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_4349894
_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 Dy F9 N4 O6 S3'
_chemical_formula_sum            'C38 H22 Dy F9 N4 O6 S3'
_chemical_formula_weight         1060.27
_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     iterative
_audit_creation_date             2017-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.894(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2806(8)
_cell_length_b                   21.385(3)
_cell_length_c                   18.8697(16)
_cell_measurement_reflns_used    1802
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0910
_cell_measurement_theta_min      4.3820
_cell_volume                     4027.1(8)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -49.00   23.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854   38.0000  120.0000 72

  2 omega  -47.00   33.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854   38.0000    0.0000 80

  3 omega   26.00   77.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854   38.0000 -120.0000 51

  4 omega   79.00  130.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854  178.0000    0.0000 51

  5 omega   53.00   82.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  -60.0000 29

  6 omega   40.00   84.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000   60.0000 44

  7 omega   86.00  178.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000 -120.0000 92

  8 omega   57.00  109.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -90.0000 52

  9 omega   87.00  178.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000  -60.0000 91

 10 omega   43.00   98.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000  -90.0000 55

 11 omega   40.00   90.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -30.0000  120.0000 50

 12 omega   98.00  125.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000  -30.0000 27

 13 omega  143.00  178.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  125.0000  -30.0000 35

 14 omega   42.00   79.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000   90.0000 37

 15 omega -105.00  -32.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854  -38.0000   60.0000 73

 16 omega  -27.00   13.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.1854   38.0000  -60.0000 40

 17 omega   62.00   89.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854  178.0000  150.0000 27

 18 omega   60.00  106.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854   77.0000 -150.0000 46

 19 omega   16.00   79.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -       41.1854  -99.0000   60.0000 63

 20 omega   96.00  122.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  120.0000 26

 21 omega   79.00  106.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000 -180.0000 27

 22 omega   87.00  118.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   90.0000 31

 23 omega  113.00  165.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   45.0000   30.0000 52

 24 omega   45.00   90.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -180.0000 45

 25 omega   89.00  172.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   30.0000  150.0000 83

 26 omega   68.00   95.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -60.0000 27

 27 omega   50.00  121.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -125.0000   60.0000 71

 28 omega   38.00   65.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -95.0000  -60.0000 27
;
_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      -0.1043336000
_diffrn_orient_matrix_UB_12      0.0222008000
_diffrn_orient_matrix_UB_13      -0.0683688000
_diffrn_orient_matrix_UB_21      0.0264970000
_diffrn_orient_matrix_UB_22      -0.0589283000
_diffrn_orient_matrix_UB_23      -0.0413306000
_diffrn_orient_matrix_UB_31      -0.1105940000
_diffrn_orient_matrix_UB_32      -0.0350804000
_diffrn_orient_matrix_UB_33      0.0262673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2303
_diffrn_reflns_av_unetI/netI     0.2197
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28131
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.992
_diffrn_reflns_theta_min         3.177
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71589
_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    1.749
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.078
_refine_diff_density_min         -2.051
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7578
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+39.6065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2099
_refine_ls_wR_factor_ref         0.2691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4018
_reflns_number_total             7578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst80
_cod_original_cell_volume        4027.1(7)
_cod_database_code               4349894
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'dy1 N4 C38 h22 f9 s3 o6'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     70.14
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C23-S3A
 1.69 with sigma of 0.02
 S3A-C6
 1.69 with sigma of 0.02
 C3A-C35
 1.44 with sigma of 0.02
 C3-C35
 1.44 with sigma of 0.02
 C31-C21A
 1.44 with sigma of 0.02
 C31-C21
 1.44 with sigma of 0.02
 C21A-C19
 1.46 with sigma of 0.02
 C35-C3A
 1.46 with sigma of 0.02
 C35-C3
 1.46 with sigma of 0.02
 C3A-C1
 1.46 with sigma of 0.02
 C7-C23
 1.46 with sigma of 0.02
 C7-C6
 1.46 with sigma of 0.02
 C23-C7A
 1.46 with sigma of 0.02
 C7A-C5
 1.46 with sigma of 0.02
 S1A-C2
 1.68 with sigma of 0.02
 S2A-C20
 1.68 with sigma of 0.02
 S2-C31
 1.68 with sigma of 0.02
3. Restrained planarity
 C31, C21A, C19, C20, S2A
 with sigma of 0.1
 C23, S3A, C6, C5, C7A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Dy1) = Uanis(O6)
Uanis(C31) = Uanis(S2) = Uanis(C19) = Uanis(C20) = Uanis(S2A) = Uanis(C21) =
Uanis(C21A)
Uanis(C35) = Uanis(C3) = Uanis(S1A) = Uanis(C2) = Uanis(C1) = Uanis(S1) =
Uanis(C3A)
Uanis(C23) = Uanis(S3) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(S3A) =
Uanis(C7A)
5. Others
 Sof(C3A)=Sof(H3A)=Sof(S1A)=Sof(H2B)=Sof(H1B)=1-FVAR(1)
 Sof(S1)=Sof(C3)=Sof(H3)=Sof(H2A)=Sof(H1A)=FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(S2A)=Sof(H20A)=Sof(H19A)=1-FVAR(2)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H20)=Sof(H19)=FVAR(2)
 Sof(C7A)=Sof(H7A)=Sof(S3A)=Sof(H6B)=Sof(H5B)=1-FVAR(3)
 Sof(S3)=Sof(H6A)=Sof(H5A)=Sof(C7)=Sof(H7)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C21A(H21A), C3A(H3A), C3(H3), C21(H21), C17(H17), C20(H20A),
 C20(H20), C14(H14), C19(H19), C19(H19A), C9(H9), C22(H22), C18(H18), C10(H10),
 C16(H16), C6(H6B), C6(H6A), C12(H12), C15(H15), C8(H8), C13(H13), C4(H4),
 C2(H2B), C2(H2A), C1(H1A), C1(H1B), C11(H11), C5(H5A), C5(H5B), C7(H7)
;
_shelx_res_checksum              43328
_shelx_hkl_checksum              970
_olex2_submission_special_instructions 'No special instructions were received'