#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/17/7011765.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_7011765
loop_
_publ_author_name
'Jean-Claude Berthet'
'Yannick Miquel'
'Peter B. Iveson'
'Martine Nierlich'
'Pierre Thuéry'
'Charles Madic'
'Michel Ephritikhine'
_publ_section_title
;
 The affinity and selectivity of terdentate nitrogen ligands towards
 trivalent lanthanide and uranium ions viewed from the crystal
 structures of the 1 ∶ 3 complexes
;
_journal_issue                   16
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3265
_journal_page_last               3272
_journal_paper_doi               10.1039/b203725d
_journal_year                    2002
_chemical_formula_sum            'C51 H42 Ce I3 N12'
_chemical_formula_weight         1343.79
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :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            3
_cell_length_a                   12.6180(18)
_cell_length_b                   12.6180(18)
_cell_length_c                   27.903(6)
_cell_measurement_reflns_used    7985
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     3847.4(11)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997)'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997)'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick,1997)'
_computing_publication_material  'SHELXTL (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       'φ rotation scans with 2°steps'
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            7985
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         3.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.740
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'MULABS in PLATON;Spek,1998'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1947
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0333
_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)+(0.0468P)²+26.9124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                1316
_reflns_number_total             1362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203725d.txt
_cod_data_source_block           2.3MeCN
_cod_original_sg_symbol_H-M      R32
_cod_database_code               7011765
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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 0.6667 0.3333 0.8333 0.0180(2) Uani 1 6 d S . .
I I 1.0000 0.30898(6) 1.0000 0.0415(2) Uani 1 2 d S . .
N1 N 0.6879(6) 0.1818(5) 0.89289(18) 0.0323(13) Uani 1 1 d . . .
N2 N 0.8786(6) 0.3333 0.8333 0.0202(15) Uani 1 2 d S . .
C1 C 0.5959(7) 0.1060(7) 0.9204(2) 0.0348(15) Uani 1 1 d . . .
H1A H 0.5355 0.1253 0.9276 0.042 Uiso 1 1 calc R . .
C2 C 0.5848(8) -0.0006(7) 0.9391(3) 0.0393(17) Uani 1 1 d . . .
H2A H 0.5177 -0.0508 0.9582 0.047 Uiso 1 1 calc R . .
C3 C 0.6694(7) -0.0327(6) 0.9301(3) 0.0357(16) Uani 1 1 d . . .
H3A H 0.6602 -0.1061 0.9416 0.043 Uiso 1 1 calc R . .
C4 C 0.7735(8) 0.0486(8) 0.9026(3) 0.0424(18) Uani 1 1 d . . .
H4A H 0.8361 0.0316 0.8967 0.051 Uiso 1 1 calc R . .
C5 C 0.7792(7) 0.1554(7) 0.8845(2) 0.0338(15) Uani 1 1 d . . .
C6 C 0.8880(6) 0.2465(6) 0.8576(2) 0.0309(15) Uani 1 1 d . . .
C7 C 0.9978(7) 0.2456(9) 0.8585(3) 0.046(2) Uani 1 1 d . . .
H7A H 1.0042 0.1863 0.8760 0.055 Uiso 1 1 calc R . .
C8 C 1.0969(8) 0.3333 0.8333 0.048(3) Uani 1 2 d S . .
H8A H 1.1706 0.3333 0.8333 0.058 Uiso 1 2 calc SR . .
C9 C 1.0000 0.0000 0.9728(6) 0.051(3) Uani 1 3 d S . .
N3 N 1.0000 0.0000 0.9278(9) 0.050(5) Uani 0.50 3 d SP . .
N4B N 1.0000 0.0000 0.8212(17) 0.068(8) Uani 0.50 3 d SP . .
C11 C 1.0000 0.0000 0.7859(13) 0.102(9) Uani 1 3 d S . .
C10 C 1.0000 0.0000 0.739(2) 0.141(17) Uani 1 3 d S . .
N4A N 1.0000 0.0000 0.6913(10) 0.058(7) Uani 0.50 3 d SP . .
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'
I I -0.4742 1.8119 '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
N1 Ce N1 78.7(2) 18_656 . ?
N1 Ce N1 84.73(17) 18_656 16_546 ?
N1 Ce N1 143.8(3) . 16_546 ?
N1 Ce N1 84.72(17) 18_656 17_556 ?
N1 Ce N1 124.9(3) . 17_556 ?
N1 Ce N1 84.73(17) 16_546 17_556 ?
N1 Ce N1 143.8(3) 18_656 2_655 ?
N1 Ce N1 84.73(17) . 2_655 ?
N1 Ce N1 124.9(3) 16_546 2_655 ?
N1 Ce N1 78.7(2) 17_556 2_655 ?
N1 Ce N1 124.9(3) 18_656 3_665 ?
N1 Ce N1 84.73(17) . 3_665 ?
N1 Ce N1 78.7(2) 16_546 3_665 ?
N1 Ce N1 143.8(3) 17_556 3_665 ?
N1 Ce N1 84.73(17) 2_655 3_665 ?
N1 Ce N2 71.90(13) 18_656 . ?
N1 Ce N2 62.45(13) . . ?
N1 Ce N2 140.63(11) 16_546 . ?
N1 Ce N2 62.45(13) 17_556 . ?
N1 Ce N2 71.90(13) 2_655 . ?
N1 Ce N2 140.63(11) 3_665 . ?
N1 Ce N2 62.45(13) 18_656 3_665 ?
N1 Ce N2 71.90(13) . 3_665 ?
N1 Ce N2 71.90(13) 16_546 3_665 ?
N1 Ce N2 140.63(12) 17_556 3_665 ?
N1 Ce N2 140.64(12) 2_655 3_665 ?
N1 Ce N2 62.45(13) 3_665 3_665 ?
N2 Ce N2 119.999(2) . 3_665 ?
N1 Ce N2 140.63(11) 18_656 2_655 ?
N1 Ce N2 140.64(11) . 2_655 ?
N1 Ce N2 62.45(13) 16_546 2_655 ?
N1 Ce N2 71.90(13) 17_556 2_655 ?
N1 Ce N2 62.45(13) 2_655 2_655 ?
N1 Ce N2 71.90(13) 3_665 2_655 ?
N2 Ce N2 119.999(5) . 2_655 ?
N2 Ce N2 120.002(2) 3_665 2_655 ?
C1 N1 C5 117.7(6) . . ?
C6 N2 C6 120.4(8) 17_556 . ?
N1 C1 C2 123.3(7) . . ?
C3 C2 C1 121.0(8) . . ?
C2 C3 C4 118.1(7) . . ?
C5 C4 C3 118.2(7) . . ?
N1 C5 C4 121.7(7) . . ?
N1 C5 C6 117.6(6) . . ?
C4 C5 C6 120.6(7) . . ?
N2 C6 C7 120.8(7) . . ?
N2 C6 C5 117.6(6) . . ?
C7 C6 C5 121.6(7) . . ?
C8 C7 C6 119.4(8) . . ?
C7 C8 C7 119.2(10) 17_556 . ?
N3 C9 C9 179.999(12) . 4_647 ?
N4B C11 C10 180.00(3) . . ?
C11 C10 N4A 180.000(16) . . ?
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 N1 2.646(5) 18_656 ?
Ce N1 2.646(5) . ?
Ce N1 2.646(5) 16_546 ?
Ce N1 2.646(5) 17_556 ?
Ce N1 2.646(5) 2_655 ?
Ce N1 2.646(5) 3_665 ?
Ce N2 2.674(7) . ?
Ce N2 2.674(7) 3_665 ?
Ce N2 2.674(7) 2_655 ?
N1 C1 1.321(9) . ?
N1 C5 1.370(9) . ?
N2 C6 1.343(8) 17_556 ?
N2 C6 1.343(8) . ?
C1 C2 1.383(11) . ?
C2 C3 1.342(11) . ?
C3 C4 1.421(12) . ?
C4 C5 1.407(11) . ?
C5 C6 1.481(10) . ?
C6 C7 1.391(11) . ?
C7 C8 1.378(10) . ?
C8 C7 1.378(10) 17_556 ?
C9 N3 1.25(3) . ?
C9 C9 1.52(3) 4_647 ?
N4B C11 0.99(4) . ?
C11 C10 1.30(6) . ?
C10 N4A 1.34(6) . ?
