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_7711417
_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 Y'
_chemical_formula_sum            'C31 H58 N3 O Si2 Y'
_chemical_formula_weight         633.89
_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.cc2c79rp
_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                 99.326(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.519(2)
_cell_length_b                   17.466(3)
_cell_length_c                   19.217(4)
_cell_measurement_reflns_used    7138
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.966
_cell_measurement_theta_min      2.259
_cell_volume                     3815.2(12)
_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 1.000
_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  0.1611
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27593
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.585
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.615
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6733
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0790P)^2^+4.8535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4398
_reflns_number_total             6733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02053j2.cif
_cod_data_source_block           2Y
_cod_database_code               7711417
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.718
_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
 C30A-Si2 = Si2-C31A
 1.9 with sigma of 0.02
 C30A-Si2 = Si2-C29
 1.9 with sigma of 0.02
 C31A-Si2 = Si2-C29
 1.9 with sigma of 0.02
 C25A-Si1 = Si1-C27A
 1.9 with sigma of 0.02
 C27A-Si1 = Si1-C26A
 1.9 with sigma of 0.02
 C26A-Si1 = Si1-C25A
 1.9 with sigma of 0.02
 C27A-Si1 = Si1-C24'
 1.9 with sigma of 0.02
 C25A-Si1 = Si1-C24'
 1.9 with sigma of 0.02
 C26A-Si1 = Si1-C24'
 1.9 with sigma of 0.02
 C30A-C31A
 3.103 with sigma of 0.04
 C30A-C29
 3.103 with sigma of 0.04
 C31A-C29
 3.103 with sigma of 0.04
 C25A-C27A
 3.103 with sigma of 0.04
 C27A-C26A
 3.103 with sigma of 0.04
 C26A-C25A
 3.103 with sigma of 0.04
 C27A-C24'
 3.103 with sigma of 0.04
 C25A-C24'
 3.103 with sigma of 0.04
 C26A-C24'
 3.103 with sigma of 0.04
 Si2-C30 \\sim Si2-C30A
 with sigma of 0.02
 Si2-C31 \\sim Si2-C31A
 with sigma of 0.02
 Si2-C0AA \\sim Si2-C29
 with sigma of 0.02
 Y1-C24' \\sim Y1-C24
 with sigma of 0.02
 Si1-C24' \\sim Si1-C24
 with sigma of 0.02
 C26-C24 \\sim C25-C24 \\sim C27-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C27A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C25A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C24') \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31A) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
4. Rigid body (RIGU) restrains
 Si2, C0AA, C30, C31, C29, C31A, C30A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Si1, C24, C27, C25, C26, C24', C27A, C25A, C26A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C24')=Sof(H24C)=
 Sof(H24D)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C25A)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C0AA)=
 Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C20(H20A,
 H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C24'(H24C,H24D)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C15(H15), C5(H5)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C3(H3A,H3B,H3C),
 C27(H27A,H27B,H27C), C11(H11A,H11B,H11C), C0AA(H0AA,H0AB,H0AC), C12(H12A,H12B,
 H12C), C30(H30A,H30B,H30C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C31(H31A,
 H31B,H31C), C29(H29A,H29B,H29C), C31A(H31D,H31E,H31F), C30A(H30D,H30E,H30F),
 C27A(H27D,H27E,H27F), C25A(H25D,H25E,H25F), C26A(H26D,H26E,H26F)
;
_olex2_submission_special_instructions 'No special instructions were received'