#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/20/4302078.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_4302078
loop_
_publ_author_name
'Alberto Donzelli'
'Pierre G. Potvin'
_publ_section_title
;
Dithiocarbamate Complexes of Ti(IV) Alkoxides: Synthesis, Characterization,
and Electrochemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4171
_journal_page_last               4178
_journal_paper_doi               10.1021/ic802394a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C38 H31 N1 O S1 Ti'
_chemical_formula_sum            'C38 H31 N O S Ti'
_chemical_formula_weight         545.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.811(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0462(3)
_cell_length_b                   14.5216(5)
_cell_length_c                   15.7630(5)
_cell_measurement_reflns_used    17187
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2498.68(14)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'SHELXTL V6.12'
_computing_publication_material  'SHELXTL V6.12'
_computing_structure_refinement  'SHELXTL V6.12(Sheldrick, 2001)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offsets'
_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  0.0708
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17187
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.62
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0699P)²+0.7976P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                3938
_reflns_number_total             5697
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic802394a_si_001_1.cif
_cod_data_source_block           k0611
_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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C38 H31 N1 O S1 Ti'
_cod_database_code               4302078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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 0.26281(5) 0.27555(4) 0.60626(3) 0.02821(16) Uani 1 1 d . A .
S5 S 0.33092(7) 0.13663(6) 0.52349(5) 0.0327(2) Uani 1 1 d . . .
S6 S 0.46494(7) 0.30445(6) 0.55397(5) 0.0319(2) Uani 1 1 d . . .
S3 S 0.33408(8) 0.43610(6) 0.64980(5) 0.0372(2) Uani 1 1 d . . .
S4 S 0.13709(7) 0.34566(6) 0.71516(5) 0.0336(2) Uani 1 1 d . . .
S2 S 0.37849(7) 0.19782(6) 0.74032(5) 0.0333(2) Uani 1 1 d . . .
S1 S 0.13921(7) 0.13886(5) 0.65244(5) 0.0300(2) Uani 1 1 d . . .
O1 O 0.15348(19) 0.30329(15) 0.51575(14) 0.0352(5) Uani 1 1 d . . .
N3 N 0.5206(2) 0.17783(18) 0.44306(16) 0.0298(6) Uani 1 1 d . . .
N2 N 0.2277(2) 0.50899(17) 0.77412(16) 0.0316(6) Uani 1 1 d . . .
N1 N 0.2547(2) 0.05745(18) 0.79317(16) 0.0299(6) Uani 1 1 d . . .
C3 C 0.4490(3) 0.2020(2) 0.49856(19) 0.0288(7) Uani 1 1 d . . .
C2 C 0.2294(3) 0.4398(2) 0.72005(19) 0.0296(7) Uani 1 1 d . . .
C1 C 0.2571(3) 0.1238(2) 0.73599(19) 0.0290(7) Uani 1 1 d . . .
C4 C 0.6197(3) 0.2356(2) 0.4184(2) 0.0349(7) Uani 1 1 d . . .
H4A H 0.6905 0.2383 0.4652 0.042 Uiso 1 1 calc R . .
H4B H 0.5905 0.2990 0.4042 0.042 Uiso 1 1 calc R . .
C5 C 0.6535(3) 0.1871(3) 0.3400(2) 0.0468(9) Uani 1 1 d . . .
H5A H 0.6083 0.2140 0.2867 0.056 Uiso 1 1 calc R . .
H5B H 0.7425 0.1925 0.3384 0.056 Uiso 1 1 calc R . .
C6 C 0.6180(4) 0.0884(3) 0.3492(3) 0.0490(9) Uani 1 1 d . . .
H6A H 0.6845 0.0541 0.3851 0.059 Uiso 1 1 calc R . .
H6B H 0.6001 0.0583 0.2923 0.059 Uiso 1 1 calc R . .
C7 C 0.5039(3) 0.0921(2) 0.3923(2) 0.0363(8) Uani 1 1 d . . .
H7A H 0.4287 0.0948 0.3492 0.044 Uiso 1 1 calc R . .
H7B H 0.4993 0.0379 0.4297 0.044 Uiso 1 1 calc R . .
C8 C 0.1548(3) 0.5096(2) 0.8453(2) 0.0366(8) Uani 1 1 d . . .
H8A H 0.1637 0.4509 0.8776 0.044 Uiso 1 1 calc R . .
H8B H 0.0669 0.5204 0.8239 0.044 Uiso 1 1 calc R . .
C9 C 0.2097(3) 0.5889(3) 0.9003(2) 0.0460(9) Uani 1 1 d . . .
H9A H 0.2796 0.5680 0.9429 0.055 Uiso 1 1 calc R . .
H9B H 0.1478 0.6179 0.9309 0.055 Uiso 1 1 calc R . .
C30 C 0.2520(4) 0.6555(2) 0.8364(2) 0.0475(9) Uani 1 1 d . . .
H10A H 0.3148 0.6984 0.8653 0.057 Uiso 1 1 calc R . .
H10B H 0.1824 0.6915 0.8061 0.057 Uiso 1 1 calc R . .
C31 C 0.3053(3) 0.5919(2) 0.7750(2) 0.0394(8) Uani 1 1 d . . .
H11A H 0.2989 0.6195 0.7170 0.047 Uiso 1 1 calc R . .
H11B H 0.3923 0.5774 0.7963 0.047 Uiso 1 1 calc R . .
C32 C 0.1598(3) -0.0143(2) 0.7880(2) 0.0336(7) Uani 1 1 d . . .
H12A H 0.1470 -0.0439 0.7308 0.040 Uiso 1 1 calc R . .
H12B H 0.0811 0.0115 0.7996 0.040 Uiso 1 1 calc R . .
C33 C 0.2119(3) -0.0820(2) 0.8572(2) 0.0447(9) Uani 1 1 d . . .
H13A H 0.2642 -0.1284 0.8345 0.054 Uiso 1 1 calc R . .
H13B H 0.1458 -0.1140 0.8813 0.054 Uiso 1 1 calc R . .
C34 C 0.2875(3) -0.0211(3) 0.9248(2) 0.0404(8) Uani 1 1 d . . .
H14A H 0.2344 0.0109 0.9607 0.048 Uiso 1 1 calc R . .
H14B H 0.3498 -0.0576 0.9623 0.048 Uiso 1 1 calc R . .
C35 C 0.3471(3) 0.0468(2) 0.8709(2) 0.0369(8) Uani 1 1 d . . .
H15A H 0.3635 0.1063 0.9011 0.044 Uiso 1 1 calc R . .
H15B H 0.4249 0.0221 0.8564 0.044 Uiso 1 1 calc R . .
C36 C 0.0699(4) 0.2996(4) 0.4361(3) 0.0488(15) Uani 0.823(9) 1 d P A 1
H16 H 0.1166 0.3055 0.3868 0.059 Uiso 0.823(9) 1 calc PR A 1
C37 C -0.0197(4) 0.3778(4) 0.4344(3) 0.0785(16) Uani 1 1 d . A 1
H17A H -0.0701 0.3689 0.4798 0.118 Uiso 0.823(9) 1 calc PR A 1
H17B H -0.0725 0.3794 0.3784 0.118 Uiso 0.823(9) 1 calc PR A 1
H17C H 0.0251 0.4361 0.4438 0.118 Uiso 0.823(9) 1 calc PR A 1
C38 C 0.0055(4) 0.2055(3) 0.4325(3) 0.0635(12) Uani 1 1 d . A 1
H18A H 0.0668 0.1563 0.4355 0.095 Uiso 0.823(9) 1 calc PR A 1
H18B H -0.0515 0.2003 0.3786 0.095 Uiso 0.823(9) 1 calc PR A 1
H18C H -0.0398 0.1999 0.4810 0.095 Uiso 0.823(9) 1 calc PR A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
N N 0.0061 0.0033 '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
O1 Ti1 S3 98.92(8) . . ?
O1 Ti1 S6 103.12(8) . . ?
S3 Ti1 S6 71.40(3) . . ?
O1 Ti1 S2 163.68(8) . . ?
S3 Ti1 S2 95.02(3) . . ?
S6 Ti1 S2 89.33(3) . . ?
O1 Ti1 S1 94.44(8) . . ?
S3 Ti1 S1 142.39(3) . . ?
S6 Ti1 S1 138.76(3) . . ?
S2 Ti1 S1 69.27(3) . . ?
O1 Ti1 S5 89.20(8) . . ?
S3 Ti1 S5 139.32(3) . . ?
S6 Ti1 S5 67.93(3) . . ?
S2 Ti1 S5 85.71(3) . . ?
S1 Ti1 S5 75.43(3) . . ?
O1 Ti1 S4 94.38(8) . . ?
S3 Ti1 S4 68.36(3) . . ?
S6 Ti1 S4 138.05(3) . . ?
S2 Ti1 S4 82.88(3) . . ?
S1 Ti1 S4 75.72(3) . . ?
S5 Ti1 S4 151.11(3) . . ?
C3 S5 Ti1 88.52(11) . . ?
C3 S6 Ti1 89.73(11) . . ?
C2 S3 Ti1 89.52(11) . . ?
C2 S4 Ti1 88.13(11) . . ?
C1 S2 Ti1 87.42(11) . . ?
C1 S1 Ti1 86.69(11) . . ?
C36 O1 Ti1 164.0(3) . . ?
C36A O1 Ti1 135.5(7) . . ?
C3 N3 C7 123.2(3) . . ?
C3 N3 C4 124.7(3) . . ?
C7 N3 C4 111.9(2) . . ?
C2 N2 C31 124.1(3) . . ?
C2 N2 C8 124.0(3) . . ?
C31 N2 C8 111.8(2) . . ?
C1 N1 C32 124.5(2) . . ?
C1 N1 C35 123.9(3) . . ?
C32 N1 C35 111.6(2) . . ?
N3 C3 S5 124.3(2) . . ?
N3 C3 S6 122.9(2) . . ?
S5 C3 S6 112.71(17) . . ?
N2 C2 S4 125.0(2) . . ?
N2 C2 S3 121.2(2) . . ?
S4 C2 S3 113.77(18) . . ?
N1 C1 S2 121.9(2) . . ?
N1 C1 S1 121.5(2) . . ?
S2 C1 S1 116.61(18) . . ?
N3 C4 C5 103.6(3) . . ?
C6 C5 C4 105.3(3) . . ?
C5 C6 C7 104.9(3) . . ?
N3 C7 C6 103.2(3) . . ?
N2 C8 C9 102.9(3) . . ?
C8 C9 C30 104.0(3) . . ?
C9 C30 C31 102.9(3) . . ?
N2 C31 C30 102.7(3) . . ?
N1 C32 C33 103.3(3) . . ?
C32 C33 C34 103.5(3) . . ?
C35 C34 C33 102.9(3) . . ?
N1 C35 C34 103.2(3) . . ?
O1 C36 C37 108.7(4) . . ?
O1 C36 C38 107.3(4) . . ?
C37 C36 C38 111.8(4) . . ?
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 O1 1.769(2) . ?
Ti1 S3 2.5221(10) . ?
Ti1 S6 2.5308(9) . ?
Ti1 S2 2.5583(10) . ?
Ti1 S1 2.5765(9) . ?
Ti1 S5 2.5766(10) . ?
Ti1 S4 2.5771(10) . ?
S5 C3 1.707(3) . ?
S6 C3 1.721(3) . ?
S3 C2 1.720(3) . ?
S4 C2 1.700(3) . ?
S2 C1 1.711(3) . ?
S1 C1 1.718(3) . ?
O1 C36 1.440(5) . ?
O1 C36A 1.482(17) . ?
N3 C3 1.313(4) . ?
N3 C7 1.477(4) . ?
N3 C4 1.478(4) . ?
N2 C2 1.319(4) . ?
N2 C31 1.477(4) . ?
N2 C8 1.478(4) . ?
N1 C1 1.323(4) . ?
N1 C32 1.471(4) . ?
N1 C35 1.478(4) . ?
C4 C5 1.518(5) . ?
C5 C6 1.498(5) . ?
C6 C7 1.522(5) . ?
C8 C9 1.511(5) . ?
C9 C30 1.520(5) . ?
C30 C31 1.522(5) . ?
C32 C33 1.515(5) . ?
C33 C34 1.530(5) . ?
C34 C35 1.517(5) . ?
C36 C37 1.505(7) . ?
C36 C38 1.538(6) . ?
