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_4349891
_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 Tm'
_chemical_formula_sum            'C38 H22 F9 N4 O6 S3 Tm'
_chemical_formula_weight         1066.70
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7870(4)
_cell_length_b                   18.7993(5)
_cell_length_c                   15.3065(3)
_cell_measurement_reflns_used    8781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.9680
_cell_measurement_theta_min      3.6890
_cell_volume                     4236.39(18)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega -115.00    6.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  -19.0000  120.0000 121

  2 omega  -35.00   31.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787   38.0000  -60.0000 66

  3 omega -118.00  -60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.3787  178.0000  -90.0000 58

  4 omega  101.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       40.3787  178.0000   60.0000 27

  5 omega   36.00   85.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 49

  6 omega   36.00  107.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -90.0000 71

  7 omega   35.00   78.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  150.0000 43

  8 omega  110.00  167.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000 -120.0000 57

  9 omega  107.00  178.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000   90.0000 71

 10 omega  103.00  169.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  120.0000 66

 11 omega   68.00   94.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000  -60.0000 26

 12 omega   36.00   71.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  -30.0000 35

 13 omega   38.00   88.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000 -112.0000 -150.0000 50
;
_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      0.0676906000
_diffrn_orient_matrix_UB_12      0.0444384000
_diffrn_orient_matrix_UB_13      -0.0477733000
_diffrn_orient_matrix_UB_21      0.0720907000
_diffrn_orient_matrix_UB_22      -0.0587631000
_diffrn_orient_matrix_UB_23      0.0173814000
_diffrn_orient_matrix_UB_31      -0.0340259000
_diffrn_orient_matrix_UB_32      -0.0358646000
_diffrn_orient_matrix_UB_33      -0.0874637000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17128
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.490
_diffrn_reflns_theta_min         3.734
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56772
_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    1.672
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8235
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+10.3804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7080
_reflns_number_total             8235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst100
_cod_original_cell_volume        4236.41(17)
_cod_database_code               4349891
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C38 H22 tm1 N4 O6 s3 f9'
_reflns_odcompleteness_completeness 99.19
_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
 C31-S2A
 1.68 with sigma of 0.02
 S2A-C20
 1.68 with sigma of 0.02
 C31-S2
 1.68 with sigma of 0.02
 S2-C19
 1.68 with sigma of 0.02
 C23-S3
 1.68 with sigma of 0.02
 S3-C5
 1.68 with sigma of 0.02
 C23-S3A
 1.68 with sigma of 0.02
 C35-S1A
 1.68 with sigma of 0.02
 C35-S1
 1.68 with sigma of 0.02
 S1-C1
 1.68 with sigma of 0.02
 C35-C3A
 1.46 with sigma of 0.02
 C3A-C1
 1.46 with sigma of 0.02
 C2-C3
 1.46 with sigma of 0.02
 C3-C35
 1.46 with sigma of 0.02
 C21-C20
 1.46 with sigma of 0.02
 C31-C19
 1.46 with sigma of 0.02
 C23-C7
 1.46 with sigma of 0.02
 C23-C7A
 1.46 with sigma of 0.02
 S1A-C2
 1.68 with sigma of 0.02
 S3A-C6
 1.68 with sigma of 0.005
 C31-C21A
 1.46 with sigma of 0.02
 C21A-C19
 1.46 with sigma of 0.02
 C6-C7
 1.46 with sigma of 0.02
 C31-C21
 1.46 with sigma of 0.005
 C7A-C5
 1.46 with sigma of 0.005
 C7-C6
 1.46 with sigma of 0.005
 C3-C2
 1.46 with sigma of 0.005
 C35-C3
 1.46 with sigma of 0.005
3. Restrained planarity
 S2A, C31, C21A, C19, C20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C35) = Uanis(C3) = Uanis(S1A) = Uanis(C2) = Uanis(C1) = Uanis(S1) =
Uanis(C3A)
Uanis(C23) = Uanis(C7) = Uanis(S3A) = Uanis(C6) = Uanis(C5) = Uanis(S3) =
Uanis(C7A)
Uanis(C31) = Uanis(C21) = Uanis(S2) = Uanis(C19) = Uanis(C20) = Uanis(C21A) =
Uanis(S2A)
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(C7A)=Sof(H7A)=Sof(S3A)=Sof(H6B)=Sof(H5B)=1-FVAR(2)
 Sof(S3)=Sof(C7)=Sof(H7)=Sof(H6A)=Sof(H5A)=FVAR(2)
 Sof(C21A)=Sof(H21A)=Sof(S2A)=Sof(H19A)=Sof(H20A)=1-FVAR(3)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H19)=Sof(H20)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C21A(H21A), C3A(H3A), C7A(H7A), C7(H7), C3(H3), C15(H15), C8(H8), C21(H21),
 C4(H4), C18(H18), C22(H22), C2(H2B), C2(H2A), C16(H16), C19(H19), C19(H19A),
 C1(H1A), C1(H1B), C9(H9), C14(H14), C13(H13), C17(H17), C20(H20A), C20(H20),
 C12(H12), C10(H10), C6(H6B), C6(H6A), C5(H5A), C5(H5B), C11(H11)
;
_shelx_res_checksum              98079
_shelx_hkl_checksum              21671
_shelx_fab_checksum              64412
_olex2_submission_special_instructions 'No special instructions were received'