Synthesis of rare-earth metal complexes with a morpholine-functionalized β-diketiminato ligand and their catalytic activities towards C-O and C-N bond formation.
Zhu, Xiancui; He, Jinqiang; Yang, Yuanqing; Zhou, Shuangliu; Wei, Yun; Wang, Shaowu; Dalton transactions (Cambridge, England : 2003) 51 (2022) 13227–13235; doi:10.1039/d2dt02053j

data_7711418
_publ_section_title
;
 Synthesis of rare-earth metal complexes with a morpholine-functionalized
 \b-diketiminato ligand and their catalytic activities towards C-O and C-N
 bond formation.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13227
_journal_page_last               13235
_journal_paper_doi               10.1039/d2dt02053j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C31 H58 N3 O Si2 Yb'
_chemical_formula_sum            'C31 H58 N3 O Si2 Yb'
_chemical_formula_weight         718.02
_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_block_doi                 10.5517/ccdc.csd.cc2c79sq
_audit_creation_date             2021-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-06-25 deposited with the CCDC.	2022-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5135(6)
_cell_length_b                   17.4563(10)
_cell_length_c                   19.1193(10)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.547
_cell_measurement_theta_min      2.232
_cell_volume                     3794.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33002
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.589
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.551
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1215 before and 0.0441 after correction. The Ratio of minimum to maximum transmission is 0.5071. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8678
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0334P)^2^+1.7162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6220
_reflns_number_total             8678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           2Yb
_cod_database_code               7711418
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.629
_shelx_estimated_absorpt_t_min   0.604
_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
 C26A-Si1 = Si1-C27A
 1.9 with sigma of 0.02
 C26A-Si1 = Si1-C25A
 1.9 with sigma of 0.02
 C25A-Si1 = Si1-C27A
 1.9 with sigma of 0.02
 C31A-Si2 = Si2-C29A
 1.9 with sigma of 0.02
 C29A-Si2 = Si2-C30A
 1.9 with sigma of 0.02
 C31A-Si2 = Si2-C30A
 1.9 with sigma of 0.02
 C26A-C27A
 3.103 with sigma of 0.04
 C26A-C25A
 3.103 with sigma of 0.04
 C25A-C27A
 3.103 with sigma of 0.04
 C31A-C29A
 3.103 with sigma of 0.04
 C29A-C30A
 3.103 with sigma of 0.04
 C31A-C30A
 3.103 with sigma of 0.04
 Si1-C26 \\sim Si1-C26A
 with sigma of 0.02
 Si1-C27 \\sim Si1-C27A
 with sigma of 0.02
 Si1-C25 \\sim Si1-C25A
 with sigma of 0.02
 Yb1-C28 \\sim Yb1-C28'
 with sigma of 0.02
 Si2-C28 \\sim Si2-C28'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C27)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C29) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C28') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C30A) \\sim Ueq, Uanis(C29A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 Si1, C25, C26, C27, C25A, C26A, C27A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si2, C28, C30, C31, C29, C28', C29A, C30A, C31A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28')=Sof(H28C)=
 Sof(H28D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=
 Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C19(H19A,H19B), C18(H18A,H18B), C28(H28A,H28B), C28'(H28C,H28D)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C5(H5), C7(H7), C6(H6)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C1(H1A,H1B,H1C),
 C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C12(H12A,H12B,H12C), C11(H11A,H11B,
 H11C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C29(H29A,
 H29B,H29C), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F)
;
_olex2_submission_special_instructions 'No special instructions were received'