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_7714290
_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 H70 Ce O6 Si3'
_chemical_formula_sum            'C72 H70 Ce O6 Si3'
_chemical_formula_weight         1255.67
_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
_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                 92.3110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8866(11)
_cell_length_b                   18.9660(15)
_cell_length_c                   23.8269(18)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    300.00
_cell_measurement_theta_max      27.104
_cell_measurement_theta_min      2.312
_cell_volume                     6270.3(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker SMART APEX II 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 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.550
_diffrn_reflns_theta_min         1.373
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.835
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1066 before and 0.0481 after correction.
The Ratio of minimum to maximum transmission is 0.5418.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.098
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     956
_refine_ls_number_reflns         14379
_refine_ls_number_restraints     1262
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0499P)^2^+2.7111P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8684
_reflns_number_total             14379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02519e2.cif
_cod_data_source_block           7
_cod_database_code               7714290
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C68B-C67B = C67B-C66B = C66B-C65B = C62-C61 = C64-C61 = C63-C61 = C68A-C67A =
 C66-C65 = C67-C66 = C68-C67 = C67A-C66A = C66A-C65A = C64A-C61A = C63A-C61A =
 C62A-C61A
 1.54 with sigma of 0.01
 O5-C65A = O5-C65 = O5-C68A = O5-C68 = O4-C68B = O4-C65B
 1.43 with sigma of 0.01
 C68A-C66A = C65A-C67A = C68-C66 = C67-C65 = C66B-C68B = C67B-C65B
 2.515 with sigma of 0.02
 C62-C63 = C62-C64 = C63-C64
 2.515 with sigma of 0.02
 C68B-C65B = C68A-C65A = C68-C65
 2.36 with sigma of 0.02
 C62A-C63A = C62A-C64A = C63A-C64A
 2.515 with sigma of 0.02
 Si3-C55 \\sim Si3-C55A
 with sigma of 0.02
 Si3-C49A \\sim Si3-C49
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C49A \\sim C50A \\sim C51A \\sim C52A
\\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C57A \\sim C58A \\sim C59A
\\sim C60A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C69 \\sim C70 \\sim C71 \\sim C72 \\sim C69A \\sim C70A \\sim C71A \\sim C72A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C66B \\sim C68B \\sim C65B \\sim C67B:
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
\\sim C61A \\sim C64A \\sim C63A \\sim C62A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 O6, C69, C70, C71, C72, C69A, C70A, C71A, C72A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Si3, C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C49A, C50A,
 C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A, C60A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O4, C61, C62, C63, C64, C66B, C65B, C67B, C68B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O5, C65, C66, C67, C68, C65A, C66A, C67A, C68A, C61A, C64A, C63A, C62A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Same fragment restrains
{O6, C69A, C70A, C71A, C72A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{O6, C69, C70, C71, C72}
6. Others
 1*[Sof(C65)+Sof(H65A)+Sof(H65B)+Sof(C66)+Sof(H66A)+Sof(H66B)+Sof(C67)+
 Sof(H67A)+Sof(H67B)+Sof(C68)+Sof(H68A)+Sof(H68B)]+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*[Sof(C66B)+Sof(H66E)+Sof(H66F)+Sof(C68B)+
 Sof(H68E)+Sof(H68F)+Sof(C65B)+Sof(H65E)+Sof(H65F)+Sof(C67B)+Sof(H67E)+
 Sof(H67F)]=1 with esd of 0
 1*[Sof(C61)+Sof(C62)+Sof(H62A)+Sof(H62B)+Sof(H62C)+Sof(C63)+Sof(H63A)+
 Sof(H63B)+Sof(H63C)+Sof(C64)+Sof(H64A)+Sof(H64B)+Sof(H64C)]+1*[Sof(C61A)+
 Sof(C64A)+Sof(H64D)+Sof(H64E)+Sof(H64F)+Sof(C63A)+Sof(H63D)+Sof(H63E)+
 Sof(H63F)+Sof(C62A)+Sof(H62D)+Sof(H62E)+Sof(H62F)]=1 with esd of 0
 Sof(C49A)=Sof(C50A)=Sof(H50A)=Sof(C51A)=Sof(H51A)=Sof(C52A)=Sof(H52A)=
 Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)=Sof(C55A)=Sof(C60A)=Sof(H60A)=
 Sof(C59A)=Sof(H59A)=Sof(C58A)=Sof(H58A)=Sof(C57A)=Sof(H57A)=Sof(C56A)=
 Sof(H56A)=1-FVAR(1)
 Sof(C49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=Sof(C53)=
 Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(C60)=Sof(H60)=Sof(C59)=Sof(H59)=
 Sof(C58)=Sof(H58)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(H56)=FVAR(1)
 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(2)
 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(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(3)
 Sof(C65A)=Sof(H65C)=Sof(H65D)=Sof(C66A)=Sof(H66C)=Sof(H66D)=Sof(C67A)=
 Sof(H67C)=Sof(H67D)=Sof(C68A)=Sof(H68C)=Sof(H68D)=FVAR(4)
 Sof(C66B)=Sof(H66E)=Sof(H66F)=Sof(C68B)=Sof(H68E)=Sof(H68F)=Sof(C65B)=
 Sof(H65E)=Sof(H65F)=Sof(C67B)=Sof(H67E)=Sof(H67F)=FVAR(5)
 Sof(C61)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C63)=Sof(H63A)=Sof(H63B)=
 Sof(H63C)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(H64C)=FVAR(6)
 Sof(C61A)=Sof(C64A)=Sof(H64D)=Sof(H64E)=Sof(H64F)=Sof(C63A)=Sof(H63D)=
 Sof(H63E)=Sof(H63F)=Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=FVAR(7)
7.a Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,
 H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C65A(H65C,H65D),
 C66A(H66C,H66D), C67A(H67C,H67D), C68A(H68C,H68D), C69A(H69C,H69D), C70A(H70C,
 H70D), C71A(H71C,H71D), C72A(H72C,H72D), C66B(H66E,H66F), C68B(H68E,H68F),
 C65B(H65E,H65F), C67B(H67E,H67F)
7.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), C60(H60), C59(H59), C58(H58), C57(H57), C56(H56),
 C50A(H50A), C51A(H51A), C52A(H52A), C53A(H53A), C54A(H54A), C60A(H60A),
 C59A(H59A), C58A(H58A), C57A(H57A), C56A(H56A)
7.c Fitted hexagon refined as free rotating group:
 C49(C50,C51,C52,C53,C54), C55(C60,C59,C58,C57,C56), C49A(C50A,C51A,C52A,C53A,
 C54A), C55A(C60A,C59A,C58A,C57A,C56A)
7.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C64A(H64D,H64E,
 H64F), C63A(H63D,H63E,H63F), C62A(H62D,H62E,H62F)
;
_shelx_res_checksum              54701
_olex2_submission_special_instructions 'No special instructions were received'