#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013748.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_7013748
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            'C32 H44 N U'
_chemical_formula_weight         680.71
_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                98.333(4)
_cell_angle_beta                 110.235(4)
_cell_angle_gamma                96.726(3)
_cell_formula_units_Z            2
_cell_length_a                   10.6759(9)
_cell_length_b                   10.8331(9)
_cell_length_c                   13.6419(8)
_cell_measurement_reflns_used    9649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.06
_cell_volume                     1440.8(2)
_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 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.1123
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9649
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    5.652
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.441
_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    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             670
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.876
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'calc w=1/[σ²(Fo²)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                3811
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313992a.txt
_cod_data_source_block           (U,Bu^t^,pyridine)
_cod_original_cell_volume        1440.76(19)
_cod_database_code               7013748
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 0.49864(3) 0.72188(3) 0.27703(2) 0.02721(10) Uani 1 1 d . . .
N N 0.6229(6) 0.5220(6) 0.2889(5) 0.0317(15) Uani 1 1 d . . .
C1 C 0.7779(8) 0.8533(7) 0.3592(6) 0.0344(18) Uani 1 1 d . . .
C2 C 0.6997(8) 0.9396(7) 0.3157(6) 0.0343(19) Uani 1 1 d . . .
H2 H 0.6998 0.9722 0.2563 0.041 Uiso 1 1 calc R . .
C3 C 0.6187(8) 0.9704(7) 0.3771(6) 0.038(2) Uani 1 1 d . . .
H3 H 0.5550 1.0237 0.3638 0.046 Uiso 1 1 calc R . .
C4 C 0.6535(8) 0.9052(7) 0.4603(6) 0.0352(19) Uani 1 1 d . . .
H4 H 0.6191 0.9103 0.5145 0.042 Uiso 1 1 calc R . .
C5 C 0.7494(8) 0.8297(7) 0.4500(6) 0.0367(19) Uani 1 1 d . . .
H5 H 0.7868 0.7750 0.4941 0.044 Uiso 1 1 calc R . .
C6 C 0.8947(8) 0.8154(7) 0.3286(6) 0.0365(19) Uani 1 1 d . . .
C7 C 0.9691(9) 0.7277(10) 0.3990(8) 0.062(3) Uani 1 1 d . . .
H7A H 0.9905 0.7640 0.4726 0.093 Uiso 1 1 calc R . .
H7B H 1.0514 0.7182 0.3872 0.093 Uiso 1 1 calc R . .
H7C H 0.9118 0.6461 0.3810 0.093 Uiso 1 1 calc R . .
C8 C 0.9966(9) 0.9360(9) 0.3463(8) 0.059(3) Uani 1 1 d . . .
H8A H 0.9558 0.9878 0.2969 0.088 Uiso 1 1 calc R . .
H8B H 1.0757 0.9135 0.3351 0.088 Uiso 1 1 calc R . .
H8C H 1.0222 0.9824 0.4179 0.088 Uiso 1 1 calc R . .
C9 C 0.8475(8) 0.7486(8) 0.2111(6) 0.042(2) Uani 1 1 d . . .
H9A H 0.7876 0.6700 0.1994 0.063 Uiso 1 1 calc R . .
H9B H 0.9249 0.7321 0.1943 0.063 Uiso 1 1 calc R . .
H9C H 0.8004 0.8022 0.1662 0.063 Uiso 1 1 calc R . .
C10 C 0.3618(8) 0.8171(7) 0.0888(6) 0.0327(18) Uani 1 1 d . . .
C11 C 0.4889(8) 0.7996(7) 0.0814(6) 0.0362(19) Uani 1 1 d . . .
H11 H 0.5580 0.8629 0.0849 0.043 Uiso 1 1 calc R . .
C12 C 0.4900(8) 0.6667(7) 0.0677(5) 0.0315(18) Uani 1 1 d . . .
H12 H 0.5615 0.6284 0.0625 0.038 Uiso 1 1 calc R . .
C13 C 0.3647(8) 0.6031(7) 0.0635(6) 0.0304(18) Uani 1 1 d . . .
H13 H 0.3378 0.5159 0.0532 0.036 Uiso 1 1 calc R . .
C14 C 0.2880(9) 0.6968(7) 0.0780(6) 0.0361(19) Uani 1 1 d . . .
H14 H 0.2015 0.6811 0.0800 0.043 Uiso 1 1 calc R . .
C15 C 0.3076(9) 0.9427(7) 0.0898(6) 0.0379(19) Uani 1 1 d . . .
C16 C 0.2223(9) 0.9502(8) 0.1619(7) 0.050(2) Uani 1 1 d . . .
H16A H 0.2792 0.9496 0.2338 0.076 Uiso 1 1 calc R . .
H16B H 0.1494 0.8786 0.1363 0.076 Uiso 1 1 calc R . .
H16C H 0.1857 1.0270 0.1600 0.076 Uiso 1 1 calc R . .
C17 C 0.2073(10) 0.9385(8) -0.0264(7) 0.052(2) Uani 1 1 d . . .
H17A H 0.1575 1.0068 -0.0263 0.079 Uiso 1 1 calc R . .
H17B H 0.1452 0.8591 -0.0523 0.079 Uiso 1 1 calc R . .
H17C H 0.2578 0.9472 -0.0720 0.079 Uiso 1 1 calc R . .
C18 C 0.4192(9) 1.0571(7) 0.1255(7) 0.039(2) Uani 1 1 d . . .
H18A H 0.4821 1.0564 0.1955 0.059 Uiso 1 1 calc R . .
H18B H 0.3809 1.1328 0.1273 0.059 Uiso 1 1 calc R . .
H18C H 0.4659 1.0549 0.0766 0.059 Uiso 1 1 calc R . .
C19 C 0.2738(8) 0.5502(7) 0.2962(5) 0.0295(17) Uani 1 1 d . . .
C20 C 0.2454(8) 0.6747(7) 0.3024(6) 0.0301(17) Uani 1 1 d . . .
H20 H 0.1741 0.7003 0.2526 0.036 Uiso 1 1 calc R . .
C21 C 0.3407(7) 0.7532(7) 0.3947(6) 0.0297(17) Uani 1 1 d . . .
H21 H 0.3436 0.8392 0.4169 0.036 Uiso 1 1 calc R . .
C22 C 0.4322(8) 0.6792(7) 0.4485(6) 0.0355(19) Uani 1 1 d . . .
H22 H 0.5062 0.7076 0.5123 0.043 Uiso 1 1 calc R . .
C23 C 0.3911(7) 0.5543(7) 0.3879(6) 0.0287(17) Uani 1 1 d . . .
H23 H 0.4337 0.4860 0.4051 0.034 Uiso 1 1 calc R . .
C24 C 0.1818(8) 0.4273(7) 0.2265(6) 0.0341(18) Uani 1 1 d . . .
C25 C 0.1049(10) 0.3711(8) 0.2922(7) 0.051(2) Uani 1 1 d . . .
H25A H 0.1688 0.3517 0.3548 0.077 Uiso 1 1 calc R . .
H25B H 0.0428 0.2951 0.2497 0.077 Uiso 1 1 calc R . .
H25C H 0.0555 0.4319 0.3129 0.077 Uiso 1 1 calc R . .
C26 C 0.2634(9) 0.3314(7) 0.1980(6) 0.040(2) Uani 1 1 d . . .
H26A H 0.3203 0.3689 0.1650 0.060 Uiso 1 1 calc R . .
H26B H 0.2026 0.2580 0.1496 0.060 Uiso 1 1 calc R . .
H26C H 0.3188 0.3069 0.2616 0.060 Uiso 1 1 calc R . .
C27 C 0.0784(8) 0.4487(7) 0.1258(6) 0.040(2) Uani 1 1 d . . .
H27A H 0.0253 0.5075 0.1435 0.061 Uiso 1 1 calc R . .
H27B H 0.0201 0.3696 0.0863 0.061 Uiso 1 1 calc R . .
H27C H 0.1240 0.4826 0.0834 0.061 Uiso 1 1 calc R . .
C28 C 0.6855(8) 0.4951(7) 0.3856(6) 0.0348(19) Uani 1 1 d . . .
H28 H 0.6865 0.5494 0.4454 0.042 Uiso 1 1 calc R . .
C29 C 0.7477(8) 0.3917(7) 0.4005(6) 0.0373(19) Uani 1 1 d . . .
H29 H 0.7867 0.3752 0.4685 0.045 Uiso 1 1 calc R . .
C30 C 0.7516(8) 0.3127(8) 0.3130(7) 0.042(2) Uani 1 1 d . . .
H30 H 0.7954 0.2434 0.3209 0.050 Uiso 1 1 calc R . .
C31 C 0.6876(8) 0.3401(7) 0.2118(7) 0.040(2) Uani 1 1 d . . .
H31 H 0.6876 0.2888 0.1509 0.048 Uiso 1 1 calc R . .
C32 C 0.6257(8) 0.4430(7) 0.2046(6) 0.0336(18) Uani 1 1 d . . .
H32 H 0.5826 0.4595 0.1372 0.040 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 117.47(19) . . ?
N U C22 89.7(2) . . ?
C21 U C22 29.9(2) . . ?
N U C3 126.0(2) . . ?
C21 U C3 83.8(2) . . ?
C22 U C3 91.4(2) . . ?
N U C13 83.9(2) . . ?
C21 U C13 116.3(2) . . ?
C22 U C13 127.8(2) . . ?
C3 U C13 133.0(2) . . ?
N U C12 80.6(2) . . ?
C21 U C12 143.1(2) . . ?
C22 U C12 155.5(2) . . ?
C3 U C12 112.5(2) . . ?
C13 U C12 29.2(2) . . ?
N U C4 106.3(2) . . ?
C21 U C4 73.4(2) . . ?
C22 U C4 68.8(2) . . ?
C3 U C4 28.9(2) . . ?
C13 U C4 161.4(2) . . ?
C12 U C4 135.5(2) . . ?
N U C14 112.2(2) . . ?
C21 U C14 95.7(2) . . ?
C22 U C14 118.6(2) . . ?
C3 U C14 114.2(2) . . ?
C13 U C14 29.1(2) . . ?
C12 U C14 47.6(2) . . ?
C4 U C14 140.6(2) . . ?
N U C20 112.68(18) . . ?
C21 U C20 29.0(2) . . ?
C22 U C20 47.9(2) . . ?
C3 U C20 107.4(2) . . ?
C13 U C20 87.7(2) . . ?
C12 U C20 115.9(2) . . ?
C4 U C20 102.1(2) . . ?
C14 U C20 71.0(2) . . ?
N U C2 107.2(2) . . ?
C21 U C2 113.2(2) . . ?
C22 U C2 116.0(2) . . ?
C3 U C2 29.5(2) . . ?
C13 U C2 115.4(2) . . ?
C12 U C2 88.4(2) . . ?
C4 U C2 47.2(2) . . ?
C14 U C2 110.7(2) . . ?
C20 U C2 135.7(2) . . ?
N U C5 79.6(2) . . ?
C21 U C5 95.2(2) . . ?
C22 U C5 79.0(2) . . ?
C3 U C5 47.9(2) . . ?
C13 U C5 148.4(2) . . ?
C12 U C5 120.6(2) . . ?
C4 U C5 28.9(2) . . ?
C14 U C5 157.6(2) . . ?
C20 U C5 123.5(2) . . ?
C2 U C5 46.9(2) . . ?
N U C11 106.45(19) . . ?
C21 U C11 131.7(2) . . ?
C22 U C11 161.5(2) . . ?
C3 U C11 86.4(2) . . ?
C13 U C11 47.9(2) . . ?
C12 U C11 29.0(2) . . ?
C4 U C11 113.6(2) . . ?
C14 U C11 47.1(2) . . ?
C20 U C11 115.6(2) . . ?
C2 U C11 68.4(2) . . ?
C5 U C11 112.2(2) . . ?
C32 N C28 116.6(6) . . ?
C2 C1 C5 107.9(7) . . ?
C2 C1 C6 124.5(6) . . ?
C5 C1 C6 126.4(7) . . ?
C1 C2 C3 109.0(6) . . ?
C4 C3 C2 106.7(7) . . ?
C3 C4 C5 109.5(7) . . ?
C4 C5 C1 107.0(7) . . ?
C1 C6 C7 111.4(6) . . ?
C1 C6 C9 112.5(6) . . ?
C7 C6 C9 108.5(7) . . ?
C1 C6 C8 108.1(6) . . ?
C7 C6 C8 107.9(7) . . ?
C9 C6 C8 108.2(6) . . ?
C14 C10 C11 107.4(6) . . ?
C14 C10 C15 126.3(7) . . ?
C11 C10 C15 125.7(7) . . ?
C12 C11 C10 107.1(7) . . ?
C13 C12 C11 108.7(7) . . ?
C14 C13 C12 107.0(7) . . ?
C10 C14 C13 109.7(7) . . ?
C18 C15 C10 112.5(7) . . ?
C18 C15 C16 110.5(7) . . ?
C10 C15 C16 109.8(6) . . ?
C18 C15 C17 110.3(6) . . ?
C10 C15 C17 107.0(6) . . ?
C16 C15 C17 106.6(7) . . ?
C20 C19 C23 106.2(6) . . ?
C20 C19 C24 128.4(7) . . ?
C23 C19 C24 123.5(6) . . ?
C21 C20 C19 109.6(7) . . ?
C20 C21 C22 107.9(7) . . ?
C23 C22 C21 107.6(7) . . ?
C22 C23 C19 108.8(7) . . ?
C27 C24 C19 112.4(6) . . ?
C27 C24 C26 109.3(6) . . ?
C19 C24 C26 111.5(6) . . ?
C27 C24 C25 108.1(7) . . ?
C19 C24 C25 107.0(6) . . ?
C26 C24 C25 108.5(7) . . ?
N C28 C29 123.5(7) . . ?
C28 C29 C30 119.0(7) . . ?
C29 C30 C31 118.1(7) . . ?
C32 C31 C30 118.7(7) . . ?
N C32 C31 124.1(8) . . ?
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(6) . ?
U C21 2.717(7) . ?
U C22 2.752(7) . ?
U C3 2.769(7) . ?
U C13 2.790(7) . ?
U C12 2.798(7) . ?
U C4 2.804(7) . ?
U C14 2.815(8) . ?
U C20 2.840(7) . ?
U C2 2.849(7) . ?
U C5 2.864(8) . ?
U C11 2.884(7) . ?
U C10 2.885(7) . ?
U C1 2.899(7) . ?
U C23 2.900(7) . ?
U C19 2.970(7) . ?
N C32 1.341(9) . ?
N C28 1.349(9) . ?
C1 C2 1.388(11) . ?
C1 C5 1.424(10) . ?
C1 C6 1.525(11) . ?
C2 C3 1.430(10) . ?
C3 C4 1.390(11) . ?
C4 C5 1.414(11) . ?
C6 C7 1.539(11) . ?
C6 C9 1.538(10) . ?
C6 C8 1.531(11) . ?
C10 C14 1.402(10) . ?
C10 C11 1.427(11) . ?
C10 C15 1.539(10) . ?
C11 C12 1.427(10) . ?
C12 C13 1.409(10) . ?
C13 C14 1.410(10) . ?
C15 C18 1.507(11) . ?
C15 C16 1.554(11) . ?
C15 C17 1.567(12) . ?
C19 C20 1.414(10) . ?
C19 C23 1.422(10) . ?
C19 C24 1.524(10) . ?
C20 C21 1.394(10) . ?
C21 C22 1.412(10) . ?
C22 C23 1.411(10) . ?
C24 C27 1.504(10) . ?
C24 C26 1.522(11) . ?
C24 C25 1.548(10) . ?
C28 C29 1.372(10) . ?
C29 C30 1.380(11) . ?
C30 C31 1.406(11) . ?
C31 C32 1.359(10) . ?
