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_4349896
_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 Ho N4 O6 S3'
_chemical_formula_sum            'C38 H22 F9 Ho N4 O6 S3'
_chemical_formula_weight         1062.70
_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     iterative
_audit_creation_date             2018-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-22 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.004(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3064(4)
_cell_length_b                   21.3468(7)
_cell_length_c                   18.8868(7)
_cell_measurement_reflns_used    4872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.0180
_cell_measurement_theta_min      4.3910
_cell_volume                     4031.8(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    '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 0.960
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
  1 omega  -38.00   32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000  -90.0000 70

  2 omega  -49.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000 -150.0000 57

  3 omega  -46.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.8162   38.0000  -30.0000 81

  4 omega  -30.00   51.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       39.8162  -38.0000   60.0000 81

  5 omega   30.00   84.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  -30.0000 54

  6 omega   85.00  173.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 88

  7 omega   83.00  176.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   61.0000 -120.0000 93

  8 omega   45.00   88.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000  120.0000 43

  9 omega   47.00   79.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000 -150.0000 32

 10 omega  146.00  175.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  112.0000  -30.0000 29

 11 omega   54.00   79.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -30.0000    0.0000 25

 12 omega   40.00   73.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -95.0000  120.0000 33
;
_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      0.0838841000
_diffrn_orient_matrix_UB_12      0.0505654000
_diffrn_orient_matrix_UB_13      -0.0265026000
_diffrn_orient_matrix_UB_21      -0.0212302000
_diffrn_orient_matrix_UB_22      -0.0336842000
_diffrn_orient_matrix_UB_23      -0.0740704000
_diffrn_orient_matrix_UB_31      -0.1275147000
_diffrn_orient_matrix_UB_32      0.0388948000
_diffrn_orient_matrix_UB_33      -0.0296137000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12909
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.998
_diffrn_reflns_theta_min         3.178
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34851
_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    1.751
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.550
_refine_diff_density_min         -6.693
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7284
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.834
_refine_ls_R_factor_all          0.1849
_refine_ls_R_factor_gt           0.1593
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4291
_refine_ls_wR_factor_ref         0.4484
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5642
_reflns_number_total             7284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst40
_cod_database_code               4349896
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'O9 C38 h20ho11 N6 f9 s3'
_reflns_odcompleteness_completeness 95.73
_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-C7A
 1.5 with sigma of 0.02
 C35-C3
 1.5 with sigma of 0.02
 C31-C21A
 1.5 with sigma of 0.02
 C31-C21
 1.5 with sigma of 0.02
 C23-C7
 1.5 with sigma of 0.02
 C23-S3A
 1.7 with sigma of 0.02
 S3A-C6
 1.7 with sigma of 0.02
 C23-S3
 1.7 with sigma of 0.02
 S3-C5
 1.7 with sigma of 0.02
 C31-S2A
 1.7 with sigma of 0.02
 S2A-C20
 1.7 with sigma of 0.02
 S2-C31
 1.7 with sigma of 0.02
 S2-C19
 1.7 with sigma of 0.02
 C35-S1
 1.7 with sigma of 0.02
 S1-C1
 1.7 with sigma of 0.02
 S1A-C35
 1.7 with sigma of 0.02
 S1A-C2
 1.7 with sigma of 0.02
 C3-C35
 1.5 with sigma of 0.02
 C35-C3A
 1.5 with sigma of 0.02
 C3A-C1
 1.5 with sigma of 0.02
 C7A-C5
 1.5 with sigma of 0.02
 C21A-C19
 1.5 with sigma of 0.02
3. Restrained planarity
 C3A, S1A, C2, C1, C35
 with sigma of 0.1
 S1, C3, C35, C2, C1
 with sigma of 0.1
 C35, C3, C2, C1, S1
 with sigma of 0.1
 C35, C3A, C1, C2, S1A
 with sigma of 0.1
 C31, C21A, C19, C20, S2A
 with sigma of 0.1
 S2, C19, C20, C21, C31
 with sigma of 0.1
 C7A, C5, C6, S3A, C23
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(S3) = Uanis(S3A)
Uanis(S1) = Uanis(S1A)
Uanis(C21A) = Uanis(C21)
Uanis(C3A) = Uanis(C3)
Uanis(O5) = Uanis(O3) = Uanis(O2) = Uanis(O1) = Uanis(O6) = Uanis(O4) =
Uanis(Ho1)
Uanis(N4) = Uanis(N3) = Uanis(N2) = Uanis(N1)
Uanis(C7A) = Uanis(S3)
5. Others
 Sof(H2B)=Sof(H1B)=Sof(S1A)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(H2A)=Sof(H1A)=Sof(S1)=Sof(C3)=Sof(H3)=FVAR(1)
 Sof(H19A)=Sof(H20A)=Sof(S2A)=Sof(C21A)=Sof(H21A)=1-FVAR(2)
 Sof(H19)=Sof(H20)=Sof(S2)=Sof(C21)=Sof(H21)=FVAR(2)
 Sof(H5B)=Sof(H6B)=Sof(S3A)=Sof(C7A)=Sof(H7A)=1-FVAR(3)
 Sof(H5A)=Sof(H6A)=Sof(S3)=Sof(C7)=Sof(H7)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2B), C2(H2A), C1(H1B), C1(H1A), C4(H4), C5(H5A), C5(H5B), C6(H6A),
 C6(H6B), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C19(H19A), C20(H20),
 C20(H20A), C22(H22), C3A(H3A), C3(H3), C21(H21), C21A(H21A), C7(H7), C7A(H7A)
;
_shelx_res_checksum              21570
_shelx_hkl_checksum              41824
_olex2_submission_special_instructions 'No special instructions were received'