Synthesis and photophysical properties of rare earth (La, Nd, Gd, Y, Ho) complexes with silanediamido ligands bearing a chelating phenylbenzothiazole chromophore
Mironova, Olga A.; Ryadun, Aleksey A.; Sukhikh, Taisiya S.; Pushkarevsky, Nikolay A.; Konchenko, Sergey N.; New Journal of Chemistry 47 (2023) 3406–3416; doi:10.1039/D2NJ05540F

data_7062248
_publ_section_title
;
 Synthesis and photophysical properties of rare earth (La, Nd, Gd, Y, Ho)
 complexes with silanediamido ligands bearing a chelating
 phenylbenzothiazole chromophore
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3406
_journal_page_last               3416
_journal_paper_doi               10.1039/D2NJ05540F
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety
'C56 H44 N8 Nd S4 Si2, C16 H32 Li O4, 2(C4 H8 O)'
_chemical_formula_sum            'C80 H92 Li N8 Nd O6 S4 Si2'
_chemical_formula_weight         1597.21
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-11-05 deposited with the CCDC.	2022-12-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8134(8)
_cell_length_b                   22.6439(8)
_cell_length_c                   17.0123(5)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.78
_cell_measurement_theta_min      2.39
_cell_volume                     7632.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_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      150(2)
_diffrn_detector                 PIXEL
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Incoatec HELIOS multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.891
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1051 before and 0.0686 after correction. The Ratio of minimum to maximum transmission is 0.9450. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       prism
_exptl_crystal_F_000             3324
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9096
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+9.2445P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6824
_reflns_number_total             9096
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa381
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_database_code               7062248
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C37
 2.35 with sigma of 0.04
 C42-C43 \\sim C43-C44 \\sim C44-C45
 with sigma of 0.02
 O4-C42 \\sim O4-C45
 with sigma of 0.02
 O4-C43 \\sim O4-C44
 with sigma of 0.04
 C43-C45 \\sim C42-C44
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C42, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H29C)=Sof(H29D)=Sof(H36C)=Sof(H36D)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(O4)=
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=
 Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(H36A)=Sof(H36B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(O3)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C39)=Sof(H39A)=
 Sof(H39B)=Sof(C41)=Sof(H41A)=Sof(H41B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C29(H29C,H29D), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C36(H36C,H36D), C36(H36A,H36B),
 C38(H38A,H38B), C40(H40A,H40B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              10205
_olex2_submission_special_instructions 'No special instructions were received'