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_7062246
_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_absolute_configuration ad
_chemical_formula_moiety         'C44 H54 Li2 N4 O4 S2 Si'
_chemical_formula_sum            'C44 H54 Li2 N4 O4 S2 Si'
_chemical_formula_weight         809.00
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            8
_cell_length_a                   14.2687(5)
_cell_length_b                   23.7559(9)
_cell_length_c                   25.5065(10)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.74
_cell_volume                     8645.8(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0726
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            90962
_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         25.685
_diffrn_reflns_theta_min         1.635
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0930 before and 0.0695 after correction. The Ratio of minimum to maximum transmission is 0.9474. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       prism
_exptl_crystal_F_000             3440
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.37(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1042
_refine_ls_number_reflns         16400
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+4.5490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1474
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13024
_reflns_number_total             16400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa391
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_database_code               7062246
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.967
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.63(12)
 0.37(12)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C33_1) \\sim Ueq, Uanis(C43_1) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C10_1, C13_1, C32_1, C33_1, C43_1, C34_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H19C)=Sof(H19D)=Sof(H25C)=Sof(H25D)=Sof(C44)=Sof(H44A)=Sof(H44B)=1-FVAR(1)
 Sof(H19A)=Sof(H19B)=Sof(H25A)=Sof(H25B)=Sof(C45)=Sof(H45A)=Sof(H45B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C16(H16A,H16B), C17(H17A,H17B), C19(H19C,H19D), C19(H19A,H19B),
 C20(H20A,H20B), C22(H22A,H22B), C25(H25C,H25D), C25(H25A,H25B), C27(H27A,H27B),
  C31(H31A,H31B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C40(H40A,
 H40B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B),
 C19(H19A,H19B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B)
6.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C18(H18), C21(H21), C23(H23),
 C24(H24), C26(H26), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
  C43(H43), C1(H1), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C15(H15), C17(H17), C18(H18), C20(H20), C33(H33), C35(H35), C37(H37), C38(H38),
  C39(H39)
6.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              48803
_olex2_submission_special_instructions 'No special instructions were received'