Synthesis and photophysical properties of rare earth complexes bearing silanediamido ligands Me2Si(NAryl)22− (Aryl = Dipp, Mes)
Mironova, Olga A.; Lashchenko, Daniil I.; Ryadun, Aleksey A.; Sukhikh, Taisiya S.; Bashirov, Denis A.; Pushkarevsky, Nikolay A.; Konchenko, Sergey N.; New Journal of Chemistry 46 (2022) 2351–2359; doi:10.1039/D1NJ05722G

data_7061145
_publ_section_title
;
 Synthesis and photophysical properties of rare earth complexes bearing
 silanediamido ligands Me2Si(NAryl)22&#x2212; (Aryl = Dipp, Mes)
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2351
_journal_page_last               2359
_journal_paper_doi               10.1039/D1NJ05722G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C68 H112 Cl2 N4 O4 Si2 Tb2'
_chemical_formula_sum            'C68 H112 Cl2 N4 O4 Si2 Tb2'
_chemical_formula_weight         1494.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6405)
;
_audit_update_record
;
2021-11-19 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5890(3)
_cell_length_b                   17.5439(4)
_cell_length_c                   21.9363(4)
_cell_measurement_reflns_used    8547
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.45
_cell_volume                     7153.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24694
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.374
_diffrn_reflns_theta_min         2.156
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.116
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0528 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.8723.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7292
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+3.1397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5367
_reflns_number_total             7292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05722g2.cif
_cod_data_source_block           ss11
_cod_depositor_comments
'Adding full bibliography for 7061141--7061148.cif.'
_cod_database_code               7061145
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.609
_shelx_estimated_absorpt_t_min   0.551
_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. Rigid body (RIGU) restrains
 C28, C29B, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C29A, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29A)=Sof(H29B)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(H28A)=Sof(H28B)=Sof(H30A)=Sof(H30B)=Sof(C29A)=Sof(H29C)=Sof(H29D)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
4.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28C,H28D), C28(H28A,H28B), C29B(H29A,H29B), C30(H30C,
 H30D), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C29A(H29C,H29D)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              61584
_olex2_submission_special_instructions 'No special instructions were received'