#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:31:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179451 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/48/4334885.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_4334885
loop_
_publ_author_name
'Fabrice Pointillart'
'Boris Le Guennic'
'Thomas Cauchy'
'Stéphane Golhen'
'Olivier Cador'
'Olivier Maury'
'Lahcène Ouahab'
_publ_section_title
;
 A Series of Tetrathiafulvalene-Based Lanthanide Complexes Displaying
 Either Single Molecule Magnet or Luminescence-Direct Magnetic and
 Photo-Physical Correlations in the Ytterbium Analogue
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5978
_journal_page_last               5990
_journal_paper_doi               10.1021/ic400253m
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C20 H20 N2 O3 S8'
_chemical_formula_weight         592.0
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                82.012(2)
_cell_angle_beta                 80.795(2)
_cell_angle_gamma                77.391(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3312(3)
_cell_length_b                   9.1008(2)
_cell_length_c                   17.5597(7)
_cell_measurement_reflns_used    5439
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      33.142
_cell_measurement_theta_min      0.998
_cell_volume                     1275.04(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13472
_diffrn_reflns_theta_full        33.21
_diffrn_reflns_theta_max         33.21
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.871
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       plate
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         9644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.0699
_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)+(0.1361P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2535
_reflns_number_gt                4629
_reflns_number_total             9644
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400253m_si_002_1.cif
_cod_data_source_block           import-meslr2
_cod_original_cell_volume        1275.04(7)
_cod_database_code               4334885
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O3W O 1.1827(6) 0.4897(5) 0.0527(3) 0.1341(15) Uani 1 1 d .
S5 S 0.23649(11) 0.79640(8) 0.35946(5) 0.0526(2) Uani 1 1 d .
S4 S 0.28410(10) 0.93962(8) 0.51416(5) 0.0506(2) Uani 1 1 d .
S3 S 0.10533(10) 1.23751(8) 0.44960(5) 0.0515(2) Uani 1 1 d .
S6 S 0.06186(11) 1.09839(8) 0.29897(5) 0.0538(2) Uani 1 1 d .
S8 S 0.17143(10) 0.64910(9) 0.22398(5) 0.0537(2) Uani 1 1 d .
S2 S 0.13199(11) 1.39051(8) 0.58683(5) 0.0546(2) Uani 1 1 d .
S1 S 0.34208(12) 1.07104(9) 0.65572(5) 0.0580(2) Uani 1 1 d .
S7 S -0.02366(11) 0.97837(10) 0.16173(5) 0.0610(2) Uani 1 1 d .
C8 C 0.1554(3) 0.8097(3) 0.27199(17) 0.0434(6) Uani 1 1 d .
C4 C 0.2572(3) 1.0924(3) 0.56935(17) 0.0423(6) Uani 1 1 d .
C3 C 0.1750(3) 1.2270(3) 0.53978(16) 0.0439(6) Uani 1 1 d .
C7 C 0.0755(3) 0.9467(3) 0.24454(17) 0.0468(6) Uani 1 1 d .
C6 C 0.1639(4) 0.9878(3) 0.37419(17) 0.0447(6) Uani 1 1 d .
N2 N 0.5340(3) 0.4001(3) 0.18046(15) 0.0540(6) Uani 1 1 d .
C5 C 0.1817(4) 1.0454(3) 0.43811(17) 0.0448(6) Uani 1 1 d .
C16 C 0.4873(4) 0.4854(3) 0.24163(18) 0.0485(7) Uani 1 1 d .
N1 N 0.3188(3) 0.8413(3) 0.04226(15) 0.0558(6) Uani 1 1 d .
O1 O 0.1979(3) 0.8168(3) 0.00883(16) 0.0763(8) Uani 1 1 d .
C10 C 0.2937(4) 0.9622(3) 0.08322(18) 0.0531(7) Uani 1 1 d .
C9 C 0.1241(4) 1.0610(4) 0.0905(2) 0.0617(8) Uani 1 1 d .
H9A H 0.0841 1.0788 0.0404 0.074 Uiso 1 1 calc R
H9B H 0.1311 1.1581 0.1051 0.074 Uiso 1 1 calc R
O2 O 0.4230(4) 0.3422(3) 0.15613(17) 0.0772(7) Uani 1 1 d .
C15 C 0.3107(4) 0.5014(3) 0.2774(2) 0.0563(8) Uani 1 1 d .
H15A H 0.3011 0.5252 0.3303 0.068 Uiso 1 1 calc R
H15B H 0.2766 0.4055 0.2793 0.068 Uiso 1 1 calc R
C17 C 0.6040(5) 0.5465(4) 0.2660(2) 0.0645(9) Uani 1 1 d .
H17 H 0.5730 0.6062 0.3069 0.077 Uiso 1 1 calc R
C20 C 0.6956(5) 0.3744(4) 0.1460(2) 0.0674(9) Uani 1 1 d .
H20 H 0.7270 0.3149 0.1050 0.081 Uiso 1 1 calc R
C11 C 0.4215(5) 0.9853(4) 0.1174(2) 0.0664(9) Uani 1 1 d .
H11 H 0.4052 1.0673 0.1460 0.080 Uiso 1 1 calc R
C14 C 0.4684(5) 0.7459(4) 0.0340(2) 0.0673(9) Uani 1 1 d .
H14 H 0.4842 0.6643 0.0053 0.081 Uiso 1 1 calc R
C19 C 0.8105(5) 0.4352(5) 0.1709(3) 0.0768(11) Uani 1 1 d .
H19 H 0.9198 0.4178 0.1468 0.092 Uiso 1 1 calc R
C13 C 0.5955(5) 0.7691(5) 0.0676(2) 0.0754(11) Uani 1 1 d .
H13 H 0.6979 0.7031 0.0617 0.090 Uiso 1 1 calc R
C12 C 0.5741(5) 0.8882(5) 0.1100(3) 0.0795(11) Uani 1 1 d .
H12 H 0.6607 0.9037 0.1335 0.095 Uiso 1 1 calc R
C1 C 0.4260(5) 0.8738(4) 0.6704(2) 0.0720(10) Uani 1 1 d .
H1C H 0.4760 0.8516 0.7174 0.108 Uiso 1 1 calc R
H1B H 0.5084 0.8450 0.6274 0.108 Uiso 1 1 calc R
H1A H 0.3389 0.8182 0.6745 0.108 Uiso 1 1 calc R
C18 C 0.7660(5) 0.5217(5) 0.2313(3) 0.0796(11) Uani 1 1 d .
H18 H 0.8442 0.5633 0.2487 0.096 Uiso 1 1 calc R
C2 C 0.2906(5) 1.4845(4) 0.5356(3) 0.0794(11) Uani 1 1 d .
H2A H 0.2820 1.5787 0.5562 0.119 Uiso 1 1 calc R
H2B H 0.2776 1.5038 0.4816 0.119 Uiso 1 1 calc R
H2C H 0.3974 1.4216 0.5416 0.119 Uiso 1 1 calc R
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'
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
C8 S5 C6 95.54(13)
C5 S4 C4 95.28(13)
C5 S3 C3 94.79(13)
C6 S6 C7 95.27(13)
C8 S8 C15 103.49(14)
C3 S2 C2 100.34(17)
C4 S1 C1 103.85(16)
C7 S7 C9 101.64(15)
C7 C8 S5 117.3(2)
C7 C8 S8 121.3(2)
S5 C8 S8 121.35(16)
C3 C4 S1 122.0(2)
C3 C4 S4 116.7(2)
S1 C4 S4 121.19(16)
C4 C3 S2 123.5(2)
C4 C3 S3 118.1(2)
S2 C3 S3 118.43(15)
C8 C7 S7 123.4(2)
C8 C7 S6 117.3(2)
S7 C7 S6 119.15(16)
C5 C6 S5 123.1(2)
C5 C6 S6 122.5(2)
S5 C6 S6 114.44(15)
O2 N2 C16 119.3(3)
O2 N2 C20 120.7(3)
C16 N2 C20 120.0(3)
C6 C5 S3 120.9(2)
C6 C5 S4 124.0(2)
S3 C5 S4 115.13(16)
C17 C16 N2 118.7(3)
C17 C16 C15 125.2(3)
N2 C16 C15 116.0(3)
O1 N1 C14 119.1(3)
O1 N1 C10 120.1(3)
C14 N1 C10 120.8(3)
N1 C10 C11 119.0(3)
N1 C10 C9 117.5(3)
C11 C10 C9 123.4(3)
C10 C9 S7 112.7(2)
C16 C15 S8 112.6(2)
C16 C17 C18 121.4(3)
C19 C20 N2 120.7(3)
C10 C11 C12 120.7(4)
N1 C14 C13 120.2(3)
C20 C19 C18 120.1(4)
C14 C13 C12 120.6(4)
C13 C12 C11 118.6(4)
C19 C18 C17 119.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S5 C8 1.753(3)
S5 C6 1.756(3)
S4 C5 1.757(3)
S4 C4 1.758(3)
S3 C5 1.754(3)
S3 C3 1.755(3)
S6 C6 1.759(3)
S6 C7 1.760(3)
S8 C8 1.757(3)
S8 C15 1.831(3)
S2 C3 1.743(3)
S2 C2 1.785(4)
S1 C4 1.743(3)
S1 C1 1.778(3)
S7 C7 1.744(3)
S7 C9 1.816(4)
C8 C7 1.343(4)
C4 C3 1.346(4)
C6 C5 1.344(4)
N2 O2 1.310(3)
N2 C16 1.369(4)
N2 C20 1.370(4)
C16 C17 1.368(4)
C16 C15 1.489(4)
N1 O1 1.316(3)
N1 C14 1.354(4)
N1 C10 1.357(4)
C10 C11 1.370(5)
C10 C9 1.497(4)
C17 C18 1.373(5)
C20 C19 1.360(5)
C11 C12 1.379(6)
C14 C13 1.358(5)
C19 C18 1.363(6)
C13 C12 1.364(6)
