#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:49:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179265 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/85/4318582.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_4318582
loop_
_publ_author_name
'A. Otero'
'J. Fernández-Baeza'
'A. Antiñolo'
'F. Carrillo-Hermosilla'
'J. Tejeda'
'A. Lara-Sánchez'
'L. Sánchez-Barba'
'M. Fernández-López'
'A. M. Rodríguez'
'I. López-Solera'
_publ_section_title
;
 Preparation of New Monoanionic "Scorpionate" Ligands: Synthesis and
 Structural Characterization of Titanium(IV) Complexes Bearing This Class
 of Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5193
_journal_page_last               5202
_journal_paper_doi               10.1021/ic020319f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H41 Li N4 O3 S2'
_chemical_formula_weight         696.83
_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                 104.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.048(3)
_cell_length_b                   23.701(9)
_cell_length_c                   14.659(4)
_cell_measurement_temperature    220(2)
_cell_volume                     3717(2)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XCAD4 (Harms, Wocadlo, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       'ω/2θ 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  0.0887
_diffrn_reflns_av_sigmaI/netI    0.2427
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9733
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.09
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.186
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         9269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.2440
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0518P)²+1.0927P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                2418
_reflns_number_total             9269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020319f_2.cif
_cod_data_source_block           3
_cod_database_code               4318582
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
S1 S 0.15789(19) 0.11669(9) 0.56142(15) 0.0390(6) Uani 1 1 d . . .
S2 S 0.27387(19) 0.00950(9) 0.64912(16) 0.0449(7) Uani 1 1 d . . .
O1 O -0.0338(7) -0.0245(3) 0.5899(4) 0.055(2) Uani 1 1 d . . .
Li1 Li -0.0485(12) 0.0137(5) 0.6965(9) 0.038(3) Uani 1 1 d . . .
N1 N 0.1080(5) 0.0105(2) 0.8077(4) 0.0299(16) Uani 1 1 d . . .
N2 N 0.1977(5) 0.0509(3) 0.8190(4) 0.0307(16) Uani 1 1 d . . .
N3 N -0.0376(5) 0.1011(2) 0.6984(4) 0.0289(16) Uani 1 1 d . . .
N4 N 0.0745(5) 0.1266(2) 0.7361(4) 0.0254(15) Uani 1 1 d . . .
C1 C 0.1393(7) -0.0217(3) 0.8862(5) 0.028(2) Uani 1 1 d . . .
C2 C 0.2503(7) 0.0001(3) 0.9467(5) 0.038(2) Uani 1 1 d . . .
H2 H 0.2916 -0.0140 1.0054 0.046 Uiso 1 1 calc . . .
C3 C 0.2844(7) 0.0453(3) 0.9030(5) 0.033(2) Uani 1 1 d . . .
C4 C 0.0647(7) 0.1827(3) 0.7535(5) 0.031(2) Uani 1 1 d . . .
C5 C -0.0616(7) 0.1938(3) 0.7246(5) 0.037(2) Uani 1 1 d . . .
H5 H -0.1000 0.2283 0.7278 0.044 Uiso 1 1 calc . . .
C6 C -0.1208(7) 0.1435(3) 0.6898(5) 0.030(2) Uani 1 1 d . . .
C7 C 0.1889(6) 0.0928(3) 0.7465(5) 0.0242(19) Uani 1 1 d . . .
H7 H 0.2585 0.1189 0.7702 0.029 Uiso 1 1 calc . . .
C8 C 0.2049(6) 0.0714(3) 0.6498(5) 0.0226(18) Uani 1 1 d . . .
C20 C 0.0651(7) -0.0698(3) 0.9005(6) 0.033(2) Uani 1 1 d . . .
C21 C 0.0088(7) -0.1051(3) 0.8249(5) 0.036(2) Uani 1 1 d . . .
H21 H 0.0205 -0.0981 0.7653 0.043 Uiso 1 1 calc . . .
C22 C -0.0629(8) -0.1494(3) 0.8383(7) 0.055(3) Uani 1 1 d . . .
H22 H -0.1008 -0.1719 0.7871 0.066 Uiso 1 1 calc . . .
C23 C -0.0809(9) -0.1619(4) 0.9257(7) 0.063(3) Uani 1 1 d . . .
H23 H -0.1290 -0.1927 0.9344 0.076 Uiso 1 1 calc . . .
C24 C -0.0256(9) -0.1273(4) 1.0001(7) 0.076(3) Uani 1 1 d . . .
H24 H -0.0366 -0.1348 1.0597 0.091 Uiso 1 1 calc . . .
C25 C 0.0453(8) -0.0820(4) 0.9871(6) 0.051(3) Uani 1 1 d . . .
H25 H 0.0809 -0.0590 1.0382 0.061 Uiso 1 1 calc . . .
C30 C 0.3950(7) 0.0835(3) 0.9333(6) 0.034(2) Uani 1 1 d . . .
C31 C 0.4141(8) 0.1079(4) 1.0223(6) 0.057(3) Uani 1 1 d . . .
H31 H 0.3575 0.1016 1.0587 0.069 Uiso 1 1 calc . . .
C32 C 0.5176(10) 0.1413(5) 1.0559(8) 0.084(4) Uani 1 1 d . . .
H32 H 0.5305 0.1578 1.1150 0.101 Uiso 1 1 calc . . .
C33 C 0.6004(9) 0.1502(4) 1.0039(8) 0.073(4) Uani 1 1 d . . .
H33 H 0.6708 0.1721 1.0285 0.088 Uiso 1 1 calc . . .
C34 C 0.5832(7) 0.1275(4) 0.9149(7) 0.056(3) Uani 1 1 d . . .
H34 H 0.6403 0.1345 0.8792 0.068 Uiso 1 1 calc . . .
C35 C 0.4774(7) 0.0936(3) 0.8794(6) 0.045(2) Uani 1 1 d . . .
H35 H 0.4635 0.0782 0.8194 0.054 Uiso 1 1 calc . . .
C40 C 0.1725(7) 0.2187(3) 0.7938(6) 0.032(2) Uani 1 1 d . . .
C41 C 0.1803(7) 0.2461(3) 0.8778(6) 0.042(2) Uani 1 1 d . . .
H41 H 0.1159 0.2415 0.9077 0.050 Uiso 1 1 calc . . .
C42 C 0.2810(9) 0.2804(4) 0.9195(6) 0.058(3) Uani 1 1 d . . .
H42 H 0.2832 0.2990 0.9757 0.070 Uiso 1 1 calc . . .
C43 C 0.3775(8) 0.2862(4) 0.8761(7) 0.058(3) Uani 1 1 d . . .
H43 H 0.4474 0.3077 0.9038 0.070 Uiso 1 1 calc . . .
C44 C 0.3691(8) 0.2601(4) 0.7921(7) 0.058(3) Uani 1 1 d . . .
H44 H 0.4328 0.2651 0.7617 0.070 Uiso 1 1 calc . . .
C45 C 0.2684(7) 0.2263(3) 0.7507(5) 0.035(2) Uani 1 1 d . . .
H45 H 0.2655 0.2087 0.6935 0.042 Uiso 1 1 calc . . .
C50 C -0.2536(6) 0.1317(3) 0.6483(5) 0.029(2) Uani 1 1 d . . .
C51 C -0.3468(7) 0.1639(3) 0.6715(6) 0.046(2) Uani 1 1 d . . .
H51 H -0.3248 0.1937 0.7136 0.055 Uiso 1 1 calc . . .
C52 C -0.4716(7) 0.1522(4) 0.6330(7) 0.059(3) Uani 1 1 d . . .
H52 H -0.5331 0.1737 0.6497 0.071 Uiso 1 1 calc . . .
C53 C -0.5040(7) 0.1089(4) 0.5703(6) 0.050(3) Uani 1 1 d . . .
H53 H -0.5880 0.1004 0.5456 0.060 Uiso 1 1 calc . . .
C54 C -0.4149(7) 0.0780(4) 0.5433(5) 0.045(2) Uani 1 1 d . . .
H54 H -0.4381 0.0495 0.4987 0.054 Uiso 1 1 calc . . .
C55 C -0.2894(7) 0.0892(4) 0.5824(6) 0.043(2) Uani 1 1 d . . .
H55 H -0.2287 0.0678 0.5642 0.052 Uiso 1 1 calc . . .
O60 O -0.2008(4) -0.0166(2) 0.7209(4) 0.0400(15) Uani 1 1 d . . .
C61 C -0.2545(8) 0.0011(4) 0.7945(6) 0.053(2) Uani 1 1 d . . .
H61A H -0.2514 0.0418 0.8008 0.064 Uiso 1 1 calc . . .
H61B H -0.2105 -0.0155 0.8541 0.064 Uiso 1 1 calc . . .
C62 C -0.3875(8) -0.0192(4) 0.7663(6) 0.060(3) Uani 1 1 d . . .
H62A H -0.4192 -0.0266 0.8211 0.071 Uiso 1 1 calc . . .
H62B H -0.4411 0.0082 0.7265 0.071 Uiso 1 1 calc . . .
C63 C -0.3794(7) -0.0721(4) 0.7135(6) 0.059(3) Uani 1 1 d . . .
H63A H -0.4585 -0.0807 0.6692 0.070 Uiso 1 1 calc . . .
H63B H -0.3548 -0.1038 0.7559 0.070 Uiso 1 1 calc . . .
C64 C -0.2793(7) -0.0581(3) 0.6626(6) 0.043(2) Uani 1 1 d . . .
H64A H -0.2314 -0.0915 0.6560 0.052 Uiso 1 1 calc . . .
H64B H -0.3164 -0.0429 0.6005 0.052 Uiso 1 1 calc . . .
O70 O 0.6831(9) 0.2991(5) 0.8026(7) 0.161(5) Uani 1 1 d . . .
C71 C 0.7508(12) 0.3452(5) 0.8055(10) 0.122(5) Uani 1 1 d . . .
H71A H 0.7019 0.3780 0.8137 0.146 Uiso 1 1 calc . . .
H71B H 0.7752 0.3495 0.7468 0.146 Uiso 1 1 calc . . .
C72 C 0.8618(11) 0.3413(6) 0.8838(11) 0.122(5) Uani 1 1 d . . .
H72A H 0.8711 0.3745 0.9236 0.146 Uiso 1 1 calc . . .
H72B H 0.9367 0.3365 0.8614 0.146 Uiso 1 1 calc . . .
C73 C 0.8358(13) 0.2904(7) 0.9347(9) 0.124(5) Uani 1 1 d . . .
H73A H 0.8935 0.2602 0.9304 0.149 Uiso 1 1 calc . . .
H73B H 0.8435 0.2988 1.0007 0.149 Uiso 1 1 calc . . .
C74 C 0.7185(17) 0.2756(8) 0.8921(14) 0.190(9) Uani 1 1 d . . .
H74A H 0.6625 0.2885 0.9292 0.228 Uiso 1 1 calc . . .
H74B H 0.7125 0.2348 0.8874 0.228 Uiso 1 1 calc . . .
HA H -0.083(9) -0.061(4) 0.538(7) 0.13(4) Uiso 1 1 d . . .
HB H 0.023(7) -0.021(4) 0.571(6) 0.06(4) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 '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'
C C 0.0033 0.0016 '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'
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'
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 Li1 O60 103.7(6) . . ?
O1 Li1 N1 114.7(7) . . ?
O60 Li1 N1 115.8(7) . . ?
O1 Li1 N3 118.9(7) . . ?
O60 Li1 N3 114.6(7) . . ?
N1 Li1 N3 89.5(5) . . ?
C1 N1 N2 105.7(6) . . ?
C1 N1 Li1 132.8(6) . . ?
N2 N1 Li1 120.8(6) . . ?
N1 N2 C3 111.5(6) . . ?
N1 N2 C7 118.9(5) . . ?
C3 N2 C7 129.5(6) . . ?
C6 N3 N4 103.6(5) . . ?
C6 N3 Li1 135.1(6) . . ?
N4 N3 Li1 119.4(6) . . ?
C4 N4 N3 113.7(5) . . ?
C4 N4 C7 128.1(6) . . ?
N3 N4 C7 118.0(5) . . ?
N1 C1 C2 108.9(6) . . ?
N1 C1 C20 122.2(7) . . ?
C2 C1 C20 128.9(7) . . ?
C3 C2 C1 107.0(6) . . ?
C2 C3 N2 106.8(6) . . ?
C2 C3 C30 130.1(7) . . ?
N2 C3 C30 123.1(7) . . ?
N4 C4 C5 104.5(6) . . ?
N4 C4 C40 123.3(6) . . ?
C5 C4 C40 132.2(7) . . ?
C4 C5 C6 107.3(7) . . ?
N3 C6 C5 110.9(6) . . ?
N3 C6 C50 119.0(7) . . ?
C5 C6 C50 130.1(7) . . ?
N2 C7 N4 110.5(6) . . ?
N2 C7 C8 116.4(6) . . ?
N4 C7 C8 111.9(6) . . ?
C7 C8 S2 116.9(5) . . ?
C7 C8 S1 114.5(5) . . ?
S2 C8 S1 128.4(4) . . ?
C25 C20 C21 117.5(7) . . ?
C25 C20 C1 121.7(7) . . ?
C21 C20 C1 120.7(7) . . ?
C22 C21 C20 120.4(8) . . ?
C21 C22 C23 121.7(8) . . ?
C24 C23 C22 118.0(8) . . ?
C25 C24 C23 120.8(9) . . ?
C24 C25 C20 121.5(8) . . ?
C35 C30 C31 120.1(7) . . ?
C35 C30 C3 123.1(7) . . ?
C31 C30 C3 116.8(8) . . ?
C32 C31 C30 119.4(9) . . ?
C33 C32 C31 120.7(10) . . ?
C32 C33 C34 121.4(9) . . ?
C33 C34 C35 118.5(9) . . ?
C30 C35 C34 119.9(8) . . ?
C41 C40 C45 117.8(7) . . ?
C41 C40 C4 119.9(8) . . ?
C45 C40 C4 122.2(7) . . ?
C40 C41 C42 122.3(8) . . ?
C43 C42 C41 118.8(8) . . ?
C44 C43 C42 119.2(8) . . ?
C43 C44 C45 121.7(9) . . ?
C40 C45 C44 120.2(8) . . ?
C55 C50 C51 118.1(7) . . ?
C55 C50 C6 120.6(7) . . ?
C51 C50 C6 121.3(7) . . ?
C52 C51 C50 121.0(8) . . ?
C53 C52 C51 119.6(8) . . ?
C52 C53 C54 120.8(8) . . ?
C53 C54 C55 119.8(8) . . ?
C50 C55 C54 120.6(8) . . ?
C61 O60 C64 110.4(6) . . ?
C61 O60 Li1 125.3(6) . . ?
C64 O60 Li1 124.3(6) . . ?
O60 C61 C62 105.2(7) . . ?
C63 C62 C61 103.4(7) . . ?
C62 C63 C64 102.5(7) . . ?
O60 C64 C63 105.2(6) . . ?
C71 O70 C74 106.2(11) . . ?
O70 C71 C72 109.3(10) . . ?
C71 C72 C73 102.5(10) . . ?
C74 C73 C72 105.3(12) . . ?
C73 C74 O70 110.4(13) . . ?
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
S1 C8 1.663(7) . ?
S2 C8 1.655(7) . ?
O1 Li1 1.849(15) . ?
Li1 O60 1.943(13) . ?
Li1 N1 2.060(13) . ?
Li1 N3 2.074(13) . ?
N1 C1 1.351(8) . ?
N1 N2 1.359(7) . ?
N2 C3 1.364(8) . ?
N2 C7 1.440(8) . ?
N3 C6 1.347(8) . ?
N3 N4 1.365(7) . ?
N4 C4 1.363(8) . ?
N4 C7 1.472(8) . ?
C1 C2 1.419(9) . ?
C1 C20 1.449(10) . ?
C2 C3 1.349(9) . ?
C3 C30 1.497(10) . ?
C4 C5 1.378(9) . ?
C4 C40 1.465(9) . ?
C5 C6 1.393(9) . ?
C6 C50 1.468(9) . ?
C7 C8 1.556(9) . ?
C20 C25 1.373(10) . ?
C20 C21 1.404(10) . ?
C21 C22 1.359(10) . ?
C22 C23 1.378(11) . ?
C23 C24 1.378(12) . ?
C24 C25 1.371(11) . ?
C30 C35 1.368(10) . ?
C30 C31 1.394(10) . ?
C31 C32 1.377(11) . ?
C32 C33 1.346(14) . ?
C33 C34 1.379(13) . ?
C34 C35 1.406(11) . ?
C40 C41 1.375(10) . ?
C40 C45 1.375(9) . ?
C41 C42 1.390(11) . ?
C42 C43 1.378(12) . ?
C43 C44 1.361(11) . ?
C44 C45 1.381(10) . ?
C50 C55 1.384(10) . ?
C50 C51 1.389(10) . ?
C51 C52 1.381(10) . ?
C52 C53 1.363(11) . ?
C53 C54 1.364(11) . ?
C54 C55 1.387(9) . ?
O60 C61 1.419(9) . ?
O60 C64 1.442(8) . ?
C61 C62 1.502(11) . ?
C62 C63 1.488(11) . ?
C63 C64 1.518(10) . ?
O70 C71 1.319(12) . ?
O70 C74 1.388(15) . ?
C71 C72 1.459(14) . ?
C72 C73 1.485(16) . ?
C73 C74 1.337(16) . ?
