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_4349893
_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 H23 Eu F9 N4 O6 S3'
_chemical_formula_sum            'C38 H23 Eu F9 N4 O6 S3'
_chemical_formula_weight         1050.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-01-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-01-23 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.893(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.2613(11)
_cell_length_b                   10.2407(5)
_cell_length_c                   16.5383(6)
_cell_measurement_reflns_used    9528
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7680
_cell_measurement_theta_min      3.4050
_cell_volume                     4099.5(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 0.9973
_diffrn_measured_fraction_theta_max 0.9973
_diffrn_measurement_details
;
  1 omega  -26.00   93.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       12.8719   19.0000  150.0000 119

  2 omega   46.00   95.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       12.8719 -178.0000    0.0000 49

  3 omega  -53.00   19.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       12.8719  -38.0000  150.0000 72

  4 omega  -20.00    3.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1536  -99.0000 -180.0000 23
;
_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      0.0287513000
_diffrn_orient_matrix_UB_12      -0.0111820000
_diffrn_orient_matrix_UB_13      -0.0014792000
_diffrn_orient_matrix_UB_21      -0.0049711000
_diffrn_orient_matrix_UB_22      -0.0338895000
_diffrn_orient_matrix_UB_23      -0.0372220000
_diffrn_orient_matrix_UB_31      0.0025695000
_diffrn_orient_matrix_UB_32      0.0593760000
_diffrn_orient_matrix_UB_33      -0.0214798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26576
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84075
_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    1.702
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         5.508
_refine_diff_density_min         -5.056
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         9364
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0988
_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^)+(0.0487P)^2^+110.8898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7670
_reflns_number_total             9364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst74a
_cod_database_code               4349893
_chemical_oxdiff_formula         'c38 h22 n4 eu1 o6 s3 f9'
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C7-C23
 1.46 with sigma of 0.02
 C7A-C23
 1.46 with sigma of 0.02
 S3A-C6
 1.69 with sigma of 0.02
 C28-C27
 1.46 with sigma of 0.02
3. Restrained planarity
 S1, C35, C3, C2
 with sigma of 0.1
 C35, S1, C1, C2, C3
 with sigma of 0.1
 C35, S1, C1A, C2A, C3A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C27) = Uanis(N4) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
Uanis(C35) = Uanis(C3) = Uanis(C2) = Uanis(C2A) = Uanis(C3A) = Uanis(C1) =
Uanis(C1A)
Uanis(C7) = Uanis(C23) = Uanis(C7A) = Uanis(C5) = Uanis(C6)
Uanis(C12) = Uanis(C12A) = Uanis(C27) = Uanis(C27A) = Uanis(N4A) = Uanis(N4) =
Uanis(C9A) = Uanis(C10A) = Uanis(C10) = Uanis(C11A) = Uanis(C11)
Uanis(N2) = Uanis(N3) = Uanis(C28) = Uanis(C13) = Uanis(C14) = Uanis(C29)
Uanis(C31) = Uanis(S2) = Uanis(C19) = Uanis(C20) = Uanis(C21)
Uanis(C8) = Uanis(C25) = Uanis(C24)
5. Others
 Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C1A)=Sof(H1A)=1-FVAR(1)
 Sof(C3)=Sof(H3)=Sof(C2)=Sof(H2)=Sof(C1)=Sof(H1)=FVAR(1)
 Sof(N4A)=Sof(H4AA)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(H12A)=
 Sof(C11A)=Sof(H11A)=Sof(C27A)=1-FVAR(2)
 Sof(C27)=Sof(C12)=Sof(H12)=Sof(C11)=Sof(H11)=Sof(N4)=Sof(H4A)=Sof(C9)=Sof(H9)=
 Sof(C10)=Sof(H10)=FVAR(2)
 Sof(S3A)=Sof(H5B)=Sof(H6B)=Sof(C7A)=Sof(H7A)=1-FVAR(3)
 Sof(S3)=Sof(H5A)=Sof(H6A)=Sof(C7)=Sof(H7)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C16(H16), C15(H15), C13(H13), C18(H18), C20(H20), C22(H22),
 C17(H17), C14(H14), C4(H4), C5(H5A), C5(H5B), C6(H6B), C6(H6A), C8(H8),
 C12(H12), C11(H11), C19(H19), N4(H4A), C9(H9), C10(H10), C2A(H2A), C3A(H3A),
 C3(H3), C2(H2), C7A(H7A), C7(H7), C1A(H1A), C1(H1), N4A(H4AA), C9A(H9A),
 C10A(H10A), C12A(H12A), C11A(H11A)
;
_shelx_res_checksum              15000
_shelx_hkl_checksum              3355
_shelx_fab_checksum              7713
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'