#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:53:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179768 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/64/7006487.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_7006487
loop_
_publ_author_name
'Foreman, Mark R. S.'
'Hudson, Michael J.'
'Drew, Michael G. B.'
'Hill, Clément'
'Madic, Charles'
_publ_section_title
;
 Complexes formed between the quadridentate, heterocyclic molecules
 6,6'-bis-(5,6-dialkyl-1,2,4-triazin-3-yl)-2,2'-bipyridine (BTBP) and
 lanthanides(III): implications for the partitioning of actinides(III)
 and lanthanides(III).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1645
_journal_page_last               1653
_journal_paper_doi               10.1039/b511321k
_journal_year                    2006
_chemical_formula_sum            'C24 H28 Ce N11 O10'
_chemical_formula_weight         770.69
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.834(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.859(9)
_cell_length_b                   11.992(13)
_cell_length_c                   15.897(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1664(3)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1042
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8614
_diffrn_reflns_theta_full        25.91
_diffrn_reflns_theta_max         25.91
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIFABS, Walker, N. and Stuart, D., Acta Cryst 1983 A39 158.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       needle
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         9.701
_refine_diff_density_min         -1.807
_refine_diff_density_rms         0.333
_refine_ls_extinction_coef       0.0156(43)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         3201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_obs          0.1202
_refine_ls_shift/esd_max         0.083
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.1894P)²+37.5152P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3225
_refine_ls_wR_factor_obs         0.3036
_reflns_number_observed          2585
_reflns_number_total             3201
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b511321k.txt
_cod_data_source_block           ce
_cod_original_cell_volume        1664.0(30)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7006487
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ce1 Ce 0.0000 0.20717(9) 0.2500 0.0214(5) Uani 1 d S .
N1 N 0.1618(18) 0.3184(11) 0.0781(10) 0.042(3) Uani 1 d . .
N2 N 0.1372(15) 0.2167(12) 0.1128(9) 0.037(3) Uani 1 d . .
C3 C 0.1725(16) 0.1264(13) 0.0744(9) 0.029(3) Uani 1 d . .
N4 N 0.2387(16) 0.1224(13) 0.0031(9) 0.043(3) Uani 1 d . .
C5 C 0.2726(21) 0.2205(16) -0.0268(13) 0.048(5) Uani 1 d . .
C6 C 0.2299(25) 0.3201(16) 0.0092(13) 0.054(5) Uani 1 d . .
C7 C 0.1386(18) 0.0125(14) 0.1085(10) 0.037(4) Uani 1 d . .
N8 N 0.0661(14) 0.0132(11) 0.1781(8) 0.033(3) Uani 1 d . .
C9 C 0.0370(22) -0.0859(13) 0.2117(10) 0.038(4) Uani 1 d . .
C10 C 0.0523(36) -0.1936(12) 0.1654(17) 0.054(5) Uani 1 d . .
H10 H 0.0012 -0.2590 0.1745 0.065 Uiso 1 calc R .
C11 C 0.1532(27) -0.1830(16) 0.1068(13) 0.055(5) Uani 1 d . .
H11 H 0.2018 -0.2462 0.0905 0.066 Uiso 1 calc R .
C12 C 0.1820(21) -0.0801(15) 0.0727(11) 0.044(4) Uani 1 d . .
H12 H 0.2309 -0.0759 0.0254 0.052 Uiso 1 calc R .
C51 C 0.3559(25) 0.2196(19) -0.1032(13) 0.059(6) Uani 1 d . .
H51A H 0.2919 0.2566 -0.1506 0.071 Uiso 1 calc R .
H51B H 0.4494 0.2627 -0.0888 0.071 Uiso 1 calc R .
C52 C 0.3966(26) 0.1042(21) -0.1321(15) 0.071(6) Uani 1 d . .
H52C H 0.4486 0.0631 -0.0839 0.085 Uiso 1 calc R .
H52D H 0.4622 0.1112 -0.1740 0.085 Uiso 1 calc R .
H52E H 0.3047 0.0656 -0.1565 0.085 Uiso 1 calc R .
C61 C 0.2592(38) 0.4328(19) -0.0270(18) 0.087(9) Uani 1 d . .
H61A H 0.3661 0.4356 -0.0334 0.104 Uiso 1 calc R .
H61B H 0.1986 0.4378 -0.0838 0.104 Uiso 1 calc R .
C62 C 0.2272(42) 0.5314(19) 0.0206(21) 0.100(10) Uani 1 d . .
H62C H 0.1262 0.5257 0.0345 0.120 Uiso 1 calc R .
H62D H 0.2333 0.5967 -0.0136 0.120 Uiso 1 calc R .
H62E H 0.3009 0.5367 0.0722 0.120 Uiso 1 calc R .
O41 O 0.1872(19) 0.1958(14) 0.3923(10) 0.068(4) Uani 1 d . .
N43 N 0.3113(20) 0.1968(15) 0.3645(11) 0.056(4) Uani 1 d . .
O44 O 0.4361(21) 0.2091(21) 0.4067(13) 0.108(8) Uani 1 d . .
O42 O 0.2947(16) 0.1867(13) 0.2810(10) 0.063(4) Uani 1 d . .
O51 O -0.1093(20) 0.4025(12) 0.2149(12) 0.079(5) Uani 1 d . .
O52 O 0.0000 0.5605(18) 0.2500 0.125(13) Uani 1 d S .
N53 N 0.0000 0.4569(17) 0.2500 0.057(6) Uani 1 d S .
O100 O 0.5000 0.4403(46) -0.2500 0.088(15) Uiso 0.50 d SP .
O200 O 0.5000 0.4223(41) 0.2500 0.077(13) Uiso 0.50 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'
O O 0.0106 0.0060 '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
O51 Ce1 O51 47.5(7) . 4_556 ?
O51 Ce1 O41 113.8(5) . . ?
O51 Ce1 O41 72.2(5) 4_556 . ?
O51 Ce1 O41 72.2(5) . 4_556 ?
O51 Ce1 O41 113.8(5) 4_556 4_556 ?
O41 Ce1 O41 173.9(7) . 4_556 ?
O51 Ce1 O42 73.3(5) . 4_556 ?
O51 Ce1 O42 117.4(5) 4_556 4_556 ?
O41 Ce1 O42 129.9(5) . 4_556 ?
O41 Ce1 O42 49.3(5) 4_556 4_556 ?
O51 Ce1 O42 117.4(5) . . ?
O51 Ce1 O42 73.3(5) 4_556 . ?
O41 Ce1 O42 49.3(5) . . ?
O41 Ce1 O42 129.9(5) 4_556 . ?
O42 Ce1 O42 169.1(7) 4_556 . ?
O51 Ce1 N2 86.0(5) . 4_556 ?
O51 Ce1 N2 89.5(5) 4_556 4_556 ?
O41 Ce1 N2 66.4(5) . 4_556 ?
O41 Ce1 N2 113.9(5) 4_556 4_556 ?
O42 Ce1 N2 64.8(5) 4_556 4_556 ?
O42 Ce1 N2 115.7(5) . 4_556 ?
O51 Ce1 N2 89.5(5) . . ?
O51 Ce1 N2 86.0(5) 4_556 . ?
O41 Ce1 N2 113.9(5) . . ?
O41 Ce1 N2 66.4(5) 4_556 . ?
O42 Ce1 N2 115.7(5) 4_556 . ?
O42 Ce1 N2 64.8(5) . . ?
N2 Ce1 N2 175.1(6) 4_556 . ?
O51 Ce1 N8 142.9(5) . . ?
O51 Ce1 N8 141.2(5) 4_556 . ?
O41 Ce1 N8 99.9(5) . . ?
O41 Ce1 N8 74.7(4) 4_556 . ?
O42 Ce1 N8 97.1(5) 4_556 . ?
O42 Ce1 N8 73.4(4) . . ?
N2 Ce1 N8 122.9(4) 4_556 . ?
N2 Ce1 N8 61.9(4) . . ?
O51 Ce1 N8 141.2(5) . 4_556 ?
O51 Ce1 N8 142.9(5) 4_556 4_556 ?
O41 Ce1 N8 74.7(4) . 4_556 ?
O41 Ce1 N8 99.9(5) 4_556 4_556 ?
O42 Ce1 N8 73.4(4) 4_556 4_556 ?
O42 Ce1 N8 97.1(5) . 4_556 ?
N2 Ce1 N8 61.9(4) 4_556 4_556 ?
N2 Ce1 N8 122.9(4) . 4_556 ?
N8 Ce1 N8 61.0(5) . 4_556 ?
C6 N1 N2 117.9(14) . . ?
C3 N2 N1 118.8(13) . . ?
C3 N2 Ce1 121.6(10) . . ?
N1 N2 Ce1 119.4(9) . . ?
N2 C3 N4 126.1(14) . . ?
N2 C3 C7 120.1(12) . . ?
N4 C3 C7 113.8(14) . . ?
C5 N4 C3 115.1(15) . . ?
N4 C5 C6 121.1(16) . . ?
N4 C5 C51 116.8(16) . . ?
C6 C5 C51 122.1(17) . . ?
N1 C6 C5 120.7(16) . . ?
N1 C6 C61 117.2(19) . . ?
C5 C6 C61 122.1(19) . . ?
C12 C7 N8 123.9(15) . . ?
C12 C7 C3 120.5(14) . . ?
N8 C7 C3 115.5(14) . . ?
C9 N8 C7 117.6(13) . . ?
C9 N8 Ce1 121.5(9) . . ?
C7 N8 Ce1 120.8(10) . . ?
N8 C9 C9 118.0(8) . 4_556 ?
N8 C9 C10 121.7(13) . . ?
C9 C9 C10 119.5(9) 4_556 . ?
C11 C10 C9 111.6(17) . . ?
C12 C11 C10 121.3(15) . . ?
C7 C12 C11 119.2(15) . . ?
C52 C51 C5 114.7(17) . . ?
C62 C61 C6 117.9(21) . . ?
N43 O41 Ce1 99.4(11) . . ?
O44 N43 O41 125.7(20) . . ?
O44 N43 O42 120.6(20) . . ?
O41 N43 O42 113.6(15) . . ?
N43 O42 Ce1 96.8(10) . . ?
N53 O51 Ce1 98.6(12) . . ?
O51 N53 O51 115.4(22) 4_556 . ?
O51 N53 O52 122.3(11) 4_556 . ?
O51 N53 O52 122.3(11) . . ?
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 O51 2.56(2) . ?
Ce1 O51 2.56(2) 4_556 ?
Ce1 O41 2.570(15) . ?
Ce1 O41 2.570(15) 4_556 ?
Ce1 O42 2.584(14) 4_556 ?
Ce1 O42 2.584(14) . ?
Ce1 N2 2.674(13) 4_556 ?
Ce1 N2 2.674(13) . ?
Ce1 N8 2.699(13) . ?
Ce1 N8 2.699(13) 4_556 ?
N1 N2 1.37(2) . ?
C3 N2 1.31(2) . ?
C3 N4 1.36(2) . ?
N4 C5 1.32(2) . ?
C5 C6 1.40(3) . ?
C5 C51 1.52(2) . ?
C6 N1 1.34(2) . ?
C6 C61 1.51(3) . ?
N8 C7 1.37(2) . ?
N8 C9 1.35(2) . ?
C9 C9 1.48(3) 4_556 ?
C9 C10 1.50(2) . ?
C10 C11 1.40(3) . ?
C11 C12 1.39(3) . ?
C12 C7 1.33(2) . ?
C7 C3 1.52(2) . ?
C61 C62 1.46(4) . ?
C51 C52 1.52(3) . ?
O41 N43 1.25(2) . ?
N43 O44 1.20(2) . ?
N43 O42 1.32(2) . ?
O51 N53 1.22(2) . ?
N53 O51 1.22(2) 4_556 ?
N53 O52 1.24(3) . ?
