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_4349888
_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 Sm'
_chemical_formula_sum            'C38 H22 F9 N4 O6 S3 Sm'
_chemical_formula_weight         1048.12
_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     direct
_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                 94.9294(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8835(3)
_cell_length_b                   18.8542(4)
_cell_length_c                   15.3188(3)
_cell_measurement_reflns_used    6834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3340
_cell_measurement_theta_min      3.0880
_cell_volume                     4282.81(15)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2096
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -88.00  -53.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2678  -57.0000   90.0000 35

  2 omega  -22.00   11.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2678  -99.0000  -60.0000 33

  3 omega  -38.00   50.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2678   57.0000 -120.0000 88

  4 omega  -92.00  -17.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2678    0.0000   90.0000 75
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0002198000
_diffrn_orient_matrix_UB_12      -0.0193344000
_diffrn_orient_matrix_UB_13      0.0397236000
_diffrn_orient_matrix_UB_21      0.0475861000
_diffrn_orient_matrix_UB_22      -0.0031546000
_diffrn_orient_matrix_UB_23      0.0018715000
_diffrn_orient_matrix_UB_31      0.0045403000
_diffrn_orient_matrix_UB_32      0.0321689000
_diffrn_orient_matrix_UB_33      0.0239975000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19971
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.832
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.605
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99555
_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    1.626
_exptl_crystal_description       prizm
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         9421
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0279P)^2^+4.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7554
_reflns_number_total             9421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qi00712h2.cif
_cod_data_source_block           hst70a
_cod_original_cell_volume        4282.83(14)
_cod_database_code               4349888
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'sm1 s3 F9 N4 C38 o6'
_reflns_odcompleteness_completeness 96.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C35-S1
 1.68 with sigma of 0.02
 C35-S1A
 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
 C35-C3
 1.46 with sigma of 0.02
 C31-S2
 1.68 with sigma of 0.02
 S2-C19
 1.68 with sigma of 0.02
 C31-S2A
 1.68 with sigma of 0.02
 C31-C21A
 1.46 with sigma of 0.02
 C21A-C19
 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
 C23-S3
 1.68 with sigma of 0.02
 S3-C5
 1.68 with sigma of 0.02
 C23-C7
 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
 C23-S3A
 1.68 with sigma of 0.02
 S3A-C6
 1.68 with sigma of 0.02
 C7-C6
 1.46 with sigma of 0.005
 C7-C23
 1.46 with sigma of 0.005
 S2A-C20
 1.68 with sigma of 0.005
 S1A-C2
 1.68 with sigma of 0.005
 C3-C2
 1.46 with sigma of 0.005
 C3-C35
 1.46 with sigma of 0.005
3. Restrained planarity
 S3A, C23, C7A, C5, C6
 with sigma of 0.1
 S2A, C21A, C31, C20, C19
 with sigma of 0.1
 S1A, C3A, C35, C1, C2
 with sigma of 0.1
 C7A, C23, S3A, C6, C5
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C23) = Uanis(S3) = Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(S3A) =
Uanis(C7A)
Uanis(C31) = Uanis(C21) = Uanis(S2A) = Uanis(C20) = Uanis(C19) = Uanis(S2) =
Uanis(C21A)
Uanis(C35) = Uanis(S1) = Uanis(C3A) = Uanis(C1) = Uanis(C2) = Uanis(S1A) =
Uanis(C3)
5. Others
 Sof(S1A)=Sof(C3A)=Sof(H3A)=Sof(H1B)=Sof(H2B)=1-FVAR(1)
 Sof(S1)=Sof(C3)=Sof(H3)=Sof(H1A)=Sof(H2A)=FVAR(1)
 Sof(S2A)=Sof(C21A)=Sof(H21A)=Sof(H20A)=Sof(H19A)=1-FVAR(2)
 Sof(S2)=Sof(C21)=Sof(H21)=Sof(H20)=Sof(H19)=FVAR(2)
 Sof(C7A)=Sof(H7A)=Sof(H6B)=Sof(H5B)=Sof(S3A)=1-FVAR(3)
 Sof(S3)=Sof(H6A)=Sof(H5A)=Sof(C7)=Sof(H7)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C7A(H7A), C18(H18), C10(H10), C9(H9), C3A(H3A), C3(H3), C6(H6B),
 C6(H6A), C4(H4), C17(H17), C5(H5A), C5(H5B), C7(H7), C8(H8), C12(H12),
 C11(H11), C1(H1A), C1(H1B), C14(H14), C15(H15), C2(H2B), C2(H2A), C13(H13),
 C21A(H21A), C21(H21), C22(H22), C20(H20A), C20(H20), C19(H19), C19(H19A)
;
_shelx_res_checksum              7118
_shelx_hkl_checksum              39814
_shelx_fab_checksum              26703
_olex2_submission_special_instructions 'No special instructions were received'