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_7045669
_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 H36 Lu N6 O6 S2, Cl'
_chemical_formula_sum            'C42 H36 Cl Lu N6 O6 S2'
_chemical_formula_weight         995.31
_chemical_name_systematic
'lutetium 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                87.312(2)
_cell_angle_beta                 73.030(2)
_cell_angle_gamma                85.7230(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6091(7)
_cell_length_b                   11.4231(7)
_cell_length_c                   17.4138(11)
_cell_measurement_reflns_used    4877
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.554
_cell_measurement_theta_min      2.446
_cell_volume                     2012.1(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0546
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20050
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.680
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0640 before and 0.0506 after correction. The Ratio of minimum to maximum transmission is 0.8224. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       irregular
_exptl_crystal_F_000             996
_exptl_crystal_recrystallization_method 'crystallized from ???'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.806
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         8227
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0350P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6591
_reflns_number_total             8227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04387b2.cif
_cod_data_source_block           a
_cod_database_code               7045669
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N41-H41
 0.9 with sigma of 0.02
 N17-H17
 0.9 with sigma of 0.02
3.a 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)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              50434
_olex2_exptl_crystal_mounting_method 'mounted on a needle'
_olex2_submission_special_instructions 'No special instructions were received'