Crystal structures and intense luminescence of tris(3-(2'-pyridyl)-pyrazolyl)borate Tb(3+) and Eu(3+) complexes with carboxylate co-ligands.
Mikhalyova, Elena A.; Yakovenko, Anastasiya V.; Zeller, Matthias; Gavrilenko, Konstantin S.; Kiskin, Mikhail A.; Smola, Sergey S.; Dotsenko, Vladimir P.; Eremenko, Igor L.; Addison, Anthony W.; Pavlishchuk, Vitaly V.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3457–3469; doi:10.1039/c6dt04757b

data_7041706
_publ_section_title
;
 Crystal structures and intense luminescence of
 tris(3-(2'-pyridyl)-pyrazolyl)borate Tb(3+) and Eu(3+) complexes with
 carboxylate co-ligands.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3457
_journal_page_last               3469
_journal_paper_doi               10.1039/c6dt04757b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C60 H48 B2 N18 O10 Tb2, 6(C H4 O), 1.084(H2 O)'
_chemical_formula_sum            'C66 H74.17 B2 N18 O17.08 Tb2'
_chemical_formula_weight         1732.33
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-22 deposited with the CCDC.
2017-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                111.837(3)
_cell_angle_beta                 116.813(3)
_cell_angle_gamma                94.321(4)
_cell_formula_units_Z            1
_cell_length_a                   12.432(3)
_cell_length_b                   13.512(3)
_cell_length_c                   13.553(3)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.57
_cell_measurement_theta_min      2.32
_cell_volume                     1803.0(7)
_computing_cell_refinement       'Apex2 v2011.2-0'
_computing_data_collection       'Apex2 v2011.2-0 (Bruker, 2011)'
_computing_data_reduction        'SAINT, V7.66A (Bruker, 2011)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2015), 
SHELXLE Rev780 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21240
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.763
_diffrn_reflns_theta_min         1.698
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.026
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.5945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2  v2011.2-0 (Bruker, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             872.8
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_refine_diff_density_max         5.918
_refine_diff_density_min         -3.471
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         11026
_refine_ls_number_restraints     107
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0431P)^2^+9.4808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9891
_reflns_number_total             11026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04757b2.cif
_cod_data_source_block           12mz340_0m
_cod_depositor_comments
'Adding full bibliography for 7041696--7041708.cif.'
_cod_original_cell_volume        1803.0(8)
_cod_database_code               7041706
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.572
_shelx_estimated_absorpt_t_max   0.664
_shelx_res_checksum              24708