#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304138.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_4304138
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 La N3 P6 Se6'
_chemical_formula_weight         1857.93
_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                   15.1824(5)
_cell_length_b                   15.1824(5)
_cell_length_c                   57.129(4)
_cell_measurement_temperature    141(2)
_cell_volume                     11404.3(10)
_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 0.991
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       75
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            35543
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.606
_exptl_absorpt_correction_T_max  0.8128
_exptl_absorpt_correction_T_min  0.6716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5484
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.694
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.729
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.729
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0206P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                1813
_reflns_number_total             3114
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701618a_si_04.cif
_cod_data_source_block           apx141
_cod_original_cell_volume        11404.2(10)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4304138
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
La1 La 0.6667 0.3333 0.0833 0.01390(11) Uani 1 6 d S . .
Se1 Se 0.50802(2) 0.20908(2) 0.044441(5) 0.02170(9) Uani 1 1 d . . .
P1 P 0.41602(6) 0.25480(6) 0.063389(12) 0.01676(19) Uani 1 1 d . . .
N1 N 0.4884(2) 0.3333 0.0833 0.0140(8) Uani 1 2 d S . .
C1 C 0.3044(2) 0.1453(2) 0.07519(5) 0.0187(7) Uani 1 1 d . . .
C2 C 0.2901(2) 0.1234(2) 0.09895(5) 0.0237(8) Uani 1 1 d . . .
H2 H 0.3399 0.1655 0.1096 0.028 Uiso 1 1 calc R . .
C3 C 0.2024(2) 0.0394(2) 0.10690(6) 0.0322(9) Uani 1 1 d . . .
H3 H 0.1935 0.0255 0.1229 0.039 Uiso 1 1 calc R . .
C4 C 0.1281(3) -0.0240(2) 0.09137(6) 0.0332(9) Uani 1 1 d . . .
H4 H 0.0688 -0.0800 0.0968 0.040 Uiso 1 1 calc R . .
C5 C 0.1419(2) -0.0039(2) 0.06761(6) 0.0312(9) Uani 1 1 d . . .
H5 H 0.0926 -0.0472 0.0570 0.037 Uiso 1 1 calc R . .
C6 C 0.2286(2) 0.0799(2) 0.05967(5) 0.0271(8) Uani 1 1 d . . .
H6 H 0.2371 0.0935 0.0437 0.032 Uiso 1 1 calc R . .
C7 C 0.3616(2) 0.3093(2) 0.04374(5) 0.0181(7) Uani 1 1 d . . .
C8 C 0.4072(2) 0.3513(2) 0.02240(5) 0.0239(8) Uani 1 1 d . . .
H8 H 0.4659 0.3511 0.0179 0.029 Uiso 1 1 calc R . .
C9 C 0.3650(3) 0.3934(2) 0.00792(5) 0.0342(9) Uani 1 1 d . . .
H9 H 0.3964 0.4225 -0.0062 0.041 Uiso 1 1 calc R . .
C10 C 0.2773(3) 0.3928(3) 0.01421(6) 0.0381(10) Uani 1 1 d . . .
H10 H 0.2489 0.4204 0.0043 0.046 Uiso 1 1 calc R . .
C11 C 0.2318(2) 0.3513(2) 0.03527(5) 0.0315(9) Uani 1 1 d . . .
H11 H 0.1727 0.3511 0.0396 0.038 Uiso 1 1 calc R . .
C12 C 0.2734(2) 0.3099(2) 0.05010(5) 0.0228(8) Uani 1 1 d . . .
H12 H 0.2424 0.2824 0.0644 0.027 Uiso 1 1 calc R . .
C13 C 0.0859(8) -0.0136(13) -0.00001(8) 0.099(3) Uani 1 1 d . . .
H13 H 0.1422 -0.0226 -0.0001 0.119 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'
La La -0.2871 2.4523 '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 La1 N1 120.0 2_655 3_665 ?
N1 La1 N1 120.0 2_655 . ?
N1 La1 N1 120.0 3_665 . ?
N1 La1 Se1 133.446(6) 2_655 17_554 ?
N1 La1 Se1 77.384(6) 3_665 17_554 ?
N1 La1 Se1 62.014(6) . 17_554 ?
N1 La1 Se1 62.012(6) 2_655 16_544 ?
N1 La1 Se1 133.446(6) 3_665 16_544 ?
N1 La1 Se1 77.386(6) . 16_544 ?
Se1 La1 Se1 74.979(10) 17_554 16_544 ?
N1 La1 Se1 77.383(6) 2_655 18_654 ?
N1 La1 Se1 62.013(6) 3_665 18_654 ?
N1 La1 Se1 133.447(6) . 18_654 ?
Se1 La1 Se1 74.978(10) 17_554 18_654 ?
Se1 La1 Se1 74.978(10) 16_544 18_654 ?
N1 La1 Se1 62.014(6) 2_655 2_655 ?
N1 La1 Se1 77.385(6) 3_665 2_655 ?
N1 La1 Se1 133.445(6) . 2_655 ?
Se1 La1 Se1 154.769(12) 17_554 2_655 ?
Se1 La1 Se1 124.026(12) 16_544 2_655 ?
Se1 La1 Se1 93.108(12) 18_654 2_655 ?
N1 La1 Se1 77.385(6) 2_655 . ?
N1 La1 Se1 133.445(6) 3_665 . ?
N1 La1 Se1 62.014(6) . . ?
Se1 La1 Se1 124.028(12) 17_554 . ?
Se1 La1 Se1 93.109(12) 16_544 . ?
Se1 La1 Se1 154.768(12) 18_654 . ?
Se1 La1 Se1 74.976(10) 2_655 . ?
N1 La1 Se1 133.445(6) 2_655 3_665 ?
N1 La1 Se1 62.014(6) 3_665 3_665 ?
N1 La1 Se1 77.385(6) . 3_665 ?
Se1 La1 Se1 93.109(12) 17_554 3_665 ?
Se1 La1 Se1 154.770(12) 16_544 3_665 ?
Se1 La1 Se1 124.028(12) 18_654 3_665 ?
Se1 La1 Se1 74.976(10) 2_655 3_665 ?
Se1 La1 Se1 74.976(10) . 3_665 ?
P1 Se1 La1 82.85(2) . . ?
N1 P1 C1 113.20(11) . . ?
N1 P1 C7 113.27(12) . . ?
C1 P1 C7 102.59(13) . . ?
N1 P1 Se1 106.40(11) . . ?
C1 P1 Se1 110.74(10) . . ?
C7 P1 Se1 110.72(10) . . ?
P1 N1 P1 143.8(2) 17_554 . ?
P1 N1 La1 108.11(11) 17_554 . ?
P1 N1 La1 108.11(11) . . ?
C2 C1 C6 118.4(3) . . ?
C2 C1 P1 123.1(2) . . ?
C6 C1 P1 118.5(2) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C3 C2 120.5(3) . . ?
C3 C4 C5 119.7(3) . . ?
C6 C5 C4 119.9(3) . . ?
C5 C6 C1 121.1(3) . . ?
C8 C7 C12 119.1(3) . . ?
C8 C7 P1 121.0(2) . . ?
C12 C7 P1 119.9(2) . . ?
C9 C8 C7 119.9(3) . . ?
C10 C9 C8 120.7(3) . . ?
C11 C10 C9 119.7(3) . . ?
C10 C11 C12 120.5(3) . . ?
C11 C12 C7 120.2(3) . . ?
C13 C13 C13 120.000(6) 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
La1 N1 2.706(3) 2_655 ?
La1 N1 2.706(3) 3_665 ?
La1 N1 2.706(3) . ?
La1 Se1 3.1228(3) 17_554 ?
La1 Se1 3.1229(3) 16_544 ?
La1 Se1 3.1229(3) 18_654 ?
La1 Se1 3.1230(3) 2_655 ?
La1 Se1 3.1230(3) . ?
La1 Se1 3.1230(3) 3_665 ?
Se1 P1 2.1386(8) . ?
P1 N1 1.6179(12) . ?
P1 C1 1.810(3) . ?
P1 C7 1.819(3) . ?
N1 P1 1.6177(12) 17_554 ?
C1 C2 1.389(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.381(4) . ?
C3 C4 1.379(4) . ?
C4 C5 1.384(4) . ?
C5 C6 1.372(4) . ?
C7 C8 1.389(4) . ?
C7 C12 1.393(4) . ?
C8 C9 1.383(4) . ?
C9 C10 1.375(4) . ?
C10 C11 1.373(4) . ?
C11 C12 1.381(4) . ?
C13 C13 1.419(4) 20 ?
C13 C13 1.419(4) 21 ?
