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_7061147
_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 Sm2'
_chemical_formula_sum            'C68 H112 Cl2 N4 O4 Si2 Sm2'
_chemical_formula_weight         1477.39
_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             2021-11-04
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_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                   18.671(3)
_cell_length_b                   17.547(2)
_cell_length_c                   21.967(3)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.17
_cell_measurement_theta_min      2.44
_cell_volume                     7196.8(17)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_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                 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 0.999
_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  0.1006
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.151
_diffrn_source                   'Incoatec IuS3.0 microfocus X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.769
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1068 before and 0.0944 after correction.
The Ratio of minimum to maximum transmission is 0.5753.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             3064
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.455
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6832
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0511P)^2^+43.2899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4874
_reflns_number_total             6832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05722g2.cif
_cod_data_source_block           moa223
_cod_depositor_comments
'Adding full bibliography for 7061141--7061148.cif.'
_cod_original_cell_volume        7197.0(17)
_cod_database_code               7061147
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.796
_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. Uiso/Uaniso restraints and constraints
Uanis(C33B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C32, C34, C33B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C34, C33A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H32C)=Sof(H32D)=Sof(H34C)=Sof(H34D)=Sof(C33A)=Sof(H33C)=Sof(H33D)=1-FVAR(1)
 Sof(H32A)=Sof(H32B)=Sof(H34A)=Sof(H34B)=Sof(C33B)=Sof(H33A)=Sof(H33B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12), C21(H21), C24(H24)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32C,H32D), C32(H32A,H32B), C34(H34C,H34D), C34(H34A,H34B),
 C33B(H33A,H33B), C33A(H33C,H33D)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19)
5.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              8551
_olex2_submission_special_instructions 'No special instructions were received'