#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:51:55 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180452 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/21/7212192.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_7212192
loop_
_publ_author_name
'Zucchi, Gaël'
'Jeon, Taewoo'
'Tondelier, Denis'
'Aldakov, Dmitry'
'Thuéry, Pierre'
'Ephritikhine, Michel'
'Geffroy, Bernard'
_publ_section_title
;
 White electroluminescence of lanthanide complexes resulting from exciplex
 formation
;
_journal_issue                   11
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              2114
_journal_paper_doi               10.1039/b921740a
_journal_volume                  20
_journal_year                    2010
_chemical_formula_sum            'C38 H48 N4 O12 Tb2'
_chemical_formula_weight         1070.64
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.977(5)
_cell_angle_beta                 97.121(6)
_cell_angle_gamma                96.480(6)
_cell_formula_units_Z            1
_cell_length_a                   9.2276(6)
_cell_length_b                   9.8575(10)
_cell_length_c                   12.4828(13)
_cell_measurement_reflns_used    28924
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.06
_cell_volume                     1064.22(17)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and four ω scans with 2° steps (372 frames)'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28924
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.358
_exptl_absorpt_correction_T_max  0.818
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.673
_refine_diff_density_min         -1.499
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0744
_reflns_number_gt                3569
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921740a.txt
_cod_data_source_block           2
_cod_database_code               7212192
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Tb Tb 0.704144(18) 0.747256(19) 0.839968(15) 0.02370(8) Uani 1 1 d .
O1 O 0.8204(3) 0.6672(3) 0.9801(2) 0.0308(6) Uani 1 1 d .
O2 O 0.5426(3) 0.7479(3) 0.9690(2) 0.0286(6) Uani 1 1 d .
O3 O 0.7857(3) 0.5459(3) 0.7291(3) 0.0319(7) Uani 1 1 d .
O4 O 0.4946(3) 0.5917(3) 0.7272(2) 0.0324(7) Uani 1 1 d .
O5 O 0.7941(3) 0.8270(3) 0.6986(2) 0.0320(7) Uani 1 1 d .
O6 O 0.5465(3) 0.9002(3) 0.7913(2) 0.0283(6) Uani 1 1 d .
N1 N 0.9889(3) 0.8373(3) 0.8854(3) 0.0257(7) Uani 1 1 d .
N2 N 1.1963(3) 1.0071(3) 0.9993(3) 0.0266(7) Uani 1 1 d .
C1 C 1.0503(4) 0.9567(4) 0.9679(3) 0.0228(8) Uani 1 1 d .
C2 C 1.2853(5) 0.9274(5) 0.9405(4) 0.0315(9) Uani 1 1 d .
H2 H 1.3868 0.9585 0.9588 0.038 Uiso 1 1 calc R
C3 C 1.2323(5) 0.7999(5) 0.8530(4) 0.0322(9) Uani 1 1 d .
H3 H 1.2959 0.7448 0.8139 0.039 Uiso 1 1 calc R
C4 C 1.0814(4) 0.7595(4) 0.8274(4) 0.0290(9) Uani 1 1 d .
H4 H 1.0419 0.6761 0.7683 0.035 Uiso 1 1 calc R
C5 C 0.9095(5) 0.5941(6) 1.1370(4) 0.0441(12) Uani 1 1 d .
H5A H 0.9409 0.5105 1.0899 0.066 Uiso 1 1 calc R
H5B H 0.8732 0.5725 1.1999 0.066 Uiso 1 1 calc R
H5C H 0.9917 0.6710 1.1648 0.066 Uiso 1 1 calc R
C6 C 0.7871(5) 0.6389(5) 1.0676(4) 0.0334(10) Uani 1 1 d .
C7 C 0.6482(5) 0.6454(5) 1.1026(4) 0.0351(10) Uani 1 1 d .
H7 H 0.6320 0.6136 1.1639 0.042 Uiso 1 1 calc R
C8 C 0.5334(5) 0.6967(4) 1.0507(4) 0.0305(9) Uani 1 1 d .
C9 C 0.3891(5) 0.6979(5) 1.0955(4) 0.0380(10) Uani 1 1 d .
H9A H 0.3760 0.7954 1.1305 0.057 Uiso 1 1 calc R
H9B H 0.3902 0.6474 1.1507 0.057 Uiso 1 1 calc R
H9C H 0.3090 0.6518 1.0340 0.057 Uiso 1 1 calc R
C10 C 0.8359(5) 0.3475(5) 0.5867(4) 0.0467(12) Uani 1 1 d .
H10A H 0.9133 0.4076 0.5697 0.070 Uiso 1 1 calc R
H10B H 0.7843 0.2776 0.5177 0.070 Uiso 1 1 calc R
H10C H 0.8781 0.2994 0.6368 0.070 Uiso 1 1 calc R
C11 C 0.7286(5) 0.4392(5) 0.6437(4) 0.0328(10) Uani 1 1 d .
C12 C 0.5774(5) 0.3994(5) 0.6003(4) 0.0339(10) Uani 1 1 d .
H12 H 0.5472 0.3168 0.5385 0.041 Uiso 1 1 calc R
C13 C 0.4697(5) 0.4770(5) 0.6448(4) 0.0298(9) Uani 1 1 d .
C14 C 0.3089(5) 0.4208(5) 0.5928(4) 0.0397(11) Uani 1 1 d .
H14A H 0.2712 0.3494 0.6250 0.059 Uiso 1 1 calc R
H14B H 0.3009 0.3788 0.5122 0.059 Uiso 1 1 calc R
H14C H 0.2527 0.4985 0.6084 0.059 Uiso 1 1 calc R
C15 C 0.8784(5) 0.9487(5) 0.5762(4) 0.0402(11) Uani 1 1 d .
H15A H 0.9635 1.0090 0.6269 0.060 Uiso 1 1 calc R
H15B H 0.8376 0.9981 0.5267 0.060 Uiso 1 1 calc R
H15C H 0.9070 0.8617 0.5318 0.060 Uiso 1 1 calc R
C16 C 0.7635(5) 0.9126(5) 0.6445(4) 0.0325(10) Uani 1 1 d .
C17 C 0.6323(5) 0.9715(5) 0.6423(4) 0.0336(10) Uani 1 1 d .
H17 H 0.6130 1.0231 0.5919 0.040 Uiso 1 1 calc R
C18 C 0.5295(4) 0.9559(4) 0.7124(4) 0.0301(9) Uani 1 1 d .
C19 C 0.3841(5) 1.0110(5) 0.6935(4) 0.0372(10) Uani 1 1 d .
H19A H 0.3066 0.9312 0.6566 0.056 Uiso 1 1 calc R
H19B H 0.3927 1.0723 0.6465 0.056 Uiso 1 1 calc R
H19C H 0.3612 1.0644 0.7653 0.056 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'
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'
Tb Tb -0.1723 4.1537 '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_3
O1 Tb O2 73.19(10) .
O1 Tb O3 79.58(10) .
O2 Tb O3 125.85(10) .
O1 Tb O5 131.64(10) .
O2 Tb O5 152.20(10) .
O3 Tb O5 76.93(10) .
O1 Tb O4 114.50(10) .
O2 Tb O4 77.27(10) .
O3 Tb O4 72.91(10) .
O5 Tb O4 97.98(10) .
O1 Tb O6 148.06(10) .
O2 Tb O6 80.30(10) .
O3 Tb O6 131.47(10) .
O5 Tb O6 72.04(9) .
O4 Tb O6 75.51(10) .
O1 Tb N1 67.98(10) .
O2 Tb N1 127.38(10) .
O3 Tb N1 80.25(10) .
O5 Tb N1 66.76(10) .
O4 Tb N1 151.71(11) .
O6 Tb N1 118.30(10) .
O1 Tb N2 79.29(10) 2_777
O2 Tb N2 77.45(10) 2_777
O3 Tb N2 141.26(10) 2_777
O5 Tb N2 93.74(11) 2_777
O4 Tb N2 145.78(10) 2_777
O6 Tb N2 77.81(10) 2_777
N1 Tb N2 61.80(10) 2_777
C6 O1 Tb 136.3(3) .
C8 O2 Tb 135.9(3) .
C11 O3 Tb 135.6(3) .
C13 O4 Tb 136.1(3) .
C16 O5 Tb 137.4(3) .
C18 O6 Tb 135.2(3) .
C1 N1 C4 116.8(3) .
C1 N1 Tb 122.7(3) .
C4 N1 Tb 120.5(3) .
C2 N2 C1 115.6(4) .
C2 N2 Tb 122.8(3) 2_777
C1 N2 Tb 121.5(3) 2_777
N1 C1 N2 126.1(4) .
N1 C1 C1 117.3(4) 2_777
N2 C1 C1 116.5(4) 2_777
N2 C2 C3 122.8(4) .
N2 C2 H2 118.6 .
C3 C2 H2 118.6 .
C4 C3 C2 116.6(4) .
C4 C3 H3 121.7 .
C2 C3 H3 121.7 .
N1 C4 C3 122.0(4) .
N1 C4 H4 119.0 .
C3 C4 H4 119.0 .
C6 C5 H5A 109.5 .
C6 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C6 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
O1 C6 C7 124.9(4) .
O1 C6 C5 115.6(4) .
C7 C6 C5 119.5(4) .
C8 C7 C6 123.8(4) .
C8 C7 H7 118.1 .
C6 C7 H7 118.1 .
O2 C8 C7 124.4(4) .
O2 C8 C9 116.6(4) .
C7 C8 C9 119.0(4) .
C8 C9 H9A 109.5 .
C8 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C8 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C11 C10 H10A 109.5 .
C11 C10 H10B 109.5 .
H10A C10 H10B 109.5 .
C11 C10 H10C 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
O3 C11 C12 125.5(4) .
O3 C11 C10 115.8(4) .
C12 C11 C10 118.7(4) .
C13 C12 C11 123.5(4) .
C13 C12 H12 118.3 .
C11 C12 H12 118.3 .
O4 C13 C12 125.2(4) .
O4 C13 C14 116.2(4) .
C12 C13 C14 118.7(4) .
C13 C14 H14A 109.5 .
C13 C14 H14B 109.5 .
H14A C14 H14B 109.5 .
C13 C14 H14C 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
C16 C15 H15A 109.5 .
C16 C15 H15B 109.5 .
H15A C15 H15B 109.5 .
C16 C15 H15C 109.5 .
H15A C15 H15C 109.5 .
H15B C15 H15C 109.5 .
O5 C16 C17 124.6(4) .
O5 C16 C15 115.7(4) .
C17 C16 C15 119.7(4) .
C18 C17 C16 122.7(4) .
C18 C17 H17 118.7 .
C16 C17 H17 118.7 .
O6 C18 C17 125.7(4) .
O6 C18 C19 116.6(4) .
C17 C18 C19 117.7(4) .
C18 C19 H19A 109.5 .
C18 C19 H19B 109.5 .
H19A C19 H19B 109.5 .
C18 C19 H19C 109.5 .
H19A C19 H19C 109.5 .
H19B C19 H19C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb O1 2.317(3) .
Tb O2 2.325(3) .
Tb O3 2.327(3) .
Tb O5 2.334(3) .
Tb O4 2.338(3) .
Tb O6 2.360(3) .
Tb N1 2.612(3) .
Tb N2 2.634(3) 2_777
O1 C6 1.268(5) .
O2 C8 1.271(5) .
O3 C11 1.265(5) .
O4 C13 1.262(5) .
O5 C16 1.260(5) .
O6 C18 1.262(5) .
N1 C1 1.329(5) .
N1 C4 1.348(5) .
N2 C2 1.338(5) .
N2 C1 1.349(5) .
N2 Tb 2.633(3) 2_777
C1 C1 1.481(8) 2_777
C2 C3 1.392(6) .
C2 H2 0.9300 .
C3 C4 1.375(6) .
C3 H3 0.9300 .
C4 H4 0.9300 .
C5 C6 1.521(6) .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.406(6) .
C7 C8 1.393(6) .
C7 H7 0.9300 .
C8 C9 1.507(6) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 C11 1.518(6) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.400(6) .
C12 C13 1.393(6) .
C12 H12 0.9300 .
C13 C14 1.515(6) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C16 1.514(6) .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 C17 1.402(6) .
C17 C18 1.394(6) .
C17 H17 0.9300 .
C18 C19 1.521(6) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
