Lanthanide Complexes Based on β-Diketonates and a Tetradentate Chromophore Highly Luminescent as Powders and in Polymers
Eugen S. Andreiadis; Nicolas Gauthier; Daniel Imbert; Renaud Demadrille; Jacques Pécaut; Marinella Mazzanti; Inorganic Chemistry 52 (2013) 14382–14390; doi:10.1021/ic402523v

data_4337047
_publ_section_title
;
 Lanthanide Complexes Based on \b-Diketonates and a Tetradentate
 Chromophore Highly Luminescent as Powders and in Polymers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              14382
_journal_page_last               14390
_journal_paper_doi               10.1021/ic402523v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C27 H22 F6 N3 O7 Tb'
_chemical_formula_weight         773.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.927(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7241(5)
_cell_length_b                   15.0734(3)
_cell_length_c                   22.6068(8)
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9323
_cell_measurement_theta_min      3.0560
_cell_volume                     5835.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
Mercury 3.1 New software for searching the Cambridge Structural Database 
and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, 
M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, 
Acta Cryst., 2002, B58, 389-397)
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   56.00   94.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550 -163.0000  121.0000 38

  2 omega   37.00   85.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550   67.0000  209.0000 48

  3 omega  -51.00   42.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  -67.0000  330.0000 93

  4 omega  -43.00   -3.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7175   67.0000  209.0000 40

  5 omega  -42.00    3.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7175  -67.0000  255.0000 45

  6 omega  -35.00    0.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.7175  -45.0000  330.0000 35

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\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  0.0628
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32248
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.058
_exptl_absorpt_coefficient_mu    2.511
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       needle
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.675
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.093
_refine_diff_density_max         2.196
_refine_diff_density_min         -1.400
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         11894
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1270
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+70.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1444
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6836
_reflns_number_total             11894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic402523v_si_003_1.cif
_cod_data_source_block           1
_cod_database_code               4337047
_shelx_estimated_absorpt_t_min   0.282
_shelx_estimated_absorpt_t_max   0.800
_shelxl_version_number           2013-4
_shelx_res_checksum              58525