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_7714549
_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         'C34 H50 N3 O Si Y'
_chemical_formula_sum            'C34 H50 N3 O Si Y'
_chemical_formula_weight         633.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                117.206(3)
_cell_angle_beta                 92.833(3)
_cell_angle_gamma                100.856(3)
_cell_formula_units_Z            6
_cell_length_a                   14.531(4)
_cell_length_b                   20.424(5)
_cell_length_c                   20.587(5)
_cell_measurement_reflns_used    7391
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      20.480
_cell_measurement_theta_min      2.265
_cell_volume                     5272(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.1448
_diffrn_reflns_av_unetI/netI     0.2028
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52223
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.154
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1126 before and 0.0602 after correction.
The Ratio of minimum to maximum transmission is 0.4305.
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    1.198
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         19585
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1958
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0382P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8372
_reflns_number_total             19585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03374k2.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
Adding full bibliography for 7714545--7714552.cif.

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C102 H150 N9 O3 Si3 Y3'
_cod_original_formula_weight         1901.30
_cod_original_formula_moiety         '3(C34 H50 N3 O Si Y)'
_cod_original_formula_units_Z            2
_cod_database_code               7714549
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.703
_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
C20B \\sim C21B \\sim C22B \\sim C24B \\sim C23B \\sim C19B: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C26) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26B) \\sim Ueq,
Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C25A(H25A), C25(H25), C28B(H28B), C28(H28), C25B(H25B), C28A(H28A)
3.b Secondary CH2 refined with riding coordinates:
 C9B(H9BA,H9BB), C10B(H10C,H10D), C13B(H13C,H13D), C12A(H12A,H12B), C12B(H12C,
 H12D), C9A(H9AA,H9AB), C33B(H33C,H33D), C10(H10E,H10F), C10A(H10A,H10B),
 C13A(H13A,H13B), C13(H13E,H13F), C33A(H33A,H33B), C33(H33E,H33F), C12(H12E,
 H12F), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C15A(H15A), C15B(H15B), C15(H15), C21B(H21B), C22B(H22B), C23B(H23B),
 C5A(H5A), C4A(H4A), C23A(H23A), C4B(H4B), C22A(H22A), C7B(H7B), C21(H21),
 C7A(H7A), C21A(H21A), C23(H23), C4(H4), C6A(H6A), C22(H22), C5B(H5B), C5(H5),
 C6B(H6B), C6(H6), C7(H7)
3.d Fitted hexagon refined as free rotating group:
 C19B(C20B,C21B,C22B,C23B,C24B)
3.e Idealised Me refined as rotating group:
 C17(H17G,H17H,H17I), C17B(H17D,H17E,H17F), C34B(H34D,H34E,H34F), C18(H18G,
 H18H,H18I), C18B(H18D,H18E,H18F), C18A(H18A,H18B,H18C), C17A(H17A,H17B,H17C),
 C11B(H11D,H11E,H11F), C34A(H34A,H34B,H34C), C27A(H27A,H27B,H27C), C32B(H32D,
 H32E,H32F), C31A(H31A,H31B,H31C), C26A(H26A,H26B,H26C), C31B(H31D,H31E,H31F),
 C11(H11G,H11H,H11I), C32A(H32A,H32B,H32C), C11A(H11A,H11B,H11C), C32(H32G,H32H,
 H32I), C27B(H27D,H27E,H27F), C31(H31G,H31H,H31I), C27(H27G,H27H,H27I),
 C29A(H29A,H29B,H29C), C26(H26G,H26H,H26I), C30(H30G,H30H,H30I), C29B(H29D,H29E,
 H29F), C30A(H30A,H30B,H30C), C29(H29G,H29H,H29I), C30B(H30D,H30E,H30F),
 C34(H34G,H34H,H34I), C26B(H26D,H26E,H26F)
;
_shelx_res_checksum              28541
_olex2_submission_special_instructions 'No special instructions were received'