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_7062249
_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         'C76 H84 K La N8 O5 S4 Si2'
_chemical_formula_sum            'C76 H84 K La N8 O5 S4 Si2'
_chemical_formula_weight         1551.94
_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                 96.461(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0298(9)
_cell_length_b                   17.5784(11)
_cell_length_c                   26.4091(16)
_cell_measurement_reflns_used    9368
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.48
_cell_measurement_theta_min      2.22
_cell_volume                     7394.2(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 0.999
_diffrn_measured_fraction_theta_max 0.971
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            99343
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.606
_diffrn_reflns_theta_min         1.897
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0937 before and 0.0658 after correction. The Ratio of minimum to maximum transmission is 0.9354. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       prism
_exptl_crystal_F_000             3216
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         20204
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0290P)^2^+3.3827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16942
_reflns_number_total             20204
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05540f2.cif
_cod_data_source_block           moa340
_cod_depositor_comments
'Adding full bibliography for 7062243--7062251.cif.'
_cod_database_code               7062249
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.851
_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
 C83-C82 = C71-C70 = C84-C83 = C72-C71 = C72-C69 = C84-C81
 1.5 with sigma of 0.02
 C73-C74 \\sim C74-C75 \\sim C75-C76
 with sigma of 0.02
 O2-C73 \\sim O2-C76
 with sigma of 0.02
 O2-C74 \\sim O2-C75
 with sigma of 0.04
 C74-C76 \\sim C73-C75
 with sigma of 0.04
 C77-C78 \\sim C78-C79 \\sim C79-C80
 with sigma of 0.02
 O1-C77 \\sim O1-C80
 with sigma of 0.02
 O1-C78 \\sim O1-C79
 with sigma of 0.04
 C78-C80 \\sim C77-C79
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O2 \\sim C73 \\sim C74 \\sim C75 \\sim C76: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O1 \\sim C77 \\sim C78 \\sim C79 \\sim C80: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O2, C73, C74, C75, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C77, C78, C79, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C81, C82, C83, C84
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O7, C69, C70, C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(C79)=
 Sof(H79A)=Sof(H79B)=Sof(C80)=Sof(H80B)=Sof(H80A)=1-FVAR(1)
 Sof(O2)=Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=
 Sof(H75A)=Sof(H75B)=Sof(C76)=Sof(H76A)=Sof(H76B)=FVAR(1)
 Sof(O7)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=
 Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=1-FVAR(2)
 Sof(O6)=Sof(C81)=Sof(H81A)=Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=
 Sof(H83A)=Sof(H83B)=Sof(C84)=Sof(H84A)=Sof(H84B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C57(H57A,H57B), 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),
  C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B),
 C80(H80B,H80A), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C12(H12), C18(H18),
 C19(H19), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29),
  C34(H34), C36(H36), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44),
 C45(H45), C46(H46), C49(H49), C50(H50), C51(H51), C53(H53), C55(H55), C56(H56),
  C58(H58)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              21065
_olex2_submission_special_instructions 'No special instructions were received'