The peculiarities of complex formation and energy transfer processes in lanthanide complexes with 2-(tosylamino)-benzylidene-N-benzoylhydrazone
Kovalenko, Anton D.; Bushmarinov, Ivan S.; Burlov, Anatoly D.; Lepnev, Leonid; Ilina, Elena G.; Utochnikova, Valentina V.; Dalton Transactions  (2018) –; doi:10.1039/C7DT04387B

data_7045671
_publ_section_title
;
 The peculiarities of complex formation and energy transfer processes in
 lanthanide complexes with 2-(tosylamino)-benzylidene-N-benzoylhydrazone
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT04387B
_journal_year                    2018
_chemical_formula_moiety         'C42 H35 N6 O6 S2 Yb, 2(C2 H6 O), H2 O'
_chemical_formula_sum            'C46 H49 N6 O9 S2 Yb'
_chemical_formula_weight         1067.07
_chemical_name_systematic
'ytterbium 2-(tosylamino)benzylidene-N-benzoylhydrazonate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-06-16 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                77.5710(10)
_cell_angle_beta                 83.1210(10)
_cell_angle_gamma                75.2430(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7608(6)
_cell_length_b                   12.5093(7)
_cell_length_c                   17.4399(10)
_cell_measurement_reflns_used    5409
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      2.23
_cell_volume                     2211.7(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26258
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.894
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0866 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8335.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       prism
_exptl_crystal_F_000             1082
_exptl_crystal_recrystallization_method 'crystallized from ethanol'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.552
_refine_diff_density_min         -1.246
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10988
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0302P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8740
_reflns_number_total             10988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04387b2.cif
_cod_data_source_block           adk175
_cod_database_code               7045671
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1W-H1WA
 0.9 with sigma of 0.02
 O1W-H1WB
 0.9 with sigma of 0.02
 O1S-H1S
 0.9 with sigma of 0.02
3. Others
 Fixed Uiso: H2S(0.07)
 Fixed X: H2S(0.911489)
 Fixed Y: H2S(0.853971)
 Fixed Z: H2S(0.721061)
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C3S(H3SA,H3SB)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39),
 C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
4.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C31(H31A,H31B,H31C), C2S(H2SA,H2SB,H2SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              74771
_olex2_exptl_crystal_mounting_method 'mounted on a needle'
_olex2_submission_special_instructions 'No special instructions were received'