Structural and Photophysical Properties of Visible- and Near-IR-Emitting Tris Lanthanide(III) Complexes Formed with the Enantiomers of N,N'-Bis(1-phenylethyl)-2,6-pyridinedicarboxamide
KimNgan T. Hua; Jide Xu; Eliseo E. Quiroz; Sabrina Lopez; Andrew J. Ingram; Victoria Anne Johnson; Angela R. Tisch; Ana de Bettencourt-Dias; Daniel A. Straus; Gilles Muller; Inorganic Chemistry 51 (2012) 647–660; doi:10.1021/ic202094p

data_4327878
_publ_section_title
;
 Structural and Photophysical Properties of Visible- and Near-IR-Emitting
 Tris Lanthanide(III) Complexes Formed with the Enantiomers of
 N,N'-Bis(1-phenylethyl)-2,6-pyridinedicarboxamide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              647
_journal_page_last               660
_journal_paper_doi               10.1021/ic202094p
_journal_volume                  51
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_sum            'C70.5 H76.25 Cl3 N9 O7.5 Tb'
_chemical_formula_weight         1434.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.938
_cell_length_b                   25.938
_cell_length_c                   25.938
_cell_measurement_reflns_used    9681
_cell_measurement_temperature    151(2)
_cell_measurement_theta_max      25.393
_cell_measurement_theta_min      2.221
_cell_volume                     17450.564
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_molecular_graphics    DIAMOND
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      151(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            103517
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.34
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6508
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_description       Rhombic
_exptl_crystal_F_000             5906
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5337
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+13.8204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                5234
_reflns_number_total             5337
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202094p_si_002_6.cif
_cod_data_source_block           TbRR
_cod_original_cell_volume        17450.6
_cod_original_formula_sum        'C70.50 H76.25 Cl3 N9 O7.50 Tb'
_cod_database_code               4327878