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_7061148
_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         'C84 H144 Cl4 Li2 N4 O8 Si2 Y2, C4 H8 O'
_chemical_formula_sum            'C88 H152 Cl4 Li2 N4 O9 Si2 Y2'
_chemical_formula_weight         1799.81
_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             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                 95.133(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6828(18)
_cell_length_b                   18.077(2)
_cell_length_c                   21.843(3)
_cell_measurement_reflns_used    3070
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.61
_cell_measurement_theta_min      2.24
_cell_volume                     4987.8(11)
_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 7.41
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_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  0.1552
_diffrn_reflns_av_unetI/netI     0.1291
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44099
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.405
_diffrn_reflns_theta_max         24.405
_diffrn_reflns_theta_min         2.185
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1042 before and 0.0928 after correction.
The Ratio of minimum to maximum transmission is 0.8086.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     140
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+10.1691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4991
_reflns_number_total             8197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05722g2.cif
_cod_data_source_block           moa222a
_cod_depositor_comments
'Adding full bibliography for 7061141--7061148.cif.'
_cod_original_cell_volume        4987.7(12)
_cod_database_code               7061148
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.766
_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. Restrained distances
 C46-C43 = C43-C44 = C44-C45
 1.5 with sigma of 0.02
 O5-C46 = O5-C45
 1.42 with sigma of 0.02
 C34-C33 = C33-C32 = C32-C31
 1.5 with sigma of 0.02
 O3-C38 = O3-C37 = O3-C49 = O3-C28
 1.4 with sigma of 0.02
 C47-C38 = C37-C36 = C48-C47 = C36-C35 = C49-C48 = C35-C28
 1.5 with sigma of 0.02
 O5-C43 \\sim O5-C44
 with sigma of 0.04
 C43-C45 \\sim C46-C44
 with sigma of 0.04
 C38-C49 \\sim C28-C37
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim C46 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C33) \\sim Ueq, Uanis(C40) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uiso(C43) = Uiso(O5) = Uiso(C46) = Uiso(C45) = Uiso(C44)
Uiso(C35) = Uiso(C37) = Uiso(C36) = Uiso(C47) = Uiso(C38) = Uiso(C49) =
Uiso(C48) = Uiso(C28)
4. Rigid body (RIGU) restrains
 O5, C46, C43, C44, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C34, C33, C32, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C42, C41, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C27, C28A, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C27, C28B, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H27C)=Sof(H27D)=Sof(H29C)=Sof(H29D)=Sof(C28B)=Sof(H28A)=Sof(H28B)=1-FVAR(1)
 Sof(H27A)=Sof(H27B)=Sof(H29A)=Sof(H29B)=Sof(C28A)=Sof(H28C)=Sof(H28D)=FVAR(1)
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C49)=Sof(H49A)=
 Sof(H49B)=Sof(C48)=Sof(H48A)=Sof(H48B)=1-FVAR(2)
 Sof(C28)=Sof(H28E)=Sof(H28F)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C37)=Sof(H37A)=
 Sof(H37B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(2)
 Fixed Sof: O5(0.5) C46(0.5) H46A(0.5) H46B(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 C44(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5) H45B(0.5)
6.a Ternary CH refined with riding coordinates:
 C21(H21), C12(H12), C24(H24), C9(H9)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27C,H27D), C27(H27A,H27B), C30(H30A,H30B), C42(H42A,H42B), C41(H41A,
 H41B), C31(H31A,H31B), C29(H29C,H29D), C29(H29A,H29B), C39(H39A,H39B),
 C40(H40A,H40B), C32(H32A,H32B), C34(H34A,H34B), C28B(H28A,H28B), C33(H33A,
 H33B), C46(H46A,H46B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B),
 C28A(H28C,H28D), C28(H28E,H28F), C35(H35A,H35B), C37(H37A,H37B), C36(H36A,
 H36B), C47(H47A,H47B), C38(H38A,H38B), C49(H49A,H49B), C48(H48A,H48B)
6.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C5(H5), C7(H7), C17(H17), C18(H18), C6(H6)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C),
 C26(H26A,H26B,H26C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C25(H25A,H25B,
 H25C), C14(H14A,H14B,H14C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              99717
_olex2_submission_special_instructions 'No special instructions were received'