9) Uani 1 d . .
F3 F 0.3596(2) 0.4767(2) 0.8901(2) 0.0816(8) Uani 1 d . .
C4 C 0.3675(2) 0.3437(3) 0.8937(3) 0.0585(9) Uani 1 d . .
F4 F 0.4554(2) 0.3480(2) 0.8990(2) 0.0848(9) Uani 1 d . .
C5 C 0.3264(3) 0.2746(3) 0.8905(3) 0.0567(9) Uani 1 d . .
F5 F 0.3736(2) 0.2108(2) 0.8926(2) 0.0770(8) Uani 1 d . .
C6 C 0.2359(3) 0.2713(2) 0.8849(3) 0.0521(8) Uani 1 d . .
F6 F 0.1980(2) 0.20315(14) 0.8822(2) 0.0665(6) Uani 1 d . .
C7 C 0.1378(2) 0.2511(2) 0.5630(3) 0.0478(7) Uani 1 d . .
C8 C 0.1754(2) 0.1784(2) 0.5616(3) 0.0491(7) Uani 1 d . .
F8 F 0.2061(2) 0.14747(14) 0.6418(2) 0.0615(6) Uani 1 d . .
C9 C 0.1831(2) 0.1374(2) 0.4781(3) 0.0556(8) Uani 1 d . .
F9 F 0.2212(2) 0.0690(2) 0.4795(2) 0.0765(7) Uani 1 d . .
C10 C 0.1537(2) 0.1676(3) 0.3947(3) 0.0582(9) Uani 1 d . .
F10 F 0.1585(2) 0.1272(2) 0.3145(2) 0.0774(8) Uani 1 d . .
C11 C 0.1194(2) 0.2398(3) 0.3924(3) 0.0577(9) Uani 1 d . .
F11 F 0.0916(2) 0.2703(2) 0.3101(2) 0.0778(8) Uani 1 d . .
C12 C 0.1127(2) 0.2806(2) 0.4753(3) 0.0523(8) Uani 1 d . .
F12 F 0.0819(2) 0.3519(2) 0.4686(2) 0.0677(6) Uani 1 d . .
C13 C 0.0166(3) 0.1183(2) 0.8371(3) 0.0574(9) Uani 1 d . .
H13A H -0.0382(3) 0.0919(2) 0.8545(3) 0.069 Uiso 1 calc R .
H13B H 0.0319(3) 0.1542(2) 0.8888(3) 0.069 Uiso 1 calc R .
C14 C 0.0900(3) 0.0600(3) 0.8295(4) 0.0735(12) Uani 1 d . .
H14A H 0.0974(3) 0.0334(3) 0.8901(4) 0.110 Uiso 1 calc R .
H14B H 0.1450(3) 0.0857(3) 0.8140(4) 0.110 Uiso 1 calc R .
H14C H 0.0748(3) 0.0233(3) 0.7796(4) 0.110 Uiso 1 calc R .
N20 N -0.0080(17) 0.4920(5) 0.7684(16) 0.099(6) Uani 0.50 d PD -1
H20A H -0.0452(17) 0.4638(5) 0.7300(16) 0.119 Uiso 0.50 calc PR -1
H20B H 0.0354(17) 0.4599(5) 0.7910(16) 0.119 Uiso 0.50 calc PR -1
C21 C -0.0579(12) 0.5198(18) 0.8488(14) 0.166(15) Uani 0.50 d PD -1
H21A H -0.0300(12) 0.5674(18) 0.8713(14) 0.199 Uiso 0.50 calc PR -1
H21B H -0.0516(12) 0.4822(18) 0.9007(14) 0.199 Uiso 0.50 calc PR -1
C22 C -0.1529(10) 0.5347(9) 0.8333(13) 0.113(5) Uani 0.50 d PD -1
H22A H -0.1784(10) 0.5530(9) 0.8923(13) 0.169 Uiso 0.50 calc PR -1
H22B H -0.1825(10) 0.4877(9) 0.8135(13) 0.169 Uiso 0.50 calc PR -1
H22C H -0.1609(10) 0.5732(9) 0.7838(13) 0.169 Uiso 0.50 calc PR -1
C23 C 0.0334(14) 0.5506(6) 0.7101(11) 0.138(8) Uani 0.50 d PD -1
H23A H 0.0725(14) 0.5820(6) 0.7511(11) 0.166 Uiso 0.50 calc PR -1
H23B H -0.0130(14) 0.5842(6) 0.6833(11) 0.166 Uiso 0.50 calc PR -1
C24 C 0.0863(13) 0.5184(11) 0.6301(13) 0.099(5) Uani 0.50 d PD -1
H24A H 0.1121(13) 0.5601(11) 0.5940(13) 0.148 Uiso 0.50 calc PR -1
H24B H 0.0477(13) 0.4883(11) 0.5882(13) 0.148 Uiso 0.50 calc PR -1
H24C H 0.1333(13) 0.4861(11) 0.6561(13) 0.148 Uiso 0.50 calc PR -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
N N 0.0311 0.0180 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
N Ti S1 119.86(3) . . ?
N Ti S1 119.86(3) . 2_556 ?
S1 Ti S1 120.27(6) . 2_556 ?
N Ti S2 105.90(3) . 2_556 ?
S1 Ti S2 80.92(3) . 2_556 ?
S1 Ti S2 83.39(3) 2_556 2_556 ?
N Ti S2 105.90(3) . . ?
S1 Ti S2 83.39(3) . . ?
S1 Ti S2 80.92(3) 2_556 . ?
S2 Ti S2 148.20(5) 2_556 . ?
C1 S1 Ti 114.83(12) . . ?
C7 S2 Ti 108.31(11) . . ?
C13 N C13 117.3(4) 2_556 . ?
C13 N Ti 121.3(2) 2_556 . ?
C13 N Ti 121.3(2) . . ?
C2 C1 C6 115.8(3) . . ?
C2 C1 S1 120.1(3) . . ?
C6 C1 S1 124.0(3) . . ?
F2 C2 C3 117.7(4) . . ?
F2 C2 C1 119.7(3) . . ?
C3 C2 C1 122.7(4) . . ?
F3 C3 C4 119.7(3) . . ?
F3 C3 C2 120.8(4) . . ?
C4 C3 C2 119.4(4) . . ?
F4 C4 C5 120.5(4) . . ?
F4 C4 C3 119.4(4) . . ?
C5 C4 C3 120.1(3) . . ?
F5 C5 C4 120.3(4) . . ?
F5 C5 C6 120.2(4) . . ?
C4 C5 C6 119.5(4) . . ?
F6 C6 C5 118.0(4) . . ?
F6 C6 C1 119.5(3) . . ?
C5 C6 C1 122.5(4) . . ?
C12 C7 C8 115.7(3) . . ?
C12 C7 S2 122.3(3) . . ?
C8 C7 S2 121.7(3) . . ?
F8 C8 C9 118.3(4) . . ?
F8 C8 C7 119.8(3) . . ?
C9 C8 C7 121.9(4) . . ?
F9 C9 C10 120.0(4) . . ?
F9 C9 C8 120.1(4) . . ?
C10 C9 C8 120.0(4) . . ?
F10 C10 C9 120.1(4) . . ?
F10 C10 C11 119.9(4) . . ?
C9 C10 C11 120.0(4) . . ?
F11 C11 C10 120.2(4) . . ?
F11 C11 C12 120.0(4) . . ?
C10 C11 C12 119.8(4) . . ?
F12 C12 C11 117.3(4) . . ?
F12 C12 C7 120.1(3) . . ?
C11 C12 C7 122.6(4) . . ?
N C13 C14 114.0(3) . . ?
C21 N20 C23 115.7(15) . . ?
N20 C21 C22 117.7(18) . . ?
N20 C23 C24 113.3(10) . . ?
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
Ti N 1.849(4) . ?
Ti S1 2.4166(9) . ?
Ti S1 2.4166(9) 2_556 ?
Ti S2 2.4273(8) 2_556 ?
Ti S2 2.4273(8) . ?
S1 C1 1.761(3) . ?
S2 C7 1.758(4) . ?
N C13 1.463(5) 2_556 ?
N C13 1.463(5) . ?
C1 C2 1.384(5) . ?
C1 C6 1.392(5) . ?
C2 F2 1.349(5) . ?
C2 C3 1.380(5) . ?
C3 F3 1.342(5) . ?
C3 C4 1.372(6) . ?
C4 F4 1.338(4) . ?
C4 C5 1.368(6) . ?
C5 F5 1.332(5) . ?
C5 C6 1.378(6) . ?
C6 F6 1.332(5) . ?
C7 C12 1.388(5) . ?
C7 C8 1.403(5) . ?
C8 F8 1.332(5) . ?
C8 C9 1.389(5) . ?
C9 F9 1.337(5) . ?
C9 C10 1.360(6) . ?
C10 F10 1.340(5) . ?
C10 C11 1.376(7) . ?
C11 F11 1.340(5) . ?
C11 C12 1.379(6) . ?
C12 F12 1.342(5) . ?
C13 C14 1.522(6) . ?
N20 C21 1.463(10) . ?
N20 C23 1.470(9) . ?
C21 C22 1.481(10) . ?
C23 C24 1.510(10) . ?
