The conjugate base of methyl 3-oxobutanoate as antenna-ligand in visible-emitting photoluminescent lanthanide complexes
Bortoluzzi, Marco; Reolon, Andrea; Castro, Jesús; Enrichi, Francesco; Albertin, Gabriele; Bragato, Carlo; RSC Adv.  (2016) –; doi:10.1039/C6RA01741J

data_7224720
_publ_section_title
;
 The conjugate base of methyl 3-oxobutanoate as antenna-ligand in
 visible-emitting photoluminescent lanthanide complexes
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA01741J
_journal_year                    2016
_chemical_formula_sum            'C27 H29 N2 O9 Tb'
_chemical_formula_weight         684.44
_chemical_name_systematic        '[Tb(MAA)3(phen)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-01-18 deposited with the CCDC.
2016-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.1135(10)
_cell_angle_beta                 88.7925(10)
_cell_angle_gamma                87.0863(8)
_cell_formula_units_Z            4
_cell_length_a                   9.3684(2)
_cell_length_b                   16.6936(3)
_cell_length_c                   18.2672(4)
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.58
_cell_measurement_theta_min      3.39
_cell_volume                     2832.25(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Incoatec Quazar MX multilayer optics'
_diffrn_radiation_source         'Incoatec I\muS microsource'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0612
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_laue_measured_fraction_full 0.976
_diffrn_reflns_laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57616
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.172
_diffrn_reflns_theta_min         2.437
_exptl_absorpt_coefficient_mu    12.743
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.3489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethylether - dichloromethane'
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         10084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+3.5341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7399
_reflns_number_total             10084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra01741j2.cif
_cod_data_source_block           flip_RLN_37
_cod_database_code               7224720
_shelx_estimated_absorpt_t_min   0.244
_shelx_estimated_absorpt_t_max   0.340
_shelxl_version_number           2014/6
_shelx_res_checksum              38884