Lanthanide Complexes with 2-(Tosylamino)-benzylidene-N-(aryloyl)hydrazones: Universal Luminescent Materials
Kovalenko, Anton; Rublev, Pavel O.; Tcelykh, Lyubov O.; Goloveshkin, Alexander S.; Lepnev, Leonid S.; Burlov, Anatolii S.; Vashchenko, Andrey A.; Marciniak, Łukasz; Magerramov, Abel M.; Shikhaliyev, Namig G.; Vatsadze, Sergey Z.; Utochnikova, Valentina V.; Chemistry of Materials 31 (2019) 759–; doi:10.1021/acs.chemmater.8b03675

data_4003083
_publ_section_title
;
 Lanthanide Complexes with
 2-(Tosylamino)-benzylidene-N-(aryloyl)hydrazones: Universal Luminescent
 Materials
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              759
_journal_paper_doi               10.1021/acs.chemmater.8b03675
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C40 H33 N8 O6 S2 Yb, 0.5(C2 H6 O)'
_chemical_formula_sum            'C41 H36 N8 O6.5 S2 Yb'
_chemical_formula_weight         981.94
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.490(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.876(3)
_cell_length_b                   13.3570(19)
_cell_length_c                   19.197(3)
_cell_measurement_reflns_used    2817
_cell_measurement_temperature    120
_cell_measurement_theta_max      21.70
_cell_measurement_theta_min      2.24
_cell_volume                     4103.9(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1758
_diffrn_reflns_av_unetI/netI     0.1369
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            47469
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.89
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0799 after correction.
The Ratio of minimum to maximum transmission is 0.8027.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.969
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10208
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+7.5347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1441
_reflns_number_gt                5968
_reflns_number_total             10208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm8b03675_si_001.cif
_cod_data_source_block           a
_cod_original_cell_volume        4103.8(10)
_cod_original_formula_sum        'C41 H36 N8 O6.50 S2 Yb'
_cod_database_code               4003083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2SB,H2SA,H3} of C2S
 At 1.5 times of:
  All O(H) groups, {H20A,H20B,H20C} of C20, {H40A,H40B,H40C} of C40, {H3SC,
  H3SB,H3SA} of C3S
2. Restrained distances
 O1S-C2S
 1.4 with sigma of 0.02
 C2S-C3S
 1.5 with sigma of 0.02
 N3-H3
 0.85 with sigma of 0.02
 N8_$1-H3
 2 with sigma of 0.02
 H3-N8_$1
 1.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3S) = Uanis(C2S) = Uanis(O1S)
4. Others
 Fixed Sof: O1S(0.5) H1S(0.5) C3S(0.5) H3SC(0.5) H3SB(0.5) H3SA(0.5) C2S(0.5)
 H2SB(0.5) H2SA(0.5)
5.a Riding coordinates:
 O1S(H1S)
5.b Secondary CH2 refined with riding coordinates:
 C2S(H2SB,H2SA)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C18(H18), C27(H27), C15(H15), C32(H32), C3(H3A), C24(H24), C7(H7),
 C5(H5), C6(H6), C4(H4), C10(H10), C26(H26), C16(H16), C35(H35), C11(H11),
 C19(H19), C31(H31), C9(H9), C38(H38), C39(H39), C23(H23), C36(H36), C12(H12),
 C29(H29), C30(H30)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C40(H40A,H40B,H40C), C3S(H3SC,H3SB,H3SA)
;
_olex2_submission_special_instructions 'No special instructions were received'