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_7062244
_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         'C36 H38 Cl2 Ho Li N4 O2 S2 Si, 0.5(C7 H8)'
_chemical_formula_sum            'C39.5 H42 Cl2 Ho Li N4 O2 S2 Si'
_chemical_formula_weight         939.75
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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                 92.411(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7223(5)
_cell_length_b                   39.088(2)
_cell_length_c                   11.8281(6)
_cell_measurement_reflns_used    4026
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.39
_cell_volume                     4029.1(4)
_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 0.995
_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  0.0865
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34357
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.101
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         2.327
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    2.269
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0873 before and 0.0693 after correction. The Ratio of minimum to maximum transmission is 0.8798. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       plate
_exptl_crystal_F_000             1892
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         7143
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0217P)^2^+10.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5455
_reflns_number_total             7143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa382
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_original_formula_sum        'C39.50 H42 Cl2 Ho Li N4 O2 S2 Si'
_cod_database_code               7062244
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.757
_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
 O2-C33 = O3-C44 = O3-C46 = O2-C35
 1.4 with sigma of 0.02
 C45-C44 = C34-C33 = C47-C45 = C36-C34 = C36-C35 = C47-C46
 1.45 with sigma of 0.02
 C38-C39 = C39-C40 = C40-C41 = C41-C42 = C42-C43 = C43-C38
 1.39 with sigma of 0.01
 C44-C35 = C33-C46
 2.35 with sigma of 0.04
 C38-C42 \\sim C38-C40 \\sim C43-C41 \\sim C39-C43 \\sim C40-C42 \\sim C39-C41
 with sigma of 0.04
 C37-C43 \\sim C37-C39
 with sigma of 0.04
3. Restrained planarity
 C37, C38, C39, C40, C41, C42, C43
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(C39) = Uiso(C40) = Uiso(C41) = Uiso(C42) = Uiso(C38) = Uiso(C43) =
Uiso(C37)
5. Rigid body (RIGU) restrains
 O2, C33, C34, C35, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C38, C39, C40, C41, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=1-FVAR(1)
 Sof(O2)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(1)
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) C39(0.5) H39(0.5)
 C40(0.5) H40(0.5) C41(0.5) H41(0.5) C42(0.5) H42(0.5) C43(0.5) H43(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C44(H44A,H44B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28), C29(H29),
  C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
7.c Idealised Me refined with riding coordinates:
 C37(H37A,H37B,H37C)
7.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              53413
_olex2_submission_special_instructions 'No special instructions were received'