#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:53:29 +0100 (vie 25 de mar de 2016) $
#$Revision: 179768 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/64/7006496.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_7006496
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            'C26 H29 N12 O9 Y'
_chemical_formula_weight         742.52
_chemical_name_systematic
;
?
;
_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
_cell_angle_alpha                92.459(10)
_cell_angle_beta                 95.228(10)
_cell_angle_gamma                106.756(10)
_cell_formula_units_Z            2
_cell_length_a                   10.040(11)
_cell_length_b                   10.168(12)
_cell_length_c                   16.869(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1638(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 0.893
_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  0.0927
_diffrn_reflns_av_sigmaI/netI    0.1406
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9406
_diffrn_reflns_theta_full        25.80
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    1.849
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
DIFABS, Walker, N. and Stuart, D., Acta Cryst 1983 A39 158.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       needle
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.641
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.058
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.1337
_refine_ls_R_factor_obs          0.1144
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.1796P)²+5.7707P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3109
_refine_ls_wR_factor_obs         0.2899
_reflns_number_observed          4179
_reflns_number_total             5348
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b511321k.txt
_cod_data_source_block           y
_cod_original_cell_volume        1637.8(30)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7006496
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Y1 Y 0.25207(9) 0.25717(9) 0.22734(5) 0.0377(3) Uani 1 d . .
N1 N 0.2427(9) 0.4283(9) 0.0580(5) 0.047(2) Uani 1 d . .
N2 N 0.1650(9) 0.3151(8) 0.0919(5) 0.044(2) Uani 1 d . .
C3 C 0.0462(10) 0.2353(10) 0.0533(6) 0.042(2) Uani 1 d . .
N4 N -0.0039(10) 0.2517(10) -0.0213(5) 0.052(2) Uani 1 d . .
C5 C 0.0676(12) 0.3572(11) -0.0556(6) 0.050(2) Uani 1 d . .
C6 C 0.1958(12) 0.4504(11) -0.0134(6) 0.049(2) Uani 1 d . .
C7 C -0.0344(11) 0.1153(10) 0.0945(6) 0.044(2) Uani 1 d . .
N8 N 0.0208(8) 0.0969(8) 0.1669(5) 0.042(2) Uani 1 d . .
C9 C -0.0554(11) -0.0106(10) 0.2087(6) 0.048(2) Uani 1 d . .
C10 C -0.1812(14) -0.0955(13) 0.1766(8) 0.068(3) Uani 1 d . .
H10 H -0.2271 -0.1697 0.2041 0.082 Uiso 1 calc R .
C11 C -0.2426(13) -0.0728(13) 0.1028(8) 0.071(3) Uani 1 d . .
H11 H -0.3317 -0.1269 0.0824 0.085 Uiso 1 calc R .
C12 C -0.1650(13) 0.0357(12) 0.0596(8) 0.062(3) Uani 1 d . .
H12 H -0.2007 0.0526 0.0095 0.075 Uiso 1 calc R .
N21 N 0.5136(11) 0.3535(11) 0.3819(6) 0.058(2) Uani 1 d . .
N22 N 0.3927(10) 0.2577(10) 0.3587(5) 0.053(2) Uani 1 d . .
C23 C 0.3362(15) 0.1685(13) 0.4112(7) 0.061(3) Uani 1 d . .
N24 N 0.3981(15) 0.1626(13) 0.4866(6) 0.077(3) Uani 1 d . .
C25 C 0.5201(16) 0.2616(17) 0.5079(7) 0.075(4) Uani 1 d . .
C26 C 0.5775(15) 0.3557(17) 0.4533(8) 0.076(4) Uani 1 d . .
C27 C 0.2005(14) 0.0658(14) 0.3881(7) 0.066(3) Uani 1 d . .
N28 N 0.1323(8) 0.0757(7) 0.3137(4) 0.037(2) Uani 1 d . .
C29 C 0.0155(14) -0.0209(13) 0.2877(7) 0.063(3) Uani 1 d . .
C30 C -0.0388(17) -0.1302(19) 0.3383(10) 0.105(6) Uani 1 d . .
H30 H -0.1153 -0.2035 0.3178 0.126 Uiso 1 calc R .
C31 C 0.0153(24) -0.1303(21) 0.4119(11) 0.125(8) Uani 1 d . .
H31 H -0.0317 -0.1920 0.4464 0.150 Uiso 1 calc R .
C32 C 0.1428(21) -0.0372(19) 0.4371(9) 0.104(6) Uani 1 d . .
H32 H 0.1900 -0.0430 0.4863 0.125 Uiso 1 calc R .
C51 C 0.0170(14) 0.3837(13) -0.1392(7) 0.064(3) Uani 1 d . .
H51D H 0.0868 0.3782 -0.1743 0.077 Uiso 1 calc R .
H51E H 0.0100 0.4769 -0.1384 0.077 Uiso 1 calc R .
C52 C -0.1188(17) 0.2885(15) -0.1729(8) 0.080(4) Uani 1 d . .
H52A H -0.1275 0.1985 -0.1548 0.095 Uiso 1 calc R .
H52B H -0.1244 0.2841 -0.2301 0.095 Uiso 1 calc R .
H52C H -0.1930 0.3210 -0.1557 0.095 Uiso 1 calc R .
C61 C 0.2785(14) 0.5773(14) -0.0506(8) 0.072(4) Uani 1 d . .
H61A H 0.3085 0.5481 -0.0997 0.087 Uiso 1 calc R .
H61B H 0.2167 0.6325 -0.0646 0.087 Uiso 1 calc R .
C62 C 0.4066(17) 0.6680(16) 0.0013(10) 0.087(4) Uani 1 d . .
H62C H 0.3845 0.6762 0.0551 0.104 Uiso 1 calc R .
H62D H 0.4343 0.7577 -0.0189 0.104 Uiso 1 calc R .
H62E H 0.4818 0.6275 0.0003 0.104 Uiso 1 calc R .
C251 C 0.5869(22) 0.2601(23) 0.5915(9) 0.111(6) Uani 1 d . .
H25A H 0.6807 0.2538 0.5877 0.133 Uiso 1 calc R .
H25B H 0.5963 0.3483 0.6194 0.133 Uiso 1 calc R .
C252 C 0.5184(25) 0.1535(26) 0.6410(10) 0.133(8) Uani 1 d . .
H25C H 0.4356 0.1713 0.6571 0.159 Uiso 1 calc R .
H25D H 0.5809 0.1528 0.6875 0.159 Uiso 1 calc R .
H25E H 0.4934 0.0657 0.6113 0.159 Uiso 1 calc R .
C261 C 0.7187(22) 0.4693(24) 0.4725(11) 0.124(8) Uani 1 d . .
H26D H 0.7147 0.5205 0.5216 0.149 Uiso 1 calc R .
H26E H 0.7912 0.4245 0.4828 0.149 Uiso 1 calc R .
C262 C 0.7592(31) 0.5612(26) 0.4168(19) 0.165(11) Uani 1 d . .
H26A H 0.7370 0.5141 0.3646 0.198 Uiso 1 calc R .
H26B H 0.8583 0.6046 0.4264 0.198 Uiso 1 calc R .
H26C H 0.7109 0.6298 0.4200 0.198 Uiso 1 calc R .
O41 O 0.1760(10) 0.3682(10) 0.3469(5) 0.070(2) Uani 1 d . .
O42 O 0.0629(9) 0.3679(9) 0.2329(5) 0.062(2) Uani 1 d . .
N43 N 0.0845(10) 0.4125(10) 0.3048(6) 0.055(2) Uani 1 d . .
O44 O 0.0316(11) 0.4945(11) 0.3334(6) 0.080(3) Uani 1 d . .
O51 O 0.3001(10) 0.1202(10) 0.1123(5) 0.073(2) Uani 1 d . .
O52 O 0.3754(9) 0.0788(9) 0.2276(5) 0.063(2) Uani 1 d . .
N53 N 0.3705(9) 0.0571(9) 0.1540(6) 0.052(2) Uani 1 d . .
O54 O 0.4313(12) -0.0178(12) 0.1223(7) 0.094(3) Uani 1 d . .
O61 O 0.4822(8) 0.3717(8) 0.1910(5) 0.056(2) Uani 1 d . .
O62 O 0.3718(9) 0.5034(9) 0.2413(5) 0.068(2) Uani 1 d . .
N63 N 0.4850(10) 0.4947(11) 0.2141(6) 0.063(3) Uani 1 d . .
O64 O 0.5812(9) 0.5974(8) 0.2116(7) 0.076(3) Uani 1 d . .
N71 N 0.8256(28) 0.1603(25) 0.3843(14) 0.130(8) Uani 1 d . .
C72 C 0.7778(21) 0.1849(18) 0.3262(12) 0.097(5) Uani 1 d . .
C73 C 0.7272(17) 0.2256(17) 0.2510(10) 0.090(4) Uani 1 d . .
H73A H 0.6704 0.2848 0.2606 0.108 Uiso 1 calc R .
H73B H 0.6724 0.1451 0.2184 0.108 Uiso 1 calc R .
H73C H 0.8052 0.2738 0.2242 0.108 Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 '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
O61 Y1 O62 52.9(3) . . ?
O61 Y1 N28 140.9(3) . . ?
O62 Y1 N28 137.5(3) . . ?
O61 Y1 O42 124.0(3) . . ?
O62 Y1 O42 75.1(3) . . ?
N28 Y1 O42 90.7(3) . . ?
O61 Y1 O52 74.9(3) . . ?
O62 Y1 O52 123.5(3) . . ?
N28 Y1 O52 72.6(3) . . ?
O42 Y1 O52 160.9(3) . . ?
O61 Y1 O51 71.3(3) . . ?
O62 Y1 O51 117.4(3) . . ?
N28 Y1 O51 103.0(3) . . ?
O42 Y1 O51 128.1(3) . . ?
O52 Y1 O51 50.6(3) . . ?
O61 Y1 N2 85.0(3) . . ?
O62 Y1 N2 82.3(3) . . ?
N28 Y1 N2 129.1(3) . . ?
O42 Y1 N2 67.1(3) . . ?
O52 Y1 N2 116.1(3) . . ?
O51 Y1 N2 65.5(3) . . ?
O61 Y1 N8 140.3(3) . . ?
O62 Y1 N8 138.4(3) . . ?
N28 Y1 N8 64.2(3) . . ?
O42 Y1 N8 68.9(3) . . ?
O52 Y1 N8 94.8(3) . . ?
O51 Y1 N8 72.8(3) . . ?
N2 Y1 N8 65.0(3) . . ?
O61 Y1 N22 81.2(3) . . ?
O62 Y1 N22 83.4(3) . . ?
N28 Y1 N22 66.5(3) . . ?
O42 Y1 N22 115.3(3) . . ?
O52 Y1 N22 67.2(3) . . ?
O51 Y1 N22 116.2(3) . . ?
N2 Y1 N22 164.3(3) . . ?
N8 Y1 N22 130.7(3) . . ?
O61 Y1 O41 116.2(3) . . ?
O62 Y1 O41 70.1(3) . . ?
N28 Y1 O41 70.1(3) . . ?
O42 Y1 O41 50.4(3) . . ?
O52 Y1 O41 127.7(3) . . ?
O51 Y1 O41 172.3(3) . . ?
N2 Y1 O41 115.7(3) . . ?
N8 Y1 O41 100.6(3) . . ?
N22 Y1 O41 64.9(3) . . ?
C6 N1 N2 117.0(8) . . ?
C3 N2 N1 120.2(8) . . ?
C3 N2 Y1 120.2(6) . . ?
N1 N2 Y1 119.5(6) . . ?
N2 C3 N4 124.7(9) . . ?
N2 C3 C7 117.4(8) . . ?
N4 C3 C7 117.9(9) . . ?
C5 N4 C3 116.7(9) . . ?
N4 C5 C6 119.9(9) . . ?
N4 C5 C51 119.8(10) . . ?
C6 C5 C51 120.3(10) . . ?
N1 C6 C5 121.3(9) . . ?
N1 C6 C61 117.5(10) . . ?
C5 C6 C61 121.2(10) . . ?
N8 C7 C12 123.4(10) . . ?
N8 C7 C3 116.9(8) . . ?
C12 C7 C3 119.5(9) . . ?
C7 N8 C9 118.2(8) . . ?
C7 N8 Y1 120.4(6) . . ?
C9 N8 Y1 121.3(6) . . ?
N8 C9 C10 121.3(10) . . ?
N8 C9 C29 113.5(9) . . ?
C10 C9 C29 125.3(11) . . ?
C11 C10 C9 120.8(12) . . ?
C10 C11 C12 118.2(11) . . ?
C11 C12 C7 118.0(11) . . ?
C26 N21 N22 120.3(11) . . ?
C23 N22 N21 118.4(9) . . ?
C23 N22 Y1 118.6(8) . . ?
N21 N22 Y1 122.5(7) . . ?
N22 C23 N24 124.7(13) . . ?
N22 C23 C27 119.4(10) . . ?
N24 C23 C27 115.9(11) . . ?
C23 N24 C25 114.9(12) . . ?
N24 C25 C26 120.0(11) . . ?
N24 C25 C251 115.7(14) . . ?
C26 C25 C251 124.3(15) . . ?
N21 C26 C25 121.6(14) . . ?
N21 C26 C261 115.5(14) . . ?
C25 C26 C261 122.9(13) . . ?
N28 C27 C32 121.5(13) . . ?
N28 C27 C23 116.6(10) . . ?
C32 C27 C23 122.0(12) . . ?
C29 N28 C27 118.6(9) . . ?
C29 N28 Y1 122.2(7) . . ?
C27 N28 Y1 118.7(7) . . ?
N28 C29 C30 118.7(12) . . ?
N28 C29 C9 118.4(9) . . ?
C30 C29 C9 122.9(12) . . ?
C31 C30 C29 122.6(16) . . ?
C30 C31 C32 118.5(15) . . ?
C31 C32 C27 119.1(13) . . ?
C5 C51 C52 115.0(11) . . ?
C62 C61 C6 115.6(11) . . ?
C252 C251 C25 118.5(17) . . ?
C262 C261 C26 117.7(17) . . ?
N43 O41 Y1 95.0(6) . . ?
N43 O42 Y1 100.0(6) . . ?
O44 N43 O41 121.7(11) . . ?
O44 N43 O42 124.4(10) . . ?
O41 N43 O42 113.8(9) . . ?
N53 O51 Y1 95.8(6) . . ?
N53 O52 Y1 98.0(6) . . ?
O54 N53 O52 123.5(11) . . ?
O54 N53 O51 121.2(11) . . ?
O52 N53 O51 115.3(9) . . ?
N63 O61 Y1 96.9(6) . . ?
N63 O62 Y1 95.9(7) . . ?
O64 N63 O62 119.8(11) . . ?
O64 N63 O61 126.0(10) . . ?
O62 N63 O61 114.2(9) . . ?
N71 C72 C73 175.2(22) . . ?
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
Y1 O61 2.416(7) . ?
Y1 O62 2.436(9) . ?
Y1 N28 2.499(7) . ?
Y1 O42 2.478(8) . ?
Y1 O52 2.473(8) . ?
Y1 O51 2.503(9) . ?
Y1 N2 2.525(8) . ?
Y1 N8 2.516(8) . ?
Y1 N22 2.515(9) . ?
Y1 O41 2.551(9) . ?
N1 C6 1.305(14) . ?
N2 N1 1.372(11) . ?
N2 C3 1.327(13) . ?
C3 C7 1.494(14) . ?
N4 C3 1.348(13) . ?
C5 N4 1.298(14) . ?
C5 C51 1.516(15) . ?
C6 C5 1.46(2) . ?
C6 C61 1.52(2) . ?
C7 N8 1.339(13) . ?
C7 C12 1.388(15) . ?
C9 N8 1.399(13) . ?
C9 C29 1.48(2) . ?
C10 C9 1.36(2) . ?
C11 C10 1.40(2) . ?
C12 C11 1.43(2) . ?
N21 N22 1.332(14) . ?
C23 N22 1.34(2) . ?
C23 N24 1.375(15) . ?
N24 C25 1.35(2) . ?
C25 C26 1.40(2) . ?
C25 C251 1.51(2) . ?
C26 N21 1.31(2) . ?
C26 C261 1.55(2) . ?
C27 N28 1.396(14) . ?
C27 C23 1.47(2) . ?
C29 N28 1.32(2) . ?
C29 C30 1.44(2) . ?
C30 C31 1.31(2) . ?
C32 C31 1.37(3) . ?
C32 C27 1.39(2) . ?
C52 C51 1.47(2) . ?
C61 C62 1.52(2) . ?
C251 C252 1.45(3) . ?
C262 C261 1.36(3) . ?
O41 N43 1.303(13) . ?
N43 O44 1.216(13) . ?
N43 O42 1.254(12) . ?
O51 N53 1.271(13) . ?
N53 O54 1.238(13) . ?
N53 O52 1.246(12) . ?
N63 O64 1.206(13) . ?
N63 O62 1.289(13) . ?
N63 O61 1.285(13) . ?
N71 C72 1.12(3) . ?
C72 C73 1.44(2) . ?
