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_7714546
_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         'C36 H52 Gd N3 O Si'
_chemical_formula_sum            'C36 H52 Gd N3 O Si'
_chemical_formula_weight         728.14
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_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                 93.4440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8562(12)
_cell_length_b                   20.653(2)
_cell_length_c                   14.1698(13)
_cell_measurement_reflns_used    9939
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      24.661
_cell_measurement_theta_min      2.206
_cell_volume                     3755.6(6)
_computing_cell_refinement       '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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.703
_diffrn_reflns_theta_min         1.745
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.826
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0978 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.6246.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0342P)^2^+1.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6008
_reflns_number_total             8723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03374k2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7714545--7714552.cif.'
_cod_database_code               7714546
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.689
_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. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10), C27(H27), C30(H30)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C33(H33A,H33B), C15(H15A,H15B), C9(H9A,H9B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C4(H4), C5(H5), C7(H7), C6(H6), C23(H23), C25(H25), C24(H24)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C31(H31A,H31B,H31C), C35(H35A,H35B,
 H35C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C28(H28A,H28B,H28C), C34(H34A,
 H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              9955
_olex2_submission_special_instructions 'No special instructions were received'