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_7714288
_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         '0.5(C144 H138 Ce2 O12 Si6)'
_chemical_formula_sum            'C72 H69 Ce O6 Si3'
_chemical_formula_weight         1254.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 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                 119.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7971(13)
_cell_length_b                   18.7106(17)
_cell_length_c                   14.0466(13)
_cell_measurement_reflns_used    9765
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      27.265
_cell_measurement_theta_min      2.736
_cell_volume                     3171.3(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker D8 Venture 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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0945
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            120329
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         2.737
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1075 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.7953.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+3.1026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6364
_reflns_number_total             7514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02519e2.cif
_cod_data_source_block           2
_cod_database_code               7714288
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.855
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C64 = O4-C61
 1.43 with sigma of 0.01
 C64-C63 = C63-C62 = C62-C61
 1.54 with sigma of 0.01
 O5-C65 = O5-C68
 1.43 with sigma of 0.01
 C68-C67 = C67-C66 = C66-C65
 1.54 with sigma of 0.01
 C70-C69 = C71-C70 = C72-C71
 1.54 with sigma of 0.01
 O6-C72 = O6-C69
 1.43 with sigma of 0.01
 O4-C63
 2.426 with sigma of 0.02
 C64-C62 = C61-C63
 2.515 with sigma of 0.02
 O4-C62
 2.426 with sigma of 0.02
 C61-C64
 2.336 with sigma of 0.02
 C65-C68
 2.336 with sigma of 0.02
 O5-C66
 2.426 with sigma of 0.02
 C65-C67 = C68-C66
 2.515 with sigma of 0.02
 O5-C67
 2.426 with sigma of 0.02
 C69-C71 = C72-C70
 2.515 with sigma of 0.02
 C69-C72
 2.336 with sigma of 0.02
 O6-C71
 2.426 with sigma of 0.02
 O6-C70
 2.426 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C68 \\sim C67 \\sim C66 \\sim C65 \\sim C69 \\sim C72 \\sim C71 \\sim C70 \\sim
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C51 \\sim C52 \\sim C53: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
4. Others
 Fixed Sof: Si2(0.5) O2(0.5) O4(0.5) C1(0.5) C2(0.5) H2(0.5) C3(0.5) C4(0.5)
 H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5)
 C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5) C13(0.5) C14(0.5) H14(0.5)
 C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) H17(0.5) C18(0.5) H18(0.5)
 C19(0.5) C24(0.5) H24(0.5) C23(0.5) H23(0.5) C22(0.5) H22(0.5) C21(0.5)
 H21(0.5) C20(0.5) H20(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5)
 C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5) C31(0.5) C36(0.5) H36(0.5)
 C35(0.5) H35(0.5) C34(0.5) H34(0.5) C33(0.5) H33(0.5) C32(0.5) H32(0.5)
 C37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5)
 H41(0.5) C42(0.5) H42(0.5) C48(0.5) C47(0.5) H47(0.5) C46(0.5) H46(0.5)
 C45(0.5) H45(0.5) C44(0.5) H44(0.5) C43(0.5) C49(0.5) C50(0.5) H50(0.5)
 C51(0.5) H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5)
 C55(0.5) C56(0.5) H56(0.5) C57(0.5) H57(0.5) C58(0.5) H58(0.5) C59(0.5)
 H59(0.5) C60(0.5) H60(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) C64(0.5) H64A(0.5) H64B(0.5) O5(0.5)
 C65(0.5) H65A(0.5) H65B(0.5) C68(0.5) H68A(0.5) H68B(0.5) C66(0.5) H66A(0.5)
 H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5) O6(0.5) C69(0.5) H69A(0.5) H69B(0.5)
 C70(0.5) H70A(0.5) H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5) C72(0.5) H72A(0.5)
 H72B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,
 H65B), C68(H68A,H68B), C66(H66A,H66B), C67(H67A,H67B), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B)
5.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), C24(H24), C23(H23), C22(H22), C21(H21),
  C20(H20), C26(H26), C27(H27), C28(H28), C29(H29), C36(H36), C35(H35),
 C34(H34), C33(H33), C32(H32), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C47(H47), C46(H46), C45(H45), C44(H44), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
5.c Fitted hexagon refined as free rotating group:
 C7(C8,C9,C10,C11,C12), C13(C14,C15,C16,C17,C18), C19(C24,C23,C22,C21,C20),
 C25(C26,C27,C28,C29,C30), C31(C36,C35,C34,C33,C32), C37(C38,C39,C40,C41,C42),
 C48(C47,C46,C45,C44,C43), C49(C50,C51,C52,C53,C54), C55(C56,C57,C58,C59,C60)
;
_shelx_res_checksum              87664
_olex2_submission_special_instructions 'No special instructions were received'