#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:56:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178761 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/15/4101517.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_4101517
loop_
_publ_author_name
'Roger, Mathieu'
'Barros, Noémi'
'Arliguie, Thérèse'
'Thuéry, Pierre'
'Maron, Laurent'
'Ephritikhine, Michel'
_publ_section_title
;
 U(SMes*)n, (n = 3, 4) and Ln(SMes*)3 (Ln = La, Ce, Pr, Nd):
 lanthanide(III)/actinide(III) differentiation in agostic interactions
 and an unprecedented eta3 ligation mode of the arylthiolate ligand,
 from X-ray diffraction and DFT analysis.
;
_journal_issue                   27
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8790
_journal_page_last               8802
_journal_paper_doi               10.1021/ja0584830
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C90 H134 S4 U'
_chemical_formula_weight         1582.24
_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     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.758(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9906(8)
_cell_length_b                   32.6564(19)
_cell_length_c                   19.4059(7)
_cell_measurement_reflns_used    26639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.73
_cell_volume                     8443.8(8)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Kappa-CCD software (Nonius B.V., 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'φ scans with 2° steps'
_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  0.0682
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26639
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    2.063
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.588
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'opaque dark brown'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0340
_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)+(0.0123P)²+14.3932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0735
_reflns_number_gt                6408
_reflns_number_total             7392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0584830si20060516_095639.cif
_cod_data_source_block           4.3C~6~H~6~
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4101517
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U U 0.5000 0.633516(6) 0.2500 0.02527(7) Uani 1 2 d S
S1 S 0.36584(7) 0.58739(3) 0.15984(5) 0.0321(2) Uani 1 1 d .
S2 S 0.50677(7) 0.68963(3) 0.15443(5) 0.0285(2) Uani 1 1 d .
C1 C 0.3259(3) 0.53920(11) 0.18722(18) 0.0280(8) Uani 1 1 d .
C2 C 0.2740(3) 0.53812(11) 0.23996(19) 0.0295(8) Uani 1 1 d .
C3 C 0.2480(3) 0.49978(11) 0.26114(18) 0.0297(8) Uani 1 1 d .
H3 H 0.2159 0.4987 0.2966 0.036 Uiso 1 1 calc R
C4 C 0.2681(3) 0.46331(11) 0.23132(18) 0.0291(8) Uani 1 1 d .
C5 C 0.3148(3) 0.46602(11) 0.17795(19) 0.0294(8) Uani 1 1 d .
H5 H 0.3278 0.4418 0.1571 0.035 Uiso 1 1 calc R
C6 C 0.3433(3) 0.50278(11) 0.15361(18) 0.0284(8) Uani 1 1 d .
C7 C 0.2424(3) 0.57641(12) 0.2741(2) 0.0335(9) Uani 1 1 d .
C8 C 0.3313(3) 0.60598(12) 0.3094(2) 0.0365(9) Uani 1 1 d .
H8A H 0.3259 0.6303 0.2775 0.055 Uiso 1 1 d R
H8B H 0.3939 0.5900 0.3203 0.055 Uiso 1 1 d R
H8C H 0.3243 0.6182 0.3537 0.055 Uiso 1 1 d R
C9 C 0.1593(3) 0.59909(13) 0.2158(2) 0.0430(10) Uani 1 1 d .
H9A H 0.1841 0.6067 0.1766 0.064 Uiso 1 1 calc R
H9B H 0.1399 0.6232 0.2365 0.064 Uiso 1 1 calc R
H9C H 0.1022 0.5814 0.1980 0.064 Uiso 1 1 calc R
C10 C 0.1985(4) 0.56551(13) 0.3356(2) 0.0483(11) Uani 1 1 d .
H10A H 0.1393 0.5491 0.3167 0.073 Uiso 1 1 calc R
H10B H 0.1815 0.5902 0.3561 0.073 Uiso 1 1 calc R
H10C H 0.2473 0.5504 0.3724 0.073 Uiso 1 1 calc R
C11 C 0.2367(3) 0.42225(12) 0.2566(2) 0.0367(9) Uani 1 1 d .
C12 C 0.1229(3) 0.42226(15) 0.2421(2) 0.0539(12) Uani 1 1 d .
H12A H 0.0902 0.4263 0.1913 0.081 Uiso 1 1 calc R
H12B H 0.1048 0.4440 0.2689 0.081 Uiso 1 1 calc R
H12C H 0.1025 0.3965 0.2568 0.081 Uiso 1 1 calc R
C13 C 0.2872(3) 0.41735(14) 0.3382(2) 0.0469(11) Uani 1 1 d .
H13A H 0.2687 0.3914 0.3538 0.070 Uiso 1 1 calc R
H13B H 0.2656 0.4390 0.3635 0.070 Uiso 1 1 calc R
H13C H 0.3587 0.4185 0.3485 0.070 Uiso 1 1 calc R
C14 C 0.2656(5) 0.38592(13) 0.2182(3) 0.0696(17) Uani 1 1 d .
H14A H 0.3373 0.3852 0.2287 0.104 Uiso 1 1 calc R
H14B H 0.2348 0.3886 0.1669 0.104 Uiso 1 1 calc R
H14C H 0.2432 0.3611 0.2347 0.104 Uiso 1 1 calc R
C15 C 0.3890(3) 0.50028(12) 0.0902(2) 0.0336(9) Uani 1 1 d .
C16 C 0.3256(3) 0.52507(12) 0.0238(2) 0.0378(9) Uani 1 1 d .
H16A H 0.3273 0.5536 0.0363 0.057 Uiso 1 1 calc R
H16B H 0.2574 0.5155 0.0098 0.057 Uiso 1 1 calc R
H16C H 0.3527 0.5215 -0.0156 0.057 Uiso 1 1 calc R
C17 C 0.4982(3) 0.51478(14) 0.1143(2) 0.0456(10) Uani 1 1 d .
H17A H 0.5356 0.4994 0.1560 0.068 Uiso 1 1 calc R
H17B H 0.5006 0.5434 0.1263 0.068 Uiso 1 1 calc R
H17C H 0.5268 0.5106 0.0758 0.068 Uiso 1 1 calc R
C18 C 0.3902(4) 0.45607(12) 0.0626(2) 0.0444(11) Uani 1 1 d .
H18A H 0.4197 0.4558 0.0239 0.067 Uiso 1 1 calc R
H18B H 0.3228 0.4458 0.0452 0.067 Uiso 1 1 calc R
H18C H 0.4290 0.4390 0.1014 0.067 Uiso 1 1 calc R
C19 C 0.6104(3) 0.69483(10) 0.11824(18) 0.0252(7) Uani 1 1 d .
C20 C 0.7027(3) 0.71183(10) 0.16125(18) 0.0266(8) Uani 1 1 d .
C21 C 0.7861(3) 0.70651(11) 0.13681(19) 0.0281(8) Uani 1 1 d .
H21 H 0.8478 0.7164 0.1655 0.034 Uiso 1 1 calc R
C22 C 0.7821(3) 0.68738(11) 0.07243(19) 0.0290(8) Uani 1 1 d .
C23 C 0.6877(3) 0.67578(10) 0.02789(19) 0.0274(8) Uani 1 1 d .
H23 H 0.6827 0.6650 -0.0174 0.033 Uiso 1 1 calc R
C24 C 0.6000(3) 0.67954(10) 0.04765(18) 0.0264(8) Uani 1 1 d .
C25 C 0.7184(3) 0.73699(11) 0.23225(18) 0.0287(8) Uani 1 1 d .
C26 C 0.8184(3) 0.76102(12) 0.2526(2) 0.0381(9) Uani 1 1 d .
H26A H 0.8221 0.7788 0.2927 0.057 Uiso 1 1 calc R
H26B H 0.8217 0.7771 0.2119 0.057 Uiso 1 1 calc R
H26C H 0.8736 0.7421 0.2658 0.057 Uiso 1 1 calc R
C27 C 0.6361(3) 0.76958(11) 0.2231(2) 0.0351(9) Uani 1 1 d .
H27A H 0.5724 0.7564 0.2151 0.053 Uiso 1 1 calc R
H27B H 0.6338 0.7867 0.1823 0.053 Uiso 1 1 calc R
H27C H 0.6508 0.7861 0.2660 0.053 Uiso 1 1 calc R
C28 C 0.7237(3) 0.70917(12) 0.2970(2) 0.0352(9) Uani 1 1 d .
H28A H 0.7381 0.7254 0.3402 0.053 Uiso 1 1 calc R
H28B H 0.7758 0.6892 0.3022 0.053 Uiso 1 1 calc R
H28C H 0.6605 0.6955 0.2891 0.053 Uiso 1 1 calc R
C29 C 0.8743(3) 0.68160(12) 0.0461(2) 0.0332(9) Uani 1 1 d .
C30 C 0.9716(3) 0.69410(19) 0.1034(2) 0.0650(15) Uani 1 1 d .
H30A H 0.9824 0.6768 0.1452 0.097 Uiso 1 1 calc R
H30B H 0.9668 0.7221 0.1170 0.097 Uiso 1 1 calc R
H30C H 1.0268 0.6912 0.0841 0.097 Uiso 1 1 calc R
C31 C 0.8816(4) 0.63756(14) 0.0231(3) 0.0624(14) Uani 1 1 d .
H31A H 0.9364 0.6350 0.0033 0.094 Uiso 1 1 calc R
H31B H 0.8202 0.6299 -0.0128 0.094 Uiso 1 1 calc R
H31C H 0.8929 0.6199 0.0644 0.094 Uiso 1 1 calc R
C32 C 0.8625(3) 0.70885(14) -0.0203(2) 0.0485(11) Uani 1 1 d .
H32A H 0.9198 0.7056 -0.0371 0.073 Uiso 1 1 calc R
H32B H 0.8572 0.7370 -0.0075 0.073 Uiso 1 1 calc R
H32C H 0.8029 0.7011 -0.0580 0.073 Uiso 1 1 calc R
C33 C 0.4992(3) 0.66808(11) -0.00969(18) 0.0293(8) Uani 1 1 d .
C34 C 0.5119(3) 0.66203(13) -0.08515(19) 0.0367(9) Uani 1 1 d .
H34A H 0.5543 0.6388 -0.0842 0.055 Uiso 1 1 calc R
H34B H 0.5420 0.6861 -0.0982 0.055 Uiso 1 1 calc R
H34C H 0.4474 0.6575 -0.1200 0.055 Uiso 1 1 calc R
C35 C 0.4570(3) 0.62780(11) 0.0095(2) 0.0359(9) Uani 1 1 d .
H35A H 0.3961 0.6210 -0.0279 0.054 Uiso 1 1 calc R
H35B H 0.4431 0.6308 0.0547 0.054 Uiso 1 1 calc R
H35C H 0.5052 0.6063 0.0135 0.054 Uiso 1 1 calc R
C36 C 0.4225(3) 0.70291(12) -0.0186(2) 0.0343(9) Uani 1 1 d .
H36A H 0.3612 0.6955 -0.0548 0.051 Uiso 1 1 calc R
H36B H 0.4489 0.7275 -0.0331 0.051 Uiso 1 1 calc R
H36C H 0.4096 0.7075 0.0266 0.051 Uiso 1 1 calc R
C37 C 0.4088(3) 0.12287(13) 0.5792(2) 0.0438(10) Uani 1 1 d .
H37 H 0.4353 0.0985 0.6020 0.053 Uiso 1 1 calc R
C38 C 0.4338(3) 0.15979(14) 0.6155(2) 0.0442(10) Uani 1 1 d .
H38 H 0.4770 0.1601 0.6627 0.053 Uiso 1 1 calc R
C39 C 0.3951(3) 0.19591(13) 0.5820(2) 0.0395(10) Uani 1 1 d .
H39 H 0.4117 0.2206 0.6065 0.047 Uiso 1 1 calc R
C40 C 0.3314(3) 0.19525(12) 0.5118(2) 0.0380(9) Uani 1 1 d .
H40 H 0.3058 0.2196 0.4887 0.046 Uiso 1 1 calc R
C41 C 0.3057(3) 0.15839(13) 0.4759(2) 0.0377(9) Uani 1 1 d .
H41 H 0.2619 0.1580 0.4289 0.045 Uiso 1 1 calc R
C42 C 0.3448(3) 0.12224(12) 0.5095(2) 0.0365(9) Uani 1 1 d .
H42 H 0.3280 0.0975 0.4851 0.044 Uiso 1 1 calc R
C43 C 0.0017(3) 0.46448(14) 0.5383(2) 0.0512(12) Uani 1 1 d .
H43A H 0.0029 0.4404 0.5642 0.061 Uiso 1 1 calc R
C44 C 0.0663(3) 0.49621(13) 0.5687(2) 0.0471(11) Uani 1 1 d .
H44 H 0.1110 0.4935 0.6151 0.057 Uiso 1 1 calc R
C45 C 0.0643(3) 0.53152(14) 0.5304(2) 0.0480(11) Uani 1 1 d .
H45A H 0.1076 0.5529 0.5508 0.058 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 '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
S1 U S1 109.73(4) . 2_655
S1 U S2 95.87(3) . .
S1 U S2 134.41(3) 2_655 .
S1 U S2 134.41(3) . 2_655
S1 U S2 95.87(3) 2_655 2_655
S2 U S2 91.64(4) . 2_655
C1 S1 U 121.92(12) . .
C19 S2 U 123.17(11) . .
C6 C1 C2 120.6(3) . .
C6 C1 S1 119.0(3) . .
C2 C1 S1 120.3(3) . .
C3 C2 C1 117.9(3) . .
C3 C2 C7 117.7(3) . .
C1 C2 C7 124.4(3) . .
C4 C3 C2 122.7(3) . .
C5 C4 C3 117.3(3) . .
C5 C4 C11 122.7(3) . .
C3 C4 C11 120.0(3) . .
C4 C5 C6 123.9(3) . .
C5 C6 C1 117.5(3) . .
C5 C6 C15 117.0(3) . .
C1 C6 C15 125.5(3) . .
C2 C7 C10 112.3(3) . .
C2 C7 C9 108.9(3) . .
C10 C7 C9 106.8(3) . .
C2 C7 C8 113.4(3) . .
C10 C7 C8 104.8(3) . .
C9 C7 C8 110.3(3) . .
C14 C11 C12 109.1(4) . .
C14 C11 C13 108.5(4) . .
C12 C11 C13 108.4(3) . .
C14 C11 C4 112.3(3) . .
C12 C11 C4 108.9(3) . .
C13 C11 C4 109.5(3) . .
C17 C15 C18 106.3(3) . .
C17 C15 C16 111.0(3) . .
C18 C15 C16 105.3(3) . .
C17 C15 C6 110.8(3) . .
C18 C15 C6 112.1(3) . .
C16 C15 C6 111.2(3) . .
C20 C19 C24 120.7(3) . .
C20 C19 S2 120.2(3) . .
C24 C19 S2 119.0(3) . .
C21 C20 C19 117.1(3) . .
C21 C20 C25 117.2(3) . .
C19 C20 C25 125.6(3) . .
C22 C21 C20 123.7(3) . .
C21 C22 C23 116.9(3) . .
C21 C22 C29 123.3(3) . .
C23 C22 C29 119.6(3) . .
C22 C23 C24 123.5(3) . .
C23 C24 C19 117.0(3) . .
C23 C24 C33 117.6(3) . .
C19 C24 C33 125.3(3) . .
C28 C25 C27 110.6(3) . .
C28 C25 C26 106.1(3) . .
C27 C25 C26 105.4(3) . .
C28 C25 C20 111.7(3) . .
C27 C25 C20 111.3(3) . .
C26 C25 C20 111.4(3) . .
C31 C29 C30 110.0(4) . .
C31 C29 C32 107.6(4) . .
C30 C29 C32 107.5(4) . .
C31 C29 C22 110.6(3) . .
C30 C29 C22 112.1(3) . .
C32 C29 C22 108.8(3) . .
C35 C33 C36 110.8(3) . .
C35 C33 C34 106.6(3) . .
C36 C33 C34 105.5(3) . .
C35 C33 C24 111.5(3) . .
C36 C33 C24 110.6(3) . .
C34 C33 C24 111.7(3) . .
C42 C37 C38 120.0(4) . .
C39 C38 C37 120.2(4) . .
C38 C39 C40 119.7(4) . .
C39 C40 C41 120.1(4) . .
C42 C41 C40 120.1(4) . .
C37 C42 C41 119.9(4) . .
C45 C43 C44 120.0(4) 5_566 .
C45 C44 C43 119.8(4) . .
C44 C45 C43 120.2(4) . 5_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U S1 2.6173(9) .
U S1 2.6173(9) 2_655
U S2 2.6294(9) .
U S2 2.6295(9) 2_655
U H8A 2.6498 .
U H8B 2.7045 .
U C8 3.061(4) 2_655
U C8 3.061(4) .
S1 C1 1.804(4) .
S2 C19 1.801(3) .
C1 C6 1.413(5) .
C1 C2 1.424(5) .
C2 C3 1.400(5) .
C2 C7 1.542(5) .
C3 C4 1.390(5) .
C4 C5 1.385(5) .
C4 C11 1.537(5) .
C5 C6 1.393(5) .
C6 C15 1.552(5) .
C7 C10 1.542(5) .
C7 C9 1.542(6) .
C7 C8 1.558(5) .
C11 C14 1.520(6) .
C11 C12 1.529(6) .
C11 C13 1.533(5) .
C15 C17 1.530(6) .
C15 C18 1.542(5) .
C15 C16 1.550(5) .
C19 C20 1.420(5) .
C19 C24 1.423(5) .
C20 C21 1.399(5) .
C20 C25 1.561(5) .
C21 C22 1.383(5) .
C22 C23 1.393(5) .
C22 C29 1.537(5) .
C23 C24 1.397(5) .
C24 C33 1.552(5) .
C25 C28 1.534(5) .
C25 C27 1.538(5) .
C25 C26 1.547(5) .
C29 C31 1.518(6) .
C29 C30 1.527(6) .
C29 C32 1.533(5) .
C33 C35 1.534(5) .
C33 C36 1.537(5) .
C33 C34 1.541(5) .
C37 C42 1.376(6) .
C37 C38 1.386(6) .
C38 C39 1.376(6) .
C39 C40 1.382(6) .
C40 C41 1.383(6) .
C41 C42 1.379(6) .
C43 C45 1.377(6) 5_566
C43 C44 1.383(6) .
C44 C45 1.368(6) .
C45 C43 1.377(6) 5_566
