#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:53:29 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179768 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/64/7006489.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_7006489
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 N11 Nd O10'
_chemical_formula_weight         774.82
_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                 99.983(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.826(9)
_cell_length_b                   11.906(12)
_cell_length_c                   15.829(17)
_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 0.99
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8192
_diffrn_reflns_theta_full        24.69
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.711
_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    1.571
_exptl_crystal_description       needle
_exptl_crystal_F_000             778
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.585
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0068(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.148
_refine_ls_goodness_of_fit_obs   1.163
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_restrained_S_obs      1.163
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_obs          0.0357
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0395P)²+5.8522P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0969
_refine_ls_wR_factor_obs         0.0956
_reflns_number_observed          2633
_reflns_number_total             2765
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b511321k.txt
_cod_data_source_block           nd
_cod_original_cell_volume        1638.2(29)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7006489
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
Nd1 Nd 0.0000 0.20494(3) 0.2500 0.0223(2) Uani 1 d S .
N1 N 0.1595(6) 0.3213(4) 0.0801(3) 0.0417(11) Uani 1 d . .
N2 N 0.1316(5) 0.2198(3) 0.1129(3) 0.0329(9) Uani 1 d . .
C3 C 0.1700(5) 0.1283(4) 0.0745(3) 0.0281(10) Uani 1 d . .
N4 N 0.2376(5) 0.1263(4) 0.0047(3) 0.0361(10) Uani 1 d . .
C5 C 0.2690(6) 0.2231(5) -0.0270(3) 0.0391(13) Uani 1 d . .
C6 C 0.2270(7) 0.3238(5) 0.0114(4) 0.0458(14) Uani 1 d . .
C7 C 0.1389(5) 0.0180(4) 0.1097(3) 0.0292(10) Uani 1 d . .
N8 N 0.0669(4) 0.0150(3) 0.1792(2) 0.0251(8) Uani 1 d . .
C9 C 0.0392(6) -0.0862(4) 0.2116(3) 0.0289(10) Uani 1 d . .
C10 C 0.0831(7) -0.1859(4) 0.1773(4) 0.0427(13) Uani 1 d . .
H10 H 0.0644 -0.2545 0.2016 0.051 Uiso 1 calc R .
C11 C 0.1551(8) -0.1816(5) 0.1062(4) 0.049(2) Uani 1 d . .
H11 H 0.1845 -0.2475 0.0820 0.059 Uiso 1 calc R .
C12 C 0.1829(7) -0.0797(5) 0.0720(3) 0.0404(13) Uani 1 d . .
H12 H 0.2306 -0.0757 0.0241 0.048 Uiso 1 calc R .
C51 C 0.3514(8) 0.2240(7) -0.1032(4) 0.060(2) Uani 1 d . .
H51A H 0.2865 0.2614 -0.1506 0.073 Uiso 1 calc R .
H51B H 0.4447 0.2680 -0.0884 0.073 Uiso 1 calc R .
C52 C 0.3934(8) 0.1100(7) -0.1328(4) 0.067(2) Uani 1 d . .
H52C H 0.4619 0.0734 -0.0874 0.081 Uiso 1 calc R .
H52D H 0.4433 0.1182 -0.1818 0.081 Uiso 1 calc R .
H52E H 0.3020 0.0657 -0.1483 0.081 Uiso 1 calc R .
C61 C 0.2556(13) 0.4370(6) -0.0260(6) 0.093(3) Uani 1 d . .
H61A H 0.3606 0.4379 -0.0366 0.111 Uiso 1 calc R .
H61B H 0.1884 0.4435 -0.0811 0.111 Uiso 1 calc R .
C62 C 0.2337(13) 0.5355(6) 0.0239(6) 0.097(3) Uani 1 d . .
H62C H 0.1313 0.5352 0.0368 0.116 Uiso 1 calc R .
H62D H 0.2482 0.6017 -0.0083 0.116 Uiso 1 calc R .
H62E H 0.3069 0.5350 0.0764 0.116 Uiso 1 calc R .
O41 O 0.1855(5) 0.1937(4) 0.3922(3) 0.0535(11) Uani 1 d . .
O42 O 0.2922(5) 0.1821(4) 0.2813(3) 0.0562(11) Uani 1 d . .
N43 N 0.3083(6) 0.1931(4) 0.3614(3) 0.0501(13) Uani 1 d . .
O44 O 0.4339(6) 0.2039(6) 0.4067(4) 0.097(2) Uani 1 d . .
O51 O -0.1128(5) 0.3978(3) 0.2128(3) 0.0607(12) Uani 1 d . .
O52 O 0.0000 0.5564(6) 0.2500 0.113(4) Uani 1 d S .
N53 N 0.0000 0.4539(5) 0.2500 0.056(2) Uani 1 d S .
O100 O 0.5000 0.4542(14) -0.2500 0.085(5) Uiso 0.50 d SP .
O200 O 0.5000 0.4151(12) 0.2500 0.070(4) 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'
Nd Nd -0.1943 3.0179 '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 Nd1 O51 49.8(2) . 4_556 ?
O51 Nd1 O41 71.07(15) . 4_556 ?
O51 Nd1 O41 114.8(2) 4_556 4_556 ?
O51 Nd1 O41 114.8(2) . . ?
O51 Nd1 O41 71.07(15) 4_556 . ?
O41 Nd1 O41 174.0(2) 4_556 . ?
O51 Nd1 O42 73.0(2) . 4_556 ?
O51 Nd1 O42 119.0(2) 4_556 4_556 ?
O41 Nd1 O42 49.48(14) 4_556 4_556 ?
O41 Nd1 O42 129.68(14) . 4_556 ?
O51 Nd1 O42 119.0(2) . . ?
O51 Nd1 O42 73.0(2) 4_556 . ?
O41 Nd1 O42 129.68(14) 4_556 . ?
O41 Nd1 O42 49.48(14) . . ?
O42 Nd1 O42 167.8(2) 4_556 . ?
O51 Nd1 N8 140.27(15) . 4_556 ?
O51 Nd1 N8 141.96(15) 4_556 4_556 ?
O41 Nd1 N8 99.98(14) 4_556 4_556 ?
O41 Nd1 N8 74.72(13) . 4_556 ?
O42 Nd1 N8 72.43(13) 4_556 4_556 ?
O42 Nd1 N8 96.86(14) . 4_556 ?
O51 Nd1 N8 141.96(15) . . ?
O51 Nd1 N8 140.27(15) 4_556 . ?
O41 Nd1 N8 74.72(13) 4_556 . ?
O41 Nd1 N8 99.98(14) . . ?
O42 Nd1 N8 96.86(14) 4_556 . ?
O42 Nd1 N8 72.43(13) . . ?
N8 Nd1 N8 61.8(2) 4_556 . ?
O51 Nd1 N2 85.4(2) . 4_556 ?
O51 Nd1 N2 87.7(2) 4_556 4_556 ?
O41 Nd1 N2 115.0(2) 4_556 4_556 ?
O41 Nd1 N2 65.4(2) . 4_556 ?
O42 Nd1 N2 65.99(14) 4_556 4_556 ?
O42 Nd1 N2 114.90(14) . 4_556 ?
N8 Nd1 N2 62.94(13) 4_556 4_556 ?
N8 Nd1 N2 124.76(12) . 4_556 ?
O51 Nd1 N2 87.7(2) . . ?
O51 Nd1 N2 85.4(2) 4_556 . ?
O41 Nd1 N2 65.4(2) 4_556 . ?
O41 Nd1 N2 115.0(2) . . ?
O42 Nd1 N2 114.90(14) 4_556 . ?
O42 Nd1 N2 66.00(14) . . ?
N8 Nd1 N2 124.76(12) 4_556 . ?
N8 Nd1 N2 62.94(13) . . ?
N2 Nd1 N2 172.3(2) 4_556 . ?
C6 N1 N2 118.1(5) . . ?
C3 N2 N1 118.8(4) . . ?
C3 N2 Nd1 120.5(3) . . ?
N1 N2 Nd1 120.7(3) . . ?
N2 C3 N4 125.4(5) . . ?
N2 C3 C7 118.9(4) . . ?
N4 C3 C7 115.8(4) . . ?
C5 N4 C3 117.1(5) . . ?
N4 C5 C6 119.4(5) . . ?
N4 C5 C51 118.4(5) . . ?
C6 C5 C51 122.2(5) . . ?
N1 C6 C5 121.3(5) . . ?
N1 C6 C61 118.0(6) . . ?
C5 C6 C61 120.7(5) . . ?
N8 C7 C12 121.9(5) . . ?
N8 C7 C3 118.2(4) . . ?
C12 C7 C3 119.9(4) . . ?
C9 N8 C7 118.0(4) . . ?
C9 N8 Nd1 122.5(3) . . ?
C7 N8 Nd1 119.4(3) . . ?
N8 C9 C10 122.3(4) . . ?
N8 C9 C9 116.6(2) . 4_556 ?
C10 C9 C9 121.1(3) . 4_556 ?
C11 C10 C9 118.9(5) . . ?
C12 C11 C10 119.6(5) . . ?
C11 C12 C7 119.2(5) . . ?
C52 C51 C5 114.9(6) . . ?
C62 C61 C6 117.6(6) . . ?
N43 O41 Nd1 97.1(3) . . ?
O44 N43 O42 122.4(6) . . ?
O44 N43 O41 121.8(6) . . ?
O42 N43 O41 115.8(5) . . ?
N43 O42 Nd1 96.8(3) . . ?
N53 O51 Nd1 97.2(4) . . ?
O52 N53 O51 122.1(3) . . ?
O52 N53 O51 122.1(3) . 4_556 ?
O51 N53 O51 115.8(6) . 4_556 ?
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
Nd1 O51 2.531(4) . ?
Nd1 O51 2.531(4) 4_556 ?
Nd1 O41 2.547(4) 4_556 ?
Nd1 O41 2.547(4) . ?
Nd1 O42 2.555(5) 4_556 ?
Nd1 O42 2.555(5) . ?
Nd1 N8 2.635(4) 4_556 ?
Nd1 N8 2.636(4) . ?
Nd1 N2 2.639(5) 4_556 ?
Nd1 N2 2.640(5) . ?
N1 N2 1.354(6) . ?
C3 N2 1.320(6) . ?
C3 N4 1.343(6) . ?
N4 C5 1.306(7) . ?
C5 C6 1.422(9) . ?
C5 C51 1.512(8) . ?
C6 N1 1.327(7) . ?
C6 C61 1.510(9) . ?
C7 C3 1.472(7) . ?
N8 C9 1.349(6) . ?
N8 C7 1.364(6) . ?
C9 C10 1.387(7) . ?
C9 C9 1.500(9) 4_556 ?
C10 C11 1.386(8) . ?
C11 C12 1.368(8) . ?
C12 C7 1.392(7) . ?
C51 C52 1.503(10) . ?
C61 C62 1.446(11) . ?
O41 N43 1.263(7) . ?
N43 O44 1.218(7) . ?
N43 O42 1.258(7) . ?
O51 N53 1.257(5) . ?
N53 O52 1.220(9) . ?
N53 O51 1.257(5) 4_556 ?
