Synthesis and catalytic activity of tetradentate β-diketiminato rare-earth metal monoalkyl complexes in tandem Oppenauer oxidation and cross-aldol condensation.
Zou, Haiyan; Wang, Ziqian; Guo, Dianjun; Zhang, Lijun; Wang, Shaowu; Zhu, Xiancui; Dalton transactions (Cambridge, England : 2003) 53 (2023) 267–275; doi:10.1039/d3dt03374k

data_7714551
_publ_section_title
;
 Synthesis and catalytic activity of tetradentate &#x3b2;-diketiminato
 rare-earth metal monoalkyl complexes in tandem Oppenauer oxidation and
 cross-aldol condensation.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              267
_journal_page_last               275
_journal_paper_doi               10.1039/d3dt03374k
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         '2(C34 H50 N3 O Si Yb)'
_chemical_formula_sum            'C68 H100 N6 O2 Si2 Yb2'
_chemical_formula_weight         1435.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-08-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-22 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.797(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.46(5)
_cell_length_b                   23.07(3)
_cell_length_c                   23.60(3)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      23.933
_cell_measurement_theta_min      2.247
_cell_volume                     14833(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81118
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.730
_diffrn_reflns_theta_min         1.157
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1198 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.6060. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       block
_exptl_crystal_F_000             5872
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         16820
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0504P)^2^+6.4998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10334
_reflns_number_total             16820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03374k2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7714545--7714552.cif.'
_cod_original_cell_volume        14828(33)
_cod_database_code               7714551
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.626
_shelx_estimated_absorpt_t_min   0.601
_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
 Si2A-C33A \\sim Si2-C33A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si2) \\sim Ueq, Uanis(C33A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C34A)
\\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C67A) \\sim Ueq,
Uanis(C66A) \\sim Ueq, Uanis(Si2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C10A) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Si2, Si2A, C31A, C66A, C32A, C67A, C34A, C68A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(Si2A)=Sof(H31C)=Sof(H31D)=Sof(C66A)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C67A)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C68A)=Sof(H68A)=Sof(H68B)=
 Sof(H68C)=1-FVAR(1)
 Sof(Si2)=Sof(H33C)=Sof(H33D)=Sof(C31A)=Sof(H31F)=Sof(H31G)=Sof(H31H)=
 Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34A)=Sof(H34D)=Sof(H34E)=
 Sof(H34F)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C25A(H25A), C28A(H28A)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C33(H33A,H33B),
 C9A(H9AA,H9AB), C10A(H10C,H10D), C12A(H12C,H12D), C13A(H13C,H13D), C33A(H33C,
 H33D), C33A(H31C,H31D)
6.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C15(H15), C21(H21), C22(H22), C23(H23),
 C4A(H4A), C5A(H5A), C6A(H6A), C7A(H7A), C15A(H15A), C23A(H23A), C22A(H22A),
 C21A(H21A)
6.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31E), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C11A(H11D,H11E,H11F),
 C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F), C27A(H27D,H27E,H27F), C26A(H26D,
 H26E,H26F), C30A(H30D,H30E,H30F), C29A(H29D,H29E,H29F), C31A(H31F,H31G,H31H),
 C66A(H66A,H66B,H66C), C32A(H32D,H32E,H32F), C67A(H67A,H67B,H67C), C34A(H34D,
 H34E,H34F), C68A(H68A,H68B,H68C)
;
_shelx_res_checksum              33112
_shelx_fab_checksum              28410
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'