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_7045670
_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(H2 O)'
_chemical_formula_sum            'C42 H39 N6 O8 S2 Yb'
_chemical_formula_weight         992.95
_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                103.12(3)
_cell_angle_beta                 101.74(3)
_cell_angle_gamma                93.34(3)
_cell_formula_units_Z            4
_cell_length_a                   12.530(3)
_cell_length_b                   15.640(3)
_cell_length_c                   22.612(5)
_cell_measurement_reflns_used    200
_cell_measurement_temperature    100
_cell_measurement_theta_max      50
_cell_measurement_theta_min      2
_cell_volume                     4199.9(18)
_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      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42603
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         2.058
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.544
_exptl_absorpt_correction_T_max  0.2208
_exptl_absorpt_correction_T_min  0.0926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1644 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.4194. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             1996
_exptl_crystal_recrystallization_method 'crystallized from DMSO'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.366
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         14262
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+9.2354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10006
_reflns_number_total             14262
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04387b2.cif
_cod_data_source_block           a_CCDC1
_cod_original_cell_volume        4200.2(16)
_cod_database_code               7045670
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C44-C43 = C48-C43 = C48-C47 = C46-C47 = C46-C45 = C45-C44
 1.4 with sigma of 0.02
 C44'-C43 = C45'-C44' = C45'-C46' = C47'-C48' = C48'-C43
 1.4 with sigma of 0.02
 N41A-H41A = N41-H41
 0.9 with sigma of 0.02
3. Restrained planarity
 C43, C48, C47, C44, C45, C46
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C43 \\sim C48 \\sim C47 \\sim C46' \\sim C44' \\sim C45' \\sim C44 \\sim C45
\\sim C46 \\sim C47' \\sim C48': within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C44')=Sof(H44')=Sof(C45')=Sof(H45')=Sof(C46')=Sof(H46')=Sof(C47')=
 Sof(H47')=Sof(C48')=Sof(H48')=1-FVAR(1)
 Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=
 Sof(C48)=Sof(H48)=FVAR(1)
6.a Riding coordinates:
 O3W(H3WA,H3WB), O2W(H2WA,H2WB), O1W(H1WA,H1WB), O4W(H4WA,H4WB)
6.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'), C44(H44), C45(H45),
  C46(H46), C47(H47), C48(H48), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A),
 C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C15A(H15A), C20A(H20A),
 C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A),
 C29A(H29A), C30A(H30A), C34A(H34A), C35A(H35A), C36A(H36A), C37A(H37A),
 C39A(H39A), C44A(H44A), C45A(H45A), C46A(H46A), C47A(H47A), C48A(H48A)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C31(H31A,H31B,H31C), C7A(H7AA,H7AB,H7AC), C31A(H31D,H31E,H31F)
;
_shelx_res_checksum              72763
_olex2_exptl_crystal_mounting_method 'mounted on a needle'
_olex2_submission_special_instructions 'No special instructions were received'