#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304140.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_4304140
loop_
_publ_author_name
'Andrew J. Gaunt'
'Sean D. Reilly'
'Alejandro E. Enriquez'
'Brian L. Scott'
'James A. Ibers'
'Perumal Sekar'
'Kieran I. M. Ingram'
'Nikolas Kaltsoyannis'
'Mary P. Neu'
_publ_contact_author_address
;
Los Alamos National Laboratory
MS F629
Los Alamos, NM  87544
;
_publ_contact_author_email       gaunt@lanl.gov
_publ_contact_author_name        'Andrew J. Gaunt'
_publ_section_title
;
Experimental and Theoretical Comparison of Actinide and Lanthanide Bonding
in M[N(EPR2)2]3 Complexes (M = U, Pu, La, Ce; E = S, Se, Te; R = Ph,iPr, H)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              29
_journal_page_last               41
_journal_paper_doi               10.1021/ic701618a
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C79 H68 Ce N3 P6 Se6'
_chemical_formula_weight         1859.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.1571(3)
_cell_length_b                   15.1571(3)
_cell_length_c                   57.057(3)
_cell_measurement_temperature    141(2)
_cell_volume                     11352.0(7)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      141(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_diffrn_measurement_method       'ω 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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            39972
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.659
_exptl_absorpt_correction_T_max  0.7111
_exptl_absorpt_correction_T_min  0.7111
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5490
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0232
_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)+(0.0190P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0489
_reflns_number_gt                2022
_reflns_number_total             3021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701618a_si_06.cif
_cod_data_source_block           apx175me
_cod_original_cell_volume        11352.0(6)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4304140
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Ce1 Ce 0.6667 0.3333 0.0833 0.01388(10) Uani 1 6 d S . .
Se1 Se 0.50954(2) 0.20926(2) 0.044580(5) 0.02135(9) Uani 1 1 d . . .
P1 P 0.41680(5) 0.25475(6) 0.063383(12) 0.01663(17) Uani 1 1 d . . .
N1 N 0.48912(19) 0.3333 0.0833 0.0139(7) Uani 1 2 d S . .
C1 C 0.30456(19) 0.1449(2) 0.07519(5) 0.0187(6) Uani 1 1 d . . .
C2 C 0.2903(2) 0.1231(2) 0.09890(5) 0.0235(7) Uani 1 1 d . . .
H2 H 0.3402 0.1651 0.1095 0.028 Uiso 1 1 calc R . .
C3 C 0.2020(2) 0.0390(2) 0.10684(5) 0.0320(8) Uani 1 1 d . . .
H3 H 0.1925 0.0254 0.1228 0.038 Uiso 1 1 calc R . .
C4 C 0.1281(2) -0.0245(2) 0.09127(5) 0.0335(8) Uani 1 1 d . . .
H4 H 0.0689 -0.0807 0.0967 0.040 Uiso 1 1 calc R . .
C5 C 0.1421(2) -0.0047(2) 0.06753(6) 0.0316(8) Uani 1 1 d . . .
H5 H 0.0928 -0.0482 0.0570 0.038 Uiso 1 1 calc R . .
C6 C 0.2294(2) 0.0796(2) 0.05950(5) 0.0266(7) Uani 1 1 d . . .
H6 H 0.2382 0.0931 0.0435 0.032 Uiso 1 1 calc R . .
C7 C 0.3626(2) 0.3092(2) 0.04358(5) 0.0189(6) Uani 1 1 d . . .
C8 C 0.4083(2) 0.3513(2) 0.02224(5) 0.0238(7) Uani 1 1 d . . .
H8 H 0.4673 0.3512 0.0178 0.029 Uiso 1 1 calc R . .
C9 C 0.3660(2) 0.3935(2) 0.00761(5) 0.0333(8) Uani 1 1 d . . .
H9 H 0.3970 0.4220 -0.0066 0.040 Uiso 1 1 calc R . .
C10 C 0.2785(2) 0.3932(2) 0.01408(5) 0.0380(9) Uani 1 1 d . . .
H10 H 0.2503 0.4211 0.0042 0.046 Uiso 1 1 calc R . .
C11 C 0.2325(2) 0.3515(2) 0.03522(5) 0.0303(8) Uani 1 1 d . . .
H11 H 0.1732 0.3514 0.0395 0.036 Uiso 1 1 calc R . .
C12 C 0.2743(2) 0.3100(2) 0.05011(5) 0.0227(7) Uani 1 1 d . . .
H12 H 0.2435 0.2828 0.0644 0.027 Uiso 1 1 calc R . .
C13 C 0.0897(6) -0.0048(12) 0.00002(8) 0.123(5) Uani 1 1 d D . .
H13 H 0.1494 -0.0079 0.0001 0.147 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
H H 0.0000 0.0000 '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
N1 Ce1 N1 120.0 2_655 3_665 ?
N1 Ce1 N1 120.0 2_655 . ?
N1 Ce1 N1 120.0 3_665 . ?
N1 Ce1 Se1 133.405(6) 2_655 17_554 ?
N1 Ce1 Se1 77.147(5) 3_665 17_554 ?
N1 Ce1 Se1 62.309(5) . 17_554 ?
N1 Ce1 Se1 62.307(5) 2_655 16_544 ?
N1 Ce1 Se1 133.406(6) 3_665 16_544 ?
N1 Ce1 Se1 77.149(5) . 16_544 ?
Se1 Ce1 Se1 74.790(9) 17_554 16_544 ?
N1 Ce1 Se1 77.147(5) 2_655 18_654 ?
N1 Ce1 Se1 62.308(5) 3_665 18_654 ?
N1 Ce1 Se1 133.407(6) . 18_654 ?
Se1 Ce1 Se1 74.790(9) 17_554 18_654 ?
Se1 Ce1 Se1 74.789(9) 16_544 18_654 ?
N1 Ce1 Se1 62.309(5) 2_655 2_655 ?
N1 Ce1 Se1 77.148(5) 3_665 2_655 ?
N1 Ce1 Se1 133.404(6) . 2_655 ?
Se1 Ce1 Se1 154.296(11) 17_554 2_655 ?
Se1 Ce1 Se1 124.615(11) 16_544 2_655 ?
Se1 Ce1 Se1 93.189(11) 18_654 2_655 ?
N1 Ce1 Se1 77.148(5) 2_655 . ?
N1 Ce1 Se1 133.404(6) 3_665 . ?
N1 Ce1 Se1 62.309(5) . . ?
Se1 Ce1 Se1 124.617(11) 17_554 . ?
Se1 Ce1 Se1 93.190(11) 16_544 . ?
Se1 Ce1 Se1 154.295(11) 18_654 . ?
Se1 Ce1 Se1 74.787(9) 2_655 . ?
N1 Ce1 Se1 133.404(6) 2_655 3_665 ?
N1 Ce1 Se1 62.309(5) 3_665 3_665 ?
N1 Ce1 Se1 77.148(5) . 3_665 ?
Se1 Ce1 Se1 93.191(11) 17_554 3_665 ?
Se1 Ce1 Se1 154.297(11) 16_544 3_665 ?
Se1 Ce1 Se1 124.617(11) 18_654 3_665 ?
Se1 Ce1 Se1 74.787(9) 2_655 3_665 ?
Se1 Ce1 Se1 74.787(9) . 3_665 ?
P1 Se1 Ce1 82.88(2) . . ?
N1 P1 C1 113.23(10) . . ?
N1 P1 C7 113.40(11) . . ?
C1 P1 C7 102.59(13) . . ?
N1 P1 Se1 106.15(11) . . ?
C1 P1 Se1 110.88(9) . . ?
C7 P1 Se1 110.68(9) . . ?
P1 N1 P1 143.9(2) 17_554 . ?
P1 N1 Ce1 108.05(10) 17_554 . ?
P1 N1 Ce1 108.05(10) . . ?
C2 C1 C6 118.9(3) . . ?
C2 C1 P1 123.0(2) . . ?
C6 C1 P1 118.1(2) . . ?
C1 C2 C3 120.2(3) . . ?
C4 C3 C2 120.5(3) . . ?
C3 C4 C5 119.9(3) . . ?
C6 C5 C4 119.9(3) . . ?
C5 C6 C1 120.6(3) . . ?
C8 C7 C12 119.3(3) . . ?
C8 C7 P1 121.3(2) . . ?
C12 C7 P1 119.4(2) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 120.2(3) . . ?
C9 C10 C11 120.3(3) . . ?
C10 C11 C12 120.2(3) . . ?
C11 C12 C7 120.0(3) . . ?
C13 C13 C13 120.000(7) 20 21 ?
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
Ce1 N1 2.691(3) 2_655 ?
Ce1 N1 2.691(3) 3_665 ?
Ce1 N1 2.691(3) . ?
Ce1 Se1 3.1013(3) 17_554 ?
Ce1 Se1 3.1014(3) 16_544 ?
Ce1 Se1 3.1014(3) 18_654 ?
Ce1 Se1 3.1015(3) 2_655 ?
Ce1 Se1 3.1015(3) . ?
Ce1 Se1 3.1015(3) 3_665 ?
Se1 P1 2.1381(8) . ?
P1 N1 1.6157(11) . ?
P1 C1 1.813(3) . ?
P1 C7 1.819(3) . ?
N1 P1 1.6155(11) 17_554 ?
C1 C2 1.384(3) . ?
C1 C6 1.397(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.375(4) . ?
C4 C5 1.381(4) . ?
C5 C6 1.379(4) . ?
C7 C8 1.388(3) . ?
C7 C12 1.396(4) . ?
C8 C9 1.388(4) . ?
C9 C10 1.374(4) . ?
C10 C11 1.378(4) . ?
C11 C12 1.385(4) . ?
C13 C13 1.398(4) 20 ?
C13 C13 1.398(4) 21 ?
