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_4349897
_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 Pr S3'
_chemical_formula_sum            'C38 H22 F9 N4 O6 Pr S3'
_chemical_formula_weight         1038.68
_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
_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                 95.551(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0472(7)
_cell_length_b                   18.9230(10)
_cell_length_c                   15.2845(8)
_cell_measurement_reflns_used    12194
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.8180
_cell_measurement_theta_min      3.0630
_cell_volume                     4331.7(4)
_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)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega    4.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000 -150.0000 88

  2 omega  -47.00   53.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -77.0000   90.0000 100

  3 omega   14.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000  150.0000 46

  4 omega  -41.00   -9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -57.0000  -60.0000 32

  5 omega  -99.00  -64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  178.0000   90.0000 35

  6 omega   54.00   82.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000  -60.0000 28

  7 omega   11.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   38.0000  -60.0000 85

  8 omega   -3.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000  120.0000 59
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0229106000
_diffrn_orient_matrix_UB_12      -0.0303390000
_diffrn_orient_matrix_UB_13      -0.0131982000
_diffrn_orient_matrix_UB_21      -0.0307753000
_diffrn_orient_matrix_UB_22      -0.0220293000
_diffrn_orient_matrix_UB_23      0.0195065000
_diffrn_orient_matrix_UB_31      -0.0277590000
_diffrn_orient_matrix_UB_32      -0.0007886000
_diffrn_orient_matrix_UB_33      -0.0402208000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40312
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.678
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.356
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72160
_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    1.593
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.256
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         9738
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0355P)^2^+15.5181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0951
_refine_ls_wR_factor_ref         0.1125
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7704
_reflns_number_total             9738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst90
_cod_database_code               4349897
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C38 H20 N5 s3 pr1 o6 f9'
_reflns_odcompleteness_completeness 97.27
_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
 C6-S3A
 1.68 with sigma of 0.02
 S3A-C23
 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
 C31-S2A
 1.68 with sigma of 0.02
 C31-S2
 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
 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
 C35-C3
 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
 C31-C21
 1.46 with sigma of 0.02
 C21-C20
 1.46 with sigma of 0.02
 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
 C23-C7
 1.46 with sigma of 0.02
 C3-C2
 1.46 with sigma of 0.02
 C2-S1A
 1.68 with sigma of 0.02
 C23-S3A
 1.68 with sigma of 0.02
 C20-S2A
 1.68 with sigma of 0.02
 S1A-C2
 1.68 with sigma of 0.02
 S1A-C35
 1.68 with sigma of 0.02
 S2-C19
 1.68 with sigma of 0.02
 S2A-C20
 1.68 with sigma of 0.02
3. Restrained planarity
 C23, C7A, C5, C6, S3A
 with sigma of 0.1
 C3A, C35, S1A, C2, C1
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(S3A) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(S3) =
Uanis(C7A)
Uanis(C31) = Uanis(C21) = Uanis(S2A) = Uanis(C20) = Uanis(C19) = Uanis(S2) =
Uanis(C21A)
Uanis(C35) = Uanis(S1A) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(C3A) =
Uanis(S1)
5. Others
 Sof(C21A)=Sof(H21A)=Sof(S2A)=Sof(H20A)=Sof(H19A)=1-FVAR(1)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H20)=Sof(H19)=FVAR(1)
 Sof(C3A)=Sof(H3A)=Sof(S1A)=Sof(H1B)=Sof(H2B)=1-FVAR(2)
 Sof(S1)=Sof(C3)=Sof(H3)=Sof(H1A)=Sof(H2A)=FVAR(2)
 Sof(C7A)=Sof(H7A)=Sof(S3A)=Sof(H5B)=Sof(H6B)=1-FVAR(3)
 Sof(S3)=Sof(C7)=Sof(H7)=Sof(H5A)=Sof(H6A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C21A(H21A), C3A(H3A), C9(H9), C12(H12), C15(H15), C3(H3), C7(H7),
 C5(H5A), C5(H5B), C10(H10), C1(H1A), C1(H1B), C14(H14), C8(H8), C2(H2B),
 C2(H2A), C16(H16), C22(H22), C13(H13), C18(H18), C17(H17), C6(H6B), C6(H6A),
 C21(H21), C4(H4), C20(H20A), C20(H20), C19(H19), C19(H19A), C11(H11)
;
_shelx_res_checksum              93312
_shelx_hkl_checksum              23705
_shelx_fab_checksum              66246
_olex2_submission_special_instructions 'No special instructions were received'