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_7714291
_publ_section_title
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 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 Lu O6 Si3, 0.7[C4H8O]'
_chemical_formula_sum            'C72 H69 Lu O6 Si3'
_chemical_formula_weight         1289.51
_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
_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                90
_cell_angle_beta                 108.165(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.643(4)
_cell_length_b                   15.923(3)
_cell_length_c                   19.313(3)
_cell_measurement_reflns_used    5703
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      19.530
_cell_measurement_theta_min      2.220
_cell_volume                     6908(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker SMART APEX II diffractrometer'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II 300K'
_diffrn_measurement_method       '\f and \w 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  0.1799
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.568
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    1.528
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1050 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.5542.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.980
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         12164
_refine_ls_number_restraints     653
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0762
_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^)+(0.0700P)^2^+25.1990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6262
_reflns_number_total             12164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02519e2.cif
_cod_data_source_block           5
_cod_database_code               7714291
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.826
_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 = O5-C65 = O5-C65A = O5-C68 = O5-C68A =
 O6-C72A = O6-C69 = O6-C69A = O6-C72
 1.43 with sigma of 0.01
 C62-C61 = C62A-C61A = C63A-C62A = C63-C62 = C64A-C63A = C64-C63 = C66-C65 =
 C66A-C65A = C67A-C66A = C67-C66 = C68-C67 = C68A-C67A = C72-C71 = C71-C70 =
 C72A-C71A = C71A-C70A = C70A-C69A
 1.54 with sigma of 0.01
 C61A-C63A = C64A-C62A = C61-C63 = C64-C62 = C65-C67 = C68-C66 = C66A-C68A =
 C67A-C65A = C72-C70 = C69-C71 = C72A-C70A = C71A-C69A
 2.515 with sigma of 0.02
 C65A-C68A = C68-C65 = C64-C61 = C61A-C64A = C72-C69 = C72A-C69A
 2.336 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C61A \\sim C62A \\sim C63A \\sim C64A:
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 C68A \\sim C67A \\sim C66A \\sim C65A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C69 \\sim C70 \\sim C71 \\sim C69A \\sim C70A \\sim C71A \\sim C72A \\sim C72:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C52) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C60) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(C51) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C50) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C63A, C64A, O4, C62A, C61A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C71A, C70A, C69A, C72A, O6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C62, C61, O4, C63, C64
 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
 C66A, C65A, O5, C67A, C68A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C72, C71, C70, O6, C69
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C70A)=Sof(H70C)=Sof(H70D)=Sof(C71A)=
 Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)=1-FVAR(1)
 Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=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)=1-FVAR(2)
 Sof(C61A)=Sof(H61C)=Sof(H61D)=Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C63A)=
 Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64C)=Sof(H64D)=FVAR(2)
 Sof(C68A)=Sof(H68C)=Sof(H68D)=Sof(C67A)=Sof(H67C)=Sof(H67D)=Sof(C66A)=
 Sof(H66C)=Sof(H66D)=Sof(C65A)=Sof(H65C)=Sof(H65D)=1-FVAR(3)
 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(3)
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), C69A(H69C,H69D), C70A(H70C,
 H70D), C71A(H71C,H71D), C72A(H72C,H72D), C61A(H61C,H61D), C62A(H62C,H62D),
 C63A(H63C,H63D), C64A(H64C,H64D), C68A(H68C,H68D), C67A(H67C,H67D), C66A(H66C,
 H66D), C65A(H65C,H65D)
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)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 1104\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.7[C4H8O] per Asymmetric Unit 
which account for 112 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11348
_shelx_fab_checksum              28747
_olex2_submission_special_instructions 'No special instructions were received'