#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:23:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179841 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013749.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_7013749
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 Ce N Si3'
_chemical_formula_weight         631.04
_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                98.786(6)
_cell_angle_beta                 109.589(5)
_cell_angle_gamma                96.900(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1698(11)
_cell_length_b                   11.2011(11)
_cell_length_c                   13.7417(9)
_cell_measurement_reflns_used    10763
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.11
_cell_volume                     1573.4(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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.916
_diffrn_measured_fraction_theta_max 0.916
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0791
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10763
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2000)'
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.924
_refine_diff_density_min         -1.079
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5467
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0426
_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)+(0.0446P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                4505
_reflns_number_total             5467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313992a.txt
_cod_data_source_block           (Ce,SiMe~3~,pyridine)
_cod_original_cell_volume        1573.4(2)
_cod_database_code               7013749
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
Ce Ce 0.49224(3) 0.71955(3) 0.27760(2) 0.02839(11) Uani 1 1 d . . .
Si1 Si 0.89146(14) 0.81734(16) 0.32315(12) 0.0419(4) Uani 1 1 d . . .
Si2 Si 0.29759(16) 0.93933(16) 0.07938(14) 0.0455(4) Uani 1 1 d . . .
Si3 Si 0.16927(17) 0.41397(15) 0.21982(13) 0.0480(4) Uani 1 1 d D . .
N N 0.6209(4) 0.5295(4) 0.2931(3) 0.0350(10) Uani 1 1 d . . .
C1 C 0.7488(5) 0.8560(5) 0.3557(4) 0.0382(12) Uani 1 1 d . . .
C2 C 0.6694(5) 0.9384(5) 0.3115(4) 0.0376(12) Uani 1 1 d . . .
H2 H 0.6669 0.9673 0.2510 0.045 Uiso 1 1 calc R . .
C3 C 0.5958(5) 0.9695(5) 0.3725(5) 0.0427(13) Uani 1 1 d . . .
H3 H 0.5348 1.0203 0.3592 0.051 Uiso 1 1 calc R . .
C4 C 0.6315(5) 0.9090(5) 0.4588(4) 0.0404(13) Uani 1 1 d . . .
H4 H 0.5992 0.9146 0.5132 0.048 Uiso 1 1 calc R . .
C5 C 0.7232(5) 0.8398(5) 0.4475(4) 0.0411(13) Uani 1 1 d . . .
H5 H 0.7618 0.7905 0.4931 0.049 Uiso 1 1 calc R . .
C6 C 0.9787(6) 0.7245(8) 0.4152(6) 0.072(2) Uani 1 1 d . . .
H6A H 1.0620 0.7215 0.4101 0.108 Uiso 1 1 calc R . .
H6B H 0.9297 0.6426 0.3970 0.108 Uiso 1 1 calc R . .
H6C H 0.9896 0.7613 0.4862 0.108 Uiso 1 1 calc R . .
C7 C 0.8460(5) 0.7353(6) 0.1831(5) 0.0502(15) Uani 1 1 d . . .
H7A H 0.9228 0.7311 0.1669 0.075 Uiso 1 1 calc R . .
H7B H 0.7916 0.7790 0.1368 0.075 Uiso 1 1 calc R . .
H7C H 0.8004 0.6536 0.1737 0.075 Uiso 1 1 calc R . .
C8 C 1.0005(6) 0.9644(6) 0.3420(5) 0.0602(19) Uani 1 1 d . . .
H8A H 1.0258 1.0087 0.4134 0.090 Uiso 1 1 calc R . .
H8B H 0.9562 1.0129 0.2945 0.090 Uiso 1 1 calc R . .
H8C H 1.0760 0.9478 0.3277 0.090 Uiso 1 1 calc R . .
C9 C 0.3654(5) 0.7959(5) 0.0867(4) 0.0366(12) Uani 1 1 d . . .
C10 C 0.4857(5) 0.7778(5) 0.0804(4) 0.0333(11) Uani 1 1 d . . .
H10 H 0.5509 0.8399 0.0833 0.040 Uiso 1 1 calc R . .
C11 C 0.4924(5) 0.6533(5) 0.0689(4) 0.0345(11) Uani 1 1 d . . .
H11 H 0.5621 0.6185 0.0636 0.041 Uiso 1 1 calc R . .
C12 C 0.3748(5) 0.5894(5) 0.0670(4) 0.0377(12) Uani 1 1 d . . .
H12 H 0.3534 0.5050 0.0607 0.045 Uiso 1 1 calc R . .
C13 C 0.2955(5) 0.6752(5) 0.0762(4) 0.0369(12) Uani 1 1 d . . .
H13 H 0.2117 0.6572 0.0755 0.044 Uiso 1 1 calc R . .
C14 C 0.1936(7) 0.9339(7) -0.0617(6) 0.0675(19) Uani 1 1 d . . .
H14A H 0.1519 1.0040 -0.0652 0.101 Uiso 1 1 calc R . .
H14B H 0.1294 0.8601 -0.0878 0.101 Uiso 1 1 calc R . .
H14C H 0.2466 0.9347 -0.1041 0.101 Uiso 1 1 calc R . .
C15 C 0.1928(7) 0.9513(7) 0.1610(6) 0.071(2) Uani 1 1 d U . .
H15A H 0.2460 0.9689 0.2345 0.107 Uiso 1 1 calc R . .
H15B H 0.1337 0.8751 0.1443 0.107 Uiso 1 1 calc R . .
H15C H 0.1450 1.0163 0.1459 0.107 Uiso 1 1 calc R . .
C16 C 0.4308(6) 1.0740(5) 0.1222(5) 0.0528(15) Uani 1 1 d . . .
H16A H 0.4767 1.0862 0.1968 0.079 Uiso 1 1 calc R . .
H16B H 0.3957 1.1458 0.1062 0.079 Uiso 1 1 calc R . .
H16C H 0.4891 1.0596 0.0856 0.079 Uiso 1 1 calc R . .
C17 C 0.2812(4) 0.5574(4) 0.2992(4) 0.0335(11) Uani 1 1 d D . .
C18 C 0.2533(5) 0.6793(5) 0.3113(4) 0.0389(12) Uani 1 1 d . . .
H18 H 0.1852 0.7053 0.2640 0.047 Uiso 1 1 calc R . .
C19 C 0.3432(5) 0.7530(5) 0.4041(4) 0.0416(13) Uani 1 1 d . . .
H19 H 0.3455 0.8355 0.4292 0.050 Uiso 1 1 calc R . .
C20 C 0.4300(6) 0.6803(6) 0.4532(4) 0.0474(15) Uani 1 1 d . . .
H20 H 0.5002 0.7059 0.5164 0.057 Uiso 1 1 calc R . .
C21 C 0.3917(5) 0.5636(5) 0.3902(4) 0.0407(13) Uani 1 1 d . . .
H21 H 0.4330 0.4978 0.4055 0.049 Uiso 1 1 calc R . .
C22A C 0.2721(12) 0.3007(9) 0.1903(11) 0.081(4) Uiso 0.552(9) 1 d PDU . .
C22B C 0.1861(14) 0.3411(11) 0.1000(8) 0.061(4) Uiso 0.448(9) 1 d PDU . .
C23A C 0.0588(10) 0.4341(11) 0.0908(7) 0.070(4) Uiso 0.552(9) 1 d PD . .
C23B C -0.0010(8) 0.4535(14) 0.1738(13) 0.078(5) Uiso 0.448(9) 1 d PD . .
C24A C 0.0797(11) 0.3513(10) 0.2992(9) 0.060(3) Uiso 0.552(9) 1 d PDU . .
C24B C 0.1538(15) 0.3036(10) 0.3067(10) 0.066(4) Uiso 0.448(9) 1 d PDU . .
C25 C 0.6836(5) 0.5102(5) 0.3915(4) 0.0377(12) Uani 1 1 d . . .
H25 H 0.6821 0.5646 0.4492 0.045 Uiso 1 1 calc R . .
C26 C 0.7484(5) 0.4155(6) 0.4099(5) 0.0441(13) Uani 1 1 d . . .
H26 H 0.7900 0.4065 0.4786 0.053 Uiso 1 1 calc R . .
C27 C 0.7516(6) 0.3333(5) 0.3257(5) 0.0487(14) Uani 1 1 d . . .
H27 H 0.7951 0.2680 0.3365 0.058 Uiso 1 1 calc R . .
C28 C 0.6889(6) 0.3502(5) 0.2249(5) 0.0458(14) Uani 1 1 d . . .
H28 H 0.6898 0.2966 0.1665 0.055 Uiso 1 1 calc R . .
C29 C 0.6248(5) 0.4479(5) 0.2123(4) 0.0384(12) Uani 1 1 d . . .
H29 H 0.5820 0.4578 0.1441 0.046 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'
Ce Ce -0.2486 2.6331 '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 Ce C19 117.34(15) . . ?
N Ce C20 89.72(16) . . ?
C19 Ce C20 29.07(17) . . ?
N Ce C12 81.60(14) . . ?
C19 Ce C12 119.89(16) . . ?
C20 Ce C12 128.25(16) . . ?
N Ce C3 126.90(15) . . ?
C19 Ce C3 81.76(16) . . ?
C20 Ce C3 91.25(17) . . ?
C12 Ce C3 133.82(16) . . ?
N Ce C13 109.60(14) . . ?
C19 Ce C13 99.57(16) . . ?
C20 Ce C13 119.98(16) . . ?
C12 Ce C13 28.81(15) . . ?
C3 Ce C13 115.37(17) . . ?
N Ce C2 108.96(14) . . ?
C19 Ce C2 110.23(15) . . ?
C20 Ce C2 115.25(16) . . ?
C12 Ce C2 115.82(16) . . ?
C3 Ce C2 28.53(15) . . ?
C13 Ce C2 110.79(16) . . ?
N Ce C5 81.23(15) . . ?
C19 Ce C5 91.95(16) . . ?
C20 Ce C5 78.34(16) . . ?
C12 Ce C5 148.06(16) . . ?
C3 Ce C5 47.30(17) . . ?
C13 Ce C5 157.69(16) . . ?
C2 Ce C5 46.97(16) . . ?
N Ce C1 81.47(15) . . ?
C19 Ce C1 117.68(15) . . ?
C20 Ce C1 107.18(16) . . ?
C12 Ce C1 121.49(15) . . ?
C3 Ce C1 47.87(16) . . ?
C13 Ce C1 131.06(15) . . ?
C2 Ce C1 28.97(16) . . ?
C5 Ce C1 28.84(15) . . ?
N Ce C9 125.26(14) . . ?
C19 Ce C9 107.25(16) . . ?
C20 Ce C9 135.32(17) . . ?
C12 Ce C9 48.08(16) . . ?
C3 Ce C9 88.00(17) . . ?
C13 Ce C9 29.37(15) . . ?
C2 Ce C9 81.67(16) . . ?
C5 Ce C9 128.61(15) . . ?
C1 Ce C9 105.04(15) . . ?
N Ce C4 107.29(15) . . ?
C19 Ce C4 70.46(15) . . ?
C20 Ce C4 68.28(16) . . ?
C12 Ce C4 162.16(16) . . ?
C3 Ce C4 29.00(16) . . ?
C13 Ce C4 142.06(17) . . ?
C2 Ce C4 47.02(16) . . ?
C5 Ce C4 28.30(16) . . ?
C1 Ce C4 47.48(15) . . ?
C9 Ce C4 116.69(16) . . ?
N Ce C11 78.22(14) . . ?
C19 Ce C11 146.58(16) . . ?
C20 Ce C11 154.90(16) . . ?
C12 Ce C11 28.78(14) . . ?
C3 Ce C11 113.63(16) . . ?
C13 Ce C11 47.28(15) . . ?
C2 Ce C11 89.61(15) . . ?
C5 Ce C11 120.58(15) . . ?
C1 Ce C11 92.86(15) . . ?
C9 Ce C11 47.60(15) . . ?
C4 Ce C11 136.26(15) . . ?
C8 Si1 C6 108.9(3) . . ?
C8 Si1 C7 107.5(3) . . ?
C6 Si1 C7 110.4(3) . . ?
C8 Si1 C1 107.3(3) . . ?
C6 Si1 C1 109.6(3) . . ?
C7 Si1 C1 112.9(2) . . ?
C16 Si2 C9 109.8(3) . . ?
C16 Si2 C15 111.8(3) . . ?
C9 Si2 C15 110.1(3) . . ?
C16 Si2 C14 108.2(3) . . ?
C9 Si2 C14 109.0(3) . . ?
C15 Si2 C14 107.9(4) . . ?
C22B Si3 C17 119.2(4) . . ?
C17 Si3 C23A 112.7(4) . . ?
C17 Si3 C24A 109.2(4) . . ?
C23A Si3 C24A 112.2(6) . . ?
C22B Si3 C24B 112.8(7) . . ?
C17 Si3 C24B 110.4(4) . . ?
C17 Si3 C22A 106.9(4) . . ?
C23A Si3 C22A 106.8(6) . . ?
C24A Si3 C22A 108.9(6) . . ?
C22B Si3 C23B 104.2(7) . . ?
C17 Si3 C23B 106.6(4) . . ?
C24B Si3 C23B 101.6(8) . . ?
C29 N C25 116.0(5) . . ?
C29 N Ce 126.2(3) . . ?
C25 N Ce 117.8(3) . . ?
C2 C1 C5 105.8(5) . . ?
C2 C1 Si1 125.6(4) . . ?
C5 C1 Si1 126.2(4) . . ?
C2 C1 Ce 75.0(3) . . ?
C5 C1 Ce 75.6(3) . . ?
Si1 C1 Ce 128.5(2) . . ?
C3 C2 C1 109.6(5) . . ?
C3 C2 Ce 75.4(3) . . ?
C1 C2 Ce 76.0(3) . . ?
C2 C3 C4 107.2(5) . . ?
C2 C3 Ce 76.0(3) . . ?
C4 C3 Ce 76.5(3) . . ?
C5 C4 C3 107.9(5) . . ?
C5 C4 Ce 75.6(3) . . ?
C3 C4 Ce 74.5(3) . . ?
C4 C5 C1 109.4(5) . . ?
C4 C5 Ce 76.1(3) . . ?
C1 C5 Ce 75.6(3) . . ?
C10 C9 C13 105.5(5) . . ?
C10 C9 Si2 126.7(4) . . ?
C13 C9 Si2 126.4(4) . . ?
C10 C9 Ce 76.3(3) . . ?
C13 C9 Ce 74.5(3) . . ?
Si2 C9 Ce 124.6(2) . . ?
C11 C10 C9 110.0(5) . . ?
C11 C10 Ce 75.4(3) . . ?
C9 C10 Ce 75.0(3) . . ?
C10 C11 C12 107.8(5) . . ?
C10 C11 Ce 76.4(3) . . ?
C12 C11 Ce 74.2(3) . . ?
C13 C12 C11 108.1(5) . . ?
C13 C12 Ce 75.9(3) . . ?
C11 C12 Ce 77.0(3) . . ?
C12 C13 C9 108.6(5) . . ?
C12 C13 Ce 75.3(3) . . ?
C9 C13 Ce 76.2(3) . . ?
C21 C17 C18 103.7(4) . . ?
C21 C17 Si3 124.4(4) . . ?
C18 C17 Si3 127.7(4) . . ?
C21 C17 Ce 73.7(3) . . ?
C18 C17 Ce 72.9(3) . . ?
Si3 C17 Ce 135.5(2) . . ?
C19 C18 C17 110.0(5) . . ?
C19 C18 Ce 73.5(3) . . ?
C17 C18 Ce 78.4(3) . . ?
C18 C19 C20 107.7(5) . . ?
C18 C19 Ce 78.0(3) . . ?
C20 C19 Ce 75.8(3) . . ?
C21 C20 C19 107.4(5) . . ?
C21 C20 Ce 78.4(3) . . ?
C19 C20 Ce 75.1(3) . . ?
C20 C21 C17 111.2(5) . . ?
C20 C21 Ce 73.4(3) . . ?
C17 C21 Ce 78.0(3) . . ?
N C25 C26 123.5(5) . . ?
C25 C26 C27 119.4(5) . . ?
C28 C27 C26 118.5(5) . . ?
C27 C28 C29 118.9(5) . . ?
N C29 C28 123.6(5) . . ?
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
Ce N 2.704(4) . ?
Ce C19 2.797(5) . ?
Ce C20 2.807(5) . ?
Ce C12 2.816(5) . ?
Ce C3 2.823(5) . ?
Ce C13 2.825(5) . ?
Ce C2 2.830(5) . ?
Ce C5 2.843(5) . ?
Ce C1 2.843(5) . ?
Ce C9 2.847(5) . ?
Ce C4 2.849(5) . ?
Ce C11 2.851(5) . ?
Ce C18 2.853(5) . ?
Ce C10 2.863(5) . ?
Ce C21 2.868(5) . ?
Ce C17 2.924(5) . ?
Si1 C8 1.855(6) . ?
Si1 C6 1.858(7) . ?
Si1 C7 1.871(6) . ?
Si1 C1 1.873(6) . ?
Si2 C16 1.854(6) . ?
Si2 C9 1.859(6) . ?
Si2 C15 1.876(6) . ?
Si2 C14 1.884(7) . ?
Si3 C22B 1.802(8) . ?
Si3 C17 1.844(4) . ?
Si3 C23A 1.855(8) . ?
Si3 C24A 1.865(7) . ?
Si3 C24B 1.877(8) . ?
Si3 C22A 1.896(8) . ?
Si3 C23B 1.922(8) . ?
N C29 1.343(6) . ?
N C25 1.362(6) . ?
C1 C2 1.419(8) . ?
C1 C5 1.416(7) . ?
C2 C3 1.393(7) . ?
C3 C4 1.420(8) . ?
C4 C5 1.391(8) . ?
C9 C10 1.413(7) . ?
C9 C13 1.438(7) . ?
C10 C11 1.394(7) . ?
C11 C12 1.409(7) . ?
C12 C13 1.403(8) . ?
C17 C21 1.418(7) . ?
C17 C18 1.435(7) . ?
C18 C19 1.392(8) . ?
C19 C20 1.406(8) . ?
C20 C21 1.383(8) . ?
C25 C26 1.362(8) . ?
C26 C27 1.378(8) . ?
C27 C28 1.380(8) . ?
C28 C29 1.378(8) . ?
