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_4349895
_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 Nd O6 S3'
_chemical_formula_sum            'C38 H22 F9 N4 Nd O6 S3'
_chemical_formula_weight         1042.01
_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             2017-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-03 deposited with the CCDC.
2018-09-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.492(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4079(7)
_cell_length_b                   12.7965(5)
_cell_length_c                   19.1081(7)
_cell_measurement_reflns_used    13035
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.7040
_cell_measurement_theta_min      3.0490
_cell_volume                     4252.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -89.00  -62.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -63.0000  -92.0000 27

  2 omega   21.00   46.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   57.0000    0.0000 25

  3 omega  -80.00  -36.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241 -178.0000    0.0000 44

  4 omega  -65.00  -28.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -57.0000  120.0000 37

  5 omega  -45.00   38.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       23.5178  -57.0000  -30.0000 83

  6 omega    3.00   78.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       23.5178   57.0000  -30.0000 75

  7 omega   -7.00   94.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       23.5178   77.0000 -150.0000 101

  8 omega  -25.00   65.00   1.0000    1.1200
omega____ theta____ kappa____ phi______ frames
    -       23.5178  -99.0000   90.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0211959000
_diffrn_orient_matrix_UB_12      -0.0278583000
_diffrn_orient_matrix_UB_13      -0.0247584000
_diffrn_orient_matrix_UB_21      0.0337392000
_diffrn_orient_matrix_UB_22      0.0276693000
_diffrn_orient_matrix_UB_23      0.0110163000
_diffrn_orient_matrix_UB_31      0.0086407000
_diffrn_orient_matrix_UB_32      -0.0391074000
_diffrn_orient_matrix_UB_33      0.0254519000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39898
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.946
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.240
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.100
_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         9743
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+10.3835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8386
_reflns_number_total             9743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst110
_cod_database_code               4349895
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c38 h29 o6 f9 n2 nd1 s3'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.51
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 S2-C19
 1.68 with sigma of 0.02
 C21-C31
 1.46 with sigma of 0.02
 C20-C19
 1.46 with sigma of 0.02
 C21A-C31
 1.46 with sigma of 0.02
 C21A-C19
 1.46 with sigma of 0.02
 C7A-C23
 1.46 with sigma of 0.02
 C7A-C5
 1.46 with sigma of 0.02
 C23-C7
 1.46 with sigma of 0.02
 C7-C6
 1.46 with sigma of 0.02
 C35-C3A
 1.46 with sigma of 0.02
 C3A-C1
 1.46 with sigma of 0.02
 C3-C2
 1.46 with sigma of 0.02
 C35-S1A
 1.68 with sigma of 0.02
 S1A-C2
 1.68 with sigma of 0.02
 C1-S1
 1.68 with sigma of 0.02
 S1-C35
 1.68 with sigma of 0.02
 S3A-C23
 1.68 with sigma of 0.02
 C5-S3
 1.68 with sigma of 0.02
 C23-S3
 1.68 with sigma of 0.02
 S2A-C20
 1.68 with sigma of 0.005
 S3A-C6
 1.68 with sigma of 0.005
3. Restrained planarity
 C21A, C31, S2A, C20, C19
 with sigma of 0.1
 C7A, C23, S3A, C6, C5
 with sigma of 0.1
 C3A, C1, C2, S1A, C35
 with sigma of 0.1
 C23, C7A, C5, C6, S3A
 with sigma of 0.1
 C23, S3, C7, C6, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C21) = Uanis(S2A) = Uanis(C20) = Uanis(C19) = Uanis(S2) =
Uanis(C21A)
Uanis(C23) = Uanis(S3) = Uanis(C5) = Uanis(C6) = Uanis(C7A) = Uanis(C7) =
Uanis(S3A)
Uanis(C35) = Uanis(C3A) = Uanis(S1) = Uanis(C1) = Uanis(C2) = Uanis(C3) =
Uanis(S1A)
5. Others
 Sof(S1A)=Sof(H1B)=Sof(H2B)=Sof(C3A)=Sof(H3A)=1-FVAR(1)
 Sof(S1)=Sof(H1A)=Sof(H2A)=Sof(C3)=Sof(H3)=FVAR(1)
 Sof(H19)=Sof(H20)=Sof(S2A)=Sof(C21A)=Sof(H21A)=1-FVAR(2)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H19A)=Sof(H20A)=FVAR(2)
 Sof(H5B)=Sof(H6B)=Sof(C7A)=Sof(H7A)=Sof(S3A)=1-FVAR(3)
 Sof(S3)=Sof(C7)=Sof(H7)=Sof(H5A)=Sof(H6A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C21(H21), C10(H10), C18(H18), C22(H22), C5(H5A), C5(H5B), C19(H19A),
 C19(H19), C17(H17), C4(H4), C1(H1A), C1(H1B), C11(H11), C14(H14), C16(H16),
 C6(H6A), C6(H6B), C9(H9), C8(H8), C2(H2B), C2(H2A), C20(H20A), C20(H20),
 C12(H12), C15(H15), C13(H13), C3(H3), C3A(H3A), C21A(H21A), C7A(H7A)
;
_shelx_res_checksum              46887
_shelx_hkl_checksum              16047
_shelx_fab_checksum              29960
_olex2_submission_special_instructions 'No special instructions were received'