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_7062247
_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 La N8 S4 Si2, C16 H32 Li O4, 1(C7 H8)'
_chemical_formula_sum            'C79 H84 La Li N8 O4 S4 Si2'
_chemical_formula_weight         1539.81
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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
_cell_angle_beta                 96.833(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5473(11)
_cell_length_b                   21.5497(13)
_cell_length_c                   20.7855(15)
_cell_measurement_reflns_used    7517
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.19
_cell_volume                     7359.2(8)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0753
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41488
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         2.260
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1296 before and 0.0707 after correction.
The Ratio of minimum to maximum transmission is 0.8908.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     879
_refine_ls_number_reflns         12080
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+2.2405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8613
_reflns_number_total             12080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa318
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_database_code               7062247
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.841
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7S-C1S = C7T-C1T
 1.5 with sigma of 0.02
 C2S-C1S = C3S-C2S = C4S-C3S = C5S-C4S = C6S-C5S = C6S-C1S = C6T-C1T = C2T-C1T
 = C3T-C2T = C4T-C3T = C5T-C4T = C6T-C5T
 1.39 with sigma of 0.02
 C2S-C7S \\sim C6S-C2T \\sim C7T-C6T
 with sigma of 0.02
3. Restrained planarity
 C1S, C2S, C3S, C4S, C5S, C6S, C7S
 with sigma of 0.1
 C1T, C2T, C3T, C4T, C5T, C6T, C7T
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uiso(C1S) = Uiso(C2S) = Uiso(C3S) = Uiso(C4S) = Uiso(C5S) = Uiso(C6S) =
Uiso(C7S) = Uiso(C1T) = Uiso(C2T) = Uiso(C6T) = Uiso(C7T) = Uiso(C3T) =
Uiso(C5T) = Uiso(C4T)
5. Others
 Sof(C1T)=Sof(C2T)=Sof(H2T)=Sof(C3T)=Sof(H3T)=Sof(C4T)=Sof(H4T)=Sof(C5T)=
 Sof(H5T)=Sof(C6T)=Sof(H6T)=Sof(C7T)=Sof(H7TA)=Sof(H7TB)=Sof(H7TC)=1-FVAR(1)
 Sof(C1S)=Sof(C2S)=Sof(H2S)=Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=
 Sof(H5S)=Sof(C6S)=Sof(H6S)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C47(H47A,H47B), C50(H50A,H50B), C53(H53A,H53B), C54(H54A,
 H54B), C60(H60A,H60B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
 C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C9(H9), C10(H10), C12(H12), C14(H14), C15(H15), C19(H19),
 C20(H20), C23(H23), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C36(H36), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45),
 C46(H46), C49(H49), C51(H51), C56(H56), C57(H57), C58(H58), C59(H59), C61(H61),
  C62(H62), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C2T(H2T),
 C3T(H3T), C4T(H4T), C5T(H5T), C6T(H6T)
6.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C37(H37A,H37B,H37C), C42(H42A,H42B,H42C), C52(H52A,H52B,
 H52C), C7S(H7SA,H7SB,H7SC), C7T(H7TA,H7TB,H7TC)
;
_shelx_res_checksum              11864
_olex2_submission_special_instructions 'No special instructions were received'