#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013750.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_7013750
loop_
_publ_author_name
'Mehdoui, Thouraya'
'Berthet, Jean-Claude'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Lanthanide(III)/actinide(III) differentiation in coordination of azine
 molecules to tris(cyclopentadienyl) complexes of cerium and uranium.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              579
_journal_page_last               590
_journal_paper_doi               10.1039/b313992a
_journal_year                    2004
_chemical_formula_sum            'C29 H44 N Si3 U'
_chemical_formula_weight         728.95
_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                98.747(6)
_cell_angle_beta                 109.359(8)
_cell_angle_gamma                97.321(6)
_cell_formula_units_Z            2
_cell_length_a                   11.1739(14)
_cell_length_b                   11.1737(15)
_cell_length_c                   13.7093(16)
_cell_measurement_reflns_used    10766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.96
_cell_volume                     1566.8(4)
_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)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       'φ 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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10766
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.96
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.312
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.822
_refine_diff_density_min         -2.915
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5488
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0521
_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)+(0.0550P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                4350
_reflns_number_total             5488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313992a.txt
_cod_data_source_block           (U,SiMe~3~,pyridine)
_cod_original_cell_volume        1566.8(3)
_cod_database_code               7013750
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
_atom_site_disorder_assembly
_atom_site_disorder_group
U U 0.49302(3) 0.71890(3) 0.27756(3) 0.02939(13) Uani 1 1 d . . .
Si1 Si 0.8911(3) 0.8164(3) 0.3222(2) 0.0441(7) Uani 1 1 d . . .
Si2 Si 0.2990(3) 0.9385(3) 0.0814(3) 0.0446(7) Uani 1 1 d . . .
Si3 Si 0.1687(3) 0.4127(3) 0.2188(2) 0.0425(7) Uani 1 1 d D . .
N N 0.6216(7) 0.5314(7) 0.2943(6) 0.0353(18) Uani 1 1 d . . .
C1 C 0.7488(9) 0.8520(10) 0.3543(8) 0.043(3) Uani 1 1 d . . .
C2 C 0.6696(9) 0.9359(9) 0.3111(7) 0.037(2) Uani 1 1 d . . .
H2 H 0.6680 0.9664 0.2513 0.044 Uiso 1 1 calc R . .
C3 C 0.5948(10) 0.9653(9) 0.3721(8) 0.042(2) Uani 1 1 d . . .
H3 H 0.5324 1.0144 0.3580 0.050 Uiso 1 1 calc R . .
C4 C 0.6308(9) 0.9076(9) 0.4582(7) 0.037(2) Uani 1 1 d . . .
H4 H 0.5994 0.9142 0.5133 0.045 Uiso 1 1 calc R . .
C5 C 0.7217(9) 0.8391(9) 0.4465(7) 0.038(2) Uani 1 1 d . . .
H5 H 0.7600 0.7907 0.4931 0.046 Uiso 1 1 calc R . .
C6 C 0.9765(11) 0.7251(15) 0.4143(11) 0.073(4) Uani 1 1 d . . .
H6A H 1.0477 0.7026 0.3960 0.109 Uiso 1 1 calc R . .
H6B H 0.9181 0.6518 0.4097 0.109 Uiso 1 1 calc R . .
H6C H 1.0083 0.7732 0.4851 0.109 Uiso 1 1 calc R . .
C7 C 0.8466(10) 0.7343(11) 0.1815(8) 0.050(3) Uani 1 1 d . . .
H7A H 0.9234 0.7343 0.1646 0.075 Uiso 1 1 calc R . .
H7B H 0.7893 0.7758 0.1355 0.075 Uiso 1 1 calc R . .
H7C H 0.8045 0.6508 0.1726 0.075 Uiso 1 1 calc R . .
C8 C 1.0007(11) 0.9656(13) 0.3424(9) 0.070(4) Uani 1 1 d . . .
H8A H 1.0225 1.0109 0.4133 0.105 Uiso 1 1 calc R . .
H8B H 0.9579 1.0130 0.2932 0.105 Uiso 1 1 calc R . .
H8C H 1.0780 0.9499 0.3310 0.105 Uiso 1 1 calc R . .
C9 C 0.3653(8) 0.7959(10) 0.0888(8) 0.038(2) Uani 1 1 d . . .
C10 C 0.4887(9) 0.7789(9) 0.0823(7) 0.036(2) Uani 1 1 d . . .
H10 H 0.5544 0.8410 0.0852 0.044 Uiso 1 1 calc R . .
C11 C 0.4922(9) 0.6513(9) 0.0708(7) 0.034(2) Uani 1 1 d . . .
H11 H 0.5609 0.6155 0.0649 0.040 Uiso 1 1 calc R . .
C12 C 0.3744(9) 0.5876(9) 0.0699(7) 0.034(2) Uani 1 1 d . . .
H12 H 0.3525 0.5030 0.0641 0.041 Uiso 1 1 calc R . .
C13 C 0.2960(9) 0.6737(10) 0.0790(8) 0.041(2) Uani 1 1 d . . .
H13 H 0.2124 0.6551 0.0788 0.049 Uiso 1 1 calc R . .
C14 C 0.1957(11) 0.9324(11) -0.0580(10) 0.060(3) Uani 1 1 d . . .
H14A H 0.1657 1.0088 -0.0632 0.090 Uiso 1 1 calc R . .
H14B H 0.1230 0.8658 -0.0799 0.090 Uiso 1 1 calc R . .
H14C H 0.2452 0.9196 -0.1027 0.090 Uiso 1 1 calc R . .
C15 C 0.1962(13) 0.9528(12) 0.1648(12) 0.073(4) Uani 1 1 d . . .
H15A H 0.2505 0.9735 0.2382 0.109 Uiso 1 1 calc R . .
H15B H 0.1382 0.8758 0.1508 0.109 Uiso 1 1 calc R . .
H15C H 0.1472 1.0164 0.1483 0.109 Uiso 1 1 calc R . .
C16 C 0.4346(11) 1.0737(10) 0.1242(9) 0.048(3) Uani 1 1 d . . .
H16A H 0.4843 1.0823 0.1978 0.072 Uiso 1 1 calc R . .
H16B H 0.4003 1.1471 0.1132 0.072 Uiso 1 1 calc R . .
H16C H 0.4890 1.0613 0.0836 0.072 Uiso 1 1 calc R . .
C17 C 0.2813(7) 0.5562(7) 0.2966(6) 0.034(2) Uani 1 1 d D . .
C18 C 0.2547(9) 0.6777(9) 0.3096(9) 0.040(2) Uani 1 1 d . . .
H18 H 0.1871 0.7043 0.2628 0.048 Uiso 1 1 calc R . .
C19 C 0.3459(10) 0.7513(10) 0.4036(8) 0.043(3) Uani 1 1 d . . .
H19 H 0.3482 0.8339 0.4293 0.052 Uiso 1 1 calc R . .
C20 C 0.4330(10) 0.6797(10) 0.4525(8) 0.044(3) Uani 1 1 d . . .
H20 H 0.5041 0.7056 0.5151 0.053 Uiso 1 1 calc R . .
C21 C 0.3915(9) 0.5615(10) 0.3885(7) 0.039(2) Uani 1 1 d . . .
H21 H 0.4308 0.4946 0.4037 0.047 Uiso 1 1 calc R . .
C22A C 0.0609(18) 0.4326(18) 0.0883(10) 0.067(7) Uiso 0.531(14) 1 d PD . .
C22B C -0.0008(9) 0.447(2) 0.174(2) 0.084(10) Uiso 0.469(14) 1 d PD . .
C23A C 0.2653(18) 0.2971(14) 0.183(2) 0.077(7) Uiso 0.531(14) 1 d PDU . .
C23B C 0.189(2) 0.344(2) 0.0976(14) 0.071(7) Uiso 0.469(14) 1 d PDU . .
C24A C 0.0774(18) 0.3501(16) 0.2980(14) 0.056(5) Uiso 0.531(14) 1 d PDU . .
C24B C 0.156(2) 0.3021(15) 0.3068(15) 0.060(6) Uiso 0.469(14) 1 d PDU . .
C25 C 0.6835(9) 0.5122(10) 0.3915(7) 0.039(2) Uani 1 1 d . . .
H25 H 0.6830 0.5675 0.4493 0.047 Uiso 1 1 calc R . .
C26 C 0.7464(9) 0.4172(11) 0.4103(8) 0.046(3) Uani 1 1 d . . .
H26 H 0.7874 0.4085 0.4792 0.055 Uiso 1 1 calc R . .
C27 C 0.7491(10) 0.3344(10) 0.3268(9) 0.049(3) Uani 1 1 d . . .
H27 H 0.7911 0.2682 0.3379 0.058 Uiso 1 1 calc R . .
C28 C 0.6883(10) 0.3511(10) 0.2261(8) 0.045(2) Uani 1 1 d . . .
H28 H 0.6901 0.2975 0.1679 0.054 Uiso 1 1 calc R . .
C29 C 0.6242(9) 0.4497(8) 0.2127(8) 0.036(2) Uani 1 1 d . . .
H29 H 0.5813 0.4594 0.1444 0.043 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'
Si Si 0.0817 0.0704 '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
_geom_angle_publ_flag
N U C19 117.1(3) . . ?
N U C3 126.5(3) . . ?
C19 U C3 81.4(3) . . ?
N U C20 89.3(3) . . ?
C19 U C20 29.3(3) . . ?
C3 U C20 90.7(3) . . ?
N U C12 82.1(3) . . ?
C19 U C12 119.3(3) . . ?
C3 U C12 134.7(3) . . ?
C20 U C12 127.7(3) . . ?
N U C13 110.3(3) . . ?
C19 U C13 99.0(3) . . ?
C3 U C13 115.7(3) . . ?
C20 U C13 119.7(3) . . ?
C12 U C13 29.0(3) . . ?
N U C2 108.4(3) . . ?
C19 U C2 110.4(3) . . ?
C3 U C2 29.1(3) . . ?
C20 U C2 115.0(3) . . ?
C12 U C2 116.6(3) . . ?
C13 U C2 111.4(3) . . ?
N U C1 80.2(3) . . ?
C19 U C1 118.1(3) . . ?
C3 U C1 48.9(3) . . ?
C20 U C1 106.9(3) . . ?
C12 U C1 121.9(3) . . ?
C13 U C1 131.9(3) . . ?
C2 U C1 29.5(3) . . ?
N U C11 78.3(3) . . ?
C19 U C11 146.5(3) . . ?
C3 U C11 114.5(3) . . ?
C20 U C11 154.6(3) . . ?
C12 U C11 29.1(3) . . ?
C13 U C11 47.8(3) . . ?
C2 U C11 90.0(3) . . ?
C1 U C11 92.9(3) . . ?
N U C5 80.7(3) . . ?
C19 U C5 91.7(3) . . ?
C3 U C5 47.3(3) . . ?
C20 U C5 77.8(3) . . ?
C12 U C5 148.9(3) . . ?
C13 U C5 158.4(3) . . ?
C2 U C5 47.0(3) . . ?
C1 U C5 29.1(3) . . ?
C11 U C5 121.1(3) . . ?
N U C9 126.3(3) . . ?
C19 U C9 106.7(3) . . ?
C3 U C9 88.0(3) . . ?
C20 U C9 135.0(3) . . ?
C12 U C9 48.8(3) . . ?
C13 U C9 29.7(3) . . ?
C2 U C9 81.9(3) . . ?
C1 U C9 105.8(3) . . ?
C11 U C9 48.5(3) . . ?
C5 U C9 128.9(3) . . ?
N U C4 106.8(3) . . ?
C19 U C4 70.2(3) . . ?
C3 U C4 28.9(3) . . ?
C20 U C4 67.8(3) . . ?
C12 U C4 163.1(3) . . ?
C13 U C4 142.0(3) . . ?
C2 U C4 47.3(3) . . ?
C1 U C4 48.3(3) . . ?
C11 U C4 137.0(3) . . ?
C5 U C4 28.3(3) . . ?
C9 U C4 116.5(3) . . ?
C6 Si1 C1 108.9(5) . . ?
C6 Si1 C8 108.8(6) . . ?
C1 Si1 C8 107.6(6) . . ?
C6 Si1 C7 110.9(6) . . ?
C1 Si1 C7 112.8(5) . . ?
C8 Si1 C7 107.8(5) . . ?
C9 Si2 C14 109.1(5) . . ?
C9 Si2 C16 109.3(5) . . ?
C14 Si2 C16 108.6(5) . . ?
C9 Si2 C15 110.4(5) . . ?
C14 Si2 C15 108.2(6) . . ?
C16 Si2 C15 111.2(6) . . ?
C23B Si3 C17 116.6(7) . . ?
C17 Si3 C22A 112.1(6) . . ?
C17 Si3 C24A 110.0(5) . . ?
C22A Si3 C24A 112.8(10) . . ?
C23B Si3 C24B 114.4(11) . . ?
C17 Si3 C24B 110.3(6) . . ?
C17 Si3 C23A 108.4(6) . . ?
C22A Si3 C23A 103.5(11) . . ?
C24A Si3 C23A 109.8(11) . . ?
C23B Si3 C22B 104.4(13) . . ?
C17 Si3 C22B 108.2(6) . . ?
C24B Si3 C22B 101.5(13) . . ?
C29 N C25 116.3(9) . . ?
C29 N U 125.2(6) . . ?
C25 N U 118.4(6) . . ?
C5 C1 C2 103.7(9) . . ?
C5 C1 Si1 127.7(8) . . ?
C2 C1 Si1 125.5(8) . . ?
C5 C1 U 75.5(5) . . ?
C2 C1 U 74.5(5) . . ?
Si1 C1 U 129.9(5) . . ?
C3 C2 C1 109.9(9) . . ?
C3 C2 U 74.5(5) . . ?
C1 C2 U 76.0(5) . . ?
C4 C3 C2 107.6(10) . . ?
C4 C3 U 77.8(5) . . ?
C2 C3 U 76.4(5) . . ?
C5 C4 C3 107.6(9) . . ?
C5 C4 U 75.5(5) . . ?
C3 C4 U 73.4(5) . . ?
C4 C5 C1 111.1(9) . . ?
C4 C5 U 76.2(5) . . ?
C1 C5 U 75.3(5) . . ?
C13 C9 C10 105.5(9) . . ?
C13 C9 Si2 127.1(7) . . ?
C10 C9 Si2 126.1(7) . . ?
C13 C9 U 73.9(6) . . ?
C10 C9 U 75.7(5) . . ?
Si2 C9 U 125.3(5) . . ?
C11 C10 C9 108.2(8) . . ?
C11 C10 U 74.5(5) . . ?
C9 C10 U 74.8(5) . . ?
C12 C11 C10 108.7(8) . . ?
C12 C11 U 74.1(5) . . ?
C10 C11 U 76.5(5) . . ?
C13 C12 C11 108.2(9) . . ?
C13 C12 U 76.1(5) . . ?
C11 C12 U 76.7(5) . . ?
C12 C13 C9 109.4(9) . . ?
C12 C13 U 74.9(5) . . ?
C9 C13 U 76.3(5) . . ?
C18 C17 C21 103.7(8) . . ?
C18 C17 Si3 127.8(7) . . ?
C21 C17 Si3 123.6(7) . . ?
C18 C17 U 72.9(5) . . ?
C21 C17 U 73.7(5) . . ?
Si3 C17 U 136.7(4) . . ?
C19 C18 C17 109.8(9) . . ?
C19 C18 U 73.0(5) . . ?
C17 C18 U 78.4(5) . . ?
C20 C19 C18 108.7(9) . . ?
C20 C19 U 75.7(5) . . ?
C18 C19 U 78.0(5) . . ?
C21 C20 C19 106.2(9) . . ?
C21 C20 U 78.7(6) . . ?
C19 C20 U 75.1(5) . . ?
C20 C21 C17 111.5(10) . . ?
C20 C21 U 72.6(6) . . ?
C17 C21 U 77.6(5) . . ?
N C25 C26 124.1(10) . . ?
C25 C26 C27 119.4(10) . . ?
C26 C27 C28 118.5(10) . . ?
C27 C28 C29 119.0(10) . . ?
N C29 C28 122.7(9) . . ?
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
U N 2.683(8) . ?
U C19 2.769(9) . ?
U C3 2.774(9) . ?
U C20 2.776(10) . ?
U C12 2.784(8) . ?
U C13 2.799(9) . ?
U C2 2.797(9) . ?
U C1 2.817(9) . ?
U C11 2.816(9) . ?
U C5 2.820(9) . ?
U C9 2.830(10) . ?
U C4 2.829(8) . ?
U C18 2.832(9) . ?
U C10 2.843(10) . ?
U C21 2.853(8) . ?
U C17 2.903(9) . ?
Si1 C6 1.840(13) . ?
Si1 C1 1.858(11) . ?
Si1 C8 1.863(12) . ?
Si1 C7 1.876(10) . ?
Si2 C9 1.845(11) . ?
Si2 C14 1.862(12) . ?
Si2 C16 1.865(11) . ?
Si2 C15 1.874(13) . ?
Si3 C23B 1.818(9) . ?
Si3 C17 1.835(7) . ?
Si3 C22A 1.861(9) . ?
Si3 C24A 1.869(9) . ?
Si3 C24B 1.877(9) . ?
Si3 C23A 1.895(9) . ?
Si3 C22B 1.897(9) . ?
N C29 1.343(12) . ?
N C25 1.346(12) . ?
C1 C5 1.418(14) . ?
C1 C2 1.430(15) . ?
C2 C3 1.398(14) . ?
C3 C4 1.397(15) . ?
C4 C5 1.382(14) . ?
C9 C13 1.445(14) . ?
C9 C10 1.444(13) . ?
C10 C11 1.418(14) . ?
C11 C12 1.409(13) . ?
C12 C13 1.399(14) . ?
C17 C18 1.424(13) . ?
C17 C21 1.427(12) . ?
C18 C19 1.403(14) . ?
C19 C20 1.402(16) . ?
C20 C21 1.397(15) . ?
C25 C26 1.357(15) . ?
C26 C27 1.369(15) . ?
C27 C28 1.375(15) . ?
C28 C29 1.391(14) . ?
