Tripodal tris(siloxide) Ligand Supported Trivalent Rare-earth Metal Complexes and Redox Reactivity
Guo, Hui; Hong, Dongjing; Cui, Peng; Dalton Transactions  (2023) –; doi:10.1039/D3DT02519E

data_7714293
_publ_section_title
;
 Tripodal tris(siloxide) Ligand Supported Trivalent Rare-earth Metal
 Complexes and Redox Reactivity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02519E
_journal_year                    2023
_chemical_formula_moiety         'C72 H69 O6 Si3 Y, 2[C7H8]'
_chemical_formula_sum            'C72 H69 O6 Si3 Y'
_chemical_formula_weight         1203.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-07-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-07-14 deposited with the CCDC.	2023-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                106.098(2)
_cell_angle_beta                 99.033(2)
_cell_angle_gamma                93.239(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3274(9)
_cell_length_b                   14.4251(11)
_cell_length_c                   24.4081(17)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      27.162
_cell_measurement_theta_min      2.632
_cell_volume                     3763.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker D8 Venture diffractrometer'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture 300K'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1660
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            141216
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.559
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0885 before and 0.0744 after correction.
The Ratio of minimum to maximum transmission is 0.7550.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13253
_refine_ls_number_restraints     452
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0660P)^2^+5.7240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8642
_reflns_number_total             13253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02519e2.cif
_cod_data_source_block           4
_cod_database_code               7714293
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C61A = O4-C61 = O4-C64 = O4-C64A
 1.43 with sigma of 0.01
 C64-C63 = C64A-C63A = C63-C62 = C63A-C62A = C62A-C61A = C62-C61
 1.54 with sigma of 0.01
 C66-C65 = C68A-C67A = C68-C67 = C67-C66 = C67A-C66A = C66A-C65A
 1.54 with sigma of 0.01
 O5-C68 = O5-C68A = O5-C65A = O5-C65
 1.43 with sigma of 0.01
 C62-C64 = C63-C61 = C61A-C63A = C62A-C64A
 2.515 with sigma of 0.02
 C64A-C61A = C61-C64
 2.336 with sigma of 0.02
 C65-C67 = C68-C66 = C68A-C66A = C65A-C67A
 2.515 with sigma of 0.02
 C65-C68 = C68A-C65A
 2.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C62 \\sim C63 \\sim C64 \\sim C62A \\sim C63A \\sim C64A \\sim C61 \\sim C61A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C65A \\sim C66A \\sim C67A \\sim C68A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C61)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C64, C63, C62, O4, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C64A, C63A, C62A, O4, C61A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C66A, C65A, O5, C67A, C68A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C66, C65, O5, C67, C68
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C61A)=Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C63A)=
 Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64C)=Sof(H64D)=1-FVAR(1)
 Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=
 Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)=FVAR(1)
 Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=
 Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=1-FVAR(2)
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(C68)=Sof(H68A)=Sof(H68B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 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), C61A(H61C,H61D), C62A(H62C,
 H62D), C63A(H63C,H63D), C64A(H64C,H64D), C65A(H65C,H65D), C66A(H66C,H66D),
 C67A(H67C,H67D), C68A(H68C,H68D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 186 electrons were 
found in a volume of 918\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C7H8] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              30954
_shelx_fab_checksum              32131
_olex2_submission_special_instructions 'No special instructions were received'