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_7062250
_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 Gd N8 S4 Si2, C24 H48 K O6, C4 H8 O'
_chemical_formula_sum            'C84 H100 Gd K N8 O7 S4 Si2'
_chemical_formula_weight         1714.48
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-31
_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                90.2130(10)
_cell_angle_beta                 91.5590(10)
_cell_angle_gamma                108.2600(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3738(3)
_cell_length_b                   18.5982(4)
_cell_length_c                   18.9764(5)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.93
_cell_measurement_theta_min      2.41
_cell_volume                     4145.26(17)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50322
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.103
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0667 before and 0.0585 after correction. The Ratio of minimum to maximum transmission is 0.9422. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_description       prism
_exptl_crystal_F_000             1782
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.063
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         18167
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.9206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14685
_reflns_number_total             18167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa351
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_database_code               7062250
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.860
_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
 O6-C85 = O5-C64 = O5-C79 = O6-C88
 1.45 with sigma of 0.02
 C82-C64 = C86-C85 = C87-C86 = C88-C87 = C82-C78 = C79-C78
 1.5 with sigma of 0.02
 O7-C80 = O7A-C80A = O7-C75 = O7A-C75A
 1.45 with sigma of 0.02
 C84-C80 = C84A-C80A = C84-C83 = C83-C75 = C84A-C83A = C83A-C75A
 1.5 with sigma of 0.02
 C79-C82 = C88-C86 = C64-C78 = C85-C87 = C82-C79
 2.35 with sigma of 0.02
 O6-C86 \\sim O6-C87
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O6 \\sim C85 \\sim C86 \\sim C87 \\sim C88: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O7) = Uanis(O7A)
4. Rigid body (RIGU) restrains
 O6, C85, C86, C87, C88
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C64, C78, C79, C82
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C75, C80, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7A, C75A, C80A, C83A, C84A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O6)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=Sof(C87)=
 Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=1-FVAR(1)
 Sof(O5)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C82)=Sof(H82A)=Sof(H82B)=FVAR(1)
 Sof(H58C)=Sof(H58D)=Sof(C74)=Sof(H74A)=Sof(H74B)=1-FVAR(2)
 Sof(H58A)=Sof(H58B)=Sof(C89)=Sof(H89A)=Sof(H89B)=FVAR(2)
 Sof(O7A)=Sof(C75A)=Sof(H75C)=Sof(H75D)=Sof(C80A)=Sof(H80C)=Sof(H80D)=
 Sof(C83A)=Sof(H83C)=Sof(H83D)=Sof(C84A)=Sof(H84C)=Sof(H84D)=1-FVAR(3)
 Sof(O7)=Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(C83)=
 Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=FVAR(3)
6.a Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C58(H58C,H58D), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,
 H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
  C70(H70A,H70B), C72(H72A,H72B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,
 H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C82(H82A,H82B),
 C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
  C88(H88A,H88B), C89(H89A,H89B), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,
 H3SB), C4S(H4SA,H4SB), C75A(H75C,H75D), C80A(H80C,H80D), C83A(H83C,H83D),
 C84A(H84C,H84D)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C17(H17),
 C18(H18), C19(H19), C21(H21), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41),
 C44(H44), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55),
  C57(H57)
6.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C43(H43A,H43B,H43C), C47(H47A,H47B,
 H47C)
;
_shelx_res_checksum              70646
_olex2_submission_special_instructions 'No special instructions were received'