#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013752.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_7013752
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            'C33 H46 N U'
_chemical_formula_weight         694.74
_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     patter
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.090(7)
_cell_angle_beta                 98.889(8)
_cell_angle_gamma                98.832(5)
_cell_formula_units_Z            2
_cell_length_a                   10.8282(13)
_cell_length_b                   10.8431(12)
_cell_length_c                   14.0262(11)
_cell_measurement_reflns_used    10168
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.76
_cell_volume                     1500.4(3)
_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, 1997)'
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10168
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.429
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.455
_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    1.538
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             686
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.287
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0434
_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)+(0.0532P)²+0.4427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                4432
_reflns_number_total             5247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313992a.txt
_cod_data_source_block           (U,Bu^t^,picoline)
_cod_database_code               7013752
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 0.78382(3) 0.99487(3) 0.72034(2) 0.03114(12) Uani 1 1 d . . .
N N 0.9876(8) 0.8848(7) 0.7191(6) 0.0510(19) Uani 1 1 d . . .
C1 C 0.6426(9) 0.7177(8) 0.6543(7) 0.050(2) Uani 1 1 d . . .
C2 C 0.5552(9) 0.7994(9) 0.6784(7) 0.050(2) Uani 1 1 d . . .
H2 H 0.5143 0.8088 0.7331 0.060 Uiso 1 1 calc R . .
C3 C 0.5382(10) 0.8658(10) 0.6070(9) 0.066(3) Uani 1 1 d U . .
H3 H 0.4855 0.9259 0.6066 0.079 Uiso 1 1 calc R . .
C4 C 0.6124(13) 0.8254(11) 0.5407(9) 0.075(3) Uani 1 1 d U . .
H4 H 0.6176 0.8526 0.4848 0.091 Uiso 1 1 calc R . .
C5 C 0.6824(11) 0.7356(10) 0.5660(9) 0.071(3) Uani 1 1 d U . .
H5 H 0.7418 0.6965 0.5323 0.085 Uiso 1 1 calc R . .
C6 C 0.6658(11) 0.6119(9) 0.6987(10) 0.068(3) Uani 1 1 d U . .
C7 C 0.8071(19) 0.608(2) 0.7269(15) 0.139(6) Uani 1 1 d U . .
H7A H 0.8187 0.5669 0.7778 0.208 Uiso 1 1 calc R . .
H7B H 0.8582 0.6976 0.7545 0.208 Uiso 1 1 calc R . .
H7C H 0.8330 0.5574 0.6662 0.208 Uiso 1 1 calc R . .
C8 C 0.5876(13) 0.4812(12) 0.6347(10) 0.082(3) Uani 1 1 d U . .
H8A H 0.4991 0.4817 0.6351 0.123 Uiso 1 1 calc R . .
H8B H 0.6123 0.4155 0.6615 0.123 Uiso 1 1 calc R . .
H8C H 0.5996 0.4597 0.5652 0.123 Uiso 1 1 calc R . .
C9 C 0.6392(18) 0.6452(18) 0.8079(14) 0.125(6) Uani 1 1 d U . .
H9A H 0.5519 0.6535 0.8056 0.187 Uiso 1 1 calc R . .
H9B H 0.6955 0.7279 0.8534 0.187 Uiso 1 1 calc R . .
H9C H 0.6535 0.5749 0.8328 0.187 Uiso 1 1 calc R . .
C10 C 0.6840(8) 1.1271(8) 0.8981(6) 0.0395(18) Uani 1 1 d . . .
C11 C 0.6962(8) 1.0029(8) 0.9044(6) 0.0400(19) Uani 1 1 d . . .
H11 H 0.6292 0.9337 0.8980 0.048 Uiso 1 1 calc R . .
C12 C 0.8295(8) 1.0011(8) 0.9224(6) 0.0391(18) Uani 1 1 d . . .
H12 H 0.8646 0.9300 0.9281 0.047 Uiso 1 1 calc R . .
C13 C 0.8966(8) 1.1238(8) 0.9298(6) 0.0375(18) Uani 1 1 d . . .
H13 H 0.9852 1.1512 0.9435 0.045 Uiso 1 1 calc R . .
C14 C 0.8078(7) 1.2004(8) 0.9131(6) 0.0372(18) Uani 1 1 d . . .
H14 H 0.8283 1.2864 0.9122 0.045 Uiso 1 1 calc R . .
C15 C 0.5622(9) 1.1798(8) 0.8931(9) 0.055(3) Uani 1 1 d . . .
C16 C 0.5542(12) 1.2534(13) 0.8182(11) 0.080(3) Uani 1 1 d U . .
H16A H 0.6296 1.3233 0.8376 0.121 Uiso 1 1 calc R . .
H16B H 0.4799 1.2915 0.8200 0.121 Uiso 1 1 calc R . .
H16C H 0.5481 1.1920 0.7496 0.121 Uiso 1 1 calc R . .
C17 C 0.5682(12) 1.2780(12) 1.0049(10) 0.086(4) Uani 1 1 d U . .
H17A H 0.6266 1.3610 1.0184 0.129 Uiso 1 1 calc R . .
H17B H 0.5973 1.2390 1.0543 0.129 Uiso 1 1 calc R . .
H17C H 0.4845 1.2942 1.0107 0.129 Uiso 1 1 calc R . .
C18 C 0.4427(10) 1.0698(11) 0.8672(10) 0.067(3) Uani 1 1 d . . .
H18A H 0.3689 1.1087 0.8720 0.100 Uiso 1 1 calc R . .
H18B H 0.4514 1.0238 0.9150 0.100 Uiso 1 1 calc R . .
H18C H 0.4324 1.0075 0.7981 0.100 Uiso 1 1 calc R . .
C19 C 0.9585(7) 1.2207(7) 0.7036(6) 0.0330(16) Uani 1 1 d . . .
C20 C 0.8337(8) 1.2475(7) 0.6972(6) 0.0370(18) Uani 1 1 d . . .
H20 H 0.8100 1.3168 0.7451 0.044 Uiso 1 1 calc R . .
C21 C 0.7516(8) 1.1519(8) 0.6060(6) 0.0369(17) Uani 1 1 d . . .
H21 H 0.6645 1.1458 0.5844 0.044 Uiso 1 1 calc R . .
C22 C 0.8261(9) 1.0671(8) 0.5538(6) 0.043(2) Uani 1 1 d . . .
H22 H 0.7971 0.9971 0.4904 0.052 Uiso 1 1 calc R . .
C23 C 0.9508(8) 1.1069(8) 0.6140(7) 0.0403(19) Uani 1 1 d . . .
H23 H 1.0181 1.0656 0.5982 0.048 Uiso 1 1 calc R . .
C24 C 1.0828(8) 1.3132(8) 0.7728(6) 0.0410(19) Uani 1 1 d . . .
C25 C 1.1455(10) 1.3889(9) 0.7105(8) 0.057(2) Uani 1 1 d . . .
H25A H 1.1559 1.3258 0.6475 0.086 Uiso 1 1 calc R . .
H25B H 1.2277 1.4427 0.7507 0.086 Uiso 1 1 calc R . .
H25C H 1.0918 1.4454 0.6946 0.086 Uiso 1 1 calc R . .
C26 C 1.1762(9) 1.2331(9) 0.8045(8) 0.053(2) Uani 1 1 d . . .
H26A H 1.1378 1.1821 0.8410 0.080 Uiso 1 1 calc R . .
H26B H 1.2538 1.2935 0.8485 0.080 Uiso 1 1 calc R . .
H26C H 1.1954 1.1737 0.7437 0.080 Uiso 1 1 calc R . .
C27 C 1.0628(9) 1.4152(8) 0.8712(7) 0.050(2) Uani 1 1 d . . .
H27A H 1.0238 1.3691 0.9105 0.076 Uiso 1 1 calc R . .
H27B H 1.0081 1.4695 0.8528 0.076 Uiso 1 1 calc R . .
H27C H 1.1441 1.4711 0.9118 0.076 Uiso 1 1 calc R . .
C28 C 1.0627(9) 0.8894(10) 0.8073(9) 0.059(3) Uani 1 1 d . . .
H28 H 1.0456 0.9420 0.8689 0.071 Uiso 1 1 calc R . .
C29 C 1.1624(9) 0.8244(10) 0.8162(9) 0.059(3) Uani 1 1 d . . .
H29 H 1.2107 0.8324 0.8796 0.070 Uiso 1 1 calc R . .
C30 C 1.1824(10) 0.7520(10) 0.7290(8) 0.057(3) Uani 1 1 d . . .
H30 H 1.2449 0.7025 0.7320 0.068 Uiso 1 1 calc R . .
C31 C 1.1213(10) 0.7405(8) 0.6328(7) 0.051(2) Uani 1 1 d . . .
C32 C 1.0159(10) 0.8144(9) 0.6306(8) 0.057(3) Uani 1 1 d . . .
H32 H 0.9700 0.8114 0.5678 0.069 Uiso 1 1 calc R . .
C33 C 1.1422(13) 0.6588(11) 0.5313(9) 0.075(3) Uani 1 1 d . . .
H33A H 1.2310 0.6812 0.5298 0.113 Uiso 1 1 calc R . .
H33B H 1.0908 0.6765 0.4772 0.113 Uiso 1 1 calc R . .
H33C H 1.1184 0.5656 0.5212 0.113 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'
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 C21 118.8(2) . . ?
N U C4 103.5(4) . . ?
C21 U C4 76.2(3) . . ?
N U C3 125.5(3) . . ?
C21 U C3 81.4(3) . . ?
C4 U C3 27.9(4) . . ?
N U C22 91.4(3) . . ?
C21 U C22 29.8(3) . . ?
C4 U C22 69.4(3) . . ?
C3 U C22 87.7(3) . . ?
N U C12 80.9(2) . . ?
C21 U C12 142.6(2) . . ?
C4 U C12 133.2(3) . . ?
C3 U C12 114.3(3) . . ?
C22 U C12 157.2(3) . . ?
N U C13 83.2(2) . . ?
C21 U C13 117.0(2) . . ?
C4 U C13 160.5(3) . . ?
C3 U C13 135.1(3) . . ?
C22 U C13 129.4(2) . . ?
C12 U C13 28.7(2) . . ?
N U C14 110.9(2) . . ?
C21 U C14 95.3(2) . . ?
C4 U C14 144.1(4) . . ?
C3 U C14 117.1(3) . . ?
C22 U C14 118.3(2) . . ?
C12 U C14 47.4(2) . . ?
C13 U C14 28.9(2) . . ?
N U C20 112.5(2) . . ?
C21 U C20 29.3(2) . . ?
C4 U C20 105.5(3) . . ?
C3 U C20 106.6(3) . . ?
C22 U C20 47.9(2) . . ?
C12 U C20 115.7(2) . . ?
C13 U C20 88.3(2) . . ?
C14 U C20 70.6(2) . . ?
N U C2 110.9(3) . . ?
C21 U C2 110.4(2) . . ?
C4 U C2 46.3(3) . . ?
C3 U C2 29.2(3) . . ?
C22 U C2 114.7(3) . . ?
C12 U C2 88.1(3) . . ?
C13 U C2 114.2(3) . . ?
C14 U C2 109.3(3) . . ?
C20 U C2 132.9(3) . . ?
N U C5 77.9(3) . . ?
C21 U C5 100.8(3) . . ?
C4 U C5 29.3(4) . . ?
C3 U C5 47.8(4) . . ?
C22 U C5 83.9(3) . . ?
C12 U C5 115.0(3) . . ?
C13 U C5 142.1(3) . . ?
C14 U C5 154.9(3) . . ?
C20 U C5 129.3(3) . . ?
C2 U C5 46.8(3) . . ?
N U C11 107.7(2) . . ?
C21 U C11 129.0(2) . . ?
C4 U C11 113.4(3) . . ?
C3 U C11 88.7(3) . . ?
C22 U C11 158.8(3) . . ?
C12 U C11 29.3(2) . . ?
C13 U C11 47.3(2) . . ?
C14 U C11 46.5(2) . . ?
C20 U C11 113.8(2) . . ?
C2 U C11 67.8(3) . . ?
C5 U C11 108.8(3) . . ?
C32 N C28 116.4(9) . . ?
C32 N U 121.5(7) . . ?
C28 N U 121.9(6) . . ?
C2 C1 C5 105.9(9) . . ?
C2 C1 C6 125.4(9) . . ?
C5 C1 C6 127.5(10) . . ?
C2 C1 U 72.8(5) . . ?
C5 C1 U 72.8(5) . . ?
C6 C1 U 129.1(7) . . ?
C1 C2 C3 110.0(10) . . ?
C1 C2 U 79.2(5) . . ?
C3 C2 U 72.4(5) . . ?
C4 C3 C2 106.6(10) . . ?
C4 C3 U 76.1(7) . . ?
C2 C3 U 78.4(5) . . ?
C3 C4 C5 111.5(10) . . ?
C3 C4 U 76.1(6) . . ?
C5 C4 U 78.7(6) . . ?
C4 C5 C1 105.9(10) . . ?
C4 C5 U 72.0(6) . . ?
C1 C5 U 78.5(5) . . ?
C8 C6 C1 112.3(10) . . ?
C8 C6 C7 112.0(11) . . ?
C1 C6 C7 114.1(11) . . ?
C8 C6 C9 107.8(11) . . ?
C1 C6 C9 112.1(10) . . ?
C7 C6 C9 97.5(12) . . ?
C14 C10 C11 106.8(7) . . ?
C14 C10 C15 126.2(7) . . ?
C11 C10 C15 126.4(7) . . ?
C14 C10 U 73.1(4) . . ?
C11 C10 U 74.5(5) . . ?
C15 C10 U 124.9(6) . . ?
C10 C11 C12 108.1(7) . . ?
C10 C11 U 77.3(5) . . ?
C12 C11 U 71.9(4) . . ?
C13 C12 C11 107.5(7) . . ?
C13 C12 U 76.0(4) . . ?
C11 C12 U 78.7(5) . . ?
C12 C13 C14 108.2(7) . . ?
C12 C13 U 75.4(5) . . ?
C14 C13 U 77.3(5) . . ?
C10 C14 C13 109.3(7) . . ?
C10 C14 U 78.7(5) . . ?
C13 C14 U 73.8(4) . . ?
C16 C15 C10 110.7(8) . . ?
C16 C15 C18 111.5(10) . . ?
C10 C15 C18 112.3(7) . . ?
C16 C15 C17 110.0(9) . . ?
C10 C15 C17 106.5(9) . . ?
C18 C15 C17 105.7(8) . . ?
C20 C19 C23 106.2(7) . . ?
C20 C19 C24 127.3(7) . . ?
C23 C19 C24 124.5(7) . . ?
C20 C19 U 71.6(4) . . ?
C23 C19 U 73.1(4) . . ?
C24 C19 U 132.7(5) . . ?
C21 C20 C19 109.0(7) . . ?
C21 C20 U 70.4(4) . . ?
C19 C20 U 80.1(4) . . ?
C20 C21 C22 107.5(7) . . ?
C20 C21 U 80.3(4) . . ?
C22 C21 U 77.3(4) . . ?
C23 C22 C21 108.2(7) . . ?
C23 C22 U 80.1(5) . . ?
C21 C22 U 72.9(4) . . ?
C22 C23 C19 109.1(8) . . ?
C22 C23 U 71.4(4) . . ?
C19 C23 U 78.6(4) . . ?
C19 C24 C27 112.9(7) . . ?
C19 C24 C26 110.9(7) . . ?
C27 C24 C26 108.3(7) . . ?
C19 C24 C25 107.9(7) . . ?
C27 C24 C25 108.8(7) . . ?
C26 C24 C25 107.9(7) . . ?
N C28 C29 127.3(11) . . ?
C30 C29 C28 114.4(11) . . ?
C29 C30 C31 126.7(11) . . ?
C30 C31 C33 128.0(10) . . ?
C30 C31 C32 115.2(8) . . ?
C33 C31 C32 116.7(10) . . ?
N C32 C31 119.9(10) . . ?
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 2.665(7) . ?
U C21 2.718(7) . ?
U C4 2.766(11) . ?
U C3 2.766(10) . ?
U C22 2.774(8) . ?
U C12 2.778(8) . ?
U C13 2.785(8) . ?
U C14 2.830(8) . ?
U C20 2.844(7) . ?
U C2 2.844(8) . ?
U C5 2.851(10) . ?
U C11 2.866(8) . ?
U C23 2.883(7) . ?
U C10 2.900(8) . ?
U C1 2.925(11) . ?
U C19 2.953(10) . ?
N C32 1.336(11) . ?
N C28 1.353(13) . ?
C1 C2 1.398(14) . ?
C1 C5 1.433(14) . ?
C1 C6 1.508(14) . ?
C2 C3 1.418(13) . ?
C3 C4 1.332(17) . ?
C4 C5 1.422(17) . ?
C6 C8 1.447(15) . ?
C6 C7 1.53(2) . ?
C6 C9 1.54(2) . ?
C10 C14 1.396(11) . ?
C10 C11 1.404(11) . ?
C10 C15 1.516(12) . ?
C11 C12 1.431(12) . ?
C12 C13 1.378(11) . ?
C13 C14 1.404(12) . ?
C15 C16 1.513(15) . ?
C15 C18 1.526(13) . ?
C15 C17 1.566(15) . ?
C19 C20 1.420(11) . ?
C19 C23 1.425(11) . ?
C19 C24 1.518(11) . ?
C20 C21 1.414(11) . ?
C21 C22 1.415(12) . ?
C22 C23 1.398(12) . ?
C24 C27 1.530(12) . ?
C24 C26 1.535(12) . ?
C24 C25 1.543(12) . ?
C28 C29 1.388(13) . ?
C29 C30 1.290(14) . ?
C30 C31 1.366(14) . ?
C31 C33 1.484(13) . ?
C31 C32 1.493(14) . ?
