Heteroleptic β-diketonate Ln(iii) complexes decorated with pyridyl substituted pyridazine ligands: synthesis, structure and luminescence properties
Khistiaeva, Viktoria V.; Melnikov, Alexey S.; Slavova, Sofia O.; Sizov, Vladimir V.; Starova, Galina L.; Koshevoy, Igor O.; Grachova, Elena V.; Inorganic Chemistry Frontiers 5 (2018) 3015–; doi:10.1039/C8QI00712H

data_4349892
_publ_section_title
;
 Heteroleptic \b-diketonate Ln(iii) complexes decorated with pyridyl
 substituted pyridazine ligands: synthesis, structure and luminescence
 properties
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              3015
_journal_paper_doi               10.1039/C8QI00712H
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C38 H22 F9 N4 O6 S3 Tb'
_chemical_formula_sum            'C38 H22 F9 N4 O6 S3 Tb'
_chemical_formula_weight         1056.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-09
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.036(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2761(3)
_cell_length_b                   21.4121(9)
_cell_length_c                   18.9121(7)
_cell_measurement_reflns_used    11216
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9420
_cell_measurement_theta_min      4.3950
_cell_volume                     4037.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3829
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9997
_diffrn_measurement_details
;
  1 omega    2.00   46.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       39.8162  -99.0000  -30.0000 44

  2 omega   43.00   98.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 55

  3 omega   61.00  103.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000 -180.0000 42

  4 omega   52.00   91.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -90.0000 39

  5 omega   55.00   82.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 27

  6 omega   49.00   82.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000   90.0000 33

  7 omega   48.00   98.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  120.0000 50

  8 omega   48.00  106.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  120.0000 58

  9 omega   44.00   72.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 28

 10 omega   79.00  147.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 68

 11 omega  122.00  176.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 54

 12 omega  145.00  172.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000    0.0000 27

 13 omega  106.00  170.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  150.0000 64

 14 omega  -69.00  -35.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162  178.0000  -90.0000 34

 15 omega -119.00   -7.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162  -77.0000  120.0000 112

 16 omega -128.00  -39.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162 -178.0000 -180.0000 89

 17 omega  -49.00   30.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000 -180.0000 79

 18 omega  -18.00   27.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   36.0000  123.0000 45

 19 omega    7.00   34.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000  150.0000 27

 20 omega  -50.00   36.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000 -120.0000 86

 21 omega   63.00  108.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       39.8162 -178.0000 -150.0000 45

 22 omega   31.00   59.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       39.8162  -99.0000 -120.0000 28

 23 omega   50.00  103.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000    0.0000 53

 24 omega   52.00   90.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   90.0000 38

 25 omega   51.00   78.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000   30.0000 27

 26 omega   68.00   93.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  150.0000 25

 27 omega   44.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000   90.0000 71

 28 omega   88.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -150.0000 27

 29 omega   57.00   84.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 27

 30 omega  102.00  129.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -150.0000 27

 31 omega   87.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -120.0000 28

 32 omega   68.00  115.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000  -30.0000 47

 33 omega   86.00  177.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000  -90.0000 91

 34 omega   30.00   55.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 25

 35 omega   87.00  156.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   30.0000    0.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0479958000
_diffrn_orient_matrix_UB_12      -0.0664472000
_diffrn_orient_matrix_UB_13      -0.0247987000
_diffrn_orient_matrix_UB_21      -0.0533378000
_diffrn_orient_matrix_UB_22      0.0238145000
_diffrn_orient_matrix_UB_23      -0.0785485000
_diffrn_orient_matrix_UB_31      0.1368545000
_diffrn_orient_matrix_UB_32      -0.0139661000
_diffrn_orient_matrix_UB_33      -0.0162968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0986
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29434
_diffrn_reflns_theta_full        69.99
_diffrn_reflns_theta_max         69.99
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.05183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.586
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0920
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+111.3449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2061
_reflns_number_gt                6508
_reflns_number_total             7605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst60a
_cod_original_cell_volume        4037.1(3)
_cod_database_code               4349892
_chemical_oxdiff_formula         'tb1 C38 n4 h32 o8 f9 s3'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97